A method for producing carbon black using an extender fluid

© Agent (s): CABINET WEINSTEIN.

© PROCESS FOR PRODUCING CARBON BLACK USING A CHARGE FLUID.

The present invention relates to processes for the production of carbon black using feed fluid (s) as well as to methods for controlling one or more properties of carbon black particles using feed fluids and to 'other techniques.

FR 3 003 263 - A1

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BACKGROUND OF THE INVENTION

The present invention relates to carbon black and methods for making carbon black. In addition, the present invention relates to the control of one or more properties of carbon black particles.

In the manufacture of carbon black, changes in carbon black processing controls and / or apparatus configurations are typically necessary when a production line is adapted to manufacture different grades of carbon black, or to accommodate different types. raw material, and these changes interfere with the continuous and / or efficient operation of the production line. Effective operational adjustments to modify the properties of the particles can be used when a change in a particle property (eg, structure or surface) of carbon black, is desired for production reasons. These adjustments cause a process disruption of the carbon black reactor, which may even include shutdown, and the ejection nozzles used to introduce the raw material to form the carbon black are replaced to change the jet dynamics or fluid that can adjust tint or other properties. Obviously, shutting down the reactor and modifying the nozzles can be time consuming and expensive.

In addition, in the production of carbon black, some raw materials may be more problematic than others, for example the use of coal tar raw materials and the resulting rate of nozzle tip wear. This may also be true for other raw materials which are considered to be raw materials with higher amounts of small particles, such as ash, which may be problematic in making carbon blacks and / or may be problematic with the use of small tip sizes for the points of introduction of raw materials due to the risk of clogging. In fact, peak clogging can be caused by particles that can come from raw material, coking, potassium, water, among others. In the context of the present invention, the terms “ejection nozzle” or “nozzle” or “tip” refer to the same component.

In addition, it would be desirable to improve the processes for the production of carbon black by using a preheated raw material as described in International Patent Application No. WO 2011/103015. In this previous process, a preheated raw material is used to obtain beneficial properties with respect to carbon black and on an industrial scale. It would be beneficial to improve this process to obtain even more efficiency.

Accordingly, it would be beneficial to describe methods for producing carbon black which can achieve one or more of the objects mentioned above.

SUMMARY OF THE PRESENT INVENTION

Accordingly, it is an object of the present invention to describe methods for controlling at least one property of carbon black particle without any process disturbance or shutdown of the carbon black reactor.

Another object of the present invention is to describe a method for controlling at least one property of carbon black particle without requiring any change of nozzles at points of introduction for the raw material.

Another object of the present invention is to describe the ability to further increase raw material preheating temperatures in the production of carbon black with control of thermally induced fouling of raw material lines at raw material temperatures. increased.

An additional object of the present invention is to describe a process for producing carbon black using raw materials with high amounts of particles, such as ash.

Additional objects and advantages of the present invention are described in part in the description given below, and will become apparent in part on reading the description, or may be deduced by practice of the present invention. The objectives and other advantages of the present invention will appear and will be achieved by means of the elements and combinations particularly described in the description.

To achieve these and other advantages and in the context of the present invention, as generally carried out and described herein, the present invention relates, in part, to a process for producing carbon black. The method includes introducing a heated gas stream into a carbon black reactor. The method further comprises combining at least one feed fluid with at least one carbon black raw material to form a fluid-raw material mixture. The combination is preferably such that the at least one feed fluid increases the momentum of the at least one carbon black raw material in a direction which is substantially axial (within 10 degrees of an axial direction ) or axial with respect to at least one point of introduction of raw material into the carbon black reactor. The fluid-raw material mixture is supplied to at least one point of introduction of raw material (preferably several) in the carbon black reactor. The method further comprises combining at least the fluid-raw material mixture through one or more points of introduction into the carbon black reactor with the heated gas stream to form a reaction stream. , carbon black being formed in the carbon black reactor. The process may further include recovering carbon black from the reaction stream. In this process, the feed fluid may be chemically inert and is preferably chemically inert to the carbon black raw material.

Instead of or in addition to combining at least one feed fluid with at least one carbon black raw material to form a fluid-raw material mixture, the fluid-raw material mixture can be generated in the reactor. . In other words, the at least one feed fluid can be introduced into the reactor and the at least one raw material can be introduced into the reactor such that the points of introduction for each of them are arranged so that the charge fluid increases the momentum of the raw material in the combustion stream.

The present invention further comprises a method for controlling at least one property of a carbon black particle, such as structure and / or surface. The method comprises combining at least one feed fluid with at least one carbon black raw material to form a fluid-raw material mixture and feeding the fluid-raw material mixture into a carbon black reactor. . The feed of the fluid-raw material mixture is in the form of one or more jets. The method further includes controlling the amount of feed fluid present in the fluid-raw material mixture to control at least one particle property, such as hue. Other particle properties may be surface area (e.g., as measured by BET (Brunauer-Emmett Method for Surface Area), CTAB (Cetyltrimethyl Ammonium Bromide, Test Method for Measuring Specific Surface Area), and / or STSA (statistical surface area of ​​thickness, a method for measuring an external surface area) (ASTM D6556)), or structure such as OAN (oil absorption number) or DBF (Dibutyl phthalate absorption).

In the methods of the present invention, the carbon black raw material can be, or include raw materials with high particle levels of 0.01 wt% to 0.5 wt%, based on the weight of raw material, such as ash, since the methods of the present invention allow to work with these types of raw materials without the side effects described above.

In more detail, the present invention comprises the various characteristics below:

It relates to a process for producing carbon black comprising:

introducing a heated gas stream into a carbon black reactor;

combining at least one charge fluid with at least one carbon black raw material to form a fluid-raw material mixture such that the at least one charge fluid increases the momentum of the at least a carbon black raw material in a direction which is axial or substantially axial with respect to at least one point of introduction of raw material into the carbon black reactor;

supplying said fluid-raw material mixture to said at least one point of introduction of raw material into the carbon black reactor, combining at least said mixture of raw material fluid via the at least one point of introduction to said carbon black reactor with the heated gas stream to form a reaction stream in which carbon black is formed in said carbon black reactor; and recovering carbon black from the reaction stream.

The feed fluid is chemically inert to the carbon black raw material.

The charge fluid is uniformly distributed in said carbon black raw material.

The feed of the fluid-raw material mixture is in the form of one or more jets, and the one or more jets of the fluid-raw material mixture contain sufficient charge fluid to propel the carbon black raw material through. an inner part of the heated gas stream.

The charge fluid is at least one inert gas.

The feed fluid is water vapor, water, air, carbon dioxide, natural gas, carbon monoxide, hydrogen, carbon black waste gas, nitrogen, or any combinations of these.

The charge fluid is nitrogen.

The feed fluid is introduced into said carbon black raw material at a pressure sufficient to penetrate said carbon black raw material to form said fluid-raw material mixture.

The feed fluid is introduced into said carbon black raw material at a pressure of from about 6.9 Pa to about 2415 Pa to form said mixture of raw material fluid.

The carbon black raw material is atomized prior to said combination with said feed fluid.

The amount of said feed fluid which is combined with said carbon black raw material is adjustable during the continuous production of carbon black.

The feed of the fluid-raw material mixture is in the form of one or more jets and the jet penetration of the fluid-raw material mixture into said heated gas stream is adjusted by changing the feed fluid content of the mixture. fluid-raw material during the continuous production of carbon black.

The feed fluid is at least partially distributed in said carbon black raw material.

The feed fluid is present in said fluid-raw material mixture in an amount of from about 0.1 wt% to about 400 wt%, based on the weight of the carbon black raw material.

The method further comprises heating said carbon black raw material prior to combining with said feed fluid to form said fluid-raw material mixture.

The method further comprises heating said carbon black raw material to a temperature of greater than about 300 ° C prior to combining with said feed fluid to form said raw material fluid mixture.

The method further comprises heating said carbon black raw material to a temperature of from about 360 ° C to about 850 ° C prior to combining with said feed fluid to form said raw material fluid mixture.

The method further comprises heating said carbon black raw material to a first temperature of from about 300 ° C to about 850 ° C prior to combining with said feed fluid to form said fluid-raw material mixture, and then heating said fluid-raw material mixture to a second temperature which is higher than said first temperature, wherein each of said heating steps occurs prior to introduction into said carbon black reactor.

The method further comprises heating said carbon black raw material to a first temperature of from about 400 ° C to about 600 ° C prior to combining with said feed fluid to form said fluid-raw material mixture, and then heating said fluid-raw material mixture to a second temperature which is higher than said first temperature by at least 50 ° C, wherein each of said heating steps occurs prior to introduction into said carbon black reactor.

The method further comprises heating said carbon black raw material to a first temperature of about 400 ° C to about 60 0 ° C before combining with said feed fluid to form said fluid-raw material mixture, and then heating said fluid-raw material mixture to a second temperature which is higher than said first temperature by at least 100 ° C, wherein each of said heating steps occurs prior to introduction into said carbon black reactor.

The method further comprises heating said carbon black raw material to a first temperature prior to combining with said feed fluid to form said fluid-raw material mixture, and then heating said raw material fluid mixture to a second. temperature which is higher than said first temperature and up to about 950 ° C, wherein each of said heating steps occurs prior to introduction into said carbon black reactor.

Depending on the method, feed fluid adjustments are made to control the reduced flow velocity or the critical velocity, or both, of the one or more jets of the fluid-raw material mixture, so as to modify the penetration of the fluid-feed mixture. raw material in the heated gas stream.

According to another embodiment, the method for controlling at least one particle property of a carbon black comprises:

combining at least one feed fluid with at least one carbon black raw material to form a fluid-raw material mixture and supplying said fluid-raw material mixture to a carbon black reactor; and wherein said feed of the fluid-raw material mixture is in the form of one or more jets and controlling the amount of feed fluid present in said fluid-raw material mixture to control said at least one particle property.

According to this process:

Said at least one particle property is tint.

The feed fluid is chemically inert to the carbon black raw material.

The charge fluid is uniformly distributed in said carbon black raw material.

The feed of the fluid-raw material mixture is in the form of one or more jets, and the one or more jets of the fluid-raw material mixture contain sufficient charge fluid to propel the carbon black raw material through. an inner part of the heated gas stream.

The charge fluid is at least one inert gas.

The feed fluid is water vapor, water, air, carbon dioxide, natural gas, carbon monoxide, hydrogen, carbon black waste gas, nitrogen, or any combinations of these.

The charge fluid is nitrogen.

The feed fluid is introduced into said carbon black raw material at a pressure sufficient to penetrate said carbon black raw material to form said fluid-raw material mixture.

The feed fluid is introduced into said carbon black raw material at a pressure of from about 6.9 Pa to about 2415 Pa to form said mixture of raw material fluid.

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The amount of said feed fluid which is combined with said carbon black raw material is adjustable while said process produces carbon black.

The amount of said feed fluid which is combined with said carbon black raw material is adjustable during the continuous production of carbon black.

The feed of the fluid-raw material mixture is in the form of one or more jets and the jet penetration of the fluid-raw material mixture into said heated gas stream is adjusted by changing the feed fluid content of the mixture. of fluid-raw material during the continuous production of carbon black.

The feed fluid is present in said fluid-raw material mixture in an amount of from about 0.1 wt% to about 400 wt%, based on the weight of the carbon black raw material.

The feed fluid is present in said fluid-raw material mixture in an amount of from about 0.1% by weight to about 50% by weight, based on the weight of the carbon black raw material.

The method further comprises heating said carbon black raw material prior to combining with said feed fluid to form said fluid-raw material mixture.

The method further comprises heating said carbon black raw material to a temperature of greater than about 300 ° C prior to combining with said feed fluid to form said raw material fluid mixture.

The method further comprises heating said carbon black raw material to a temperature of from about 360 ° C to about 850 ° C prior to combining with said feed fluid to form said raw material fluid mixture.

The method further comprises heating said carbon black raw material to a first temperature of from about 300 ° C to about 850 ° C prior to combining with said feed fluid to form said fluid-raw material mixture, and then heating said fluid-raw material mixture to a second temperature which is higher than said first temperature, wherein each of said heating steps occurs prior to introduction into said carbon black reactor.

The method further comprises heating said carbon black raw material to a first temperature of from about 400 ° C to about 600 ° C prior to combining with said feed fluid to form said fluid-raw material mixture, and then heating said fluid-raw material mixture to a second temperature which is higher than said first temperature by at least 50 ° C, wherein each of said heating steps occurs prior to introduction into said carbon black reactor.

The method further comprises heating said carbon black raw material to a first temperature of from about 400 ° C to about 600 ° C before combining with said feed fluid to form said fluid-raw material mixture, and then heating said fluid-raw material mixture to a second temperature which is higher than said first temperature by at least 100 ° C where each of said heating steps occurs prior to introduction into said carbon black reactor.

The method further comprises heating said carbon black raw material to a first temperature prior to combining with said feed fluid to form said fluid-raw material mixture, and then heating said raw material fluid mixture to a second temperature. which is higher than said first temperature and up to about 950 ° C, wherein each of said heating steps occurs before introduction to said carbon black reactor.

The jet penetration is controlled by the feed fluid affecting the reduced flow velocity or the critical velocity or both of the one or more jets of the fluid-raw material mixture.

The invention also relates to a process for producing carbon black comprising:

introducing a heated gas stream into a carbon black reactor;

feeding at least one carbon black raw material to at least one point of introduction of raw material into the carbon black reactor;

supplying at least one feed fluid to at least one point of introduction into the carbon black reactor wherein the at least one point of introduction for the feed fluid is located so that the less one feed fluid increases the momentum of the at least one carbon black raw material when the carbon black raw material reaches the heated gas stream;

combining said at least one carbon black raw material and said at least one feed fluid, with the heated gas stream to form a reaction stream in which carbon black is formed in said carbon black reactor; and recovering carbon black from the reaction stream.

According to this process: The feed fluid is inert to the carbon black raw material.

The charge fluid is distributed in said carbon black raw material.

The feed of the carbon black raw material and the feed of the feed fluid is in the form of one or more jets, each jet having a central hollow tip with an annular sheath which introduces said feed fluid.

The feed of the carbon black raw material and the feed of the feed fluid is in the form of a pair of one or more mutually adjacent jets, wherein one jet in each pair feeds said carbon black raw material. carbon and the other jet in each pair feeds said charge fluid.

The feed fluid is introduced at a pressure sufficient to penetrate into said carbon black raw material.

This method further comprises heating said carbon black raw material to a temperature of more than about 300 ° C before feeding to said at least one point of introduction.

This method further comprises heating said carbon black raw material to a temperature of from about 360 ° C to about 80 ° C before feeding to said at least one point of introduction.

The invention relates to yet another method for controlling at least one property of a particle of a carbon black comprising:

separately feeding a) at least one feed fluid adjacent to b) at least one carbon black feedstock to a carbon black reactor and wherein said feed of a) and b) is in the form of one or more jets, and controlling the amount of charge fluid present to control said at least one particle property.

According to this method, said at least one particle property is hue.

Generally, the method further comprises heating said feed fluid to a first temperature prior to combining with said carbon black raw material to form said fluid-raw material mixture.

This method further comprises heating said carbon black raw material to a first temperature prior to combining with said charge fluid and heating said charge fluid to a second temperature prior to combining with said carbon black raw material, and then combining to form said fluid-raw material mixture, and then heating said mixture of first fluid material to a third temperature which is higher than said first temperature and up to about 950 ° C, where each of said heating steps occurs prior to introduction into said carbon black reactor.

Said at least one particle property is the surface.

Said carbon black raw material is atomized prior to said combination with said feed fluid.

The method further comprises heating said carbon black raw material to a temperature of greater than about 300 ° C prior to combining with said feed fluid to form said raw material fluid mixture, and wherein said black raw material of carbon is atomized prior to said combination with said charge fluid.

Said filler fluid is present in said fluid-raw material mixture in an amount of from about 0.1 wt% to about 50 wt%, based on the weight of the carbon black raw material.

It should be understood that the above general description and the following detailed description are exemplary and explanatory only and are intended to give a further explanation of the present invention.

The accompanying drawings, which are incorporated into and form a part of the present application, illustrate aspects of the present invention and together with the description, serve to explain the principles of the present invention. Similar digital identifiers used in the figures denote similar items.

BRIEF DESCRIPTION OF THE DRAWINGS

Figures 1 to 5 are diagrams of part of different types of furnace carbon black reactors which may be used in a process of the present invention to produce carbon black. This carbon black reactor is only illustrative of reactors which can be used in the present invention.

FIG. 6 is a diagram of an example of the injector which shows the injection of the feed fluid into an atomized raw material before entering the carbon black reactor and the primary fire.

- Figures 7 and 8 are drawings showing options for introducing the feed fluid and the raw material without pre-mixing before entering the reactor, having an annular design and a side-by-side design.

DETAILED DESCRIPTION OF THE PRESENT INVENTION

The present invention relates to methods for producing carbon black. The present invention further relates to methods for controlling at least one property of a carbon black particle. In addition, the present invention relates to the ability to use raw materials with high amounts of particles without blocking any of the points of introduction into the reactor. In addition, the present invention relates to methods for further increasing raw material preheating temperatures in carbon black production with control of thermally induced fouling of raw material lines at increased raw material temperatures.

In the manufacture of carbon black, a fuel is burned to generate a hot gas stream which flows at high velocity through a transition zone where a carbon black raw material is introduced and mixed with the hot gas stream. . Mixing continues at high speed in a hot reactor where the raw material undergoes pyrolysis to obtain carbon black particles, the reaction is then quenched, the reactants are cooled, and the carbon black product is collected on a filter.

In general, one aspect of the present invention relates to the production of carbon black by combining at least one feed fluid with at least one carbon black raw material before the introduction of the raw material (or after the introduction. raw material) into the reactor via one or more points of introduction. With the use of a charge fluid, described in more detail below, the charge fluid (s) has the ability to provide various benefits, including one or more of the following: the ability to work with different types of carbon black raw materials including what are considered to be raw materials with high amounts of particulate matter (e.g. ash), such as coal tar raw materials for the manufacture of carbon black; the ability to preheat a raw material producing carbon black to an even higher temperature than those previously described; the ability to control one or more properties of carbon black particles; the ability to use lower pressures for feedstock introduction; and / or other benefits.

The charge fluid can be a gas or a liquid. Preferred examples are gases. The feed fluid may be chemically inert to the carbon black raw material and is preferably chemically inert to the carbon black raw material. The charge fluid can be at least one inert gas (eg, argon, neon, helium, and the like). The charge fluid can be nitrogen alone or with other gases. The feed fluid can be water vapor, water, air, carbon dioxide, carbon monoxide, hydrogen, carbon black waste gas, natural gas, or nitrogen , one or more inert gases, or any combinations thereof. In general, the gas or liquid has a purity of at least 95% by weight (eg, at least 97%, at least 98%, at least 99%, at least 99.5%, or at least 99.9 % by weight) of gas or liquid. For example, when nitrogen is used (alone or with other gases / liquids), the nitrogen gas has a purity of at least 95% by weight of that gas.

The feed fluid, when combined with at least one carbon black raw material to form a fluid-raw material mixture, may optionally be evenly distributed in the carbon black raw material. The combination of the feed fluid (s) with at least one carbon black raw material results in a fluid-raw material mixture in which the feed fluid is distributed (uniformly or non-uniformly) in the black raw material. of carbon.

Before the feed fluid is combined with the carbon black raw material, the carbon black raw material can be atomized or at least partially atomized. The feed fluid is optionally not used as a means for atomizing the carbon black raw material in the present invention. The charging fluid preferably provides the momentum to the carbon black raw material after being combined with the carbon black raw material. The term "momentum" refers to the momentum as understood in fluid mechanics. Optionally, the feed fluid after being combined with the carbon black raw material produces the momentum to form a columnar jet of the fluid-raw material mixture as the mixture exits the nozzle and enters the black reactor. carbon. The charge fluid has the ability to channel the momentum of the raw material. The raw material fluid mixture is channeled into the injector so that the forward momentum of the fluid-material mixture initially entering the reactor continues in an axial direction with respect to the central axis of the injector (or substantially axial relative to the central axis of the injector, for example plus or minus 10 degrees from the axial position relative to the central axis). The fluid-raw material mixture is then projected so that it is preferably perpendicular (or substantially perpendicular, that is to say plus or minus 10 degrees) with respect to the primary fire or combustion flow, and / or is preferably perpendicular (or substantially perpendicular, ie plus or minus 10 degrees) to the wall of the carbon black reactor. Optionally, the fluid-raw material mixture or the injector used to inject the fluid-raw material mixture can be at any angle to the primary fire or combustion flow (eg, perpendicular (90 degrees), substantially perpendicular (80 to 110 degrees), or other angles (such as 20 to 79 degrees, 2 0 degrees, 3 0 degrees, 4 0 degrees, 45 degrees, 5 0 degrees, 5 5 degrees, 6 0 degrees, 6 5 degrees , 75 degrees and the like)). An example of the combination of the feed fluid and the carbon black raw material is depicted in Fig. 6. In Fig. 6, the carbon black raw material 100 enters a port 102 and exits the port as a. Atomized carbon black raw material 104. A feed fluid 106 is introduced through port 108 and is combined with atomized carbon black raw material 104 to form a raw material fluid 110 mixture. The mixture 110 has an increased momentum relative to the momentum that existed before the introduction of the charge fluid. This mixture 110 exits the injector through a nozzle or orifice 112 in the wall of the reactor 117 in the form of a columnar jet of fluid-raw material mixture with a high momentum (114) which then enters the reactor. high speed combustion flow or primary fire 116. Therefore, preferably, in the present invention, combining the at least one charge fluid with at least one carbon black raw material to form a fluid-raw material mixture is such that the at least one charge fluid increases the momentum of the au minus one carbon black raw material in a direction which is axial or substantially axial with respect to at least one point of introduction of raw material into the carbon black reactor.

The amount of charging fluid (s) which is combined with the carbon black raw material is adjustable. The amount of charge fluid which is combined with the carbon black raw material can be adjustable while the process is online and produces carbon black. In other words, the amount of charge fluid can be changed "on the fly". Therefore, since the amount of charge fluid can be combined with the carbon black raw material in an adjustable manner, it can be done without stopping the reactor. Therefore, the continuous production of carbon black can be maintained even when the reactor conditions are adjusted to achieve different grades of carbon black, or to optimize a quality of carbon black being manufactured, or adjust / change the quality of carbon black. carbon black being manufactured and / or other adjustments that are made to the process / reactor during the manufacture of carbon black.

Generally, the filler fluid can be introduced into the carbon black raw material at any pressure, but generally high pressures are preferred to achieve the desired mixture of the filler fluid with the carbon black raw material, especially when the charge fluid is a gas. Suitable pressures can be about 1 lb / inch² (6.9 Pa) at approximately 350 lbs / inch² (2415 Pa), or about 50 lbs / inch² (345 Pa) at approximately 175 lbs / inch² (1207 Pa), or about 20 lbs / inch² (138 Pa) at approximately 200 lbs / inch² (1380 Pa) or more, or about 100 lbs / inch² (690 Pa) at about 200 lbs / inch² (1380 Pa) or more.

These and other pressures can be used to introduce the feed fluid into the carbon black raw material. The pressure may be sufficient to penetrate the carbon black raw material to form the fluid-raw material mixture and preferably such that the charge fluid is evenly distributed throughout the carbon black raw material.

Any amounts of feed fluid can be present in the fluid-raw material mixture. For example, the feed fluid may be present in the fluid-raw material mixture in an amount of from about 0.1 percent by weight to about 400 percent by weight (or more), based on the weight of the batch. raw material of carbon black. Other amounts include, for example, from about 0.1 percent by weight to about 100 percent by weight or more, based on the weight of the carbon black raw material or from about 5 percent by weight. to about 15 percent by weight, based on the weight of the carbon black raw material, or about 0.1 percent by weight to about 50 percent by weight, based on the weight of the raw material carbon black, or from about 1 percent by weight to about 40 percent by weight, based on the weight of the carbon black raw material.

The feed of the fluid-raw material mixture may be in the form of one or more jets. The type of charge fluid and / or the amount of charge fluid is able to adjust the penetration of the jet of fluid-raw material mixture into the heated gas stream. As indicated above, with the use of a fluid-raw material mixture, which is delivered in the form of one or more jets, the amount of charge fluid and / or the type of charge fluid allow to adjust the penetration of the jet of fluid-raw material mixture into the heated gas stream without any change of nozzle and / or without the need to interrupt the process or to shut down the carbon black reactor.

Optionally, the feed fluid can be combined with the carbon black raw material at a point which is before the point of introduction of the raw material fluid mixture into the carbon black reactor. The fluid may be introduced such that the fluid and the raw material are mixed together before exiting the injector / nozzle. The charge fluid can be combined with the carbon black raw material at a point which is at a distance greater or less than 0.5 inch (1.27 cm), such as at least 0.75 inch (1.905 cm), at least 1 inch (2.54 cm), at least 2 inches (5.08 cm), at least 4 inches (10.16 cm), or at least 6 inches (15.24 cm) before the point introduction into the reactor.

Optionally, the feed fluid can be combined with the carbon black raw material after their respective introductions to the carbon black reactor. In other words, the feed fluid can be introduced into the carbon black reactor separately from the carbon black raw material. Any geometry to achieve the separate introduction of feed fluid and carbon black raw material into the reactor such that the two fluids are mutually adjacent or come into contact with each other in the reactor can be used. For example, as depicted in Figures 7 and 8, the introduction of the feed fluid and the carbon black raw material separately can be done with a pipeline which has an annular hollow design so that one of the fluids surrounds the line. other fluid. Another geometry that can be used is to place the points of introduction for the feed fluid and the carbon black raw material side by side. In this design, one of the entry points may be slightly in front of the other, for example, half an inch (1.27 cm) or an inch (2.54 cm) or more. When the charge fluid and the carbon black raw material are separately introduced into the reactor, the geometry is such that the charge fluid comes into contact with the carbon black raw material fluid, and the charge fluid increases the pressure. amount of movement of the raw material in the combustion flow (or cross flow). There is no limitation as to the geometry that can be used to achieve this separate dual introduction of the feed fluid and the carbon black raw material. Again, one or more points of introduction can be used, for example around the circumference of the reactor, for example at the neck section.

For each point of introduction of carbon black raw material, there may be a pre-combination of the feed fluid with the carbon black raw material before the introduction of the raw material into the carbon black reactor and / or a respective feed fluid entry point for each existing carbon black raw material feed point.

The way in which the fluid-raw material mixture is introduced into the carbon black reactor, for example at the process transition point, can be implemented in the form of one or more jets or ejection nozzles, or in combination with or alternatively with one or more lances. When ejection nozzles are used, these are typically located at a radial position around the circumference of the reactor, for example as depicted in Figure 1. When a lance is used, the position is typically more in the axial center of the reactor location.

In the present invention, for any process, the raw material producing carbon black may be or include any liquid hydrocarbon having a density of from about 0.9 to about 1.5 or more (eg, from 0.9 to. 1,3, or 1 to 1,2 and the like) or any combination thereof. The carbon black-producing raw material may have an initial boiling point of about 160 ° C to about 600 ° C, for example, 160 ° C to about 500 ° C or 20 ° C to about 450 ° C. or 215 ° C to about 400 ° C and the like. The carbon black producing raw material can be any conventional carbon black producing raw material which results in the formation of carbon black. For example, any hydrocarbon material can be used. A suitable raw material can be any hydrocarbon raw material producing any carbon black which is readily volatilizable under the conditions of the reaction. For example, unsaturated hydrocarbons such as acetylene; olefins such as ethylene, propylene, butylene; aromatics such as benzene, toluene and xylene; certain saturated hydrocarbons; and other hydrocarbons such as kerosines, naphthalenes, terpenes, ethylenic tars, aromatic ring raw materials and the like can be used.

The carbon black producing raw material which can be processed using the present invention can generally include any hydrocarbon liquid or oily raw materials useful for the production of carbon black. Suitable liquid raw materials include, for example, unsaturated hydrocarbons, saturated hydrocarbons, olefins, aromatics, and other hydrocarbons such as kerosines, naphthalenes, terpenes, ethylene tars, coal tars, cracking residues, and aromatic ring raw materials, or any combination thereof. The raw materials can be, for example, decanted oil, a coal tar product, ethylene cracking residue, an oil containing asphaltene, or any combinations thereof. The type of raw material can affect the fouling behavior. Chemistries can vary between different types of raw material and / or within one type of raw material. Based on experience and laboratory tests, decanted oil, coker oil, coal tars, and ethylene cracking tailings, for example, all can foul at different temperatures above about 300 ° C. Ethylene cracking residues (ECRs), for example, can be relatively high in asphaltenes. Other types of raw material may also contain asphaltenes and / or have chemistries subject to other fouling mechanisms.

The asphaltene content of the raw material can be, for example, 0% to about 30% by weight, or at least about 0.5% by weight, or at least about 1% by weight, or at least about 2%. by weight, or at least about 3% by weight, or from about 1% to about 10% by weight, or from about 2% to about 7.5% by weight, or from about 2.5% to about 5% by weight, based on the total weight of raw material. The raw material may have an initial boiling point, for example, from about 160 ° C to about 500 ° C, or from about 180 ° C to about 450 ° C, or from about 200 ° C to about 400 ° C, or from 225 ° C to about 350 ° C. The initial boiling point refers to the temperature at which the first component of raw material (of the raw material) evaporates. The raw material may have an intermediate boiling point, for example, from about 380 ° C to about 800 ° C, or from about 400 ° C to about 500 ° C, or from about 425 ° C. C to about 475 ° C, or 440 ° C to about 460 ° C. Intermediate boiling point refers to the temperature at which 50% of the raw material components have evaporated. The raw material may have a final boiling point, for example, from about 600 ° C to about 900 ° C, or from about 625 ° C to about 725 ° C, or from about 650 ° C to about 700 ° C, or from 670 ° C to about 690 ° C. The final boiling point refers to the temperature at which 100% of the raw material components have evaporated. Other initial, intermediate and / or final boiling points may apply, depending on the choice and the chemistry of the raw material.

The methods of the present invention can be used with furnace black reactors with adaptations and modifications as described herein. The processes of the present invention can be practiced, for example, in a modular furnace black reactor, also called "staged". Staged furnace reactors which can be adapted or modified to practice the present invention are described, for example, in US Patents No. 3,922,335; 4,383,973; 5,190,739; 5,877,250; 5,904,762; 6,153,684; 6,156,837; 6,403,695; and 6,485,693 B1.

Regarding the hot gas stream (or heated gas stream) which is combined with the raw material producing carbon black, the hot gas stream can also be considered as hot flue gas or heated gas stream. , which can be generated by contacting a solid, liquid, and / or gaseous fuel with a suitable oxidant flow such as, but not limited to, air, oxygen, air mixtures and oxygen, or the like. Alternatively, a preheated oxidant stream can be passed without adding liquid or gaseous fuel. Examples of fuels suitable for use in contacting the oxidant stream to generate the hot gases include any of the readily combustible gas, vapor or liquid streams, such as natural gas, hydrogen, monoxide. of carbon, methane, acetylene, alcohol, recycled waste gas, or kerosene. Generally, it is preferred to use fuels having a high content of carbon-containing components and in particular, hydrocarbons. The ratio of air to fuel used to produce the carbon black of the present invention can be from about 0.7: 1 to infinity, or about 1: 1 (stoichiometric ratio) to infinity. In order to facilitate the generation of hot gases, the oxidant stream can be preheated. Essentially, the heated gas stream is generated by ignition or combustion of the fuel and / or the oxidant. Temperatures such as from about 1000 degrees C to about 3500 degrees C for the heated gas stream can be achieved.

With the present invention, the jet penetration of the raw material can be adjusted by the charging fluid. For example, the feed fluid has the ability to affect the reduced flow velocity or the critical velocity or both of one or more jets of the fluid-raw material mixture which is in the form of a jet stream. when it is introduced through one or more points of introduction into the reactor. The greater the amount of charge fluid, the lower the flow rate of the mixture or the critical rate of the mixture (where reduced flow rate and critical speed denote the speed of sound for that mixture), and therefore, the greater the penetration of the jet into the heated gas stream is high.

Another advantage of the present invention is the ability to increase the overall yield of carbon black using a charging fluid. With the present invention, more carbon black can be made using the same amount of raw material fluid. For example, the yield can be increased by at least 1%, at least 2%, or at least 5%, the yield in% is based on the weight percentage of carbon black. Yields can be further increased by using optional preheating (as described herein) of the feed fluid, carbon black feedstock, or both.

Another advantage of the present invention relates to the ability to use large orifice or nozzle sizes. In some carbon black manufacturing processes, large orifice or nozzle sizes are used due to the particles present in the carbon black raw material. Large nozzle sizes are used to avoid nozzle clogging due to particles present. However, if large nozzle sizes are used, it can prevent sufficient or correct penetration of the fluid raw material into the heated gas combustion stream due to the reduced pressure and velocity of the raw material. However, with the present invention, the use of filler fluid allows the amount of movement of the raw material fluid to be increased, even from large nozzle sizes, so that the penetration is achieved at the same level as with larger nozzle sizes. small nozzle sizes to achieve the desired carbon black formation.

Optionally, the carbon black raw material which is mixed with the charge fluid can be heated before being combined with the charge fluid. In other words, the carbon black raw material can be preheated. The preheating of the raw material and the techniques used can be as described in international publication No. WO 2011/103015.

In the present invention, optionally, the raw material of carbon black, before being combined with the charging fluid can be heated to a temperature above 300 ° C or from about 360 ° C to about 850 ° C or above. , or about 400 ° C to about 600 ° C or other temperatures.

In the present invention, optionally, the feed fluid, before being combined with the carbon black raw material can be heated to a temperature of at least 100 ° C, at least 300 ° C, or at least 500 ° C, or at least 750 ° C, or at least 1000 ° C, or at least 1200 ° C, or other temperatures.

In the present invention, optionally, the feed fluid and the carbon black raw material, before being combined together, can each be separately preheated to the same or different preheating temperatures. The preheating temperatures can be the ranges described above, i.e. they can be heated to a temperature of over 300 ° C or from about 360 ° C to about 850 ° C or more, or from about 400 ° C to about 600 ° C for the carbon black raw material, and / or a temperature of at least 100 ° C, at least 300 ° C, or at least 500 ° C, or at least 750 ° C, or at least 1 0 0 0 ° C, or at least 1 2 0 0 ° C, or other temperatures for the charge fluid. In another variant, the fluid-raw material mixture can optionally be heated, to a higher temperature, with or without preheating the carbon black raw material and / or the feed fluid.

Optionally, the carbon black raw material can be heated to a first temperature such as a temperature of at least 300 ° C, for example 300 ° C to about 850 ° C, before combining with the feed fluid to form a fluid-raw material mixture and then the fluid-raw material mixture can be heated further to a second temperature which is higher than the temperature of the preheated carbon black raw material alone before being combined with the charging fluid. This heating of the fluid-raw material mixture to a higher temperature may be at least 50 ° C higher than the preheated raw material, for example at least 75 ° C higher or at least 100 ° C higher. and the like. Optionally, the carbon black raw material can be heated or preheated to a first temperature before being combined with the feed fluid to form the fluid-raw material mixture and can then be heated to a second temperature which is greater than the first temperature, for example up to about 950 ° C.

The method can include inactivating carbon black in the reaction stream. Carbon black in the reaction stream can be inactivated in one or more zones. For example, in Figure 2, at an inactivation location 18 of the inactivation zone 14, an inactivation fluid is injected, which may include water, and which can be used to completely or almost completely shut down pyrolysis of the raw material producing carbon black, or only partially cooling the raw material without stopping the pyrolysis followed by a secondary inactivation (not shown) used to stop the pyrolysis of the raw material producing carbon black. Other post-inactivation steps which are conventional in the manufacture of carbon black can be used in the methods of the present invention. After the mixture of hot flue gases and carbon black producing raw material has been inactivated, the cooled gases pass downstream into conventional cooling and separation means so that the carbon black is recovered. The separation of carbon black from the gas stream is easily accomplished by conventional means such as a precipitator, cyclone separator or filter bag. With respect to the complete inactivation of the reactions to form the final carbon black product, any conventional means for inactivating the reaction downstream of the introduction of the second carbon black producing raw material can be used and are known. of the skilled person. For example, an inactivation fluid can be injected which can be water or other fluids suitable for stopping the chemical reaction.

As described above and in detail hereinafter, a method may include introducing a heated gas stream into a carbon black reactor. The method optionally further comprises feeding at least one carbon black producing raw material having a first temperature below the preheat temperature to be reached, such as less than 300 ° C or less than 275 ° C ( for example, 40 ° C to 274 ° C, 50 ° C to 270 ° C, 70 ° C to 250 ° C, 60 ° C to 200 ° C, 70 ° C to 150 ° C, and the like ) in at least one heater (for example, at least two heaters, at least three heaters, and the like, the heaters may be the same or different from each other). The at least one feed fluid may be combined with the carbon black producing raw material at any point before and / or after the introduction of the carbon black producing raw material into the reactor. Ideally, greater benefit is obtained when the feed fluid is mixed or combined prior to introduction into the reactor. This can be done just before the point of introduction or at any point after the heater stage presently described for preheating or before the heater stage. The temperature of the raw material entering the at least one heater is below the target preheating temperature or temperature range. The raw material before being preheated can move, optionally, at a first speed of at least about 0.2 m / s (e.g. at least about 0.4 m / s, at least about 0.6 m / s, at least about 0.8 m / s, at least about 1 m / s, at least about 1.1 m / s, at least about 1.6 m / s, for example 0.2 m / s at 4 m / s, from 1.1 to 3 m / s and similar). Other speeds can be used provided that the other processing conditions are chosen so as to control fouling and / or coking in the heater (s) and the feed line to the reactor.

The method may include preheating the at least one carbon black producing raw material in the at least one heater to a second temperature of greater than about 300 ° C (eg, at least 350 ° C, at least 360 ° C, at least 400 ° C, at least 450 ° C, at least 500 ° C, for example from 300 ° C to 850 ° C, or from 360 ° C to 800 ° C, from 400 ° C to 750 ° C, 450 ° C to 700 ° C and the like) to obtain a raw material producing preheated carbon black, where (a) the at least one carbon black-producing raw material has a velocity in the at least one heater which is at least 0.2 m / s, the velocity being calculated on the basis of the raw material density measured at 60 ° C at 1 atm and based on the smallest cross-sectional area of ​​a line of raw material present in the at least one heater. Since it can be very difficult to measure the speed of a raw material at such a high temperature, in the context of the present invention, the speed as specified herein is based on these specific measurement conditions. Regardless of the smallest diameter or smallest cross-sectional area present in the actual heater, this minimum cross-sectional area is used to determine velocity as described herein in the context of the present invention. Many heaters have the same diameter throughout the heater, but in the event that multiple diameters or cross-sectional areas are present in the heater (s), this condition prevails. The speed is based on the minimum cross-sectional area. The actual speed throughout the raw material heater can generally be greater than the speed measured at 60 ° C at 1 atm.

In the process, the carbon black-producing raw material can have a first raw material residence time in the heater of less than about 120 minutes (eg, less than 100 minutes, less than 80 minutes, less than 60 minutes , less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, for example 1 second to 119 minutes, 5 seconds to 115 minutes, 10 seconds to 110 minutes, 30 seconds to 100 minutes , from 1 minute to 60 minutes, from 5 minutes to 30 minutes, and the like).

The method may include feeding the preheated carbon black-producing feedstock (optionally pre-combined with feedstock fluid) to at least one point of feedstock introduction into the carbon black reactor (e.g., at least one or two or three or four points of introduction of raw materials), wherein the preheated carbon black producing raw material has a second raw material residence time measured from the outlet of the heater (s) to the point just before the point of introduction into the carbon black reactor of less than about 120 minutes (for example, less than 100 minutes, less than 80 minutes, less than 60 minutes, less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, for example 1 second to 119 minutes , 5 seconds to 115 minutes, 10 seconds to 110 minutes, 30 seconds to 100 minutes, 1 minute to 60 minutes, 5 minutes to 30 minutes, and the like). The first raw material residence time and the second raw material residence time combined are preferably 120 minutes or less (e.g., less than 100 minutes, less minutes, less than 60 minutes, less than 40 minutes, less 30 minutes, less than 20 minutes, less than 10 minutes, for example 1 second to 119 minutes, 5 seconds to 115 minutes, 10 seconds to 110 minutes, 30 seconds to 100 minutes, 1 minute to 60 minutes , from 5 minutes to 30 minutes, and similar). For example, with reference to the figures, the second raw material residence time would be, for example, the time at which the raw material exits from the heater 19 in figure 2 or from the heater 22 in figure 3 at point d introduction into the reactor, described as point of introduction 16 in Figure 2 and Figure 3. The combination of the first raw material residence time and the second raw material residence time would be the total raw material residence time.

Optionally, if the raw material line to the heater has approximately the same cross section as the feed line passing through the heater, the carbon black producing raw material may have a velocity in the device (s) ( s) heating that is approximately the same or more (e.g. at least 1% higher, at least 2% higher, at least 3% higher, at least 5% higher, at least 7% higher, at least 10% higher, at least 100% higher, at least 200% higher, for example 1% to 200% higher or 20% to 100% higher and the like) than the first gear at the input of the heating device (s).

The process of the present invention may include pressurizing the carbon black producing raw material (s). The method may include pressurizing or using pressure for the carbon black-producing feedstock (s) so that preheating the carbon black-producing feedstock prevents formation. of vapor film in the at least one heater or before feeding to the carbon black reactor. The process of the present invention may include pressurizing the carbon black producing raw material (s) so as to achieve a pressure of, for example, more than about 10 bar before entry. in the at least one heater which preheats the raw material producing carbon black. This pressure can be at least 15 bars, at least 20 bars, at least 30 bars, at least 40 bars, for example from 10 bars to 180 bars or more, from 15 bars to 150 bars, from 20 bars to 125 bars , from 25 bars to 100 bars (these pressure values ​​can be converted into Pa by multiplying them by 10⁵) .

In the present invention, a process for producing carbon black may include introducing a heated gas stream into a carbon black reactor. The method further comprises feeding a raw material producing carbon black having a first temperature lower than the target raw material preheating temperature, such as less than 300 ° C or less than 275 ° C (e.g., 40 ° C to 274 ° C, from 50 ° C to 270 ° C, from 70 ° C to 250 ° C, from 60 ° C to 200 ° C, from 70 ° C to 150 ° C, and similar) to (x) device (s) for heating to a first pressure of more than 10 bar. This pressure can be at least 15 bars, at least 20 bars, at least 30 bars, at least 40 bars, for example from 10 bars to 180 bars or more, from 15 bars to 150 bars, from 20 bars to 125 bars , from 25 bars to 100 bars (values ​​can be converted into Pascal by multiplying them by 10⁵) .

The method may include preheating the at least one carbon black producing raw material in the heater (s) (eg, at least two heaters, at least three heaters, and the like. , where the heaters may be the same or different from each other) at a second temperature of more than about 300 ° C (e.g. at least 350 ° C, at least 360 ° C, at least 400 ° C, at least 450 ° C, at least 500 ° C, for example from 300 ° C to 850 ° C, or from 360 ° C to 800 ° C, from 400 ° C to

750 ° C, from 450 ° C to 700 ° C and the like) to obtain a preheated carbon black-producing raw material, where (a) the carbon black-producing raw material has a second pressure in the at least one heating that is approximately the same or less (for example, at least 1% lower, at least 2% lower, at least 3% lower, at least 5% lower, at least 7% lower, at least 10 % lower, at least 15% lower, at least 20% lower, e.g. 1% to 75% lower or 3% to 20% lower and the like) than the first pressing and (b) the raw material producing carbon black has a first time of raw material stay in the heater less than about 120 minutes (for example, less than 100 minutes, less than 80 minutes, less than 60 minutes, less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, e.g. 1 second to 119 minutes, 5 seconds to 115 minutes, 10 seconds to 110 minutes, 30 seconds to 100 minutes, 1 minute to 60 minutes, 5 minutes to 30 minutes, and the like).

As previously indicated, in any of the processes described herein or previously or hereinafter, the at least one feed fluid may be combined or mixed with the carbon black producing raw material preheated to any point (prior to preheating, during preheating, and / or after preheating, and / or before and / or after introduction into the carbon black reactor).

The process may include feeding the preheated carbon black-producing raw material to at least one feedstock feed point in the carbon black reactor, where the preheated carbon black-producing raw material has a second stage. of raw material stay from the outlet of the at least one heater to the point of introduction into the carbon black reactor less than about

120 minutes (for example, less than 100 minutes, less than 80 minutes, less than 60 minutes, less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, for example 1 second to 119 minutes, 5 seconds to 115 minutes, 10 seconds to 110 minutes, 30 seconds to 100 minutes, 1 minute to 60 minutes, 5 minutes to 30 minutes, and the like); and where the combined first raw material residence time and second raw material residence time are 120 minutes or less (e.g., less than 100 minutes, less than 80 minutes, less than 60 minutes, less than 40 minutes, less than 30 minutes, less than 20 minutes, less than 10 minutes, for example 1 second to 119 minutes, 5 seconds to 115 minutes, 10 seconds to 110 minutes, 30 seconds to 100 minutes, 1 minute to 60 minutes, from 5 minutes to 30 minutes, and similar).

The present invention may relate to a process for producing carbon black which comprises introducing a heated gas stream into a carbon black reactor. The method further comprises supplying at least one carbon black producing raw material having a first temperature which is lower than the target raw material preheating temperature, such as less than 300 ° C or less than 275 ° C. (for example, 40 ° C to 274 ° C, 50 ° C to 270 ° C, 70 ° C to 250 ° C, 60 ° C to 200 ° C, 70 ° C to 150 ° C, and similar) in at least one heater (e.g. at least two heaters, at least three heaters, and the like, the heaters possibly being the same or different from each other) at a first pressure of more than 10 bars (10x10⁵ Pa). Optionally, the speed of entry into the heater may be a first speed of at least about 0.2 m / s (e.g., at least about 0.4 m / s, at least about 0.6 m / s s, at least about 0.8 m / s, at least about 1 m / s, at least about 1.1 m / s, at least about 1.6 m / s, for example from 0.2 m / s to 2 m / s, from 0.4 to 1.8 m / s and the like).

The method comprises preheating the carbon black producing raw material in the heater (s) to a second temperature of greater than about 300 ° C (eg, at least 350 ° C, at least 360 ° C). ° C, at least 400 ° C, at least 450 ° C, at least 500 ° C, for example from 300 ° C to 850 ° C, or from 360 ° C to 800 ° C, from 400 ° C to 750 ° C , from 450 ° C to 700 ° C and the like) to obtain a raw material producing preheated carbon black, where (a) the raw material producing carbon black has a velocity in the heater (s) which is at least 0.2 m / s, the velocity being calculated on the basis of a mass volume of raw material measured at 60 ° C at 1 atm and the smallest cross-sectional area of ​​a row of raw material present in the at least one heater, and (b) wherein the at least one carbon black producing raw material has a second pressure in the heater (s) that is approximately the same or less (eg, at least 1% lower, than minus 2% weaker, at least 3% weaker, at least 5% weaker, at least 7% weaker, at least 10% weaker, at least 15% weaker, at least 20% weaker, e.g. 1% to 25% weaker or 3% to 20% weaker and the like) than the first pressing, the pressure can be calculated by assuming the same cross-sectional area as that in which the raw material is moving at the first press and the second press (although, in normal operation, the cross-sectional areas may be the same or different). This method of determination can be used in order to compare the pressure correctly, although it is not mandatory.

The process may include feeding the preheated carbon black-producing raw material (optionally pre-combined with feed fluid) to at least one point of introduction of raw material into the carbon black reactor and combining it. 'at least the carbon black producing raw material preheated through the point (s) of introduction into the carbon black reactor with the heated gas stream to form a reaction stream in which carbon black is formed in the carbon black reactor. The method can include inactivating carbon black in the reaction stream.

In the present invention, for any process, the specified target preheating temperatures are preferably an average temperature of the raw material prior to introduction into the carbon black reactor. The specified preheating temperatures of the raw material may be a maximum temperature of the raw material or a minimum temperature of the raw material before introduction into the carbon black reactor.

In the present invention, for any process, the declared target pressure is preferably an average pressure of the raw material. The specified pressure of the raw material can be a maximum pressure of the raw material or a minimum pressure of the raw material.

In the present invention, for any process, the specified target speed is preferably an average raw material speed. The specified speed of the raw material can be a maximum speed of the raw material or a minimum speed of the raw material.

Preheating can occur in several ways and without any limitations on how to achieve it. Preheating can occur in at least one heater (eg, one, two, three, or more). The heat source for the at least one heater can be any source, for example one or more carbon black reactors, electric heater, plasma heater, waste gas heat, heat. combustion of waste gases, fuels, and / or heat from other industrial processes and / or other forms of heat, and / or any combination of these. The preheating can occur at a location where the at least one heater partially or completely heats the raw material to the target preheating temperature for introduction into the reactor. One heater may perform partial or full preheating or two or more heaters may be used in sequence or other arrangements to achieve preheating (full or partial). If partial preheating is achieved by the at least one heater, then the remaining preheating is performed by an additional or secondary heat source or additional heaters to ultimately achieve the target preheat temperature.

For example, preheating the at least one carbon black producing raw material may include or be performed by heating the carbon black producing raw material in at least one heater which has a heat exchanger. The heat exchanger can operate at an average heat flux greater than about 10 kW / m² (such as more than about 10 kW / m² or more about 20 kW / m² or more about 30 kW / m² or more about 40 kW / m², such as about 10 kW / m² at approximately 150 kW / m² and similar).

Optionally, at least part of the preheating (or total preheating) occurs in at least one heater which has heat supplied at least partially (or totally) by the heat generated by the carbon black reactor which receives the heat. preheated raw material or other carbon black reactor (s) or both. The at least one heater may be in heat exchange with at least a part of the carbon black reactor which receives the preheated raw material or a different carbon black reactor (s) or both. . For example, at least one heater may be in contact with the reaction stream in a carbon black reactor, eg, downstream of an inactivator, the at least one heater may have a heat exchanger. having walls heated by the reaction stream on a first side (e.g., the outer wall) thereof and being in contact with the carbon black producing raw material on an opposite side (e.g., the inner wall) of it. Optionally, the at least one heater may include a heat exchanger which exchanges heat with the reaction stream in a carbon black reactor, in which a fluid heat carrier which flows through the exchanger. of heat is heated, and the heat carrier is passed through the at least one heater positioned outside the reactor and operative to transfer heat from the heat carrier to the carbon black producing feedstock. The at least one heater may be at least partially (or totally) supplied with heat by carbon black waste gas (eg, heat from the waste gas or heat generated by combustion of the waste gas) from the gas source. carbon black reactor or different carbon black reactor (s) or both, for heating the raw material producing carbon black. Preheating can be partially or fully performed using one or more plasma heaters or other heaters or heat sources.

Introducing the heated gas stream to the reactor may include plasma heating a plasma heatable gas stream in a plasma heater to provide at least a portion of the heated gas stream.

In the present invention, a non-catalytic surface may be used on some or all of the carbon black producing raw material coming into contact with the walls of the at least one heater and / or the internal walls of the heater. at least one raw material feed line which feeds the preheated carbon black producing raw material into the carbon black reactor (s). The surface can be non-catalytic for cracking (eg, thermal cracking) or polymerization of hydrocarbons.

In the present invention, the feeding step may comprise or be the feed of the preheated carbon black producing feedstock through at least one feedstock line which feeds the reactor (s). carbon black (s), and the method may optionally further comprise periodically charging a purge gas (s) which may be an oxidizer for carbon via the at least one material feed line (s) first producing carbon black. The feed line of raw material exiting from the at least one heater which preheats the raw material may have a cross-sectional area (for example, a diameter) which is the same or different from the feed line which feeds. the raw material in the at least one heater (eg, may have a smaller or larger cross-sectional area).

In the present invention, the feed may include charging the preheated carbon black producing raw material through at least one raw material feed line which feeds the black reactor (s). of carbon, and the method may comprise injecting the preheated carbon black-producing raw material into the carbon black reactor with at least partial (or total) vaporization (e.g., raw material evaporation, for example, carried out by reducing the pressure) of the raw material producing carbon black.

As indicated, the raw material can be heated to a temperature above about 300 ° C, or other temperatures above 500 ° C using the present fouling control approaches. The raw material temperature, thanks to the advances of the present invention, can be, for example, at least 310 ° C, at least 350 ° C, at least 375 ° C, at least 400 ° C, at least 425 ° C, at least about 450 ° C, or at least about 500 ° C, or at least about 550 ° C, or at least about 600 ° C, or at least about 650 ° C, or at least about 700 ° C, or at least about 750 ° C, or at least about 800 ° C, at least 850 ° C, or about 305 ° C to about 850 ° C, or from about 350 ° C to about 850 ° C, or from about 450 ° C to about 750 ° C, or from about 450 ° C to about 700 ° C, or from about 500 ° C to about 750 ° C, or from about 500 ° C to about 700 ° C. This raw material temperature is the temperature of the raw material forming carbon black immediately after leaving the heating device (s) used to preheat the raw material and / or just before being introduced into the black reactor. of carbon. The raw material temperature in this context can be measured or detected at one or more points along the raw material supply line from the point at which the raw material temperature has been raised to a value exceeding about 300 ° C to the discharge end of the feed line where the raw material is introduced into the reactor. This raw material supply line comprises any length of tubing in a raw material heating device at and after which the raw material temperature has been raised to a value exceeding about 300 ° C and before transport to part of additional feed line extending from the raw material heater to the reactor. Optionally, the temperature of preheated raw material can have an absolute minimum value in the preheated raw material feed line of not less than 301 ° C, and / or optionally, a maximum temperature variability in the feed line of preheated raw material may be, for example, ± 20%, or ± 10%, or ± 5%, or ± 2.5%, or ± 1%, or ± 0.5%, taking into account all points along of the raw material supply line. These stated raw material temperatures can be used in combination with the various fouling control process variables listed herein.

The fouling control using the specified raw material speed, at least in part, may include loading the raw material (s) at that speed into the heater and / or through the device. heater which preheats the raw material and / or via the raw material feed line to the reactor. The speed may be, for example, at least about 0.2 m / s, or at least about 0.5 m / s, or at least about 1 m / s, or at least about 1.6 m / s, or at least about 2 m / s, or at least about 3 m / s, or from about 0.2 m / s to about m / s, or about 1 m / s to about 7 m / s, or about

1.5 m / s to 3 m / s, or from about 2 m / s to about 6 m / s, or from about 3 m / s to about 5 m / s. The raw material speed is a linear speed with respect to the longitudinal axis of the pipe or other feed line structure. The raw material speed (first speed) is measured at the point of being fed into the heater which preheats the raw material. The raw material speed through the heater (s) and / or after exiting the heater (s) may be the same or different from the first speed and, for example, may be higher (eg at least 1% higher, at least 2% higher, at least 3% higher, at least 5% higher, at least 7% higher, at least 10% higher, at least 100% higher, at least 200% higher, e.g. 1% to 300% higher or 50% to 200% higher and the like). The rate is measured or calculated based on a density of raw material measured at 60 ° C at 1 atm and based on the smallest cross-sectional area present in the line of raw material being measured. This raw material supply line may include a any length of tubing in a raw material heater at and / or after which the raw material temperature has been raised to a value exceeding about 300 ° C and before transportation. in an additional feed line portion extending from the raw material heater to the reactor. For example, the raw material speed can have an absolute minimum value in the raw material feed line of not less than 0.2 m / s, and / or optionally, a maximum variability of the raw material speed in the raw material feed line can be, for example, ± 20%, or ± 10%, or ± 5%, or ± 1%, or ± 0.5%, taking into account all points along the line feed of raw material.

The fouling control using the pressurization of the raw material, at least in part, can include pressurizing the raw material producing carbon black, for example, to a pressure of more than about 10 bar. , or more than about 20 bars, or more than about 30 bars, or more than about 40 bars, or more than about 50 bars, or about 10 to about 180 bars, or about 20 to about 180 bars, or from around 40 to around 180 bars, or from around 50 to around 180 bar or more (these pressure values ​​can be converted to Pa by multiplying them by 10⁵). The raw material pressures are presently shown as absolute pressures. The pressure (first press) is the pressure measured at the point before introduction into the heater to be preheated. The pressure through the heating device (s) which preheats the raw material and / or then at the point (s) of introduction (s) to the reactor may be the same or different from the first pressure, for example lower than the first press (for example, at least 1% lower, at least 2% lower, at least 3% lower, at least 5% lower, at least 7% lower, at least 10% more low, at least 15% lower, at least 20% lower, e.g. 1% to 25% lower or 3% to 20% lower and the like). The gauge pressure readings should be adjusted to absolute values ​​in a known manner to make comparisons to the ranges described herein. The raw material pressure can be measured or detected at one or more points along the raw material supply line from the point at which the raw material temperature has been raised to a value exceeding about 300 ° C at the end of discharge from the feed line where the raw material is introduced into the reactor. This raw material supply line may include any length of tubing in a raw material heating device at and after which the raw material temperature has been raised to a value exceeding about 300 ° C and before transportation to a part. additional feed line extending from the raw material heater to the reactor. The pressure can directly strain with the raw material temperature for fouling control. For example, a raw material pressure of 10 bars (10xlO⁵ Pa) may be adequate to control fouling at a raw material temperature of 300 ° C, while a pressure increased by more than 10 bar, such as 20 bar (20xl0⁵ Pa) or higher, may be more useful in producing the same level of fouling control if the raw material temperature is increased to 500 ° C, all other things being equal.

Contamination control using a low total raw material residence time can be used. The total raw material residence time may be the combined time spent in the at least one preheater heater including the time that the preheated carbon black producing raw material spends before introduction to the reactor. The total residence time may be, for example, less than about 120 minutes, or less than about 90 minutes, or less than about 60 minutes, or less than about 45 minutes, or less than about 30 minutes, or less than 15 minutes , or less than 10 minutes, or less than 5 minutes, or less than 4 minutes, or less than 3 minutes, or less than 2 minutes, or less than 1 minute, or less than 30 seconds, or less than 15 seconds, or from about 1/60 minute to about 120 minutes, or about 0.5 minutes to about 120 minutes, or about 1 minute to about 90 minutes, or about 2 minutes to about 60 minutes, or about 3 minutes to about 45 minutes, or about 4 minutes to about 30 minutes, or 5 to 30 minutes, or 5 to 40 minutes, or 10 to 30 minutes, or about 5 minutes to about 15 minutes. The residence time can be an average value or a maximum value or a minimum value. The residence time of the raw material can be determined from the point at which the temperature of the raw material has been raised to a value exceeding about 300 ° C to the point where the raw material is introduced into the reactor. The residence time can tend inversely to the temperature of the raw material. For example, a raw material residence time of up to about 120 minutes can be tolerated without fouling problems at a raw material temperature of 310 ° C, while the residence time can preferably be reduced to less than 120 minutes to achieve the same level of fouling control if the raw material temperature is increased to 500 ° C, all other things being equal.

The control of fouling during the preheating of the raw material, for example, in a raw material heater, may include the use of a heater operating at an average heat flux, for example, over about 10 kW / m², or more about 20 kW / m², or more about 30 kW / m², or more about 50 kW / m², or more than about 100 kW / m², or about 10 kW / m² at approximately 150 kW / m² (or more), or from about 20 to about 150 kW / m², or about 30 to about 100 kW / m², or about 40 to about 75 kW / m², or about 50 to about 70 kW / m². Operation at a higher heat flux can be considered a fouling control measure, because the higher heat flux results in the raw material producing carbon black heats up more quickly and / or allows the use of a carbon black. shorter residence time in the heater as less time is required to reach the target preheating temperature.

Contamination control using a non-catalytic surface for cracking (e.g. thermal cracking) and / or polymerization of hydrocarbons on the internal walls in contact with the raw material of the raw material feed line, at least in part, may include, for example, one or more protective coating layer (s), such as a ceramic coating (eg, silica, alumina, chromium oxide).

The fouling control using the periodic on-line supply of a purge gas through the raw material supply line may include the injection of a carbon oxidant (eg, CO2, oxygen, water vapor, water vapor and air mixtures) in the raw material feed line to an accessible point or points along the raw material line. The purge gas can be introduced at a temperature of 150 ° C or more or above 300 ° C downstream of any liquid raw material pumping means. The water vapor velocity in the purge line can be, for example, at least about 6 m / s. Any backbone of raw material can be removed so that the purge immediately drives all the raw material into the reactor. Purge gas can be introduced upstream of a raw material heater to further ensure that all feed lines exposed to processing temperatures exceeding 300 ° C are processed.

As indicated, the control of fouling by removing coke from the raw material lines can include, for example, chipping or mechanical scraping. Spalling, for example, can involve cooling a coke-coated in-line pipe so that at least a portion of the coke deposited inside the pipe is chipped and or otherwise detaches from the internal walls of the pipe. pipe when the pipe contracts during cooling. The loose coke can be purged out of the pipe, and the chipped pipe is again ready for use. During chipping, the raw material can be diverted from the pipe to be chipped, for example by using the switching of valves, through another feed line or other in-line feed lines to the reactor arranged on the device. Once cleaned, the chipped pipe is once again ready for use. Another method of cleaning coke deposited on raw material pipes may involve moving a mechanical scraper through the pipe to mechanically remove coke from inside the pipes. During mechanical pigging, the raw material can be diverted, for example by using switching valves, through another feed line or other in-line feed lines to the reactor arranged on the reactor. appliance, while the hose is offline for cleaning, it is temporarily out of service. Mechanical chipping and / or scraping, if used, can be performed periodically on the raw material feed lines.

Referring to Figure 1, there is described a furnace 1 which consists of five zones, a primary combustion zone 10, a transition zone 13, a first reaction zone 31, a throttle zone 33, and a second reaction zone 35 in which an inactivation probe 41 is placed to terminate the carbon black formation reaction.

The combustion zone 10 is defined by an upstream wall 6 and a side wall 4, and ends at point 12 which is the start of the transition zone 13. Through the wall 6 is inserted a pipe 8 by means of which a fuel is introduced into the combustion zone 10. Through the side wall 4 is inserted a pipe 5 through which an oxidant is introduced into the combustion zone 10. There is contained in the combustion zone 10 a flame support 11 which is fixed to the pipe 3 which is inserted into the combustion zone 10 through the orifice 7 in the wall 6. It is located downstream of and connected to the combustion zone 10 a transition zone 13 which is defined by the wall 17 which begins at point 12 and ends at point 14. It is located circumferentially around the wall 17 a plurality of orifices oriented substantially radially, the orifices 21 (or the ejection nozzles 21) through which the mixture of fluid-raw material 87 can be injected. in the transition zone 13. Figure 1 also shows the feed fluid 85 being combined with the raw material 83 to form the fluid-raw material mixture 87 before being introduced (e.g., injected) through one or more orifices 21 (or nozzles). ejection 21).

It is located downstream of and connected to the transition zone 13 a first reaction zone 31 which is defined by the wall 37. The zone 31 can be of variable length and width depending on the desired reaction conditions. The interior cross-sectional area of ​​the first reaction zone 31 may be larger than that of the transition zone 13. Preferably, the ratio of the internal cross-sectional area of ​​the first reaction zone to that of the transition zone is between 1.1 and 4.0. Wall 37 then converges at an angle of 45 ° to the center line of furnace 1 and leads into wall 38 at point 32. Wall 38 defines constriction area 33. The internal cross-sectional area of ​​the furnace. constriction zone 33 is less than the internal cross-sectional area of ​​transition zone 13. Preferably, the ratio of the internal cross-sectional area of ​​the constriction zone 33 to the internal cross-sectional area of ​​the transition zone 13 is between about 0.25 and 0.9. The downstream end 34 of the wall 38 leads into the wall 39. The wall 39 diverges by an angle of 30 degrees from the center line of the furnace 1 and defines a second reaction zone 35. The internal cross-sectional area of ​​the second reaction zone 35 is larger than the internal cross-sectional area of ​​the constriction zone 33. Preferably, the ratio of the internal cross-sectional area of ​​the second zone reaction 35 to that of transition zone 13 is between about 1.1 and 16.0. Through the wall 39 in the second reaction zone 35 is placed an inactivation probe 41 through which an inactivation medium such as water can be injected in order to terminate the carbon black formation reaction. .

As depicted in Figures 2 to 5, at least one feed fluid 85 is combined with the carbon black-producing raw material 15 to form the fluid-raw material mixture 17 before it is introduced into the reactor 2, for example into the reactor. transition zone 12. As depicted in Fig. 2, the carbon black producing raw material 15 is preheated to a temperature of over about 300 ° C before it is combined with the feed fluid 85 and then introduced into the reactor 2 under the form of a mixture of raw material 17. The preheated carbon black-producing raw material is fed into at least one fluid-raw material mixture feed line 17 at the at least one point of introduction of raw material 16 into the reactor 2. After introduction, the raw material is combined with the heated gas stream to form a reaction stream in which carbon black is formed in the reactor. Carbon black in the reaction stream can be inactivated in one or more zones. For example, at the inactivation location 18 of the inactivation zone 14, inactivation fluid is injected, which may include water, and which may be used to completely or largely stop the pyrolysis of the raw material producing carbon black, or only partially cool the raw material without stopping the pyrolysis followed by a secondary inactivation (not shown) used to stop the pyrolysis of the carbon black producing raw material.

As further described in Figure 2, the raw material heater may include a heat exchanger 19 (HXR), which may have heater walls (not shown), as used in designs of. heat exchanger, heated by the reaction stream on a first side thereof and contacting the raw material on an opposite side thereof before the raw material is fed to the at least one raw material feed line . As indicated, the raw material is heated in the heat exchanger to a temperature above about 300 ° C. Although it is described to be arranged downstream of an inactivator, the raw material heat exchanger may be located upstream of the inactivator in the reaction stream, provided that the heater has a construction which can tolerate and operate at higher pre-inactivation temperatures in the reactor. The raw material heater can be arranged as being in physical contact with at least part of the reactor, for example, as a coil or tubing housed therein and or against and in contact with. a heated wall or walls of the reactor, for heating the raw material to a temperature above about 300 ° C. Although not depicted in Figure 2, the heat exchanger can optionally heat the raw material to an intermediate temperature (for example, above 250 ° C or from 50 ° C to 350 ° C, or d 'other temperatures below the target preheating temperature) or be used to achieve the preheating temperature above 300 ° C, and then a heat exchanger or additional heater external or internal to the reactor can be used to heat to the final preheating temperature.

The reaction stream in the reactor may have an inactivation temperature, for example, from about 600 ° C to about 2000 ° C, or from about 800 ° C to about 1800 ° C, or from about 10 0 0 ° C to about 15 0 0 ° C, or other elevated temperatures reflecting an extremely exothermic reaction which is generated in the furnace reactor. The present invention can enable heat exchange of raw material with the high exothermic heat generated by reactions in the reactor without fouling problems occurring in the raw material feed lines. The present invention can therefore make it feasible to improve energy recovery and save raw material costs as compared to conventional carbon black production carried out at much lower raw material temperatures.

As further described in Fig. 2, at least one pump 20 may be installed in-line on the raw material line upstream of the raw material heater 19 used to increase the temperature of raw material to a value exceeding 300 ° C. . The pump can be used to pressurize the raw material before it enters the raw material heater. In this way, the raw material can be already pressurized by the time when the raw material temperature is increased to high values ​​where the fouling problems in the raw material feed line could otherwise arise in the absence of pressurization or other indicated fouling control approaches. Since the raw material can generally experience a pressure drop during passage through the raw material heater under normal operating conditions (for example, a pressure drop from 0 to about 20 bar), following, for example , the design of the heat exchanger and the operational mode, any pressurization applied to the raw material as a fouling control measure should compensate for any pressure drop that may occur or be expected in a raw material heat exchanger, as well as any other pressure drop that occurs or may be provided in feed line pipes or other conduits used to transport the preheated raw material to the reactor, in particular, if necessary, to maintain the raw material pressure within a pre-targeted value range. Although only a single feed line of raw material and the point of injection of raw material on the reactor is illustrated in Fig. 2, and other figures presently, for the sake of simplification of the illustrations, it is understood that multiple raw material feed lines and injection points on the reactor can be used for which the indicated fouling controls can also be applied.

Once the mixture of hot flue gases and carbon black producing raw material is inactivated, the cooled gases are passed downstream in any conventional cooling and separation stages so that the carbon black is recovered. The separation of the carbon black from the gas stream can be easily accomplished by conventional devices such as a precipitator, cyclone separator or filter bag. With regard to the complete inactivation of the reactions to form the final carbon black product, a conventional method for inactivating the reaction downstream of the introduction of the raw material producing carbon black can be used and is known to the art. skilled in the art. For example, an inactivation fluid can be injected which can be water or other fluids suitable for stopping the chemical reaction.

Figure 3 shows a part of another type of furnace black reactor which may be used in a process of the present invention to produce carbon blacks in which at least part of the preheating comprises contacting a heat exchanger 21 with the reaction flow in the reactor where a fluid thermally conductive medium or vector 28, such as water vapor or nitrogen, flowing through the heat exchanger is heated in the reactor, and the heated steam (for example, superheated steam) exits the heat exchanger and the reactor and is channeled through a separate raw material heater 22 positioned outside the reactor where it is operative to exchange heat with the raw material in the raw material heater for heating the raw material to a temperature above about 300 ° C, such as 370 ° C or above.

Figure 4 shows a part of another type of furnace black reactor which can be used in a process of the present invention to produce carbon blacks in which at least part of the preheating comprises contacting a raw material heater 23 with waste gas which has come out of the reactor to heat the raw material in the raw material heater to a temperature above about 300 ° C (or at less partially at the target temperature).

Figure 5 shows another type of furnace black reactor which may be used in a process of the present invention in which the heated gas stream further comprises at least part or all of a heated gas 24 which has been at least heated. partly or totally using a plasma heater 25. Plasma heating of the gas can be carried out, for example, according to methods known to those skilled in the art. A plasma torch can be used, for example, as described in U.S. Patent No. 5,486,674, the disclosure of which is fully incorporated by reference herein, and reference may be made to the plasma heater disclosed in U.S. Patents Nos. ° 4,101,639 and 3,288,696.

As also depicted in Figure 5, the raw material can be heated indirectly by a thermally conductive medium (e.g. water vapor) which has exchanged heat with the reaction stream in the heat exchanger 26 in the reactor, or, alternatively, the raw material can be directly heated in the heat exchanger 26 in the reactor as indicated by the hatched lines.

As depicted in Figure 7, the raw material (FS) can be introduced separately from the feed fluid using a pipeline design which has a ring. The "primary fire" in Figure 7 and Figure 8 refers to the combustion flow. Figure 8 shows a design in which the carbon black (FS) raw material is introduced separately from the feed fluid in a design in which the lines are side by side.

The heat exchanger design used to preheat the raw material, in or outside the reactor, in these various process schemes of the present invention may be a conventional heat exchanger design, such as shell and tube. , envelope and coil, plate and frame, and the like. When the heat exchanger has an in-line coil configuration, class 80 pipe and elbows can be used, for example, to keep the in-line coil from corrosion / erosion problems. In addition, a constant pitch between the tubes can be used in the construction of the in-line coil pipeline and the coil can use the total cross section of the flue gas manifold. Heat transfer coefficients for in-line coils can vary significantly for different grades and plants.

In addition, any of the raw materials for the processing schemes and methods described may contain additional materials or compositions which are commonly used to make conventional carbon black. The method of the present invention may further comprise introducing at least one substance which is or which contains at least one element of Group IA and / or Group I IA (or an ion thereof) of the Periodic Table. . The substance containing at least one element of Group IA and / or Group IIA (or an ion thereof) contains at least one alkali metal or alkaline earth metal. Examples include lithium, sodium, potassium, rubidium, cesium, francium, calcium, barium, strontium, or radium, or combinations thereof. Any mixtures of one or more of these components may be present in the substance. The substance can be a solid, a solution, a dispersion, a gas, or any combination thereof. More than one substance having the same or different Group IA and / or Group I IA metals (or ions thereof) may be used. If multiple substances are used, the substances can be added together, separately, sequentially, or at different reaction locations. In the context of the present invention, the substance may be the metal (or metal ion) itself, a compound containing one or more of these elements, including a salt containing one or more of these elements, and the like. The substance may be able to introduce a metal or metal ion into the reaction which occurs to form the carbon black product. In the context of the present invention, the substance containing at least one metal of Group IA and / or IIA (or an ion thereof), if used, can be introduced at any point in the reactor, for example , before total inactivation. For example, the substance can be added at any point before complete inactivation, including before the introduction of the carbon black-producing raw material into a first reaction stage; during the introduction of the raw material producing carbon black into a first reaction stage; after the introduction of the raw material producing carbon black in a first reaction stage; before, during, or immediately after the introduction of a possible second raw material producing carbon black; or any step after the introduction of a second raw material producing carbon black but before total inactivation. Several points of introduction of the substance can be used.

Further, in the present invention, as indicated above, the present invention relates to a method for controlling at least one particle property of a carbon black. This method implements the combination of at least one feed fluid with at least one carbon black raw material (before and / or after entry into the reactor) to form a fluid-raw material mixture. The method may further include feeding the fluid-raw material mixture to a carbon black reactor or separately feeding the feed fluid and raw material to the reactor. The feed of the fluid-raw material mixtures can be in the form of one or more jets. The method involves controlling the amount of feed fluid present in the fluid-raw material mixture to control at least one particle property. References to "feedstock fluid", "carbon black raw material", and "fluid-raw material mixture" have the same meaning as the way these terms have been defined and explained above.

An example of at least one property of a particle is tint. The particle property can be a surface property or a structure property.

The present invention will become more clearly apparent from the following examples, which are intended to be exemplary of the present invention.

EXAMPLES

Example 1

In an example of the present invention, a hot gas stream at high speed (over 200 m / s) from a natural gas flame is burned in a transition zone (D = 135 mm) of a reactor at carbon black, such as that depicted in Figure 1, at an equivalence ratio of 0.8. Settled raw material is injected into the transition using four injectors at an overall equivalence ratio of 3.33. The raw material injectors each have a 0.76mm orifice followed by an expansion section 76mm in length and 6.5mm in diameter. The raw material is preheated to approx.

500 ° C before entering the injectors. Nitrogen is added to the raw material in the form of a feed fluid at flow rates between 0% by weight and 20% by weight (see table below) of the raw material flow immediately downstream of the 'orifice. Nitrogen is added in such a way that it is mixed with the raw material before entering the transition.

The penetration of the fluid-raw material jets into the transition zone is observed visually by means of an observation port in the reactor. Without charge fluid, the raw material jets only penetrate the transverse stream of the high velocity hot gas stream to a depth of ~ 25% of the transition diameter (i.e., jet penetration of approx. 34 mm). As feed fluid is added to the feedstock, the feedstock fluid jet penetration continuously increases until the opposing feedstock fluid jets touch each other at the center of the transition (i.e. say, a jet penetration of about 68 mm). It is observed that this occurs at a nitrogen flow rate of 20% by weight, based on the weight of injected raw material. In addition, the tint value of carbon black is measured by the ASTM D3265 method and it is observed that it increases for a given area of ​​carbon black when more nitrogen is added to the raw material in the fluid mixture. -raw material. The table below shows how hue and jet penetration vary with nitrogen flow.

Table 1

<td>Flow of N2 (% by weight of raw material)</td><td>Jet penetration (% transition diameter)</td><td>Tint% (ASTM D3265)</td>

<td> 0</td><td> 25 %</td><td> 122</td>

<td> 5</td><td> 35 %</td><td> 127</td>

<td> 10</td><td> 45 %</td><td> 130</td>

<td> 20</td><td>&gt; 50% (jets touching in the center)</td><td> 132</td>

Example 2

In a second example of the present invention, using the same reactor as in Example 1, nitrogen is added in a ring (as depicted in Figure 7) around the jets of raw material so that the fluid from charge in the ring and the raw material do not mix before entering the transition. The charge fluid is in close proximity to the raw material so that it increases the momentum of the raw material jet so as to increase the penetration of the fluid-raw material jet. The same reactor conditions as in Example 1 are used and nitrogen is added to the ring at flow rates from 0% by weight to 20% by weight of the raw material stream, based on the weight of material. first injected. As in the previous example, the penetration of the raw material jet is only ~ 25% of the transition diameter with no fluid flowing through the ring. Jet penetration increases with the flow rate of feed fluid through the ring up to ~ 40% of the transition diameter at a flow rate of 20% by weight, based on the weight of raw material injected.

Therefore, adding the charge fluid in this manner increases the penetration of the fluid-raw material jet, but not as effectively as in the previous example. The hue also increases with the addition of nitrogen to the ring.

Table 2

<td>N2 flow (% by weight of PM)</td><td>Jet penetration (% of transition diameter)</td><td>Tint (ASTM D3265)</td>

<td> 0</td><td> ~25 %</td><td> 122</td>

<td> 5</td><td> ~30 %</td><td> 123,5</td>

<td> 10</td><td> ~35 %</td><td> 126</td>

<td> 20</td><td> ~40 %</td><td> 127,5</td>

The present invention may include any combination of these different features or embodiments above and / or below as described in the sentences and / or paragraphs. It is believed that any combination of the features described herein forms part of the present invention and no limitation is intended as to the features which can be combined.

Applicants specifically incorporate all of the content of all references cited in the present description. In addition, when an amount, concentration, or other value or parameter is specified in the form of a range, a preferred range, or a list of higher preferable values ​​and lower preferable values, this should be understood. as specifically describing all ranges formed from any pair of an upper preferred range limit or value and a lower preferred range or value limit, regardless of whether the ranges are separately described. If a range of numeric values ​​is presently mentioned, unless otherwise specified, the range is intended to include the limits thereof, and all integers and fractions within the range. It is not intended that the scope of the invention be limited to the specific values ​​mentioned when defining a range.