Multigrade asphalt cement product and process

The present invention relates to a new universal bituminous binder and to a process for its production. It is also associated with the use of this new product as a useful substitute for conventional bitumen used in road construction, for roofing, and for applications where lower temperature sensitivity and hardening are important desirable properties over time.

Over 90% of US roads have asphalt pavements.

Natural bitumen found in lake bottoms has been in use since 1874. Subsequently, natural asphalt reserves were found in the mountains of southern and western states. They were milled, laid and rolled to produce surface coatings. However, since the early 20th century, asphalt from oil refining has dominated both road construction and roofing.

Asphalt is a dark brown to black highly viscous material based on bitumen. Many crude oil products contain varying amounts of it. Residues from asphalt residues from oil refining that contain virtually no lighter fractions above are commonly referred to as asphalt.

Asphalt used in road construction is divided into bituminous binders, liquid bitumen and bitumen emulsions. In this case, the bituminous binder is of most interest to us, although references to liquefied asphalt and bitumen emulsions are possible in perspective.

Bituminous binder is bitumen which due to its properties is suitable for road construction, roofing and special purpose products. For road construction, the bitumen is heated to a fluidity and mixed with a filler heated to approximately the same temperature (typically up to 250 ° -350 ° F). It is then laid on a pre-prepared surface, compressed and maintained until it becomes asphalt concrete. Throughout the long history of asphalt paving, the hot mixing process of bituminous binder and aggregate has remained the most cost-effective process. During the hot mixing process, at10 the contact of the heated liquid bitumen with the heated filler occurs, and a suitable filler with coating and compression is formed.

The binders used in road construction are divided into three parameters: viscosity, viscosity after a certain period of aging and penetration. The most widely used grading system in the US is based on a viscosity at 140 ° F expressed in pools (AASHTO M-22 6). (AASHTO is an abbreviated designation for the American Vals20 Highway and Transportation Workers Association). Thus, the bituminous binder, which has a viscosity of 150 pools at 140 ° F, is designated AC-2.5 and is considered soft asphalt. On the other side of the range, the 4000 pools at 140 ° F are labeled with AC-40 and treated as hard asphalt. Asphalts in the middle of the interval are designated AC-5, AC-10, AC-20 and AC-30 and are similarly related to their respective viscosities. In addition, the AC-50 has been used in certain hot climates and the AC-1 has been used in cooler climates. Standard grades of asphalt are listed and discussed in Principles of Construction of Hot-Mix Asphalt Pavements, Manual Series no. 22 (MS-22), 1983. January, p. 14 courtesy of The Asphalt Institute.

Some western states have adopted a classification based on viscosity after aging for some time. This system more accurately reflects the viscosity characteristics of an already laid pavement. The test simulates the aging of asphalt by accelerating the aging of the thin asphalt film at 140 ° F (AASHTO M-226). The results obtained are expressed, for example, in the form of AR-10 for soft asphalt 1000 pore viscosity or AR-16 for hard asphalt 16000 pore viscosity. This classification system is discussed on page 15 of the above publication. Asphalt may also be classified according to standard penetration test results (AASHTO M-20). In these tests, penetration of the specified weight of the exposed needle into the 77 ° F asphalt over a given time indicates the hardness or softness of the asphalt. This test is described on page 16 of the above publication.

For roofing, bituminous binders are used in the construction of prefabricated roofs and shingles, and as a saturating material for roofing rolls. Bituminous binders used in the construction of prefabricated roofs shall be classified according to their softness point according to ASTM D-312. (ASTM stands for American Society for Testing Materials). Type 1 asphalt with a low softening point is considered as soft asphalt. Type 4 roofing asphalt has a high softening point and is considered as hard asphalt. The assignment to this and intermediate classes is based on the asphalt's propensity to flow at specified roof temperatures and gradients. Prefabricated roofs are constructed by unrolling the bituminous rags for construction purposes. The bitumen binder is then applied to them. This process is repeated several times until a waterproof roof is obtained.

There are other special applications of bituminous binders. It can, for example, be used as a filler for joints and crevices, as an additive to increase moisture resistance and to reduce water permeability. Requirements vary by destination and can be varied.

Liquid bitumen is used when it is desired that the pavement be liquefied to below normal temperatures. It can be used with or without bituminous binders (see below). Liquid bitumen is usually sprayed. It is prepared by dissolving bitumen in a petroleum-based solvent such as naphtha, kerosene or fuel oil. The use of liquefied bitumen in both spraying and cooling by mixing involves environmental and safety concerns as solvent is released into the atmosphere. In addition, during the energy crisis of the 1970s, such use of petroleum-based solvents for these purposes was at odds with the austerity measures required at that time. As a result, the utilization of liquefied bitumen is significantly reduced today.

Solvents are generally not used for preparing bitumen emulsions, although liquefied bitumen may be used as a component (usually a water-in-oil type emulsion). The bitumen stream is liquefied by heating it. Its spherical particles are dispersed in water and triturated with the surfactant. A stable oil-in-water emulsion is obtained. Bitumen emulsions can be of several types. Depending on the surfactants used to make the emulsion, they may be anionic, cationic or nonionic. Emulsions are used to repair existing road surfaces. For this purpose, a thin film is applied to the road surface, which is then covered with filler. Provides waterproofing. BiLT 3721 B Volume Emulsions can also be mixed with the filler directly at the coating application site or, after applying a cold clay kneading process, mixed with the filler, which is distributed across the machine. The use of emulsions is usually associated with cooling mixing processes. Hot working temperatures generally require lower temperatures than those encountered in conventional hot processes.

Bitumen emulsions may be used in hot mixing processes for the production of asphalt concrete, but the associated production difficulties provide all the common advantages for the use of bituminous binders. Some of the problems associated with the use of bitumen emulsions in hot mixing operations are discussed below.

In large-scale asphalt concrete production plants, the emulsion heat generated by the steam release of water (typically about 30% by weight) when the aggregate reaches a relatively high temperature can sometimes produce an explosive force, causing environmental and occupational safety problems. Short-time mixing times in continuous-action drum-type hot-mix asphalt plants are sometimes insufficient to achieve the required water drainage. Both hot-mixing methods require a relatively large amount of additional energy to evaporate the water contained in the emulsion. When stored at relatively low temperatures, these oil-in-water emulsions freeze. This can lead to their premature breakdown. If, for any reason, the emulsions overheat, water is lost prematurely and inversion of the emulsion can occur, which can lead to potentially serious handling problems and even loss of product performance.

From the quality point of view, the most important thing is to remove water from the emulsion sediment adhering to the filler as quickly and completely as possible. The aqueous phase of the emulsion inevitably contributes to the high water content of the asphalt concrete during its laying. The subsequent evaporation rate may be influenced by environmental conditions. Thus, the drying speed and volume of asphalt concrete produced and laid with bituminous emulsions are subject to certain uncertainties. As a result, it is possible that important characteristics may be different at any time during the retention process.

Hot mixing bitumen emulsions include a class of anionic emulsions called high-flotation emulsions. The process for preparing such emulsions has long been well established - emulsions are stabilized simply by saponification with organic acids on site, usually using tallow resin. Removal of water during the hot mixing process results in improved bitumen with improved sedimentation properties.

For example, U.S. Pat. No. 2,855,319 describes an emulsion wherein saponification of phallic resin is performed with sodium hydroxide. A phallic resin soap with emulsifier function is formed. It is claimed that the retained asphalt concrete emulsion thus provides better properties. U.S. Pat. 3.904.428 describes a bitumen emulsion in which saponification of phallic resin with sodium hydroxide is carried out in large quantities. At a certain temperature range, everything is mixed with the bituminous binder. A viscous gelatinous mass is obtained which contains a bitumen content higher than usual. Higher bitumen content is said to reduce the likelihood that the bitumen will absorb moisture from the wet aggregate and increase the uniformity of the coating.

U.S. Pat. 4.422.084 High flotation emulsion based processes in which phallic resin is initially mixed with bitumen previously treated with various modifiers that affect bitumen properties but do not respond to bitumen cracking. It also refers to the process by which an emulsifier containing phallic resin reacts with caustic in an aqueous solution and mixes with bitumen. The proportions of the emulsifier components can vary, depending on the bitumen composition.

Tali Oil And Its Uses (FW Dodge Company, 1965), a member of Pulp Chemicals Associations, emphasizes the role of surfactants in the emulsion in displacing filler water and facilitating adherence of the bituminous binder. To this end, the use of fatty acids of phallic resin to perform the function of emulsifiers for fluidizing bitumen for road construction is described.

For a general overview of the hot and cold mixing processes used in road construction, see Highway Engineering, Wright and Pauuette, 4th Edition (John Wiley and Sons, 1979). A more recent overview of hot mixing processes can be found in Principles of Construction of Hot-Mix Asphalt Pavements, The Asphalt Institute, Manual Series no. 22 (MS-22), January 1983, to which reference has already been made. An overview of cold mixing processes using bitumen emulsion is given in A Basic Asphalt Emulsion Manual, The Asphalt Institute, Manual Series no. 19 (MS-19), March 1973.

The saponification reaction has been used to harden typically liquid hydrocarbons, such as gasoline, to increase the safety of their use and handling. For example, U.S. Pat. 2,338,817 refers to the solidification of a highly liquid hydrocarbon by saponification of a mixture of stearic acid and rosin with sodium hydroxide and a small amount of methyl alcohol directly on site. Metal soap is obtained.

Spirits are said to accelerate the reaction. Liquid hydrocarbons are considered to be gasoline and other product distillates which are highly flammable and intended for use as a fuel for combustion. As such, during the distillation of petroleum products, they form much lighter fractions than bitumen-derived sediment fractions.

Lockhart in American Lubricants (Chemical Publishing Company, 1927), p. 163 et seq. And U.S. Pat. 3,098,823 reads similarly to soap fats derived from lighter fractions of gasoline. It is recognized, and not at all surprising, that water is an unwanted fat component of soap. For example, U.S. Pat. The 2,339,907 fat is prepared by suspending sodium hydroxide in a non-reactive liquid medium such as mineral oil. 1 it is triturated with sodium hydroxide and, in the absence of additional water, saponification of the fatty acid. It is stated that the reaction must be brought to the saponification temperature to start the reaction. As a by-product, unwanted water is formed and must be removed further.

U.S. Pat. No. 2,888,402 describes a similar reaction involving a metal hydroxide containing hydration water released during heating. It is assumed that this water triggers the saponification reaction. Lithium hydroxide, referred to as a water source, begins the first stage of saponification, followed by the second stage, with other metal hydroxides. Despite long-standing practice and widespread use of fats that produce organogenes simply by on-site saponification, bitumen application methods have never displaced or applied fat-based technology to reap the significant benefits of jelly formation in bituminous materials. In contrast, prior to the present invention, the use of bitumen in road construction, roofing and its special applications has remained within the scope of conventional bituminous binders for the purposes of technology. To a lesser extent, the same can be said for processes based on the use of liquid bitumen and emulsions.

Currently, bituminous binders for road paving have to be chosen, bearing in mind that asphalt concrete cannot soften too much at higher temperatures or crack at lower temperatures. The necessity of this choice has led to the introduction of softer species in the northern or colder climates, and the use of softer species in the southern or warmer climates. In many climate zones, road surfaces are exposed to both high and low temperatures. This requires a trade-off in the selection, as no particular species fully meets the temperature requirements of all climate zones.

In this context, the sensitivity of bituminous binders to temperature in cases involving asphalt concrete is of paramount importance. Asphalt must maintain structural integrity at high temperatures and must not become too hard or shrink to low. The asphalt pavement must maintain these properties over many cycles of temperature change, in cold and thaw conditions, and under constant changing load.

The higher the slope of the viscosity / temperature curve plotted on a double logarithmic scale, the more favorable the thermal sensitivity of the bituminous binders is.

Bituminous binders harden over time. The reason for this is oxidation due to long-term environmental and traffic effects. Strengthening over time is another characteristic of asphalt concrete that requires considerable attention. The slower the viscosity / temperature curve plotted on a double logarithmic scale, the more acceptable the asphalt curing characteristics over time.

It is also significant that bituminous binder laid in asphalt concrete has good durability properties under normal erosion and aging conditions. Durability is defined as the resistance to degradation over time under normal weather and traffic conditions. Freezing colds and thawing, as well as oxidation associated with the aging process, are considered to be factors that influence longevity.

Obviously, in a qualitative sense, bituminous binders will approach the ideal. This requires that their lowest grades, which meet the requirements for brittleness and fracture, be able to be used without sacrificing the high-temperature, viscous, higher grades of bituminous binders. It is regrettable that the mixing of binders during hot preparation of asphalt, which is technically feasible, does not, however, provide a satisfactory combination of these properties. For example, when mixing the specified species, the temperature-dependent viscosity of each species is not maintained in the resulting mixture. The viscosity characteristics of that mixture are in the intermediate range of initial values.

Similarly, the results of the use of bituminous binders for roofing raise problems of temperature sensitivity and aging over time. Bituminous roofing materials are the most common in commercial and industrial construction in the United States. For roofing, bitumen and bitumen impregnated coatings are applied in turn. During this work, hot bitumen is laid in the form of bituminous binders for roofing.

Specialty bitumen materials, including joint and crack fillers, recirculating products, impregnation and waterproofing materials (ASTM D449), also have problems with temperature sensitivity and aging over time. They are encountered when it comes to determining the final performance of the products used.

Accordingly, the present invention seeks to: (1) provide a jelly bituminous binder which has better properties than conventionally used, including less sensitivity to temperature and slower aging over time, and (2) achieve these results by conventional hot mixing techniques. methods, using the equipment available for this purpose, standard roofing and special purpose bitumen applications.

By working with the method according to the present invention, giving the liquid bituminous material a jelly-like form, a new universal bituminous binder is obtained. This is achieved by saponifying at least one fatty acid and at least one resinous acid with an alkali metal base in liquefied bitumen substantially free of water, or by adding a saponified product to the liquefied bitumen, which will be discussed below. The resulting jelly-like bituminous binder is used for routine road construction, roofing and special applications.

High temperature common bituminous materials used in hot mixing processes have fluid-specific rheological properties. During mixing with asphalt concrete and asphalt concrete, the bitumen remains fluid and fluid, consistent with its inherently interdependent viscosity and temperature. Because of its physical state, and depending on factors such as temperature, origin and surface area of ​​the aggregate, as well as the size and configuration of the voids, it may leak from the aggregate.

It has been discovered that bitumen can be given a jelly-like shape by direct saponification reaction. Only a negligible amount of ionizing liquid is required for the ionizing zone in the liquefied bitumen, which may undergo a saponification reaction. The water formed during the reaction is sufficient to maintain the reaction, which penetrates the entire mixture of bitumen and saponification components. Water removal is an integral part of this process.

Due to the qualitative advantages of the universal jelly bituminous binder prepared by the method according to the present invention, it is possible to select lower grade (lower viscosity) bitumen and obtain asphalt concrete with the characteristic low temperature characteristics of the grade, higher viscosity) properties.

The viscosity / temperature curve of such bituminous materials is smoother than that of any single species or mixture of species. It also shows better aging properties over time and a greater smoothness of the viscosity / time curve.

Accordingly, the term universal bituminous binder, as used herein, has been chosen to describe a novel jelly-like bituminous binder with reduced temperature sensitivity and better aging properties over conventional bituminous binder. Universal bituminous binder is manufactured in an innovative way, the description of which is given below. Another characteristic of this material is that it is essentially water-free. This is evidenced by its ability to be stored at temperatures of 220 ° F and above, at which foam does not form. It is suitable for mixing with aggregate to produce asphalt concrete by conventional hot mixing techniques. It can also be used for common roofing and special applications.

Applying the process of the present invention yields a substantially water-free universal bitumen in jelly form by curing the liquid-free water-free bituminous binder. To this end, it shall saponify at least one fatty acid and at least one resin acid. This is accomplished by reaction with a well-pulverized alkali metal base in substantially dry particulate form. The resulting mixture is then removed from the reaction water. Usually, the water associated with the reaction components is sufficient to initiate the saponification reaction. The rate of the reaction is not accelerated to such an extent that, as the water agitates from the reaction mixture, excessive foaming of the water involved occurs.

The bituminous binder can be obtained from any source of bitumen, such as natural bitumen, mountain asphalt or, preferably, petroleum asphalt formed during the distillation of gasoline. It can be selected from the space currently classified by AASHTO and ASTM or it can be a mixture of different bitumens for which no specific type definition is appropriate. These include oxidized asphalt, vacuum-distilled asphalt, steam-distilled asphalt, liquefied bitumen and roofing bitumen. The bitumen composition can be enriched with admixtures such as bitumen admixtures or polymers. In cases where road bitumen is required, it is desirable to use softer grades such as AC-5 according to the present invention. Accordingly, gilsonite, both natural and synthetic, can be selected, either alone or in combination with petroleum asphalt. For example, U.S. Pat. No. 4,437,896 describes mixtures of synthetic asphalt suitable for use in a process according to the invention.

Liquefied bitumen containing saponification-promoting components is passed through a high-speed mill. The purpose is to reduce the particle size of the alkali metal base and to accelerate the saponification reaction, to disperse the constituent base and the organic acid under the liquefied bitumen. The high-speed mill must be capable of grinding base particles to a size less than 425 microns.

Accordingly, jelly-like bituminous binder can be obtained by adding pressed soap to the liquid bitumen. Since this soap is essentially free of water involved in the reaction, it is quite cool. Therefore, it is recommended to grind or dissolve it before adding it to liquefied bitumen. The choice between saponification, either locally or elsewhere, requires a combination of several factors. Although undesirable water is formed during the on-site reaction in the liquefied bitumen, it evaporates rapidly at ambient temperatures. Reactions elsewhere require additional work and equipment for storage, grinding (when the saponification product is stored in the form of solid soap), and transportation. When melting soaps, the issue of temperature control and the use of temperatures generally higher than liquid bitumen is of paramount importance. For this reason, it is desirable to perform a saponification reaction directly on site.

The bituminous material, preferably petroleum asphalt, is heated to a well-flowing fluid or to a slightly higher temperature to promote evaporation of the water resulting from saponification. Ga20 Enables temperatures from about 350 ° F to about 450 ° F, but about 400 ° F is most appropriate. The alkali metal base may be an alkali metal, an alkali metal oxide, an alkali metal hydroxide, or an alkali metal salt. Examples thereof include metal sodium, sodium oxide, sodium carbonate or, preferably, sodium hydroxide. They may also contain the corresponding potassium or lithium compounds. Preferably the base is substantially dry and finely divided into small particles during use.

The saponifying organic acids (including esters thereof) may contain one or more saturated or unsaturated, branched or straight chain fatty acids having from about

12th to about 24 carbon atoms. Examples include stearic acid, oleic acid, linoleic acid, linolenic acid and organic sulfuric acid.

Examples of the resin acids include abietic acid, neoabietic acid, dioxiabetic acid, palutic acid or isodextrimpleic acid, or mixtures thereof.

It is desirable and most convenient to add the organic acid-compatible component in the form of a tallow resin. Tall resin is a liquid resinous material obtained by boiling wood purée during paper making. Commercial tallow resin usually contains a complete complex of fatty acids. These are usually 18 carbon atoms, resin acids and non-saponifying substances, which may include sterols, higher spirits, waxes and hydrocarbons. The amount of tallow resin in these components varies. This depends on a number of factors, including the geographical area from which the wood for purée production is obtained. Preferably, the amount of non-saponifying material in the wall resin is less than 30% (ASTM D803). The ratio of fatty acids to tar acids should be between about 0.7 and about 2, preferably about 1: 1. The reaction requires about 2% by weight of bitumen and at least a stoichiometric amount of an alkali metal base for the reaction with crude tallow. For purified tallow resins or single fatty acids that have nothing to do with tallow resin sources, or if the fatty acids are mixed with resin acids in synthetic phallic resin, these amounts should be approximately the same as the amount of acidic components in the crude phallic resin. In general, complete neutralization of the alkali metal base with phallic resin is desirable. This would indicate that the acid and base molecules are more or less the same.

Only a very small amount of ionizing medium, such as water, is required to initiate the saponification reaction. For example, the amount of water normally found on the surface of the hygroscopic base is usually sufficient. An example of such a base may be a substantially dry sodium hydroxide reagent. Usually, the amount of water in a commercial untreated tallow resin is more than sufficient to initiate the reaction. If a base containing one or more hydrotated water molecules, such as hydrogenated lithium hydroxide, is selected, the heat emitted by the liquefied bitumen allows for a water jet that is sufficient to initiate the reaction.

When the overall reaction system is completely free of water or other ionizing medium (which may be the case with a dry, non-hydroscopic base and water-free purified tallow resin), the reaction begins by adding a small amount of water to the liquefied bitumen. Of course, it is important that water is added at such a time that it can penetrate the liquefied bitumen before it begins to evaporate. It is usually quite convenient to carry out the injection through or near the mouth of the mill. It has been found that water content of less than 0.001% by weight of bitumen is approximately sufficient. In fact, in practice, the saponification reaction is carried out using water that is not measurable by standard methods.

Regardless of the ionizing medium, simple mixing at the milling stage is sufficient to achieve the desired distribution even before evaporation begins. Certainly, the formation of water during the reaction generates an abundance of ionizing medium. It is desirable for the evaporation to begin at this time and to obtain a substantially dry bituminous binder.

Similarly, small amounts of alcohol may be used in the ionizing medium. Examples include methyl alcohol and other lower aliphatic alcohols. The alcoholate formed during the reaction with the alkali metal hydroxide also facilitates the saponification reaction which produces water. U.S. Pat. 2,338,817 describes the property of alcoholates to accelerate saponification of liquid hydrocarbons such as gasoline. Generally speaking, the use of spirits should be avoided as this makes the process more complicated as it involves storing and working on another component.

The following examples illustrate the practice of the present invention.

Example 1

In a one-gallon preheated and insulated container with a cone bottom add 1500 g of pre-heated AC-20 grade bituminous binder. At the bottom of the cone there is a damper which allows the bitumen to pass through the high speed mill and return it to the upper part of the vessel. 3.7 grams of sodium hydroxide grains are added to the rotating mill bitumen. The grain is protected from moisture to prevent unwanted water penetration. The mixture is spun in the mill for two minutes, and the samples taken are then passed through the no. 40 sieve (with 425 micron holes). add 30 g of crude tall oil to the rotating mixture. During the reaction, one mole of water is produced for each mole of the acid contained in the crude tall oil present. Upon further heating and stirring, the water disappears in the form of foam. As the reaction proceeds, the viscosity of the mixture increases. Stirring is continued until the foam ceases. This occurs approximately 15 minutes after the addition of tallow resin and indicates the end of the reaction. Removal of test samples.

The results of the various tests are shown in Table 1 and Fig. 1-3. At the same time, the test results obtained with bituminous binder samples prior to their universal processing as described above are shown.

Example 2

In the manner described in Example 1, the grade of AC-20 grade bituminous binder used is set to grade AC-5. The physical properties of the resulting bituminous binder are shown in Table 1. 1-3 comparing the properties of the same bituminous binder before machining it with the universal method described in the example.

Example 3

When operating in the manner described in Example 1, the grade AC-20 grade is used instead of grade AC-10. The physical properties of the resulting bituminous binder are shown in Table 1, Fig. 1-3. They are compared with the properties of the same bituminous binder before machining in the universal way described in Example 1.

For a visual representation of the universal bituminous binder, see Table 1 and Fig. 1-3 are grouped by both conventional and equivalent grades based on their viscosity at 140 ° F which they acquire during universal machining. For example, the MG-5-20 designation refers to a universal bituminous binder derived from grade AC-5 and having the characteristics of grade AC-20 at 140 ° F.

The results shown in Table 1 allow a direct comparison of the properties of the various grades of bituminous binder therein before and after universal machining (which is a conventional hot mix bitumen binder). Two widely used methods were used to determine the temperature sensitivity of bitumen during the test.

The first method based on penetration rate capability is reported in the Journal of the Institute of Petroleum Technologists 12: 144 (1936). This method assumes that typical bituminous materials used in road construction are valued at zero. Compared to conventional materials, grades below zero are considered to be less sensitive to temperature and those above zero to be more sensitive. Table 1 shows that universal machining has greatly improved the penetration rate of all brands tested.

The second method is based on the use of the penetration-viscosity number created by McLeod. It is described in Proceedings of Asphalt Paving Technologists 41: 424 (1972). In this method, bitumen viscosity at high temperatures and its penetration values ​​are compared with good and bad control values ​​of penetration - viscosity of bitumen considered as good. The data shown in Table 1 show that universal processing has resulted in a similar degree of improvement in the temperature sensitivity of all bitumen tested.

Fig. 1 shows the relationship of penetration, which is an indicator of viscosity, with temperature. Universal bituminous binders have a slower curve, which increases their sensitivity to temperature.

Fig. 2 similarly graphically shows the slope of the slope of the viscosity of the viscosity temperature of the bituminous binders due to the universal process. Again, it is noted that all univer5 saline-treated bituminous binders have a steeper curve. This proves that they are more sensitive to the effects of temperature than conventional untreated bituminous materials.

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Table 1 also shows the effect of the process of the present invention on the aging of bituminous binders over time. TFOT is a method for testing the influence of heat and air on bituminous materials over time, ASTM D1754. The table also shows that the rate of aging over time is obtained by dividing the bitumen viscosity before the start of the TFOT test by its viscosity at the end of such a test. This ratio of viscosity after heating a thin layer of bitumen in the furnace to the viscosity before heating is called the aging factor. The data in Table 1 suggest that universal processing, both in terms of TFOT and aging factor, leads to a significant improvement in bituminous binders.

The TFOT Test for Thin Bitumen Furnace was extended to show the effect of long-term aging of thin bitumen layers by extending the shelf life from 5 hours to 15 hours. Table 1 shows that the processing of bituminous binders in the manner shown in the examples has greatly reduced their curing time over time.

Fig. 3 is a graph of the viscosity change of a thin layer of bitumen in a furnace test as a function of aging time. It is easy to see that the viscosity / TFOT curve of universal bituminous binders is slower. This means that the aging of these binders over time is slower than that of the conventional bituminous binders.

It should be noted that conventional methods for measuring the viscosity of bituminous binders, such as ASTM D2170 and ASTM D2171, are not suitable for use with universal bituminous binders as bitumen is not a new material. Due to its non-tonic properties, tinLT 3721 B is the most potent test method using a vacuum capillary viscometer (1984) to test ASTM P-160 Bitumen Emulsion Sediment and Non-New Bitumen. Table 1 shows the results of the various tests and the test results for the bituminous binder samples as described above.

From the comparative tests described above, it can be concluded that universal machining has a significant positive effect on penetration, viscosity and viscosity after 5 and 15 hours of aging by TFOT. For example, the viscosity of the AC-5 grade bituminous binder was 530 pools at 140 ° before machining. Thanks to the universal treatment of the same material, the viscosity has increased to 2,200 pools, which meets the AASHTO M-226 AC-2G requirements. Similarly, versatile machining has resulted in a change in the aging characteristics of each bituminous binder over time.

Example 4

In the manner described in Example 1, the bituminous binder used is then replaced with 1500 g of AC-10 grade and 5.25 grams of anhydrous potassium hydroxide are used in place of the sodium hydroxide used. The results obtained are shown in Table 2.

Example 5

In the manner described in Example 4, 2.24 grams of anhydrous lithium hydroxide are used in place of the potassium hydroxide used. The results obtained are shown in Table 2.

Example 6

In the manner described in Example 4, 5 grams of anhydrous sodium carbonate are used in place of the potassium hydroxide used. The results obtained are shown in Table 2.

Table 2

<td colspan="2">An example ^z</td><td>; An example</td><td colspan="2">5 Example 6 AC-1C</td>

<td></td><td>KO H</td><td>LiOK</td><td>Well_zCO,</td><td>control</td>

<td>Penetration, dmm</td><td> 75</td><td> 87</td><td> 70</td><td> 90</td>

<td>Viscosity at 140 ° FP</td><td> 1850</td><td> 1340</td><td> 2300</td><td> 1150</td>

<td>Softening point, ° F</td><td> 128</td><td> 126</td><td> 149</td><td> 122</td>

<td>Penetration number</td><td> 4-0,8</td><td> 10, 6</td><td> 4-2, 9</td><td> 4-0,2</td>

<td>Viscosity, P, after 5 h. duration of TFOT test</td><td> 2743</td><td> 2860</td><td> 4189</td><td> 3050</td>

<td>Aging factor</td><td> 1,49</td><td> 2, 13</td><td> 1,82</td><td> 2, 65</td>

<td>Viscosity, P, after 15 h. TFOT test</td><td> 5600</td><td> 8174</td><td> 6417</td><td> 11400</td>

<td>Aging factor</td><td> 3, 03</td><td> 6,1</td><td></td><td></td>

Table 2 shows a significant improvement in the temperature sensitivity of all bituminous binders compared to the control grade prepared on AC-10 basis. This improvement in temperature sensitivity is determined by the penetration rate and the aging rate over time.

Example 7

In the manner described in Example 4, 2.2 grams of metallic sodium are then used instead of the potassium hydroxide used.

A smaller amount of foam is observed. The results obtained are shown in Table 3.

Example 8

Using the method described in Example 4, the following talc resin is added to the bituminous binder. This is followed by mixing and pouring sodium hydroxide pellets into a high speed colloidal mill. The results obtained are shown in Table 3.

This example demonstrates that the reversal of chemical addition does not substantially affect the properties of the bitumen binder processed by the universal process.

Example 9

Add 500 grams of heated tallow resin to 62.5 grams of sodium hydroxide granules with vigorous stirring in the vessel described in Example 1. The 33.75 grams of the resulting mixture are extracted and poured into 1500 grams of AC-10 grade bituminous binder maintained at 400 ° F. The resulting mixture is passed through a high-speed colloidal mill. The universal product is tested as described above. The results of the tests are given in Table 3.

Table 3

Example 7 Example 8 Example 9 Control

Metallic First of all, tall earth disinfectant tallow and caustic soda are added together

Penetration

Viscosity at 140 ° F, P

67 72 90

3105

3275

2400

1150

Table 3 (continued)

<td rowspan="3"></td><td colspan="2">Example 7 Example 8</td><td>Example 9</td><td>Control</td>

<td colspan="2">Metallic First of all</td><td rowspan="2">Tall resin and caustic soda are poured together</td><td rowspan="2">AC-10</td>

<td>sodium</td><td>tall resin</td>

<td>Softening point, ° F</td><td> 159</td><td> 150</td><td> 145</td><td> 122</td>

<td>Penetration number of cs</td><td> 13,8</td><td>17 c</td><td> 12,5</td><td> 4 0,2</td>

<td>Viscosity (ATFOT) after 5 h.</td><td> 5650</td><td> 5900</td><td> 5620</td><td> 3050</td>

<td>Aging factor</td><td> 1,82</td><td> 1,80</td><td> 2,34</td><td> 2,65</td>

<td>Viscosity (ΑΤΕΌΤ) after 15 h.</td><td> 4804</td><td> 8275</td><td> 8125</td><td> 11400</td>

<td>Aging factor</td><td> 2,71</td><td> 2, 53</td><td> 3, 39</td><td> 9, 91</td>

The above results describe the physical properties of the universal bitumen products obtained by the methods described in Examples 7-9. They show that, regardless of the order of the components, the universal bituminous binder has a significantly better temperature sensitivity than the control AC-10 based sample.

Example 10

Tests are carried out to demonstrate the sensitivity of bitumen emulsion sediment containing high buoyancy sediment to moisture retained in the mixture. ASTM no. Washed limestone corresponding to 8 is coated with 4% by weight universal bitumen binder made of SC-5 grade bitumen (MG 5-20 grade bituminous binder is formed) and compared with similarly prepared conventional AC-20 grade bituminous binder. HFMS 2h grade bitumen emulsion (AASHTO M-140) is also mixed with filler. For this purpose, 5.7% by weight of the emulsion is added and 4% by weight of the residual bituminous mixture is obtained. Each batch of bituminous binder is mixed with filler at 300 ° F for 90 seconds. The emulsion filler is heated to 100 ° F higher temperature to remove water. In all cases, the final mixture temperature is 275 ° F.

Place about 300 grams of each mixture on an 8-inch, fourth-number sieve and place in an oven at 300 ° F for one hour. A trough is placed under each sieve to collect bitumen effluent. The following results are obtained:

MG5-20 AC-20 HMFS-2h

Bituminous binder content in trough, g: 0 9,9 1,3

These tests demonstrate the higher resistance of the all-purpose bituminous binder to aggregate migration compared to the conventional AC-20 grade bituminous binder and the ability of the bitumen emulsion to form high-flotation and moderately sedimented sediments. It is said that the unique property of high flotation sediment is reduced migration of bitumen particles in hot-prepared mixtures. These tests confirm that this is true for the AC-20 brand. However, in this sense universal bituminous binders are much better than HFMS type emulsion sediments.

Example 11

Measure the properties of the mixtures prepared in the manner described in Example 10 over a very wide temperature range. The purpose of these tests is to determine whether the improvement achieved through the use of the universal bituminous binder LT 3721 B also allows the properties of the bituminous mixture to be improved (this is the ultimate ultimate purpose of this material).

The bituminous binder test described in this example uses the same bituminous binder as the leak test described in Example 10. Mixed ASTM5 compliant filler, no. δ aggregate and fine grain sand. A 3/4 inch density mixture is obtained (ASTM D-3515). The aggregate and bituminous binder are heated to 300 ° F before mixing. The HFMS-2h is heated for 90 seconds at 77 ° C and mixed with the filler at 400 ° F. Each such blend contains 4.5% by weight of a bituminous binder. In accordance with ASTM D-1559, each mixture is compressed by 75 Marshalling Compressions. With each filler, four mixtures are prepared and tested at four temperatures: 140 ° F, 100 ° F, 77 ° F, and 40 ° F. This range of temperatures reflects a wide range of actual pavement temperatures. Hardness is measured by Marshall and Hveem design apparatus in accordance with ASTM D-1559 and ASTM D-1560. The results obtained are shown in Table 4.

Table 4

Test temp., ° F MG-5-20 AC-20 Emulsion HFMS-2h

Hveem construction apparatus

<td> 140</td><td> 56</td><td> 55</td><td> 20</td>

<td> 100</td><td> 55</td><td> 63</td><td> 27</td>

<td> 77</td><td> 55</td><td> 66</td><td> 33</td>

<td> 40</td><td> 79</td><td> 87</td><td> 56</td>

Table 4 (continued)

Test temp., ° F MG-5-20 AC-20 Emulsion HFMS-2h

Marshall construction apparatus

<td> 140</td><td> 2450</td><td> 2550</td><td> 900</td>

<td> 100</td><td> 2850</td><td> 4150</td><td> 2150</td>

<td> 77</td><td> 3100</td><td> 4750</td><td> 1850</td>

<td> 40</td><td> 10000</td><td> 17500</td><td> 2900</td>

These results demonstrate that with a universal bituminous binder, the hardness (ie, its stability) of asphalt concrete is not increased as much as with conventional bituminous binder.

these results also indicate that the emulsion mixture (HFMS ~ 2h) exhibits extremely low stability at high temperatures. This may be due to incomplete retention (ie presence of residual moisture).

The tests described in Examples 12-14 have been carried out to show that even a very small amount of water is necessary to initiate the saponification reaction which is an integral part of the process of making this universal bituminous binder.

Example 12

1500 Heat a gram of AC-10 grade bituminous binder to 400 ° F and place in the same container as used for Test 1. 3.75 grams of sodium hydroxide is preheated to a dry molten state. It is poured into a bituminous binder and milled for one minute. The tallow resin is heated at 275 ° F for two hours until completely dried. 30th grams of phallic resin are added to a mixture of binder and caustic soda in bitLT 3721 B and ground for 15 minutes. The test results are shown in Table 5.

Example 13

In the manner described in Example 12, 2.2 grams of metal sodium is replaced by sodium hydroxide. The test results are shown in Table 5.

Example 14

Using the procedure described in Example 13, add 0.015 grams of water to the tallow resin and mix before mixing with the biofilm binder.

Table 5

Example 12 Example 13 Example 14 (dry) (dry) (dry)

<td colspan="4">Penetration at 39 ° F,</td>

<td>200 g, 60 sec, dmm</td><td> 31</td><td> 31</td><td> 31</td>

<td>Penetration at 77 ° F, 100 g, 5 sec, dmm</td><td> 83</td><td> 111</td><td> 85</td>

<td>Viscosity at 140 ° F, 1 sec, - 1, P</td><td> 3075</td><td> 920</td><td> 2750</td>

<td>Softening point, ° F</td><td> 158</td><td> 117</td><td> 149</td>

<td>Penetration number</td><td> 14,3</td><td> 10,7</td><td> 13,8</td>

<td>Viscosity after 5 h. duration of TFOT test</td><td> 4250</td><td> 1785</td><td> 4010</td>

<td>Aging factor</td><td> 1,38</td><td> 1,92</td><td> 1,45</td>

<td>Viscosity after 15 h. duration of TFOT test</td><td> 4975</td><td> 6820</td><td> 6795</td>

<td>Aging factor</td><td> 1,62</td><td> 7,41</td><td> 2,47</td>

The results obtained indicate that the tests described in Examples 12 and 14 underwent a saponification reaction which showed suitable properties of a bituminous binder for comparison. Such a reaction occurred during the assay described in Example 12, where all reagents were specifically dried. Nonetheless, the system contained sufficient (albeit not measurable) laboratory-level moisture to initiate the reaction.

No reaction occurred in the test described in Example 13, although the phallic resin was dried in the same manner. At present, metal sodium is used in place of the sodium dry ground hydroxide used in the test described in Example 12.

The use of metallic sodium and dried phallic resin, as well as the addition of a small amount of water (0.001% by weight of the bituminous binder), resulted in a saponification reaction, as discussed in Example 14.

Example 15

In the manner described in Example 1, a bitumen binder for the first type of roofing is used in place of AC-20. Table 6 compares the results of typical roofing tests with those of the original bituminous binder.

Table 6

Before After Processing ASTM D-312 Tia (MG Type 1-2) at 2 CharacterType 1 Type 1

Softening temperature of 158 vol., ° F 146 171 to 176

Penetration at 32 ° F,

200 g, 60 sec, dmm

Table 6 (continued)

<td></td><td>Pre-treatment Type 1</td><td>After machining (MG Type 1-2) Type 1</td><td>ASTM D-312 Type 2 Characteristics</td>

<td>Penetration at 77 ° F, 100 g, 5 sec, dmm</td><td> 40</td><td> 34</td><td>from 18 to 40</td>

<td>Penetration at 115 ° F, 50 g, 5 sec, dmm</td><td> 102</td><td> 70</td><td> 100</td>

<td>Penetration number</td><td> -22</td><td></td><td></td>

The test results show that the processed bituminous binder 5 has low temperature properties of the first type of bituminous binder used for roofing and the same properties of the second type of high temperature material.

The penetration rate of processed bituminous binders is significantly lower, which indicates a lower sensitivity to the effects of temperature.