Process for preparing linear polymers from carbon monoxide and at leastone olefin-unsaturated compound

Process for the production of linear pots and at least one olefinically unsaturated carbon monoxide compound

Field of technology

The present invention relates to a process for the production of polymers from carbon monoxide and one or more olefinically unsaturated compounds.

Prior art

The polymers to which the present invention relates are linear alternating polymers, i.e. straight chain polymers in which the groups formed from carbon monoxide and the groups formed from olefinically unsaturated compounds occur in a substantially alternating arrangement. These polymers can be prepared by reacting monomers at elevated temperature and pressure in the presence of a catalyst and in the presence of a diluent in which the polymers are insoluble or substantially insoluble and where the polymers thus form a suspension.

For several years, the owner of the present invention has been conducting extensive research into the production of this type of polymer. Initially, research was essentially focused on the need for this research with reactors containing less to ensure thorough mixing of the improved catalysts. The experiments were essentially performed in less than 1 kg of diluent. In order to make the reactants, these reactors were equipped with a stirring device. The mixing speed was completely arbitrary and was too high. In view of the relatively low costs associated with small reactor mixing in the past, attention has not been paid to the question of whether the same or substantially the same polymerization results can be achieved with slower mixing.

Taking into account the production of polymers on an industrial scale, some of the polymerization experiments were carried out in larger reactors which contained more than 10 kg of diluent. Using these reactors, and in view of the much larger size of the reactors used for industrial production, which contain more than 1000 kg of diluent, the costs associated with mixing in such reactors play an important role.

Prior to the transition from small reactors to larger reactors containing more than 10 kg of diluent, research was carried out to determine whether, when using larger reactors, there was a relationship between the force transmitted by the agitator to the reactor. polymer suspension (hereinafter referred to as density-force for shortening, expressed as JcW / mjL, in relation to volume_with. suspensions present in the individual reactor) on the one hand and the polymerization results on the other. Research has shown that for a stirred reactor with geometrical parameters suitable for the homogenisation of a slurry, the density-force at which the polymerisation rate is approximately 90% of the maximum value is below 0.5 kW / ra.³. ·

Since no indications have been obtained, it can be used to carry out the polymerization of reactors containing more than 10 kg of solvent at a force density of more than 0.5 kW / m³After switching from small reactors to larger reactors containing more than 10 kg of diluent, a force density of not more than 0.5 kW / m 2 was used.³.

It has now been found that the block polymerization of alternating polymers, when produced in reactors containing more than 10 kg of diluent, depends considerably on the force density used in the production. It has been found that if high force densities are used, high block density polymers can be produced.

Furthermore, it has been found that high force densities can be transferred to the reaction mixture. by forced circulation of the suspension containing the polymer particles through a discharge line through at least one mechanical contact zone.

The essence of the invention

The present invention relates to a process for the production of polymers in which linear alternating polymers are produced from carbon monoxide and one or more olefinically unsaturated compounds by contacting the monomers at elevated temperature and pressure with a catalyst in a diluent in which the catalyst is dissolved and the resulting polymers form a suspension. , wherein the contacting takes place in a system comprising at least one reactor and at least one mechanical contact zone, wherein the volume of slurry present in the mechanical contact zone or zones is substantially less than the volume of the slurry present in the reactor or reactors, the slurry being _tleads through the mechanical contact zone or mechanical contact zones and a high shear force is applied to the polymer particles, - dispersed .... in the suspension present in the mechanical contact zone or mechanical contact zones^-Those skilled in the art are aware that block density is one of the most important properties of a polymer powder recovered from a polymerization reactor. Block density plays an important role in the production, purification, storage and processing of alternating polymers. In the production of polymers, the block density determines the amount of polymer that can be produced in a certain reaction volume. In polymer purification, such as filtration, washing and drying, the amount of entrapped liquid largely determines the block density of the polymer. In terms of transport and storage, as a rule, the higher block density of the polymer will lead to more favorable flow properties and less space for the polymer. In connection with the processing of polymers into shaped articles, high block density polymer powders do not need to be compressed in order to obtain suitable properties for further processing in conventional equipment.

It is believed that the solid polymer particles that form in the diluent in the reactor grow in a random direction instead of forming regular spherical particles. The particles can thus have an irregular shape, which means that their surface area is larger than the surface area of ​​spherical particles of the same weight. This is due to a certain fluffiness of the product, which means that the product has a low specific gravity. The present invention therefore results in essentially every irregularly shaped particle being subjected to m A tn ** A i Ί 1 IT TřX rt

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JQ VO UŮ x '• protrusions a ^; similar to the shape of a particle ... it becomes a force ^J whereas' irregular irregularities are - removed ..... and more regular (spherical). Stated differently, the specific surface area (surface area per unit weight) of a substantial portion of the solid polymer particles decreases. The term a substantial portion of the solid polymer particles, as used herein, means at least 50%, preferably at least 50%.

The mechanical contact zone or mechanical contact zones may be supplemented with or replaced by any conventional agitators located in the reactor or reactors. It should be noted that prior to the present invention, in larger reactors, setting the power density of any stirrer at a higher level than necessary to achieve good mixing of the reactants (as determined by reaction rate) was not promoted. , to achieve a substantial decrease in the surface area of ​​the polymer particles.

The mechanical contact zone is the part of the system located inside or outside the reaction vessel or vessels and their volume is substantially less than the volume of slurry present in the particle suspension reactor or reactors. In mechanical contact high shear forces on polymer particles, expediently the total volume of slurry present in the mechanical contact zone or mechanical contact zones is less than 10% of the total volume of slurry present in the reactor or reactors. Preferably, the ratio of the total volume of slurry present in the mechanical contact zone or mechanical contact zones to the total volume of slurry present in the reactor or reactors is from 1: 500,000 to 1:20, more preferably from 1: 50,000 to 1:50. Expediently, the mechanical contact zone is part of a system in which the diluent containing the catalyst is contacted, by the action of a mechanical means, with the polymer particles to form other parts._:c of the reactor system, and optionally also with a monomeric starting material.

The slurry, which is subjected to a high shear force in the mechanical contact zone, can be taken from one reactor and discharged into the same reactor after passing through the mechanical contact zone. If the system comprises two or more reactors, it may be advantageous to take the slurry from the first reactor and introduce it into the second reactor after being subjected to a high shear force in the mechanical contact zone. In the case of a continuous process, the latter embodiment can be particularly advantageous.

As mentioned above, the shear force transmitted to the polymer slurry should be high in the polymerization process of the present invention. For example, in a pilot plant unit, it has been found that very good polymerization results can be obtained if the mechanical force transmitted in the mechanical contact zone or zones is in the range of 0.25 to 50 kW / m³, in relation to the total volume of polymer suspension present in the reactor or reactors, preferably from 2 to 40 kW / m³, in relation to the total volume of polymer suspension present in the reactor or reactors and in particular from 4 to 25 kW / m 2³, in relation to the total volume of polymer suspension present in the reactor or reactors.

The mechanical contact zone expediently comprises devices for intensive mixing, dispersing, homogenizing, emulsifying and / or reducing the size of solid particles in a liquid medium, such as (tooth, colloidal or disk corundum) devices consisting of stator and rotor, ball mill, rod mill, spindle. pump or .in jektoro.vá. mixing nozzle. Good results are obtained with the injector mixing nozzle.

The injector mixing nozzle or injector mixing nozzles can be designed as a venturi tube (see JH Perry, Chemical Engineers' Handbook, 3rd ed. (1953), p. JL285, Fig. 61), preferably as an injector mission (see JH Perry, Chemical Engeneers * .Handbook¹', 3rd ed. - / - 1-95-3 - / -; - str-i — .1-20-3-ř — fig. 2 — aR. H-Perry and C. H-Ghi-1-ton-, Chemical Engeneers¹ Handbook, 5th ed. / 1973 /, pp. 6 to JL5, Figs._Lor particularly preferably as a water jet ejector (see GG Brown et al., Unit Operations, 4th ed. (1953), p. 194, fig. 210).

In a preferred embodiment, the process is carried out using an injector mixing nozzle, wherein the polymer suspension in diluent is withdrawn from the reactor and at least partially recirculated through the injector mixing nozzle, the injector injector sucking one or more monomers through at least one opening in its (side) wall. and at least a portion of the suspension is removed from the system. It has been found that the solid particles are recycled by recirculating the suspension and returning the suspension through a mechanical contact zone

- 7 polymers to grow into a relatively regular shape.

Although the injector mixing nozzle can be located anywhere on the reactor wall, very good polymerization results can be obtained when the injector mixing nozzle is located at the top of the reactor and the suspension of polymer particles in diluent is discharged from the reactor from below. Therefore, the reactor is preferably provided in its upper part with an injector mixing nozzle and the suspension of polymer in the diluent is preferably taken from the bottom of the reactor. This slurry is at least partially recirculated through an injector mixing nozzle located at the top of the reactor, the monomers being sucked through one or more orifices in the side wall of the injector mixing nozzle.

2a, in order to achieve a high efficiency of polymer production in the process according to the invention, the concentration of polymers in the suspension should be as high as possible. In contrast, the amount of polymer per cubic meter of suspension is limited from a practical point of view, because too high a concentration of polymer in the suspension cannot be recirculated by the suspension pump and can in no case pass through the injector-mixing nozzle. at a level of from at least 5% by weight to a maximum of 60% by weight.

To achieve a sufficiently high productivity, the reaction mixture should be present in the reactor for a period of time. It has been found that the average residence time of the slurry in the reactor is preferably in the range of 1 to 30 hours.

The preferred residence time of the slurry in the reactor and the preferred uniform flow rate of the slurry in the injector mixing nozzle are determined based on the ratio between the volume of slurry that is recirculated in one hour and the volume of the reactor. This ratio is preferably from 2 to 100.

The polymerization reaction is slightly exothermic. If the reaction is carried out on a relatively small scale, the ratio of the outer surface of the reactor to its volume is such that most of the heat. leaves the wall of the reactor in which the reaction takes place. Therefore, the polymer suspension in the diluent is preferably heated as it is recirculated through the injector mixing nozzle if the process is carried out in a relatively small volume. In contrast, when

When carrying out the process on a relatively large scale, the polymerization reaction generates relatively more heat than is lost by the walls of the apparatus. Therefore, in this case, the polymer suspension in the diluent is preferably cooled. .before ... JietjL .. to, goes__k. _ je.jímp. injection into the reactor.

In the method according to the invention, for practical reasons

The reactor is expediently not completely filled, so that a gas cushion containing one or more monomers to be polymerized is present in the upper part of the reactor above a specified level of suspension. Preferably the volume of gas. pillows "is not bigger.

-than 40% of the reactor volume --—---- _ Injector mixing. the nozzle may spray _.

recirculated slurry to the reactor above or below the slurry level. In order to minimize clogging, it is preferred that the spraying occurs below the level of the suspension.

Preferably, the gaseous mixture containing the monomer or monomers to be polymerized is discharged from the reactor wall from the gas cushion and recirculated through an opening or openings in the side wall of the injector mixing nozzle or nozzles and a fresh charge containing monomer or monomers is added to the recirculated gas mixture. In this way, the mass of gas sucked in by the injector mixing nozzle or injector nozzles increases, as compared with the case in which no recirculation of monomers from the gas cushion occurs. Increasing the dispersed amount of gas in the injector mixing nozzle or injector mixing nozzles and in the reactor improves the reaction conditions, leading to a higher block density of the polymer.

Another advantage of recirculating the monomer from the gas cushion to the injector mixing nozzle is that in this way it can be advantageous to control the reactor temperature by cooling or heating the gas mixture in a heat exchanger located outside the reactor.

This control can be further improved if a fresh charge containing monomers is added to the recirculated gas before cooling or heating is performed.

As mentioned above, the reaction temperature can be controlled by cooling or heating the recirculated slurry stream. However, a process in which only the recirculated gas stream is cooled, cooled or heated to control the reaction temperature is preferred.

This process can be carried out batchwise or continuously, with the continuous process being preferred.

In the continuous process, part of the suspension is continuously discharged from the working system and the diluent is removed from the polymers. This diluent is preferably recycled to the system, preferably after separating the spent catalyst and adding the fresh catalyst. Polymers are obtained as the end product of this process.

The volume of suspension removed from the system is preferably in the range from 0.03 to 1.0 m³ per hour am³volume of slurry in the reactor.

It is known that in the batch production of the respective polymers it is possible to avoid clogging the reactor before the monomers come into contact with the catalyst, the suspended polymer having essentially the same properties as the polymer to be produced in diluent in the amount given by the formula ................. a> .100 xbxc, in which a represents the number of grams of polymer per liter: _ _______: __ „diluents., .___________________Λ.......-...-, ....

I v. Ř ...

b means the mean particle size of the polymer in meters and c - - represents - the block density of the polymer expressed in kg / m³.

If the production of the polymer according to the invention is carried out in an additional manner, it is probable that this finding be used.

The process of the present invention uses a catalyst capable of catalyzing the formation of the linear alternating polymers mentioned above, which are based on a mixture of carbon monoxide and one or more olefinically unsaturated compounds.

Catalysts suitable for the purpose of this invention include, but are not limited to, metals. VIII ... groups-periodic table of elements. In this patent, the metal in VIII. groups of the Periodic Table of the Elements means the precious metals ruthenium, rhodium, palladium, osmium, iridium and platinum, as well as metals from the iron group iron, cobalt and nickel.

II Preference is given to catalysts which, as the metal of VIII. groups of the Periodic Table of the Elements include palladium, nickel and cobalt, with the particularly preferred metal of VIII. groups of the periodic table are palladium. If the catalysts used in the process of the present invention comprise the metal of VIII. groups of the Periodic Table of the Elements, this metal is preferably introduced into the catalyst in the form of a carboxylic acid salt, in particular in the form of acetate.

In addition to the metal from VIII. groups of the Periodic Table of the Elements The catalysts preferably contain a bidentate ligand which may form a complex with the metal of VIII. groups of the Periodic Table of the Elements to form dental groups containing two phosphorus atoms, containing a nitrogen atom or containing a sulfur atom. If a nitrogenous bidentate ligand of the general formula in which

X represents an organic bridging group containing or 4 bridging atoms, of which at least 2 are carbon atoms, such as 2,2'-bipyridine or 1,10-phenanthroline. If a sulfur bidentate ligand is used, it is preferred to use compounds of the formula

R ^ -S - R - SR¹ in which each of the substituents

R¹ 'represents a hydrocarbon group which is optionally polarly substituted by a

R represents a divalent organic bridging group which contains at least two carbon atoms in the bridge, such as 1,2-di (ethylthio) ethane and cis-1,2-di (benzylthio) ethane. The use of phosphorus bidentate ligands of the general formula (R¹) ^ - R - P (r1) '2 in which

R and R¹ have the meanings given above.

It is further preferred to use phosphorus bidentate ligands in which the R-state is a hydrocarbon-containing hydrocarbon group containing at least one alkoxy group. as a substituent in the ortho position, due to the phosphorus atom of the compound which is very suitable for the purposes of the present invention, is

If a nitrogen or sulfur bidentate ligand is used in the catalysts, the amount applied is preferably 0.5 to 100 mol per mol of metal from VIII. groups of the Periodic Table of the Elements, in particular 1 to 50 mol per mol of metal from Vlil. groups of the periodic table. If. If a phosphorus bidentate ligand is used, the amount applied is preferably from - = - -0 -, - 5 =, 40. =. = 2- = mol --.- na ,, mol ^ metal z. vttt .. .. groups, periodic table elements, in particular from 0.75 to 1.5 mol per mol of metal from VIII. groups of the periodic table.

In addition to the metal from VIII. groups of the Periodic Table of the Elements and a phosphorus, nitrogen or sulfur bidentate ligand, the catalysts preferably contain an acid anion whose pK value_and is less than 6, more preferably an acid anion whose pK value_and is less than 4 and particularly preferably an acid anion whose pK value_and is less than 2. Examples of suitable acids whose pK value_and is less than 2, there are sulfonic acids such as p-toluenesulfonic acid and halocarboxylic acids such as trifluoroacetic acid. An acid anion whose pK value_and is less than 6, it can be incorporated into the catalysts in the form of an acid and / or in the form of a salt with a transition metal which is not a noble metal, such as in the form of a chromium or iron salt. The anion is preferably in an amount of from 1 to 100 mol per mol of elemental systems, in particular from 2 to 50 mol per mol of metal from VIII. groups of the periodic table.

present in the catalysts mol of metal from VIII. groups

Notwithstanding the catalysts named above, based on three components

a) metal compounds of VIII. groups of periodic assemblies of elements,

b) acids with a pK value_and less than 6 or its salts with a transition metal other than precious metals and

c) a bidentate ligand containing dental groups comprising two phosphorus atoms, comprising a nitrogen atom or comprising a sulfur atom, corresponding catalysts based on two components, a combination of components a) and b) can also be prepared, as using palladium trifluoroacetate or palladium p-tosylate, or to a combination of components b) and c), such as when using o- (diphenylphosphino) benzenesulfonic acid or 3- (diphenylphosphino) propanesulfonic acid.

To increase the activity of metal-containing catalysts from VIII. groups of the Periodic Table of the Elements, an additional quinone, such as 1,4-quinone or a nitro compound, can be additionally introduced into the catalyst. For this purpose, 1,4-benzoquinone and 1,4-naphthoquinone are particularly preferred.

The organic oxidizing agent is preferably from 5 to 5000 moles per mole of VIII metal. groups of the Periodic Table of the Elements, in particular from 10 to 1000 mol per mol of metal of VIII. groups of the periodic table of elements.

As olefinically unsaturated compounds which can be polymerized with S-carbon monoxide using. Suitable according to the process of the invention are compounds which consist only of carbon and hydrogen, as well as compounds in which, in addition to carbon and hydrogen atoms, one or more^_ heteroatoms. The process according to the invention is preferably used for the production of polymers from oxide

a carbonaceous hydrocarbon and at least one olefinically unsaturated hydrocarbon. Examples of such suitable hydrocarbon monomers^—are ethylene, propylene, 1-butene, 1-hexene, 1-octene, styrene, cyclopentene, norbornene and dicyclopentadiene. Way^:According to the present invention, there is also a suitable use for the production of carbon monoxide-ethylene polymers and for the production of carbon monoxide terpolymers. with ethylene and α-olefins, especially propylene.

The production of the polymers is carried out in a diluent in which the catalyst is dissolved and in which the polymers formed are insoluble or practically insoluble, so that they form a suspension.

As diluents they are. very suitable lower aliphatic alcohols.

. 2 'more methanol. ______ .... _ _ ............_..... ................

The amount of catalyst mixture used in the process of the present invention can vary widely. If a metal-containing catalyst from VIII is used. group of the Periodic Table of the Elements, it is preferable to use an amount of catalyst mixture which includes 10 "⁷ up to 10 μmol of metal from VIII. groups of the Periodic Table of the Elements per mole of olefinically -6 unsaturated compound to be polymerized, in particular from 10 to 10 '^{* 4} metal from VIII. groups of the Periodic Table of the Elements per mole of olefinically unsaturated compound to be polymerized.

The process according to the invention is preferably carried out at a temperature of from 25 to 150 ° C and a pressure of 0.2 to 15 MPa, in particular at a temperature of from 30 to 130 ° C and a pressure of from 0.5 to 10 MPa. The molar ratio of olefinically unsaturated compounds to carbon monoxide is preferably from 10: 1 to 1:10, in particular from 5: 1 to 1: 5. The process according to the invention is preferably carried out in a reactor containing more than 1000 kg of diluent.

m.

Overview of figures in the drawings ir «»

The invention is now illustrated by means of the figure, which in no way limits the scope of the invention.

The catalyst solution in the diluent is introduced via line 1 into line 2, through which the polymer suspension is recirculated through the injector mixing nozzle 2. an example is carbon monoxide and ethylene, which are introduced into the injector mixing nozzle 3 through a tube 4. Fresh monomers are fed into a tube through a supply line 5.

4, which recirculates the unpolymerized monomers from the gas cushion 6, which is present in the upper part of the reactor 7, the lower part of which contains a suspension 8 of polymers in a diluent. Upper level of suspension 8ⁱⁿ of the reactor 7, representing the level 9, is indicated in dashed lines in the figure.

By heating or cooling in the heat exchanger IQ, the gaseous mixture passing through the tube 4 is kept at the correct operating temperature. In the lowest® outlet of the injector mixing nozzle 2^se a mixture of fresh and recirculated monomers and recirculated polymer suspension in diluent is introduced into the reactor 7 below the level 9 of the suspension 8.

The suspension is discharged from the bottom of the reactor 2 via the outlet line 11 and is recirculated by the pump 12 through the recirculation line 13 and through the line 2 to the injector mixing nozzle 3. The recirculated suspension in the recirculation line 13 is maintained

at the correct operating temperature by heating or cooling in the heat exchanger 14.

Through a drain line 15, the polymer suspension in the diluent is discharged from the system. By means of a suitable separation device (not shown), such as a centrifuge or a filter, the polymer produced is separated from the diluent which contains the spent catalyst. The spent catalyst is removed from the diluent. . Fresh catalyst and catalyst are added to the diluent. the solution of fresh catalyst in the diluent is introduced into the system via line l .--—- “----—

Examples of embodiments of the invention ...... · · -, -,

The invention is now illustrated by the following examples.

Example 1

In the continuous production method illustrated in FIG.

.. at the water pipe 5 _ introduces. ..0.,. 0 04 „tons. for jien ^ í.t / dl. of a monomer mixture containing an equimolar amount of ethylene and carbon monoxide into a monomer mixture weighing 5 tons per day, which is recirculated through a tube 4 to the injector mixing nozzle 3. By means of a heat exchanger 10, the monomers are kept under

- 17 temperatures 83 ° C. In the injector mixing nozzle 3, the monomers are sprayed into a suspension weighing 70 tons per day of polymers in methanol, which is recirculated from the bottom of the reactor 7 through the outlet line 11 by means of a pump 12, recirculation line 13 and tube 2 to the top of the injector mixing nozzle 3. By means of the heat exchanger 14, the temperature of the recirculated suspension is maintained at 83 ° C. The suspension contains 15% by weight of polymers. Through line 1, 0.023 tons per day of fresh methanol containing 3.5 ppm by weight of catalyst, expressed as palladium content, is fed into the system. The catalyst consists of palladium acetate, 1,3-bis / bis- (2-methoxyphenyl) phosphino / propane and trifluoroacetic acid.

The polymerization is carried out at a temperature of 83 DEG C. and a pressure of 2.5 MPa in reactor 7. This reactor has a volume of 0.1 m³, with 30% by volume being filled with a gas cushion.

0.04 tons per day of polymers in 0.023 tons per day of methanol are discharged from the system via the discharge line 15, together with the spent catalyst. The polymer produced is separated from the diluent on a filter and by means of a dryer.

After washing and drying, the polymer has a block density expressed as a specific gravity of 540 kg / m 2³ and its mean particle size is 80 μιη.

During recirculation through the injector mixing nozzle, the force transmitted to the polymer suspension is 9 kW per 1 m³polymer suspension.

The production speed is 6.3 kg of polymers per 1 m³methanol per hour.

Example 2

In the batch process, as illustrated in the figure, reactor 7 is charged with 31 kg of methanol and an alternating polymer of carbon monoxide and ethylene in an amount of 4% by weight, based on methanol. The system is pressurized with 1.56 MPa of carbon monoxide and 0.7 MPa of ethylene. The slurry present in the reactor is pumped through the outlet line 1Γ and the injector mixing nozzle 2 in an amount of about 0.55 kg / s, the force supplied to the system by the pump 12 being approximately 10 kW per 1 m³suspension. The monomers are recirculated through the tube 4 to the injector mixing nozzle 3. The discharge line 15 is closed. The suspension is brought to a temperature of 84 ° C and maintained at this temperature, and the resulting pressure is maintained by metering a 1: 1 mixture of carbon monoxide and ethylene through a supply line 5. Over time, a 7'-solution of the catalyst, from palladium acetate, 1,3-bis / bis- (2-methoxyphenyl) phosphino / propane · and trifluoroacetic acid in acetone, is introduced into the reactor by reaching the initial line 1 consisting of concentration of palladium in the suspension, 1.4 ppm by weight, based on the weight of methanol, and after 7, 11, 13 and 15 hours the weight concentration of palladium reaches. 2.-75, 4.1, 5.5 and 6.9 ppmmethanolT '^' “' ^—’

After 19 hours, the product produced is discharged from reactor 7 via a drain. line 15, collected by filtration, washed with methanol and dried. Thus, 14.4 kg of polymer are produced, which has a block density, expressed as a specific gravity of 600 kg / m 2³.

- 19 List of line pipe reference marks. .

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supply line gas cushion.

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PATENT NÁ

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1. A process for the production of polymers in which a linear alternating polymer is produced from carbon monoxide and at least one olefinically unsaturated compound by contacting the monomers with a catalyst at elevated temperature and pressure in a diluent in which the catalyst is dissolved. further contacts in a system comprising at least one reactor and at least one mechanical contact zone, wherein the volume of slurry present in the mechanical contact zone or mechanical contact zones is substantially less than the volume of slurry present in the reactor or reactors, the slurry leading through the mechanical contact zone or mechanical contact zones and to the polymer particles dispersed in the slurry present in the mechanical contact zone or mechanical contact zones. high shear force is applied to the zones.

2. Way