DE1694038A1 - Process for the production of polymer particles with an extremely large surface - Google Patents

Description

Eastman Kodak Company, 343 State Street, Rochester, New York State, United States of America

Process for the production of polymer particles with extremely

large surface

A wide variety of processes are known for producing polymer particles with a large surface area. This is how it is, for example known to dissolve a polymer at high temperatures in a solvent and then by cooling the solution to precipitate the polymer particles. Another known method is to use a polymer in to be ground in a suitable grinder. The marriage of the Polymers can be carried out at elevated temperatures or at low temperatures, with the latter being the case effective cooling devices are required.

Also the so-called "ureiphasen" process in the NJaderdruckpolymerLiiation of olefins has already become direct

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Used in the manufacture of powdered polyolefins. In this process, the polymer is not in solution before, rather it forms as a solid precipitate around the catalyst used in the process.

The polymer particles which can be produced by the known processes generally have a particle size of 900 microns or larger.

Although particles less than 900 microns in size were known, it was not possible to produce such particles with a particularly large surface.

Accordingly, the invention was based on the object. Process for making polymer particles having a particle diameter of 0.1 to 900 microns and a to develop an enlarged surface compared to previously known particles.

The invention was based on the knowledge that the problem posed can be achieved by using a polymer, which may optionally contain additives, in a closed reaction vessel at an elevated temperature Dissolves pressure, allows the solution obtained to cool under pressure and the resulting polymer particles from Separates solvent.

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Accordingly, the invention relates to a method for producing polymer particles having a particle diameter from 0.1 to 900 microns and a surface area of at least 5 m / g, which is characterized in that one

1. a polymer, optionally together with additives, in a SMwfc vessel in contact with a solvent brings that one

2. the mixture obtained is heated under pressure to a temperature sufficient to dissolve the polymer so that

3. the solution of the polymer cools down to a temperature at which the polymer precipitates out of the solution, that he

ty, during the cooling process the. the pressure prevailing in the rice vessel is maintained, and that one

5. The precipitated, finely divided polymer particles are separated from the solvent and any particles that are present Extracts additives.

Carrying out the process of the invention enables the production of finely divided polymer particles or so-called polymer powders with a particle size of 0.1 to 900 microns

and a surface area of at least 5 m / g.

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In the process of the invention, a polymer, for example a polyolefin, is thus first in a suitable one "Solvent, for example a volatile" hydrocarbon in a closed reaction vessel dissolved at elevated temperature under pressure. While the pressure in the reaction vessel is maintained, is the solution obtained is cooled, the polymer precipitating out. After the solution has cooled, the pressure vessel can deaerated, whereby the solvent can either be evaporated or otherwise separated. The polymer remains in the form of clear dry particles or particles and forms a powder that is excellent suitable as an absorption medium.

Wipes made from various polymer particles can also be used and optionally various additives, the latter being present in the starting polymer can be or can be added to the solvent. To produce particularly advantageous particles, they can optionally be extracted. '

Polymers suitable for producing the polymer particles are for example polyolefins made from ethylene, propylene, butene-1, iJ-methyl-1-pentene, 3-methyl-1-butene, 4,4-dimethyl-1-peten, 3-methyl-pentene-l, ^ -Methyl-hexen-l, 5-ethyl-

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hexene-1, 6-methyl-hepten-1, hexene-1, hepten-1, octene-1, Non-1, decene-1 or other monomers with preferably 2 to 12 carbon atoms, whereby the polyolefins can be in the form of homopolymers or copolymers » The molecular weights of the polyolefins are not critical. You can e.g. B. between 1000 and several million lie.

To carry out the method of the invention, suitable polymers have a melting point of preferably 50 to 25O ° C, preferably 80-175 ⁰ C. Also suitable are crystalline and amorphous polymers.

Particularly suitable solvents for carrying out the process of the invention are hydrocarbons and chlorinated hydrocarbons and aromatic compounds with boiling points from -104 to 100 ° C. Suitable are both saturated and unsaturated hydrocarbons with in particular 1 to 12, preferably 2 to 5 carbon atoms. Examples are; Ethane, ethylene, propane, propylene, butene, butane, pentane, pentene, hexane, hexene, heptane, beepten and their isomers. Particularly advantageous solvents are pentane and butane and propane.

BATH ORIGINAL

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Particularly suitable halogenated hydrocarbons and aromatic compounds are, for example: methyl chloride, Methyl bromide, methyl iodide, ethyl fluoride, ethyl chloride, ethyl bromide, ethyl iodide, N-propyl fluoride, N-propyl chloride, isopropyl chloride, N-propyl bromide, isopropyl bromide, N-propyl iodide, isopropyl iodide, II-butyl chloride, Fluorotrichloromethane, fluorodichloromethane, benzene and fluorobenzene,

Most oxygen-containing compounds, such as B. Aldehydes, ketones, alcohols and acids have proven less effective.

The most favorable solvent in each individual case depends on the polymer used. So it can occasionally be advantageous to use a special solvent, such as cyclohexanone, e.g. B. when using polymers such as vinyl polymers, polyamides, polyesters and copolymers of ethylene and vinyl and acrylic monomers.

The specified solvents are therefore intended only as a guide and not the method of the invention limit to their use.

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The concentration of the polymers in the solutions produced can vary widely. However, it has been shown that at polymer concentrations of more than 30%, the polymer particles agglomerate and form solid, larger polymer lumps. Furthermore is obtained at low polymer concentrations in the solution (1 to 5%) the smallest polymer particles, whereas at higher concentrations, larger particles are obtained * Preferably, therefore the process of the invention, with polymer concentrations of from 1 to 20 wt - worked.%.

When performing the method of the invention the temperature to be used must only be so high that a solution of the polymer in the solvent under Pressure is reached.

The pressure to be applied can be very different. It has proven to be useful when pressing over 7.0 kg / cm to work. The most favorable pressure in the individual case depends on the temperature, the solvent, the Volume of the reaction vessel as well as other variables. Of course, highly volatile substances must be included higher pressure must be held to make sure an amount of solvent sufficient to dissolve the polymer remains in the reaction vessel. Therefore requires a At room temperature the gaseous solvent has a high pressure so that it is in higher concentrations in the pressure pot

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Is present and available to dissolve the polymer. Normally the density of the gas phase should be in be about the same as the density of the liquid phase, d. H. the density of the gas should be greater than 0.2

It is not necessary that the mixture or solution is moved in performing the method of the invention. At higher polymer concentrations it has however, it proved beneficial to move the solution.

After the polymer is dissolved in the solvent, will the resulting solution was allowed to cool. The cooling down the solution should expediently be within the narrow temperature range, which is called the "precipitation" or "cloud point" is known and is usually only a few degrees, go as slowly as possible. Within this narrow temperature range or at the "precipitation point" the dissolved polymer separates out. This "felling point" occurs before the closed reaction vessel has reached room temperature and while it is still under pressure stands.

After complete precipitation of the polymer, the Passing through the "precipitation point" or "cloud point" takes place, and after sufficient cooling of the solution

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BATH

. ■. ι β e 4 ü 3 j

To prevent the particles from sticking together during the subsequent ventilation, the autoclave or the closed reaction vessel used to carry out the process is ventilated. The solvent can "evaporate", leaving a relatively dry layer of uniform, fine, multicellular particles with a particle diameter of about 0.1 to about 900 microns. If a slowly evaporating solvent is used, this can be removed by heating or peeling off in vacuo. to increase the drying speed of the precipitate.

The following examples are intended to illustrate the process of the invention in more detail.

Example 1 '

20 g of a crystalline polypropylene with an EIgen ~

viscosity, determined from the equation :. ^ Nj = In No.

■ "■ .Λ;" - - C

wherein: Nr means the ratio of viscosity one

dilute solution of the polymer and

C is the concentration of the polymer in 100 cm ■ solution j

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of 1.53 were into a 110 ml autoclave filled. Now so much ethylene was blown into the autoclave that after 'heating to 140 ° C in it Internal pressure of 1406 kg / cm (20,000 psi) prevailed. Afterward the autoclave was closed so that it was air-tight

gradually heated to 140 ⁰ C. The temperature and internal pressure of 1406 kg / cm (20,000 psi) were maintained with agitation of the mixture and solution for 8 hours to ensure that the polypropylene was dissolved from the ethylene. After 8 hours the autoclave was cooled to room temperature. When the solution passed the "precipitation" or "tearing point" occurring at about 80 ° C., the polypropylene fell out of the solution. As soon as the autoclave reached room temperature, it was vented to allow the ethylene solvent to evaporate. The precipitated propylene polymer was obtained in the form of a powder.

The majority of the particles produced under these conditions predicted had a diameter of 30Ö

up to 800 microns and a surface area of at least 43 m / g

for the particles of the lower size limit and 18 m 7g for

da «the particles of the upper size limit. Compared to, possessed particles of the same particle size, which after previously cheapest known processes were produced, a maximum surface area of 1.7 m / g »It was found

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also that the surface of other particles produced by other known processes is less than 1 m / g.

Example 2 (comparative example)

The procedure described in Example 1 was repeated, with the exception that the autoclave was ventilated, before the polymer solution passed its "precipitation point" and before the autoclave had completely cooled to room temperature (about 25 ° C). Here fell the polymer in the autoclave in a compact manner and not in the form of fine particles.

This example clearly shows how important it is to maintain the pressure in the closed reaction vessel until the polymer solution has passed its "precipitation point ^11. In this case, the polymer can slowly precipitate out of the solvent.

Example 3

20 g of a crystalline polypropylene with an inherent viscosity, measured at 145 ° C., of 1.96 and 60 ml of pentane were introduced into a 110 ml autoclave. The autoclave was ^{heated to 150 °} C. for 8 hours and

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then cooled. When the cooling was complete, the autoclave was ventilated. A considerable part of the precipitated Polymer was in the form of a finely divided uniform powder with a particle size of 500

up to 900 microns and an average surface

ρ
of about 35 m / g.

Example ¹ J (comparative example)

The procedure described in Example 3 was repeated, with the exception that 100 g of polypropylene were used instead of 20 g of polypropylene. After performing the The polymer obtained in the process fell in the form of 10 to 12 large pieces of polymer and not in the desired powder form.

This result shows that if one exceeds a Polymer concentration in the solution of about $ 50 to one

Caking and the appearance of solid, large polymer lumps can coimen.

Example 5

20 g of low density polyethylene and 60 ml of pentane were placed in a 110 ml autoclave. Once this had been heated to 15O ⁰ C, it was

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Maintained 8 hours at this temperature and under the autogenous pressure of the heated pentane. The autoclave was then cooled to room temperature and ventilated.
Most of the precipitated polyethylene was in the form of a finely divided uniform powder with a particle diameter of 500 to 800 microns and

an average surface of 30 m / g.

Example 6

10 g of a viscous low crystalline polypropylene wax having an inherent viscosity, measured at 1 ^ 5 ° C, of 0.38 and 190 ml of pentane were introduced into a 300 ml autoclave and heated to 150 ⁰ C for 4 hours. After the autoclave was cooled to room temperature, it was vented. The polypropylene obtained was in the form of a powder with an average particle diameter of about 10 microns. These particularly small particles had an extremely high surface area of W m ² / g «

Stable emulsions could be made from the particles. It was found that the particles could be easily dispersed in water when they were used in a known manner together with surface active agents.

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The precipitation of the polymer took place in the presence of Additives which are insoluble in the solvent used were, they were uniformly dispersed in the polymer up to a weight ratio of Additive to polymer from 19: 1

The following example 7 illustrates various possibilities according to which mixtures of finely divided polymers and additives can be produced.

Example 7

Four grams of low density polyethylene and 16 grams of rice starch were placed in a 300 ml autoclave with 200 ml of pentane. The autoclave was ^{heated to 150 °} C. for 4 hours and then cooled, the contents of the autoclave being under pressure. After the pentane had evaporated, the polymer and starch were in the form of a uniform mixture of particles having a particle diameter of 300 to 400 microns and an average

Surface area of 5.2 m / g. The relatively small surface of the particles was due to the additive particles in the structure of the polyethylene particles were installed.

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Example 8

4 g of a crystalline polypropylene and 16 g rice starch were processed in the manner described in Example 7. The uniform mixture obtained consisted of Particles 300 to 400 microns in diameter and

ρ an average surface area of 6.9 m / g.

Example 9 , ° ■ "

4 g of polyethylene and 16 g of carbon black were used in Example 7 processed in the manner described »As is well known, soot has a relatively large surface area. The powder obtained passed of particles of a very uniform particle size of 300 to 400 microns. The particles had one relatively large surface area of 60.0 m / g.

Example 10

5 g of highly crystalline polypropylene and 19O ml of pentane were introduced into an autoclave and heated to 150 ⁰ C. The "autoclave was kept at this temperature and under the autogenous pressure of the heated pentane for 8 hours. The autoclave was then cooled to room temperature and vented. The precipitated polymer fell in the form of uniform particles with a particle size of 1 to 5 microns

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2 and an average surface area of 42.5 m / g,

Example 11

4 g of polypropylene and 16 g of polymethyl methacrylate were made

ι -

processed in the manner described in Example 7. Dfe Polymer particles were obtained in the form of a homogeneous powder mixture.

Example 12

4 g of a 50-50 wt .- # mixture of polyethylene and Polypropylene were processed in the manner described in Example 7. It became a homogeneous powder Polyethylene-polypropylene particles and rice starch evenly distributed therein.

Example 13 (comparative example)

A polycrystalline polypropylene was produced by the usual pulp phase process. The particles obtained had a particle size of 1 to 5 microns and an average surface area of 1.5 m ² / g.

The polymer resulting from the pulp phase process is in Obtained in the form of a powder without any carrier * medium, such as a liquid, is present

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is. The polyolefin powder produced by the pulp phase process can be produced, but does not contain particles with a large surface. Such particles are suitable Not particularly useful as an absorbent.

If appropriate, certain additives can be used from the particles obtained in the process of the invention extracted, whereby the remaining particles have an open-cell structure with particularly large surfaces own. These additives, which are easy to extract from the polymer particles precipitated, include for example finely divided substances such as rice, corn and Potato starch. Other suitable additives are, for example, sodium chloride, calcium carbonate, magnesium sulfate and Sodium sulfite.

Substances such as carbon black, soluble and insoluble polymers, pigments, antioxidants, dyes and the like can also be dispersed excellently in the polymer particles, but generally cannot be extracted.

By suitable choice of the size and type of additive or of the additives included in the precipitated polymer Is it possible to produce exactly the desired cell structure · For example, rice starch has an average particle size of about 5 microns, corn starch

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about 15 microns, potato starch about 70 microns.

In the case of a starch additive, for example, the Starch by adding the particles to boiling water and then extracting them with a dilute acid, such as HCl can be extracted. Other additions of this kind can also be done by (out) -ijös or by Decomposition can be removed.

The precipitated, multicellular particles are characterized by that they have an unusually large surface area and a very, small particle size (with a suitable choice the process conditions, especially when used a polyolefin wax).

The particles which can be produced by the process of the invention are outstandingly suitable for the production of tobacco smoke filters. They can also be used successfully wherever small polymer particles with a large surface area are used ^;

The can be produced by the method of the invention Particles with or without additive and regardless of whether the additive was removed, used will.

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Apart from their particularly advantageous usability for the production of tobacco smoke filters, can the particles producible by the process of the invention, for example for dip coating hot molded articles made of metal, for spray coating, e.g. B. by means of nozzles, for example a so-called flame of plasma jet, as well as for coating the back of carpets. Most of the uses mentioned will be the particle powder is applied first and then melted together into a continuous thin coating. Since the particle powders obtained in the process of the invention consist of finer particles than the powders that could be produced up to now, they can be used for production extremely thin coatings can be used. The large surface area of the particles that can be produced also enables them for example as an absorber in chromatography, for Manufacture of various filters and as a replacement for Activated carbon, which has a surface area of 20 m / g and larger,

z. B. Cabot ** Sterling V lampblack with a surface

ρ
of 27 m / g; Whitco FI single-surface gas furnace soot

2 *

of 25 m / g to use "In all the cases where it does not depend on the black color of the soot or the activated carbon _t producible particles can thus be used by the process of registration.

ORIGiNAL INSPECTED

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Furthermore, the particles can, for. B. also as a matting agent, ζ. B, in the form of paints, varnishes and emulsions, for the production of suede-like textured, non-glassy surface coatings or lacquers. The addition of powders to paints and varnishes increases also their scratch resistance · Furthermore, the particles obtained by the process of the invention z. B. for the production of molded articles by the rotational molding process use.

A known process for the production of porous particles or particles containing an additive, which has hitherto been regarded as advantageous, consisted in incorporating starch into an ethylene polymer by means of hot rollers. The starch introduced into the polyethylene could then optionally be extracted to produce a porous material. Another known method consisted in mixing additives and monomers, such as styrene, with one another and pouring the mixture obtained into a solid form. Subsequently, the additive was leached, whereupon a porous mass remained «

Another known method for the production of microporous fabrics is to use a pore-forming fabric, for example starch, a mixture of powdered »

Polyvinyl chloride and a temporary plasticizer incorporated, with the pore-forming substance either with the polymer or with the plasticizer must be incompatible. After the mixture has been deformed into a film, for example by extrusion had been, the pore-forming substance was removed from the mass, with a large number of uniformly sized pores or micropores whose size is different from the original size the strength depended.

It was also used to produce cellular, polymeric bodies known to incorporate a normally gaseous expansion agent into the polymeric material under pressure and then to bring about a pressure release.

In the known methods, however, they are always porous Produces substances which are of irregular size and randomly distributed pores with uneven filter properties own. Furthermore, the known methods usually quite expensive. Often there are also products that cannot be processed without additional processing can be used

The following table shows the improved effectiveness of tobacco smoke filters obtained using nach! particles which can be produced using the registration process

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before and after the extraction of various additives. For comparison purposes, some filters were prepared using particles that ^w according to the so-called hot-roll ^tr method, as described in US Patent 2,676,929 were prepared.

TABLE I.

Filter No. * Addition used

12 13 14 15 16

β ¹⁷ to 18 19 co ₂₀ - * 21 S ²²

m 23 24

25th

Rice starch rice place rice starch rice starch Rice starch rice starch rice starch

Rice starch rice starch

Rice starch rice starch

Calcium carbonate with a particle size of 4 microns

TrIcalcium Phosphate with a particle size of 4 microns

% Addition

50 70 80 80 80 80 80

80 80

80 80

80

80

Extracts additive

Yes

Yes

Yes

Yes

no

no

Yes

Yes / Yes

Yeah yeah

Yes

Yes

Used
polymer

Polypropylene

Polypropylene

Polypropylene

Polypropylene

Polypropylene

Polypropylene

Polypropylene

Polyethylene

Polyethylene

Polystyrene

Polycarbonate

polyester

Mixing process

Filter weight mg

Surface

% of the extra tar material removed

Particles

precipitation

precipitation

precipitation

hot rollers

precipitation

hot rollers

precipitation

hot rollers

precipitation

precipitation

precipitation

precipitation

Polypropylene precipitation

Polypropylene precipitation

106
68
52
70
44

179
144
100

58
60

38 62 72 60

75 39 55 40

63

66 70

68

70

69

m ² / g 41.0

1.5 11.9

4> C OO OO

In all cases, particles between 300 and 400 microns were used, regardless of whether whether the material was extracted or not.

Those used in these experiments, according to the procedure Particles made according to the invention were made as follows:

200 ml of solvent, usually pentane, and a total of 20 g of polymer and additive (if such was used) were mixed with one another in an autoclave with a capacity of 310 ml. The mixture obtained in each case was heated to 150 ° C. for 4 hours while shaking the autoclave under the autogenous pressure created by the gases given off by the constituents in the pressure pot. The autoclave was then slowly cooled to room temperature and opened. The ^eirtge-: sat polymer additive mixture was in the form of finely divided polymer particles before. The remaining solvent was separated off. The resulting particles were sieved to isolate the particle size range of 300 to 400 microns. The additive to polymer ratio has been changed. The amount of solvent used was kept constant.

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Particles produced by both methods became

Filter units made by placing the loose particles in a sheath. These filter units were either molded or then cut into 17 mm long rods with a circumference of 24.5 mm. If necessary or appropriate, the ends of the units have been sealed using small amounts of cellulose acetate or similar material to prevent the particles from falling out of the envelope. The obtained tobacco smoke filters were then attached to cigarettes to produce filter cigarettes. Such a cigarette is shown in the drawing. The cigarette consists of the tobacco part 1 and the filter part 2. The filter part 2 consists of the particles 4 enclosed in a filter envelope 3 and the stoppers 5 and 5a. The tobacco part 1 and the filter part 2 are surrounded by the casing 6. The filter cigarettes obtained were then examined for their tar and solids removal properties by the method described by McConnel in the journal "Tabacco Science 4", pages 55-61, 1960.

The particles which can be produced by the process of the invention are equally advantageously suitable as additives in tobacco smoke filter elements which are produced in a known continuous manner from endless filter cables.

The No. 12 cigarette filter of Table I was identified as Reference or comparison filters made using pure, precipitated polypropylene particles. Filter no. 13 has improved filter properties through the addition of 5055 rice starch additive. Filter # 14 also shows improved results through the addition of 70S »additive.

The results with filter nos. 15 and 16 illustrate the difference in the filtering effectiveness when using particles which were produced once by the precipitation process and the other time by the mixing process on “hot rollers”. In both cases, the starch additive was extracted before the precipitated material was processed into cigarette filters. The comparison of filter nos. 17 and 18 shows the difference when the starch is not extracted. It was found that the unextracted , precipitated, multicellular material used to manufacture Filter No. 18 gives practically as good results as the best material obtained by mixing on hot rollers and subsequent extraction.

Filters # 19 and # 20 again illustrate the different effectiveness of polyethylene particles produced by the two different processes became. .

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Filters Nos. 21, 22 and 23 demonstrate the utility of particles made from polymers other than polyolefins exist. The one used to make the # 23 filter Polyester consisted of polyethylene terephthalate; butyrolactone was used as a solvent instead of pentane used. This replacement of the solvent was necessary because polyester and polyamides are very polar Solvents require and differ from the polyolefins herein differentiate.

fr. -. "
Filters Nos. 2k and 25 further illustrate the versatility of the method of the invention. During the manufacture of the filters, various extractable additives were added to the polymer particles of Stäfrke.

If you compare. Photomicrographs enlarged 125 times

of filter cross-sections of one of the well-known microporous

the polyethylene filter and a filter, according to the procedure of the invention was made, it can be clearly seen find that the structure of the precipitated multicellular Material differs from the structure of the microporous polyethylene filter starjc. The tobacco smoke ' filter element with the precipitated, multicellular poly · » ethylene according to the invention, has much smaller

, Pores and consists of smaller particles. At a 500 times magnification of a tobacco smoke filter element

'i i *

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with the precipitated, multicellular polymeric material produced by the process of the invention, it is easy to see that this has a completely different physical structure from the toicroporous material, since it consists of a large number of very small spherical particles arranged in such a way that that together they form larger particles or strands. In the known microporous filters, on the other hand, there are smooth, connected rods. _v '

In summary, the tobacco smoke filters that produced from the particles which can be produced according to the invention say the following:

1. They are highly effective, regardless of whether the additive has been extracted or not,

2. they are light in weight,

3. They have a very high surface area and

Ij. they show compared to that made by rolling Filter material, a different structure that can be seen on photomicrographs.

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Claims (13)

Claims 1. Process for the production of polymer particles with a particle diameter of 0.1 to 900 microns ο and a surface of at least 5 m / g, thereby marked that one 1. a polymer, optionally together with additives, in a container with a solvent that one brings in contact 2. the mixture obtained under pressure on a for Solution of the polymer heated sufficient temperature that one 3. the solution of the polymer cools to a temperature at which the polymer falls out of the solution that one _t 4. During the cooling process, the container in bed * t # e sustains the prevailing pressure and that one 5. the failed, finely divided polymer particles separated from the solvent and optionally present Extracts additives. ORIGINAL IKSPECTEO 108120 / T3 & 6 2. The method according to claim 1, characterized in that that the solvent used is saturated or unsaturated hydrocarbons having 2 to 5 carbon atoms used. 3. Process according to Claims 1 and 2, characterized in that the solvent used is ethane, ethylene, Propane, propylene, butane, butene, pentane, pentene and their isomers are used. 4. The method according to claim 1, characterized in that that the solvent used is aromatic compounds, halogenated hydrocarbons or halogenated aromatic compounds used. 5 «Method according to claims 1 to 4, characterized in that that 1 to 50% by weight solutions of the Polymers manufactures. 6. The method according to claims 1 to 5 »characterized in that 1 to 20 weight-strength solutions of the Polymers manufactures. 10982 »/ 1 , 1 % k Ä T _oWQ "4AU 7. The method according to claims 1 to 6, characterized in that that one in the closed pressure vessel ρ
generates a pressure of at least 7 kg / cm. 8. The method according to claims 1 to 7 »characterized in that that the mixture or solution consisting of polymer and solvent further, in which Solvent adds insoluble particles. 9. The method according to claim 8, characterized in that the particles in a ratio of particles to polymer from 1: 1 to 19: 1 added. 10. The method according to claims 8 and 9, characterized in that the dispersed in the polymer particles Particles extracted. 11. The method according to claims 1 to 10, characterized in that that one of polymers, especially polyolefins, from monomers having 2 to 12 carbon atoms goes out. 109829/13 95 12. The method according to claims 1 to 11, characterized in that one starts from polymers with molecular weights of 100 to several million and melting points of 50 ° to 35O ⁰ C. 13. The method according to claims 1 to 12, characterized in that one of polyesters, polyolefins and Polyolefin copolymers, in particular ethylene copolymers, goes out. . _ ·, 10982Ö / 1395