Method of producing para-subsituted aromatic polyamide particles

FIELD: chemistry.

SUBSTANCE: invention relates to a method of producing completely para-substituted aromatic polyamide particles for use as filler, which comprises the following steps: a) adding an aramide polymer solution to a water-based coagulation liquid to obtain a hydrogen-containing moulded product and b) crushing the frozen non-dried or partially dried moulded product, having water content from 10 to 99 wt %.

EFFECT: method enables simple and efficient production of small aromatic polyamide particles which cannot be obtained through traditional grinding methods.

8 cl, 1 tbl, 6 ex


This invention relates to a method for producing a fully para-substituted aromatic polyamide particles, which are suitable for use as the filling material for such precise details as gears and stuff, and have excellent resistance to abrasion, friction, heat, conservation of sizes. This invention also relates to such particles, which are obtained by grinding during freezing, and their application.

Fully para-substituted aromatic polyamide fibers have excellent heat resistance, high strength, high toughness, chemical resistance, etc. and are widely used in various industrial materials. Moreover, in addition to these properties fully para-substituted aromatic polyamide particles are also excellent in terms of resistance to abrasion, friction, as lubricants, and so they were used as an additive for thermoplastic resins.

The methods of production fully para-substituted aromatic polyamide particles include, for example, methods of grinding of bulk polymers using the crushing and grinding mills, such as ball mill or jet mill. Methods of grinding for freezing for the production of thermoplastic resins at lower the Noah temperature have been disclosed in Japanese patent application No. H7-234551, not pass the examination, and the manner in which the cooling of the resin to -196°C was performed using liquid nitrogen to obtain a brittle thermoplastic resins at low temperatures. In addition, used the method of dispersing the water dispersion of the powder, such as cellulose using high-pressure homogenizer, and a good way to directly obtain particles using emulsion polymerization and the like disclosed in Japanese patent application No. H3-152130, will not pass the examination. In addition, in order to obtain particles of a smaller size, use the sorting machine for sorting pellets on the appropriate particle size.

In addition, some of the above methods used in the production of fully para-substituted aromatic polyamide particles. However, since fully para-substituted aromatic polyamides are very solid, above-mentioned mechanical grinding to be done several times in order to obtain fine particles for sorting. Because these stages are extremely complex, inevitably increasing the cost. In the case of fully para-substituted aromatic polyamide polymer particles can be directly obtained by polymerization or can be recycled after polymerization in other fourmeau the data particles, such as flocks, fibres, febrile and the like.

When used as the filling material for small precise parts, where dispersion in thermoplastic resins, and their possible uses, and the like are most suitable are particles most small size, and require a lot from the way the efficient production of these para-substituted aromatic polyamide particles.

It was found that after the introduction of the solution of aramid polymer in the coagulation liquid, and after washing with water, the obtained amorphous slurry molded product is not subjected to the stage of drying, have not shown sufficient crystallization, and found that the molded product contains a large amount of water.

The essence of this invention is to provide a simple and efficient method for the production of fully para-substituted aromatic polyamide particles, which can produce small particles that cannot be easily accepted methods of grinding.

Finally, the invention relates to the finding that the molded product obtained by injection of a solution of aramid polymer in the coagulation liquid is water-based and that the product is not dried or partially what about the dried, contains at least 10 wt.% water and can be crushed into fine particles by crushing after freezing, the product can not be obtained by conventional methods of grinding. In addition, it was found that the method according to the present invention allows grinding in a short time.

According to the present invention a simple and effective way of obtaining fully para-substituted aromatic polyamide particles, which is particularly suitable for producing small particles.

The formed product with a high water content, which is obtained by introduction of a solution of aramid polymer in the coagulation liquid, and, passing the stage of drying after washing with water, can be easily crushed into small particles by grinding during freezing. The obtained particles are particularly suitable, for example, as the filling material for precision parts such as gears, etc.

Fully para-substituted aromatic polyamide, i.e. aramid polymer in this invention is a polymer which can be obtained by polycondensation of a mixture of monomers, which mainly consists of terephthaloylchloride and p-phenylenediamine. This reaction may occur in the N-organic, however, because of the insolubility of the polymer in N-organic as the accelerator is olymerization the polymer is mainly soluble in sulfuric acid, and this sulfuric acid solution is used as an additive for molding.

The form used in this invention aramid polymer grinding stage can be any, such as fiber, fibril, palpi, particles of leaf shapes, film particles, the polymer layer of particles, or fibers, as well received as short fibers, by cutting fibers, commonly known as the flock, and the like. The size of the resulting particles, as well as length, thickness, size and cross section, etc. are not limited to; although febrile, palpi and flocks are the preferred particles for use in grinding stage during freezing. Febrile in the present invention refers to both small film of the particle shape, similar to a thin sheet obtained, as for example described in WO 2005/059247, in which is disclosed a method of their production, for example, a solution of aramid polymer is mixed in the system, using coagulation liquid solution of aramid polymer with application of shear forces. The term "pulp" means small short fibers, randomly fibrillated, such as found in WO 2004/099476. The term "Fibril" means fully fibrillated polymer and, thus, that mainly contains fibrillary part, and the main fibers not longer fibers in the pulp, as described, e.g. the, in WO 2005/059211.

In the present invention, the formed product of aramid polymer used for grinding stage, must be the product of a slurry form. The product can be amorphous or crystalline. The term "amorphous" here refers to the structure formed due to hydrogen bonding which takes place before the crystal structure. It can be assumed that any part of the molded product, which has not led, can be amorphous molded product. Moreover, these amorphous structure containing water, called amorphous slurry molded products. Slurry molded product is usually obtained directly or after washing koagulirovannogo product water. The product in accordance with the present invention, previously crushed, not dried or partially dried. The partially dried product, the water content may be at least 10 wt.%. If the water content of the slurry molded product is maintained in the range from 10 to 99% by weight, preferably between 10 and 95% by weight, then randomly fibrillated particles by applying a mechanical force cutting at the aforementioned particles using known processing or milling, and the like may also be used in the process Ismail is to be placed during freezing.

The water content may be from 10 to 99% by weight, preferably from 20 to 95% by weight. Below 10%, even if the composition contains water, the grinding process is not as effective and the required particles of small size cannot be obtained. Moreover, above 99%, the fine particles can be obtained, however, the number of the resulting product is so small that the performance decreases dramatically.

Although not clarified some reason, the influence of water should be taken into account. In General, the crystallinity of these materials is so low, as they contain many inter - and intracrystalline water, it accelerates the destruction of small particles. A large number of inter/intracrystalline water due to the fact that the material is not fully dried, as always increases (sintering) of the resulting crystals containing much less water. Moreover, water in the gaps between the crystals in the polymer after freezing, leading to improvements in grinding in those places where the contained water. It was further established that the polymer, which was fully dried and then moistened and containing from 10 to 99 wt.% water, preferably between 10 and 95% by weight, can not be crushed into small particles by freezing. Thus, it is necessary to use not the polymer, or who are partially dried polymer with a water content, at least 10 wt.%, preferably, at least 20 wt.%.

In the present invention, the method of freezing the water contained in the polymer, which must be crushed, not particularly limited, however, taking into account the working properties or potential value, despite the fact that freezing is possible when using or dry ice, or liquid nitrogen, it is preferable to use liquid nitrogen.

Moreover, there are no special restrictions to the device, which should be used for grinding by freezing the formed product, and can be used any known device for grinding after freezing. In addition, the conditions of grinding is not particularly limited, and a suitable device can be made depending on the desired size or shape of particles.

Further, in the present invention are described in detail stages of the particles.

First, prepare a solution of aramid polymer. Instead of a solution of aramid polymer can be used solution is polymerized in a solvent aramid polymer or a solution dissolved in a solvent, in which the aramid polymer (here referred to as polymer) is dissolved after the Department received aramid polymer. For example, in the case of poly-p-phenyleneterephthalamide, terephthaloyl is chloride and p-phenylenediamine polycondensed in N-organic. The polymer solution in N-organic can be used as such, or as an alternative can be used a polymer solution in sulfuric acid. Due to the poor solubility of the polymer in the polymerization accelerator N-organic polymer can be separated or can be dissolved in sulphuric acid.

In this case, the concentration or viscosity of the polymer solution is not particularly limited; however, in order to achieve the desired working or operating characteristics of the obtained polymer solution, to some extent, the restrictions may be necessary for practical reasons.

Next, the polymer solution is introduced into the coagulation liquid is water-based (here referred to as coagulation liquid). The method of introduction of the solution has no special limitation, but usually can be used known methods such as molding system using a coagulation liquid under the action of mechanical shear forces, extrusion methods in coagulation liquid through the nozzle, methods of forming polymer solution in a coagulation liquid through the die plate and methods of extrusion through a slit, etc. moreover, if necessary, the application of shear force to the polymer solution immediately prior to extrusion through a nozzle or by using an air gap to forming solution is alimera the coagulation liquid through the die plate does not cause any special problems. In addition, as the coagulation liquid in this invention uses the contained water or preferably water, which as a main component, and there are no particular restrictions to the additives added to the water.

After forming the coagulation fluid conducting washing with water and if necessary, perform the stage of neutralization. From this point without the use of a stage of drying the polymer still containing water, collect. After collecting the fibers may be applied mechanical shear force, if necessary, using known processing and grinding devices, etc. for chaotic atrial. At this time, the water content in the polymer is from 10 to 99 wt.%, preferably from 20 to 95 wt.%.

If the grinding when freezing is not carried out immediately after collection or if, for example, the fibers must be cut into short fibers after their production, as a special warning is required, so that the water does not evaporate from the polymer. Preferably, the polymer was stored in airtight vessel or placed in a humid environment, where temperature is monitored and there is no access to sunlight.

Next, the polymer is subjected to grinding by freezing. At this time, the shape of the polymer is not particularly limited. However, for napoleonica particles is preferable, if the fiber length or particle size less than 1 mm, the particles that exceed 1 mm, can be without any problems used, but in this case shall be governed by the terms of grinding, such as increased productivity grinding or acceleration of the rotation, etc.

Before chopping polymer water contained in the polymer should be frozen. Special restrictions to the methods of freezing, however, taking into account the working properties or potential value, etc. preferred freezing with liquid nitrogen.

The polymer containing the frozen water, then subjected to the step of grinding using a known device for grinding after freezing. Moreover, in addition to devices for grinding during freezing can also be used suitable mill-crusher, equipped with a device capable of grinding at a temperature below 0°C. the grinding Conditions can be suitably adjusted in accordance with a functioning device, or according to the quantity of polymer used and depending on the desired size or shape of particles, etc. Though, despite the conditions of grinding, using this method can be obtained particles with a wide range of particle size, in this case, as we know from the level of the ehniki can be used in a sorting device for sorting without any problems, and, therefore, can be obtained particles of the desired size with less varying particle size.

Therefore, the aim of the invention is also getting a pair of fully-substituted aromatic polyamide particles with a size less than can be obtained by using common methods. Thus, the invention also relates to grinding when freezing completely para-substituted aromatic polyamide particles having a size of d50less than 75 microns, preferably less than 50 microns, and most preferably less than 30 μm. Because the distribution of particle sizes symmetric or nearly symmetric, the value of d50corresponds exactly to the average diameter of the particles.

As described in this invention, a molded product with a water content of from 10 to 99 wt.%, obtained by introducing a solution of aramid polymer in the coagulation of the water-based liquid, is subjected to grinding by freezing for productive obtain small para-substituted wholly aromatic polyamide particles.

Further in the present invention is described in detail, based on different implementation. However, this invention has no particular restrictions on these were the areas. The following method was used for measurements.

1) particle Size (µm):

Without sorting the obtained particles were collected and were measured particle size instrument that measures particle size by laser diffraction (Microtrac X100, manufactured by Leeds & Northrup Co.). Fixed value for 0.50 means that 50% of all particles smaller than this value. Accordingly, it is also established that d10and d90respectively 10% and 90% of all particles are smaller than this value.

2) water Content (%):

The water content is calculated based on the formula below after measurements according to JIS L1013.


WO is the weight before drying; W is the weight after drying.

3) Thickness:

Measured according to JIS L1013.

4) fiber Length (mm):

Is measured using a device for measuring the fiber length Pulp Expert" (Metso automation Co).

Example 1

Fiber in the form of pulp poly-p-phenyleneterephthalamide were obtained as in example 1 of WO 2004/099476. In addition, the length-weighted average fiber length and the water content of the obtained fibers was 0.81 mm and 91.5 wt.% respectively. Next, after freezing fibers with liquid nitrogen was conducted grinding during freezing using a device performing grinding during freezing (device name: Linrexmill LX-1, about Sweden Hosokawamicron). Without sorting, etc. of the obtained particles were collected and measured the particle size of the instrument that measures particle size by laser diffraction. The result after a single grinding stage were obtained particles of the desired size (d50) less than 30 μm. As stage drying was removed after forming the coagulation liquid and washing the polymer with water in between crystals fibers was attended by a large quantity of water, and due to frozen water part containing the frozen water, became the starting points for faster grinding.

Example 2

A polymer solution in which was dissolved in sulfuric acid poly-p-phenyleneterephthalamide, was prepared and further formed with use of the device for forming through an air gap of a die in a coagulation liquid consisting of sulfuric acid and water. After washing with water and neutralization before the step of drying the yarn was twisted to get fiber. Moreover, the fineness of the fiber was 5830 decitex (fineness after drying: equivalent to 1680 dtex, number of filaments was 1000, and the water content was 71,2 wt.%. Further, the filament was cut into short fibers guillotine knife so that the cut-off length was 1,00 mm water Content in the obtained short fibers with the set 55.2 wt.%. As for the obtained short fibers has been carried out grinding during freezing using the same method and conditions as in example 1, and was measured particle size. Also after a single stage grinding this has resulted in particles with the desired size less than 30 μm, as in example 1.

Example 3

The fibers of the pulp obtained in example 1, without complete drying, the fibers with a weighted average fiber length 0.79 mm and water content to 21.4 wt.% were obtained after incubation for several hours at a temperature of 20°C with relative humidity of 65%.

The shredding of the fibers during freezing was carried out using the same method and conditions as in example 1, and was then measured particle size. After a single grinding as in example 1 were obtained particles of the desired size less than 30 microns.

Comparative example 1

After complete drying of the fibers obtained in example 1, controlled humidity, and were obtained fibers with a weighted average fiber length of 0.79 mm and a water content of 6.6%.

The shredding of the fibers during freezing was carried out using the same method and conditions as in example 1, and then was measured particle size. As a result of the low water content in hair is nah size of the obtained particles was equal to more than 100 microns. It happened, as it was expected, due to the complete drying, and as the water was completely removed from beneath the crystals, it has intensified the process of crystallization of the polymer, but there was not enough water to start grinding for freezing and therefore grinding during freezing has not led to fine grinding.

Comparative example 2

Grinding by freezing pulp (product name "Twaron® 1094", produced by Teijin Twaron, fiber length weighted average fiber length: 0.91 μm; content of water: 64,5 wt.%), here vysokomineralizovannyh fibers of poly-p-phenyleneterephthalamide, was carried out using the same method and conditions as in example 1, and then was measured particle size. As a result of the low water content in the pulp the size of the resulting particles was equal to more than 100 microns. It happened, as it was expected, due to the fact that after molding of the polymer solution filament were obtained by washing with water, neutralization and drying, and then were cut into short fibers, which were then subjected to mechanical processing so that they become vysokomineralizovannye, and to increase the yield of pulp. Further, the removal of water from between the crystals due to the stage of drying promotes crystallization of the polymer that is eleet the solid polymer and moreover, since the crystallization becomes irreversible, even if a large amount of water would contain once was a little water in between the crystals, and would be only in the pulp, grinding during freezing was achieved only minimal grinding.

Comparative example 3

Filament poly-p-phenyleneterephthalamide (product name "Twaron® 1000"produced by Teijin Twaron, fineness: 1680 dtex, number of filaments: 1000; water content: 5.1 wt.%) were cut by guillotine thus, to obtain a short fiber length of 1.0 mm

Grinding during freezing obtained short fibers was carried out using the same method and conditions as in example 1, was then measured particle size. As a result, the size of the obtained particles was equal to more than 100 μm, which is similar to the results obtained in comparative example 1, as suggested for the same reason.

The measurement results of the particle size obtained in the examples shown in the table.

Example 1Example 2Example 3Comparative example 1Comparative example 2 Comparative example 3
Water content (%)91,555,221,46,664,55,1
Stage dryingNoNoNoYesYesYes
d10(µm)9,112,214,270,6to 121.0199,2

Fully dried polymer weighed again, gave no small particles after grinding by freezing (Comparative example 2).

The particles obtained in this invention is particularly useful in the manufacture of highly abrasive materials used for brake, such as automotive disc brakes or drum brakes, or as materials-fillers for precision parts such as gears of polymeric materials, reinforced fiber, and the like.

1. The way to obtain completely para-substituted aromatic polyamide particles, comprising the following stages:
a) introduction of a solution of aramid polymer in the coagulation of the water-based liquid to obtain an aqueous molded product; and
b) grinding when not freeze or partially dried molded product having a water content of from 10 to 99 wt.%.

2. The method according to claim 1, in which the molded product is subjected to a stage of washing before chopping when not freeze or partially dried molded product, and stage leaching carry out water.

3. The method according to claim 1 or 2, in which the molded product is not dried when exposed to crushing when frozen.

4. The method according to claim 3, in which fully para-substituted aromatic polyamide is poly-p-phenyleneterephthalamide.

5. The method according to any one of claims 1, 2 or 4, which receive a pair of fully-substituted aromatice the Kie polyamide particles having a size distribution of particles of d50less than 75 microns, preferably less than 50 μm, most preferably less than 30 microns.

6. The method according to any one of claims 1, 2 or 4, in which the molded product is fibred, fibril, pulp, layered particle or the flock.

7. Particles completely para-substituted aromatic polyamide obtained by grinding when not freeze or partially dried molded completely para-substituted aromatic polyamide according to claim 1, having the dimension d50less than 75 microns, preferably less than 50 μm, most preferably less than 30 microns.

8. The use of particles of aramid polymer according to claim 7 as the filling material.


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6 cl, 2 tbl, 3 ex

FIELD: chemistry.

SUBSTANCE: invention relates to a granule used in making multi-component industrial articles with improved barrier properties and a method for thermal treatment of said granule. The granule has two sections. The first section contains an oxygen-sensitive component which does react with oxygen before bonding with a sufficient amount of promoter during stirring in a melt. The second section contains a promoter and component which is inert towards oxygen. The promoter is contained in an amount which is sufficient for initiating and/or catalysing the reaction between oxygen and the oxygen-sensitive component during treatment of the granules when stirring in the melt. The promoter may also be present in the first sectioned zone in an amount which is insufficient for initiating and/or catalysing the reaction between oxygen and the oxygen-sensitive component. The first and section sectioned zones are assembled into a side by side configuration. Not one zone surrounds the other in any plane of the granule. The method involves heating granules to a temperature ranging from 40°C to temperature which is at least 5°C lower than temperature at which the granules become liquid.

EFFECT: obtaining granules which can be stored in an oxygen-containing medium such as air, and can undergo thermal treatment in the presence of oxygen since the oxygen-sensitive compound cannot react with oxygen until final mixture in a melt.

67 cl, 7 dwg, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to a method for thermal treatment of polyester granules for fractional crystallisation, where molten polyester is fed into an underwater granulation system and granulates. The obtained granulated material is loaded at a short distance from the underwater granulation system into a device for separating the water/solid phase. The dried granulated material is fed into a treatment apparatus without supply or external energy or heat at temperature above 100°C, and thermal treatment for fractional crystallisation takes place due to inherent heat of the granulated material. The treatment apparatus is made in form of reactor which at least inclined, in which the granulated material is fed at temperature above 100°C, passes through it from the loading point to the discharge point under the effect of its own weight and comes out at temperature above 130°C.

EFFECT: disclosed thermal treatment method simplifies the process of fractional crystallisation owing to use of inherent heat of the granules.

7 cl, 2 dwg

FIELD: metallurgy.

SUBSTANCE: here is disclosed powder corresponding to composition with more retarded semi-period of crystallisation, due to which it can be implemented in die casting. Powder consists of at least two sections. The first section with the biggest surface area contacting air contains the first crystallising thermo-plastic resin (polymer). The second section contains the second crystallising thermo-plastic resin (polymer). At least a part of the second section is positioned between centroid of powder and the second section. Viscosity of melt of the first resin (polymer) differs from viscosity of melt of the second resin (polymer); in particular, viscosity of melt of the second resin (polymer) is higher, than viscosity of melt of the first resin (polymer). Also there is disclosed procedure for production of divided to sections powder with lowered gradient XB. Procedure consists in production of powder divided into sections. Further the first crystallising thermoplastic polymer is crystallised. Powder is heated at presence of moving force at temperature within an interval from 140°C to temperature at 1°C below temperature whereat the first crystallising thermo-plastic polymer turns into liquid. Finally powder is cured in temperature range at presence of moving force during time interval sufficient for raise of characteristic viscosity at least at 0.05 dcl/g.

EFFECT: produced sectioned powder possesses more prolonged semi-period of crystallisation, than homogenous mixture, facilitating decreased cycle of die casting in comparison to equivalent homogenous mixtures.

35 cl, 4 dwg, 6 tbl

FIELD: process engineering.

SUBSTANCE: proposed method can be used in armoring rocket solid propellant rocket charges, as well as in civil engineering, to be coated with TEPC-based polymer enclosures. Proposed method comprises shotting multi-component armoring composition based on thermo elastoplasts, dry mixing of components and subsequent plastification, homogenisation and extrusion of armoring mass in screw extruder. Note here that dry mixing of components lasts for at least 15 min. After mixing, 1-2%-solution of thermo elastoplasts in butyl acetate in introduced, in some 3 to 5 steps, into said mix of components. Content of said solution makes 10 to 15 percent by weight wit respect to armoring composition. Then armoring composition is discharged onto pans and uniformly distributed thereon to have layer thickness not over 10 mcm. Now, this composition is dried at 15 - 35°C for 3 to 12 hours and loaded into screw extruder to be extruded there in and cut into granules.

EFFECT: method of shotting TEPC-based multi-component armoring composition with higher homogeneity of granules and better thermo-physical properties, higher quality of armot and reduced power consumption.

1 dwg, 1 tbl, 1 ex

FIELD: chemistry.

SUBSTANCE: invention relates to polyester particles having small molecular mass gradient from the surface to the centre for making containers. Described is a particle made from polyester, particularly a homopolymer and copolymer of polyethyleneterephthalate which has characteristic viscosity of not less than 0.70 dl/g, crystallinity degree of at least 15%, acetaldehyde content of 10 parts per million or less and characteristic viscosity on the surface of the particle higher than characteristic viscosity at the centre of the particle by less than 0.25 dl/g, where molecular mass of the particle is increased in solid state. Also described is a method of making a container using the said polyester particles with characteristic viscosity of not less than 0.70 dl/g, involving feeding the particles into an extrusion zone, melting the particles in that zone to form a molten polymer composition and moulding a sheet or a component from the extruded molten polymer.

EFFECT: proposed polyester particle reduces loss of characteristic viscosity compared to traditional granules and enables to carry out the process at low temperature.

48 cl, 3 tbl, 4 ex

FIELD: pharmacology.

SUBSTANCE: polymer tablet includes oxygen-sensitive component, oxygen-indifferent component and reaction promoter. Oxygen-sensitive component is placed in first sectioned area, oxygen-indifferent component is placed in second sectioned area. Oxygen-sensitive component becomes oxygen-active in the presence of promoter. Promoter is represented by any substance initiating or accelerating reaction of oxygen-sensitive component with oxygen, and oxygen-indifferent component contacting promoter causes oxygen consumption increase not more than by 10% compared to oxygen consumption without promoter. Promoter amount in direct contact with oxygen-sensitive component is insufficient to initiate of catalyse reaction with oxygen significantly. Also invention claims other versions of polymer tablet and method of thermal tablet processing.

EFFECT: possible thermal processing of components in multicomponent tablets and/or storage in open air or in the presence of oxygen without significant quality deterioration.

178 cl, 4 dwg

FIELD: polymer materials and composites.

SUBSTANCE: composite granulate, consisting of cylindrical granules 1-2 mm in diameter and 3-4 mm in height possessing residual magnetization 0.4-0.5 mTl, contains: (i) high-pressure polyethylene or polypropylene; (ii) filler dispersed in granulate functioning as modifying additive and being represented by powdered magnetically hard strontium ferrite in concentration 5-25%; and dioctyl phthalate as plasticizing agent with residual magnetization 0.4-0.52 mTl (2%).

EFFECT: improved adsorption properties of filter materials based on fibers made from composite granulate of invention.

2 tbl, 2 ex