DE2930192A1 - METHOD FOR PRODUCING A SYNTHETIC FIBER MATERIAL AND DEVICE FOR IMPLEMENTING IT - Google Patents

Description

SHIP ν. FONER STREHL SCHDBEL-HOPF EBBINGHAUS FINCK 2930192

description

The present invention relates to methods and apparatus for the production of synthetic fiber pulp, the invention can be most successful in the production borrowed from papierahn and non-woven, e.g. nonwovens can be applied.

Notwithstanding the fact that paper-like materials based on several synthetic polymers were more than Having been manufactured for 20 years, the problem of providing a simple and inexpensive technology for manufacturing is lost of synthetic fiber mass is still not important today. An indirect confirmation of this fact provides a large number of patents issued in many countries on various methods of fibrillation of Polymers

One of the first technological processes to manufacture

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The production of synthetic fiber pulp, which is suitable for the production of paper-like materials, is ours In my opinion, the fibrid method (see BE-PS No. 564-206 and FR-PS No. 13504-55) “The fibrids are polymeric anisodiametric Particles and have the form of loosened or interconnected flakes, lamellae, fibers and or or bands on «. The mass preferably contains a mixture of some types of these structures · The method of making fibrids involves dissolving a polymer in a solvent and pouring it the solution obtained in a filling liquid under its continuous agitation or whirling provided "

According to the aforementioned French patent, a polymer solution is added dropwise to a precipitant added «

Under the action of stirring the precipitation liquid When shear stresses occur, the droplets are given the shape of the structures described above and the polymer precipitates with the formation of a synthetic fiber mass. After the precipitation, the fiber mass is released from the solvent and the precipitation liquid deposited. It goes without saying that the performance with such technology as a result of the dropwise introduction of the solution into the precipitation liquid is extremely low is the implementation of the procedure described with a

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n a considerable consumption of solvent and precipitation liquid connected, since the solvent and precipitant after the deposition of fibrids is repeated in the process cannot be used The use of high-speed J-agitators according to BE-FS Kr 564206 made it possible to accelerate the process of introducing a polymer solution into the precipitation bath significantly * The one for the actual The main features of the process - a large consumption of solution and precipitation initia t 1, impossibility of direct Use of the mixture of solvents and precipitation agents in the process without a complicated regeneration of the Components of the mixture - but remained · The fibrids basically have an amorphous structure and are characterized by a relatively low strength «

Several attempts have been made to use the method cheaper and to increase the output in the production of synthetic fiber pulp "

Among other things is a procedure. known which in the dissolution of a synthetic polymer in a suitable Solvent at temperatures above the boiling point of the solvent, injection of the polymer solution from the high pressure to the low pressure zone with simultaneous evaporation of the solvent or part of it and Subsequent purification of the polymer from the solvent consists «The process is essentially for manufacturing

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ORfGfNAL INSPECTED

of polymeric fiber masses of ^ polyolefins applicable (GB-PS 1416894, FR-PSs 2255398, 22554000, 2221543, ■ 2258469; US-PSs 3891499, 3902957, 3904804, 3920509, 3920507; JA-PS 50-13385, Natl. Cl. 47E0, 47E 21).

There is also known a process for the production of a synthetic paper stock, which is available from the company "Crown Zellerbach International Inc. "and described in SU-PS No. 457231 and US-PS No. 38914-99.

According to this proposal, a synthetic made of a thermoplastic polymer material * which is suitable for the production of paper, prepared at a rapid evaporation of the solvent from a polymer solution) in which there is a rapid precipitation of the polymer, ta be observed special evaporation conditions so that in the subsequent a baffination is made possible, whereby a paper stock consisting of individual paser elements is produced «

Notwithstanding that the according to the known method produced fabric has paper-forming properties (The strength of this paper exceeds that of ordinary cellulose paper), the manufacturing technology shows

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Such a substance has a number of disadvantages, which include being costly and complicated to use Pressure equipment, as well as complication of the technological process due to compulsory application of Eaff ineuren exist.

The known method is characterized by an unequal ' precipitation from,. which leads to the production of an easermass which has sufficient thermal stability of the manufactured substance does not secure. In addition, the strength of the fibers is mainly due to the amorphous. Structure poor, which has a negative effect on the strength of the end product manufactured.

In our opinion, a more promising technology is one in which a polymer is deposited from the solution by crystallization (see DT-AS Hr · 1660634 ·). According to this patent specification, the above-mentioned process for the production of polymer fibers consists in dissolving a polymer ( oC polyolefin) in an organic solvent, cooling the solution produced to the crystallization temperature of the polymer, crystallization of the polymer with continuous or discontinuous stirring of the solution and deposition of free Morphological crystallized structures from the solvent · The free morphological polymer structures formed have predominantly "shish kebab" structures.

The "Shish-Kebab" structure creates a thread-like cri-

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"" ORfGlNAL INSPECTED

stable structure, which has a central fiber, perpendicular to the crystal elements at a certain distance from each other are distributed. Compared to the fibrids of a predominantly amorphous structure, the fibers of the crystalline Fiber mass has a higher strength, which ensures better mechanical properties of the paper-like material be what an undoubted virtue of the one described Procedure exists "

However, such a technology can only be used for the production of synthetic mass from oL polyolefins »The investigations showed that polyamides, polyesters, polyurethanes and other polymers practically no free morphological structures from the hyp" Shish-Kebab "when they are used in this process. · Are formed · This significantly limits the raw material base and the range of end products «In addition, the need for fast drilling makes the tough. Polymer solution requires a significant expenditure of energy «It should also be pointed out that the structures formed during stirring of a structure of the" Shish-Kebab "type are destroyed by QuJ.Tlflügel, while the greater the dimensions of, the better the binding capacity of the fiber mass free morphological structures are · an extremely important disadvantage «; represents the deposition of fiber bundles on the agitator blades of the agitator, which makes it difficult to carry out a continuous process for the production of a fiber mass «

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Concrete examples of the technology discussed testify that the accompanying the stirring process Disadvantages due to a simple exclusion of the guiding process in most cases it is practically impossible to avoid this. This is due to the fact that the crystallization aJ

tion of polymers with the agitator at a standstill and compliance with the temperature values provided by the technology either does not take place at all, or is extended to several days * In the second lalle occurs Part of the solution simultaneously with the formation of fine crystallization structures in the form of gel or crumbs the end"

The invention is based on the object of a method and a device for the production of synthetic To develop fiber mass, through its operating parameters? and structural features conditions for a fast-moving Crystallization of a polymer can be guaranteed without stirring the solution «

The task set is in a process for the production of synthetic fiber mass, which the dissolving * Solution of a crystallizable polymer in an organic solvent '* Cooling of the resulting solution for crystallization of the named polymer and separation of morphological crystallized structures from the solvent provides .Invention according to the fact that the cooling at a rate of 0.1 to 5 O / min a temperature which is the lower melt dissolving temperature

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of the polymer in the solvent used by 0.5 to 40 ° C falls below, for the crystallization of the mentioned polymer with the formation of free morphological structures, mainly made of spherulites and "Shish-Kebab" structures ·

Under such cooling conditions in a solution without their stirring takes a relatively rapid development and intensive growth of free morphological structures, mainly spherulite and "shish kebab" structures rather than _# Here and further is unigr the technical term "spherulitic" a spherical crystal form Polymers understood, which is made up of fibrillar and lamellar crystals that grow from a polymerization nucleus *

Eliminating the need to stir the viscous polymer solution allows the specific energy input to significantly reduce the production of a synthetic fiber mass. As it turned out, a synthetic fiber mass not only made of o (_- polyolefins, but also practical Manufacture from all crystallizable polymers · In addition, the crystallization without drilling reduces the damage and destruction of free morphological structures formed is practically prevented.

• It is useful to have a polymer during its dissolution Cooling after reaching the lower melt dissolution temperature of the polymer a suspension of free morphological

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-'14 -

Adding structures in an organic solvent · This allows larger free morphological structures to be added and thereby improve the binding capacity of the synthetic! "asermasse»

By the same factor it is possible to obtain a tight composition of free morphological structures favored "

The solution of a polymer is expediently the suspension of free morphological structures in an organic one Solvent in an amount of 0.1 to £ 0 weight percent based on the polymer. This is where the effect is most noticeable «

The simplest and most suitable for production are the suspension and the solution from the same organic solvents and to manufacture polymers «

It is advisable to keep the above-mentioned solution of a polymer at this temperature for 1 to 60 minutes after cooling to a temperature which falls below the lower melt-dissolving temperature of the polymer by 0.5 to 40 ° C. In most cases this time is sufficient for most of the polymer to crystallize.

To increase profitability, it is useful » to cool the solution of a polymer to a temperature which is the lower melt-dissolving temperature of the polymer in the the solvent used falls below 10 to 40 C,

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and to mix the free morphological structures formed and separated from the solvent with fibers * thereby it is also possible to give the fiber mass and the fabric made from it the desired properties. When mixing with synthetic fibers, it is advantageous that at most free morphological structures 30% smaller than 50 µm

Best results will be obtained when mixed with minral fibers Achieved if of free morphological structures no more than 10% are smaller than 10 µm *

It is desirable that when blended with natural fibers at most 50% of free morphological structures smaller than 10 um «

For the production of synthetic fiber mass, which is used for the fabrication of an intermediate layer in electrolytic capacitors to be used paper is suitable, it is appropriate to use polyamide as the polymer and its from Solvent-secreted free morphological structures, of which at most 20% are smaller than 20 μm, with 20 to 40 ° C SR of ground cellulose in the below to mix the specified ratio (in% by weight):

Cellulosic fibers 20-95

free morphological structures of polyamide 5-80.

It is advisable to combine the free morphological structures of polyamide with cellulose in the following ratio (in % By weight):

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Cellulose fibers ·. ·. 50-80

free morphological structures of polyamide 20-50, This ratio gives the best results *

For the production of synthetic fiber mass, which is suitable for f fabrication of Preßspanteilen with reduced Dielektrizitätskennzahl, it is to be applied suitably _f polyamide as the polymer and its separated from the solvent-free morphological structures of which at least 80% are in a size range of 2 to 50 yum, to be mixed with cellulose fibers in the following ratio (in% by weight):

Cellulosic fibers 50-95

Free morphological structures of polyamide 5-70 · The free morphological structures with Mix cellulose fibers in the following ratio (in weight " "):

Cellulosic fibers 40-80

free morphological structures of polyamide 60-20. The object set is also achieved in that in a device for carrying out the method, which ' a chamber for dissolving the polymer, a buffer capacity, which is connected to the mentioned chamber, and a crystallizer, which through a pipeline with the buffer capacity is in communication and is designed in the form of a container with a split cooling jacket, and a device to separate the crystalline mass from the organic

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see solvents, which with the exit of the crystallizer is connected, contains, according to the invention, a second drilling line with a heat exchanger, which supply line and Has discharge stubs for coolant, parallel to the buffer capacity and the inlet of the crystallizer connected to the first pipeline mentioned above

The above-mentioned structural design of the device allows it to realize the preferred execution of the method according to the invention «

To ensure control of the crystallization rate and the change in the size of the structure, it is necessary to use the aforementioned nozzle of the said heat exchanger to be provided with adjustable throttles "

It is advantageous that the cross-sectional area ratio of the mentioned second pipeline and the mentioned first Pipeline is in a range from 0.001 to 0.3 «In In this area, such a quantitative ratio of suspension and polymer solution is secured, in which the enlargement effect the dimensions of spherulites and "Shish-Kebab'V .t Structures is maximum "

To ensure the effective change in the dimensions of structures in the continuous process is mentioned in the second pipe in series with said heat exchanger a controllable valve arranged

It is useful to implement a technology in which a holding time of more than 60 minutes is provided

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ORIGINAL INSPECTED

Intermediate container, which has a temperature control jacket, to the exit of the crystallizer and to the device to be connected to the separation of the crystalline mass of the polymer from the organic solvent *

Furthermore, the essence of the invention will become apparent through a detailed description of the method and the device its implementation is explained with reference to the accompanying drawing, in which a basic scheme a device according to the invention is shown

The method for the production of synthetic fiber mass is carried out according to the invention with the aid of a device shown in the accompanying drawing is equipped with a gear metering pump 4 "A feed pipe 5 for solvents is connected to the chamber 3, which is connected to a metering device 6" In the chamber 3 there is a shaft 7 which has blades 8 and is provided with a drive for rotating it «By a drilling line 10, the chamber 3 is connected to a buffer capacity 11. The buffer capacity 11 is connected to the inlet of a crystallizer 12 by two parallel drilling lines 13 and 14. The drilling line 14 contains a heat exchanger 15 according to the invention. The drilling line 13 is with a valve 16 equipped the poor

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Exchanger 15 has nozzles 17 and 18 ″ to feed and discharge of the coolant to · In a preferred embodiment of the device, the area ratio of the area of the pipeline is 14 and the drilling line 13 from 0.001 to 0.3. In row with the heat exchanger 15 is a controllable valve 19 in of the drilling line 14 and 21 equipped. The crystallizer 12 is designed in the form of a horizontally arranged cylindrical container, which has a split cooling jacket 22 · The exit of the crystallizer 12 is through a drilling line 23 with a Device 24 for separating the crystalline mass of the polymer from the solvent connected * The device 24 can be used in Executed in the form of a centrifuge, a filter or a settler be. In the pipeline 23 is a controllable valve 25 mounted *! [Parallel to pipe 23 is to the outlet of the crystallizer 12 and an intermediate container 28 connected to the device 24 with the aid of nozzles 26 and 27, which contains a temperature control jacket 29. The nozzle 26 and 27 are provided with valves 30 and 31.

A synthetic fiber mass is produced in the following manner by means of the device described. A crystallizable one Polymer is poured into the melting vessel 1 and in the presence of a small amount of an organic solvent on the melting temperature is heated. Through the gear metering pump 4

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the polymer melt via the drilling line 2 into the chamber 3 conveyed «At the same time, an organic solvent is conveyed into chamber 3 by the dosing device 7 · Through the drive 7, the shaft 9 is set in motion, whereby the polymer melt and the organic solvent through wing 8 should be stirred intensively «During the mixing process, the polymer dissolves« The polymer solution is through the buffer capacity 11 is passed into the crystallizer 12 «Io Kristallisacor 12 is the polymer solution according to the invention

a rate of 0.1 to 5 C / min to a temperature

cooled, which falls below the lower melt dissolving temperature of the given polymer in the given organic solvent by 0.5 to 40 ^° C. During the cooling, the polymer crystallizes with the formation of free morphological structures, preferably spherulite and "shish kebab" structures, The cooling temperature and the cooling rate of the solution are regulated by changing the flow rate of the solution through the crystallizer 12 with the aid of the valve 25 and by changing the temperature of the coolant in the divided cooling jacket , the suspension enters the drilling line 23. If, however, a long holding time (more than 30 minutes) is required for the end of the crystallization, the valve 25 is closed and the valves 30 and 31 are opened. The solution enters the device 24 through the Intermediate container 28, in

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ORIGINAL INSPECTED

which a constant temperature is maintained, the the temperature of the solution at the exit of the crystallizer 12 is the same, and the crystallization of the polymer is terminated. The crystallized free morphological structures are removed from the organic solvent with the aid of the device 24 separated by known methods (by centrifuging, filtering or separating in a gravity separator).

After the suspension has been separated out, a synthetic fiber mass is obtained «

According to a preferred variant of the method, a synthetic fiber mass is essentially based on that described above Much is made, but the polymer solution is used to accelerate the crystallization process the suspension of free morphological structures in an organic one Solvent added * The said suspension is added during the cooling of the polymer solution after reaching the lower melt dissolving temperature of this polymer in the solvent used «

The mentioned suspension is made from the same polymer and the same solvent used for the production of synthetic fiber mass can be used The suspension is added to the polymer solution in an amount of 0.1 to 30% by weight (based on the polymer) supplied · To carry out this variant of the technology according to the invention, the valve 19 and the adjustable throttles 20 and 21 open. Thereby be * - The circulation of the coolant begins through the heat exchanger 15 and part of the polymer solution is released from the buffer capacity

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in the drilling line 14- passed. This part of the polymer solution is by flowing through the heat exchanger 15, cooled and germs of free morphological structures (spherulites, "Shish-Kebab 'VStrukturen, adrithen or single crystals).

The suspension fed through the pipeline 14 is in the crystallizer 12 with the flowing through the pipeline 13 Polymer solution mixed. The germs of free morphological Structures become centers of crystallization and guide the formation and growth process of spherulites and "Shish-Kebab" structures a «

If necessary, the suspension consumption is calculated using the \ Valve 19 adjusted while the size and number of seed structures can be adjusted with the help of chokes 20 and 21.

According to one variant of the method, the polymer solution in the crystallizer 12 is cooled to a temperature which falls below the lower melt dissolution temperature of the polymer in the solvent used by 10 to 40.degree. The free morphological structures that have crystallized out under these treatment conditions and separated from the solvent are mixed with fibers. Different embodiments of this process variant are possible, which make it possible to produce a synthetic fiber mass with different properties. In particular, the free separated from the solvent become morphological

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Structures of which at most J> 0% are smaller than 50 μm, mixed with synthetic fibers «

According to another variant embodiment, the solvent deposited free morphological structures, of which at most 10% are smaller than 10 µm, with mineral fibers mixed · According to a third variant of the embodiment, the free, separated from the solvent, become morphological Structures of which at most 50% are smaller than 10 Aim are mixed with natural fibers "

Two other process variants permit a synthetic one

To manufacture fiber mats, which are used for the manufacture of paper

-Share ren for JELectrolytic capacitors and pressboard with reduced Dielectric number is suitable for electrical engineering · According to one of these process variants uses polyamide as the polymer and the polymer that is separated from the solvent free morphological structures, of which at most

20% smaller than 20 µm are made with cellulose fibers, we Ιο y
before 20, .. 40 SR are ground, in the following ratio

(in% by weight) mixed:

Cellulose fibers ......... 20-95

free morphological structures of polyamide. 5-80. According to the second variant of the process, polyamide is used as the polymer and its separated from the solvent free morphological structures, at least 80% of which are from 2 to 50 µm in size, are made with cellulosic fibers in the following Ratio (in% by weight) mixed:

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Cellulose fibers. 30-95

free morphological structures of polyamide. 5-70. Below are specific embodiments of the invent according to the procedure. The synthetic composition obtained in these examples was used to produce paper-like materials are used. The fabrics have been subjected to various tests, the following being distinguished Methodologies.

Determination of tensile strength and elongation at break.

The method "is based on determining the size of the Breaking load and elongation at break.

Vertical tensile testing machines with pendulum are used for testing tester, mechanical drive and strain gauge used.

The machines have flat clamps for fastening the paper and cardboard strips of the required width. Of the The distance between the clamps is 180 ± 1 mm in the initial position.

The rate of loading is set in such a way that the test piece breaks after 20 to 5 seconds after it becomes effective the load takes place.

The ^ results of the testing of specimens, which in broken at a distance of less than 10 mm from the clamps are not taken into account. The width of the paper strip is 15> +0.1 mm.

The tensile strength (u) in kp / mm is calculated according to the equation

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ORfGlNAL INSPECTED

bra
determined.

Herein means:

b - width of the test piece, mm;
h - average thickness of the specimen, mm; R - breaking load (arithmetic mean of 10 measurements) ^ kp.

The relative elongation (<£) in percent is called arithmetic Means expressed by direct readings. If the reading is in millimeters, the elongation will be determined according to the following equation:

8 = ^ LJL 100%

Herein means:
^ 1 - average elongation value, mm;

JL - initial length of the working section of the test piece, mm.

The specific breaking load in the tensile test (P) in kp / mm is determined using the following equation:

Herein means:

h- average thickness of the test piece, R - breaking load, kp.

* Dielectric constant (the method is based on determining the ratio

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the electrical resistivity of one with the K electrolyte impregnated paper to the specific electrical resistance of the electrolyte, which under given conditions are measured

The measurement is carried out on an electrode cell with cylindrical electrodes made of stainless steel. The electrode diameter should be 2.50 ± 0.01 cm, while its thickness should be at least 0.5 cm. The electrodes should have a contact area with a Sundung radius on the strip comprise from 0.25 cm * the electrode cell has a device for pressing the electrodes on the test piece, through which a pressure of 0.20 ± 0.02 kg / cm (2.0 ± p, 2 '10 ^4' Pa) is produced·

With the measuring device described above, the measurement of the electrical resistance is in a range of 0.01 to 30 kSL with a measurement error of at most 3% a frequency of at least 3 kHz guaranteed «

The paper to be tested is folded twice and specimens are made with dimensions of at least 30x30 cm cut out «

The electrolyte is made up by dissolving 100 g of ammonium » pentaborate in 675 ml of ethyl glycol and a maximum of 30 ml of distilled water produced in a tilas with a capacity of 1 1 when heated to a temperature of 60 to? 0 ° C « The specific electrical resistance of the electrolyte at a temperature of 25 ° 0 is 700 to 100052./csu

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ORfGlNAL ₁ NSPECTED

The sample to be tested is placed in the glass with electrolyte introduced with a fit of 0.1 1 and at Maintained 25 ° C for 15> ± 1 min.

The specimens to be tested are after the removal of the excess electrolyte (for this they are removed from the electrolyte and left on the glass wall for 1 min) between placed in a thermostat to the electrodes of the device for measuring the resistance of the impregnated paper

held at 25 C for 15 to 16 min, after which the resistance of the respective sample is measured

The dielectric constant (^) is based on the following Calculated equation:

a.

Herein means:

r, - electrical resistance of the impregnated paper specimen, SH. ;

P- specific electrical resistance of the electrolyte, -SH / cm j

d - thickness of the double folded paper test piece, cm;

D - diameter of the contact area of the electrodes, cm;

Determination of the dielectric strength with alternating voltage

(with a frequency of 50 Hz) The test electrodes, which have reliable contact with

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to ensure the test piece to be tested are made of stainless steel, non-ferrous or precious metals. The measurement takes place on cylindrical electrodes of different Diameters, the diameter of the lower electrode at least is three times larger than the diameter of the top electrode. Preferably, the top electrode has a diameter of 25 ram and a height of at least 25 ranif during the Diameter of the lower electrode 75 mm and the width 15 mm · The pressure on the test piece, which is arranged between the electrodes, should be (20 ± 10) · 10 Pa.

Through the supply current source of the system, the test transformer and the control device is on the test piece to be tested a sinusoidal curve of the test voltage with a frequency of 50 Hz, so that the amplitude factor of the test voltage (the ratio of the peak value to the effective value) is in a range of 2 ^ 5%. Through the Hegel facility a stepless voltage regulation is to be guaranteed, so that the breakdown is in a range of 10 to 20 Y from the beginning the voltage increase takes place «The tests are not folded paper. The average breakdown voltage value (U,) in V _ "is used as an arithmetic Average of 20 measurements calculated

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Herein means:

U ^ - breakdown _{voltage in V eff}

The dielectric strength (% _s ) ^ ⁰ - kV _{eff #} / mm is determined according to the following equation:

Herein means:

cLj - nominal thickness of the paper, mm «

To determine the l ^ _{s of} an impregnated material, the material is impregnated, as explained in the methodology for determining the dielectric coefficient. The impregnation is carried out with converter oil «The impregnation liquid must not have any influence on the material being tested *

Determination of the dielectric loss factor and the dielectric constant at a frequency

of 50 Hz

The requirements for the surface quality of electrodes are the same as for determining the dielectric constant and the dielectric strength "

The test pieces are kept at a temperature of ⁰

and a best pressure of 1.33 · 1CT ² 3? ^a i® run of 2 + 0.5 dried «The diameter of the two electrodes is 50 + ρ, ΟΙ mm» The electrodes should have a contact surface with a radius of 0.15 cm on the band and a device

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have device for pressing the electrodes against the specimen through which a bridge of (2.0 ^ 0.2). 10 ra is generated.

The measurement takes place in a chamber when required Temperature and a best pressure of 1.33 1Ο Pa,

The dielectric loss factor and the dielectric constant are determined with the help of such systems, which Allow measurements by any method provided that the device used in determining of the dielectric loss factor guaranteed measurement errors in a range of ± (5% * - 0.0002) and when determining the Capacity - lies in a range of i (i% f1 pF) »

When measuring on the test piece, a sinusoidal curve should be used the test voltage with a frequency of 50 Hz be so that the amplitude factor of the voltage in a range of 2 ± 5% is «

The measuring voltage is 1000 V.

The dielectric loss factor is shown on the basis of device displays determined »The reading error must not exceed ± 10%.

Determination of the dielectric constant (£) of test pieces soaked with transformer oil The requirements for the surface finish of the Electrodes are the same as for determining the dielectric constant and dielectric strength.

The test pieces are at a temperature of 10 ^ 5 0 and a core pressure of 133 to 660 Pa over the course of 24 hours

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iNSPECTED

The dried and soaked with dry hot (transformer oil with a temperature of 90 + 2 ⁰ G in the course of 4 hours Measuring electrode, mm -75

Diameter of the high voltage electrode, mm -100 Width of the guard ring electrode, mm - 10

Clearance between the measuring and guard ring electrodes, mm - 2 Pressure of the measuring electrode on the test piece, kPa - 9 »8 The dielectric constant is determined with the help of systems that allow a measurement by any method, provided that the measurement error in the Determination of the capacitance ± (.Λ ° Μ · 1pF) does not exceed * During the measurement on the test piece, a sinusoidal curve of the test voltage with an frequency of 50 Hz should be ensured so that the amplitude factor of the voltage is in a range of 2 ± $% .
The measuring voltage is 1000 V.

The tests are carried out on test pieces immersed in transformer oil.

The dielectric constant of the material is determined using the following equation:

S.

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Herein means:
£ - dielectric constant;
J- 3

C - capacity of the normal capacitor, in cm; JL · phase-free normal resistance of 318 $ O5E; h - bead of the sample, cm;

S - area of the measuring electrode, cm $

R, - resistance, Si «
Example 1.

A synthetic saser mass was made in the following manner according to the present invention manufactured.

12 parts by weight of isotactic polypropylene were dissolved in 150 parts by weight of oleic acid. (The lower dissolution temperature of the isotactic polypropylene in the oleic acid is 14-Q ⁰ C) To accelerate the dissolution process, the isotactic polypropylene was dissolved at a temperature of 160 ° C. After the polymer had completely dissolved, the solution obtained was increased to a temperature of 100 0 (ie 40 ⁰ O below the lower temperature of the polymer in the solvent mentioned) cooled at a rate ^ of 1 ° C / min. The solution was kept at a temperature of 10O ⁰ O over the course of 20 minutes. The free morphological structures which crystallized out were separated from the solvent and washed. The synthetic fiber mass obtained was examined with the aid of an optical microscope. The investigations carried out have shown that the

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ORfGlNAL INSPECTED

free morphological structures predominantly represent "Shish-Kebab ¹¹ -structures · At most 5% of free morphological structures were smaller than 50 µm ·

The fiber mass obtained can be used as a fibrous binder for the production of paper-like materials. In addition, a film material can be produced directly from the fiber mass, which consists of free morphological structures consists.

A film material was obtained from the fiber mass obtained as described above by producing a suspension of free morphological structures in the water, pouring, pressing and (drying of the material obtained.

The film material produced had the following characteristics

Density, g / cm ⁵ 0.3?

Thickness to ...... 140

Tensile strength, kp / mm ² 0.09

Example 2,

EdLne synthetic fiber mass was according to the invention as follows manufactured,

8 "parts by weight of nylon-6 became 50 parts by weight Propanol and 50 parts by weight of distilled water mixed C is the minimum dissolution temperature of nylon-6 in the above specified solvent is 162 0). To accelerate the dissolution process of the polymer mentioned, the obtained mixture heated to a temperature of 175 ° 0

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After complete dissolution of the polymer, the obtained solution to a temperature of 122 ° C (ie 4O ° 0 below the lower dissolution temperature of Wylon-6 in the aforementioned solvent) was treated with öiner rate of O _t 1 ° C / cooled min and at this temperature Held for 20 minutes. The crystallized free morphological structures of nylon-6 were separated from the solvent by centrifugation. The synthetic fiber mass obtained was examined with the aid of an optical microscope. The tests carried out showed that the free morphological structures were predominantly spherulites with an average particle size of 80 to 85 µm represent. Example 5,

A synthetic pulp was made according to the invention as follows manufactured"

10 parts by weight of polyoxymethylene were mixed with 80 weight parts of 3 caprolactam and 20 parts of distilled water mixed (the minimum dissolution temperature of the polyoxymethylenes in the above-mentioned solvent is 150 C) ₉ The mixture prepared was to accelerate the Lösungsvor-f transition of said polymer to a temperature of 170 0 warmed up. After the polymer had completely dissolved, the solution obtained was cooled to a temperature of 130 ° C. (ie 20 ° C. below the lower melt dissolution temperature of the polyoxymethylene in the solvent mentioned) at a rate of 5 ° C./min and at this temperature for 40 minutes

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ORONAL INSPECTED

held long. The crystallized free morphological structures of polyoxymethylene were from the solvent deposited by centrifugation. The obtained synthetic fiber mass was examined with the aid of an optical microscope. The investigations carried out have shown that the free morphological structures are predominantly spherulites with a average size from 70 to 85 pm.

Example 4.

A synthetic fiber pulp was produced according to the invention as follows.

6 parts by weight of Wylon-6 were mixed with 50 parts by weight of propanol and 50 parts by weight of distilled water mixed (the lower dissolution temperature of Wylon-6 in the above-mentioned solvent is 162 ° C). The resulting mixture was used for acceleration the process of dissolving the polymer mentioned is heated to a temperature of 175 ° 0. After complete dissolution of the polymer, the resulting solution was heated to a temperature of 135 ° C (i.e. 27 C below the lower dissolution temperature of nylon-6 in the mentioned solvent) at one rate cooled by 1 ° 0 / min and held at this temperature over the course of 15 min. The crystallized free morphological Structures of Uylon-6 were made by the solvent Spin deposited. The synthetic fiber mass obtained was examined with the aid of an optical microscope. the Investigations carried out.; have shown that the free morphological structures predominantly spherulites with a

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average particle size of 75 to 85 μm, with a maximum of 15% of the spherulites being smaller than 50 μm,

Example 5

A synthetic fiber pulp was made in the following manner in accordance with the present invention manufactured· ·

A narrow fraction of polyoxymethylene with a molecular mass of 55,000 was mixed with <£ -caprolactam (the lower solution temperature ... of this polyoxymethylene in the above-mentioned solvent is 140 ⁰ ). The mixture obtained was heated to a temperature of 170 ° C. in order to accelerate the dissolution process of the polymer mentioned The melting dissolution temperature of the given fraction of polyoxymethylene in the solvent mentioned) was cooled at a rate of 0.1 ° C./min and held at this temperature for 96 hours. The obtained synthetic

The fiber mass was examined with the aid of an optical microscope. The investigations carried out have shown that the free morphological structures predominantly with spherulites an average size of 2500 µm represented example 6 (negative).

A synthetic fiber pulp was prepared essentially in the manner described in Example 2, except that the

030008/0680

ORIGINAL INSPECTED

Process technology was somewhat disrupted by bringing the resulting solution of the polymer to a temperature of 161.7 O (i.e. 0.3 C below the lower temperature of dissolution of nylon-6 in the mentioned solvent). the The cooling rate of the resulting solution of the polymer was 2 C / min.

The holding time of the two-phase system obtained at a temperature of 161 _f 7 ° G was 80 hours

No crystallization took place under such conditions

Example 7 (negative).

A synthetic fiber composition was prepared substantially as described in Example 2, but with the process technology has been somewhat disturbed by the solution (ie, 50 ° 0 below the lower dissolution temperature of the polymer in the solvents mentioned) to a temperature of 112 ⁰ C cooled became.

The cooling rate of the obtained polymer solution was 2 ° C / min.

The holding time of the obtained two-phase system at a temperature of 112 ° C. was 0 minutes. The fiber mass consisted of spherulites of nylon-6, of which 80% by weight were not larger than 15 μm «

The application of such a synthetic fiber mass as of a synthetic fibrous binder was impossible

030008/0680 ORIGINAL! MSPSCTED

like their independent exploitation. Example 8 (negative).

A synthetic fiber mass was produced essentially in the manner described in Example 2, but the process technology was somewhat disrupted by the | Solution was cooled to a temperature of 142 ⁰ C (ie 20 C below the lower melt dissolving temperature of the polymer in the solvent mentioned) at a rate of 6.5 C / min, which exceeds the cooling rate specified in the claims by 1.5 C / min .

The holding time of the two-phase system obtained at a temperature of 142 ° C. was $ 0 min.

There were spherulites of nylon-6 obtained, of which 70 Gew.j. were smaller than 20 µm. The application of such a synthetic Pulp as a synthetic fibrous binder is impossible in the same way as their independent exploitation.

Example 9 (negative).

A synthetic pulp was produced as follows. ■

10 parts by weight of isotactic polypropylene were dissolved in 150 parts by weight of oleic acid (the lower melt-dissolving temperature of isotactic polypropylene in oleic acid is 140 ° C.). The mixture obtained was used to accelerate the dissolution process of the polymer mentioned. a temperature of 160 ⁰ C is heated. After the polymer had completely dissolved, the resulting solution was heated to a temperature of

030008/0680

'G (i.e. 5 ° G below the lower melt dissolution temperature of the polymer in the mentioned solvent) at a rate of 0.05 ° C / min, i.e. Oy05 ° G / min below that in the claims specified SPEED and cooled down at this temperature was maintained over the course of 48 hours.

No crystallization took place under such conditions

Example 10.

According to the invention, a synthetic mass was made as follows manufactured"

9, parts by weight of nylon-6 were mixed with 50 parts by weight Propanol and 50 parts by weight of distilled water mixed (the lower temperature of dissolution of nylon-6 in the mentioned solvent is 162 G). The mixture obtained was used to accelerate the dissolution process of the polymer mentioned heated to a temperature of 175 G

After complete dissolution of said polymer, the solution (ie, 15 ° G below the lower dissolution temperature of nylon 6 in the mentioned solvents) at a temperature of 147 ° C at a rate of 0.1 ⁰ C / -. min cooled, the suspension of spherulites in the same solvent in an amount of 10% by weight, based on the polymer, being introduced into the solution mentioned at a temperature of 160 ° C. After reaching a temperature of 147 ° 0, the two-phase mixture obtained was held for 40 minutes

030008/0680

Yakuumfilter separated from the solvent. The average The size of the spherulites obtained was 115 to 120 Aim.

Example 11.

A synthetic fiber pulp was made in the following manner in accordance with the present invention manufactured.

8.5 parts by weight of nylon-6 were te ile with 50 parts by weight Propanol and 50 parts by weight of distilled water mixed (the lower dissolution temperature of nylon-6 in the mentioned Solvent is 162 ° C). The mixture obtained was used to accelerate the dissolution process of the above-mentioned polymer

heated to 175 0.

After the above-mentioned polymer had completely dissolved, the resulting solution was up to a temperature of 145 (i.e. 17 C below the lower temperature of dissolution of nylon-6 in the mentioned solvent) at one rate cooled by 4 C / min, wherein in the solution mentioned at a temperature of 160 C, the suspension of spherulites in based on the same solvent in an amount of 10% by weight on the polymer. After reaching a temperature of 145 O was the obtained two-phase Mixture held for 25 minutes. The crystallized Free morphological structures, which were spherulites, were removed from the solvent with the help of a vacuum filter deposited. The average size of spherulites obtained was 80 to 85 µm.

030008/0680

ORfGfNAL INSPECTED

Example 12.

A synthetic fiber mass was produced according to the invention in the following way «

12, parts by weight of polyoxymethylene were mixed with 100 parts by weight of £ caprolactam mixed (the lower dissolution temperature of the polyoxymethylenes in the mentioned solvents is 14-5 ° C) · The resulting mixture was heated to speed up the dissolving process of the said polymer to a temperature of 166 ⁰ C * After the complete dissolution of the polymer mentioned, the solution obtained was cooled to a temperature of 120 ° C. (ie 15 ° C. below the lower dissolution temperature of the polymer in the mentioned solvent) at a rate of 2.5 ° C./min of 14-3 ° G, the suspension of spherulites in the organic solvent (£ caprolactam) in an amount of 0.1 wt.%, based on the polymer, was introduced · the resulting two-phase system was stirred at a temperature of 120 ⁰ C 40 held for min

The crystallized free morphological structures were removed from the mentioned solvent with the help of a vacuum filter secluded *

The synthetic fiber mass obtained was examined with the aid of an optical microscope. The investigations carried out have shown that the free morphological structures were predominantly spherulites, the average size of which was 120 to 125 m .

030008/0680

Example 13.

The same procedure as in Example 12 was followed, but into the solution of polyoxymethylene in an organic solvent (£ -Caprolactam) at a temperature of 143 C the Suspension of spherulites in a similar solvent

in an amount of 10% by weight based on the polymer. The two-phase system obtained was at a temperature held at 120 0 in the course of 10 min.

The crystallized free morphological structures were removed from the mentioned solvent with the help of a vacuum filter deposited.

Examination of the synthetic fiber mass obtained with the aid of a microscope has shown that the free morphological structures are predominantly spherulites with an average particle size of 75 to 80 μm.

Example 14.

The procedure was the same as in Example 12, except that the suspension of spherulites in the same solvent was introduced into the solution of the polymer in an organic solvent in an amount of 0 % by weight. There were spherulites with an average particle size of 65 to 70 µm

behavior,

Example 15 (negative) *

The same procedure as in Example 12 was followed, except that the polymer was dissolved in an organic solvent the suspension of spherulites in the same solvent

050008/0600

ORIGINAL INSPECTED

the permissible specified in the claims amount exceeds introduced in an amount of 40 wt% _# what to 10 wt.%, and the solution was kept for 10 minutes.

Spherulites with an average size of 43 to 48 µm were obtained.

Carrying out the crystallization under the conditions which are explained in example 1, brings? similar results, suggesting that the introduction of such a crowd the suspension has no noticeable effect, example 16,

A synthetic fiber mass was also made according to the invention manufactured as in example 4 «

The obtained synthetic fiber mass, which from free mphological structures, predominantly spherulites, was made with phenylon fibers in the following ratio (in weight, $) mixed"

Pheny & on fibers ···· ·· 85

free morphological structures of Hylon-6 · · · 15 · The mixture described was used for the production of a paper-like substance. The mentioned substance was in the usual process (by producing the suspension from free morphological structures and synthetic fibers, Pouring the suspension obtained, pressing, drying and Kalan- dration of the obtained substance) produced. The paper-like material produced was according to the method described in Example 1 methodology.

030008/0680
ORfGiNAL INSPECTED

The test results are given below «

Density, g / cnr 0.83

Thickness, mm ····. . 0.13

Specific breaking load, kp / mm 3.0

Dielectric strength, kV / mm ··. · .. ··· ».8.0

dielectric dissipation factor, % . 0.27

related to ene ^. elongation,% ··· 2.5

Example 17

A synthetic fiber pulp was also made according to the invention produced as in example 4

The obtained synthetic fiber mass, which from free morphological structures, predominantly spherulites, were made with phenylon fibers in the following ratio (in weight, $) mixed:

Phenylon fibers,, 13

free morphological structures of nylon-6 ·. · 85 · The mixture described was used for the production of a paper-like substance. The mentioned substance was in the usual process (by producing the suspension from free morphological structures and synthetic lasers, casting the suspension produced, pressing, drying and calendering The paper-like material prepared was prepared according to that described above Methodology checked.

The test results are given below;

Density, g / cnr 0.99

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Thickness, mm · · .. ·. ·· 0.12

specific breaking load, kp / mm 5.9

Dielectric strength, klT / mm. ·· .. · .... 13.5

dielectric dissipation factor, % 0.55

related elongation,% 5.5

Example 18.

A synthetic fiber mass has also been invented according to the invention manufactured as in example 4 »

The synthetic Easermasse prepared, which consists of free morphological structures vorweigend _v spherulites, was mixed with Phenylonfasern in the following ratio (in wt.%):

Phenylpn fibers ..... 70

free morphological structures of nylon-6 ·. . .30 The mixture described was used for the production of a paper-like substance. The mentioned substance was in the usual process (by producing the suspension from free morphological structures and synthetic fibers, Pouring the suspension produced, pressing, drying and Calendering of the obtained fabric) produced · The produced paper-like material was tested according to the methodology described above.

The test results are given below;

Density, g / cm 0.92 ⁵

Thickness, mm 0.12

specific breaking load, kp / mm x 6.0

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Dielectric strength, kV / mm ... 14.0

dielectric dissipation factor, % · · · · 0.29

related elongation, $ ···. .5.3

Example 19 (negative)

A synthetic fiber pulp was produced as follows «

10 parts by weight of polyamide (liylon-6) were mixed with 50 parts by weight of propanol and 50 parts by weight of distilled water. (The lower dissolution temperature of nylon-6 in the above-mentioned solvent is 162 ° 0) The prepared mixture was heated ^{to a temperature of 175 G to accelerate the dissolution of the polymer.} After complete dissolution of the polymer, the solution was ^{heated to a temperature of 132 C (ie 30 G} below the lower dissolution temperature of nylon-6 in the solvent mentioned) with a mixture

speed of 2.5 C / rain and cooled down at this! temperature Held for 10 minutes. The crystallized free morphological Structures of nylon-6 were spin deposited from the solvent.

Analysis by means of a microscope showed that the free morphological structures obtained were spherulites. The average size of spherulites was 34 to 40 µm, with 90 % of the spherulites produced being in a size range of £ to 50 µm.

The synthetic fiber mass produced, which from free morphological structures, predominantly spherulites,

030008/08 80
- ORIGINAL INSPECTED

was made with polyformaldehyde fibers in the following ratio (in% by weight) mixed "

Polyformaldehyde fibers ··. .. · ? O

free morphological structures of nylon-6 .... 30.

The mixture described above was used for the preparation of a paper-like substance "The aforementioned fabric was in the usual process (by making the suspension of free morphological structures and synthetic fibers _t casting of the prepared suspension, pressing and drying of the material produced) was prepared. The paper-like material obtained was of poor mechanical strength, which made it impossible to calender it. It follows that the manufacture of a paper-like material using such a synthetic fiber pulp on paper machines operating in the wet process owing to the very poor mechanical strength of the paper-like material obtained in the wet and dry State is impossible.

Example 20 (negative).

A synthetic fiber mass was produced according to the invention in the same way as in Example 1 *

The synthetic fiber mass produced, which consisted of free morphological structures, predominantly of spherulites, was mixed with fibers of nylon-6 in the following ratio (in wt. ^;

Nylon-6 fibers · .. ····. .90

free morphological structures of nylon-6 ·. . .10,

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ORIGINAL INSPEGTED

The mixture described was used for the production of a paper-like substance applied. The mentioned substance was in the usual process (by producing the suspension from free morphological structures and synthetic fibers, Pouring of the suspension produced, pressing, drying and calendering of the paper-like material obtained) The material obtained was tested according to the methodology described in the example «

The test results are given below »

Density, g / cm ^ 0.65

Thickness, mm x 0.16

specific breaking load, kp / mm ·. . 2.1

Dielectric strength, kV / mra · · · · · 3 * 5

dielectric dissipation factor,% ·. . 0.36

related elongation,% 1.1

The test results show that the material produced cannot be used as an electrical insulating material due to its characteristics.
Example 21 (negative) «

A synthetic fiber pulp was made in the same way as in the i Example 2 produced.

The synthetic fiber mass produced, consisting of free morphological structures, predominantly spherulites was made with phenylon fibers in the following ratio (in% by weight) mixed:

Phenylon fibers. · 5

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ORIGINAL INSPECTED

free morphological structures of nylon 6 ... 95 _# The mixture described was used for the production of a paper-like material , Pressing, drying and calendering of the paper-like material obtained). The material obtained was tested according to the methodology described in Example 21.

The test results are given below:

3
Density, g / cm 0.99

Thickness, mm. 0.12

specific breaking load, kp / mm ·. 2.9

Dielectric strength, kV / mm 4.6

dielectric dissipation factor, % 0.37

related elongation,% · 5 »1

The test results show that the material produced cannot be used as an electrical insulating material due to its characteristics.
Example 22.

An synthetic fiber pulp was produced according to the invention as follows.

5 parts by weight of polyamide (nylon-6) were mixed with 50 parts by weight of propanol and 50 parts by weight of distilled water (The lower dissolution temperature of nylon-6 in the solvent mentioned is 162 C). The mixture produced was

030008 / 0Θ8Ο

de heated to a temperature of 175 ° to accelerate the dissolution of the polymer. After the polymer had completely dissolved, the solution was cooled to a temperature of 128 ° C. (ie 34 ° C. below the lower dissolving temperature of nylon-6 in the solvent mentioned) at a rate of 4.5 ° C./min and at this temperature Held for 5 min. »The crystallized free morphological structures of nylon-6 were deposited by centrifugation · ELne analysis by means of a. Microscope has shown that the free morphological structures obtained were spherulites. The average size of the spherulites was 25 nm, with a maximum of 10% of the spherulites being smaller than 10 μm.

The manufactured synthetic fiber mass consisting of free morphological structures, predominantly of spherulites! was mixed with basalt fibers in the following ratio (in weight Sfc):

Basalt fibers

free morphological structures of nylon-6 2

The mixture described was used for the production of a paper-like substance.

The substance mentioned was produced in the usual way (by producing the suspension from free morphological structures and basalt fibers, pouring the suspension produced, eating and drying) produced »

The paper-like material obtained was tested according to the methodology described above.

030008/0680

ORIGINAL INSPECTED

The test results are given below:

Fat, jum 95

Density, g / cnr 0.27

ρ
Tensile strength, kp / mm · ·. ·. 0.09.

Example 23.

The same procedure as in Example 22 was followed, but the synthetic fiber mass with basalt fibers in the following ratio (in wt.%) mixed ι

Basalt fibers ♦. · 50

free morphological structures of nylon-6. ····, · 5Ρ ·

The test results are given below: Thickness, µm x 97

Density, g / cm ⁵ 0.25

2
Tensile strength, kp / mm .0.09

Example 24.

The same procedure as in Example 22 was followed, except that the synthetic fiber mass with glass fibers was in the following ratio (in% by weight) mixed:

Fiberglass 80

free morphological structures of nylon-6 ♦ .20,

The test results are given below:

Thickness to «

Density, g / cm 0, J2

2
Tensile strength, kp / mm 0.14

Example 25 (negative).

The same procedure as in Example 22 was followed, but

030008/0680

the synthetic 3? aser mass mixed with basalt fibers in the following ratio (in% by weight):

Basalt fibers ...... ....... 99

free morphological structures of nylon-6 · · 1 _# The «test results are given below«

Bead, Wm 91

^ 3
Density, g / cm 0.24

2
Tensile strength, kp / mm 0.05

With such a ratio of components, the paper-like material produced was less mechanical Strength, which limited its applicability «Example 26 (negative).

The same procedure as in Example 22 was followed, but the synthetic fiber paste was mixed with basalt fibers in the following ratio (in% by weight):

Basalt fibers 40

free morphological structures of nylon-6. ·. ·. 60. The test results are given below: Thickness to i 90.

Density, g / cm ........... 0.28

2
Tensile strength, kp / mm. 0.04

Defects in the material produced - see Example 25 Example 27 (negative).

A synthetic fiber paste was prepared as follows.

6. Parts by weight of polyamide (nylon-6) were mixed with 50 parts by weight

030008/0680

0RK3IMAL INSPECTED

share propanol and 50 parts by weight of distilled water mixed (the lower dissolving temperature of nylon-6 in the mentioned solvent is 162 0) · The prepared mixture was used to accelerate the dissolution of the polymer to a

Heated temperature of 175 C »After complete dissolution

ο of the polymer, the solution was cooled to a temperature of 124 G (ie. 38 ⁰ O below the lower dissolution temperature, of nylon-6 in the solvent mentioned) at a rate of 4.8 ° Q / nin and at this temperature in the course of Held for 5 min. The crystallized free morphological structures of nylon-6 were deposited by centrifugation. Analysis by means of a microscope showed that the free morphological structures obtained were spherulites. The average size of the spherulites was 15 μm, with 15% of the spherulites being smaller than 10 μm was.

The synthetic Easermasse prepared was (w G _e in%.) With basalt fibers mixed in the following ratio:

Basalt fibers 97

free morphological structures of Hylon-6. . . . · 3 · The paper-like material was produced from the mixture described in the same way as in Example 22 and examined. The test results are given below:

Thickness, mm-; 93

^J 3
Density, g / cm 0.21

2
Tensile strength, kp / mm 0.02

030008/0680

The paper-like substance that is etched with synthetic Fiber mass was produced, which predominantly from spherulites of which 15% were smaller than 10 µm insufficient mechanical strength, which limits the possibilities of its use,

Example 28.

A synthetic jasmine paste was made in the following manner according to the present invention manufactured.

6 parts by weight of polyamide (nylon-6) were mixed with 50 parts by weight Propanol and 50 parts by weight of distilled water » mixed (the lower dissolution temperature of nylon-6 in the mentioned solvent is 162 G). The mixture produced was pure accelerating the dissolution of the polymer to one

Heated to a temperature of 175 G, it was completely dissolved

of the polymer, the solution was heated to a temperature of 124 ° C (i.e. 38 ° G below the lower dissolution temperature of Ny -._

lon-6) cooled in the mentioned solvent at a rate of f? ° G / min and kept at this temperature for 10 minutes. The crystallized free morphological structures of nylon-6 were deposited by centrifugation. Microscopic analysis revealed that the free morphological structures obtained were spherulites. The average size of the spherulites was 15, at most 50% of the spherulites were less than 10 in order.

The synthetic fiber pulp produced was ground with Cellulose fibers in the following ratio (in% by weight)

03 00 08/0680

ORIGINAL INSPECTED "

mix s

Cellulosic fibers 99.7

free morphological structures of Hylon-6 ·. . 0.5 The mixture described became a paper-like one Substance in the usual process (by creating a suspension of free morphological structures and cellulose fibers, Pouring the suspension produced, pressing, drying and calendering) produced · The paper-like obtained Material was tested according to the methodology described in Example 1

The test results are given below:

Thickness, mm 6.5

Density, g / cnr * 1.21

Breaking load, kp 1.18

Breakdown voltage, V · JOO

Example 29.

A synthetic fiber pulp was produced according to the invention as follows.

6 parts by weight of polyamide (nylon-6) were combined with 50 parts by weight Propanol and 50 parts by weight of distilled water mixed (the lower dissolution temperature of nylon-6 in The solvent mentioned is 162 ° 0). The mixture produced was used to accelerate the dissolution of the polymer heated to a temperature of 175 C · After complete dissolution of the polymer, the solution was reduced to a temperature of 124 ° C (i.e. 38 ° 0 below the lower dissolution temperature

030008/0680

of nylon-6 in the mentioned solvent) at one rate cooled by 5 G / min and kept at this temperature for 10 min «The crystallized free morphological Structures of Jtfylon-6 were spun deposited A microscopic analysis has shown that the free morphological structures obtained were spherulites, their average size was 15 µm, with at most 50% of the spherulites being smaller than 10 µm.

The synthetic fiber mass produced was mixed with ground cotton cellulose in the following ratio ζ-in wt _# %):

Cotton fibers .95

free morphological structures of nylon-6 5.

A paper-like substance was made from the mixture described in a process known per se (by manufacturing a suspension of free morphological structures and Cotton fibers, pouring the suspension produced, pressing and! Drying).

The obtained paper-like cloth was made as above described methodologies checked *

The test results are given below «

Thickness, ρ 74

Density, g / cnr,. , 0.58

Breaking load, kp 1.7

030008/0680

ORIGINAL INSPECTED

Example 50 (negative)

You ginj in the same way as in Example 28 above, but was the synthetic "fiber mass with ground cellulose fibers mixed in the following ratio (in% by weight):

Cellulosic fibers 99.8

free morphological structures of nylon-6 .... 0.2. The test results are given below:

Thickness, 6.4 mm

5
Density, g / cm 1.15

Breaking load, kp. 0.93

Breakdown voltage, Y.. . . . · .. ·· 280.

At the same time, samples of the paper-like material were made from pure cellulose fibers in the same way. The test results are given below:

Thickness, around ··. ·· .. ···. ··· 6.5

Density, g / cm ⁵ 1.17

Breaking load, kp 0.94

Breakdown voltage, V ....... 280.

As can be seen from the above test results, a paper-like material produced with the use of free morphological structures of nylon-6 had no advantages compared to a material produced from pure cellulose fibers.
Example 51.
A synthetic fiber mass was produced as follows

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ORIGINAL INSPECTED

6 parts by weight of polyamide (nylon-6) were mixed with 50 parts by weight Propanol and 50 parts by weight of distilled Water mixed (the lower solution temperature of nylon-6 in the mentioned solvent is 162 ° G). The mixture produced was used to accelerate the dissolution of the polymer

heated to a temperature of 175 °. After complete dissolution of the polymer, the solution was brought to a temperature of 135 ° O (i.e. 40 ° 0 below the lower solution temperature of nylon-6 in the mentioned solvent) at one rate cooled by 5 C / min and at this temperature for 1 min held. The free morphological structures of nylon-6 that crystallized out were deposited by centrifugation. A microscopic analysis has shown that the free morphological structures are spherulites, the average of them Size 8 um cheating, being 60% of the spherulites were smaller than 10 µm.

The synthetic fiber mass produced was also ground . Cotton fibers mixed in the following ratio (in% by weight) t

Cotton fibers .95

free morphological structures of nylon-6 «... 5 · A paper-like material was made from the mixture described similarly manufactured and examined as discussed above.

The test results are given below:

Thick, around 71

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Density, g / cm ^ 0.37

Breaking load, kp. 0.86.

Mn paper-like substance made from a mixture with an additive Another synthetic 3-mass, which consists of spheroiths, whose size is smaller than that provided in the patent claims, has a low mechanical strength, making it difficult to process "

Example 32.

A synthetic fiber pulp was made in the following manner in accordance with the present invention manufactured,

12 parts by weight of polyamide (nylon-6) were mixed with 100 parts by weight of S.- caprolactam (the lower solution temperature of nylon-6 in the above-mentioned solvent is 150 ° C). The mixture produced was heated to a temperature of 170 G to accelerate the dissolution of the polymer mentioned. After complete dissolution of the polymer solution was die.erhaltene / min cooled at a rate of 1.0 ° G at a temperature of 120 ⁰ O (in the solvents mentioned nylon 6) that is 30 ° C below the melting lower dissolution temperature of the polyamide () and held at this temperature for 15 minutes.

The crystallized free morphological structures of nylon-6 were separated from the solvent by decantation and washed. The synthetic fiber mass produced was examined with the help of an optical microscope « The investigations carried out showed that the free mor-

030008/0680

Phological structures were predominantly spherulites, from which were 20% smaller than 20 µm. The said synthetic

J
see fiber pulp was refined with unbleached on JO SR

ground sulphate cellulose in the following ratio (in% by weight)

mixed: _t

Cellulose fibers ·. · ·. 95

free morphological structures of polyamide

(Nylon-6) 5.

The mixture described was used for the production of the paper for electrolytic condensate furnace, which in the usual Process (by producing a suspension of free morphological structures and cellulose fibers, casting the produced Suspension, pressing and drying) was produced

The paper produced was tested according to the methodology described above

The test results are given below »

Thickness to · ....... 56

Density, g / cm x 0.28

Breaking load, kp 0.31

The power factor at 25 ° C .... 7.5 Example 33

A synthetic pulp was prepared as described in Example 32. The pulp made with refined unbleached sulphate ground to 20 SR

030008/0680

ORIGINAL INSPECTED

Cellulose mixed in the following ratio (in% by weight) »

Cellulosic fibers 50

free morphological structures of polymer

(Nylon-6) 50.

Bas paper for electrolytic capacitors was developed from the

Prepare the mixture in the same way as in Example 32

is described, manufactured and tested. The test results are given below »

Thickness to ···. ·. .... 65

Density, g / cnr 0.29

Breaking load, kp. . 0.24

Dielectric constant at 25 ° c ........ 6.6.

example

A synthetic fiber pulp was made in the following manner in accordance with the present invention manufactured.

10 parts by weight of polyamide (nylon-6) were mixed with 100 parts by weight of £ - aprolaktam (the lower solution temperature of nylon-6 in the above-mentioned solvent is 150 ⁰ ). * The resulting mixture was heated to speed up the dissolving process of the aforementioned polymer to a! Temperature of 170 ⁰ G. After complete dissolution of the polymer, the solution obtained was cooled to a temperature of 125 ° CJ (ie 25 C below the lower solution temperature of nylon-6 in the solvent mentioned) at a rate of 0.5 ° C / rain and at this temperature im Held for 40 min. The crystallizing

030008/0680

ORIGINAL INSPECTED

th free morphological structures of polyamide (nylon-6) were separated from the solvent by decantation and washed " I.

The obtained synthetic fiber mass was with the help of a optical microscope examined. The examinations carried out I Research has shown that the free morphological structure * doors are predominantly spherulites, but spheroidalites with a particle size below 20 µm were not found. ■

The synthetic fiber mass produced was finished with * ter unbleached sulfate cellulose ground to 40 SS in following ratio (in uew.%) mixed "

Cellulosic fibers x 50

free morphological structures of polyamide

(Nylon-6). . 50.

The paper for electrolytic capacitors was made from the Mixture prepared and tested in the same way as described in Example 32.

The test results are given below

Thick, around 77

Density, g / cm 0.28

Breaking load, kp · 0.48

Dielectric constant at 25 ° C

Example 35. j

A synthetic pulp was prepared similarly as described in Example 32.

030008/0680

ORIGINAL INSPECTED

. ₆ 3 * 1 2930132

The synthetic saser mass produced was mixed with refined, unbleached ^{sulphate cellulose} ground to 30 ° Sfi in the following ratio (in% by weight):

Cellulose fibers · «20

free morphological structures of polyamide

(Nylon-6) 80.

The paper for electrolytic capacitors was made from the mixture obtained in the same way as described in Example 32 is, manufactured and tested "

The test results are given below:

Thickness, around ^ B

J 3
Density, g / cm x 0.28

Breaking load, kp 0.34

Dielectric constant at 25 ° 0 8.0

Example 36 (negative).

A synthetic Sasermass.e was produced as follows.

8 parts by weight of nylon-6 were ξ with 100 parts by weight, -JC.aprolaktam mixed (the lower solution temperature of Nylon-6 is in the above-mentioned solvents 150 ⁰ C). The mixture obtained was heated to a temperature of 170 ° C. in order to accelerate the dissolution process of the polymer mentioned. After complete dissolution of the polymer, the resulting solution was heated to a temperature of 1 ^ 5 ^C (i.e. 35 ° C below the lower solution temperature of nylon-6 in the mentioned solvent) at a rate of

03DQ08 / 0680

Cooled 4 ° 0 / min and held at this temperature over the course of 15 min. The crystallized free morphological Sfcruicturen of nylon-6 were separated from the solvent by DekantierUEg and washed "The synthetic fiber mass prepared was studied using an optical microscope · The investigations carried out have shown that the free morphological structures constituted mainly spherulites, of which 40% smaller when 20jam were

The obtained synthetic saser mass was refined with unbleached sulfate cellulose ground to 45 SE in the following Ratio (in wt.%) Mixed »

Cellulose fibers ··. 60

free morphological structures of polyamide

(Nylon-6) .40.

The paper for electrolytic capacitors was made from the mixture obtained exactly as explained in Example 32 is, manufactured and tested.

The test results are given below:

Thickness, around 37

Density, g / cm ⁵ 0.58

Breaking load, kp. 2.0

Dielectric constant at 25 ° C 15 _t 5

Example 37 (negative)

The procedure was exactly as in Example 32, but the components were in the following weight ratio (in% by weight) mixed:

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Cellulose fibers ·· ... ·· .. 10

free morphological structures of polyamide (Nylon-6). 90

The paper for electrolytic capacitors was produced and tested as described in Example 32.

The test results are given below

Thick, around 83

Density, g / ciif 0.23

Breaking load, kp ........ 0.09

Dielectric constant at 25 ° 0 ........ 4.9

Example 38 (negative).

A synthetic pulp became · like this

is described in Example 32 is prepared.

The produced synthetic asermass was refined with mixed with unbleached sulfate cellulose, the degree of freeness of which was 54 ° Sfi, which roughly exceeds the permissible fourth.

The components mentioned were in the following ratio C in wt.%) Mixed ι

Cellulose fibers ..... 5P

free morphological structures of polyamide

(Nylon-6) 50.

The paper for electrolytic capacitors was made from the obtained mixture. as described in example 32

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ORIGINAL INSPECTED

ben is, manufactured and tested *

The test results are given below *

Thick, around 71

Density, g / cm 59

Breaking load, fcp «0.40

Dielectric constant at 25 ° C 15.9

Example, 39

A synthetic fiber mass was made according to the invention manufactured.

12 parts by weight of nylon-6 were mixed with 50 parts by weight of propanol and 50 parts by weight of distilled water (the lower dissolving temperature of nylon-6 in the above-mentioned solvent is 162 ° C) of 175 0 · After the polymer had completely dissolved, the solution was ^{cooled to a temperature of 132 0} C (ie 30 C below the lower dissolution temperature of nylon-6 in the solvent mentioned) at a rate of 2.5 C / min and at kept this temperature for 20 minutes "

The crystallized free morphological structures of nylon-6 were separated from the solvent by centrifugation. A microscopic analysis showed that the free morphological structures obtained were spherulites, the average size of which was 35 to 40 µm, with 30% of the spherulites ranging in size from 2 to

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lying down «

The synthetic fiber mass produced was ground with unbleached sulphate cellulose mixed in the following ratio (in% by weight):

Cellulose fibers .......... 70

free morphological structures of P _o lyamid

(Nylon-6) 30.

The mixture described above was mixed, poured, pressed, dried and calendered. The material made was made according to the methodologies described above with transformer oil soaked and tested.

The test results for the material produced are below

specified:

3
Volume mass, g / cm x 1.01

Dielectric strength, kV / mm · 57 »β

oil capacity,% · «.... · ..... ... 16 dielectric constant ............. 2 »5

The dielectric constant of a pure pulp, which is produced and tested under the same conditions worde, is 3.96 with a volume mass of 1.03 g / cur. Example 4O.

Analogously to Example 28, the synthetic fiber mass produced with ground unbleached sulfate cellulose was im the following ratio (in% by weight) mixed:

Cellulose fibers .70

free morphological structures of polyamide (nylon-6) 30.

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The mixture described above was stirred, poured, pressed and dried. The dielectric constant of the material produced was 1.33 with a density of 0.54 g / cm ·

The dielectric constant: of a material made exclusively from the unbleached sulphate cellulose under the same operating conditions is 2.14 with a density of 0.55 g / cm.
Example 41

The same procedure as in Example 28 was followed, but the procedure was followed the manufactured synthetic fiber mass with »ground unbleached Sulphate cellulose veapmischts in the following ratio (in weight flo)

Cellulose fibers 95

free morphological structures of polyamide

(Nylon-6) 5

The mixture described above was stirred, poured, pressed and dried. The material produced was iron dielectric constant of 1.72 at a density of 0.61 g / cm on «The dielectric constant one of the same unbleached sulphate cellulose material produced under the same operating conditions is 2.14 at one Density of 0.55

Example 42.

A synthetic fiber mass was made according to the invention as follows manufactured,

8 parts by weight of nylon-6 were mixed with 50 parts by weight

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ORIGINAL INSPECTED

_ ₆₉ _ 29301S2

Propanol and 50 parts by weight of distilled water mixed (the lower dissolution temperature of nylon-6 in the above-mentioned solvent is 162 ° O) Polymers, the solution was cooled to a temperature of 130 ⁰ O (ie 32 C below the lower dissolution temperature of Hylon-6 in the solvent mentioned) at a rate of 3 C / min and kept at this temperature for 15 min.

The crystallized free morphological structures of nylon-6 were separated from the solvent by centrifugation. A microscopic analysis showed that the free morphological structures obtained were spherulites, whose average size was 35 to 40 µm, with 80% of the spherulites in a size range from 2 to 50 um layers.

The synthetic fiber pulp produced was unbleached with Sulphate cellulose mixed in the following ratio (in% by weight) s

Cellulose fibers 30

free morphological structures of polyamide (nylon-6) 70 »

The mixture described above was stirred, poured, pressed and dried. The material produced was dielectric Constant of 1.69 at a density of 0.51 g / cm.

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The dielectric constant of one made from the same cellulose material produced under the same operating conditions is 2.14 at a density of 0.55 g / car

Example 43

A synthetic fiber pulp was made in the following manner in accordance with the present invention manufactured"

7.3 parts by weight of nylon-6 were mixed with 50 parts by weight of propanol and 50 parts by weight of distilled water (the lower dissolution temperature of nylon-6 in the above-mentioned solvent is 162 ° C.). Polymer warms to a temperature of 175 ° C. After complete dissolution of the polymer, the solution was heated to a temperature of 132 ° C (ie, 30 ⁰ C below the lower dissolution temperature of nylon 6 in the mentioned solvents) at a rate of 2.5 C / min and cooled min at this temperature for 20 held long *

The crystallized free morphological structures of nylon-6 were removed from the solvent by spinning divorced · A microscopic analysis showed that the obtained free morphological structures represented spherules, the average size of which was 35 to 40 µm, with 90% of the spherulites obtained in a size range of 2 to 50 µm layers «

The synthetic saser mass produced was ground with

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0RK3INAL INSPECTED

ner unbleached sulphate cellulose in the following ratio (in% by weight) mixed:

Cellulose fibers, «... 80

free morphological structures of. Polyamide (Ny-

lon-6) 20.

The mixture described above was stirred, poured, pressed and dried. The material produced had a dielectric constant of 1.37 at a density of 0.56 g / cm ^ on

The dielectric constant of a material made from the same cellulose under the same operating conditions is 2.14 x at a density of 0.56 g / cmr. Example 44 ·.

A synthetic fiber pulp was made in the following manner in accordance with the present invention manufactured.

6, parts by weight of polyamide (nylon-6) were mixed with 50 parts by weight of propanol and 50 parts by weight of distilled water (the lower temperature of dissolution of nylon-6 in the above-mentioned solvent is 162 ° C). The mixture prepared was used to accelerate the dissolution of the polymer to a temperature heated by 175 ° C. After the polymer had completely dissolved, the solution was cooled to a temperature of 1J2 0 (ie JO ⁰ C below the lower dissolution temperature of nylon-6 in the solvent mentioned) at a rate of 2.5 ° G / min and at this temperature in the course held for 20 min. The detailed free morphological structures of nylon-6 were discovered by the Lo-

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solvents deposited by spin "fiLne microscopic analysis revealed that the resulting free morphological structures represented spherulites whose average size was 55 to 40 microns, wherein 90% of the obtained Sparoli- * then are in a size range of 2 ° to 5 ° P ^ lay"

The synthetic fiber mass produced was ground with unbleached suIf at cellulose in the following ratio «·· nis (in% by weight) mixed:

Cellulose fibers 20

free morphological structures of polyamide

(Nylon-6) 80,

The equipment described above was stirred, poured, pressed, and dried. «The material produced had a dielectric constant of 3» 09 at a density of 0.48 & / gwl »

The dielectric constant of a material made from the same unbleached sulfate cellulose under the same operating conditions is 2.14 at a density of 0.55 g / cm of components compared to a material made of pure cellulose is much larger «
Example 45 (negative).

A synthetic pulp was produced as follows.

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ORIGINAL INSPECTED

6.5 parts by weight of nylon-6 was mixed with 50 parts by weight Propanol and 50 parts by weight of distilled water mixed (the lower dissolution temperature 'of nylon-6 in the above Solvent "is 162 ° C)" The mixture produced was to accelerate the dissolution process of the mentioned Polymer heated to a temperature of 175 C * After complete Dissolution of the polymer, the solution was

o ο

temperature of 127 0 (i.e. 35 C below the lower Dissolution temperature of nylon-6 in the solvent mentioned) cooled at a rate of 0.5 0 / min and kept at this temperature for 10 min. The th free morphological structures of nylon-6 were separated from the solvent by centrifugation. The manufactured Fiber mass was examined with the aid of an optical microscope. The investigation has shown that the free morphological structures are predominantly spherulites, their average size was 60 µm, 45% of that obtained Spherolites ranged in size from 2 to 50 µm.

The synthetic saser mass produced was unbleached with Sulphate cellulose mixed in the following ratio (in Grw.%) «

Cellulose fiber core. . ·. ·. 95

free morphological structures of polyamide

(Nylon-6) 5.

The mixture described above was stirred, poured, pressed and dried. The material produced had a di-

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ORiQiNAL INSPECTED

electrical constant of 2.21 at a density of 0.57 g / ea on «The dielectric constant of one made from the same cellulose and under the same operating conditions Material is 2.14 at a density of 0.55 g / cm · Es it is clear that the dielectric constant is one of the cellulose fibers and free morphological structures of polyamide (Nylon-6) produced material using a polymer produced by the method described above, if 45% of the obtained spherulites of nylon-6 in a size range from 2 to 50 µm, compared to which a "material made of pure cellulose is larger"

It is very clear that only a few specific embodiments of the invention are presented above, including other embodiments of the invention are possible, with preserve the essence of the invention within the scope of the patent claims » remain.

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Claims (1)

SHIP ν. FÜNER STREHL SCHÜBEL-HOPF EBB1NGHAUS FINCK MARIAHILFPLATZ 2 * 3, MÖNCHEN 9O POST ADDRESS: POSTBOX 95 O1 6O. D-800O MÖNCHEN 95 Ukrainskoe nautschno-proizvodstvennoe objedinenie celljjulozno-bumaschnoj promyschlennosti (UkrNPOBumprom) PROFESSIONAL REPRESENTATIVES SO BEFORE THE EUROPEAN PATENT OFFICE _k * rl ludw.q ^DIPL · ^1Νβ ' ^{PETER STREHL} DIPL. CHEM. DR. URSULA SCHÜBEL-HOPF DIPL. INQ. DIETER EBBINQHAUS DR. INQ. DIETER FINCK TELEPHONE (OBO) 4BaoS4 telex b-q3 56b auro d auromarcpat Munich DEA-19608
July 25, 1979 Process for the production of a synthetic fiber mass and device for its implementation Patent claims 1 · Process for the production of a synthetic fiber mass which provides for the dissolution of a crystallizable polymer in an organic solvent, cooling of the prepared solution for crystallization of the mentioned polymer and separation of the crystallized free morphological structures from the solvent, characterized in that the cooling takes place at a rate of 0 , 1 to 5 ° C / min to a temperature of 0.5 to 40 ° 0 below the lower temperature of the polymer in the solvent used to crystallize the said polymer with the formation of free morphological structures, predominantly spherulites and "shish kebab" structures is carried out" 2 «The method according to claim 1, characterized « that the polymer solution is cooled at a rate of 0.1 to 4 C / min and this a suspension of free morphological 030008/0680 Structures in the organic solvent is introduced after the lower dissolution temperature of the polymer has been reached. _# 5 The method of claim 2, characterized in that the suspension of free morphological structures in the organic solvent in an amount of I to O ₉ $ 0 wt "%, based on the polymer, is introduced into the polymer solution * 4 «Method according to claim 2, characterized in that the suspension and the solution are produced from the same organic solvents and the same polymers * 5 · Method according to claim 1, characterized in that the above-mentioned polymer solution after cooling to a Temperature of 0.5 to 40 G below the lower dissolution temperature of the polymer in the solvent used is kept at this temperature for 1 to 60 minutes * 6 _Φ Process according to claim 1, characterized in that the polymer solution is cooled to a temperature of 10 to 40 ⁰ C below the lower dissolution temperature of the polymer in the solvent used and that the free morphological structures formed and separated from the solvent are mixed with fibers. j A method according to claim 6, characterized in that the free morphological structures separated from the solvent, of which at most 50% are smaller than $ O um, are mixed with synthetic jasers in the following ratio (in% by weight): synthetic fibers · 15 ·· «85 free morphological structures ··· 85 ··· 15 · 030008/0680 8. The method according to claim 6, characterized in that it fifrftrmg- eichnet . that the free morphological structures separated from the solvent, of which no more than 10% are smaller than 10, are mixed with mineral fibers in the following ratio (in weight per cent): Mineral fibers * · · 50 ... 97 free morphological structures ....... 50 ... J. Process according to Claim 6, characterized in that the free morphological structures separated from the solvent, of which at most 50% are smaller than 10 µm, are mixed with natural fibers in the following ratio (in% by weight) » Natural fibers 20 ... 99.7 free morphological structures ........ 80 ... 0.5 10. The method according to claim 1, characterized in that polyamide is used as the polymer and its separated from the solvent free morphological structures of which at most 20% smaller than 20 / um are provided with ground to 20 SR .. .40 cellulose in the following ratio (in wt% _#) are mixed: Cellulose fibers. ..... 20 ... 95 free morphological structures of polyamide 80 ... .5. 11 «The method according to claim 10, characterized in . that free morphological structures of polyamide are mixed with cellulose in the following ratio (in% by weight): Cellulose fibers, 50 ... 80 free morphological structures of polyamide 50 · · .20 · D30008 / 0680 12. The method according to claim 1, characterized in that «that polyamide is used as a polymer and its free morphological structures separated from the solvent, of which at least 60% have a size of 2 to 30 μm , with cellulose fibers in the following ratio (in% by weight) to be mixed » Cellulose fibers 30 ... 95 free morphological structures of polyamide 70 ... 5 13. The method according to claim 12, characterized »that free morphological structures of polyamide are mixed with cellulose fibers in the following ratio (in wt. ^): Cellulose fibers, 40 ... 80 free morphological structures 60..20. 14. Device for performing the method according to claims 1 to 4, which has a chamber (3) for dissolving the polymer, a buffer capacity (11), which is connected to said chamber (3), a crystallizer (12), which by a Pipeline (13) is connected to the buffer capacity (11) and is designed in the form of a container with a split cooling jacket (22), as well as a device (24) for separating the crystalline hate of the polymer from the organic solvent, which is connected to the outlet of the crystallizer (12) is connected, contains, characterized . that a second drilling line (14) with a heat exchanger (15), which feed and discharge nozzles (17) and (18) for coolant, parallel to the first drilling line (13) to the buffer capacity (11) and the inlet of the crystallizer (12) is connected. 030008/0680 15 · Device according to claim 14, characterized in that the mentioned supply and discharge connections (17) and (18) for the coolant of the said heat exchanger (15) are provided with adjustable throttles (20) and (21) » 16% device according to claim 14, characterized in that the cross-sectional area ratio of the mentioned second pipeline (14) and the first mentioned drill line (13) is in a range from 0.001 to 0.3 « 17 · Device according to claim 14, characterized in that a controllable valve (19) is arranged in said second pipe (14) in series with said heat exchanger (15). 18. Device according to claim 14, characterized in that an intermediate container (28), which has a temperature control jacket (29), is connected to the outlet of said crystallizer (12) and to said device (24) for separating the crystalline mass of the polymer connected by the organic solvent 030008 / oeeo