Continuous fiber and method thereof

 

(57) Abstract:

The inventive solution mixture polyparaphenyleneterephtalamide with 3-30% polyvinylpyrrolidone (mol. capabilities from 10,000 to 40,000 in sulfuric acid ekstragiruyut through the die plate and the air layer in a water bath having a temperature of 5C. the Extrudate is pulled into the air space of 6.3 times. Washed with water and/or dilute aqueous alkali solution. 2 N. p. and 1 C.p. f-crystals, 1 tab., 2 Il.

The invention relates to the technology of chemical fibres, in particular the production of fibers of aromatic polyamide mixed with polyvinylpyrrolidone.

Known fibers obtained from a mixture of polyparaphenyleneterephtalamide (ECD-T) with different polymers, for example with another aromatic polyamide [1 and 2] , polyacrylonitrile [3]. These fibers possess or increased strength or improved nakashibetsu.

The closest of the invention is a fiber obtained from a mixture of PEG-T polyamide containing links diaminobenzanilide. Fiber has the strength to 23.9 g/denier, specific strength to 26.8 g/denier, has a round cross-sectional shape [4].

The fiber is made by extrusion of the solution mixture Nnu with subsequent washing with water and/or dilute aqueous alkali solution [4].

Having good strength characteristics, high abrasion values in bending, known fibers do not have such important properties as improved abrasivejet, increased resistance to fire or high adhesion in composite structures.

The problem to which this invention is directed is to obtain fibers of the PEG-T, having a set of these properties that enable their use for technical purposes.

The technical result obtained by carrying out the invention, is achieved due to the fact that ekstragiruyut through the die plate and the air layer in an aqueous coagulation bath solution mixture ECD-T 3-30 wt.% polyvinylpyrrolidone (mol. weighing 10-40 thousand taken as another polymer, and in the air space of the extrudate is pulled 6.3 times, and the coagulation is carried out at a bath temperature of 5aboutC. the Thickness of the air gap is 0.5 to 2.5, see the Fiber is washed with water and/or dilute aqueous alkali solution. The resulting fiber has strength to 23.9 g/denier, specific strength - to 26.8 g/denier, an irregular shape of the cross section and density 1,3484-1,4048 g/cm3.

Amnesia ECD-T and PVP in the form of finely pulverized particles with the solvent of the spinning solution, for example with concentrated sulfuric acid. The acid should be heated for complete dissolution of the PEG-T and PVP, and the temperature should be as low as possible to minimize degradation of the polymer. Alternatively, the spinning solution can be obtained by mixing one of the polymers in the form of finely ground particles with the solvent of the spinning solution, followed by the addition of another polymer.

It should be noted that the total concentration of the polymer must be such that the spinning solution was anisotropic.

Fiber of the present invention, basically, made from a mixture of PVP and PEG-T and standard additives, such as dyes, fillers, matting agents, UV stabilizers, antioxidants, flame retardants, etc. that can also be added to the mixture as needed.

When using ECD-T homopolymer and concentrated sulfuric acid, the melting point of the spinning solution of the present invention is reduced slightly from 72 (3% PVP) to 71about(With 6% PVP), and then increases to approximately 75aboutWith (15% PVP) and again reduced to 72aboutWith about 20% PVP.

The freezing point of the solution SN the melt to approximately 38aboutWith about 15% PVP, and decreases again to the 24aboutWith about 20% PVP.

Spinning solutions of the present invention can be extruded at any temperature at which they are liquids. Since the degree of degradation of the polymer is in some way a function of time and temperature, it is desirable to use as low as possible temperature within the allowable range. The solutions of the present invention are optically anisotropic, i.e., in the mass they depolarizes plane-polarized light because the light transmission in microscopic volumes of a solution varies depending on the direction. Microscopic domains in solutions are docosatetraenoic.

The solutions of the present invention is subjected to molding in a standard way [5].

Fiber on the proposed method can be subjected to heat treatment after drying or during drying. Heat treatment is carried out at 250-550aboutC for 1-6 with in terms of tension 11-12 g/denier thermal treatment leads to the increase of the effective modulus of elasticity of the fibers. Up to the present time, in the heat treatment, the strength para-aramid in the broken off from a mixture of PEG-T and PVP with PVP content of about 12-17%, not undergo deterioration of strength in the heat treatment under similar conditions.

Obviously, it plays the role of the use of PVP in combination with PEG-So you Know that PVP is soluble in water, and the use of PVP in an amount up to 30% of the fibers in a significant amount of PVP is not leached in water. As described above, only that the spun fiber is subjected to coagulation in aqueous solutions. A significant amount of PVP is not leached from the coagulated fiber in a coagulation bath.

Many quality fibers can be regulated or modified by using a certain number of PVP entered into the fibers. As it stands, PVP may be present in amounts of 3 to 30 wt.% (by weight PEG-T). Fibers of the proposed method with good characteristics can be obtained practically at any concentration, PVP, however, at concentrations less than the above lower limit, these benefits are difficult to define.

Exceeding the specified upper limit of the concentration of PVP leads to deterioration of some of the characteristics of the fiber. In this regard, it should be noted that the experts do not consider PVP to the category of those materials, including the and the present invention has led in General to an unexpected improvement of the quality specified fiber, there are also PVP concentration above which some quality fibers become unacceptable. It is obvious that the amount of PVP in excess of 30 wt.% (in relation to ECD-T), irreversibly leached from the fibers in the coagulation bath during processing.

Abrasivejet. Fibers made entirely of para-aramid, are difficult to paint, because dyes are not easily penetrate into the molecular structure of these fibers. On the contrary, the proposed fiber is easily painted. When the concentration of PVP only 3 wt% of the para-aramid) for dyeing fibers can be used for basic dyes by standard methods of dyeing. Basic dyes are dyes having a cationic group in its molecule. Abrasivejet using basic dyes increases with increasing PVP concentration to a value of 15 wt.% (with respect to para-aramid), while increasing the PVP concentration is higher than 15 wt. % the ability to colour main colour changes slightly.

When using acid dyes abrasivejet fibers is quite low at PVP concentrations below approximately 12-15 wt.% (based on para-aramid), and when it reaches increasing the concentration of PVP. To acid dyes include dyes having anionic group in its molecule.

On the basis of the above, it is obvious that any concentration of PVP in the fibres according to the invention improves okrashivaemoy fibers regardless of whether the specified concentration within the preferred range of up to 30 wt.% or not.

The density of the fiber. The density of fibers made from PEG-T, is approximately 1.45 g/cm3. The density of fibers from PVP usually is 1.29 g/cm3. The density of the fibers of the present invention varies depending on the concentration of PVP in the fibers. At low concentrations of PVP fibre density decreases sharply from 1,4048 g/cm3to its minimal value, approximately 1,3484 g/cm3and then again gradually increases with increase in concentration.

A non-circular shape. Fibers formed by using all nozzles typically have a circular shape, and, in General, the fibers take the form of a die, through which they were extruded. Fiber receive a non-circular shape in some way by chance, i.e., regardless of the form of the die. It was found that after processing in the coagulation bath the fiber us the Jena photography fibers of the present invention, obtained using 12 wt.% PVP (by weight PEG-T). Fiber shown in this figure were prepared using multi-channel mouthpiece with round holes with a diameter of 0,063 mm (pictures obtained by magnification x 1000).

The reason for obtaining fibers of the proposed method with a non-circular shape, are not completely understood. A non-circular shape are fiber of the present invention, in which the content of PVP relatively ECD-T exceeds approximately 9%. Fibers with non-circular profile have a greater surface area than the fiber round shape, and as a result, they have the best ability to bonding with the matrix material, in comparison with the circular fibers of the same denier, and in addition they are much softer to the touch than the fiber with a round profile.

Temperature resistance. In addition to the above superior qualities of the fibers according to the invention, it was discovered that made from these fibers products have a high resistance to heat and fire resistant. It was also established that products made from fibers of the present invention containing 6-20 wt.% PVP (in relation to ECD-T), show a significant increase in resistance.

The durability is would be the fact these fibers were found significantly higher compared to the fibers of the prototype (made from PEG-T), the strength after heat exposure. In tests on maintaining strength after heat exposure, it was found that the fibers of the present invention, containing 12% PVP in relation to ECD-T retain 94% of its initial strength, while fibers made only from ECD-T with the same size under the same conditions, save 82% of its original strength.

The bonding of the elastomeric matrix. Para-aramid fibers are often used as reinforcing materials in polymer matrices, for example in rubber products. To use the para-aramid fibers as a suitable reinforcement materials they need to possess the appropriate ability to stick together with matrices. Improving the adhesive ability of the fibers improves the reinforcement. It was found that the fibers of the present invention show the ability to bonding with rubber, 2 times found ability ECD-T fibers of the prototype.

Test methods

The linear density of

The weight room fiber or denier means a lot in Eskie tensile properties

Strength is defined as the ultimate tensile stress divided by the linear density. The modulus of elasticity is defined as the angle of the primary curve stress-strain and is measured in the same units as the strength. The elongation is expressed as a percentage increase in the length of the fiber at break. The strength and modulus of elasticity is first calculated in g/denier, and then multiplying by 0,8838, get the value in units of kN/Tex. Each measurement is taken as the average of 10 breaks.

Specific strength determine how destructive voltage divided by the linear density adjusted for the number of PVP. Because the presence of PVP very little effect on the strength of the fibers, compared with the PEG-T, fiber strength can be adjusted for the presence of PVP. Specific strength is a measure of the strength ECD-T fiber and is measured by dividing the strength by the weight fraction of PEG-T fiber.

In Fig.2 presents the dependence of the specific strength on the content of PVP in the fibers of the present invention.

The mechanical properties of the yarn under tension was measured using the 24aboutC and a relative humidity of 55% after moistening when the test conditions for menim weight room 1500 twisted from about 0.8 to about/cm). Each woven sample had a length of 25.4 cm and stretched by 50% min (relative to the original length of the unstretched state) using standard recording stress - strain devices.

The coefficient of twist (TM) aligns the dependence of torsion per unit linear density Unscrew yarn. The specified rate is calculated by the formula:

TM = (denier)1/2(turns/inch)/73 where R/inch = turns/inch;< / BR>
TM = (decitex)1/2(R/cm/30,3, where rpm = revolutions/see

Abrasivejet.

Abrasivejet fibers of the present invention was determined by means of dyeing fibers with a red dye and measuring the color component "a" with a colorimeter "Hunter", for example Huntelab ob heston.

As a way of defining colors used method of testing AUTOS 153-1985; AUTOS - American Association of certified dyes for fabrics.

For the purposes of the present invention, the absolute value of the value "a" defined by the specified tests are not so important. The difference in okrashivaemoy fibers easily see using relative values for different fibers. On a scale of "a" is 0 LASS="ptx2">

This test is used to simulate the heat from the combustion of fuel oil at 50/50-education convection and radiant heat to full heat flux of 2.0 cal/cm2C. This test identified as test method NFPA 1971. Section 5-1.NFPA - national Association for fire protection.

For the purposes of the specified tests have produced a sample in the form of a single layer of the product obtained with the use of fibers intended for evaluation; however, the heat sensor is not used, because the rate and extent of charring was investigated parameters.

Save strength when heat aging (HASR).

The result of this test was determined by the degree of conservation of strength after thermal ageing in relation to the initial strength of the fibers. HASR is expressed as a percentage of the tensile strength, which had a sample of regulated after heat exposure.

For this test, a fresh sample of the fiber was subjected to moisture at a relative humidity of 55% and 23aboutC for 14 h Then a portion of this sample was subjected to dry heat at a temperature of 240aboutC for 3 h, after which the sample was twisted to determine the portion of the sample, not subjected to heat treatment, and which was also subjected to torsion in order to determine the ultimate tensile strength (strengthonold.).

HASR = 100.

Sleevenote with rubber.

Test the bonding of rubber was carried out to evaluate only the adhesive clutch (strength of resdir) performed nesognutoy between the rubber material and the reinforcing cord layers introduced in this rubber material. Samples for the tests themselves were reinforced products. The test was performed according to ASTM D 2630-71, except for a few omitted or slightly modified parts, which will be specified below.

All 12 samples (including at least 2 control) cut from one set of turns of yarn. Each test sample had a width of 1 inch (11,4 cm) and in the middle of their thickness contained a typed sheet complex polyester, protruding from the inside of 2.5 cm from one end to the next break ends for testing. Each study sample consisted of eight layers, two of which consisted of layers of rubber mixture; then came a layer of parallel, spaced at a distance from each other to the; the two extreme layers was also the layers of rubber compound. As the rubber compound used standard commercially available product. He was a sheet of rubber compound on the basis of natural rubber with high modulus of elasticity, the thickness of which was of 0.015 inch (0.38 mm) and a width of 12 inches (305 mm). Researched cord layers were made of aramid yarn weight room 1500 denier, and identified as 1500/1/2 with winding 36 conc./inch (14,2 conc./cm). The tension coiling was 225 25, the Coefficient of twist = 6,5. The final shaping was carried out in the mold, preheated to 160 2aboutC at a pressure of 7 tons (of 62.3 kN) for 20 min.

Test the bonding of rubber at room temperature includes the following procedures: connector ends of the sample to remove a piece of polyester film, the introduction of one separated end of each clamp laboratory device for determining the tension/strain on at least 1 inch (2.5 cm), so that the sample was concentrated; and the breeding of the clamps when the speed crosses the 5 inch (12.5 cm) min. Full load was brought to 100 pounds (45,45 kg), and the preferred speed on the chart with the note, if the peak height decreased to the end of the test, was considered only peaks in 1 inch (2.5 cm). Then through the peaks were in the line and was determined by the distance from the zero line, component of the total load. Multiplying this factor at full load received "tensile strength".

The destruction of each sample during testing can occur either only in a rubber layer or at the boundary between the rubber and cord layers or two layers at once. Each gap has also been classified by its appearance on a scale from 1 to 5, where 1 means that the cords are completely open, and 5 means that the cords are completely closed.

Description of the preferred embodiment of the invention

In the examples below, all parts are given by weight, except in those cases where it is explicitly stated.

P R I m e R 1. This example describes the obtaining of fibers in accordance with the present invention.

23,04 hours of concentrated sulfuric acid (101%) was stirred and cooled in a closed vessel to -5aboutC. Then, to this vessel was added a mixture of poly(n-phenylene of terephthalamide) (PEG-T, 5 h), having a characteristic viscosity of 6.3, and poly(vinylpyrrolidone) (PVP, 0,60 h) with mol. the weight of 40 thousand CME is ivali for 2 h at 85aboutWith under reduced pressure (25 mm RT.CT.) in order to remove bubbles. The resulting spinning solution was extrudible through multi-channel mouthpiece with 267 holes with a diameter of 0,063 mm; and extruded spinning solution was passed through an air gap length of 0.7 cm in water coagulation bath at the 5aboutC. In the air gap extruded solution was covered in 6.3 times. The resulting fiber was washed diluted in water, alkali and water, dried on the drum 180aboutWith, was reeled at 594 m/min.

The resulting fibers, the concentration of PVP was 12% by weight of PEG, the Strength (tensile/modulus of elasticity) linear strength filaments obtained yarn was, respectively, of 23.9 g/denier (totaling 3.04%), 753 g/denier of 1.5 denier), 2111 DN/Tex (totaling 3.04%), 665 DN/Tex, 117 decitex.

As control samples, produced yarn in a similar manner, except that only used ECD-T (without adding PVP) at the same concentration of the spinning solution; the strength (tensile/modulus of elasticity) of the linear density of the specified yarn amounted respectively to 22.5 g/denier (3,01%), 690 g/denier of 1.5 denier), 19,9 DN/Tex (3,01%), 610 DN/Tex (1.7 dtex).

As the left 94%, the control fibers only 82%.

P R I m e R s 2-9. In these examples, the described changes in the mechanical properties depending on the changes in the content of PVP in the fibers.

Repeating the procedure described in example 1, using the same materials and the same conditions, except that the amount of PEG-T, PVP and sulfuric acid were changed as shown in table.1. Strength properties of the fibers of the described examples and fibers of example 1 and control fibers are presented in table.2, and Fig.1 shows a specific strength to the fibers of the case, as a function of the content of PVP in the fibers.

P R I m e R s 10 and 11. In these examples, the described fiber of the present invention, obtained with the use of PVP with different molecular weights.

Repeating the procedure described in example IX, using the same conditions, except that there were used to PVP with different molecular weights, as shown in the table.3.

P R I m e R 12. This example describes the ability to dyeing fibers of the present invention.

Using 1 g of the red dye Mach 1 red CPI (CI Basic Red 446), 6 ml of glacial acetic acid and 500 ml of distilled water is asnyk fibers was immersed in a dye bath at 110aboutC and kept there for about 2 hours Then the fibers were rinsed, washed with liquid soap at 110aboutAnd again thoroughly washed with water. Using the described procedures were dyed fibers of examples 1-7 with the purpose of their assessment in this example. This evaluation showed that abrasivejet increases significantly when PVP content 6%, reaches a maximum at 15% PVP and remains very high at 30% PVP.

The described procedure is repeated for dyeing the fibre samples using acid dye, identified as E Red (C. IX Acid Red 182). Evaluation of okrashivaemoy fibers with acid dye showed that abrasivejet sharply increases when the content of PVP in the range of 15-20% and remains approximately at the same level up to 30% PVP.

The degree of okrashivaemoy was determined by the above test method EATS 153-1985 scale values for red. The specified values for each test are given in table.4.

P R I m e p 13. In this example, tests for fire resistance of the fibers of the present invention.

Of the fibers obtained in accordance with the description in example 1 and containing 12% PVP, linked products in one C. This product has been evaluated by comparison with the product connected from the control yarn of example 1. The control product was charred with the formation of the through holes 8, and 10 with the product have discovered significant gaps, accompanied by shrinkage. The product is made from fibers of the present invention, showed no breaks or wrinkling even after 10 sec.

P R I m e R 14. This example describes the testing of the fibers of the present invention for bonding with the rubber when using the minimum quantity of stimulating the adhesion of the cushioning material.

The samples were manufactured in accordance with the procedure described above, using the fibers obtained from a mixture of PVP and PEG-T, and the PVP content was 15% by weight of PEG, the Control fibers were made only from ECD-Cords So received in accordance with the process described above, was immersed in a bath of coating, containing 26 wt.% epoxy resin (pFL), then was dried and utverjdali 60 seconds at a temperature of 450aboutC. After which the cords were subjected to testing in accordance with the described procedure.

The tensile strength of the control samples was 22.6 pounds (9.2 kg), and appearance with the deposits of view corresponded to the index of 4.5.

1. Continuous fiber made from a mixture of polyparaphenyleneterephtalamide with another polymer having the strength to 23.9 g/denier and a specific strength to 26.8 g/denier, wherein the other polymer it contains polyvinylpyrrolidone (mol.m. capabilities from 10,000 to 40,000 in the amount of 3-30 wt. % . , has an irregular cross-sectional shape and density 1,3484-1,4048 g/cm3.

2. The method of obtaining continuous fibers preparing a homogeneous solution of a mixture of polyparaphenyleneterephtalamide with another polymer in sulfuric acid under heating, extruding it through a die plate and the air layer in an aqueous coagulation bath followed by rinsing with water and/or dilute aqueous alkali solution, wherein the other polymer is used polyvinylpyrrolidone (mol.m. capabilities from 10,000 to 40,000 in the amount of 3-30% by weight polyparaphenyleneterephtalamide, the extrudate is pulled in the air gap is 6.3 times, and the coagulation is carried out at a bath temperature of 5oC.

3. The method according to p. 2, characterized in that the thickness of the air gap is 0.5 to 2.5, see

 

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