Polyparaphenyleneterephtalamide pulp

 

(57) Abstract:

The invention relates to the production of high-quality fiber pulp. Create a mixed polyparaphenyleneterephtalamide system, adding stoichiometric amount polyparaphenyleneterephtalamide components to their solvent and polyvinylpyrrolidone with srednevozrastnoe molecular weight of at least 100 000, taken in an amount of 5-30%, based on the weight of the obtained polymer. Continue interaction polymerizable components for the transition system in the anisotropic phase and before the formation of the mixture polyparaphenyleneterephtalamide with polyvinylpyrrolidone. Then separate it from polimerizuet system. Fibrous pulp contains 70-95 wt.% polyparaphenyleneterephtalamide and 5-30 wt.% polyvinylpyrrolidone. Individual particles of the pulp does not contain hair and have a length of from 0.5 to 10 mm, a diameter of from 0.1 to 50 μm, and the ratio of length to diameter of the short fibers is greater than 100. The formation of the pulp is greatly simplified due to the optional intensive mixing or exposure components of shear strain. 2 S. and 4 C.p. f-crystals, 2 tab., 7 Il.

The present invention relates to the production of visocekas is of molded aramid fibers, after mechanical refining take the form of a fiber or bundle of fibrils protruding from it.

In the present invention is proposed pulp derived not from spun fibers, and in which beams of particles of the pulp have a high proportion of fibrils and a very low share of the awn.

In the description of the U.S. patent N 5073440 and 5135687 issued on applications of Kiu-Seung Lee, offers a continuous monofilament, containing paraaramid and method of forming such fibers.

In applications for Europatent N 381172 and 395020, published September 8, 1990 and November 7, 1990, disclosed a homogeneous mixture of some aromatic polyamides with polyvinylpyrrolidone and continuous fibers and films prepared on the basis of them.

In the description of the U.S. patent N 4511623 issued on the application of H. S. Yoon, disclosed is a method of obtaining short aramid fibers, namely, that the solution of polymerizable aramid subjected to shear stress.

In the description of the U.S. patent N 5028372 issued on the application Brierre and other features of the method of producing pulp, which consists in the fact that anisotropic solutions containing paraaramid undergoing polymerization, is subjected to shear deformation with the purpose of orientation on the buy offers a way of fibrous pulp from a mixture of PPD-T and polyvinylpyrrolidone (PVP), namely, that:

get mixed PPD-T-polymerized system comprising a solvent for the polymerizable components, and PVP with srednevozrastnoe molecular weight of at least 100,000, taken at a concentration of at least 5 wt.%, preferably at least 10 wt.%, based on the weight of the obtained polymer; add stoichiometric amounts of the components for the polymerization of PPD-T for interoperability of components in a polymerization system; continue cooperation polymerizable components for a period of time sufficient to move polymerizable system in the anisotropic phase, perform a full reaction of PPD-T-polymerizable components with the formation of a mixture of PPD-T and PVP; and separating the mixture of PPD-T and PVP from polimerizuet system.

The fibrous pulp is obtained in accordance with the method of the present invention includes a heterogeneous mixture containing polyparaphenyleneterephtalamide and at least 5 wt.% polyvinylpyrrolidone having srednevozrastnoe molecular weight of more than 100,000, in which individual particles of the pulp does not contain a long thread and have a length of from 0.5 to 10 mm, a diameter of from 0.1 to 50, 1-5 shows pictures of polymeric materials on the basis of aramid fiber, executed in various conditions, including the conditions of the method of the present invention. In Fig. 1 shows a product with heterogeneous fibrous texture, and Fig. 2-5 shows the products obtained from the fibrous pulp of the present invention.

In Fig. 6 shows thermogravimetric analysis of a heterogeneous mixture of PPD-T and PVP of the present invention.

In Fig. 7 is a curve of thermogravimetric analysis of a homogeneous mixture of the aromatic polyamide and PVP disclosed in the prototype.

Detailed description of the invention

Fibrous pulp of the present invention is obtained from two-component polymer mixture. As one component used polyparaphenyleneterephtalamide (PPD-T) and polyvinylpyrrolidone (PVP).

The term PPD-T in this description should be understood a homopolymer obtained by polymerization mechanism "mole-to-mole" paraphenylenediamine and terephthaloylchloride, as well as copolymers obtained by adding small amounts of other diamines to para-phenylenediamine and small amounts of other acid chlorides dick is but used in amounts up to about 10 mol.% of the total weight of paraphenylenediamine or terephthaloylchloride, or maybe a little higher concentrations, provided that the other diamines and acid chlorides of dicarboxylic acids do not contain any reactive groups which interfere with the polymerization reaction. Under PPD-T should also be understood in this description, the copolymers obtained by adding small amounts of other aromatic diamines and other aromatic anhydrides of dicarboxylic acids such as 2,6-naftanaila or chlorine - or dichlorotetrafluoroethane. In the description of the U.S. patent N 4308374 and 4698414 disclosed is a method of obtaining the PPD-T.

PVP is an additive polymer contained in the pulp fibers of the present invention. The term PVP in this description should be understood polymeric material obtained by linear polymerization of monomer units of N-vinyl-2-pyrrolidone and which also contains small amounts of comonomers which may be present in the polymerization mixture at concentrations below those which do not inhibit the interaction of PVP with PPD-T.

The mixture of the polymer components produced by polymerization of PPD-T in the presence of PVP. The preferred medium for carrying out the polymerization of PPD-T is a fully waterless see is never the same after its formation. To increase the solubility of the PPD-T is possible to use other salts, including chloride Quaternary ammonium, lithium chloride, magnesium chloride, strontium chloride, and the like, which are soluble in NMP. In accordance with the present invention the system is used as a solvent may also contain PVP dissolved as the reaction of polymerization of the PPD-T.

For practical reasons preferably dissolving PVP in NMP before adding any of the aforementioned salts. It was found that salt, though, and increases the solubility of PPD-T in polimerizuet system, it can reduce the initial solubility of PVP in NMP.

I believe that PVP is present dissolved in NMP during the polymerization process PPD-T, where the set of anisotropic phase, leads to the fact that the polymerizable PPD-T forms oriented or aligned domains of polymer molecules, which ultimately leads to the formation of fibers of the pulp. In the formation of fibers of the pulp, due to the anisotropic nature of the system, PPD-T and PVP, as I believe, are mixed so that the domains PPD-T surrounded PVP, resulting in a gain of a particle slurry containing a heterogeneous combination of these two materials.

Thermogravimetric analysis (TGA) is carried out by heating the sample material and registration of shrinkage weight of the sample in dependence on temperature. Weight changes occur at temperatures volatility of the components of the sample. The material shown in Fig. 6, which were subjected to thermogravimetric analysis is a mixture consisting of PPD-T and 20 wt.% PVP, obtained in accordance with the present invention. PPD-T had a characteristic viscosity of 5.1 and PVP had srednevozrastnoe molecular weight 630000. It should be noted that the curve shown in Fig. 6 has two steepness. The first slope begins at the point a temperature of about 440oC and represents the volatilization component of PVP. Rapid volatilization of PVP takes place at a temperature of approximately 500oC, and then more slowly at a temperature of approximately 600oC. a Second slope begins at the point a temperature of about 600oC and demonstrates the volatilization component of the PPD-T. Thus, two separate steep angle in the curve of the TGA give a clear proof of the existence of physically separate components in the composition of the present invention.

In Fig. 7 shows a curve based on data thermogravimetrical)phenyl]propertiestoload (BAPP-T), which, as disclosed in the description, forms associated homogeneous composition comprising 20 wt.% PVP. BAPP-T, polymerized in the presence of PVP, leads to the establishment of isotropic and not anisotropic phase components, and as is clear from the above-mentioned applications Europatent is a tightly associated homogeneous composite alloy. It should be noted that the curve shown in Fig. 7 has a curvature that starts at point a temperature of about 380oC and passes through the point 600oC, demonstrating the volatilization of a homogeneous mixture BAPP-T and PVP. Thus, only the curvature in the TGA curve gives a clear proof of the existence of the associated homogeneous composition of the materials disclosed in the prototype.

It is established that for the practical implementation of the invention requires that PVP had srednevozrastnoe molecular weight of more than about 100,000, and a concentration of at least 5%, preferably at least 10%, based on the weight of the PPD-t and PVP with srednevozrastnoe molecular weight less than about 100,000, as it turns out, does not provide an adequate basis for the orientation of the growing polymer chains PPD-T and, consequently, does not give effective results. Materialet to get solutions suitable for use at required concentrations of PVP. PVP with srednevozrastnoe molecular weight greater than 100,000, as determined suitable for use in practice of the present invention. For the purposes of the present invention PVP with the desired molecular weight distribution can be obtained by mixing materials based PVP with different molecular weight. For example, PVP, having srednevozrastnoe molecular weight of 50000, can be mixed with PVP having srednevozrastnoe molecular weight of 500000 taken in such quantities as to produce an overall srednevozrastnoe the molecular weight of PVP in polimerizuet system that exceeds 100,000, calculated as mole fraction.

We need the presence of PVP in the amount of at least 5 wt.% in the calculation of the mass formed by the PPD-T, although if you want you can use it in larger quantities. The use of PVP in the amount of less than 5 wt.%, as it turns out, does not provide sufficiently obtain the desired effect from PVP. The upper limits for the concentration of PVP is chosen as a practical expedient. In the course of invention found that the size and quality colocasia on the mass formed by the PPD-T. The concentration of PVP more than 30%, as installed, does not affect the results, but they do not cause a substantial increase in either the size or the output of the fibrous product.

The polymerization process of the PPD-T involves the step of introducing into the polymerization system of stoichiometric amounts of a diamine and acid chlorides of dicarboxylic acids. Diamino component, usually dissolved in a polymerization system, and the acid chloride dicarboxylic acid is then added to the mixture for polymerization or immediately at once or in several portions.

System components for the polymerization of PPD-T are introduced with stirring, and the stirring of the mixture is usually continued until the formation of the anisotropic solution and then during the polymerization PPD-T to the complete termination of the polymerization reaction. PPD-T and polymerizing system become extremely viscous in the course of the polymerization reaction, and therefore it is preferable to continue the stirring for maintaining contact between the reacting components. However, it is not necessary that the components in the polymerization system was subjected to intensive mixing or shear stress; and, in fact, there is no need for such mixing, as tolie can be used in practice of the present invention, it should be understood that the length and quality of the fibrous product depends on the concentration and molecular weight of PVP, which is present in the polymerization system. Rational grain of the present invention and that, according to the authors, significant from the point of view of patentability is to ensure that the pulp is a heterogeneous reaction product of polymerization of PPD-T, carried out in the presence of PVP in the conditions described earlier in this description, using anisotropic polimerizuet system.

At the completion of the polymerization reaction of PPD-T fiber pulp PPD-T is separated from the polymerization system by decomposing the obtained solid product in water, followed by several washing, filtering or centrifuging the slurry to separate from the liquid.

The obtained fibrous pulp is a polymer based on PPD-T containing 5 to 30, preferably from 10 to 25% PVP, based on the weight of the PPD-T. the Concentration of PVP in the pulp, to some extent, dependent on the concentration of PVP in polimerizuet system. For example, the PPD-T, containing about 10% PVP is formed from polimerizuet system, in which the concentration of PVP is 10%. However, it is becoming obvious is CE, no matter how high may be the PVP concentration in the polymerization system. I think that PVP in varying degrees mixed with PPD-T to a concentration of approximately 20% and, if it exceeds this limit, any excess PVP washed from the pulp phase separation. Of course, you may receive the pulp, where the PVP content exceeds 20% by polymerization of PPD-T in the solution containing PVP at a concentration of more than 20%, and then you need to follow in order to ensure washing of the pulp is not fully. As mentioned earlier, the PVP is present in the slurry in excess of about 20%, is not formed in the associated part of the material on the basis of PPD-T/PVP: however, he does not have an appreciable adverse impact on the characteristic performance of the pulp.

Particles of the pulp according to the invention have an average length of about 0.5 to about 10 mm, or may be slightly greater length, their diameter is only approximately from 0.1 to 50 μm, and the ratio of length to diameter of the short fibers is more than 100. Under the definition of "the ratio of the length to the diameter of the short fibers" shall mean the ratio of the length of the individual particles of the pulp to its diameter. Due to the fact that these particles are not refined from forms/BR> Although the quality of the pulp particles may present some difficulties for help can the attached Figure, which shows the fibrous particles of the pulp of varying quality at 40 times their gain:

Fig. 1 shows a stamp with a shape factor of 1, and illustrates particles, crumbs PPD-T are obtained by using additives that do not contain PVP. Particles of the brand with a shape factor of 1 does not have a fibrous structure.

Fig. 2 shows a stamp with a shape factor of 2, and illustrates the low quality fibrous pulp of the present invention. Pulp brand with a factor of the form 2 has a predominantly fibrous structure and includes a fiber length of about 2 mm

Fig. 3 shows a stamp with a shape factor 3 and illustrates the fibrous pulp of medium quality. Pulp brand with shape factor 3 has a predominantly fibrous structure and includes a fiber length of approximately 3 mm

Fig. 4 shows a stamp with a shape factor 4 and illustrates the pulp of good quality with a fiber length of approximately 5 mm

Fig. 5 shows a stamp with a shape factor 5 and illustrates the pulp of good quality fiber length p is given by the equation

IV = ln(from)/c

where c is the concentration (0.5 gram of polymer in 100 ml of solvent) PPD-T polymer solution, and

from(relative viscosity) is the ratio between the duration of the flow volume of the polymer solution and the solvent as measured at 30oC in a capillary viscometer.

The values of the characteristic viscosity given in this description, define when using concentrated sulfuric acid (96% H2SO4).

Srednevozrastnoe molecular weight PVP

As used in this description, the expression "molecular weight PVP" means srednevozrastnoe molecular weight characteristics which give Kirk-Othmer, Encyclopedia Wiley & Sons, page 968 in the article titled "Vinyl Polymers (N-Vinyl)" "Polymers based on vinyl (N-vinyl)". Srednevozrastnoe molecular mass Mvassociated with a characteristic viscosity in the following ratio:

< / BR>
The characteristic viscosity is determined by a commonly known method of measuring the relative viscosity at several concentrations of the polymer, with subsequent extrapolation of the viscosity at zero concentration (characteristic viscosity). Suppliers PVP often identify PVP-product "number K, which is associated with x is colerne mass PVP can be calculated by the values of "K", using the equations, above.

Thermogravimetric analysis

Thermogravimetric analysis to test the samples was conducted in accordance with the techniques described in the standard ASTM D 3850-84 with nitrogen.

Examples

Example 1

In the reaction vessel, a mixed PPD-T-polymerized system was obtained by dissolving 12.5 parts of calcium chloride in 147,5 parts of N-methylpyrrolidone (NMP). Calcium chloride and NMP carefully and fully dried. 9,329 parts paraphenylenediamine was dissolved in polimerizuet system, was then added and 24.2 parts of a solution containing 15 parts of PVP in 85 parts of NMP. PVP having a molecular weight 630000 obtained from company International Specialty Products, Wayne, New Jersey, USA. While continuing the stirring, polymerized system was cooled to a temperature of about 5oC, and then added 17,670 parts terephthaloylchloride.

After a very short period of time polymenorrhea system has become a matte color, indicating that the transition in the anisotropic phase, and after about 2 minutes polymerizable mixture reached a maximum viscosity with the formation of a very viscous gel (plastisol). Stirring is continued, after which the gel was crushed to particles with high mu pulp was washed several times with water in the mixer to remove NMP, CaCl2and HCl formed during polymerization. The obtained polymer had a characteristic viscosity of 5.7, and the pulp had the shape factor (the degree of sphericity of the particles) 5 elementary fibers, having a length of approximately 5-7 mm

Comparative example 1C

The polymerization reaction was conducted in a similar manner as described above in example 1, except that PVP had a molecular weight of only 38000. The resulting product was a crumb-like PPD-T without characteristics of fibrous material. PPD-T had a characteristic viscosity of 5.8.

Examples 2-6

In these examples used the same method of polymerization, which is described in example 1, except that PVP was a mixture of two materials having different molecular weight. Used PVP with molecular weight of 38000 and 630000 to get PVP with a wide variety of equivalent molecular weights; however, in each example used in the amount of 15% PVP. Table 1 shows the characteristic data regarding PVP, as well as data on the obtained fibrous pulp. Dried by distillation.

Examples 7-11

In these examples used a similar is slichnih quantities. In these examples, PVP had a molecular weight of about 630,000. Table 2 provides details of the examples, as well as data on the obtained fibrous product.

Example 12

This example shows that a continuous mixing it is not necessary for the practical implementation of the present invention. As in the above example 1, the PPD-T-polymerized system was obtained by dissolving 12.5 parts of calcium chloride in 147,5 parts of N-methylpyrrolidone (NMP), with stirring. 9,329 parts paraphenylenediamine was dissolved in polimerizuet system, was then added and 24.2 parts of a solution containing 15 parts of PVP in 85 parts of NMP. PVP has a molecular weight 630000. While continuing the stirring, polymerized system was cooled to a temperature of about 5oC and then added 17,670 parts terephthaloylchloride.

After a very short period of time polymenorrhea system has become a matte color, indicating that the transition in the anisotropic phase, after which the stirring was stopped and the polymerization mass was passed during the night.

The obtained fibrous pulp was washed several times with water in the mixer to remove NMP, CaCl2and HCl formed in PRMI (the degree of sphericity of the particles) 3 elementary fibers, having a length of approximately 2 mm

1. The method of obtaining fibrous pulp polyparaphenyleneterephtalamide and polyvinylpyrrolidone, namely, that involves the following stages: a) create a mixed polyparaphenyleneterephtalamide polimerizuet system containing a solvent for the polymerizable components and polyvinylpyrrolidone having srednevozrastnoe molecular weight of at least 100,000 and taken in an amount to obtain its concentration in polimerizuet system from 5 to 30 wt. % (based on the weight of the obtained polymer; C) adding stoichiometric quantities polyparaphenyleneterephtalamide components for interoperability of components in polimerizuet system; (C) continue the interaction polymerizable components over a period of time sufficient to (i) transition polimerizuet system in the anisotropic phase, (ii) the full flow of the reaction polyparaphenyleneterephtalamide components and (iii) formation of a mixture polyparaphenyleneterephtalamide with polyvinylpyrrolidone: and (d) separating the mixture obtained polyparaphenyleneterephtalamide and polyvinylpyrrolidone from polimerizuet system.

2. The method according to p. 1, Kay components used paraphenylenediamine and terephthaloylchloride.

4. The method according to p. 1, in which the polyvinylpyrrolidone is one polymer with srednevozrastnoe molecular weight of at least 100000.

5. The method according to p. 1, in which the polyvinylpyrrolidone is a mixture of polymers with srednevozrastnoe molecular weight of at least 100000.

6. Fibrous pulp polyparaphenyleneterephtalamide consisting of a mixture containing from 70 to 95 wt.% polyparaphenyleneterephtalamide and from 5 to 30 wt.% polyvinylpyrrolidone with srednevozrastnoe molecular weight greater than 100,000, in which individual particles of the pulp does not contain hair and have a length of from 0.05 to 10 mm, a diameter of from 0.1 to 50 μm and the ratio of the length to the diameter of the short fibers is greater than 100.

 

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