The composition of the spinning solution and yarn spun from him

 

(57) Abstract:

Describes the composition of the spinning solution comprising wholly aromatic polyamide containing links homopolymer formula [-(NH-C6H4-NHCO-C6H4-CO-)] , aliphatic polyamide containing links homopolymer polycaproamide or polyhexamethylenediamine, and concentrated sulfuric acid, characterized in that at least one polyamide is a copolymer consisting of two aromatic or two aliphatic chains of homopolymer, and aromatic copolymer has the formula

[- NH-C6H4-NHCO-C6H4-CO-)] u(-NH-C6H4-CaNH-C6H4-NHCO-C6H4-CO)w] where u = 75-90 wt.%, W = 10-25 wt.%

and aliphatic copolymer has the formula

[-(NH-(CH2)6-NHCO-(CH2)4-CO)n(-HN-(CH2)5-CO)m]

where n = 50-95 wt.%, m = 5-50 wt.%,

as for the composition of the spinning solution contains 16-19 wt.% fully aromatic polyamide, 0.6 to 4.0 wt.% aliphatic copolyamid, and the remaining amount corresponds to concentrated sulfuric acid. The technical result is a significant increase in the strength of the thread and resistance istian sinteticheskih threads, spun from anisotropic solutions in sulfuric acid of rigid-rod aromatic polyamides, mixed with aliphatic polyamides.

Spinning solutions of sulphuric acid and of aromatic and aliphatic polyamides, and also produced from these filaments are known from Japanese application N 59163418 A, which describes a spinning solution composed of 80-99 wt. % poly(para-phenyleneterephthalamide) and 1 to 20 wt.% aliphatic polyamide. The filament obtained from the specified spinning solution, in particular, suitable for the manufacture of paper.

In the European patent 392558 mentioned two-phase solution (spinning solution) of para-aramid polymer and a thermoplastic polymer, such polyhexamethylenediamine or poly( -caproamide). Suppose that produced from these filaments suitable for the manufacture termoformovannyh products (prepregs).

Although it is known that filaments of poly (para-phenyleneterephthalamide) are very heat resistant and have a very high strength, there is a need to improve their other characteristics. The prototypes of these other characteristics were improved by the use of mixtures. However, in turn, it has been found that this leads to a deterioration of other blagues use spinning solution according to the present invention can achieve improved physical properties without significant loss of other desirable properties. This improvement was achieved by use of the composition of the spinning solution comprising aromatic and aliphatic polyamide, and concentrated sulfuric acid, and it is characterized in that at least one of the aromatic and aliphatic polyamide is a copolymer consisting of units of two aromatic or two aliphatic homopolymers, respectively, and aromatic copolymer has the formula

(formula 1)

[- NH-C6H4-NHCO-C6H4-CO)u(NH-C6H4-CONH-C6H4-NHCO-C6H4-CO)w] where u = 75-90 wt.%, preferably 80-90 wt.%, and w = 10-25 wt.%, preferably 10-20 wt.%

and aliphatic copolymer has the formula

(formula II)

[-(NH-(CH2)6-NHCO-(CH2)4-CO)n(NH-(CH2)5-CO)m]

where n = 50-95 wt. %, preferably 60-93 wt.%, and m = 5-90 wt.%, preferably 7-40 wt.%.

Very good results are obtained by using a spinning solution according to the above invention, in which there is approximately 16-19.4 wt.% aromatic polyamide, 0.6-4.0 wt.% aliphatic polyamide and up to 100 wt.% concentrated sulfuric acid. This spinning solution in Order to avoid separation of the solution of aliphatic and aromatic (co)polyamides into two phases, that is anisotropic and isotropic phase, you need thorough mixing of the solution before it is processed, in particular, if the polymer mixture in solution contains more than 12 wt.% aliphatic polyamides in the calculation of the total amount of polymer in the solution.

In Japanese patent application JP 59/116411-A, as described for adhesion to rubber and other materials is usually applied finish coat. By adding aliphatic polyamide polymer spinning solution of poly(para-phenyleneterephthalamide) achieved an increase in adhesion. However, this addition is accompanied by a significant decrease in strength. By using a spinning solution of poly (para-phenyleneterephthalamide), aliphatic polymer of formula II and sulfuric acid can be obtained filaments that are suitable for the production of reinforced and savarirayan reinforced plastics and rubber products, in particular the cord for the reinforcement of tires.

When using a spinning solution of sulphuric acid, poly(para-phenyleneterephthalamide), and more than 5 wt.% normal aliphatic polymer of the total number present polymers, get yarn, characterized znachitelnie). As further illustrated by examples of test results are molded threads from mixtures of poly(para-phenyleneterephthalamide) and copolymer of formula II, reduction strength is much less. On the other hand, when using such a mixture can be increased adhesion properties of the fibres compared to threads based on poly(para-phenyleneterephthalamide). Aliphatic copolyamide preferably used in quantities of from 3 to 20 wt.% of the total number present in the polymer.

According to the patent application great Britain GB 2160878 a mixture of poly(para-phenyleneterephthalamide), aromatic-aliphatic copolyamid in concentrated sulfuric acid to produce fibers with high strength and modulus. The disadvantage of this method is the necessity of introducing into the mixture to 15 wt.% aromatic-aliphatic copolyamid, the receipt of which is very difficult, at least more difficult than obtaining poly(para-phenyleneterephthalamide). In addition, the filament density is not reduced, unlike what was found when using a spinning solution according to the present invention.

It was found that the abrasion resistance of the yarns obtained from spinning rest what to wear for prototype compositions threads, containing poly(para-phenyleneterephthalamide) and aliphatic polyamide.

It was unexpectedly found that with the introduction of the above-mentioned aliphatic copolyamid formula II at a certain ratio between the components of the strength of the thread and its abrasion resistance increase dramatically. The mechanism of increase of strength filaments of the above mixtures, obviously, differs from that which takes place by mixing aromatic-aliphatic additive poly(para-phenyleneterephthalamide), as in the patent application great Britain GB 2160878 as aliphatic copolyamide cannot be incorporated into the crystal lattice of poly(para-phenyleneterephthalamide).

By using aliphatic copolyamid formula II in the amount of 8 wt. % with the rest of the number (92 wt.%) the polymer is a poly(para-phenyleneterephthalamide), the result is a thread that has the strength to 2010 - 2059 mn/Tex, while comparable filament polymer poly(para-phenyleneterephthalamide) has a strength of about 2059 mn/Tex. The strength of the thread increases, when combined with aliphatic copolyamides formula II used aromatic copolyamide formula I. When compared with the strength of the thread based on the same poly(para-familientherapie the high concentrations of aliphatic copolyamid in the mixture of polymers (up to 20 wt.%) achieved with lower strength threads in comparison with aliphatic polyamides, such as polycaproamide or polyhexamethylenediamine or mixtures thereof.

The number of input aliphatic polyamides is 3-20 wt.% from a mixture of polymers. Adding less than 3 wt.% aliphatic copolyamids has no significant effect on the properties of the filaments. Adding more than 20 wt. % of such aliphatic polyamide leads to decrease in strength, which is not considered acceptable for use threads.

It was found that the strength of the threads is not reduced when a mixture of aromatic copolyamid formula 1 and aliphatic polyamide, such as polycaproamide or polyhexamethylenediamine (PA 6 and PA 66), in contrast to what was observed when using poly(para-phenyleneterephthalamide) and such aliphatic polyamide. Moreover, it has been found that yarns made from found compositions have a low density, which is considered favorable in applications where a low density combined with high strength thread. In particular, this occurs when the thread is used to produce reinforced plastics, reinforced rubber products and insulation materials.

Therefore, the invention also covers spinning R is the notes.

Very favorable spinning solution and spun him a yarn obtained when spinning a solution of an aromatic copolyamid formula I are used together with aliphatic copolyamides formula II and with concentrated sulfuric acid. The spinning solution preferably contains 16-18.5 wt. % aromatic copolyamid 1.5-4.0 wt.% aliphatic copolyamid, and the rest is sulfuric acid.

The invention is further illustrated by the following examples. In these examples, the logarithmic viscositylog, which is defined aslog= ln(rel)/C, where C is the concentration, determined by viscometric method for the solutions containing 0.5 g of polymer in 100 ml of 96% sulfuric acid at 25oC. the strength of the yarn with the right twist, determine when the clamp thread a length of 500 mm in the device Instron to determine the tensile strength according to standard techniques.

Example 1

20% spinning solution get in the reactor with a capacity of 63 liters. For this 9.5 kg (19 wt.%) aromatic copolyamid formula I, where u = 90, w = 10 wt.%, with logarithmic viscosity of 5.5 DL/g, 0.5 kg (1 wt.%) aliphatic copolyamid formula II, where n = 80 and m = 20 wt.%, with logarithmic visco is the target serves to filter and spinning machine. Molding is carried out by dry-wet method through an air gap of about 10 mm into the precipitation bath containing 10% sulfuric acid at a temperature of 8oC. the speed of the receiving thread is 85 m/min Using a Cup dies of precious metal with a diameter of bowl 28 mm, number of 1000 holes and hole diameter 0.07 mm, range hood Multiplicity of streams of spinning solution is 8.2. On a spinning machine, the yarn is subjected to washing under a tension of 20 to 60 mn/Tex. Then hold neutralization of the acid with the use of a 0.02% aqueous solution of sodium hydroxide. Then the thread is dried at a temperature of 120-150oC and take on the receiving device without twist after spinning.logthe mixture of polymers in the thread is 4.8 DL/, Then the thread is subjected to a twist of 80 turns per meter. The linear density of the yarn is 167 dtex, the strength of the thread (specific breaking load) - 2255 mn/Tex and elongation (at break) - 4.3%. It was found that the abrasion resistance is 23 thousand cycles.

Example 1A (comparative)

The strength of the thread being formed under conditions similar to those of example 1, a 20% aqueous solution used in example 1 copolyamid, and as described in example 1, but without adding LASS="ptx2">

Example 1B

The thread formed by the same procedure indicated in example 1, when this is used the same number of aromatic copolyamid formula I. Instead aliphatic copolyamid formula II at this time the mixture thus impose a similar number of polycaproamidelog1.2 DL/g, and a thread formed under conditions similar to those of example 1. The resulting yarn has the strength of 1990 mn/Tex and the abrasion resistance of 12 thousand cycles. It was found that the adhesion is better than the adhesion of the filaments obtained in example 1A.

Examples 2-7

Received several spinning solutions, and used various compounds and polymers with different structures. Spinning solutions containing 20 wt.% polymers obtained by mixing the polymeric component with 99.8% sulfuric acid. After 4 hours of mixing in the mixer under vacuum at 75oC obtained anisotropic solution is fed to the filter and then to the spinning machine. Threads formed in the same way as described in example 1. Measure the strength of the threads and abrasion resistance; they are listed in table 1. In table 1 also indicate the name and quantity of each polymer used. Aromatic copolyamide is copolyamide foro)of the polyamides is 1.2 DL/g

For polymer compositions that do not contain aliphatic copolyamide formula II, but contains instead a homopolymer of aliphatic polyamide such as polycaproamide or polyhexamethylenediamine, was found comparable strength derived from these threads. The threads obtained from these polymer compositions have significantly increased adhesion compared to compositions not containing an aliphatic polyamide. The superiority of the characteristics of the yarns obtained from polymer compositions containing aromatic copolyamide formula I, and aliphatic copolyamide formula II, it is evident from the above results.

Example 8

38 g (19 wt.%) poly(para-phenyleneterephthalamide)log5.8 DL/g and 2 g (1 wt. %) aliphatic copolyamid formula II when n = 85 and m = 15 wt.% and Clog1-2 DL/g is introduced into the mixture in 87.4 ml (80 wt.%) 99.8% sulfuric acid is stirred in a mixer for 3 hours at 82oC, filtered and dearyou for one hour at a temperature of dissolution. From the thus obtained anisotropic spinning solution containing 20% polymer, formed into filaments 5 mm air gap on the dry-wet method in water with a temperature of 10oC at a speed of Versti is 0.08 mm Wet the thread take on a bobbin and washed from acid. Then the thread is dried at room temperature and rolled up to 150 turns/meter.logthe polymer mixture in the thread is 4.8 DL/g, the linear density of the yarn - 29.4 Tex, the strength of the thread is 2059 mn/Tex, elongation at break - 3.4%, the abrasion resistance of the filament - 22 thousand cycles.

Example 8A (comparative)

The strength of the yarn, spun from a solution containing 20% polymer poly(para-phenyleneterephthalamide), without any aliphatic (co)polyamide is 1961 mn/Tex, and the abrasion resistance is 10 thousand cycles.

Example 9

36 g (18 wt.%) poly(para-phenyleneterephthalamide) and 4 g (2 wt.%) aliphatic copolyamid formula II when n = 85 and m = 15 wt.% (log1.2 DL/g) was injected in the form of a mixture in 87.4 ml (80 wt.%) 99.8% sulfuric acid is stirred in a mixer for 3 hours at 82oC, filtered and dearyou for one hour at a temperature of dissolution. Forming filaments carried out as described in example 8.logthe polymer mixture in the thread is 4.8 DL/g, the Strength of the thread 1961 mn/Tex, an elongation at break of 3.3%, the abrasion resistance of 20 thousand cycles.

Example 9A (comparative is isovale polycaproamide and polyhexamethylenediaminelogboth 1.2 DL/g, the obtained filament has a tensile strength of about 1441 mn/Tex and the abrasion resistance of 8 thousand cycles. The solution, from which were made these threads, has the following composition: 18.4/1.6/80 wt.% (poly(para-phenyleneterephthalamide)/PA 6 or PA 6.6/sulfuric acid).

Example 10

18.5 wt.% aromatic copolyamid formula I in which u = 90, w = 10 wt. %log5.5 DL/g and 1.5 wt.% polyhexamethylenediaminelog1.0 DL/g (7.5 wt. % of aliphatic polyamide in a mixture of polymers) dissolved in 43.7 ml (80 wt.%) 99.8% sulfuric acid is stirred in a mixer for 3 hours at 74-78oC, filtered and dearyou within 1.5-2 hours at a temperature of dissolution. Forming filaments carried out as described in example 8.logthe mixture of polymers in the thread is 5.1 DL/g Linear density yarn 29.4 Tex, density 1.35 g/cm3. Found strength filaments 2010 mn/Tex corresponds to the strength of the thread does not contain any flexible-chain polymer, but spun under the same conditions from a solution of rigid-chain polyamide containing 20% polymer. It was found that the Flexural resistance of the obtained yarn is 14000-16000 cycles, while the Flexural resistance for threads that do not contain the aliphatic polium store capacity of 60 HP For this purpose use 18 wt.% the aromatic polyamide of the formula I, where u = 85 & w = 15 wt.% withlog5.5 DL/g; 2 wt.% polyacrylamidelog1.33 DL/g (10% aromatic polyamide in the mixture of polymers); and 22 l (80 wt. %) 99.8% sulfuric acid. The preparation of the spinning solution and the formation of the thread carried out as described in example 1.logthe mixture of polymers in the thread is 4.8 DL/g Linear density yarn of 167 dtex, density of 1.35 g/cm2. The strength of the thread is 2010 mn/Tex, which corresponds to the strength of the filaments obtained in the same conditions only from poly(para-phenyleneterephthalamide), i.e. not containing any flexible-chain polymers (aliphatic polyamide). Dynamic modulus of elasticity of the thread is 98066 H/mm2, elongation at break of 3.5%.

Example 12

The preparation of the spinning solution and the formation of the thread carried out as described in example 1, except that use 17 wt.% aromatic copolyamid formula I, where u = 80, w = 20 wt.% andlog5.5 DL/g, together with 3 wt.% polycaproamidelog1.33 DL/g Thus, the polymer mixture comprises 15 wt.% aliphatic polyamide.logthe polymer mixture in the thread is 4.7 DL/g LINEST is amicucci the modulus of elasticity is 107866 H/mm2, elongation at break - 3.2-3.6%. The decline in the strength of the thread in comparison with the thread, not containing flexible chain is 7 - 12%.

Example 13

The preparation of the spinning solution and the formation of the thread carried out as described in example 1, except that use 16 wt.% aromatic copolyamid formula I, where u = 75, w = 25 wt.% withlog5.5 DL/g, together with 4 wt.% polycaproamide log1-33 DL/G. Thus, the polymer mixture comprises 20 wt.% aliphatic polyamide.logthe polymer mixture in the thread is 4.65 DL/g, the Density of the filament is 1.17 g/cm3the strength of the thread - 1617-1716 mn/Tex. Dynamic modulus of elasticity is 93157-118000 N/mm2, elongation at break - 3.3-3.7%. The decline in the strength of the thread in comparison with the thread, not containing aliphatic polyamide (2010 mn/Tex), is 15-20%.

Example 14 (comparative)

The preparation of the spinning solution and the formation of the thread carried out similarly as described in example 8, except that the use of 18.4 wt.% poly(para-phenyleneterephthalamide) (log5.8 DL/g) together with 1.6 wt. % of polycaproamide (log1.33 DL/g) and 43.7 ml (80 wt.%) 99.8% sulfuric acid.logpolymer clay strength filaments on the basis of poly(para-phenyleneterephthalamide), equal 2010 mn/Tex). Thus, the loss of strength is 30%. The resistance to bending of the thread is 6000 cycles. For filaments of poly(para-phenyleneterephthalamide) without any aliphatic polyamide, this indicator amounted to 1000 cycles.

Example 15 (comparative)

The preparation of the spinning solution and the formation of the thread carried out similarly as described in example 8, except that the use of 18.6 wt.% poly(paraphenylenediamine) (log5.8 DL/g) with 1.4 wt. % polyhexamethylenediaminelog1.33 DL/g and 43.7 ml (80 wt.%) 99.8% sulfuric acid. The density of the thread was 1.42 g/cm3and has not changed compared with the density of threads based on poly(para-phenyleneterephthalamide), not containing an aliphatic polyamide. The strength of the thread is 1441 mn/Tex. Thus, the loss of strength is 30%.

1. The composition of the spinning solution comprising wholly aromatic polyamide containing links homopolymer formula

[-(NH - C6H4-N-C6H4-CO-)],

aliphatic polyamide containing links homopolymer polycaproamide or polyhexamethylenediamine, and concentrated sulfuric acid, characterized in that minority who Nievo of homopolymer, and aromatic copolymer has the formula

[-(NH-C6H4-N-C6H4-CO)u(-NH-C6H4-N-C6H4-N-C6H4-CO)w] ,

where u = 75 - 90 wt.%, w = 10 to 25 wt.%,

and aliphatic copolymer has the formula

[-(NH-(CH2)6-N-(CH2)4-CO)n(-NH-( CH2)5-CO)m],

where n = 50 to 95 wt.%, m = 5 to 50 wt.%,

as for the composition of the spinning solution contains 16 and 19.4 wt.% fully aromatic polyamide, 0.6 to 4.0 wt.% aliphatic copolyamid, and the remaining amount corresponds to concentrated sulfuric acid.

2. The composition of the spinning solution on p. 1, wherein u = 80 - 90 wt.%, w = 10 - 20 wt.%, n = 60 to 93 wt.%, m = 7 to 40 wt.%.

3. The composition of the spinning solution under item 1 or 2, characterized in that the aromatic polyamide has the formula

[-(NH-C6H4-N-C6H4-CO)u(-NH-C6H4-N-C6H4-N-C6H4-CO)w] ,

where u = 75 - 90 wt.%, w = 10 to 25 wt.%.

4. The composition of the spinning solution under item 1 or 2, characterized in that the aliphatic copolymer has the formula

[-(NH-(CH2)6-N-(CH2)4-CO-)6H4-N-C6H4-CO-)]

and aliphatic polyamide, characterized in that at least one polyamide is a copolymer consisting of two aromatic or two aliphatic chains of homopolymer, and aromatic copolymer has the formula

[-(NH-C6H4-N-C6H4-CO)u(-NH-C6H4-N-C6H4-N-C6H4-CO)w] ,

where u = 75 - 90 wt.%, w = 10 to 25 wt.%,

and aliphatic copolymer has the formula

[-(NH-(CH2)6-N-(CH2)4-CO)n(-N-(CH2)5-CO)m],

where n = 50 to 95 wt.%, m = 5 to 50 wt.%.

6. Thread on p. 5, wherein the aromatic polyamide has the formula

[-(NH-C6H4-N-C6H4-CO)u(-NH-C6H4-N-C6H4-N-C6H4-CO)w] ,

where u = 75 - 90 wt.%, w = 10 to 25 wt.%.

7. Thread on p. 5, characterized in that the aliphatic copolymer has the formula

[-(NH-(CH2)6-N-(CH2)4-CO)n(-N-(CH2)5-CO)m],

where n = 50 to 95 wt.%, m = 5

 

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