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High-modulus poly(p-phenylene terephthalamide) (PPTA) fiber and preparation method thereof

A technology of poly-p-phenylene terephthalamide and phthaloyl-p-phenylene diamine is applied in the field of high-modulus poly-p-phenylene terephthalamide fiber and its preparation field, and can solve the difficulty of fiber technology , affecting industrial efficiency and other issues, to achieve the effect of a wide range of applications, low industrial costs, and good performance

Active Publication Date: 2011-11-23
BLUESTAR CHENGDU NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the molecular weight is too high, the process of making fibers is very difficult, which affects industrial efficiency

Method used

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  • High-modulus poly(p-phenylene terephthalamide) (PPTA) fiber and preparation method thereof
  • High-modulus poly(p-phenylene terephthalamide) (PPTA) fiber and preparation method thereof
  • High-modulus poly(p-phenylene terephthalamide) (PPTA) fiber and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0051] This example describes the preparation of polyparaphenylene terephthalamide (PPTA) polymer by low temperature solution polycondensation method

[0052] A. Preparation of raw materials

[0053] P-phenylene diamine [PPD],

[0054] Terephthaloyl chloride [TPC],

[0055] The solvent is (N-methyl pyrrolidone)[NMP],

[0056] The co-polysalt (ie co-solvent) is calcium chloride (CaCl 2 );

[0057] Among them: the molar ratio of PPD / TPC is equal to 1.0, and CaCl 2 The molar ratio of / PPD is equal to 1.2, and the solid content of the polymerization mixture is 9%;

[0058] B. Polymerization of raw materials

[0059] Pour nitrogen into the oven after drying, and then add dry NMP / CaCl 2 Solvent and dry high-purity p-phenylenediamine (PPD), turn the stirrer, and mix well, activate the chilled water jacket of the reactor, gradually dissolve the mixture of p-phenylenediamine PPD and solvent NMP and cool down within 1 minute To 20℃, then add a total of 30 % Terephthaloyl chloride (TPC), continue...

Embodiment 2

[0060] Example 2 Spinning process of dry jet wet spinning process

[0061] The polyparaphenylene terephthalamide (PPTA) polymer with a logarithmic viscosity of 6.5dL / g prepared in Example 1 was added to sulfuric acid with a concentration of 99.8%, and the mixture was stirred vigorously and heated to 80°C. A spinning pulp with a concentration of 19.4% is formed. After filtration, the slurry is metered by a gear pump and sprayed from the spinneret; the spinneret has 1000 spinning holes with a hole diameter of 0.063mm. The spinning pulp is sprayed out of the spinning holes to form a pulp The silk passes through a 6mm air layer, enters the surface of the coagulation solution, and then passes through the coagulation tube in the center of the coagulation tank, and flows out from the bottom of the tube. The coagulation bath temperature is 4℃, and the acid content of the coagulation liquid is 10%. The sulfuric acid contained in the sizing has been partially extracted to become a wet ...

Embodiment 3

[0062] Example 3 Heat treatment process

[0063] The dry filament yarn obtained in Example 2 is subjected to heat treatment outside the spinning line, such as figure 2 As shown, the specific process includes: heating a long pipe with an electric furnace, controlling the temperature of the heat pipe wall to 400, 425, 450, 475 ℃, passing the dry yarn through the heat pipe, and absorbing the heat pipe radiant heat to increase the temperature, and the tension is 3, 5. 7 g / denier, the residence time is 7 seconds, the performance of the obtained long yarn after heat treatment is shown in Table 2.

[0064] Table 2 Mechanical properties and fiber properties before and after the warp heat treatment

[0065]

[0066] It can be seen from Table 2 that although the heat-treated fiber has a higher modulus, its strength is slightly lower than that of the original spun fiber.

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Abstract

The invention discloses a high-modulus PPTA fiber which is prepared from PPTA polymers with inherent viscosity of 5.5 to 8.0 dL / g obtained through the method of low-temperature solution polycondensation by drawing undried wet strands in the procedures of washing, neutralizing and drying in the process of dry-jet wet spinning and carrying out heat treatment under high temperature and high tension on dry strands in the procedure of drying or after drying; the modulus of the PPTA fiber is 800 to 1000 g / denier and the inherent viscosity of 5.0 to 7.5 dL / g. The fiber product obtained through the method provided in the invention has excellent yarn strength, high modulus, luster of high crystallinity, a bright color, little fuzziness, superior properties and a wider application scope, and fills in gaps in market.

Description

technical field [0001] The invention relates to the field of man-made fibers, in particular to a polyparaphenylene terephthalamide (PPTA) polymer with a logarithmic viscosity of 5.5-8.0dL / g as a raw material, and in a dry-jet wet spinning process, through A high modulus poly-p-phenylene terephthalamide fiber suitable for industrial scale production obtained by stretching the wet yarn and heat-treating the dry yarn during or after drying and a preparation method thereof. Background technique [0002] Poly(p-phenylene terephthalamide) (PPTA) was synthesized by DuPont of the United States in 1965 by low-temperature solution polycondensation reaction, and then PPTA / H 2 SO 4 The solution has liquid crystal behavior, and the method of dry-jet wet spinning was invented to obtain high-performance poly-p-phenylene terephthalamide fiber (referred to as "aramid fiber II"). The patents of related technologies were published in the United States in the United States from 1970-1985, suc...

Claims

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Application Information

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IPC IPC(8): D01F6/60D01D5/12D01D10/02D01D10/04C08G69/32
Inventor 王凤德王锡璐彭涛杨其武马俊雍
Owner BLUESTAR CHENGDU NEW MATERIALS
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