Direct spinning process for preparing PPTA fibre by end capping resin method

A resin and process technology, applied in the field of chemical and polymer materials, can solve the problems of corrosion of production equipment, damage to the human body, and complicated operation processes, and achieve the effect of improving production efficiency, reducing human damage and environmental pollution

Inactive Publication Date: 2009-07-08
赵海鹏 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because PPTA is insoluble and infusible, it can only be dissolved in strong acids such as concentrated sulfuric acid and hydrofluoric acid. Therefore, the operation process is not only complicated, but also causes serious corrosion of production equipment, and causes human damage and serious environmental damage. Pollution

Method used

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  • Direct spinning process for preparing PPTA fibre by end capping resin method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0009] In a 200L polymerization kettle, inject 80 kilograms of N-methylpyrrolidone (NMP) solutions that are dissolved with 5% lithium chloride (LiCl), and add 3.244 kilograms (30mol) of p-phenylenediamine (PPDA) at 15° C. Make it fully dissolved, make NMP-LiCl-PPDA solution, carry out stirring reaction under normal pressure, keep the reaction temperature at -5°C ~ 5°C, slowly add 6.091 kg (30mol) of terephthaloyl chloride (TPC) After 1 to 5 minutes, 0.23 kg of phenylethylamine was added, and after 1 to 5 minutes of reaction, 0.23 kg of benzoic acid was added to obtain a blocked PPTA oligomer-NMP-LiCl composite solution. At room temperature, add 7L of pyridine and 5.0 kg of p-phenylenediamine powder to the composite solution, and after it is completely dissolved, cool to a certain temperature, then add 9.45 kg of terephthaloyl chloride powder, and react with high-speed stirring for 20 to 25 minutes . The solution spinning temperature was adjusted to 85°C, and PPTA fibers were ...

Embodiment 2

[0011] In a 200L polymerization kettle, inject 7% calcium chloride (CaCl 2 ) of N-methylpyrrolidone (NMP) solution 100 kg, add 3.244 kg (30mol) of p-phenylenediamine (PPDA) at 15°C to fully dissolve it, and make NMP-LiCl-PPDA solution, Stir the reaction under pressure, maintain the reaction temperature at -5°C to 5°C, slowly add 6.091 kg (30mol) of terephthaloyl chloride (TPC), add 0.30 kg of phenethylamine after 1 to 5 minutes, and react 1 to 5 minutes. Minutes later, 0.30 kg of benzoic acid was added to obtain a capped PPTA oligomer-NMP-LiCl composite solution. At room temperature, add 5 L of pyridine and 4.0 kg of p-phenylenediamine powder to the composite solution, after it is completely dissolved, cool to a certain temperature, then add 7.56 kg of terephthaloyl chloride powder, and react with high-speed stirring for 20 to 25 minutes . The solution spinning temperature was adjusted to 85°C, and PPTA fibers were obtained through extrusion-wet spinning-coagulation bath pro...

Embodiment 3

[0013] In a 200L polymerization kettle, inject 100 kg of N-methylpyrrolidone (NMP) solution that is dissolved with 5% lithium chloride (LiCl), add 3.244 kg (30mol) of p-phenylenediamine (PPDA) at 15°C, Make it fully dissolved, make NMP-LiCl-PPDA solution, carry out stirring reaction under normal pressure, keep the reaction temperature at -5°C ~ 5°C, slowly add 6.091 kg (30mol) of terephthaloyl chloride (TPC) After 1 to 5 minutes, 0.45 kg of phenylethylamine was added, and after 1 to 5 minutes of reaction, 0.45 kg of benzoic acid was added to prepare a blocked PPTA oligomer-NMP-LiCl composite solution. At room temperature, add 5 L of pyridine and 5.0 kg of p-phenylenediamine powder into the composite solution, and after it is completely dissolved, cool to a certain temperature, then add 9.45 kg of terephthaloyl chloride powder, and react with high-speed stirring for 20 to 25 minutes . The solution spinning temperature was adjusted to 85°C, and PPTA fibers were obtained through...

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Abstract

The invention provides a direct spinning technique for preparing polyphenylene terephthalamide by using end capping oligomer. The method includes steps as follows: firstly, polyesterification of phthaloyl chloride and phenylene diamine for obtaining PPTA oligomer with low molecular weight, passivating two ends of molecule using end-capping reagent for forming end capping PPTA resin; secondly, adding polar solvent and latent solvent into the resin for confecting a composite solution; finally, processing solution polyesterification in the composite solution for obtaining PPTA polymer with high molecular weight, and processing stock solution spinning preparing PPTA fibre. The method makes PPTA polymer giant molecule dissolving into the composite solution associated with polar solvent and latent solvent by using reaction inertia and solvent effect of end capping PPTA resin that is convenient for spinning. The method breaches technique difficult problem that the prior liquid crystal spinning technique for preparing aramid fiber with high quality must need concentrated sulfuric acid as solvent, avoid usage of concentrated sulfuric acid with causticity and is hoping to become an universality direct spinning technique with high effect and low cost, green and environmental protective.

Description

technical field [0001] The invention belongs to the technical field of chemical industry and polymer materials, and relates to the synthesis of polymers and direct spinning technology. Specifically, it utilizes the reaction inertness and solvent effect of end-capped PPTA resin, and uses it under the cooperation of polar solvents and co-solvents. The PPTA polymer macromolecules can be dissolved in it, and the dope is directly spun to realize it. Background technique [0002] Para-aramid is one of the three major high-performance fibers today, and its chemical name is Poly(para-Phenylene Terephthalamide), PPTA. It is indispensable in national economic construction and national defense construction. Missing new material. Its most outstanding properties are its high strength, high modulus, and excellent heat resistance. Its tensile strength is 6 times that of steel wire, 3 times that of glass fiber, and 2 times that of high-strength nylon industrial yarn; its tensile modulus i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D01F6/60C08G69/42D01D1/02
Inventor 赵海鹏雷佑安张秀欣苗东利
Owner 赵海鹏
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