Preparation method of polyphenylene terephthalamide copolymer adopting dimethylacetamide direct spinning

A manufacturing method and copolymer technology, applied in the direction of single-component copolyamide artificial filament, etc., can solve the problems of high price, insoluble, low solubility, etc., and achieve the effect of simplifying the production process

Inactive Publication Date: 2011-05-25
CHANGCHUN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the price of 3,4'-diaminodiphenyl ether is extremely expensive, and it is basically not sold in China, so it is not conducive to large-scale industrial production in China
[0005] Chinese patent CN1793199A adopts 2,4-bis(4-aminophenyl)-2,3-naphthyridine-1-one as the third monomer to prepare PPTA copolymer which can be dissolved in NMP and DMAC for dope spinning , but the third monomer production process required by this method is complicated, which greatly increases the production cost and is not conducive to large-scale industrial production
Simple introduction of the third monomer 4,4'-diaminodiphenyl ether, although a flexible group ether bond is introduced, 4,4'-diaminodiphenyl ether is still a linear structure, so it is more difficult in terms of solubility. Slightly lower than the copolymer with 3,4'-diaminodiphenyl ether as the third monomer, which cannot be well dissolved in DMAC

Method used

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  • Preparation method of polyphenylene terephthalamide copolymer adopting dimethylacetamide direct spinning

Examples

Experimental program
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Effect test

Embodiment 1

[0023] Into a 250 mL four-necked reaction flask equipped with a stirrer, dry nitrogen was passed through, and 50 mL of N,N-dimethylacetamide solution containing 2% by mass fraction of anhydrous lithium chloride was added. Add 1.50g of 4,4'-diaminodiphenyl ether and 1.42g of isophthaloyl chloride while stirring, keep the reaction system at -10-15°C, and generate inherent logarithmic viscosity after 5-15 minutes of reaction It is 0.7dL / g prepolymer. Add 0.81 g of p-phenylenediamine powder, and after it is completely dissolved, add 1.69 g of terephthaloyl chloride, and continue the reaction for 30 to 120 minutes. At this time, 0.84g CaO was added, and the reaction was continued for 2 hours in a water bath at 20-80°C to obtain a transparent, uniform and thick polymer slurry. After adjusting the polymer concentration, the stock solution could be spun in DMAC, and the PPTA copolymer was measured. The inherent viscosity is 3.6dL / g.

Embodiment 2

[0025] Into a 250 mL four-necked reaction flask equipped with a stirrer, dry nitrogen was passed through, and 50 mL of N,N-dimethylacetamide solution containing 2% by mass fraction of anhydrous lithium chloride was added. Add 1.20g of 4,4'-diaminodiphenyl ether and 1.01g of isophthaloyl chloride while stirring, keep the reaction system at -10-15°C, and generate inherent logarithmic viscosity after 5-15 minutes of reaction It is 0.6dL / g prepolymer. Add 0.97 g of p-phenylenediamine powder, and after it is completely dissolved, add 2.03 g of terephthaloyl chloride, and continue the reaction for 30 to 120 minutes. At this point add 1.09g Ca(OH) 2 , and use a water bath at 20-80°C to continue the reaction for 2 hours to obtain a transparent, uniform and thick polymerization slurry. Adjust the polymer concentration to carry out stock solution spinning in DMAC. The logarithmic viscosity of the PPTA copolymer is measured as 3.8dL / g.

Embodiment 3

[0027]In a 2L four-port reaction kettle equipped with a stirrer, dry nitrogen gas was blown in, and 400 mL of N,N-dimethylacetamide solution containing 2% by mass fraction of anhydrous lithium chloride was added. While stirring, 12.0 g of 4,4'-diaminodiphenyl ether and 11.16 g of isophthaloyl chloride were introduced, and the reaction system was kept at -10 to 15°C. After 5 to 15 minutes of reaction, an inherent logarithmic viscosity was formed. It is 0.5dL / g prepolymer. Add 6.48g of p-phenylenediamine powder, and after it is completely dissolved, add 13.72g of terephthaloyl chloride, and continue the reaction for 30-120 minutes. At this point, 6.72g of CaO was added, and the reaction was continued for 2 hours in a water bath at 20-80°C to obtain a transparent, uniform and thick polymerization slurry. After adjusting the polymer concentration, the stock solution could be spun in DMAC, and the ratio of PPTA copolymer was measured. Concentrated logarithmic viscosity is 3.5dL / g....

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Abstract

The invention discloses a preparation method of polyphenylene terephthalamide (PPTA) copolymer adopting dimethylacetamide (DMAC) direct spinning. The method comprises the following steps: 4,4'-diaminodiphenylsulfide or 4,4'-diaminodiphenyl ether is used as third monomer, m-phthaloyl chloride is introduced as fourth monomer to perform copolymerization with p-phthaloyl chloride and p-phenylenediamine in a solvent system and prepare uniform, transparent and thick PPTA copolymer size, and the concentration of the polymer is adjusted to perform dope spinning. The method of the invention effectively avoids of adopting the complicated production equipment to perform the polymerization of PPTA; cheap 4,4'-diaminodiphenylsulfide or 4,4'-diaminodiphenyl ether is used as the third monomer and the fourth monomer with a meta-structure is introduced to prepare the PPTA copolymer which can be directly dissolved in DMAC, thus avoiding of using concentrated sulfuric acid as spinning solvent; and the spinning solvent is consistent to the polymerization solvent, the concentration of the polymer is adjusted to perform dope spinning with DMAC and the production process can be greatly simplified.

Description

technical field [0001] The invention belongs to the field of chemical industry and macromolecule chemistry, relates to the polymerization reaction of macromolecules, in particular to a method for manufacturing a PPTA copolymer directly spun by DMAC technical background [0002] Para-aramid, namely Poly(para-Phenylene Terephthalamide), referred to as PPTA, is called aramid 1414 in my country. PPTA is a typical -AA-BB-type polymer. There are intermolecular hydrogen bonds between the amide bonds and a conjugated structure with the benzene ring. The internal rotation potential energy is quite high. It is characterized by regular arrangement of chain unit units and molecular crystallization. And the degree of orientation is extremely high, so the PPTA macromolecular chain is a coaxial or parallel rigid rod-like extended structure. Because of its special molecular structure, PPTA has the characteristics of high modulus, high strength, high heat resistance, etc., so para-aramid is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G69/32D01F6/80
Inventor 敖玉辉陈刚耿杰李连贵张会轩
Owner CHANGCHUN UNIV OF TECH
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