A kind of preparation method of polyamideimide precipitated fiber

A technology of polyamide-imide and polyamide-imide stock solution, which is applied in the field of fiber preparation, can solve the problems of difficult removal of catalyst and instability of trimellitic anhydride chloride in water, etc., and achieve easy control of shape and size and rich hairiness , the effect of simple operation

Active Publication Date: 2017-10-24
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the trimellitic anhydride acid chloride used in this method is unstable with water, and a large amount of subsequent catalysts that are difficult to remove will be used in the process of chemical cyclization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Under the protection of nitrogen deoxygenation, add 3L of N-methylpyrrolidone, 35.5g of lithium chloride, 56.7g of 2,6-diaminotoluene, and 105.6g of 4,4'-diaminobenzoanilide into a 5L polymerization kettle After completely dissolving, add 299.5 g of benzophenone tetra-acid dianhydride and react at 0°C for 5-10 hours. Under the protection of nitrogen, 17.76 g of the chemical cyclization catalyst isoquinoline was added dropwise, and then under the condensing and reflux device, the temperature was raised step by step, stirred, and polymerized at 100 ° C for 3 h, 120 ° C for 3 h, and 185 ° C for 3 h, and the solid content was obtained. 13% polyamideimide spinning dope with intrinsic viscosity of 3.2dl / g.

[0024] Dilute the spinning stock solution to 3% and inject it into the sedimentation solution to prepare the precipitation fiber. The injection speed is 5ml / min, the temperature of the precipitation solution is 20-30°C, and 10ml of the polyamide-imide solution is added to...

Embodiment 2

[0026] Under the protection of nitrogen deoxygenation, add 3L of dimethylacetamide, 32.3g of lithium chloride, 51.9g of 2,4-diaminotoluene, and 95.9g of 4,4'-diaminobenzanilide into a 5L polymerization kettle After completely dissolving, add 272.3 g of benzophenone tetra-acid dianhydride and react at 0°C for 5-10 hours. Under the protection of nitrogen, 16.1 g of the chemical cyclization catalyst isoquinoline was added dropwise, and then under the condensing and reflux device, the temperature was raised step by step, stirred, and polymerized at 100 ° C for 3 h, 130 ° C for 3 h, and 150 ° C for 5 h, and the solid content was obtained. 14% polyamideimide spinning dope with intrinsic viscosity of 3.5dl / g.

[0027] Dilute the spinning stock solution to 5% and inject it into the sedimentation solution to prepare the precipitation fiber. The injection speed is 5ml / min, the temperature of the precipitation solution is 20-30°C, and 10ml of the polyamide-imide solution is added to the ...

Embodiment 3

[0029] Under the protection of nitrogen deoxygenation, 3L of dimethylformamide, 32.6g of lithium chloride, 78.4g of 4,4'-diaminodiphenylmethane, 4,4'-diaminobenzoyl For aniline 89.9g, after completely dissolving, add 255.1g of benzophenone tetra-acid dianhydride and react at 0°C for 5-10h. Under the protection of nitrogen, 16.3 g of the chemical cyclization catalyst isoquinoline was added dropwise, and then under the condensing and reflux device, the temperature was raised in stages, stirred, and polymerized at 100 ° C for 3 h, 120 ° C for 3 h, and 150 ° C for 5 h, and the solid content was obtained. 15% polyamideimide spinning dope with intrinsic viscosity of 2.8dl / g.

[0030] Dilute the spinning stock solution to 4% and inject it into the sedimentation solution to prepare the precipitation fiber. The injection speed is 5ml / min, the temperature of the precipitation solution is 20-30°C, and 10ml of the polyamide-imide solution is added to the In the precipitation solution of ...

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Abstract

The invention relates to a preparation method of polyamideimide precipitated fiber, comprising: adding diamine monomer and dianhydride monomer into an aprotic polar solvent under nitrogen deoxidation protection at 0-5°C, adding compound Additives, stirred under the protection of nitrogen, polymerized for 3-10 hours, dropped into the chemical cyclization catalyst, condensed and refluxed, and carried out staged temperature-rising polymerization under stirring to obtain polyamideimide spinning stock solution, filtered, defoamed, diluted, injecting into the stirred precipitation solution with a syringe to obtain polyamideimide precipitation fiber suspension, which is obtained after washing, filtering and drying. The method of the present invention uses diamine and dianhydride as monomers to synthesize the polyamide-imide stock solution in one step, and the cost is low, and the polyamide-imide stock solution is directly obtained by realizing the cyclization reaction in the polymerization stage, the molecular weight is relatively high, and the operation is simple , the obtained fibrids can be directly used in the preparation of high-performance paper while retaining its traditional excellent properties such as thermal properties and radiation resistance.

Description

technical field [0001] The invention belongs to the field of fiber preparation methods, and in particular relates to a preparation method of polyamideimide precipitated fibers. Background technique [0002] Due to its strong mechanical properties, excellent dielectric properties, stable chemical properties and flexible designability, high-performance paper has become a popular choice in the fields of national defense, aviation, aerospace, communications, electronics, chemical industry, environmental protection and marine development. It is widely used in high-strength and lightweight honeycomb structure materials, high-temperature-resistant insulating materials and high-performance electronic communication equipment and other fields. At present, the high-performance papers on the market are mainly made of aromatic polyamide fibers, which are divided into aramid 1313 and aramid 1414 synthetic papers. The main representatives are the meta-aramid paper Nomex and para-aramid pap...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): D01F6/94C08G73/14D21H13/26
Inventor张清华吴婷婷方玉婷谭文军张殿波甘锋赵昕王士华董杰
OwnerDONGHUA UNIV