Polyimide carbon fiber sizing agent and method for producing the same

A polyimide carbon fiber, setting agent technology, applied in the direction of carbon fiber, fiber processing, textiles and papermaking, etc., can solve the molecular structure preparation method of ES-T321 setting agent Unpublished, no published reports, molecular structure or preparation method No public reports, etc.

Inactive Publication Date: 2009-07-22
DONGHUA UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the molecular structure of ES-T321 styling agent and its preparation method have not yet been disclosed
[0007] At present, although the application of the sizing agent for carbon fiber preform

Method used

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  • Polyimide carbon fiber sizing agent and method for producing the same
  • Polyimide carbon fiber sizing agent and method for producing the same
  • Polyimide carbon fiber sizing agent and method for producing the same

Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0059] Example 1

[0060] Put 54.8 g (0.1 mol) of 2,2-bis[4-(2,4-diaminophenoxy)phenyl]hexafluoropropane and 5520 ml of N,N-dimethylacetamide into the reactor After stirring and dissolving completely, cool to 0℃ in an ice-water bath, add 19.6g (0.2mol) of maleic anhydride, stir in the temperature range of 0℃-20℃, after complete dissolution, maintain the reaction for 0.5 hours, add 568.5g (1.0 mol) of 2,2-bis[3-amino-4-(4-cyanophenoxy)phenyl]hexafluoropropane, 518.5 g (1.0 mol) of 2,2-bis[4-(4 -Aminophenoxy)phenyl]hexafluoropropane, stir and dissolve completely, cool to 0°C in an ice-water bath, and add 676.2g (2.1mol) of 3,3',4,4'-tetracarboxylic acid benzophenone The dianhydride, stir in the temperature range of 0℃-20℃, after completely dissolved, maintain the reaction for 2 hours, add 552ml of toluene and 18.8g (0.11mol) of p-toluenesulfonic acid, heat to increase, reflux and separate water for reaction After 5 hours, the toluene was separated (recovered and reused) to obtain a ...

Example Embodiment

[0065] Example 2

[0066] 44.1 g (0.1 mol) of 2,2-bis[4-(2,4-diaminophenoxy)phenyl]propane, 1000 ml of N-methyl-2-pyrrolidone and 5979 ml of N,N-bis Put the methylformamide in the reaction kettle, stir and dissolve completely, cool to 0℃ in an ice-water bath, add 32.8 grams (0.2 mole) of Nadic anhydride, stir in the temperature range of 0℃-20℃, and dissolve completely , Maintain the reaction for 2 hours, add 56.8 g (0.1 mole) of 2,2-bis[3-amino-4-(4-cyanophenoxy)phenyl] hexafluoropropane, 200.2 g (0.5 mole) of 4 , 4′-bis(4-aminophenoxy)diphenyl sulfide, stir and dissolve completely, cool to 0℃ in an ice-water bath, and add 364.0 g (0.7 mol) of 2,2-bis[4-(3, 4-Dicarboxyphenoxy)phenyl]propane dianhydride, stir in the temperature range of 0℃-20℃, after complete dissolution, maintain the reaction for 4 hours, add 5979ml toluene, 1000ml xylene and 119.7g ( 0.7 mol) p-toluenesulfonic acid, heated and heated, refluxed and separated water to react for 12 hours, separated toluene and xylen...

Example Embodiment

[0071] Example 3

[0072] Put 322.0 g (1.0 mol) of 1,3-bis(2,4-diaminophenoxy)benzene and 5000 ml of N,N-dimethylacetamide into the reaction kettle, stir, and when completely dissolved, ice Cool to 0℃ in a water bath, add 19.6g (0.2mol) of maleic anhydride, stir in the temperature range of 0℃-20℃, after complete dissolution, maintain the reaction for 1.5 hours, add 56.8g (0.1mol) of 2, 2 -Bis[3-amino-4-(4-cyanophenoxy)phenyl]hexafluoropropane, 65.4 g (0.1 mole) of 2,2-bis[4-(2-trifluoromethyl-4- Aminophenoxy)phenyl]hexafluoropropane, stir and completely dissolve, cool to 0°C in an ice-water bath, and add 372.0 g (1.2 moles) of 3,3',4,4'-tetracarboxylic acid diphenyl ether dianhydride , Stir in the temperature range of 0℃-20℃, after complete dissolution, maintain the reaction for 3 hours, add 800ml of toluene and 18.8g (0.11mol) p-toluenesulfonic acid, heat and increase, reflux and separate water for 8 hours After that, toluene was separated (recovered and reused) to obtain a homog...

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Abstract

The invention relates to a polyimide carbon fiber tackifier with the molecular general formula shown at the right part. The preparation method of the tackifier comprises the steps as follows: quaternary primary aromatic amines and single anhydride are dissolved in strong-polarity aprotic organic solvent by the molar ratio of 1:2, mixed for reaction for 0.5-2 hours at the temperature of 0-20 DEG C; subsequently, binary primary aromatic amines and 2, 2-bi (3-amido-4-(4-cyano phenoxy) phenyl) Hexafluoropropane are added, mixed, dissolved and cooled by icy water bath; subsequently, binary aromatic anhydride is added and mixed for reaction for 2-4 hours at the temperature of 0-20 DEG C; subsequently, acidic catalyst and entrainer are added; after the heating refluxing water-diversion reaction for 5-12 hours, the entrainer is collected for recovery and reusing and transparent and sticky polyimide solution with uniform phase is obtained; the polyimide carbon fiber tackifier has excellent dimension stability, mechanic property and heat resistance; furthermore, the reaction condition of the preparation method is moderate, the reaction raw material has convenient source and low cost and is friendly to the environment.

Description

technical field [0001] The invention belongs to the field of carbon fiber sizing agent and its preparation, in particular to a polyimide carbon fiber sizing agent and its preparation method. Background technique [0002] Polyimide is a kind of polymer with excellent comprehensive performance, which has excellent heat resistance, low temperature resistance, solvent resistance, self-lubricating property and flame retardancy. At the same time, it also has very good mechanical properties and Dielectric properties. Therefore, it is widely used in photovoltaic materials, nonlinear optical materials; high temperature resistant materials for spacecraft, satellites or space vehicles; advanced structural composite materials in aerospace, automobiles, electromechanical, etc.; Insulating materials, high temperature resistant adhesives, etc.; and FPC or PCB substrate materials in the field of electronic microelectronics, IC interlayer insulating materials, VLSI passivation coatings and ...

Claims

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Application Information

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IPC IPC(8): D06M15/59C08G73/10D06M101/40
Inventor 虞鑫海陈梅芳
Owner DONGHUA UNIV
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