Preparation method of polyimide fibers

A technology of polyimide fiber and polyimide, which is applied in the fiber field to achieve excellent flame retardancy, inhibit combustion chain reaction, and high carbon formation rate

Active Publication Date: 2015-02-18
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Although, compared with other types of fibers, the flame retardancy of polyimide fibers is better, but the limiting oxygen index of polyimide fibers currently prepared is only about 35

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0023] The embodiment of the present invention discloses a kind of preparation method of polyimide fiber, comprises the following steps:

[0024] A) Dianhydride and diamine are polymerized in an aprotic polar solvent to obtain a polyamic acid spinning solution; the diamine includes bis(p-aminophenyl) phenylphosphonate and 3,3'-diamine One or two of triphenoxyphos;

[0025] B) extruding the polyamic acid spinning solution described in step A) through the spinneret holes, and entering the coagulation bath through the air layer to solidify, so as to obtain polyamic acid fibers;

[0026] C) subjecting the polyamic acid fiber described in step B) to thermal imidization treatment to obtain polyimide primary fiber;

[0027] D) performing hot drawing treatment on the polyimide as-spun fibers described in step C), to obtain polyimide fibers.

[0028] The present invention uses diamines and dianhydrides as raw materials, and the diamines include one or both of phenylphosphonic acid bi...

Embodiment 1

[0040] In a nitrogen atmosphere, 18.4866g (0.06mol) of 3,3'-diaminotriphenoxyphosphine and 108.1296g (0.54mol) of 4,4'-diaminodiphenyl ether were dissolved in 1600mL N , in N-dimethylacetamide, after the dissolution is complete, add 91.6104g (0.42mol) of pyromellitic dianhydride and 52.9578g (0.18mol) of 3,3′,4,4′-biphenyltetracarboxylic acid di Anhydride, after reacting for 8 hours, filter to obtain the polyamic acid spinning solution, the mass concentration of the polyamic acid spinning solution is 14.49%.

[0041] After the polyamic acid spinning solution is filtered, vacuum defoamed, extruded from the spinneret, it enters the coagulation bath composed of N,N-dimethylacetamide and water with a volume ratio of 7:18 through the air layer. Coagulate in medium, and then get polyamic acid fiber after washing and drying. The spinneret of the spinneret is 34 holes, the hole diameter is Φ0.16mm, the air layer height is 15mm, and the spray ratio is 2.1 times.

[0042] The obtained...

Embodiment 2

[0046] In a nitrogen atmosphere, dissolve 6.1256g (0.018mol) of phenylphosphonic acid bis(p-aminophenyl) ester and 62.9375g (0.582mol) of p-phenylenediamine in 500mL of N-methylpyrrolidone under stirring conditions, and wait to dissolve After completion, add 52.9578g (0.60mol) of 3,3',4,4'-biphenyltetracarboxylic dianhydride, react for 8 hours, and filter to obtain the polyamic acid spinning solution, the polyamic acid spinning solution The mass concentration is 19.62%.

[0047] After the polyamic acid spinning solution is filtered and vacuum degassed, it is extruded from the spinneret and then enters the coagulation bath composed of N-methylpyrrolidone and water with a volume ratio of 3:17 through the air layer to solidify, and then Polyamic acid fibers are obtained after washing and drying. The spinneret of the spinneret is 50 holes, the hole diameter is Φ0.08mm, the air layer height is 27mm, and the spray ratio is 3 times.

[0048] The obtained polyamic acid fibers were i...

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Abstract

The invention provides a preparation method of polyimide fibers. The method includes performing polymerization reaction to dianhydride and diamine in an aprotic polar solvent to obtain a polyamide acid spinning solution. The diamine comprises one or two of phenyl phosphonic acid (p-aminobenzene) diester and 3, 3'-diamine triphenylphosphine oxide; the polyamide acid spinning solution is squeezed out through a spinneret orifice and enters a coagulating bath to be coagulated to obtain polyamide acid fibers; the polyamide acid fibers are subjected to thermal amination process to obtain polyimide primary fibers; and the polyimide primary fibers are subjected to thermal draft process to obtain polyimide fibers. Phosphorus is contained in the molecular structure of the obtained polyimide fibers, so that not only the char yield of the polyamide fibers is high at a high temperature, but also the polyamide fibers can generate volatile phosphorus compounds to inhibit combustion chain mode reaction in a gas phase and have a superior flame retardant property. Experimental results show that the limit oxygen index of the polyamide fibers is 42 to 50.

Description

technical field [0001] The invention relates to the field of fibers, in particular to a preparation method of polyimide fibers. Background technique [0002] Fiber is a thin and long material with high elastic modulus, small plastic deformation and high strength. Fiber can be divided into natural fiber and chemical fiber, and chemical fiber can be divided into recycled fiber, synthetic fiber and inorganic fiber. Synthetic fiber is a linear organic polymer compound synthesized by addition polymerization or polycondensation reaction using small molecular organic compounds as raw materials. [0003] Polyimide is a class of polymers containing imide rings in the main chain, among which polymers containing phthalimide structures are the most important. Polyimide has outstanding characteristics in terms of performance and synthesis, and has broad application prospects whether it is used as a structural material or a functional material. At present, it is mainly used in aerospace...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): D01F6/78C08G73/10
Inventor 丁祥马晓野邱雪鹏高连勋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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