Preparation method of poly[2, 5-dyhydroxy-1, 4-phenylene pyridine diimidazole] polymer

A technology of phenylenepyridine and dihydroxy, which is applied in the field of PIPD polymer preparation, can solve the problems of difficulty in stirring and conveying, low polymer molecular weight, etc., and achieve the effects of increasing molecular weight, reducing production cost, and facilitating stirring

Active Publication Date: 2014-02-26
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] The present invention aims to solve the problems in the prior art that stirring and transportation are difficult due to the high viscosity of the PIPD polymerization system, and the molecular weight of the polymer is not high, and provides a polymer

Method used

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  • Preparation method of poly[2, 5-dyhydroxy-1, 4-phenylene pyridine diimidazole] polymer
  • Preparation method of poly[2, 5-dyhydroxy-1, 4-phenylene pyridine diimidazole] polymer

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Embodiment 1

[0037] A kind of preparation method of poly[2,5-dihydroxyl-1,4-phenylene pyridodiimidazole] polymer, comprises the following processing steps:

[0038] A. Prepolymerization

[0039] Put 2,5-dihydroxyterephthalic acid (DHTA), tetraaminopyridine trihydrochloride monohydrate (TAP) and polyphosphoric acid (PPA) together into the polymerization kettle, mix well and remove hydrogen chloride gas, Carry out prepolymerization reaction then, obtain prepolymer;

[0040] B. After polycondensation

[0041] The discharge port of the polymerization kettle in step A is connected with the feed port of the twin-screw extruder, and the prepolymer is pressed into the described twin-screw extruder using dry nitrogen, and the prepolymer is extruded in the twin-screw extruder. After completing the post-condensation reaction in the machine, poly[2,5-dihydroxy-1,4-phenylenepyridinediimidazole] polymer was obtained; the reaction time of the prepolymer in the twin-screw extruder was 10min, The twin-s...

Embodiment 2

[0043] A kind of preparation method of poly[2,5-dihydroxyl-1,4-phenylene pyridodiimidazole] polymer, comprises the following processing steps:

[0044] A. Prepolymerization

[0045] Put 2,5-dihydroxyterephthalic acid (DHTA), tetraaminopyridine trihydrochloride monohydrate (TAP) and polyphosphoric acid (PPA) together into the polymerization kettle, mix well and remove hydrogen chloride gas, Carry out prepolymerization reaction then, obtain prepolymer;

[0046] B. After polycondensation

[0047] The discharge port of the polymerization kettle in step A is connected with the feed port of the twin-screw extruder, and the prepolymer is pressed into the described twin-screw extruder using dry nitrogen, and the prepolymer is extruded in the twin-screw extruder. After finishing the polycondensation reaction in the machine, a poly[2,5-dihydroxy-1,4-phenylenepyridinediimidazole] polymer was obtained; the reaction time of the prepolymer in the twin-screw extruder was 60min, The twin-s...

Embodiment 3

[0049] A kind of preparation method of poly[2,5-dihydroxyl-1,4-phenylene pyridodiimidazole] polymer, comprises the following processing steps:

[0050] A. Prepolymerization

[0051] Put 2,5-dihydroxyterephthalic acid (DHTA), tetraaminopyridine trihydrochloride monohydrate (TAP) and polyphosphoric acid (PPA) together into the polymerization kettle, mix well and remove hydrogen chloride gas, Carry out prepolymerization reaction then, obtain prepolymer;

[0052] B. After polycondensation

[0053] The discharge port of the polymerization kettle in step A is connected with the feed port of the twin-screw extruder, and the prepolymer is pressed into the described twin-screw extruder using dry nitrogen, and the prepolymer is extruded in the twin-screw extruder. After completing the post-condensation reaction in the machine, poly[2,5-dihydroxy-1,4-phenylenepyridinediimidazole] polymer was obtained; the reaction time of the prepolymer in the twin-screw extruder was 35min, The twin-s...

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Abstract

The invention relates to a preparation method of a poly[2, 5-dyhydroxy-1, 4-phenylene pyridine diimidazole] polymer. The preparation method comprises two steps of prepolymerization reaction and post-polycondensation reaction. The reaction time of a prepolymer in a double-screw extruder is 10-60 minutes, and the double-screw extruder is provided with three temperature zones according to a sequence from a feeding port to a discharging port, wherein the temperatures of the tree temperature zones are respectively 160-180 DEG C, 180-190 DEG C and 190-200 DEG C. According to the preparation method, the double-screw extruder is used for carrying out the post-polycondensation reaction, and specific temperature and time are used for controlling parameters, so that the intrinsic viscosity [eta] of the PIPD polymer obtained in the end is 28-30dL/g, the molecular weight of the polymer is greatly increased, meanwhile, the stirring is facilitated, and the PIPD polymer can be easily conveyed and transferred to a spinning working section, thus the production efficiency is improved, and the production cost is reduced.

Description

technical field [0001] The present invention relates to a kind of method for preparing the polymer of fiber, more specifically the present invention relates to a kind of preparation method of poly[2,5-dihydroxy-1,4-phenylene pyridodiimidazole] polymer, The invention belongs to the technical field of PIPD polymer preparation. Background technique [0002] Poly[2,5-dihydroxy-1,4-phenylene pyridodiimidazole] is a liquid crystal heterocyclic rigid rod polymer. The PIPD fiber (also known as M5 fiber) prepared from this polymer has a tensile strength of The elastic modulus is 5.3GPa and 330GPa respectively, comparable to PBO fiber known as the "King of Organic Fibers". In particular, the special hydrogen bond network structure in the PIPD polymer makes the axial compressive strength of the prepared fiber as high as 1.7GPa, which is 5.7 times that of PBO fiber and comparable to carbon fiber. In addition, PIPD fiber also has excellent heat resistance, flame retardancy, electrical ...

Claims

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Application Information

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IPC IPC(8): C08G73/06D01F6/74B29C47/38B29C47/60B29C47/92B29C48/625B29C48/395B29C48/40B29C48/875B29C48/92
CPCB29C48/875B29C48/92B29C2948/92704B29C48/625B29C2948/92895B29C48/40
Inventor 赵亮严家策付兴伟范新年许伟黄治川
Owner CHINA BLUESTAR CHENGRAND CO LTD
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