A kind of preparation method of poly[2,5-dihydroxy-1,4-phenylenepyridodiimidazole] polymer

A technology of phenylene pyridine and diimidazole, 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 improving production efficiency

Active Publication Date: 2015-11-25
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

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 poly[2,5-dihydroxy-1,4-phenylenepyridine The preparation method of diimidazole] polymer can reduce the viscosity of the polymerization system, facilitate stirring and transportation, and improve the molecular weight of PIPD polymer

Method used

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  • A kind of preparation method of poly[2,5-dihydroxy-1,4-phenylenepyridodiimidazole] 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 is obtained; the reaction time of the prepolymer in the twin-screw extruder is 10min, The twin-scr...

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. The post-condensation reaction was completed in the machine to obtain poly[2,5-dihydroxy-1,4-phenylenepyridinediimidazole] polymer; the reaction time of the prepolymer in the twin-screw extruder was 60min, The twin-screw ex...

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 poly[2,5-dihydroxy-1,4-phenylenepyridodiimidazole] polymer. The present invention includes two steps of pre-polymerization and post-condensation reaction. The reaction time of the pre-polymer in the twin-screw extruder is 10-60 minutes. Zones are 160-180°C, 180-190°C and 190-200°C respectively. The present invention adopts a twin-screw extruder to carry out post-condensation reaction, and adopts specific temperature and time control parameters, so that the intrinsic viscosity [η]=28-30dL / g of the PIPD polymer produced at the end greatly improves its molecular weight , and at the same time, it is convenient to stir and transfer the PIPD polymer to the spinning section more easily, which improves the production efficiency and reduces the production cost.

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-phenylenepyridodiimidazole] 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 i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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