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Polybenzobisoxazole polymer containing thiophenic sulfur and preparation method thereof

A technology of polybenzoxazole and benzobisoxazole, which is applied in the field of polybenzoxazole polymer containing thiophene sulfur and its preparation, can solve the problems of high production cost of terephthalic acid, achieve high strength, improve Processability, good oxidation resistance effect

Inactive Publication Date: 2010-02-10
DALIAN RES & DESIGN INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Donghua University discloses a polybenzobisoxazole polymer containing hydroxyl groups and a preparation method thereof (see CN1245434C, 2006-03-15), which has disadvantages such as high preparation cost of 2,5-dihydroxyterephthalic acid

Method used

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  • Polybenzobisoxazole polymer containing thiophenic sulfur and preparation method thereof
  • Polybenzobisoxazole polymer containing thiophenic sulfur and preparation method thereof
  • Polybenzobisoxazole polymer containing thiophenic sulfur and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] In a 125mL four-neck flask equipped with a stirring device, a condenser, a drying tube and a thermometer, under the protection of an inert nitrogen gas, 10.653g (0.05mol) DAR, 4.154g (0.025mol) terephthalic acid, 4.304g (0.025mol) thiophenedicarboxylic acid, 8.315g phosphorus pentoxide, 119.093g polyphosphoric acid (the mass fraction is 82% based on phosphorus pentoxide, the same below), stir and heat the reaction materials to 40-50°C for 12 hours During this period, HCl is removed under reduced pressure, and the temperature is raised to 90-100°C for 12 hours until the pH test paper is used to detect neutrality at the gas escape port, which means that the system has completely removed HCl;

[0031] Then add 4.208g of phosphorus pentoxide, raise the temperature to 130°C for 12h, 150°C for 12h, 170°C for 12h, 180°C for 12h and 220°C for 12h to complete the polymerization reaction.

[0032] The reaction solution was refluxed with water and dilute sodium hydroxide solution,...

Embodiment 2

[0035] Raw material and its add-on, solvent adding method and its add-on are the same as embodiment 1. In the initial stage, stir and heat to 50-60°C for 12 hours, during which HCl is removed under reduced pressure, and the temperature is raised to 90-100°C for 12 hours to ensure complete removal of HCl;

[0036] Then add phosphorus pentoxide, raise the temperature to 130°C for 24h, 150°C for 24h, 170°C for 24h, 180°C for 12h and 200°C for 12h to complete the polymerization reaction.

[0037] Adopt same test method, the intrinsic viscosity of gained polymer is 5.6dL / g; Solid 13 C NMR analysis results (ppm): δ=161.67, 148.14, 139.28, 128.29, 111.19, 110.21, 109.19, 94.09.

Embodiment 3

[0039] Raw material and its add-on are with embodiment 1. The way of solvent addition and its addition amount and reaction conditions are as follows: add 29.736g phosphorus pentoxide and 91.36g polyphosphoric acid at the beginning stage, stir and heat to 50-60°C for 12 hours, during which HCl is removed under reduced pressure, and the temperature is gradually raised to React at 80-90°C for 12 hours to ensure complete removal of HCl;

[0040] Then add 14.868g of phosphorus pentoxide, raise the temperature to 130°C for 24h, 150°C for 24h, 170°C for 24h, 180°C for 12h and 200°C for 12h to complete the polymerization reaction.

[0041] Adopt same test method, the intrinsic viscosity of gained polymer is 9.8dL / g; Solid 13 C NMR analysis results (ppm): δ=161.67, 148.15, 139.28, 128.28, 111.19, 110.21, 109.18, 94.09.

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Abstract

The invention provides a polybenzobisoxazole polymer containing thiophenic sulfur and a preparation method thereof. The polymer contains a mixed structure of 2,5-thienylbenzobisoxazole section and 1,4-phenylene benzobisoxazole section which is shown in formula I. The polymer has high strength and rigidity, extremely good oxidation resistance, moisture resistance, ultraviolet resistance and insulation and is especially suitable for the production of films and fibre products.

Description

technical field [0001] The invention relates to a polybenzoxazole polymer, more specifically to a polybenzoxazole polymer containing thiophene sulfur and a preparation method thereof. Background technique [0002] High-performance fibers can be prepared from poly[(1,4)-phenylene 2,6-(1,2-d:5,4-d)-benzobisoxazole] (PBO for short). Based on the research of the U.S. Air Force Materials Laboratory and Dow Chemical Company, Japan Toyobo successfully realized the industrial production of PBO fiber in the 1990s, and its trade name was Zylon. The fiber has high strength, high modulus and excellent heat resistance and flame retardancy [see: Tadao Kuroki, Kazuyuki Yabuki. Basic physical properties and applications of PBO fiber "ザイロソ". High-tech fibers and applications. 1998, 23(5): 37-39.]. However, when the fiber is used to prepare composite materials, there are insufficient compressive strength and torsional modulus, and its axial compressive strength is only 10% to 20% of the ten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/22D01F6/74
Inventor 邵玉昌左洪亮张海涛许汉赵文武
Owner DALIAN RES & DESIGN INST OF CHEM IND
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