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A kind of polyhydroxy-p-phenylene benzobisoxazole polymer and its preparation and application

A technology of hydroxybenzoxazole and benzobisoxazole, which is applied in the field of benzobisoxazole polymers, can solve the problems of thermal performance degradation and low tensile strength of fibers

Active Publication Date: 2017-07-14
宁夏瑞鼎科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] Although the price of M5 has been greatly reduced, even more than 30% lower than the price of PBO, due to its rapid decline in thermal performance, it has dropped to 480°C, and the tensile strength of the fiber is not high.

Method used

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  • A kind of polyhydroxy-p-phenylene benzobisoxazole polymer and its preparation and application
  • A kind of polyhydroxy-p-phenylene benzobisoxazole polymer and its preparation and application
  • A kind of polyhydroxy-p-phenylene benzobisoxazole polymer and its preparation and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Embodiment 1 Preparation of AB type monomer and precursor thereof

[0056] (1) Synthesis of precursor 2-hydroxyl-4-(5-nitro-6-hydroxybenzoxazol-2-yl)benzoic acid (formula V, HNBA)

[0057] Add 5.50g (0.030mol) of hydroxyterephthalic acid and 100mL of diethylene glycol dimethyl ether to the four-port glass reactor in turn, stir well and add 3.6g (0.0303mol) of SOCl 2 , and start heating to carry out the reaction at 75-80°C for more than 1 hour. After the reaction liquid is clear and transparent, cool it to 50°C, and quickly add 6.20g (0.030mol) of 4-amino-6-nitroisophthalic acid to the reactor. Phenol hydrochloride (ANRHCl), heat up to 105°C, add 7.0g85% PPA (polyphosphoric acid) after condensation reaction for 2h, continue to heat up to reflux for ring closure and dehydration reaction for 3h, cool to room temperature, filter, wash, After drying, 8.27 g of crude HNBA as yellow-brown powder was obtained (crude yield 87.17%, purity 89.23%). The resulting crude product is...

Embodiment 2

[0061] Embodiment 2 Poly 3'-hydroxyl-1', 4'-phenylene-2,6-benzobisoxazole (formula I, ord-PBO-II) and fiber preparation

[0062] (AB type monomer polycondensation method)

[0063] Add 3.2g of P successively into the glass polymerization reactor 2 o 5 and 24.0g83%PPA, heated up to 90°C and stirred for 1h until clear and transparent, that is, the formation of 85.0%PPA 2 o 5 PPA, add 4.11g AB type monomer 2-hydroxyl-4-(5-amino-6-hydroxyl benzoxazol-2-yl) benzoic acid (HABA, 0.0143mol) to make a monomer concentration of 18.0% (wt); heat up to 110°C and stir for 1.5h to dissolve, gradually heat up to 125°C for 45min to appear whole-body fluorescence, react at 125°C for 40min and then gradually heat up to 150°C for 1h, showing silk Then the temperature was raised to 160° C. for 20 minutes to complete the polymerization reaction, and the liquid crystal stock solution of the ordered polymer (ord-PBO-II) was obtained. Directly from the liquid crystal stock solution at 120°C, the f...

Embodiment 3

[0064] Example 3 Preparation of key monomer 4,6-diaminoresorcinol hydrochloride (DARHCl)

[0065] Add 41.32g (0.20mol) 4-amino-6-nitroresorcinol hydrochloride (ANR·HCl) and 300g water in the four-hole glass reactor, after stirring and dissolving under the protection of nitrogen, add 80g water dropwise And the dilute alkali solution that 9.17g96%NaOH (0.22mol) is made into, carries out neutralization reaction 10min under the protection of nitrogen, then transfers to acid-resistant autoclave rapidly, and adds 1.0g5%Pd / C catalyst (solid content 50%), After closing the autoclave, successively use N 2 Replace the air 4 times with H 2 replace N 2 After 2 times, control the temperature of 35~45℃, under the hydrogen pressure lower than 1MPa, stir the catalytic hydrogenation for 3h to complete the reaction; 2 After protection and stirring, the filtrate was quickly added to 3.2g SnCl after the catalyst was filtered out. 2 2H 2 In the acidic aqueous solution made of O, 50g36% hydroc...

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Abstract

The present invention discloses a polyhydroxy p-phenylene benzo bisoxazole polymer and preparation and application thereof. The polyhydroxy p-phenylene benzo bisoxazole polymer can be 3'-hydroxy-1', 4 '-phenylene-2, 6-benzo bisoxazole which is shown as formula I and has orderly distributed hydroxyl, or polyhydroxy-1', 4 '-phenylene-2, 6 benzo bisoxazole which is shown as formula II and has hydroxyl in random distribution. The polyhydroxy p-phenylene benzo bisoxazole polymer can be used for the preparation of hydroxyl modified PBO (cis-poly(p-phenylene-2,6-benzo bisoxazole) fiber, and comprises an AB type monomer shown as formula III used and a precursor shown as formula V, which are used for the ordered polymer, and a composite salt monomer shown as formula IV, which is used for the random polymer. The hydroxyl is introduced into the molecular chains of the PBO, can improve the fiber UV resistance performance, and has the advantages of outstanding mechanical properties, good heat resistance, light degradation resistance and flame resistance, good bonding property with a resin matrix, and the like.

Description

technical field [0001] The invention relates to benzobisoxazole polymers, in particular to a class of polyhydroxy-p-phenylene benzobisoxazole polymers and their preparation and application, including AB monomers for polymers and their precursors and compound salt mono bodies, and their preparation. Background technique [0002] PBO is the abbreviation of cis-poly(p-phenylene-2,6-benzobisoxazole), and its fiber is a high-strength, high-modulus, low-density organic fiber with Excellent thermal stability and flame retardant performance. Zylon-HM fiber, its comprehensive performance (5.8GPa tensile strength, 270GPa modulus, 68 limiting oxygen index and 650 ℃ decomposition temperature) has fully exceeded Kevlar-49, so it is used as New materials in the fields of aerospace, national defense and military and their special civil applications have also attracted the attention of research departments and industries. [0003] However, due to the lack of polar groups in the molecular ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/22D01F6/74D01F6/78
CPCC07C51/412C07C213/00C08G73/22D01F6/74D01F6/78C07C65/03C07C215/80
Inventor 金宁人金菁
Owner 宁夏瑞鼎科技有限公司
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