A kind of preparation method of p-phenylene benzobisoxazole-silsesquioxane copolymer

A technology of benzobisoxazole and silsesquioxane, which is applied in the field of chemistry, can solve the problems of reduced mechanical properties of materials, destruction of PBO structure, and difficulty in processing and molding, achieving fewer steps, lower requirements for experimental conditions, and excellent solubility and film-forming effect

Active Publication Date: 2017-01-04
NORTHWESTERN POLYTECHNICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, due to the high rigidity of the molecular ladder structure of PBO, its structure is chemically inert and its bonding performance is poor. Except for strong acidic solvents such as polyphosphoric acid (PPA), all-aromatic PBO can only be diss

Method used

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  • A kind of preparation method of p-phenylene benzobisoxazole-silsesquioxane copolymer
  • A kind of preparation method of p-phenylene benzobisoxazole-silsesquioxane copolymer
  • A kind of preparation method of p-phenylene benzobisoxazole-silsesquioxane copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Synthesis of TBS-DAR:

[0023] Add 2.13g 4,6-diaminoresorcinol dihydrochloride (DAR) and 100mL DMF into an anhydrous and oxygen-free Schlenk bottle with an air inlet and a magnetic stirring bar, and 7.50g tert-butyldimethyl Chlorochlorosilane (TBS) was dissolved in 100 mL of anhydrous DMF to make it completely dissolved. Under rapid stirring, the TBS solution and 27.3 g of the acid-binding agent triethylamine (TEA) were added dropwise into the above-mentioned Schlenk bottle respectively, and a brown-yellow suspension was formed after the addition was complete. Seal the reaction device and stir at room temperature for 12h. After the reaction was terminated, a yellow solid was obtained by suction filtration, washed with deionized water several times, and the obtained solid product was dried in a vacuum oven at 80° C. for 24 hours to prepare TBS-DAR.

[0024] (2) Preparation of acylated POSS:

[0025] Under argon protection, dissolve 5 g of terephthaloyl chloride in...

Embodiment 2

[0033] Note: In this patent, the preparation and heat treatment of TBS-DAR, acylated POSS and PBO-POSS precursor polymer films are consistent with those described in Example 1. In the following examples, only functionalized PBO-POSS precursor polymers are introduced. preparation.

[0034] Preparation of functionalized PBO-POSS precursor polymer 2:

[0035] Under the protection of argon, TBS-DAR (0.597g, 1.0mmol) and 5mL N-methylpyrrolidone (NMP) were added dropwise into the Schlenk tube, and the acylated POSS (0.6125g, 0.5mmol) and terephthaloyl chloride (0.1020 g, 0.5mmol) was dissolved in 5mL NMP and added dropwise to the Schlenk tube. Seal the reaction device and stir at 30°C for 24h. After the reaction, the obtained wine-red liquid was added dropwise to 200mL deionized water to obtain gray-black precipitate, which was washed several times with deionized water, filtered with suction, and dried in a vacuum oven at 80°C for 24 hours to obtain PBO-POSS precursor polymer 2 ....

Embodiment 3

[0037] Preparation of functionalized PBO-POSS precursor polymer 3:

[0038] Under the protection of argon, TBS-DAR (0.597g, 1.0mmol) and 5mL N-methylpyrrolidone (NMP) were added dropwise into the Schlenk tube, and the acylated POSS (0.2450g, 0.2mmol) and terephthaloyl chloride (0.1630 g, 0.8mmol) was dissolved in 5mL NMP and added dropwise to the Schlenk tube. Seal the reaction device and stir at 30°C for 24h. After the reaction, the obtained wine-red liquid was added dropwise to 200mL deionized water to obtain gray-black precipitate, which was washed several times with deionized water, filtered with suction, and dried in a vacuum oven at 80°C for 24 hours to obtain PBO-POSS precursor polymer 3 .

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Abstract

The invention discloses a preparation method of p-phenylenebenzobisoxazole-silsesquioxane copolymer, which utilizes tert-butyldimethylchlorosilane to treat easily oxidized and poorly soluble 4,6-diaminomethylene Active amino groups and hydroxyl groups in quinone dihydrochloride monomers are chemically modified to obtain monomers protected by silane functional groups, increasing their solubility and stability in organic solvents; at the same time, using terephthaloyl chloride and The acylation reaction of the two hydroxyl POSS makes the terminal active hydroxyl group containing the regular cage structure POSS be converted into an acid chloride group; finally, the monomer protected by the silane functional group and the terminal acylated POSS and terephthaloyl chloride are dissolved in an organic solvent The polycondensation reaction is carried out, and the cage structure POSS monomer is chemically bonded to the PBO main chain by chemical methods to obtain a block copolymer. The block copolymer prepared by the invention has good solubility and film-forming property, and has excellent high temperature resistance and mechanical properties.

Description

technical field [0001] The invention belongs to the technical field of chemistry and relates to a preparation method of p-phenylenebenzobisoxazole-silsesquioxane copolymer. Background technique [0002] With the development of aviation technology, higher requirements are put forward for the high temperature resistance and corrosion resistance of materials. Therefore, it is imminent to develop polymer composite materials with good processing performance, light weight, high temperature resistance and corrosion resistance. Poly(p-phenylene benzobisoxazole) (PBO) is known as the super fiber of the 21st century, its main chain contains benzene ring and heterocyclic structure, the molecular chain has a ladder-shaped rigid structure, and the bisoxazole ring and benzene Ring coupling, under the conjugation effect of the large π bond of the benzene ring, the stability of the oxazole ring with low aromaticity has been greatly improved, showing excellent high temperature resistance, fl...

Claims

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Application Information

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IPC IPC(8): C08G73/22
Inventor 孔杰王佩唐玉生
Owner NORTHWESTERN POLYTECHNICAL UNIV
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