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A kind of benzoxazolium ion compound and the PBO fiber emulsion sizing agent containing the compound and preparation method thereof

An ionic compound, benzoxazole technology, applied in fiber types, fiber treatment, organic chemistry, etc., can solve the problems of insufficient fiber surface coverage, different chemical structures of PBO fibers, and inconformity with the concept of green chemical development. Achieve the effect of optimizing interface performance and macroscopic performance, improving compatibility and improving interface performance

Active Publication Date: 2021-10-29
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] However, the chemical structure of the above-mentioned sizing agent is very different from that of PBO fiber, resulting in poor compatibility between the two, and it is difficult for the sizing agent to disperse evenly on the surface of the fiber.
Moreover, the content of organic solvent in the sizing agent is as high as 90wt%, and the sizing process not only has the danger of inflammability and explosion, but also causes great pollution to the environment, which does not conform to the development concept of green chemistry
In addition, the nano reinforcement in the sizing agent, such as spherical TiO 2 and cage-shaped POSS cannot achieve effective coverage of the fiber surface

Method used

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  • A kind of benzoxazolium ion compound and the PBO fiber emulsion sizing agent containing the compound and preparation method thereof
  • A kind of benzoxazolium ion compound and the PBO fiber emulsion sizing agent containing the compound and preparation method thereof
  • A kind of benzoxazolium ion compound and the PBO fiber emulsion sizing agent containing the compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0096] (1) 0.1mol of 4,6-diaminoresorcinol dihydrochloride, 0.2mol of 4-aminosalicylic acid and 0.01mol of stannous chloride are added to 480g of polyphosphoric acid (phosphorus pentoxide is 80wt%), N 2 Under protection, the temperature was slowly raised to 120° C., stirred for 1 h, then the temperature was raised to 150° C., and the stirring reaction was continued for 15 h to obtain a wine red transparent solution. The above solution was poured into water for precipitation, suction filtered and the filter cake was washed repeatedly with deionized water until the pH of the filtrate was close to 7.4, and dried to obtain the crude product. The crude product was recrystallized using N,N-dimethylformamide to obtain high-purity benzoxazolediamine IV-ae.

[0097] (2) Dissolve 0.1mol of IV-ae in N-methylpyrrolidone, add 0.1mol of 1,3-propane sultone, N 2 Under protection, raise the temperature of the system to 50°C, stir and react for 12 hours, pour the reactant into acetone to pre...

Embodiment 2

[0105] (1) 0.1mol of 3,3'-dihydroxybenzidine, 0.25mol of p-aminobenzoic acid and 0.03mol of stannous chloride are added in 480g of polyphosphoric acid (phosphorus pentoxide is 85wt%), N 2 Under protection, the temperature was slowly raised to 120° C., stirred for 2 h, then the temperature was raised to 200° C., and the stirring reaction was continued for 5 h to obtain a wine red transparent solution. The above solution was poured into water for precipitation, suction filtered and the filter cake was washed repeatedly with deionized water until the pH of the filtrate was close to 7.4, and dried to obtain the crude product. The crude product was recrystallized using N-methylpyrrolidone to obtain high-purity benzoxazolediamine IV-bd.

[0106] (2) Dissolve 0.1mol of IV-bd in N,N-dimethylacetamide, add 0.4mol of 1,3-propane sultone, N 2 Under protection, raise the temperature of the system to 150°C, stir and react for 3 hours, pour the reactant into acetone to precipitate, filter ...

Embodiment 3

[0112] (1) 0.1mol of 2,2-bis(3-amino-4-hydroxyl phenyl) hexafluoropropane, 0.23mol of p-aminobenzoic acid and 0.02mol of stannous chloride are added to 480g of polyphosphoric acid (penta Phosphorus oxide is 83wt%), N 2 Under protection, the temperature was slowly raised to 120° C., stirred for 1.5 h, then the temperature was raised to 180° C., and the stirring reaction was continued for 10 h to obtain a wine red transparent solution. The above solution was poured into water for precipitation, suction filtered and the filter cake was washed repeatedly with deionized water until the pH of the filtrate was close to 7.4, and dried to obtain the crude product. The crude product was recrystallized using N-methylpyrrolidone to obtain high-purity benzoxazolediamine IV-cd.

[0113] (2) Dissolve 0.1mol of IV-cd in dimethyl sulfoxide, add 0.25mol of 1,3-propane sultone, N 2 Under protection, raise the temperature of the system to 100°C, stir and react for 7 hours, pour the reactant int...

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Abstract

A benzoxazolium ion compound represented by the following formula X, a sizing agent comprising the compound, a preparation method and use thereof. The chemical structure of the benzoxazolium ion compound represented by formula X is similar to that of PBO fiber, which is beneficial to improve the compatibility of sizing agent and PBO fiber, and its preparation process is simple and easy to operate. The sizing agent overcomes the problems of poor compatibility between the existing sizing agent and PBO fibers, the need to use a large amount of flammable and explosive organic solvents in the sizing agent, and the difficulty in effectively covering the fiber surface with nano reinforcements in the sizing agent. The sizing agent uses water as a solvent, is green and efficient, is simple to prepare, and is environmentally friendly, and the sizing agent can not only maintain the original tensile strength of the PBO fiber, but also significantly improve the IFSS of the composite material.

Description

technical field [0001] The invention belongs to the technical field of composite materials, and in particular relates to a benzoxazolium ion compound, a PBO fiber emulsion sizing agent containing the compound and a preparation method thereof. Background technique [0002] PBO (full name polyphenylene benzobisoxazole) is a rigid rod-shaped liquid crystal polymer with a full aromatic heterocycle. The PBO fiber prepared by the dry-jet wet spinning process has ultra-high strength, modulus, heat resistance and resistance. Combustibility, known as "the super fiber of the 21st century", has broad application prospects in cutting-edge fields such as aerospace, national defense and military industry, rail transportation, high-temperature production and new energy. [0003] The molecular structure of PBO fiber is as follows: [0004] [0005] However, the rigid structure makes the surface of PBO fibers very smooth, and the lack of active groups makes the surface chemically inert. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D498/04C07D263/57D06M13/352D06M101/30
CPCC07D263/57C07D498/04D06M13/352D06M2101/30D06M2200/40
Inventor 吴绍华李春成肖耀南张博
Owner INST OF CHEM CHINESE ACAD OF SCI
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