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Benzoxazole ionic compound, PBO fiber emulsion sizing agent containing benzoxazole ionic compound and preparation method of PBO fiber emulsion sizing agent

An ionic compound, benzoxazole technology, applied in fiber treatment, fiber type, organic chemistry, etc., can solve problems such as insufficient fiber surface coverage, environmental pollution, and non-compliance with the development concept of green chemistry.

Active Publication Date: 2020-10-27
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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  • Benzoxazole ionic compound, PBO fiber emulsion sizing agent containing benzoxazole ionic compound and preparation method of PBO fiber emulsion sizing agent
  • Benzoxazole ionic compound, PBO fiber emulsion sizing agent containing benzoxazole ionic compound and preparation method of PBO fiber emulsion sizing agent
  • Benzoxazole ionic compound, PBO fiber emulsion sizing agent containing benzoxazole ionic compound and preparation method of PBO fiber emulsion sizing agent

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

The invention discloses a benzoxazole ionic compound shown as a formula X, a sizing agent containing the compound, and a preparation method and application of the sizing agent. The benzoxazole ionic compound shown in the formula X is similar to the PBO fiber in chemical structure, the compatibility of the sizing agent and the PBO fiber can be improved, and the preparation process is simple and easy to operate. According to the sizing agent, the problems that an existing sizing agent is poor in compatibility with the PBO fiber, a large number of flammable and combustible organic solvents need to be used in the sizing agent, and nano reinforcements in the sizing agent are difficult to effectively cover the surfaces of the fibers are solved. The sizing agent takes water as a solvent, is greenand efficient, is simple and environment-friendly to prepare, and not only can keep the original tensile strength of PBO fibers, but also can remarkably 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 Applications(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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