Hydrophobic organic polysilazane as well as preparation method and application thereof

A polysilazane and organic technology, applied in the field of hydrophobic organopolysilazane and its preparation, can solve the problems of hydrophobic failure, difficult batch operation, cumbersome operation, etc., and achieve simple production process, improved hydrophobicity, and low cost Effect

Active Publication Date: 2022-07-29
718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the coating solves the problem of hydrophobic failure caused by the shedding of the hydrophobic coating prepared by the surface modification method to a certain extent, the hydrophobic coating contains a silane coupling agent containing hydrophobic units to treat the inorganic nanomaterials hydrophobically. The process is complicated, the treatment effect is not uniform, and the coating material needs to be used in multi-component compounding or multiple overcoating, and the operation of multiple alternate deposition on the surface of the substrate and heat treatment to form a film is more cumbersome; it is difficult to be used in industrialized batch operation

Method used

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  • Hydrophobic organic polysilazane as well as preparation method and application thereof
  • Hydrophobic organic polysilazane as well as preparation method and application thereof
  • Hydrophobic organic polysilazane as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] A preparation method of hydrophobic organopolysilazane, the specific steps of the method are as follows:

[0053] (1) carry out dehydration treatment with pentane, hexane and pyridine, make its water content no more than 5ppm, with 99.9% argon purging 1000mL three-necked round-bottomed flask 30min, ensure that the reaction vessel is anhydrous and oxygen-free;

[0054] (2) 200mL of solvent and 0.2mL of pyridine after dehydration treatment in step (1) were added to a 1000mL three-necked round-bottomed flask, wherein the volume ratio of pentane and hexane was 1:2, and then 60mL of perfluorooctylmethyl dichloride was added. Silane and 40 mL of methyldichlorosilane, the volume ratio of perfluorooctylmethyldichlorosilane to methyldichlorosilane is 6:4, and the volume of the catalyst is 0.2% of the sum of the volume of fluorochlorosilane and chlorosilane, After mixing uniformly, the ammonia gas with a purity of 99.999% was introduced for the reaction, stirred at -10°C for 8 ho...

Embodiment 2

[0059] A preparation method of hydrophobic organopolysilazane, the specific steps of the method are as follows:

[0060] (1) dehydration of methylcyclopentane, methylcyclohexane and pyridine so that the water content is no more than 5ppm, purging a 1000mL three-necked round-bottomed flask for 30min with argon with a purity of 99.9% to ensure that the reaction vessel has no water without oxygen;

[0061] (2) Into a 1000mL three-necked round-bottomed flask, add 500mL of the solvent and 0.3mL of pyridine after dehydration in step (1), wherein the volume ratio of methylcyclopentane to methylcyclohexane is 3:1, and then add 2.5mL Perfluorohexyltrichlorosilane and 47.5mL methyltrichlorosilane, perfluorohexyltrichlorosilane:methyltrichlorosilane=5:95, the catalyst volume is 0.6% of the sum of the volume of fluorochlorosilane and chlorosilane, After mixing evenly, introduce ammonia gas with a purity of 99.999% for the reaction, stir at -10°C for 10 hours, add 100 mL of the solvent af...

Embodiment 3

[0066] A preparation method of hydrophobic organopolysilazane, the specific steps of the method are as follows:

[0067] (1) toluene and pyridine are dehydrated so that their water content is no more than 5ppm, and a 1000mL three-necked round-bottomed flask is purged for 30min with a purity of 99.9% argon to ensure that the reaction vessel is anhydrous and oxygen-free;

[0068] (2) Into a 1000mL three-necked round bottom flask, add 400mL of toluene solvent and 0.2mL of pyridine after dehydration in step (1), then add 7mL of perfluorohexyltrichlorosilane, 7mL of perfluorodecylmethyldichlorosilane, 56mL of The volume ratio of ethyldichlorosilane, perfluorohexyltrichlorosilane:perfluorodecylmethyldichlorosilane:ethyldichlorosilane is 1:1:8, and the volume of the catalyst is the volume of chlorofluorosilane and chlorosilane. 0.25% of the total and 0.25%, after mixing evenly, introduce ammonia gas with a purity of 99.999% for reaction, stir at -10 °C for 9 h, add 100 mL of the solv...

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PUM

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Abstract

The invention relates to hydrophobic organic polysilazane as well as a preparation method and application thereof, and belongs to the technical field of organic polysilazane preparation. According to the method, fluorochlorosilane with fluorine-containing branched chains and chlorosilane are selected as reaction raw materials, hydrophobic organic polysilazane is synthesized through polycondensation by a one-step method according to the principle of chlorosilane ammonolysis polycondensation, and by means of molecular structure design, the Si-N bond structure of the main chain of a polysilazane molecule is reserved, so that the excellent performance of the polysilazane material is reserved; the fluorine-containing branched chain of the fluorochlorosilane is increased along with the increase of the Si-N main chain in the polycondensation process by controlling parameters such as temperature and reaction time, the branched chain is changed into a hydrophobic group, the hydrophobicity is improved, and the average hydrophobic angle of the polysilazane can reach 114 degrees or above. The polysilazane is colorless transparent liquid and can be self-cured to form a film at room temperature, complex processes such as compounding of various solutions, repeated coating or heat treatment and the like when the coating needs to be used are avoided, the using method is simplified, and the coating is uniform, transparent and high in light transmittance.

Description

technical field [0001] The invention relates to a hydrophobic organopolysilazane, a preparation method and application thereof, and belongs to the technical field of organopolysilazane preparation. Background technique [0002] Polysilazane is mainly divided into two categories, organopolysilazane (PSZ) and perhydropolysilazane (PHPS). Organopolysilazane refers to a polymer in which the main chain is composed of Si-N bonds, and some or all of the side chains R1 to R4 are methyl, propyl, phenyl and other organic groups. The general structural formula is as follows: [0003] [0004] Depending on the characteristics of its side chains, polysilazane has many different properties and can be used in a variety of applications. The research on using polysilazane as a hydrophobic material has been very extensive. The molecular structure of polysilazane is changed by modification of the molecular main chain or branched chain, and the hydrophobic properties are improved by graftin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/62C09D183/16
CPCC08G77/62C09D183/16
Inventor 商轶孙强吴小峰顾秀杰高春新李杰刘波涛肖志远李占强李献强
Owner 718TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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