Synthesis of vinyl polysilazane and application of vinyl polysilazane in anti-doodling coating

A technology of vinyl polysilazane and methyl vinyl dichlorosilane, applied in the field of chemical coatings, can solve the problems of low vinyl activity and preparation into light-curing coatings, etc., and achieve the effect of safety and repeatability

Pending Publication Date: 2022-06-03
JIANGXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Vinyl polysilazanes have low activity of vinyl groups and cannot b

Method used

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  • Synthesis of vinyl polysilazane and application of vinyl polysilazane in anti-doodling coating

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] (1) Synthesis of vinyl polysilazane.

[0019] 1) In the benzene solution of methylvinyldichlorosilane, under stirring conditions, pass dry and high-purity ammonia gas, keep the reaction at 300 °C for 4 hours, and filter out the precipitate to obtain small molecular methylvinylsilicon. Azane Vi-PZ Liquid.

[0020] 2) Preparation of polysilazane polymer PSZ: co-ammonolysis of dimethyldichlorosilane and methyldichlorohydrogen-containing silane in a molar ratio of 1.5:1 to obtain a low-molecular-weight intermediate, and then under nitrogen protection with 5 The ℃ / min heating rate was slowly raised to 300 ℃, and the reaction was kept for 4 hours. After the reaction, the low-molecular polymer PSZ was removed by vacuum distillation.

[0021] 3) After mixing the products obtained in step 1) and step 2) according to the instruction ratio of 5:1, the solvent was evaporated under nitrogen protection, and then the reaction was kept at 200 °C for 24 h to obtain vinyl polysilazane V...

Embodiment 2

[0025] (1) Synthesis of vinyl polysilazane.

[0026] 1) Pour dry and high-purity ammonia gas into the benzene solution of methylvinyldichlorosilane while stirring, keep the reaction at 300 °C for 4 hours, filter out the precipitate to obtain small molecular methylvinylsilazane Vi-PZ liquid.

[0027] 2) Preparation of polysilazane polymer PSZ, the specific preparation method is as follows: co-ammonolysis of dimethyldichlorosilane and methyldichlorohydrogen-containing silane in a molar ratio of 1.5:0.5 to obtain a low molecular intermediate, and then in Under nitrogen protection, the temperature was slowly raised to 300 °C at a heating rate of 5 °C / min, and the reaction was kept for 4 h. After the reaction, the low molecular weight polymer PSZ was removed by vacuum distillation.

[0028] 3) After mixing the products obtained in step 1) and step 2) according to the instruction ratio of 5:2, the solvent was evaporated under nitrogen protection, and then the reaction was kept at 2...

Embodiment 3

[0032] (1) Synthesis of vinyl polysilazane.

[0033] 1) Pour dry and high-purity ammonia gas into the benzene solution of methylvinyldichlorosilane while stirring, keep the reaction at 300 °C for 4 hours, filter out the precipitate to obtain small molecular methylvinylsilazane Vi-PZ liquid.

[0034] 2) Preparation of polysilazane polymer PSZ, the specific preparation method is as follows: co-ammonolysis of dimethyldichlorosilane and methyldichlorohydrogen-containing silane according to a molar ratio of 1:1 to obtain a low molecular intermediate, and then in Under nitrogen protection, the temperature was slowly raised to 300 °C at a heating rate of 5 °C / min, and the reaction was kept for 4 h. After the reaction, the low molecular weight polymer PSZ was removed by vacuum distillation.

[0035] 3) After mixing the products obtained in step 1) and step 2) according to the instruction ratio of 5:1.5, the solvent was evaporated under nitrogen protection, and then the reaction was k...

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Abstract

The invention relates to synthesis of vinyl polysilazane and application of vinyl polysilazane in an anti-doodling coating, and the synthesis comprises the following steps: 1) in a benzene solution of methyl vinyl dichlorosilane, stirring, introducing ammonia gas, reacting at 300 DEG C for more than or equal to 4 hours, filtering, and carrying out reduced pressure suction filtration to obtain micromolecular methyl vinyl silazane; (2) carrying out ammonolysis on dimethyldichlorosilane and methyl dichloro hydrogen-containing silane to obtain an intermediate, carrying out nitrogen protection, slowly heating to 300 DEG C, carrying out heat preservation reaction for more than or equal to 4 hours, and carrying out reduced pressure distillation to remove a low-molecular polymer, so as to obtain a polysilazane polymer; and (3) mixing the products in the steps (1) and (2) according to a mass ratio of 5: (1-10), evaporating to remove the solvent under the protection of nitrogen, and reacting at 200 DEG C for 24 hours to obtain vinyl polysilazane. The preparation method comprises the following steps: uniformly mixing vinyl polysilazane, high-activity UV resin, a cross-linking agent, a catalyst, a photoinitiator, a solvent and an anti-pollution additive, spraying, and curing by ultraviolet irradiation. The preparation method is safe in reaction temperature and high in repeatability, and can be used for preparing the fast-curing anti-fouling easy-to-clean vinyl polysilazane coating.

Description

technical field [0001] The invention belongs to the technical field of chemical coatings, and relates to the preparation of light-curing coatings. Background technique [0002] As a high-performance silicone resin-based ceramic precursor, polysilazane resin has outstanding application prospects in many fields, such as the preparation of ultra-high temperature resistant coatings in the national defense field, and the preparation of anti-graffiti, hydrophobic , wear-resistant and anti-corrosion coatings. At present, the curing of polysilazane coatings is mainly based on room temperature self-drying and high temperature curing, and there is little research on its photocuring method. Vinyl polysilazane has low vinyl activity and cannot be directly initiated by an initiator to prepare a photocurable coating. SUMMARY OF THE INVENTION [0003] The purpose of the present invention is to propose a synthesis of vinyl polysilazane and its application in anti-graffiti paint. After ...

Claims

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Application Information

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IPC IPC(8): C08G77/62C09D183/16C09D201/00
CPCC08G77/62C09D183/16C09D201/00C08L101/00C08L83/16
Inventor 陈义旺吴刚谈利承叶素文
Owner JIANGXI NORMAL UNIV
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