Sulfur-containing silane synthesizing method

A synthesis method and technology of sulfur silane, applied in the field of synthesis of sulfur-containing silane, can solve the problems of high environmental protection treatment cost, unstable quality, low product yield and the like, achieve good appearance characterization, ensure quality, and improve the effect of reaction

Active Publication Date: 2017-08-08
江西宏柏新材料股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The present invention provides a method for synthesizing sulfur-containing silanes in order to solve the problems of low product y

Method used

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  • Sulfur-containing silane synthesizing method
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  • Sulfur-containing silane synthesizing method

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preparation example Construction

[0064] A method for synthesizing sulfur-containing silane, using one or more of dimethylformamide, dimethylacetamide, hexamethylphosphoramide, and 1,3-dimethyl-2-imidazolidinone as a solvent, Take the following steps:

[0065] S1. Under the protection of nitrogen, put metallic sodium and the solvent into a measuring tank, heat to 98-120°C, and disperse to obtain a sodium suspension;

[0066] S2, under the protection of nitrogen, put sulfur and the solvent in a stirred tank, heat to 113-120°C, and disperse to obtain a sulfur suspension;

[0067] S3. Under the protection of nitrogen, the temperature of the sulfur suspension is controlled at 45-100°C, and the sodium suspension prepared in step S1 is added dropwise to the sulfur suspension. After the addition is completed, the temperature is maintained and the reaction is continued for 5-15 minutes. Obtain an organic solution of sodium polysulfide;

[0068] S4. Under the protection of nitrogen and stirring, control the temperature of the...

Embodiment 1

[0119] Use molecular sieve to dehydrate the dimethylformamide solvent, and then pour nitrogen into the dimethylformamide solvent under a pressure of 0.04Mpa and sonicate it for 5 minutes. The dissolved oxygen in the dimethylformamide solvent is measured to be less than 3ppm , And then proceed as follows:

[0120] S1. Under the protection of nitrogen, put metallic sodium and dimethylformamide solvent into a measuring tank, heat to 100°C, and disperse to obtain a sodium suspension with a sodium concentration of 4mol / L;

[0121] S2, under the protection of nitrogen, put sulfur and dimethylformamide solvent into a stirred tank, heat to 115°C, and disperse to obtain a sulfur suspension with a sulfur concentration of 4mol / L;

[0122] S3. Under the protection of nitrogen, the temperature of the sulfur suspension is controlled at 60°C, and the sodium suspension prepared in step S1 is added dropwise to the sulfur suspension. The volume ratio of the sodium suspension to the sulfur suspension i...

Embodiment 2

[0126] Use calcium sulfate and magnesium sulfate to dehydrate the dimethylacetamide solvent, and then pour nitrogen into the dimethylacetamide solvent under a pressure of 0.015Mpa and sonicate it for 3min. The content of the dimethylacetamide solvent is measured Dissolved oxygen is less than 3ppm, and then proceed as follows:

[0127] S1. Under the protection of nitrogen, put metallic sodium and dimethylacetamide solvent into a measuring tank, heat to 98°C, and disperse to obtain a sodium suspension with a sodium concentration of 2mol / L;

[0128] S2, under the protection of nitrogen, put sulfur and dimethylacetamide solvent into a stirred tank, heat to 120°C, and disperse to obtain a sulfur suspension with a sulfur concentration of 8mol / L;

[0129] S3. Under the protection of nitrogen, the temperature of the sulfur suspension is controlled at 100°C, and the sodium suspension prepared in step S1 is added dropwise to the sulfur suspension. The volume ratio of the sodium suspension to t...

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Abstract

The invention provides a sulfur-containing silane synthesizing method. According to the synthesizing method, one or several of dimethyl formamide, dimethyl acetamide, hexamethyl phosphoramide and 1,3-dimethyl-2-imidazolidone is utilized as a solvent; sodium and sulfur are pretreated in the solvent to obtain sodium suspension liquid and sulfur suspension liquid; the sodium suspension liquid is added into the sulfur suspension liquid to react to obtain sodium polysulfide; halogenated alkyl alkoxy silane is added into the sodium polysulfide to react and be decontaminated to obtain a sulfur-containing silane finished product. According to the synthesizing method disclosed by the invention, sulfur-containing silane is synthesized in the solvent, so that not only is reaction efficiency in production improved, but also impurity introduction in a production process is avoided, quality of a final product is guaranteed, and purity, yield and calculation yield of the final product are improved; meanwhile, potential safety hazards and environmental pollution in a sodium and sulfur treating process are avoided, and environment-friendly treating cost in the production process is reduced.

Description

Technical field [0001] The invention relates to a method for synthesizing sulfur-containing silane. Background technique [0002] Sulfur-containing silane is a conventional silane coupling agent. It has a unique "amphiphilic" (referring to both organic and inorganic groups after hydrolysis in the molecule) functional groups. It is mainly used as an additive for tire rubber. Improve the processing performance and use performance of rubber, and improve the tire's tear resistance, wear resistance, wet grip and other properties. [0003] At present, the method for synthesizing sulfur-containing silane is mainly to prepare sodium polysulfide, the crude product is obtained by reacting sodium polysulfide with haloalkylalkoxysilane, and then the product is obtained through a series of impurity removal treatments. Among them, the quality level of sodium polysulfide is the most critical factor affecting the yield and quality of sulfur-containing silane products. [0004] For the preparation ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/1888
Inventor 纪冠丞胡成发李明生黄克生田丹
Owner 江西宏柏新材料股份有限公司
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