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A kind of synthetic method of sulfur-containing silane

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

Active Publication Date: 2018-05-11
江西宏柏新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 yield, unstable quality and high cost of environmental protection treatment in the existing production process of sulfur-containing silanes

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  • A kind of synthetic method of sulfur-containing silane
  • A kind of synthetic method of sulfur-containing silane
  • A kind of synthetic method of sulfur-containing silane

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preparation example Construction

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

[0065] S1. Under nitrogen protection, put sodium metal and the solvent into a metering tank, heat to 98-120°C, disperse, and prepare a sodium suspension;

[0066] S2. Under nitrogen protection, put sulfur and the solvent into a stirred tank, heat to 113-120°C, disperse, and prepare 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 into the sulfur suspension. After the addition is completed, the temperature is maintained and the reaction is continued for 5-15 minutes. Obtain the organic solution of sodium polysulfide;

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

Embodiment 1

[0120] Use molecular sieves to dehydrate the dimethylformamide solvent, then pass nitrogen gas into the dimethylformamide solvent under a pressure of 0.04Mpa and ultrasonically treat it for 5 minutes, and the dissolved oxygen in the dimethylformamide solvent is measured to be less than 3ppm , and then proceed as follows:

[0121] S1. Under nitrogen protection, put sodium metal and dimethylformamide solvent into a metering tank, heat to 100°C, and disperse to prepare a sodium suspension with a sodium concentration of 4mol / L;

[0122]S2. Under nitrogen protection, put sulfur and dimethylformamide solvent into a stirred tank, heat to 115°C, and disperse to prepare a sulfur suspension with a sulfur concentration of 4mol / L;

[0123] 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, and the volume ratio of the sodium suspension to the sulfur...

Embodiment 2

[0127] Use calcium sulfate and magnesium sulfate to dehydrate the dimethylacetamide solvent, then under the pressure of 0.015Mpa, feed nitrogen into the dimethylacetamide solvent and ultrasonically treat it for 3min, measure the Dissolved oxygen is less than 3ppm, then proceed to the following steps:

[0128] S1. Under nitrogen protection, put sodium metal and dimethylacetamide solvent into a metering tank, heat to 98°C, and disperse to prepare a sodium suspension with a sodium concentration of 2mol / L;

[0129] S2. Under nitrogen protection, put sulfur and dimethylacetamide solvent into a stirred tank, heat to 120°C, and disperse to prepare a sulfur suspension with a sulfur concentration of 8mol / L;

[0130] S3, under the protection of nitrogen, the temperature of the sulfur suspension is controlled at 100°C, the sodium suspension prepared in step S1 is added dropwise into the sulfur suspension, the volume ratio of the sodium suspension to the sulfur suspension is 1:1, Add dro...

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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 synthesis method of sulfur-containing silane. Background technique [0002] Sulfur-containing silane is a conventional silane coupling agent with a unique "amphiphile" (referring to the molecule containing both organic and inorganic groups after hydrolysis) functional groups. It is mainly used as an additive for tire rubber. Improve the processing performance and use performance of rubber, and improve the performance of tires such as tear resistance, wear resistance, and wet grip. [0003] At present, the synthesis method of sulfur-containing silane is mainly to prepare sodium polysulfide, which is obtained by reacting sodium polysulfide with haloalkylalkoxysilane to obtain a crude product, and then undergoes a series of impurity removal treatments to obtain its product. Among them, the quality level of sodium polysulfide is the most critical factor affecting the yield and quality of sulfur-containing silane products. [00...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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