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Method for preparing mercaptoalkyl alkoxy silane

A technology of mercaptoalkylalkoxysilane and chloroalkylalkoxysilane, which is applied in the field of preparation of mercaptoalkylalkoxysilane, can solve the problems of cumbersome operation, easy mixing of products, and difficulty in removal, and achieve the goal of supply Sufficient, cheap, convenient source effect

Inactive Publication Date: 2009-05-06
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] A preparation method is disclosed in the patent document of Chinese Patent Publication No. CN1746175, which is characterized in that: using chloroalkyl alkoxysilane and thiourea as raw materials, in the presence of a catalyst in a certain proportion, with alcohol as a solvent, after adding Under pressure conditions, react at a certain temperature to generate a mixture of mercaptoalkylalkoxysilanes, statically separate the salts, and supernatant decompression distillation target substance mercaptoalkylalkoxysilanes; the disadvantage of the above method is that by-product organic Salt is soluble in the product, it is difficult to remove even if distilled, and the product is easy to mix
The disadvantage of the above method is that the process is long and the operation is relatively cumbersome

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Weigh 54.5g of sodium methoxide with a content of 99%, put it into a 500mL autoclave with stirring, pass cooling water, cool down, and start stirring. Adjust the stirring speed to 100 rpm, slowly feed 37.4 g of hydrogen sulfide with a purity of 99%, keep the temperature in the kettle at 40°C, and the pressure at 0.4Mpa.

[0029] 200g of chloropropyltrimethoxysilane was added dropwise into the small autoclave, and the dropwise addition took 0.5 hours. During the whole dropping process, the temperature was controlled at 60°C and the pressure was 0.6Mpa. After the dropwise addition, the temperature was raised to 100° C., and the reaction was completed after 4 hours of heat preservation.

[0030] Cool down, absorb excess hydrogen sulfide with sodium methoxide, filter, and collect the filtrate for distillation. The condenser is made of low-temperature freezing liquid as cooling medium (the temperature of the freezing liquid is 0° C.), and vacuum distillation collects 191 g ...

Embodiment 2

[0032] Weigh 109g of sodium methoxide with a content of 99%, put it into a stirred 1000mL autoclave, pass cooling water, cool down, and start stirring. Adjust the stirring speed to 100 rpm, slowly feed 74.8g of hydrogen sulfide with a purity of 99%, keep the temperature in the kettle at 50°C, and the pressure at 0.6Mpa.

[0033] 367g of chloropropylmethyldimethoxysilane with a content of 99% was added dropwise into the small autoclave. The dropwise addition took 1.5 hours. The temperature during the entire dropping process was controlled at 60°C and the pressure was 0.3Mpa. After the dropwise addition, the temperature was raised to 90° C., and the reaction was completed after 6 hours of heat preservation.

[0034] Cool down, absorb excess hydrogen sulfide with sodium methoxide, filter, and collect the filtrate for distillation. The condenser uses low-temperature freezing liquid as the cooling medium (the temperature of the freezing liquid is 0°C), the filtrate is distilled un...

Embodiment 3

[0036] Claim 275Kg content and be 99% sodium ethylate, put into the 2000L autoclave with stirring, feed cooling water, cool down, start stirring, adjust stirring speed to be 300 revs / min, slowly feed into 155Kg of hydrogen sulfide with a purity of 99%, keep The temperature in the kettle is 50°C, and the pressure is 0.5Mpa. After passing the hydrogen sulfide, stir, keep warm and keep the pressure for 3 hours.

[0037]965Kg of chloropropyltriethoxysilane with a content of 99% was added dropwise into the autoclave, and the dropwise addition took 4 hours. The temperature during the entire dropping process was controlled at 60°C and the pressure was 0.8Mpa. After the dropwise addition, the temperature was raised to 85° C., and the reaction was completed after 6 hours of heat preservation.

[0038] Cool down, absorb excess hydrogen sulfide with sodium ethoxide, filter, and collect the filtrate for distillation. The condenser is used as the cooling medium by the refrigerated liquid ...

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PUM

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Abstract

The invention discloses a preparation method for hydrosulfuryl alkyl alkoxy silane. The method has lower cost and is suitable for the large-scale industrialized production. The method comprises the following steps: 1 adding sodium alcoholate into an autoclave under the protection of inert gas; 2 then introducing hydrogen sulfide into the autoclave, controlling the temperature at 10 to 70 DEG C, and controlling the pressure in the autoclave at 0.01 to 2MPa; 3 then dropping chloride alkyl alkoxy silane into the autoclave, controlling the temperature at 10 to 150 DEG C, and controlling the pressure in the autoclave at 0.01 to 2MPa; and 4 then filtering the reactants, collecting the filtrate and carrying out vacuum distillation; and collecting the distillation to obtain the object of hydrosulfuryl alkyl alkoxy silane. The method has the advantages of simple process and environmental pollution reduction, together with the product yield above 90 percent, and the product purity above 98 percent.

Description

technical field [0001] The invention relates to a preparation method of mercaptoalkylalkoxysilane. Background technique [0002] Mercaptoalkylalkoxysilanes are mainly used in polymer modification—such as radial tires, light-curing resins, dyeing and finishing auxiliaries, etc., and there are many applications. Therefore, there are many studies on the synthesis of mercaptoalkylalkoxysilanes. [0003] A preparation method is disclosed in the patent document of Chinese Patent Publication No. CN1746175, which is characterized in that: using chloroalkyl alkoxysilane and thiourea as raw materials, in the presence of a catalyst in a certain proportion, with alcohol as a solvent, after adding Under pressure conditions, react at a certain temperature to generate a mixture of mercaptoalkylalkoxysilanes, statically separate the salts, and supernatant decompression distillation target substance mercaptoalkylalkoxysilanes; the disadvantage of the above method is that by-product organic ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 陶荣辉李建中赵世勇陈剑方剑慧
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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