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Method for producing novel sulfur-containing organosilicon compound

A technology of organosilicon compounds and hydrosulfides, which is applied in organic chemistry, chemical instruments and methods, and compounds of group 4/14 elements of the periodic table, can solve the problems of toxic hydrogen sulfide and many processes, and achieve simplified processes, safety effect

Inactive Publication Date: 2011-04-27
DAISO CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] However, using this method has the following problems: since sulfur is added according to the amount of sulfur chains of the sulfur-containing organosilicon compound required after making anhydrous sodium sulfide, the reaction tank needs to be opened and closed, so the process is relatively complicated. many
[0013] However, there is a problem with the production of toxic hydrogen sulfide caused by side reactions

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0099] In a 200ml three-necked flask, put 3.71g of aqueous sodium hydrosulfide with a purity of 72.3%, 3.94g of 48% aqueous sodium hydroxide solution, and 2.3g of sulfur, and heat them in an oil bath at 140°C under nitrogen flow. Mix well. The mixture turned into a dark brown solution in about 15 minutes. Afterwards it was stirred for 1 hour. Dehydration was performed by heating the reaction mixture at a temperature of 150° C. and a pressure of 3 Torr for 3 hours. This gave a reddish-brown reaction mixture containing anhydrous sodium polysulfide.

[0100] 110 g of ethanol dehydrated with molecular sieves was added to the dehydrated reaction mixture, and after stirring for 30 minutes, 20.8 g of chloropropyltriethoxysilane (abbreviated as TESPC) was added and reacted at 60°C. After 3 hours 93.4% of TESPC was consumed. After the obtained reaction mixture was filtered with filter paper, ethanol was distilled off. Thus, 20.6 g of a sulfur-containing organosilicon compound havi...

Embodiment 2

[0102] Put 3.21g of aqueous sodium hydrosulfide with a purity of 72.3%, 3.46g of 48% aqueous sodium hydroxide solution, and 3.83g of sulfur into a 200ml three-necked flask, and heat them in an oil bath at 140°C under a nitrogen stream while uniformly mixed. The mixture turned into a dark brown solution in about 15 minutes. Afterwards it was stirred for 1 hour. Dehydration was performed by heating the reaction mixture at a temperature of 150° C. and a pressure of 3 Torr for 3 hours. Thus, an orange reaction mixture containing anhydrous sodium polysulfide was obtained.

[0103] 110 g of ethanol dehydrated using molecular sieves was added to the dehydrated reaction mixture, and after stirring for 30 minutes, 19.1 g of TESPC was added and reacted at 60°C. After 3 hours 97.3% of TESPC was consumed. After the obtained product was filtered using filter paper, ethanol was distilled off. Thus, 19.7 g of a sulfur-containing organosilicon compound having a polysulfide structure was ...

Embodiment 3

[0105] 7.76g of aqueous sodium hydrosulfide, 8.23g of 48% sodium hydroxide aqueous solution, and 9.6g of sulfur with a purity of 72.3% were put into a 200ml three-necked flask, and they were uniformly mixed while heating in an oil bath at 140°C under a nitrogen stream. mix. The mixture turned into a dark brown solution in about 15 minutes. Stirring was then carried out for 30 minutes. To this reaction mixture, 52 g of toluene dehydrated using molecular sieves was added, toluene and water were azeotroped, and toluene was distilled off together with water. The above-mentioned azeotropic operation was repeated 3 times. A product containing anhydrous sodium polysulfide is thus obtained.

[0106] 55 g of ethanol dehydrated using molecular sieves was added to the dehydrated reaction mixture, and 48.3 g of TESPC was added while stirring, and reacted at 80°C. After 4 hours 98.9% of TESPC was consumed. After the obtained product was filtered using filter paper, ethanol was distill...

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PUM

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Abstract

Disclosed is a low-cost method for obtaining a high-purity sulfur-containing organosilicon compound having a polysulfide structure. A sulfur-containing silicon compound represented by formula [II] is obtained by performing a first reaction for uniformly mixing an alkali hydrosulfide, sulfur and an alkali hydroxide in the presence of water, then dehydrating the reaction mixture, and then sequentially adding a halogenoalkoxysilane represented by formula [I] into the resulting mixture in a polar solvent. (R1-O)n(R1)3-n-Si-R2-X [I] (R1-O)n(R1)3-n-Si-R2-Sm-R2-Si-(R1)3-n(O-R1)n [II] In the formulae, R1 represents a monovalent hydrocarbon group having 1-16 carbon atoms; R2 represents a divalent hydrocarbon group having 1-9 carbon atoms; X represents a halogen atom; n represents an integer of 1-3; and m represents an integer of 1-12.

Description

technical field [0001] The present invention relates to a novel preparation method of a sulfur-containing organosilicon compound useful as a rubber compounding agent. The sulfur-containing organosilicon compound is a compound in which synthetic rubber or natural rubber having an unsaturated bond is combined with a white filler such as silica, clay, talc or a filler such as surface-modified carbon black compounded in the rubber. Background technique [0002] Sulfur-containing organosilicon compounds are industrially useful compounds that have been known for a long time, and many methods for their production have been known in the past. [0003] As a representative method thereof, a method is known in which a halogenated organosilane represented by the following general formula [III], anhydrous sodium sulfide, and sulfur are reacted in a solvent at 70 to 80° C. for several hours to obtain A method of a sulfur-containing organosilicon compound represented by the following gene...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
CPCC07F7/1892
Inventor 大炭雅彦山田聿男市野智之中村正吉
Owner DAISO CO LTD
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