Method for synthesizing sulfur-containing silane coupling agent from sodium polysulfide

A technology of sulfur silane coupling agent and sodium polysulfide, which is applied in the field of synthesizing sulfur-containing silane coupling agents, can solve the problems of high cost, high impurity components, high risk factor, etc., and achieve sufficient procurement of goods, little environmental pollution, The effect of low reaction temperature

Active Publication Date: 2013-01-16
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem that former method exists is: the sodium sulfide purity of domestic production is not high, and it contains more impurity components, and the sodium polysulfide produced has greater influence on the product quality of sulfur-containing silane; Volatile oxidation is relatively serious, which will also lead to large fluctuations in product quality and serious environmental pollution
The problem that the latter method exists is: the quality of the sodium polysulfide prepared by the reaction of metal sodium and sulfur is better, but its cost is too high, so it is not suitable for large-scale industrial production
At the same time, because metal sodium is easy to spontaneously ignite, the risk factor in its production process is relatively large.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In a 1000ml flask with mechanical stirring, thermometer, and condenser, add 96g of sodium hydroxide, 200g of tap water and stir at 500~600r / min for about 10 minutes to completely dissolve the sodium hydroxide to make an aqueous solution. Increase the temperature. When the sodium hydroxide aqueous solution is heated to 80~85℃, add 86g of sulfur (S) and stir at 500~600r / min for 15 minutes. The sulfur begins to dissolve, then heat and control the temperature at 90~95℃ React for 2 hours at a stirring speed of 1000~1200r / min to generate an aqueous solution of sodium polysulfide.

[0017] It will be replaced with a distillation device. At a temperature of 100~110℃, first atmospheric distillation for 4h, when about 150g of water is distilled, the atmospheric distillation will be stopped; then at 110~130℃, the vacuum degree is higher than -0.099MPa. Press distillation for 5 hours to remove the remaining water; then naturally cool down, when the temperature of the kettle drops belo...

Embodiment 2

[0021] In a 1000ml flask with mechanical stirring, thermometer, and condenser, add 96g of sodium hydroxide, 200g of tap water and stir at 500~600r / min for about 10 minutes to completely dissolve the sodium hydroxide to make an aqueous solution. Increase the temperature. When the sodium hydroxide aqueous solution is heated to 80~85℃, add 124g of sulfur (S) and stir at 500~600r / min for 15 minutes. The sulfur begins to dissolve, then heat and control the temperature at 90~95℃ React for 2 hours at a stirring speed of 1000~1200r / min to generate an aqueous solution of sodium polysulfide.

[0022] It will be replaced with a distillation device, and the normal pressure distillation is carried out at a temperature of 100~110℃ for 4h. When about 180g of water is distilled, the normal pressure distillation will be stopped; then the reduction will be carried out at 110~130℃ and the vacuum degree is higher than -0.099MPa. Press distillation for 4~5h to remove the remaining water; let it cool ...

Embodiment 3

[0026] In a 1000ml flask with mechanical stirring, thermometer, and condenser, add 96g of sodium hydroxide, 200g of tap water and stir at 500~600r / min for about 10 minutes to completely dissolve the sodium hydroxide to make an aqueous solution. Increase the temperature. When the sodium hydroxide aqueous solution is heated to 80~85℃, add 130g of sulfur (S), and stir at 500~600r / min for 10 minutes. The sulfur begins to dissolve, then heat to increase and control at 90~95 React at a stirring speed of 1000~1200r / min for 3 hours at ℃ to generate sodium polysulfide aqueous solution.

[0027] It will be replaced in the distillation device, and the normal pressure distillation is carried out at a temperature of 100~110℃ for 4h. When about 180g of water is distilled, the normal pressure distillation will be stopped; then it will be carried out at 110~130℃ and the vacuum degree is higher than -0.099MPa. Negative pressure distillation for 4~5h to remove the remaining water; let it cool down...

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Abstract

The invention relates to a method for synthesizing a sulfur-containing silane coupling agent from sodium polysulfide, belonging to the technical field of organic chemistry. The method comprises the following steps: reacting sodium hydroxide and sulfur to prepare sodium polysulfide, and synthesizing the sulfur-containing silane coupling agent from the sodium polysulfide. The invention solves the problems of great product quality fluctuation and heavy environmental pollution in the sulfur-containing silane in the production of sodium polysulfide from sodium sulfide and sulfur, and the problem of high cost in the sodium polysulfide prepared from sodium metal and sulfur at present in China. Since the temperature is low in the whole reaction process, no sulfur is volatilized, no sulfur dioxide (SO2) gas due to contact oxidation of air is generated, thus, the environmental pollution is slight, and the produced sulfur-containing silane product has stable sulfur distribution. The invention has the advantages of low cost, high control stability, stable product quality and light color.

Description

Technical field [0001] The invention relates to a method for synthesizing a sulfur-containing silane coupling agent by using sodium polysulfide, and belongs to the technical field of organic chemistry. Background technique [0002] Sulfur-containing silane is a conventional silane coupling agent, mainly used as an additive to tire rubber to improve the tire's tear resistance, wear resistance, wet grip and other properties. The most commonly used sulfur-containing silanes are bis-[3-(triethoxysilyl)propyl]-polysulfide, mainly bis-[3-(triethoxysilyl)propyl]-disulfide and Bis-[3-(triethoxysilyl)propyl]-tetrasulfide, the amount of which accounts for more than 90% of the total sulfur-containing silane. The synthesis method of its bis-[3-(triethoxysilyl)propyl]-polysulfide is mainly to use sodium polysulfide and 3-chloropropyltriethoxysilane to react to obtain the crude product, and then undergo a series of purification treatments Get its product. The quality level of sodium polysul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
Inventor 王灿陈圣云靳军阮少阳王欣胡江华甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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