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A kind of method utilizing sodium polysulfide to synthesize sulfur-containing silane coupling agent

A technology of sulfur silane coupling agent and sodium polysulfide, applied in the field of synthesizing sulfur-containing silane coupling agent, can solve the problems of high cost, many impurity components, large risk factor, etc. The effect of low reaction temperature

Active Publication Date: 2015-08-12
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 equipped with a mechanical stirrer, a thermometer and a condenser tube, add 96g of sodium hydroxide and 200g of tap water and stir at a speed of 500~600r / min for about 10 minutes to completely dissolve the sodium hydroxide to make an aqueous solution, and Raise the temperature, add 86g of sulfur (S) when the sodium hydroxide aqueous solution is heated up to 80~85°C, and stir at a speed of 500~600r / min for 15 minutes, the sulfur begins to dissolve, then heat up and control it at 90~95°C React for 2 hours at a stirring speed of 1000~1200r / min to generate sodium polysulfide aqueous solution.

[0017] Replace it with a distillation device, first distill at 100~110°C for 4 hours at atmospheric pressure, and stop the distillation at atmospheric pressure when about 150g of water is distilled; Distill under pressure for 5 hours to remove the remaining moisture; then lower the temperature naturally, stop the pump and vent with nitrogen when the temperature of t...

Embodiment 2

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

[0022] Replace it with a distillation device, and carry out atmospheric distillation at 100~110°C for 4 hours. When about 180g of water is distilled, stop the atmospheric distillation; Distill under pressure for 4~5h to remove the remaining moisture; let it cool down naturally, stop the pump and vent with nitrogen when the temperature of the kettle drops below 50°C...

Embodiment 3

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

[0027] Replace it with a distillation device, carry out atmospheric distillation at 100~110°C for 4 hours, stop the atmospheric distillation when about 180g of water is distilled; Negative pressure distillation for 4~5h to remove the remaining water; let it cool down naturally, stop the pump and vent with nitrogen when the temperature of the kettle drops below 50°C; get ...

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PUM

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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, which belongs to the technical field of organic chemistry. Background technique [0002] Sulfur-containing silane is a conventional silane coupling agent, which is mainly used as an additive for tire rubber to improve the performance of tires such as tear resistance, wear resistance, and wet grip. Sulfur-containing silanes are currently the most widely used bis-[3-(triethoxysilyl)propyl]-polysulfide, mainly bis-[3-(triethoxysilyl)propyl]-disulfide and Bis-[3-(triethoxysilyl)propyl]-tetrasulfide, its dosage accounts for more than 90% of the total amount of sulfur-containing silanes. Its bis-[3-(triethoxysilyl)propyl]-polysulfide synthesis method mainly uses sodium polysulfide to react with 3-chloropropyltriethoxysilane to obtain the crude product, and then undergoes a series of purification treatments get its products. Among them,...

Claims

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Application Information

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Patent Type & Authority Patents(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