Method for synthesizing di-[propyltriethoxysilane]-tetrasulfide

A technology of propyltriethoxysilane and chloropropyltriethoxysilane is applied in the field of synthesis of bis-[propyltriethoxysilane]-tetrasulfide, which can solve the problem of low purity and influence on product use. , the problem of high production cost, to achieve the effect of reducing reaction temperature, improving production capacity and reducing production energy consumption

Inactive Publication Date: 2010-11-17
WEIFANG WORLD CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the above-mentioned several methods have certain advantages, they still have the following disadvantages: (1) the raw material is expensive and difficult to store, and the production cost is high; (2) it is easy to cause product Si-69 hydrolysis failure; (3) method (1) and Method (2) uses metallic sodium, and the risk of operation increases, and the operation requirements are strict, and the process conditions are difficult to control; (4) the total yield of the product is low, and the purity is low, and the product purity is only 96% (GC) (equivalent) (5) The color of the product after distilla

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Preparation of sodium tetrasulfide aqueous solution: 270Kg of demineralized water, sodium sulfide (by 100wt% content) 82Kg, sodium dithionate 5Kg, elemental sulfur 102Kg and diethylhydroxylamine 1.8Kg are added to the reactor successively, mixed and stirred for 25 minutes, Turn on the vacuum pump so that the vacuum degree in the reactor is 0.046MPa, then turn off the vacuum pump, use the vacuum in the reactor to pump 1.5Kg of n-amylamine and 2.2Kg of isobutylamine into the reactor, turn on the steam and slowly raise the temperature, and within 20 minutes, the reaction The temperature of the material in the kettle was raised to 40° C., and reacted at 40° C. for 30 minutes. When the color of the material in the reactor was dark blood red, it indicated that the reaction was over, and an aqueous solution of sodium tetrasulfide was obtained.

[0027](2) Synthetic bis-[propyltriethoxysilane]-tetrasulfide: when the pressure in the reactor was normal pressure, in the sodium ...

Embodiment 2

[0032] (1) Preparation of sodium tetrasulfide aqueous solution: demineralized water 280Kg, sodium sulfide (by 100wt% content) 83Kg, sodium dithionate 5.5Kg, elemental sulfur 105Kg and diethylhydroxylamine 2Kg were added to the reactor successively, mixed and stirred for 30 minutes, Turn on the vacuum pump so that the vacuum degree in the reactor is 0.05MPa, then turn off the vacuum pump, use the vacuum in the reactor to pump 1.8Kg of n-amylamine and 2.5Kg of isobutylamine into the reactor, turn on the steam and slowly raise the temperature, and the reaction will be carried out within 30 minutes. The temperature of the material in the still was raised to 45° C., and reacted at 45° C. for 35 minutes. When the color of the material in the reaction kettle was dark blood red, it indicated that the reaction was finished, and an aqueous solution of sodium tetrasulfide was obtained.

[0033] (2) Synthetic bis-[propyltriethoxysilane]-tetrasulfide: when the pressure in the reactor was no...

Embodiment 3

[0038] (1) Preparation of sodium tetrasulfide aqueous solution: 285Kg of demineralized water, 85Kg of sodium sulfide (according to 100wt% content), 6.5Kg of sodium dithionite, 110Kg of elemental sulfur and 2.5Kg of diethylhydroxylamine are added to the reactor successively, and mixed and stirred for 30 minutes , turn on the vacuum pump to make the vacuum in the reactor be 0.06MPa, then turn off the vacuum pump, use the vacuum in the reactor to pump 2.2Kg of n-amylamine and 2.8Kg of isobutylamine into the reactor, turn on the steam and slowly heat up, within 40 minutes The temperature of the material in the reactor was raised to 48°C, and reacted at 48°C for 40 minutes. When the color of the material in the reactor was dark blood red, it indicated that the reaction was over, and an aqueous solution of sodium tetrasulfide was obtained.

[0039] (2) Synthetic bis-[propyltriethoxysilane]-tetrasulfide: when the pressure in the reactor was normal pressure, in the sodium tetrasulfide ...

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PUM

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Abstract

The invention discloses a method for synthesizing di-[propyltriethoxysilane]-tetrasulfide, which comprises the following steps of: (1) mixing and stirring water, sodium sulfide, sodium hyposulfate, elemental sulfur and diethyl hydroxylamine, pumping n-amylamine and isobutylamine into the mixture under the vacuum degree of 0.04 to 0.06MPa, and reacting the mixture for 20 to 40 minutes at the temperature of between 30 and 50 DEG C; (2) adding dodecyltrimethylammonium chloride, tetrabutyl ammonium bromide and hydroxy pyridine into the reaction solution obtained in the (1) under normal pressure, stirring the solution, then adding gamma-chloropropyltriethoxysilane into the solution, reacting the solution for 30 to 60 minutes at the temperature of between 40 and 50 DEG C, continuously reacting the solution for 60 to 80 minutes at the temperature of between 60 and 80 DEG C, filtering the oil phase, and pumping the filtrate into a distillation still; and (3) distilling the filtrate in the distillation still under the vacuum degree of more than or equal to 0.096MPa at the temperature of less than or equal to 160 DEG C when the temperature of the top gas phase is more than 108 DEG C to obtain a product Si-69.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for synthesizing bis-[propyltriethoxysilane]-tetrasulfide. Background technique [0002] Bis-[propyltriethoxysilane]-tetrasulfide (hereinafter referred to as Si-69) is a sulfur-containing multifunctional group silane coupling agent successfully used in the rubber and plastic industry. Its application makes the rubber The physical and mechanical properties are improved, the tensile strength, tear strength, wear resistance, etc. can be significantly improved, the permanent deformation can be reduced, and the viscosity of the rubber can be reduced, and the processing performance can be improved. It is especially suitable for vulcanized rubber systems with silica or silicate as reinforcing agents. The applicable polymers include natural rubber (NR), styrene-butadiene rubber (SBR), isoprene rubber (IR), butadiene rubber Acrylic rubber (BR), nitrile rubber (NBR) and ethylene...

Claims

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Application Information

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IPC IPC(8): C07F7/18C07F7/20
Inventor 丁爱梅张中法郭学阳黄慧吕彩玲温占平李津哲
Owner WEIFANG WORLD CHEM
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