Synthetic method for novel rubber sulfur-containing silane coupling agent--bis-[gamma-(trimethoxy)silylpropyl]tetrasulfide

A technology of chloropropyltrimethoxysilane and trimethoxy is applied in the synthesis field of rubber auxiliaries, which can solve the problems of high cost and increase in cost, and achieve the effects of reducing production cost, reducing product yield and small molecular weight

Inactive Publication Date: 2015-10-07
HEZE UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

With the increasing depletion of petroleum resources, the cost of absolute ethanol will be higher and higher, which will directly lead to an increase in the cost of synthesizing Si-69

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The preparation method of novel rubber additive bis-[γ-(trimethoxy)silylpropyl] tetrasulfide adopts the following steps:

[0020] (1) Using methanol as an esterifying agent, esterify γ-chloropropyltrichlorosilane into γ-chloropropyltrimethoxysilane. During the synthesis process, a vacuum pump is used to strictly control the rate of methanol addition, while hydrogen chloride gas is discharged, hydrochloric acid is produced as a by-product, the esterification rate and time are controlled, sampling inspection is carried out in time, and the pH of γ-chloropropyltrimethoxysilane is maintained at 7.

[0021] (2) In a three-neck flask equipped with a stirrer and a thermometer, add 100g of methanol and 30g of solid sodium hydroxide in sequence, stir well to dissolve, then add 28g of sulfur powder in batches, stir and heat up to 60°C, the reaction solution gradually It turns orange red, then dark brown, and the reaction lasts for about 2 hours, and then the temperature is lo...

Embodiment 2

[0025] The preparation method of bis-[γ-(trimethoxy)silylpropyl]tetrasulfide of novel rubber auxiliary agent adopts the following steps:

[0026] (1) Using methanol as an esterifying agent, esterify γ-chloropropyltrichlorosilane into γ-chloropropyltrimethoxysilane. During the synthesis process, a vacuum pump is used to strictly control the rate of methanol addition, while hydrogen chloride gas is discharged, hydrochloric acid is produced as a by-product, the esterification rate and time are controlled, sampling inspection is carried out in time, and the pH of γ-chloropropyltrimethoxysilane is maintained at 7.

[0027] (2) In a three-neck flask equipped with a stirrer and a thermometer, add 85g of methanol and 22g of solid sodium hydroxide in sequence, stir well to dissolve, then add 21g of sulfur powder in batches, stir and heat up to 55°C, the reaction solution gradually Turn orange red, then dark brown, react for 2h, make its temperature drop to normal temperature, set aside...

Embodiment 3

[0031] (1) Using methanol as an esterifying agent, esterify γ-chloropropyltrichlorosilane into γ-chloropropyltrimethoxysilane. During the synthesis process, a vacuum pump is used to strictly control the speed of adding methanol, while hydrogen chloride gas is discharged, hydrochloric acid is produced by-product, the esterification speed and time are controlled, sampling inspection is carried out in time, and the pH of γ-chloropropyltrimethoxysilane is kept at 7.

[0032](2) In a three-necked flask equipped with a stirrer and a thermometer, add 110g of methanol and 36g of solid sodium hydroxide in sequence, stir thoroughly to dissolve, then add 33g of sulfur powder in batches, stir and heat up to 50°C, the reaction solution gradually Turn orange red, then dark brown, react for 3.0h, make its temperature drop to normal temperature, set aside.

[0033] (3) Pour the reaction solution prepared in (2) into another three-necked flask, stir, and raise the temperature to 50°C, add 2.6g...

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PUM

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Abstract

The invention relates to a synthetic method for a novel rubber chemical--bis-[gamma-(trimethoxy)silylpropyl]tetrasulfide. The method comprises the following steps: with methanol as an esterification agent, esterifying gamma-chloropropyltrichlorosilane into gamma-choropropyltrimethoxysilane; with methanol as a solvent, preparing a sodium hydroxide methanol solution with a mass concentration of 20 to 25% and reacting the sodium hydroxide methanol solution with a certain amount of sulfur powder at 50 to 60 DEG C; and pouring the prepared sodium sulfide solution into a synthetic kettle, adding a catalyst--cetyltrimethylammonium bromide prepared in advance, then adding gamma-choropropyltrimethoxysilane and judging reaction process according to color changes of a reaction solution and production of the by-product NaCl. According to the invention, methanol is used as a starting raw material, sulfur content of the novel rubber sulfur-containing silane coupling agent is increased, and production cost is substantially reduced; methanol is used both as an esterification reagent participating in reaction and as a solvent and can be easily separated from the prepared rubber sulfur-containing silane coupling agent by using a distillation method due to the low boiling point, and the purity of the prepared rubber sulfur-containing silane coupling agent is more than 99%.

Description

(1) Technical field [0001] The invention relates to a synthesis method of rubber additives, in particular to a synthesis method of a novel rubber additive sulfur-containing silane coupling agent bis-[γ-(trimethoxy)silylpropyl]tetrasulfide. (2) Background technology [0002] Rubber silane coupling agent can effectively combine silica filler with rubber molecules, improve the processing performance and mechanical properties of rubber products, reduce the rolling resistance of tires, and enhance the wet skid resistance of tires. With the vigorous development of my country's aviation and expressways, the transportation industry has a wide demand for "green tires", and the demand for rubber silane coupling agents is also increasing. [0003] The development of rubber silane coupling agent series products belongs to the frontier topic of organosilicon chemistry, among which the earliest development and production is German Digosha company, and my country began to develop and c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08K5/548C08L21/00
Inventor 田瑞亭陈艳丽许和允
Owner HEZE UNIV
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