Method for preparing bis (triethoxypropylsilane) polysulfide

A technology of propyltriethoxysilane and chloropropyltriethoxysilane, which is applied in the field of preparing double polysulfides, can solve problems affecting production costs, unstable production, and difficult handling, and achieve low production costs , High product quality, stable process effect

Inactive Publication Date: 2010-07-07
南京市化学工业研究设计院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcoming of this production method is: the production is unstable, the pr

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a 1000 milliliter three-necked flask, add 85 grams of sodium sulfide (about 90% of sodium sulfide content), 47.5 grams of sulfur, and 140 g of NaCl aqueous solution, which is 140 grams of waste liquid obtained in Comparative Example 1 (adjust the pH value with phosphoric acid is 5.5). Stir and heat up until the temperature of the material reaches 85°C, keep it warm for 30 minutes, add 2.5 grams of tetrabutylammonium bromide and 245 grams of chloropropyltriethoxysilane, keep it at 75°C-85°C for 3 hours, and take the upper layer product for analysis after the reaction is completed : Chloropropyltriethoxysilane 1.5%, average sulfur chain length 3.75, product yield 96.7%. The lower layer waste liquid is about 200 grams, and its composition is 70% water, 28% sodium chloride, a small amount of phase transfer catalyst tetrabutylammonium bromide and a small amount of chloropropyltriethoxysilane.

Embodiment 2

[0027] In a 1000 milliliter three-necked flask, add 40 grams of sodium hydrosulfide (sodium hydrosulfide content is about 71%), 18 grams of sodium hydroxide, 47.5 grams of sulfur, and add 200 g of NaCl aqueous solution, which is the waste liquid 200 in Example 1. gram (with 5 grams of sodium dihydrogen phosphate to adjust the pH value to 7.5). Stir and heat up until the temperature of the material reaches 85°C, keep it warm for 30 minutes, add 2.5 grams of tetrabutylammonium bromide and 245 grams of chloropropyltriethoxysilane, keep it at 75°C-85°C for 3 hours, and take the upper layer product for analysis after the reaction is completed : Chloropropyltriethoxysilane 1.5%, average sulfur chain length 3.72, product yield 96.1%. The lower layer waste liquid is about 201 grams, and its composition is mainly 70% water, 28% sodium chloride, a small amount of phase transfer catalyst tetrabutylammonium bromide and a small amount of chloropropyltriethoxysilane.

Embodiment 3

[0029] In a 1000 milliliter three-necked flask, add 40 grams of sodium hydrosulfide (sodium hydrosulfide content is about 71%), 20 grams of sodium hydroxide, 47.5 grams of sulfur, and 201 g of NaCl aqueous solution, which is 201 grams of waste liquid in Example 2 (adjust the pH value to 6.5 with sulfuric acid). Stir and heat up until the temperature of the material reaches 85°C, keep it warm for 30 minutes, add 2.5 grams of tetrabutylammonium bromide and 245 grams of chloropropyltriethoxysilane, keep it at 75°C-85°C for 3 hours, and take the upper layer product for analysis after the reaction is completed : Chloropropyltriethoxysilane 0.9%, average sulfur chain length 3.73, product yield 96.0%.

[0030] Carry out production according to above-mentioned process cycle, the NaCl aqueous solution that adds is the waste liquid 201g (adjusting pH value with phosphoric acid to be 6.5) in the last production, the number of cycles is 86 times, no polymerization phenomenon takes place, ...

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Abstract

The invention relates to a method for preparing bis (triethoxypropylsilane) polysulfide, which can obviously improve the yield of the product. The method for preparing the bis (triethoxypropylsilane) polysulfide is that in aqueous solution of NaCl with a concentration by mass percent of not less than 10 percent, sodium polysulfide reacts with chloropropyl triethoxy silane under the action of a phase transfer catalyst to obtain the bis (triethoxypropylsilane) polysulfide. The bis (triethoxypropylsilane) polysulfide is shown as the formula (1). The invention has the advantages that: (1) the process is simple and easy to be implemented; (2) the generated liquid waste can be totally recycled so as to correspond to the requirement for energy saving and emission reduction; and (3) the product production cost is low, the process is stable, the product has high quality, the yield is over 95 percent and no polymerism occurs by cycling tests dozens of times.

Description

technical field [0001] The invention relates to a method for preparing bis(propyltriethoxysilane) polysulfide. Background technique [0002] Sulfur-containing silane is one of the indispensable additives for the production of green tires and is widely used in sulfur vulcanized rubber products. In the tire industry, sulfur-containing silane can improve the tensile strength of the rubber compound, reduce wear, and improve fatigue resistance. Among them, bis(propyltriethoxysilane) polysulfide is a commonly used sulfur-containing silane. [0003] The production method of existing two (propyltriethoxysilane) polysulfides is: react with water, sodium hydrosulfide or sodium sulfide, sodium hydroxide and sulfur to make sodium polysulfide solution, and then react with chloropropyl triethyl Oxysilane generates bis(propyltriethoxysilane) polysulfide under the condition of phase transfer catalyst. After the reaction, the solid is removed by filtration, and then the liquid is left to s...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 李钟宝
Owner 南京市化学工业研究设计院有限公司
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