Method for producing light-color polysulfide silane coupling agent without buffer agent

A silane coupling agent and polysulfide technology, which is applied in the production field of polysulfide silane coupling agent, can solve the problems of buffer product quality, by-product treatment, unfavorable raw material input, high content of impurities, and poor quality. Guarantee and other issues to achieve the effect of reducing the possibility of introducing colored ions, reducing the input of raw materials, and low production costs

Active Publication Date: 2014-05-14
南京曙光精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The polysulfide silane coupling agents currently on the market are generally dark-colored products, which are not conducive to the use of light-colored product industries such as vulcanized rubber system shoe soles
[0003] The current large-scale industrial production method of polysulfide silane coupling agent generally has two kinds, the first kind is the synthetic method that uses alcohol solvent, hydrogen sulfide, alkali metal alcoholate etc. as raw material for organic solvent process, and this method exists raw material as Inflammable, explosive, toxic and harmful substances, unsafe production, high cost of raw materials, difficult to handle by-products, exhaust emissions and other problems;...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] Into a 1000mL three-necked flask equipped with a stirring and heating device, put 100g of saturated sodium chloride deionized aqueous solution, 60g of flake-shaped sodium hydroxide solid, 75g of sulfur powder, and 100g of deionized water, and heat up to 55°C. React at 70°C until the solid disappears completely, and keep it warm for half an hour to synthesize an aqueous solution of sodium polysulfide. Dissolve 3 g of benzyltriethylammonium chloride phase transfer catalyst in deionized water at room temperature to prepare 10 g of aqueous solution. The aqueous phase transfer catalyst solution was added to the aqueous sodium polysulfide solution. Heat the above solution to 70°C, start to add 250g of chloropropyltriethoxysilane with a purity of 98% dropwise, keep the reaction temperature at 70°C~85°C during the dropwise addition, and keep warm for half an hour after the dropwise addition is completed. Cool down to below 60°C, add 50g of deionized water to the above mixture ...

Embodiment 2

[0057] Into a 1000mL three-necked flask equipped with a stirring and heating device, put 27g of sodium chloride, 60g of flake-shaped sodium hydroxide solid, 38g of sulfur powder, and 175g of deionized water, and heat up to 55°C. React until the solid disappears completely, and keep warm for half an hour to synthesize an aqueous solution of sodium polysulfide. Dissolve 3 g of benzyltriethylammonium chloride phase transfer catalyst in deionized water at room temperature to prepare 10 g of aqueous solution. The aqueous phase transfer catalyst solution was added to the aqueous sodium polysulfide solution. Heat the above solution to 70°C, start to add 250g of chloropropyltriethoxysilane with a purity of 98% dropwise, keep the reaction temperature at 70°C~85°C during the dropwise addition, and keep warm for half an hour after the dropwise addition is completed. Cool down to below 60°C, add 50g of deionized water to the above mixture, stir for 10min, let it stand for 5min, separate ...

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Abstract

The invention provides a method for producing a light-color polysulfide silane coupling agent by an aqueous phase process without a buffer agent. The method specifically comprises the following steps: (a) synthesis of a sodium polysulfide aqueous solution, namely adding sodium chloride, sodium hydroxide, sulfur and deionized water into a reactor, stirring and heating to 50-70 DEG C, reacting until the solid is completely dissolved, and preserving heat; (b) addition of a catalyst, namely adding a phase transfer catalyst aqueous solution into the sodium polysulfide aqueous solution, and mixing uniformly; (c) synthesis of a crude product, namely in a stirring state, adding (3-chloropropyl)triethoxy-silane into the solution, controlling the reaction temperature at 70-85 DEG C, and preserving heat; (d) phase separation, namely separating an organic phase on the upper layer from an aqueous phase on the lower layer in the solution, and removing solids in the organic phase; and (e) decoloration and purification, namely decoloring the treated organic phase solution and purifying by distillation to obtain the light-color polysulfide silane coupling agent. The polysulfide silane coupling agent prepared by the method has the advantages of safety and reliability in production, no polymerization, light color, few impurities, high content of active ingredients and high yield.

Description

Technical field [0001] The present invention involves a production method of a polysulsexilane coupling agent, which is the synthesis of organic chemicals.What's more specifically is a method that does not use a buffer water phase method to produce light polysulsexilane coupling agents. Background technique [0002] Polyohydride Silicine coupling agent is an important auxiliary agent to produce green environmental protection tires. It is widely used in products that are widely used in sulfur sulfurized rubber systems. Through the intercourse of inorganic filler or fiber and rubber matrix, it can achieve improvement of product performance.It is used in tires, especially to improve the friction, rotation resistance and humidity resistance of the tire.At present, the multi -sulfids sulfids Silicine coupling agent sold on the market are generally dark products, which is not conducive to the use of the soles of the light -colored product industry such as the sulfur rubber system. [0...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 陶再山李春华王金勇刘兰香
Owner 南京曙光精细化工有限公司
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