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The method for producing light-colored polysulfide silane coupling agent without buffering agent

A technology of silane coupling agent and polysulfide, which is applied in the production field of polysulfide silane coupling agent, can solve the problem of buffer product quality, by-product treatment and unfavorable raw material input, many types of impurities, high content, poisonous and harmful Substance and other issues, to reduce the possibility of introducing colored ion substances, reduce raw material input, and reduce the effect of product polymerization

Active Publication Date: 2016-08-17
南京曙光新材料有限公司
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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; the second is the aqueous phase method, such as using alkali metal sulfide or hydrogen sulfide, Water, buffering agent, etc. are used as raw materials. The raw materials of this method are alkali metal sulfides or hydrogen sulfides. Most of the products in the domestic market are produced by mirabilite ore or liquid alkali absorption liquid process. There are many types of impurities and high content, and the quality is uncontrollable. , and the number of manufacturers is limited, the quality of the downstream polysulfide silane coupling agent cannot be guaranteed, and the existence of the buffer is not good for the quality of the product, the treatment of by-products and the input of raw materials.

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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PUM

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Abstract

The invention provides a method for producing light-colored polysulfide silane coupling agent without buffering agent aqueous phase method, the specific steps are as follows: a. Synthesis of sodium polysulfide aqueous solution: sodium chloride, sodium hydroxide, sulfur and deionized Add water into the reactor, stir and heat up to 50°C-70°C, react until the solid is completely dissolved, and keep warm; b. Add catalyst: add the phase transfer catalyst aqueous solution to the sodium polysulfide aqueous solution and mix well; c. Synthesis of crude product: Under stirring, add chloropropyltriethoxysilane to the above solution, control the reaction temperature at 70°C-85°C, and keep it warm; d. Phase separation: separate the upper organic phase and the lower aqueous phase in the above solution , and remove the solids in the organic phase; e. Decolorization and purification: decolorize the organic phase solution after the above treatment and then purify it by distillation to obtain a light-colored polysulfide silane coupling agent. The invention can obtain the polysulfide silane coupling agent with safe and reliable production, no polymerization, light color, less impurities, high active ingredient content and high yield.

Description

technical field [0001] The invention relates to a production method of a polysulfide silane coupling agent, which belongs to the synthesis of organic chemicals. More specifically, it is a method for producing a light-colored polysulfide silane coupling agent by an aqueous phase method without using a buffer. Background technique [0002] Polysulfide silane coupling agent is an important auxiliary agent for the production of green tires. It is widely used in the products of sulfur vulcanized rubber system. It can improve the performance of products by coupling inorganic fillers or fibers with rubber matrix. Used in tires, especially to improve the friction resistance, rolling resistance and wet skid resistance of tires. The polysulfide silane coupling agents currently on the market are generally dark-colored products, which are not conducive to the use in light-colored product industries such as shoe soles of vulcanized rubber systems. [0003] The current large-scale indus...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 陶再山李春华王金勇刘兰香
Owner 南京曙光新材料有限公司
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