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Synthetic method of thiocyano propyl trialkoxysilane

A technology of thiocyanopropyltrialkoxysilane and chloropropyltrialkoxysilane, which is applied in the field of synthesis of thiocyanopropyltrialkoxysilane, can solve the problem of low product yield and high production cost , environmental pollution and other issues, to achieve the effect of high yield, less catalyst consumption and shortened reaction time

Active Publication Date: 2015-11-18
JINGZHOU JIANGHAN FINE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Compared with bis-[γ-(triethoxysilyl)propyl]tetrasulfide, thiocyanopropyltrialkoxysilane has more stable performance and is not easy to burn rubber, but currently thiocyanopropyl Trialkoxysilane has the disadvantages of high energy consumption, high production cost, and easy environmental pollution in the production process; at the same time, the product yield and quality are low in the market.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 20.00g methanol and 6.00g cetyltrimethylammonium chloride quantitatively to the reactor with thermometer, constant pressure funnel, condenser and magnetic stirring, and the reactor is warmed up to 69°C after feeding under magnetic stirring. ℃ for 2 hours, after the dissolution, first add 6.00g of tetramethylurea to the reactor, stir for 0.5 hours, then drop 20.00g of chloropropyltrimethoxysilane, chloropropyltrimethoxysilane into the reactor through a constant pressure funnel The dropwise addition time of chloropropyltrimethoxysilane was 1 hour. After the dropwise addition of chloropropyltrimethoxysilane was completed, the reaction was continued at 69° C. for 4 hours, and then the temperature was lowered to obtain 51.85 g of catalyst. spare.

[0027] In the reaction vessel with mechanical stirring, drying tower, thermometer, drop into 1180.00g chloropropyltrimethoxysilane, standby catalyst 51.85g and 489.57g sodium thiocyanate successively at a speed of 180 revoluti...

Embodiment 2

[0029] Add 20.00g ethanol and 6.00g cetyltrimethylammonium chloride quantitatively to the reactor with thermometer, constant pressure funnel, condenser and magnetic stirring, and the reactor is warmed up to 70 after feeding under magnetic stirring. ℃ for 1 hour, after the dissolution is complete, first add 6.00g of tetramethylurea to the reactor, and after stirring for 1 hour, add 20.00g of chloropropyltriethoxysilane, chloropropyltriethoxysilane dropwise to the reactor through a constant pressure funnel. The dropwise addition time of ethoxysilane was 2 hours. After the dropwise addition of chloropropyltriethoxysilane was completed, the reaction was continued at 70° C. for 4 hours, and then the temperature was lowered to obtain 51.78 g of catalyst. spare.

[0030] In the reaction vessel with mechanical stirring, drying tower and thermometer, 1180.00g chloropropyltriethoxysilane, spare catalyst 51.78g and 404.02g sodium thiocyanate are successively dropped into at the speed of ...

Embodiment 3

[0032] In the reactor with thermometer, constant pressure funnel, condenser and magnetic stirring, quantitatively add 20.00g isopropanol and 6.00g cetyltrimethylammonium chloride, after feeding under magnetic stirring, the reactor is warmed up to Dissolve at 71°C for 2 hours. After the dissolution is complete, first add 6.00g of tetramethylurea to the reactor, and after stirring for 0.5 hours, add 20.00g of chloropropyltriisopropoxysilane, chloropropyl The dropwise addition time of triisopropoxysilane was 1 hour. After the dropwise addition of chloropropyltriisopropoxysilane was completed, the reaction was continued at 71° C. for 4 hours, and then the temperature was lowered to obtain 51.87 g of catalyst. spare.

[0033]In the reaction vessel with mechanical stirring, drying tower and thermometer, drop into 1180.00g chloropropyltriisopropoxysilane, 51.87g and 343.92g sulfur catalysts for the above synthesis successively at a speed of 180 revolutions per minute under mechanical...

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PUM

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Abstract

The invention relates to a synthetic method of thiocyano propyl trialkoxysilane, which belongs to the field of organic chemistry. According to the invention, a self-made catalyst is employed, chloropropyltrialkoxysilane and sodium sulfocyanate are used for synthesis of thiocyano propyl trialkoxysilane and common salt under certain reaction condition, filter residue of common salt can be filtered and separated, the filter residue is washed by a corresponding alcoholic solution, the washing lotion recovers the corresponding alcohol under normal pressure, and is distilled with crude product to obtain the thiocyano propyl trialkoxysilane product. The thiocyano propyl trialkoxysilane product has the characteristics of high quality, good stability, little impurity, no waste material discharge, no environmental pollution, and easy industrial production.

Description

technical field [0001] The invention relates to a synthesis method of thiocyanopropyltrialkoxysilane, which belongs to the field of organic chemistry. Background technique [0002] As a new type of high-tech material, silicone has been widely used in electronics, electrical appliances, aviation, aerospace, construction, textiles, medicine, daily chemicals and other fields since its industrial production in the early 1940s. New materials that are indispensable for improving living standards. Thiocyanopropyltrialkoxysilane is used as a silane coupling agent for sulfur vulcanized rubber compounds filled with non-black fillers (such as clay or white carbon black), which can significantly improve the physical and processing properties of rubber. Among them, the improvement of physical properties is based on the fact that thiocyanatopropyltrialkoxysilane can chemically bond the filler to the base rubber; the improvement of processing performance is due to the fact that thiocyanat...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 秦传俊胡江华陈圣云甘俊甘书官
Owner JINGZHOU JIANGHAN FINE CHEM
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