Method for preparing gamma-chloropropyl trichlorosilane by multicomponent compound catalysis

A technology of chloropropyltrichlorosilane and trichlorosilane, applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, etc., can solve the problem of low trichlorosilane content, Scientific research and production loss, low conversion rate of raw materials and other problems, to achieve the effect of increasing product content, improving production and operation conditions, and wide application range

Inactive Publication Date: 2010-01-13
青岛中科荣达新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And the present existing technique main productive rate is all lower than 85%; And has following deficiency: (1) production cycle is long; (2) raw material (calculated as trichlorosilane) conversion rate is low, and product yield is low; (3) ) many side reactions, the finished product γ-chloropropyl trichlorosilane has low content and high impurity content
[0006] 1. Product content problem The content of products prepared by the existing production process is generally lower than 99%. In many special use occasions, due to the different use environments and conditions, customers hope that the content is at least higher than 99%. The downstream of some special purposes Product users require that the content of γ-chloropropyltrichlorosilane be greater than 99.5%;
[0007] 2. Product appearance problems Most of the existing products are light yellow or slightly yellow liquid, some manufacturers' products are brown or brownish yellow, and some products have fine suspended matter or sediment, which directly affects the use of the product;
[0008] 3. The problem of product impurities. Some special-purpose products, such as catalyst carriers or catalysts, are synthesized from γ-chloropropyltrichlorosilane. The quality indicators such as the structure and content of impurities are extremely strict. Serious consequences such as poisoning, deactivation or even unusability of the synthesized catalyst will cause losses to scientific research and production;
[0009] 4. Product yield problem The current yield of γ-chloropropyltrichlorosilane is only about 80%. If the yield can be improved by adjusting the production process, the economic and social benefits of the product will be quite objective;

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037]The method for preparing gamma-chloropropyltrichlorosilane of the present invention comprises the steps of:

[0038] 1 Preparation of production aids

[0039] (1) Catalyst preparation Dissolve 25 g of chloroplatinic acid in 510 ml of anhydrous isopropanol, stir well, then add 510 ml of tetrahydrofuran, stir evenly and set aside.

[0040] (2) Co-catalyst preparation Weighed 11.5 g of m-phenylenediamine and 17 g of tributylamine respectively, added them into 520 ml of anhydrous isopropanol, and stirred them well in a container without iron medium to mix them evenly.

[0041] (3) Catalyst activator preparation Weigh 70 g of triisopropanolamine and 24 g of 2,4-pentanedione into 400 ml of anhydrous isopropanol, stir well and mix well in a container without iron medium.

[0042] (4) Inhibitor preparation Weigh 65 g of resorcinol and 40 g of diethylhydroxylamine respectively, add them into 450 ml of anhydrous isopropanol, and stir well and mix them evenly in a container withou...

Embodiment 2

[0061] The method for preparing gamma-chloropropyl trichlorosilane, comprises the steps:

[0062] 1 Preparation of production aids

[0063] (1) Catalyst preparation Dissolve 26 g of chloroplatinic acid in 520 ml of anhydrous isopropanol, stir well, then add 510 ml of tetrahydrofuran, stir well and set aside.

[0064] (2) Co-catalyst preparation Weighed 15 grams of m-phenylenediamine and 18 grams of tributylamine, respectively, and added them to 500 ml of anhydrous isopropanol, and stirred thoroughly and evenly in an iron-free container.

[0065] (3) Catalyst activator preparation Weigh 75 g of triisopropanolamine and 25 g of 2,4-pentanedione into 400 ml of anhydrous isopropanol, stir well and mix evenly in an iron-free container.

[0066] (4) Inhibitor preparation Weigh 80 grams of resorcinol and 40 grams of diethylhydroxylamine respectively, add them to 500 ml of anhydrous isopropanol, and stir well in an iron-free container to mix evenly.

[0067] 2 Hydrosilylation

[006...

Embodiment 3

[0085] 1 Preparation of production aids

[0086] (1) Catalyst preparation Dissolve 25 g of chloroplatinic acid in 500 ml of anhydrous isopropanol, stir well, then add 520 ml of tetrahydrofuran, stir evenly and set aside.

[0087] (2) Co-catalyst preparation Weigh 15 grams of m-phenylenediamine and 20 grams of tributylamine respectively, add them to 500 ml of anhydrous isopropanol, and stir them well in a container without iron medium.

[0088] (3) Catalyst activator preparation Weigh 90 g of triisopropanolamine and 30 g of 2,4-pentanedione into 450 ml of anhydrous isopropanol, stir well and mix evenly in a container without iron medium.

[0089] (4) Inhibitor preparation Weigh 85 grams of resorcinol and 45 grams of diethylhydroxylamine respectively, add them to 500 ml of anhydrous isopropanol, and stir them well in a container without iron medium.

[0090] 2 Hydrosilylation

[0091] (1) 750 kilograms of trichlorosilanes and 550 kilograms of chloropropenes that have been insp...

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Abstract

The invention discloses a method for preparing gamma-chloropropyl trichlorosilane by multicomponent compound catalysis, which adopts trichlorosilane and chloropropene as main raw materials to synthesize the gamma-chloropropyl trichlorosilane; besides chloroplatinic acid is taken as main catalyst, the reaction system is also added with alicyclic amine and phenylene diamines compound which are taken as cocatalyst, triisopropanolamine and 2, 4-pentandione that are taken as activator, as well as resorcinol and diethyl hydroxylamine that are used as inhibitor; after hydrosilylation, the finished product is obtained by distillation and rectification. The method can greatly increase the content of the produced product, improve the appearance of the product, reduce impurities of the product, improve the quality of the product and lower the production cost.

Description

technical field [0001] The invention belongs to the field of chemical synthesis, in particular to a method for preparing a silane coupling agent. Background technique [0002] Silane coupling agent is the fourth major category after the three major products in the silicone industry - silicone oil, silicone rubber, and silicone resin. Its position in the silicone industry is becoming increasingly important and has become a modern silicone industry. It is an indispensable supporting chemical additive in molecular industry, composite material industry and related high-tech fields, and it is an important high-tech content and high value-added silicone product. [0003] Coupling agent is a kind of substance with two different functional groups. Part of the functional groups in their molecules can react with organic molecules, and the other part of the functional groups can react with the adsorbed water on the surface of inorganic substances to form a strong bond. The role of the...

Claims

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Application Information

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IPC IPC(8): C07F7/12C07F7/20B01J31/28B01J31/02
Inventor 张中法黄慧吕彩玲丁爱梅郭学阳张庆国
Owner 青岛中科荣达新材料有限公司
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