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Method for producing gamma-chloropropyl trichlorosilane

A technology of chloropropyltrichlorosilane and its production method, which is applied in chemical instruments and methods, compounds of group 4/14 elements of the periodic table, metal/metal oxide/metal hydroxide catalysts, etc., and can solve problems affecting products Economic benefits, long reaction initiation period, large amount of catalyst, etc., to achieve the effect of reducing the number of auxiliary raw materials, reducing the cleaning workload, and reducing reaction by-products

Inactive Publication Date: 2011-07-20
郭学阳
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The disadvantage is that the amount of catalyst is large, and the yield is only about 60%
The process has many by-products, cumbersome operation, high requirements on equipment, and low product profit. This process is proposed for the comprehensive utilization of propyl trichlorosilane, a by-product of gamma-chloropropyl trichlorosilane produced from trichlorosilane and chloropropene. A process route with research significance has been established, and there are certain researches at home and abroad
[0012] The above-mentioned production process route of gamma-chloropropyltrichlorosilane with trichlorosilane and chloropropene as raw material has many advantages, but still has the following disadvantages: (1) the reaction initiation period is long; (2) the reaction temperature is higher (3) the total conversion rate of trichlorosilane is generally about 90%; (4) propene chloride generally needs a large amount of excess during the production of feed intake, which increases the burden on the synthesis kettle condensation system and the freezer system, and improves the energy consumption; (5) ) by-product SiCl generated in the reaction 4 The amount of propyltrichlorosilane and propyl trichlorosilane is large, and the post-treatment investment is large, which directly affects the economic benefits of the product; (6) the product purity is low, and the content of high boiling substances (including condensates and polymers) is high; (7) the reaction speed is slow , during the feeding process, the temperature drops or even an abnormal operation that requires a secondary initiation of the reaction occurs, resulting in a prolonged reaction time

Method used

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  • Method for producing gamma-chloropropyl trichlorosilane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 15 grams of Karstedt platinum catalyst to 500 grams of anhydrous isopropanol, stir and dissolve in an iron-free container for 10 minutes to prepare a platinum catalyst solution, and keep it sealed.

[0037] Add 10 grams of chloroplatinic acid into 350 grams of anhydrous isopropanol, stir and dissolve in an iron-free container for 10 minutes to prepare a chloroplatinic acid catalyst solution, and keep it sealed.

[0038]Under the protection of nitrogen, 360 kg of chloropropene was dried in a desiccator, and 600 kg of trichlorosilane was fully mixed with a pipeline static mixer to form a mixed solution, and the mixed solution was pressed into the head tank, and the initial reaction temperature was controlled at 30 ° C. Add 80 kg of mixed solution in the synthesis kettle, then add 40 grams of platinum catalyst solution, when the reaction temperature reaches 55°C, start to add the remaining mixed solution in the head tank evenly from the bottom of the synthesis kettle, a...

Embodiment 2

[0041] Add 20 grams of Karstedt platinum catalyst into 500 grams of anhydrous isopropanol, stir and dissolve in an iron-free container for 15 minutes to prepare a platinum catalyst solution, and keep it sealed.

[0042] Add 15 grams of chloroplatinic acid into 450 grams of anhydrous isopropanol, stir and dissolve in an iron-free container for 15 minutes to prepare a chloroplatinic acid catalyst solution, and keep it sealed.

[0043] Under the protection of nitrogen, 370 kg of chloropropene was dried in a desiccator, and 620 kg of trichlorosilane was fully mixed with a pipeline static mixer to form a mixed solution, and the mixed solution was pressed into the head tank, and the initial reaction temperature was controlled at 35 ° C. Add 110 kg of mixed solution in the synthesis kettle, then add 50 grams of platinum catalyst solution, when the reaction temperature reaches 58°C, start to add the remaining mixed solution in the head tank evenly from the bottom of the synthesis kettl...

Embodiment 3

[0046] Add 25 grams of Karstedt platinum catalyst into 550 grams of anhydrous isopropanol, stir and dissolve in an iron-free container for 15 minutes to prepare a platinum catalyst solution, and keep it sealed.

[0047] Add 15 grams of chloroplatinic acid into 450 grams of anhydrous isopropanol, stir and dissolve in an iron-free container for 15 minutes to prepare a chloroplatinic acid catalyst solution, and keep it sealed.

[0048] Under the protection of nitrogen, 390 kg of chloropropene was dried in a desiccator, and 650 kg of trichlorosilane was fully mixed with a pipeline static mixer to form a mixed solution, and the mixed solution was pressed into the head tank, and the initial reaction temperature was controlled at 40 ° C. Add 120 kg of mixed solution into the synthesis kettle, and then add 60 grams of platinum catalyst solution. When the reaction temperature reaches 60°C, start to add the remaining mixed solution in the head tank from the bottom of the synthesis kettle...

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Abstract

The invention discloses a method for producing gamma-chloropropyl trichlorosilane. The method comprises the following process steps of: forming mixed solution by using chloropropene and trichlorosilane; adding part of platinum catalyst solution into part of the mixed solution; reacting for a period of time, and uniformly adding the residual mixed solution dropwise; reacting the mixed solution with the residual platinum catalyst solution continuously; adding part of chloroplatinic acid catalyst solution and all n-butylamine; reacting for a period of time, and adding the residual chloroplatinicacid catalyst solution; and under the conditions of vacuum degree of more than or equal to 0.096 MPa and gaseous phase temperature on the top of more than or equal to 95 DEG C after the dropping of the residual mixed solution and the reaction are finished, distilling materials to obtain the product gamma-chloropropyl trichlorosilane. In the method, the mixed solution of the raw materials are added into a reaction system uniformly; the reaction catalyst at the early stage and the reaction catalyst at the later stage are added segmentally; initiation and the reaction are performed by stages; the reaction is performed completely; a small number of reaction byproducts are obtained; a reaction conversion rate is high; the purity of the product is improved; and reaction time is shortened.

Description

technical field [0001] The invention relates to the technical field of chemical synthesis, in particular to a production method of gamma-chloropropyltrichlorosilane. Background technique [0002] γ-Chloropropyltrichlorosilane is one of the largest and most widely used γ-substituted propyl silane coupling agents in China. It is one of the most basic monomers in silane coupling agents and can be synthesized as the main raw material Deep processing produces dozens of high-grade silane coupling agent products, such as γ-chloropropyltriethoxysilane, γ-chloropropyltrimethoxysilane, γ-aminopropyltriethoxysilane, rubber additives Si69 and Si75, dental composite resin, silicone antibacterial finishing agent, optical glass antifogging agent, etc. Silane coupling agent is an important type of coupling agent in the coupling agent. As an auxiliary agent commonly used in composite materials, its function is to improve the wettability of the matrix resin to fillers and glass fibers, so th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/12B01J23/42
Inventor 郭学阳张中法郭祥荣
Owner 郭学阳
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