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Device and method for preparing high-purity gamma-chloropropyl trichlorosilane

A technology of chloropropyltrichlorosilane and propyltrichlorosilane, which is applied in the field of equipment for preparing high-purity γ-chloropropyltrichlorosilane, and can solve the problems of high energy consumption, high operation precision, and excessive distillation still residue and other problems, to achieve the effect of reducing the difficulty of operation, high operation accuracy, and reducing the residual liquid in the kettle

Active Publication Date: 2021-01-05
INST OF PROCESS ENG CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing technology belongs to the traditional batch rectification, which mainly has the following disadvantages: the whole tower is a rectification section during intermittent rectification, and there is no stripping section, which requires high operation precision and has a great impact on the product; during batch rectification, the feed liquid is in the kettle Excessive heating time at high temperature will result in too much residue in the rectification kettle of γ-chloropropyl trichlorosilane, low rectification yield and high consumption
This method has the following disadvantages: during rectification, the entire tower is a rectification section, and there is no stripping section, which requires high operating precision and has a great impact on product quality; during rectification, the feed liquid is heated in the kettle for too long, which will cause γ- Chloropropyltrichlorosilane rectification still has too much residue, low rectification yield and high consumption; single tower rectification yield is low, energy consumption is large, and production cost is high

Method used

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  • Device and method for preparing high-purity gamma-chloropropyl trichlorosilane
  • Device and method for preparing high-purity gamma-chloropropyl trichlorosilane
  • Device and method for preparing high-purity gamma-chloropropyl trichlorosilane

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Experimental program
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Effect test

Embodiment 1

[0059] In this embodiment, the mass composition after the reaction of chloropropene and trichlorosilane is: 4.31% of chloropropene, 4.31% of trichlorosilane, 15.05% of silicon tetrachloride, 6.33% of propyl trichlorosilane, γ-chlorine Propyltrichlorosilane 69.5%, high boiler 0.5%.

[0060] Further, the reflux ratio of pre-separation rectification tower 1 is R=3, the operating pressure is 900kPa, and the number of theoretical plates is 30.

[0061] Further, the silicon tetrachloride removal tower 2 has a reflux ratio of R=7, an operating pressure of 260kPa, and a theoretical plate number of 30.

[0062] Further, the reflux ratio of the propyltrichlorosilane removal tower 3 is R=13, the operating pressure is 40kPa, and the number of theoretical plates is 30.

[0063] Further, the reflux ratio of the secondary rectification column 4 is R=125, the operating pressure is 40kPa, and the number of theoretical plates is 20.

[0064] Further, the γ-chloropropyltrichlorosilane removal ...

Embodiment 2

[0068] In this embodiment, the mass composition after the reaction of chloropropene and trichlorosilane is the same as that in Embodiment 1.

[0069] Further, the reflux ratio of pre-separation rectification tower 1 is R=3, the operating pressure is 900kPa, and the number of theoretical plates is 30.

[0070] Further, the silicon tetrachloride removal tower 2 has a reflux ratio of R=7, an operating pressure of 260kPa, and a theoretical plate number of 30.

[0071] Further, the reflux ratio of the propyltrichlorosilane removal tower 3 is R=13, the operating pressure is 40kPa, and the number of theoretical plates is 30.

[0072] Further, the reflux ratio of the secondary rectification column 4 is R=125, the operating pressure is 40kPa, and the number of theoretical plates is 20.

[0073] Further, the γ-chloropropyltrichlorosilane removal tower 5 has a reflux ratio of R=1, an operating pressure of 80 kPa, and a theoretical plate number of 30.

[0074] Further, the reflux ratio ...

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Abstract

The invention provides a method for preparing high-purity gamma-chloropropyl trichlorosilane, which comprises the following steps: 1, feeding a mixture obtained after trichlorosilane and chloropropenereact into a pre-separation rectifying tower, and carrying out rectification separation; 2, feeding a tower top material of the pre-separation rectifying tower into a silicon tetrachloride removing tower; 3, feeding a tower bottom material of the pre-separation rectifying tower into a propyl trichlorosilane removing tower, obtaining propyl trichlorosilane with the purity of more than or equal to99.5% at the top of the tower, and feeding the tower bottom material into a secondary rectifying tower; 4, enabling the tower top material of the secondary rectifying tower in the step 3 to flow backto the propyl trichlorosilane removal tower, and enabling the tower bottom material to enter a gamma-chloropropyl trichlorosilane removal tower; 5, feeding the tower bottom material into a product recovery tower; and 6, enabling the tower top material of the product recovery tower in the step 5 to flow back to the gamma-chloropropyl trichlorosilane removal tower, obtaining a high-boiling-point substance at the tower bottom, and periodically discharging the high-boiling-point substance. According to the whole technological process, heat in the rectification system is fully utilized, and consumption of steam and cooling water is reduced.

Description

technical field [0001] The invention relates to the technical field of chloropropyltrichlorosilane production, in particular to a device and method for preparing high-purity gamma-chloropropyltrichlorosilane. Background technique [0002] At present, the method for separating the raw material liquid after the reaction of chloropropene and trichlorosilane mainly adopts distillation and three rectification methods to extract propyl trichlorosilane and γ-chloropropyl trichlorosilane fractions from the mixed liquid, and first adopts distillation fractionation Obtain three crude fractions of silicon tetrachloride, propyltrichlorosilane and γ-chloropropyltrichlorosilane, and then use three rectifications to refine silicon tetrachloride, propyltrichlorosilane and γ-chloropropyltrichlorosilane respectively Fractions, above 99% silicon tetrachloride fraction, above 98% propyl trichlorosilane fraction and 99% γ-chloropropyl trichlorosilane fraction can be obtained respectively. The e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/12C07F7/20C01B33/107
CPCC07F7/122C07F7/20C01B33/1071C01B33/10778
Inventor 华超白芳陆平聂佳斌甘维俊杰甘维俊
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI