A method for reducing acid content in dimethyldichlorosilane hydrolyzate

A technology of dimethyldichlorosilane and hydrolyzate, applied in the direction of silicon organic compounds, etc., can solve the problems of difficulty in stabilizing and controlling the viscosity of dimethyldichlorosilane, and achieve the advantages of avoiding emulsification, increasing specific gravity and reducing production load. Effect

Active Publication Date: 2018-11-09
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The shortcomings of the alkali neutralization method are obvious; the adsorption method may introduce some mechanical impurities that cannot be removed, and there are certain problems in the continuous implementation; the steam treatment method is difficult to stabilize and control the viscosity of the dimethyl hydrolyzate due to the high temperature operation

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] Mix dimethyl hydrolysate (level 1) and 10% calcium chloride aqueous solution (level N, N≥3) with a mass ratio of 1:1 in countercurrent washing, and the hydrolysate and hydrochloric acid are successively reduced in mass fraction Contact and wash thoroughly to reduce the residual acid content in the final product. Among them, the temperature during washing is controlled to 70℃, and the feed rate of hydrolysate is 6m 3 / h, water supplement rate 3.5m 3 / h, after the hydrolysate is mixed and washed with calcium chloride-hydrochloric acid, the upper layer of hydrolysate is separated by overflow, and the lower layer of calcium chloride-hydrochloric acid solution is returned to the upper level washing system to wash the hydrolysate, and finally the calcium chloride contained in the acid water passes The falling film is removed by evaporation and returned to the system for recycling. After treatment, the acidity of dimethyl hydrolysate is reduced from the original 8-10ppm to 4-5p...

Embodiment 2

[0024] The dimethyl hydrolyzate (level 1) and the 15% mass fraction of calcium chloride aqueous solution (level N, N≥3) are mixed and washed in countercurrent at a mass ratio of 1.5:1, and the hydrolyzate and hydrochloric acid are successively reduced in mass fraction. Contact and wash thoroughly to reduce the residual acid content in the final product. Among them, the temperature during washing is controlled to 80℃, and the feed rate of hydrolysate is 6.5m 3 / h, water supplement rate 4m 3 / h, after the hydrolysate is mixed and washed with calcium chloride-hydrochloric acid, the upper layer of hydrolysate is separated by overflow, and the lower layer of calcium chloride-hydrochloric acid solution is returned to the upper level washing system to wash the hydrolysate, and finally the calcium chloride contained in the acid water passes The falling film is removed by evaporation and returned to the system for recycling. After treatment, the acidity of the dimethyl hydrolyzate is re...

Embodiment 3

[0026] Mix dimethyl hydrolysate (level 1) and 20% calcium chloride aqueous solution (level N, N≥3) with a mass ratio of 2:1 in countercurrent washing. The hydrolysate and hydrochloric acid are successively reduced in mass fraction Contact and wash thoroughly to reduce the residual acid content in the final product. Among them, the temperature during washing is controlled to 90℃, and the feed rate of hydrolysate is 7m 3 / h, water supplement rate 4.5m 3 / h, after the hydrolysate is mixed and washed with calcium chloride-hydrochloric acid, the upper layer of hydrolysate is separated by overflow, and the lower layer of calcium chloride-hydrochloric acid solution is returned to the upper level washing system to wash the hydrolysate, and finally the calcium chloride contained in the acid water passes The falling film is removed by evaporation and returned to the system for recycling. After treatment, the acidity of the dimethyl hydrolyzate is reduced from the original 8-10ppm to 5-7p...

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Abstract

Belonging to the field of chemical engineering, the invention relates to a method for reducing the acid content of a dimethyldichlorosilane hydrolysate. The method includes the steps of: (a) subjecting the dimethyldichlorosilane hydrolysate and a calcium chloride aqueous solution to countercurrent mixing and washing; (b) then continuously contacting the hydrolysate with a hydrochloric acid mass fraction gradually reduced aqueous phase, and performing full washing. On the basis of washing, the method provided by the invention introduces calcium chloride to increase the proportion of the hydrolysate and water, realizes rapid layering of the two, avoids emulsification phenomenon during washing, and improves the washing and acid removing effects. In addition, the method provided by the invention significantly reduces the consumption of washing water and lowers the production load, and the calcium chloride can be recycled, thus achieving green and clean production.

Description

Technical field [0001] The invention relates to a method for reducing the acid content in dimethyldichlorosilane hydrolysate, and belongs to the chemical industry field. Background technique [0002] At present, there are two main hydrolysis processes for organosilicon monomer dimethyldichlorosilane (dimethyl): constant boiling acid hydrolysis and concentrated acid hydrolysis. The domestic azeotropic acid hydrolysis method is the main method. The specific process is as follows: add dimethyl and 18-22wt% azeotropic hydrochloric acid in a certain proportion to the hydrolysis loop system composed of the heat exchanger provided by the hydrolysis circulation pump and the acid-resistant pipeline. In the process, the hydrolyzed product is physically stratified, and the upper oil phase is neutralized to remove acid, washed with water to remove salt, and the finished hydrolysate is obtained. Compared with the azeotropic acid hydrolysis process, the main difference of the concentrated aci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/20
CPCC07F7/20
Inventor 伊港周玲周磊张海雷张帅
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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