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Method for reducing acid content of dimethyldichlorosilane hydrolysate

A technology of dimethyldichlorosilane and hydrolyzate, applied in the direction of silicon organic compounds, etc., can solve the problem of difficulty in stabilizing and controlling the viscosity of dimethyldichlorosilane, and achieve the effect of avoiding emulsification, improving effect and reducing production load.

Active Publication Date: 2017-02-15
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] The dimethyl hydrolyzate (grade 1) and the calcium chloride aqueous solution with a mass fraction of 10% (N grade, N≥3) are mixed and washed in countercurrent at a mass ratio of 1:1, and the hydrolyzate and hydrochloric acid are continuously reduced in the water phase contact, and extensive washing to reduce the amount of residual acid in the final product. Among them, the temperature during washing is controlled at 70°C, and the feed rate of hydrolyzate is 6m 3 / h, water replenishment rate 3.5m 3 / h, after the hydrolyzate is mixed with calcium chloride-hydrochloric acid and washed, the upper layer of hydrolyzate is separated by overflow, and the lower layer of calcium chloride-hydrochloric acid solution is returned to the upper-level water washing system to wash the hydrolyzate, and finally the calcium chloride contained in the acid water passes through It is removed by falling film evaporation and returned to the system for recycling. After treatment, the acidity of...

Embodiment 2

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

Embodiment 3

[0026] The dimethyl hydrolyzate (grade 1) and the calcium chloride aqueous solution with a mass fraction of 20% (N grade, N≥3) are mixed and washed in countercurrent at a mass ratio of 2:1, and the hydrolyzate and the hydrochloric acid mass fraction are continuously reduced contact, and extensive washing to reduce the amount of residual acid in the final product. Among them, the temperature during washing is controlled at 90°C, and the feed rate of hydrolyzate is 7m 3 / h, water replenishment rate 4.5m 3 / h, after the hydrolyzate is mixed with calcium chloride-hydrochloric acid and washed, the upper layer of hydrolyzate is separated by overflow, and the lower layer of calcium chloride-hydrochloric acid solution is returned to the upper-level water washing system to wash the hydrolyzate, and finally the calcium chloride contained in the acid water passes through It is removed by falling film evaporation and returned to the system for recycling. After treatment, the acidity of ...

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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 acid content in dimethyldichlorosilane hydrolyzate, which belongs to the field of chemical industry. Background technique [0002] At present, there are two main hydrolysis processes for organosilicon monomer dimethyldichlorosilane (dimethyldichlorosilane for short): azeotropic acid hydrolysis and concentrated acid hydrolysis. Domestically, the azeotropic acid hydrolysis method is the main method, and the specific process is as follows: Add dimethylformamide and 18-22wt% azeotropic hydrochloric acid in a certain proportion to the hydrolysis loop system composed of the heat exchanger and acid-resistant pipelines that provide cooling capacity by the hydrolysis circulating pump In the process, the hydrolyzate is physically separated, and the upper oil phase is neutralized to remove acid, washed with water to remove salt, and the finished hydrolyzate is obtained. Compared with the azeotropic acid hydrolysis p...

Claims

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Application Information

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Patent Type & Authority Applications(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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