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Method of continuous concentrated acid hydrolysis of organochlorosilane

A hydrolysis technology of organochlorosilane and concentrated acid, which is applied in the direction of silicon organic compounds, can solve the problems of difficult control of hydrolyzate viscosity, achieve stable and controllable quality, reduce water consumption, and increase residence time

Active Publication Date: 2013-07-03
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Moreover, the crude product is treated with steam, and the viscosity of the hydrolyzate is finally difficult to control

Method used

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  • Method of continuous concentrated acid hydrolysis of organochlorosilane

Examples

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Effect test

Embodiment 1

[0033]Example 1: Dimethyldichlorosilane and concentrated acid enter the hydrolysis reactor 1 for hydrolysis reaction. The molar ratio of water to dimethyldichlorosilane in the reaction system is 5:1, and the water source comes from the hydrolyzed oligosiloxane In the water washing process, the concentrated acid is recycled between the hydrolysis reactor 1 and the falling film evaporator 3 . The reaction temperature is controlled at 30°C, the operating pressure is 0.4MPa, and the residence time is 60s. The volume ratio of water to oligosiloxane is 0.5:1, the operating temperature is 55°C, and the operating pressure is 0.1MPa for the first two stages of series washing. The volume ratio of dilute lye to oligosiloxane is 8:1 for alkali cleaning, the operating temperature is 55°C, and the operating pressure is 0.1MPa. The volume ratio of water to oligosiloxane is 1:1, the operating temperature is 70°C, and the operating pressure is 0.1MPa for the last two-stage series washing. Th...

Embodiment 2

[0034] Example 2: Dimethyldichlorosilane and concentrated acid enter the hydrolysis reactor for hydrolysis reaction, the molar ratio of water to dimethyldichlorosilane in the reaction system is 10:1, and the water source comes from the hydrolyzate oligosiloxane washing In the process, the concentrated acid is recycled between the hydrolysis reactor and the falling film evaporator. The reaction temperature is controlled at 20°C, the operating pressure is 0.3MPa, and the residence time is 90s. The volume ratio of water to oligosiloxane is 2:1, the operating temperature is 75°C, and the operating pressure is 0.2MPa for the first two stages of series washing. The volume ratio of dilute lye to oligosiloxane is 6:1 for alkali cleaning, the operating temperature is 65°C, and the operating pressure is 0.1MPa. The volume ratio of water to oligosiloxane is 1:1, the operating temperature is 60°C, and the operating pressure is 0.3MPa for the last two-stage series washing. The specificat...

Embodiment 3

[0035] Example 3: Dimethyldichlorosilane and concentrated acid enter the hydrolysis reactor for hydrolysis reaction, the molar ratio of water to dimethyldichlorosilane in the reaction system is 15:1, and the water source comes from the hydrolyzate oligosiloxane washing In the process, the concentrated acid is recycled between the hydrolysis reactor and the falling film evaporator. The reaction temperature is controlled at 40°C, the operating pressure is 0.2MPa, and the residence time is 1200s. The volume ratio of water to oligosiloxane is 3:1, the operating temperature is 60°C, and the operating pressure is 0.1MPa for the first two stages of series washing. The volume ratio of dilute lye to oligosiloxane is 4:1 for alkali cleaning, the operating temperature is 60°C, and the operating pressure is 0.2MPa. The volume ratio of water to oligosiloxane is 3:1 for the last two-stage series washing, the operating temperature is 70°C, and the operating pressure is 0.2MPa. The specific...

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Abstract

The invention relates to a method of continuous concentrated acid hydrolysis of organochlorosilane. The method comprises the following steps: step 1, the organochlorosilane is subject to hydrolysis reaction with a concentrated acid in a hydrolysis reactor to produce a hydrochloric acid with higher concentration, and a crude hydrolysate; step 2, after the liquid produced after hydrolysis reaction is separated through a preliminary separator, the concentrated acid enters a falling-film evaporator to generate HCL (hydrogen chloride) gas for production of methyl chloride through heat exchange; the concentrated acid at the tower bottom enters the hydrolysis reactor for cyclic use; the oil phase separated by the preliminary separator enters a primary phase separator and a secondary phase separator, the separated acid liquor returns to the hydrolysis reactor for cyclic use, and the oil phase enters the subsequent water washing procedure; and step 3, the two-stage series water-washing and the phase separation are carried out to the oil phase in the water washing procedure, then the recycle washing with a dilute alkali lye and the phase separation are carried out, and finally, the latest two-stage series water-washing and the phase separation are carried out; and the washed oil phase is a siloxane oligomer.

Description

technical field [0001] The invention relates to the technical field of organosilicon production, in particular to a process for generating oligosiloxane and anhydrous hydrogen chloride by continuous concentrated acid hydrolysis of organochlorosilane. Background technique [0002] Organochlorosilanes are transformed into linear or cyclic intermediate oligomeric organosiloxanes through hydrolysis and polycondensation, which are the basis for the synthesis of silicone oil, silicone rubber, and silicone resin. In particular, dimethyldichlorosilane (hereinafter referred to as dimethyl) is considered to be the most suitable for hydrolysis and condensation reactions. [0003] At present, most domestic dimethyl hydrolysis adopts azeotropic acid hydrolysis process. Since the product hydrogen chloride dissolves in the dilute acid, a large amount of heat is released. In order to keep the reaction temperature within the requirements of the process conditions, the heat needs to be remov...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/34C07F7/21C07F7/08
Inventor 李建隆王伟文段继海仇汝臣韩鑫凤
Owner QINGDAO UNIV OF SCI & TECH
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