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Method for hydrolyzing organochlorosilane

A technology of organochlorosilane and polysiloxane, which is applied in the field of organochlorosilane continuous hydrolysis to prepare organopolysiloxane and organochlorosilane hydrolysis. Purity and other issues

Active Publication Date: 2011-09-07
SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method of this patent document has the following deficiencies: on the one hand, the hydrogen chloride gas formed is greater than the saturation amount in water under its hydrolysis conditions. Although hydrogen chloride is recovered and energy consumption is reduced, the gas phase hydrogen chloride escaped inhibits hydrolysis or will form hydrolyzate Partial cracking, resulting in incomplete hydrolysis, requires subsequent secondary hydrolysis to complete hydrolysis; on the other hand, the escaped hydrogen chloride comes from the hydrolysis system, and the temperature of hydrogen chloride is consistent with the hydrolysis temperature, resulting in incompletely hydrolyzed chlorosilane and volatile The hydrolyzate is easily carried out
But there are following deficiencies: one, the circulating acid water flow rate is too large; two, the organochlorosilane hydrolyzate is decompressed and decompressed with the acid water and the temperature change is small after decompression, causing the gas phase hydrogen chloride to crack the hydrolyzate and carry the material seriously, Cause incomplete hydrolysis and impurity of hydrogen chloride gas; Third, the strong stirring and pressurization of the pump cannot be used to promote the rapid hydrolysis of organochlorosilanes
However, the highest concentration of acidic water is lower than or close to the highest solubility of hydrogen chloride at normal temperature and pressure, without considering the possibility that the increase in the solubility of hydrogen chloride can allow higher concentrations of acid to be hydrolyzed under pressurized conditions

Method used

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  • Method for hydrolyzing organochlorosilane
  • Method for hydrolyzing organochlorosilane
  • Method for hydrolyzing organochlorosilane

Examples

Experimental program
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Effect test

Embodiment 1

[0064] The organochlorosilane is trimethylchlorosilane, the amount of trimethylchlorosilane added to the hydrolysis system per hour is 0.670t, the amount of water added to the hydrolysis system per hour is 0.056t, and the amount of circulating acid water entering the hydrolysis system per hour is 1.089 t, the hydrolysis temperature is controlled at 40°C, the hydrolysis pressure is controlled at an absolute pressure of 1.10MPa, and the flow rate of the circulation pump of the hydrolysis system is 50m per hour 3 , hydrolysis produces high concentration (mass concentration is about 54%) unsaturated acid water and hexamethyldisiloxane; adjust the internal heat exchange system of the hydrolysis system and the desorption kettle, under the desorption pressure is an absolute pressure of 0.10MPa, The elution temperature was controlled at 0°C. The circulation ratio is (50-1.815) / 1.815; the high-concentration unsaturated acid water and hexamethyldisiloxane are overflowed into the seconda...

Embodiment 2

[0066] The organochlorosilane is a mixture of dimethylhydrochlorosilane and trimethylchlorosilane with a molar ratio of 75:2. The amount of organochlorosilane added to the hydrolysis system per hour is 0.948t, and the amount of water added to the hydrolysis system per hour is 0.147t. The amount of circulating acid water entering the hydrolysis system per hour is 3.769t, the hydrolysis temperature is controlled at 25°C, the hydrolysis pressure is controlled at an absolute pressure of 1.10MPa, and the flow rate of the circulation pump of the hydrolysis system is 50m per hour 3 , hydrolysis produces high concentration (calculation result is about 53%) unsaturated acid water and polymethylhydrogen siloxane; adjust the internal heat exchange system of the hydrolysis system and the desorption kettle, under the desorption pressure is an absolute pressure of 0.10MPa, The elution temperature was controlled at -10°C. The high-concentration unsaturated acid water and polymethylhydrogensi...

Embodiment 3

[0068] The organochlorosilane is selected from dimethyldichlorosilane, the amount of dimethyldichlorosilane added to the hydrolysis system per hour is 0.872t, the amount of water added to the hydrolysis system per hour is 0.122t, and the amount of circulating acid water entering the hydrolysis system per hour is 2.385t, the hydrolysis temperature is controlled at 40°C, the hydrolysis pressure is controlled at an absolute pressure of 1.10MPa, and the flow rate of the circulation pump of the hydrolysis system is 50m per hour 3 , hydrolysis produces high concentration (calculated result is about 53%) unsaturated acid water and dimethyl dichlorosilane hydrolyzate; adjust the internal heat exchange system of the hydrolysis system and the desorption kettle, and the desorption pressure is under the absolute pressure of 0.10MPa , so that the elution temperature was controlled at 0°C. The high-concentration unsaturated acid water and dimethyldichlorosilane hydrolyzate overflow into the...

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Abstract

The invention relates to a method for hydrolyzing organochlorosilane, which is a process for continuously preparing polysiloxane by changing the solubility of hydrogen chloride in a pressure increasing and reducing mode. The method comprises the following steps of: hydrolyzing the organochlorosilane and water in a stoichiometric ratio, and low-concentration saturated circulating acid water under the pressure increasing condition to obtain high-concentration unsaturated acid water and the polysiloxane; adding the high-concentration unsaturated acid water and the polysiloxane, which are needed to be desorbed, in a hydrolysis system into a second-stage phase separator through a first-stage phase separator, and continuously circulating the residual high-concentration unsaturated acid water in the hydrolysis system; separating on the top of the second-stage phase separator to obtain the polysiloxane, and adding the acid water at the bottom into a pressure reducing desorption kettle to obtain hydrogen chloride gas and low-concentration saturated acid water; and making the low-concentration saturated acid water return to the hydrolysis system for recycling. The organochlorosilane and the water are continuously added into the system, the hydrogen chloride and the polysiloxane are obtained, a large amount of hydrogen chloride gas is recycled, oil-containing acid water is recycled, and the method has the characteristics that the method is energy-saving, economic and environment-friendly.

Description

technical field [0001] The invention relates to a method for hydrolyzing organochlorosilanes, in particular to a method for continuously hydrolyzing organochlorosilanes to prepare organopolysiloxanes, and belongs to the technical field of organosilicon. Background technique [0002] The hydrolysis method of organochlorosilane comprises saturated acid hydrolysis and unsaturated acid hydrolysis. Using saturated acid hydrolysis, a large amount of hydrogen chloride can be recovered, avoiding a large amount of energy consumption for the dissolving heat of hydrogen chloride, because the acid water is in a saturated state, resulting in incomplete hydrolysis of chlorosilane, so secondary hydrolysis is required to obtain complete hydrolysis Product: Utilizing unsaturated acid hydrolysis can obtain relatively thorough hydrolysis products, but the common method needs to provide a large amount of energy consumption for the dissolving and exothermic hydrogen chloride, and the obtained ac...

Claims

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Application Information

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IPC IPC(8): C08G77/06C08G77/34
CPCY02P20/10
Inventor 付佃亮桑圣凯胡生祥
Owner SHANDONG DONGYUE ORGANIC SILICON MATERIAL
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