Method and device for preparing high-boiling-point silicone oil

A high-boiling silicone oil, high-boiling technology, applied in the equipment for implementing the method, alcoholysis of chlorosilane to produce alkoxy silicone oil, and alcoholysis of organosilicon high-boiling substance or/and azeotrope to produce high-boiling silicone oil field, can solve the problem. Hydrogen chloride gas is difficult to fully resolve, storage stability is affected, and the amount of neutralizer is large, so as to achieve the effects of controllable molecular weight and viscosity, reduced dosage, and fewer side reactions

Active Publication Date: 2013-02-27
湖北新四海化工股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In recent years, as the applicant of the Chinese patent CN1249127C, it has been found in industrial production that this patented technology also has certain deficiencies: (1) when methanol is added dropwise to the high-boiling monomer at room temperature, the chlorine atom with a large steric hindrance cannot be completely absorbed Substitution, causing the product to easily return to acid during storage, which has a certain impact on storage stability
(2) Deacidification is carried out at normal temperature, and the hydrogen chloride gas dissolved in it is difficult to fully analyze, and the amount of neutralizing agent in the subsequent steps is relatively large, and the cost increases

Method used

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  • Method and device for preparing high-boiling-point silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Take 100 parts of organic silicon high boilers and 40 parts of methanol. The temperature of the reactor at the bottom of the tower is pre-heated to 70°C, and from the bottom of the reactor, the organosilicon high-boiling substance and methanol are pumped into the top of the tower with a metering pump, and the materials enter the bottom of the kettle through the top of the tower through the filler in the tower. After the addition is complete, the temperature is raised to 100°C, and the reflux deacidification is continued for 3 hours. After deacidification is completed, the temperature is lowered to 40°C, and the materials are pumped into the neutralization kettle. Add 25 parts of urea, 2 parts of zinc oxide as a flux, 15 parts of ammonium bicarbonate as a neutralizer, and neutralize the dissolved hydrogen chloride. After the addition, continue to stir for 30 minutes and let stand for layering. The lower eutectic is separated into the lime pond through the neutralization ...

Embodiment 2

[0042] Take 100 parts of organic silicon high boilers and 45 parts of methanol. The temperature of the kettle is pre-heated to 50°C, the nitrogen valve is opened, and the high-boiling organic silicon and methanol are driven into the tower at a weight ratio of 2.2 / 1 with a metering pump. After the addition is completed, the temperature is raised to 60°C, and nitrogen is continued to flow back and deacidify for 2 hours. After deacidification, the temperature is lowered to 40°C, the nitrogen gas is stopped, and the materials are pumped into the neutralization kettle. Add 40 parts of urea, 6 parts of flux (zinc oxide and sodium hydroxide at a ratio of 1 / 0.5), 25 parts of neutralizer (a ratio of ammonium bicarbonate and ethylenediamine at 1 / 0.6), and continue after adding Stir for 30 minutes and let stand for layering. The lower layer material is put into the lime pond to continue neutralization to neutrality, and 3 parts of the neutralizer is added to the upper layer material, an...

Embodiment 3

[0044] Take 100 parts of organic silicon high boilers and 50 parts of methanol. The temperature of the kettle is pre-heated to 80°C, the nitrogen valve is opened, and the high-boiling organic silicon and methanol are pumped into the tower with a metering pump. After the addition is complete, the temperature is raised to 120°C, and nitrogen is continued to flow back and deacidify for 5 hours. After deacidification, the temperature is lowered to 40°C, the nitrogen gas is stopped, and the materials are pumped into the neutralization kettle. Add 10 parts of urea, 0.5 parts of flux (zinc oxide and sodium carbonate at a ratio of 1 / 0.2), 8 parts of neutralizer (a ratio of ammonium bicarbonate and triethanolamine at a ratio of 1 / 0.6), and continue to stir after adding 30 For minutes, let stand for layering. The lower layer material is put into the lime pool to continue neutralization to neutrality, 0.5 part of neutralizer is added to the upper layer material, and the high boiling sil...

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Abstract

The invention provides a method and device for preparing high-boiling-point silicone oil. The method comprises the following steps: (1) alcoholysis: preheating a reaction kettle on the bottom of a reaction column to 50-100 DEG C, and adding organosilicon high-boiling-point monomers and methanol from the upper part of the reaction column; while controlling the kettle temperature at 50-130 DEG C, continuing deacidification for 1-5 hours after finishing adding the materials; and (2) neutralization: cooling the alcoholysis material obtained in the step (1) to 30-60 DEG C, neutralizing by adding urea, a fluxing agent and a neutralizer, and filtering to obtain the finished product. By comprehensively utilizing organosilicon high-boiling-point substances, the invention solves the problem of high-boiling-point substance recycling which limits further development of the organosilicon high-boiling-point monomers. The alcoholysis process is carried out in the column, two-way adding, heating under reflux, resolving chlorine hydride by nitrogen, and other measures are adopted to reduce the side reactions, so that the alcoholysis is more sufficient, the chlorine content of the silicone oil product is low, the molecular weight and viscosity of the silicone oil product are controllable, the quality of the silicone oil product is more stable, the consumptions of the neutralizer and fluxing agent are greatly reduced, and the production cost is lowered.

Description

Technical field [0001] The invention belongs to the technical field of production technology of silicone oil, and relates to a method for producing alkoxy silicone oil by chlorosilanolysis. Specifically, it relates to a method for producing high-boiling silicone oil by alcoholysis of organosilicon high-boiler or / and azeotrope. [0002] The invention also relates to equipment for implementing the method. Background technique [0003] In recent years, with the rapid development of the organosilicon industry, the output of methylchlorosilane has become larger and larger, and the by-products produced during the synthesis of methylchlorosilane monomer-organosilicon high boiling substances have also increased. In 2010, the domestic monomer output is expected to reach 2 million tons, and the by-product high-boiler output, which accounts for about 5% of the monomer volume, will reach 100,000 tons. Because the composition of high boilers is extremely complex, and contains a large amount o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06
Inventor 龚家全王秀山杨开柱
Owner 湖北新四海化工股份有限公司
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