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Preparation method of organic silicon methoxy/ethoxy high boiling silicone oil

A high-boiling silicone oil and organosilicon technology, which is applied in the preparation field of organosilicon methyl ethoxy high-boiling silicone oil, can solve the problems of complex process, high product cost, many three wastes, etc., and achieves process rationalization, high operation flexibility, and reduced production cost. Effect

Active Publication Date: 2011-07-27
JILIN INST OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The existing technology is complex, the product cost is high, and there are many three wastes, and some manufacturers have not rationally utilized high boiling materials

Method used

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  • Preparation method of organic silicon methoxy/ethoxy high boiling silicone oil

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Experimental program
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Effect test

Embodiment 1

[0017] A method for preparing organosilicon methyl ethoxy high-boiling silicone oil, taking 100 parts (mass parts, the same below) of organosilicon high-boiling mixture with a boiling range of 80-215°C, and putting them into a reactor with condensing reflux at one time , start stirring and add dropwise 95 parts of 97wt% CH at room temperature 3 OH: In the first stage, control the temperature ≤ 35°C, add dropwise for 1h; in the second stage, control the temperature ≤ 45°C, add dropwise for 0.5h; in the third stage, control the temperature ≤ 55°C, add dropwise for 0.5h; in the fourth stage, control the temperature ≤ 60 ℃, add dropwise for 1h; CH 3 After the dropwise addition of OH, control the temperature to ≤60°C to continue the reaction for 2 hours, and the reaction ends. Cool to room temperature and stand to separate layers. After separation, the upper layer is a brownish-yellow methoxylated acidic high boiler, and the lower layer is a methoxylated raffinate. The HCl tail g...

Embodiment 2-3

[0024] Operation steps are as embodiment 1, and its technological parameters are shown in Table 1

[0025] Table 1. Embodiment 1-3 process parameter table

[0026]

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Abstract

The invention provides a preparation method of organic silicon methoxy / ethoxy high boiling silicone oil. The mixture of high boiling organic silicon in the boiling range of 80-215 DEG C serves as raw materials; yellowish methoxy / ethoxy acidic high boiling silicone oil is obtained through methoxylation, ethoxylation and catalytic cracking rearrangement, wherein the density of the yellowish methoxy / ethoxy acidic high boiling silicone oil is 0.856-0.932g / cm<3>, and the pH value of the yellowish methoxy / ethoxy acidic high boiling silicone oil is 1-2; methoxy / ethoxy neutral high boiling silicone oil (yellowish liquid) is obtained through neutralization, wherein the density of the methoxy / ethoxy neutral high boiling silicone oil is 0.844-0.924g / cm<3>; the methoxy / ethoxy neutral high boiling silicone oil can be refined to be colorless and transparent methoxy / ethoxy neutral high boiling silicone oil based on the requirements of users, wherein the density of the colorless and transparent methoxy / ethoxy neutral high boiling silicone oil is 0.821-0.823g / cm<3>, and the pH value of the colorless and transparent methoxy / ethoxy neutral high boiling silicone oil is 6; the obtained hydrogen chloride gas is circularly absorbed to obtain 25-31wt% of hydrochloric acid (byproduct), and collected KCl can be recycled; and the collected KCl can also be refined to form a byproduct with the purity being greater than or equal to 99wt%; therefore, the recycle of resources is realized, and the preparation method is an environment-friendly process.

Description

technical field [0001] The invention belongs to a preparation method of organic silicon methyl ethoxy high boiling silicone oil. Background technique [0002] Organosilicon high boilers refer to the high-boiling methylchlorosilane mixtures produced during the synthesis of methylchlorosilane monomers with a boiling range of 80-215°C and above, mainly composed of silicon-silicon bonds and silicon-oxygen-silicon bonds. About 9000-9500 tons per year. At present, the utilization of high boiling substances at home and abroad mainly includes the following types: preparation of silicone oil, silicone water repellent, silicone resin, defoamer and film release agent; preparation of monosilane by catalytic cracking. Due to the limited amount of direct utilization of high boilers and low added value, many organosilicon manufacturers have shifted the use of high boilers to cracking to prepare monosilane. Cracking process to prepare monosilane: hydrogen chloride cracking, high pressure ...

Claims

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Application Information

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IPC IPC(8): C08G77/18C08G77/06C08G77/32
Inventor 高维平李晓光周光峰董训国
Owner JILIN INST OF CHEM TECH
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