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Method for preparing dimethyl cyclosiloxane from dimethyl ether/silicon powder by one-step process

A technology of dimethylcyclosiloxane and dimethyl ether, which is applied in the direction of silicon organic compounds, and can solve problems such as environmental pollution, production control difficulties, and corrosion of equipment

Inactive Publication Date: 2014-11-19
ZHEJIANG CHANGE ORGANIC SILICON MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are also disadvantages such as long process, complicated process equipment, and difficult production control.
At the same time, the recycling of chlorine in the production process (the recycling rate is only 70%-80%) not only increases the cost, but also causes a large amount of HCl to be produced, corrodes the equipment, and pollutes the environment

Method used

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  • Method for preparing dimethyl cyclosiloxane from dimethyl ether/silicon powder by one-step process
  • Method for preparing dimethyl cyclosiloxane from dimethyl ether/silicon powder by one-step process
  • Method for preparing dimethyl cyclosiloxane from dimethyl ether/silicon powder by one-step process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Pretreatment of raw materials: dry pretreatment of dimethyl ether and methyl bromide, add a section of molecular sieve tube in the outlet channel of the storage tank of dimethyl ether and methyl bromide, that is, before entering the reactor, to remove the trace amount contained in the raw materials of dimethyl ether and methyl bromide Water; pretreatment of silicon powder, weigh hydrofluoric acid solution with a weight ratio of 5:1 and 250 μm silicon powder, stir at room temperature for 1 hour, filter, fully wash with absolute ethanol, and vacuum dry at 80°C for 5 Hours, remove the SiO on the surface layer of silicon powder 2 , standby;

[0033] Activation treatment of silicon powder: Mix CuCl, ZnO and Sn in a weight ratio of 50:1:1 to obtain a catalyst mixture, then fully mix the catalyst mixture with the above silicon powder in a weight ratio of 2:100, and treat the mixture with a microwave oven for 3 Minutes, get activated silicon powder;

[0034] Synthesis and sep...

Embodiment 2

[0038] Pretreatment of raw materials: dry pretreatment of dimethyl ether and methyl bromide, add a section of molecular sieve tube in the outlet channel of the storage tank of dimethyl ether and methyl bromide, that is, before entering the reactor, to remove the trace amount contained in the raw materials of dimethyl ether and methyl bromide Water; pretreatment of silicon powder, weigh hydrofluoric acid solution with a weight ratio of 5:1 and 250 μm silicon powder, stir at room temperature for 1 hour, filter, fully wash with absolute ethanol, and vacuum dry at 80°C for 5 Hours, remove the SiO on the surface layer of silicon powder 2 , standby;

[0039] Activation treatment of silicon powder: Mix CuCl, ZnO and Sn in a weight ratio of 50:1:1 to obtain a catalyst mixture, then fully mix the catalyst mixture with the above silicon powder in a weight ratio of 2:100, and treat the mixture with a microwave oven for 3 Minutes, get activated silicon powder;

[0040] Synthesis and sep...

Embodiment 3

[0044] Pretreatment of raw materials: dry pretreatment of dimethyl ether and methyl bromide, add a section of molecular sieve tube in the outlet channel of the storage tank of dimethyl ether and methyl bromide, that is, before entering the reactor, to remove the trace amount contained in the raw materials of dimethyl ether and methyl bromide Water; pretreatment of silicon powder, weigh hydrofluoric acid solution with a weight ratio of 5:1 and 250 μm silicon powder, stir at room temperature for 1 hour, filter, fully wash with absolute ethanol, and vacuum dry at 80°C for 5 Hours, remove the SiO on the surface layer of silicon powder 2 , standby;

[0045] Activation treatment of silicon powder: Mix CuCl and ZnO at a weight ratio of 50:1 to obtain a catalyst mixture, then fully mix the catalyst mixture with the above-mentioned silicon powder at a weight ratio of 2:100, and treat the mixture with a microwave oven for 3 minutes to obtain an activated Silica fume;

[0046] Synthesi...

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Abstract

The present invention relates to a method for preparing dimethyl cyclosiloxane from dimethyl ether / silicon powder by a one-step process. The method comprises the following steps of firstly carrying out pretreatment and activation treatment on silicon powder, adding the treated silicon powder and a solvent into a reactor together, mixing well, closing, heating to a predetermined temperature, introducing a certain amount of methyl bromide, and then metrically introducing dimethyl ether into a reactor and carrying out one-step reaction on dimethyl ether / silicon powder to obtain dimethyl cyclosiloxane, when key indexes such as the selection rate of DMC and the conversion rates of silicon powder and dimethyl ether are respectively 80%, 90% and 90%, stopping reaction, and recovering the solvent to prepare the dimethyl cyclosiloxane finished product. In the entire process, the key indexes such as the selection rate of DMC and the composition of the unreacted mixed gas are subjected to online monitoring by virtue of gas chromatography.

Description

technical field [0001] The invention relates to the technical field of production of organosilicon intermediates, in particular to a method for preparing dimethylcyclosiloxane by a one-step method of dimethyl ether / silicon powder. Background technique [0002] At present, there are more than 10,000 types of high-performance new chemical materials-organosilicon materials, and more than 5,000 kinds of usable products, mainly including high-temperature silicone rubber, room temperature silicone rubber, silicone oil and secondary processed products, silicone resin and silane. Joint agent, etc. High-temperature silicone rubber is widely used in aviation and aerospace industry, automobile industry, and electronic appliances; room temperature silicone rubber is used in construction industry, electronics industry, and road construction, and is used as sealing, bonding, pouring, coating and other materials; silicone resin is because of its excellent Excellent heat resistance, excell...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/21
Inventor 周安安
Owner ZHEJIANG CHANGE ORGANIC SILICON MATERIAL