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Method for producing dimethyl cyclosiloxane in non-halogenation direct continuous mode

A dimethylcyclosiloxane, non-halogenated technology, applied in the direction of silicon organic compounds, can solve problems such as unstable product batches, inability to realize automatic control, and reduced economies of scale

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

AI Technical Summary

Problems solved by technology

[0008] In addition, the traditional DMC preparation technology adopts a batch method for production. The inherent characteristics of the batch method bring about the disadvantages of low efficiency and unstable product batches during the preparation of dimethylcyclosiloxane, and automatic control cannot be realized, thus Increase labor costs and reduce economies of scale

Method used

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  • Method for producing dimethyl cyclosiloxane in non-halogenation direct continuous mode
  • Method for producing dimethyl cyclosiloxane in non-halogenation direct continuous mode
  • Method for producing dimethyl cyclosiloxane in non-halogenation direct continuous mode

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] 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 150 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;

[0037] 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;

[0038] Synthesis and sep...

Embodiment 2

[0043] Pretreatment of raw materials: dry pretreatment of dimethyl ether and methyl bromide, in the outlet channel of the storage tank of dimethyl ether and methyl bromide, add a section of molecular sieve tube before entering the reactor, to remove trace water contained in the raw materials of dimethyl ether and methyl bromide ; For the pretreatment of silicon powder, weigh a hydrofluoric acid solution with a weight ratio of 5:1 and 120 μm silicon powder, stir at room temperature for 1 hour, filter, wash thoroughly with absolute ethanol, and dry in vacuum at 80°C for 5 hours , to remove the SiO on the surface layer of silicon powder 2 , standby;

[0044] 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 then sinter the mixture under vacuum at 120°C for 3 hours. Get activated silicon powder;

[0045] Synthe...

Embodiment 3

[0049] Pretreatment of raw materials: dry pretreatment of dimethyl ether and methyl bromide, in the outlet channel of the storage tank of dimethyl ether and methyl bromide, add a section of molecular sieve tube before entering the reactor, to remove trace water contained in the raw materials of dimethyl ether and methyl bromide ; Pretreatment of silicon powder, weigh hydrofluoric acid solution with a weight ratio of 5:1 and 200 μm silicon powder, stir at room temperature for 1.5 hours, filter, fully wash with absolute ethanol, and vacuum dry at 80°C for 5 hours , to remove the SiO on the surface layer of silicon powder 2 , standby;

[0050] Activation treatment: Mix CuCl and Sn 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 in a microwave oven for 5 minutes to obtain activated silicon powder;

[0051] Synthesis of dimethylcyclosiloxane: After...

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Abstract

The invention relates to a method for producing dimethyl cyclosiloxane in a non-halogenation direct continuous mode. The method comprises the following steps: firstly, performing pretreatment and activation treatment on silicon powder, putting into a reaction kettle together with a solvent, sealing the reaction kettle, heating, feeding a certain amount of methyl bromide, subsequently continuously feeding dimethyl ether into the reaction kettle for performing non-halogenation direct synthesis reaction, separating the mixture generated in the reaction into a high melting point material and a low melting point material through a separation column, returning the high melting point material, circulating into a reactor again, further condensing the low melting point material, and feeding methylsiloxane condensate in the low melting point material into a distillation device for separating dimethyl cyclosiloxane (DMC). In the whole process, significant indexes such as the selection rate of DMC and the components of unreacted mixed gases are monitored on line by using a gas chromatographic method, and basis is provided for continuous on-line control. By adopting the method, continuous production and automatic process control can be achieved in the dimethyl cyclosiloxane preparation process, and thus purposes of improving the efficiency, improving the product stability and the like can be achieved.

Description

technical field [0001] The invention relates to the technical field of production of organosilicon intermediates, in particular to a method for non-halogenated direct and continuous production of dimethylcyclosiloxane. 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, excellent electric...

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
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