A kind of high conversion rate 107 silicone rubber production system and its production method

A technology with high conversion rate and production method, which is applied in the field of high conversion rate 107 silicone rubber production system, can solve the problems of unstable product quality, lower production cost, difficult process control, etc., to save dehydration consumption and related equipment investment, Promote the positive movement of the reaction balance and the effect of high comprehensive utilization of raw materials

Active Publication Date: 2020-06-09
HUBEI XINGRUI SILICON MATERIAL CO LTD
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  • Application Information

AI Technical Summary

Problems solved by technology

In the early days, due to the high content of ions and other impurities in dimethyldichlorosilane hydrolyzate, it could not meet the production needs of 107 silicone rubber. Domestic silicone manufacturers mostly used cyclic siloxane mixtures ("DMC") as 107 silicone rubber. Raw materials for rubber production
With the continuous innovation of technology in the field of silicone and the increasingly fierce market competition, silicone manufacturers widely use dimethyldichlorosilane hydrolyzate as the raw material for 107 silicone rubber production, which saves the cracking and rectification links and greatly reduces However, it also faces problems such as low primary conversion rate of polymerization reaction, complex raw material pretreatment process, and unstable product quality. There is still room for optimization in the production method of 107 silicone rubber.
[0003] Chinese patent CN200810062215 describes a new process for the synthesis of 107 silicone rubber. This process uses dimethyldichlorosilane hydrolyzate after washing and dehydration, and prepares 107 silicone rubber under the catalytic conditions of potassium hydroxide, which can reduce the impurity content of raw materials. Improve product quality, but the process is more complicated, the content of linear bodies in raw materials is low, and the polymerization temperature is high, which is not conducive to improving the primary conversion rate
Chinese patent CN201510695100 describes a method for the preparation of 107 silicone rubber. This method uses Dow Corning PMX-0156 filament as raw material and lithium hydroxide monohydrate as catalyst. The reaction conversion rate is high, but lithium hydroxide is expensive and cannot be reused. , the reaction temperature is high, the energy consumption is high, the moisture generated by the polycondensation is removed by vacuum during the polymerization process, the process control is difficult, and the low molecules released are not recycled, which is not conducive to reducing the production cost

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  • A kind of high conversion rate 107 silicone rubber production system and its production method

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Experimental program
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Effect test

Embodiment 1

[0031] A high conversion rate 107 silicone rubber production system, comprising a polymerization kettle 1, the polymerization kettle 1 is connected with a feed metering tank 2 through a pipeline, and the feed metering tank 2 is connected with a filter 5 through a pipeline, and the filter 5 is equipped with a feed pipe; the filter 5 is a laminated precision filter or other precision filter, and the filtration accuracy is 0.2-10.0 μm;

[0032] The polymerization kettle 1 is also connected with the delowering condenser 4 through a pipeline, and the delowering condenser 4 is connected with the low molecular collector 3 through a pipeline.

[0033] Preferably, the polymerization kettle 1 is provided with a nitrogen inlet pipe 7, a discharge port, an online viscometer 6 and a heat transfer oil system 8;

[0034] Preferably, the top of the low molecular collector 3 is connected to a vacuum unit, the bottom of the low molecular collector 3 is connected to a low molecular tank; the del...

Embodiment 2

[0036] Adopt the system described in embodiment 1 to carry out the production method of high conversion rate 107 silicone rubbers, described method may further comprise the steps:

[0037] 1) Feed: the raw material enters the feed metering tank 2 after being removed by the filter 5, and then feeds into the polymerization kettle 1, and the feed amount is calculated according to the liquid level change of the feed metering tank 2;

[0038] 2) Polymerization: Turn on the stirring and heat transfer oil system of the polymerization kettle 1, add a basic catalyst after reaching the polymerization temperature, and pass dry nitrogen into the polymerization kettle 1 after a period of normal pressure reaction, and further polymerize after stopping the nitrogen;

[0039] 3) Neutralization: when the online viscometer 6 shows 5,000-200,000cp, add acid to neutralize and stop the reaction;

[0040] 4) Delowering: Polymerization kettle 1 internally removes the low molecular weight in the rubb...

Embodiment 3

[0048] Adopt the system described in embodiment 1 to carry out the production method of high conversion rate 107 silicone rubbers, described method is:

[0049]The raw material hydrolyzate with high linear siloxane content of 90% is removed by the filter 5 and enters the feed metering tank 2, and then feeds 1000kg from the metering tank to the polymerization kettle 1, and the heat transfer oil of the polymerization kettle 1 is turned on and stirred, and the temperature is raised After reaching 150°C, add 117g of 50% KOH aqueous solution, stir for 1h, and then pass dry nitrogen for 0.5h, and the nitrogen flow rate is 0.1m 3 / h, stop the nitrogen and continue to stir for 0.5h, add 117g of 85% phosphoric acid solution, neutralize for 1h and then raise the temperature to 160°C, start the vacuum unit to gradually increase the vacuum degree of the system to 0.1MPa, after 0.8h, no low molecules come out, low 102kg of low molecules were collected in the molecular collector 3, the conv...

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Abstract

The invention relates to a high-conversion-rate 107 silicone rubber production system and a production method thereof. The high-conversion-rate 107 silicone rubber production system comprises a polymerization reactor, the polymerization reactor is connected to a feed metering tank through a pipe, the feed metering tank is connected to a filter through a pipe, and the filter is provided with a feed pipe. Dimethyldichlorosilane is subjected to hydrolysis, deacidification, cyclic siloxane separation and water separation so as to obtain high linear siloxane hydrolyzate, the high linear siloxane hydrolyzate is used as a raw material, under the action of an alkaline catalyst, nitrogen is adopted to remove water generated by polymerization, polymerization can be completed at a lower temperature, and a polymerization product is subjected to acid neutralization and vacuum low-molecule removal so as to obtain the product 107 silicone rubber. The content of the raw material linear siloxane used in the invention is relatively high, and no ring opening is needed in the polymerization process, the reaction activation energy is low, polymerization can be realized under the low temperature condition, the primary conversion rate can reach 90% to 95% higher than that of other raw materials, low molecules can be returned to the polymerization reactor for reuse, the total yield is up to 99.5%, and the utilization of raw materials is high.

Description

technical field [0001] The invention relates to the technical field of polysiloxane synthesis, in particular to a high-conversion 107 silicone rubber production system and a production method thereof. Background technique [0002] 107 silicone rubber is a hydroxyl-terminated polydimethylsiloxane (α, ω-dihydroxypolysiloxane), which is the basic compound for the preparation of condensation-type RTV silicone rubber, and is one of the important products in the silicone industry. In the early days, due to the high content of ions and other impurities in dimethyldichlorosilane hydrolyzate, it could not meet the production needs of 107 silicone rubber. Domestic silicone manufacturers mostly used cyclic siloxane mixtures ("DMC") as 107 silicone rubber. Raw material for rubber production. With the continuous innovation of technology in the field of silicone and the increasingly fierce market competition, silicone manufacturers widely use dimethyldichlorosilane hydrolyzate as the raw...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/16C08G77/08
CPCC08G77/08C08G77/16
Inventor 李书兵颜昌锐孙刚王文金胡东华肖靖
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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