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A continuous preparation process of high-purity and low-viscosity simethicone oil

A simethicone oil and preparation technology, which is applied in the field of continuous preparation process of high-purity and low-viscosity simethicone oil, can solve the problems of easy damage of ion exchange resin, volume expansion, impact on de-lowering effect and product quality, etc. Achieve the effects of reducing the difficulty of equipment processing, increasing the capping rate, ensuring catalytic activity and product quality

Active Publication Date: 2014-10-15
YICHANG COLLIN SILICON MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the continuous method adopts the form of a fluidized bed, the residence time of the raw material mixture in the fluidized bed must be controlled and the reaction product has a certain viscosity, so the fluidized bed often has a certain pressure. After that, its volume expands, and the ion exchange resin is easily damaged under pressure.
Therefore, as the production progresses, the reaction product may carry more and more broken resin and other solid impurities into the de-lowering process, which will affect the de-lowering effect and product quality

Method used

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  • A continuous preparation process of high-purity and low-viscosity simethicone oil
  • A continuous preparation process of high-purity and low-viscosity simethicone oil

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Experimental program
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Effect test

Embodiment 1

[0032] Dimethicone mixed ring (DMC) and end-capping agent (MD 2M) According to the mass ratio of 100:4.92, transport it to the pretreatment tank, first use liquid nitrogen to freeze and remove water, control the freezing temperature to -10°C, freeze and remove water for 2 hours, freeze and remove water and then transport it to the mixed drying tank , after heating up to 50°C, the vacuum degree is controlled at -0.085~-0.095Mpa, while stirring, dry nitrogen (nitrogen after vaporization of liquid nitrogen) is introduced to carry out deep dehydration for 2 hours, and the mixture after deep dehydration is sequentially dewatered by a vortex pump It is sent to stainless steel filter and ultrafiltration membrane filter for filtration to remove ions and solid impurities, and then sent to the preheater to preheat to 80°C, and then sent to the fluidized bed equipped with LDX-604 macroporous cation exchange resin Medium reaction, the reaction temperature is controlled at 60°C, and the re...

Embodiment 2

[0034] The dimethylsiloxane mixed ring body (DMC) and the end-capping agent (MDM) are transported to the pretreatment tank at a mass ratio of 100:2.16, and the water is first frozen with liquid nitrogen, and the freezing temperature is controlled at -5°C , the freezing and dehydration time is 3 hours, after freezing and dehydrating, it is transported to the mixed drying kettle. After the temperature is raised to 40°C, the vacuum degree is controlled at -0.090~-0.095Mpa, and dry nitrogen is introduced while stirring (the nitrogen gas after the liquid nitrogen is vaporized ) after deep dewatering for 3 hours, the mixture after deep dewatering is sent to stainless steel filter and ultrafiltration membrane filter to filter through vortex pump to remove ions and solid impurities, and then sent to preheater to preheat to 40 ℃, and then transported to the fluidized bed equipped with D72H macroporous cation exchange resin for reaction, the reaction temperature is controlled at 30 ℃, an...

Embodiment 3

[0036] Dimethicone mixed ring (DMC) and end-capping agent (MD 3 M) According to the mass ratio of 100:1.48, transport to the pretreatment tank, first use liquid nitrogen to freeze and remove water, control the freezing temperature to -15°C, freeze and remove water for 1h, freeze and remove water and then transport it to the mixed drying tank , the vacuum degree is controlled at -0.085~-0.095Mpa. After the temperature is raised to 70°C, dry nitrogen gas (nitrogen after vaporization of liquid nitrogen) is introduced while stirring to carry out deep water removal for 1 hour, and the mixture after deep water removal is removed by a vortex pump. Sequentially transported to stainless steel filter, ultrafiltration membrane filter to remove ions and solid impurities, and then transported to the preheater to preheat to 100 ° C, and then transported to the fluidized bed equipped with D72H macroporous cation exchange resin Reaction, the reaction temperature is controlled at 90°C, and the...

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Abstract

The invention discloses a continuous preparation process of high-purity and low-viscosity simethicone oil, which comprises the following steps: methylcyclosiloxane and end-capping agent are sequentially dewatered by liquid nitrogen freezing and deep dewatering to reduce the water content of the mixture to less than 300ppb, then through adsorption filtration, ultrafiltration membrane filtration, preheating, and enter the fluidized bed with catalyst to catalyze the reaction. , to obtain simethicone oil. The simethicone oil prepared by the invention has high purity, low ion content, hydroxyl content, and solid content, and can make the utilization rate of raw materials reach 100%, and achieve zero emission. It is an environmentally friendly and efficient preparation of high-purity and low-viscosity The green and environment-friendly process of silicone oil is suitable for the production of low-viscosity dimethyl silicone oil.

Description

technical field [0001] The invention relates to a continuous preparation process of high-purity and low-viscosity simethicone oil. Background technique [0002] In recent years, under the condition that the entire silicone market has developed well, simethicone, as a member of the silicone family, is generally optimistic about its development prospects. In the past five years, China's apparent consumption of simethicone has an average annual growth rate of around 15%, making it the fastest growing market in the world. There are many manufacturers of simethicone oil in China, and the technical level is uneven, and most companies still use the intermittent method to produce low-viscosity silicone oil, resulting in low production efficiency, large fluctuations in product batch quality, poor product performance, and low utilization of by-products. Inferior question. At present, domestic silicone oil has insufficient control in terms of hydroxyl content, ion content and solid c...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/06
CPCY02P20/582
Inventor 王跃林冯钦邦吴利民段先健
Owner YICHANG COLLIN SILICON MATERIAL CO LTD