Preparation method of dimethicone with controllable viscosity

A technology of dimethyl silicone oil and methylcyclosiloxane, which is applied in the field of downstream silicone products, and can solve problems such as serious corrosion, complicated procedures, and impurity in raw materials affecting product purity.

Active Publication Date: 2014-03-05
HUBEI XINGRUI SILICON MATERIAL CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The chlorosilane hydrolysis polycondensation method involves complicated procedures, severe corrosion, and many impurities in raw materials affect the purity of the product

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] The preparation method of tetramethylammonium hydroxide silicon alkoxide described in this example: put 150g of methylcyclosiloxane mixture (DMC) in a 250mL three-necked flask, decompress to -0.05MPa and blow nitrogen After soaking, heat up to 60°C-70°C and dehydrate for 1-2 hours, then add 3g of tetramethylammonium hydroxide silicon alkoxide obtained by polymerization of tetramethylammonium hydroxide crystals at 100°C-110°C, seal and store for later use.

[0015] 200g hexamethylcyclotrisiloxane (D 3 ) and 2g of hexamethyldisiloxane (MM) were added to a reactor preheated to 90°C±5°C and stirred, and dehydrated at 0.02Mpa for 0.5 to 1.5h under the protection of nitrogen; the hexamethyldisiloxane Trisiloxane (D 3 ) needs to be heated and melted in an oven to form a liquid phase hexamethylcyclotrisiloxane (D 3 );

[0016] Continue to blow nitrogen, add 0.5g of tetramethylammonium hydroxide silicon alkoxide into the above reaction kettle, and rapidly raise the temperatur...

Embodiment 2

[0018] The preparation method of tetramethylammonium hydroxide silicon alkoxide described in this example: put 168g of methylcyclosiloxane mixture (DMC) in a 250mL three-necked flask, decompress to -0.05MPa and blow nitrogen After soaking, heat up to 60°C-70°C and dehydrate for 1-2 hours, then add 3.5g of tetramethylammonium hydroxide silicon alkoxide obtained by polymerization of tetramethylammonium hydroxide crystals at 100°C-110°C, and seal it for future use.

[0019] 200g hexamethylcyclotrisiloxane (D 3 ) and 4g of hexamethyldisiloxane (MM) were added to a reactor preheated to 90°C±5°C and stirred, and dehydrated at 0.02Mpa for 0.5-1.5h under the protection of nitrogen; the hexamethyldisiloxane Trisiloxane (D 3 ) needs to be heated and melted in an oven to form a liquid phase hexamethylcyclotrisiloxane (D 3 );

[0020] Continue to blow nitrogen, add 4g of tetramethylammonium hydroxide silicon alkoxide into the above reaction kettle, and rapidly raise the temperature to ...

Embodiment 3

[0022] The preparation method of tetramethylammonium hydroxide silicon alkoxide described in this example: put 146g of methylcyclosiloxane mixture (DMC) in a 250mL three-necked flask, decompress to -0.05MPa and blow nitrogen After soaking, heat up to 60°C-70°C and dehydrate for 1-2 hours, then add 4.4g of tetramethylammonium hydroxide silicon alkoxide obtained by polymerization of tetramethylammonium hydroxide crystals at 100°C-110°C, and seal it for future use.

[0023] 200g hexamethylcyclotrisiloxane (D 3 ) and 8g of hexamethyldisiloxane (MM) were added to a reactor preheated to 90°C±5°C and stirred, and dehydrated at 0.02Mpa for 0.5-1.5h under the protection of nitrogen; the hexamethyldisiloxane Trisiloxane (D 3 ) needs to be heated and melted in an oven to form a liquid phase hexamethylcyclotrisiloxane (D 3 );

[0024] Continue to blow nitrogen, add 4g of tetramethylammonium hydroxide silicon alkoxide into the above reaction kettle, and rapidly raise the temperature to ...

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Abstract

The invention relates to a preparation method of dimethicone with controllable viscosity, and belongs to the technical field of downstream products of organic silicon. The method is characterized in that hexamethylcy (D3) is adopted as a raw material, low-viscosity dimethicone (MDnM) with the viscosity of 5 to 50 mpa.s and hexamethyldisiloxane (MM) are adopted as end-capping reagents, tetramethyl ammonium hydroxide silicon alkoxide and potassium hydroxide (KOH) silica-alkoxide are catalyzed to generate the dimethicone with controllable viscosity in a polymerization-free manner, and the viscosity range of the dimethicone is 100-100000 mpa.s. Main raw materials used in the method are dissolved without a solvent, so that pollution is avoided; the end-capping reagents are good in end-capping effect, cheap and safer; the catalyst is easy to obtain and less in consumption; the dimethicone with high purity and controllable viscosity can be prepared in a polymerization-free manner only by changing the dispensing ratio of the hexamethylcy (D3) and the low-viscosity dimethicone (MDnM).

Description

technical field [0001] The invention relates to a preparation method of simethicone oil with controllable viscosity, belonging to the technical field of silicone downstream products. Background technique [0002] Simethicone oil is a non-toxic and non-corrosive transparent liquid with physiological inertia, good chemical stability, electrical insulation and weather resistance, low freezing point and vapor pressure, high flash point and high ignition point, good hydrophobicity and low surface tension. , a wide range of viscosity, can be used for a long time in the temperature of -50 ~ 200 ℃, widely used as moisture-proof insulation, lubrication, shockproof, and cold, heat carrier, and used as defoaming, film release, paint, coating, rubber and plastic and daily cosmetics and other additives. With the development of society, the requirements for the viscosity of simethicone are becoming more and more precise, but the types and ranges of viscosities available in the market are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/04
Inventor 李利燕马会娟高英苗刚陈海平杨祝华
Owner HUBEI XINGRUI SILICON MATERIAL CO LTD
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