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Preparation method of methylsilicone oil

A technology of methyl silicone oil and polymethyl siloxane, which is applied in the field of new materials, can solve problems such as separation difficulties and sulfuric acid corrosion of production equipment, and achieve the effect of low price

Inactive Publication Date: 2013-03-20
JIANGNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although its catalytic activity is good, long-term use will bring many problems to industrial production: the residual concentrated sulfuric acid in the simethicone oil obtained after the reaction needs to be neutralized, washed with water, etc., which not only makes separation difficult, but also A large amount of industrial wastewater will be produced, and sulfuric acid will also corrode production equipment
[0005] Zhao Jianhong first reported the solid superacid TiO 2 / SO 4 2- A method for catalyzing the synthesis of dimethyl silicone oil [Fine and Specialty Chemicals, 2006, 14(18), 21], but the activity and stability of the catalyst need to be further improved. The invention patent CN101851333A discloses a method for preparing methyl phenyl silicone oil The method, this method is catalyst with rare earth superacid, specifically is that solid superacid TiO 2 / SO 4 2- It is compounded with a variety of rare earth compounds, so that the rare earth metal atoms and the original metal atoms have a synergistic effect, further improving the catalyst activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0024] The preparation of catalyst-1: 25g ZrOCl 2 ·8H 2 O was dissolved in 150mL water, ammonia water was added dropwise under strong magnetic stirring to pH=9~10, the precipitate was filtered and washed until the filtrate was mixed with 0.1mol / L AgNO 3 Check for Cl - ions, the obtained filter cake was mashed and dried at 105°C for 2 hours, then the dried solid was ground into powder with a mortar and then dried at 105°C for 20 minutes, and the dried solid was sieved with a 200-mesh sieve Powder screening, 1gZSM-5 content is 3% ZSM-5 molecular sieve and Zr(OH) 4 The mixture was added into a 1.0 mol / L sulfuric acid solution, stirred magnetically for 45 minutes, filtered, dried at 105°C for 12 hours, and then calcined at 700°C in an air atmosphere for 2 hours to obtain Catalyst-1.

[0025] Catalyst-1 is used in the synthesis reaction of simethicone oil: weigh 10gD 4 (octamethylcyclotetrasiloxane) and 0.32 gMM (hexamethyldisiloxane) in a 25 mL round bottom flask, add 0.100 g ...

example 2

[0027] Catalyst-1 is used in the synthesis reaction of simethicone oil: weigh 10gD 4 (octamethylcyclotetrasiloxane) and 0.16 gMM (hexamethyldisiloxane) in a 25 mL round bottom flask, add 0.100 g of freshly prepared Catalyst-1 into the round bottom flask, and magnetically stir at 120 °C reaction. After reacting for 2 hours, extract under reduced pressure and recover low boilers to obtain colorless and transparent simethicone oil with a rotational viscosity of 350 mpa·s at 25°C.

example 3

[0029] Catalyst-1 is used for the synthesis reaction of simethicone oil: Weigh 10g D4 (octamethylcyclotetrasiloxane) and 0.10gMM (hexamethyldisiloxane) in a 25mL round bottom flask, and pour into the round bottom flask Add 0.200 g of freshly prepared Catalyst-1 and react with magnetic stirring at 120°C. After reacting for 2 hours, remove the catalyst by filtration, extract under reduced pressure and recover low boilers to obtain a colorless and transparent simethicone oil with a rotational viscosity of 390 mpa·s at 25°C.

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Abstract

The invention discloses a preparation method of methylsilicone oil, and specifically relates to methyl silicone oil with different viscosity (molecular weight) prepared by using supported solid superacid SO4<2-> / ZrO2-ZSM-5 as a catalyst and by adopting inexpensive and commercially available methylsilicone oil (Dn), octamethylcyclotetrasiloxane (D4) and hexamethyldisiloxane (MM), so as to fit various needs. Compared with a conventional catalyst for producing methylsilicone oil, the supported solid superacid catalyst provided by the invention has higher catalytic activity, higher stability, lower cost and the like. More importantly, the supported solid superacid catalyst is in a solid state and can be separated via simple filtration and reused, thereby enabling the production to have the advantages of simple process, convenient operation, no pollutions, no corrosion toward equipment, and the like.

Description

technical field [0001] The invention relates to a method for preparing methyl silicone oil, specifically a new method for preparing silicone oil of various viscosities by using a loaded solid superacid, and belongs to the technical field of new materials. Background technique [0002] Simethicone oil is odorless and non-toxic, with physiological inertness, good chemical stability, electrical insulation and weather resistance, wide viscosity range, low freezing point, high flash point, good hydrophobicity, and high shear resistance. It can be used for a long time at a temperature of 50-180°C. It is widely used as insulation, lubrication, shockproof, dust-proof oil, dielectric fluid and heat carrier, and it is also used as an additive for defoaming, film release, paint and daily cosmetics. With the development of society, not only the demand for the amount of methyl silicone oil is increasing, but also the demand for methyl silicone oil of different viscosities (molecular weig...

Claims

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Application Information

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IPC IPC(8): C08G77/08C08G77/44
CPCY02P20/584
Inventor 丁玉强沈守宇杨淑艳王慧君施英黄以军
Owner JIANGNAN UNIV
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