Preparation method of methyl phenyl silicone oil

A technology of methyl phenyl silicone oil and diphenyl dichlorosilane is applied in the field of preparation of dimethyl diphenyl silicone oil to achieve the effects of reducing environmental pollution, mild reaction conditions and large output

Inactive Publication Date: 2013-09-18
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN 102516546A discloses a kind of using methylphenyl dichlorosilane as raw material and weak organic base aqueous solution as acid-binding agent to prepare low-viscosity methylphenyl hydroxy silicone oil. Although the raw material is cheap, this method adds a large amount of weak organic Alkali, which increases the cost of industrial production

Method used

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  • Preparation method of methyl phenyl silicone oil
  • Preparation method of methyl phenyl silicone oil
  • Preparation method of methyl phenyl silicone oil

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] The Ph / R ratio (molar ratio) was 0.1. Add 80 mL of xylene, 50 mL of acetone, 23.23 g of dimethyldichlorosilane and 5.06 g of diphenyldichlorosilane into a 500 mL three-neck flask, stir and mix evenly at 30 °C; prepare a certain proportion of hydrolyzate, of which Acetone 100 mL and distilled water 57.6 g, stir evenly, add drop by drop to the three-necked flask with a constant pressure titration funnel, control the dropping rate to keep 1d / 2s, the total titration time is about 3 h, add 0.5432 g capped Chlorotrimethylsilane, continue to react at 30°C for 5h, and the hydrolysis is completed; stand for stratification, separate the lower layer of acid water, wash the upper layer of hydrolyzate with distilled water at 50-60°C until neutral, and obtain a siloxane prepolymer , and then add 0.0570 g of condensation catalyst sodium ethylate (0.05% of the total mass of the monomer) at 100 °C for condensation reaction for 3 h. The solvent xylene and low boilers were distilled off ...

Embodiment 2

[0031] The Ph / R ratio (molar ratio) was 0.3. Add 80 mL of xylene, 50 mL of acetone, 18.07 g of dimethyldichlorosilane and 15.19 g of diphenyldichlorosilane into a 500 mL three-necked flask, and stir and mix evenly at 30 °C; prepare a certain proportion of hydrolyzate, of which Acetone 100 mL and distilled water 57.6 g, stir evenly, add drop by drop to the three-necked flask with a constant pressure titration funnel, control the dropping rate to keep 1d / 2s, the total titration time is about 3 h, add 0.5432 g capped Chlorotrimethylsilane, continue to react at 30°C for 5h, and the hydrolysis is completed; stand for stratification, separate the lower layer of acid water, wash the upper layer of hydrolyzate with distilled water at 50-60°C until neutral, and obtain a siloxane prepolymer , and then add 0.0665 g of condensation catalyst sodium ethylate (0.05% of the total monomer mass) at 100 °C for condensation reaction for 3 h. The solvent xylene and low boilers were distilled off ...

Embodiment 3

[0033] The Ph / R ratio (molar ratio) was 0.7. Add 80 mL of xylene, 50 mL of acetone, 7.74 g of dimethyldichlorosilane and 35.45 g of diphenyldichlorosilane into a 500 mL three-neck flask, stir and mix evenly at 30 °C; prepare a certain proportion of hydrolyzate, of which Acetone 100 mL and distilled water 57.6 g, stir evenly, add drop by drop to the three-necked flask with a constant pressure titration funnel, control the dropping rate to keep 1d / 2s, the total titration time is about 3 h, add 0.5432 g capped Chlorotrimethylsilane, continue to react at 30°C for 5h, and the hydrolysis is completed; stand for stratification, separate the lower layer of acid water, wash the upper layer of hydrolyzate with distilled water at 50-60°C until neutral, and obtain a siloxane prepolymer , and then add 0.0864 g of condensation catalyst sodium ethylate (0.05% of the total monomer mass) at 100 °C for condensation reaction for 3 h. The solvent xylene and low boilers were distilled off under r...

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Abstract

The invention relates to a preparation method of methyl phenyl silicone oil, which belongs to the technical field of organic silicon synthesis. The preparation method comprises the following steps of: adding dimehtyl silane dichloride and diphenyl silane dichloride monomers of a certain proportion to a solvent mixture of dimethyl benzene and acetone for uniformly mixing; dropwise adding a hydrolysate mixture of acetone and water to the solvent mixture by adopting a reverse hydrolysis method; adding a certain amount of end-capping reagent after dropwise adding, continuously reacting for a certain time at 30 DEG C to end up the hydrolysis; stewing and layering, separating out lower-layer acid water, and washing the upper-layer hydrolysate to neutral by using hot distilled water to obtain siloxane prepolymer; adding a certain amount of condensation catalyst to the siloxane prepolymer to carry out the condensation reaction, and washing the crystal to neutral by using the hot distilled water; evaporating out solvent dimethyl benzene and low-boiling-point substance under the reduced pressure to obtain the methyl phenyl silicone oil. The methyl phenyl silicone oil prepared by the preparation method disclosed by the invention is clear semi-transparent oil liquid, good in product uniformity, high in purity, simple in preparation process condition, capable of recycling the solvent and easy for the industrial production.

Description

Technical field: [0001] The invention relates to a method for preparing silicone oil, in particular to a method for preparing trimethylsiloxane-terminated dimethyldiphenyl silicone oil. The product is a clear translucent oily liquid with good uniformity and high purity. Background technique: [0002] Silicone oil usually refers to a linear polysiloxane that maintains a liquid state at room temperature. The organic groups of the most commonly used silicone oil are all methyl, called methyl silicone oil, and methyl phenyl silicone oil is part of the methyl group in methyl silicone oil that is covered with benzene. The products substituted with radicals have excellent high and low temperature resistance, lubricity and radiation resistance, and are products with broad development prospects. [0003] At present, there are many preparation methods for methylphenyl silicone oil. For example, the patent CN 102070785A discloses a method based on methylphenyldichlorosilane hydrolyza...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/06C08G77/08
Inventor 殷恒波马克超胡永明毛雨林王爱丽冯永海沈灵沁谢文静
Owner JIANGSU UNIV
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