Preparation method of methyl phenyl silicone oil with high refractive index

A technology of methyl phenyl silicone oil and high refractive index is applied in the field of preparation of high refractive index methyl phenyl silicone oil to achieve the effects of good uniformity, high catalytic activity and low cost

Inactive Publication Date: 2013-11-27
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above method mainly uses cyclosiloxane as a raw material to prepare methylphenyl silicone oil, which increases the cost of product preparation and is not conducive to industrial production. At the same time, the above-mentioned monomers cannot be used as raw materials to prepare methylphenyl silicone oil with high phenyl content.
And patent CN 102516546A has announced a kind of use methylphenyl dichlorosilane as raw material, weak organic base aqueous solution is neutralizer to prepare low viscosity methylphenyl hydroxy silicone oil, although this method raw material is cheap, but adds a large amount of weak Organic bases increase the cost of industrial production

Method used

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  • Preparation method of methyl phenyl silicone oil with high refractive index
  • Preparation method of methyl phenyl silicone oil with high refractive index

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The Ph / R ratio (molar ratio) was 0.35. Add 80 mL of xylene, 50 mL of acetone, 10.32 g of dimethyldichlorosilane, 19.11 g of methylphenyldichlorosilane, and 5.06 g of diphenyldichlorosilane into a 500 mL three-neck flask, stir and mix at 30 °C Uniform; add 100 mL of acetone and 57.6 g of distilled water to the three-necked flask drop by drop with a constant pressure titration funnel. Continue the reaction for 10 h, and the hydrolysis is completed; let stand to separate the layers, separate the lower layer of acid water, and wash the upper layer of hydrolyzate with distilled water at 50-60 °C until neutral to obtain a siloxane prepolymer, and then add 0.811 g of six Methyldisiloxane and 0.3450 g condensation catalyst stannous octoate (the mass is 1% of the total mass of the monomers) were subjected to condensation reaction for 4 h. After the reaction, the catalyst was washed away with distilled water at 50-60 °C until it was neutral, and then at 130 The solvent xylene an...

Embodiment 2

[0030] The Ph / R ratio (molar ratio) was 0.55. Add 80 mL of xylene, 50 mL of acetone, 5.16 g of dimethyldichlorosilane, 19.11 g of methylphenyldichlorosilane, and 15.19 g of diphenyldichlorosilane into a 500 mL three-neck flask, stir and mix at 30 °C Uniform; add 100 mL of acetone and 57.6 g of distilled water to the three-necked flask drop by drop with a constant pressure titration funnel. Continue the reaction for 10 h, and the hydrolysis is completed; let stand to separate the layers, separate the lower layer of acid water, and wash the upper layer of hydrolyzate with distilled water at 50-60 °C until neutral to obtain a siloxane prepolymer, and then add 0.811 g of six Methyldisiloxane and 0.3947 g condensation catalyst stannous octoate (mass is 1% of the total monomer mass) were subjected to condensation reaction for 4 h. After the reaction, the catalyst was washed with distilled water at 50-60 °C until it was neutral, and then at 130 The solvent xylene and low boilers wer...

Embodiment 3

[0032] The Ph / R ratio (molar ratio) was 0.65. Add 80 mL of xylene, 50 mL of acetone, 2.58 g of dimethyldichlorosilane, 19.11 g of methylphenyldichlorosilane, and 20.26 g of diphenyldichlorosilane into a 500 mL three-neck flask, stir and mix at 30 °C Uniform; add 100 mL of acetone and 57.6 g of distilled water to the three-necked flask drop by drop with a constant pressure titration funnel. Continue the reaction for 10 h, and the hydrolysis is completed; let stand to separate the layers, separate the lower layer of acid water, wash the upper layer of hydrolyzate with distilled water at 50-60 °C until neutral to obtain a siloxane prepolymer, and then add 0.811g of six at 100 °C Methyldisiloxane and 0.4195 g condensation catalyst stannous octoate (the mass is 1% of the total mass of the monomers) were subjected to condensation reaction for 4 h. After the reaction, the catalyst was washed with distilled water at 50-60 °C until it was neutral, and then at 130 The solvent xylene an...

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Abstract

The invention relates to a preparation method of methyl phenyl silicone oil with high refractive index, and belongs to the technical field of organosilicon synthesis. The method is as below: using dimethyl dichlorosilane, diphenyl dichlorosilane and dichloromethyl phenylsilane as polymerization monomers; adding the monomers into a solvent while stirring at 30 DEG C; uniformly stirring; dropwise adding a proper amount of a hydrolysate; continuing to react until the end of hydrolysis; standing for layering; separating out a lower layer of acid water; washing an upper layer organic phase to a neutral state to obtain a siloxane prepolymer; adding a proper amount of an end-capping reagent and a condensation catalyst into the siloxane prepolymer to carry out a condensation reaction; after the reaction, washing out the catalyst to a neutral state; and steaming out the solvent of xylene and low-boiling-point substances under reduced pressure to obtain the silicone oil. The methyl phenyl silicone oil prepared by the invention is a clarified transparent oily liquid with high refractive index, good product uniformity, high purity and good high temperature resistance; and the preparation technology is simple and easy for industrialization.

Description

Technical field: [0001] The invention relates to a method for preparing silicone oil, in particular to a method for preparing methylphenyl silicone oil with a high refractive index. Background technique: [0002] Methyl phenyl silicone oil is one of the main products of silicone oil. Due to the introduction of phenyl groups, methyl phenyl silicone oil has good heat resistance, chemical stability, electrical insulation, radiation resistance, etc., making methyl phenyl silicone oil Silicone-based oil has been widely used in many fields, especially in personal care, defense industry, aerospace, and is a product with broad development prospects. The demand for methylphenyl silicone oil is increasing year by year, and the research on its new varieties and new processes has become a hot spot in the silicone industry. [0003] At present, there are many preparation methods for methyl phenyl silicone oil, mainly by hydrolysis condensation method and catalytic equilibrium method. ...

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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