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Preparation method for low-viscosity methyl phenyl hydroxyl silicone oil

A technology of methylphenyl hydroxy silicone oil and methyl phenyl hydroxy silicon, which is applied in the field of preparation of low viscosity methyl phenyl hydroxy silicone oil, can solve problems such as difficult to obtain molecular weight and low short chain hydroxy silicone oil, and achieve equipment and The effect of simple process, low cyclosiloxane content and mild reaction conditions

Active Publication Date: 2012-06-27
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] In order to solve the problem that it is difficult to obtain short-chain hydroxy silicone oil with a lower molecular weight by direct hydrolysis in the method for preparing hydroxy silicone oil, the invention provides a method for preparing low-viscosity methylphenyl hydroxy silicone oil. The methyl phenyl hydroxy silicone oil prepared by this method is Hydroxyl silicone oil has low viscosity, high hydroxyl content and high purity, and the content of methylphenylcyclosiloxane in the obtained product is extremely low

Method used

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  • Preparation method for low-viscosity methyl phenyl hydroxyl silicone oil
  • Preparation method for low-viscosity methyl phenyl hydroxyl silicone oil
  • Preparation method for low-viscosity methyl phenyl hydroxyl silicone oil

Examples

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Embodiment 1

[0027] Example 1: In a 3 L three-necked flask equipped with a thermometer, mechanical stirring and a constant pressure dropping funnel, 1 L of deionized water and 236 g of diethylamine (equivalent ratio 1.05:1) were successively added at room temperature, and the reaction flask The internal temperature was reduced to -30°C, and then 500 mL of diethyl ether was added, and then 250 mL of MePhSiCl 2 Add it dropwise to the three-necked flask at a constant speed. After the dropwise addition was completed, stirring was continued for 10 min to stop the reaction, and the reaction mixture was transferred to a separatory funnel. Let stand, separate layers, let go of the lower aqueous solution, then repeatedly wash the organic phase with an appropriate amount of deionized water to neutrality, collect the organic phase and wash it with anhydrous Na 2 SO 4 Dry overnight, filter off Na 2 SO 4 Finally, the filtrate was distilled off the solvent under reduced pressure at 40°C to obtain a ...

Embodiment 2

[0028] Example 2: In a 3 L three-necked flask equipped with a thermometer, mechanical stirring and a constant pressure dropping funnel, 1 L of deionized water and 343 g of triethylamine (equivalent ratio 1.1:1) were successively added at room temperature, and the reaction flask The internal temperature was lowered to -60°C, and then 600 mL of ether was added, and then 250 mL of MePhSiCl 2 Add it dropwise to the three-necked flask at a constant speed. After the dropwise addition was completed, stirring was continued for 10 min to stop the reaction, and the reaction mixture was transferred to a separatory funnel. Let stand, separate layers, let go of the lower aqueous solution, then repeatedly wash the organic phase with an appropriate amount of deionized water to neutrality, collect the organic phase and wash it with anhydrous Na 2 SO 4 Dry overnight, filter off Na 2 SO 4 Finally, the filtrate was distilled off the solvent under reduced pressure at 40°C to obtain a colorles...

Embodiment 3

[0029] Example 3: In a 3 L three-necked flask equipped with a thermometer, mechanical stirring and a constant pressure dropping funnel, 1 L of deionized water and 127 g of diethylenetriamine (equivalent ratio 1.2:1) were added successively at room temperature, and the reaction The temperature in the bottle was lowered to 0°C, and then 400 mL of diethyl ether was added, and then 250 mL of MePhSiCl 2 Add it dropwise to the three-necked flask at a constant speed. After the dropwise addition was completed, stirring was continued for 10 min to stop the reaction, and the reaction mixture was transferred to a separatory funnel. Let stand, separate layers, let go of the lower aqueous solution, then repeatedly wash the organic phase with an appropriate amount of deionized water to neutrality, collect the organic phase and wash it with anhydrous Na 2 SO 4 Dry overnight, filter off Na 2 SO 4 Finally, the filtrate was distilled off the solvent under reduced pressure at 40°C to obtain ...

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Abstract

The invention relates to the technical field of organic silicon industries, and provides the preparation method for low-viscosity methyl phenyl hydroxyl silicone oil in order to solve the problem that short-chain hydroxy silicone oil with low molecular weight is difficult to obtain by adopting a direct hydrolysis method in the preparation method of the hydroxyl silicone oil. The method includes: under temperature ranging from -60 DEG C to 40 DEG C and full stirring, adding MePhSiCI2 solution in weak organic alkali aqueous solution or a weak organic alkali aqueous solution / organic solvent two-phase system in dropwise mode, continuously stirring to lead full reaction after feeding is finished, standing reaction products, separating an organic phase after the reaction products are delaminated completely, washing the organic phase to neutral, drying and dewatering the organic phase and removing organic solvent to obtain the low-viscosity methyl phenyl hydroxyl silicone oil. The methyl phenyl hydroxyl silicone oil prepared by the method is low in viscosity, high in hydroxyl content and purity and very low in methyl phenyl cyclic siloxane content.

Description

technical field [0001] The invention relates to the technical field of organosilicon industry, in particular to a method for preparing low-viscosity methylphenyl hydroxy silicone oil. Background technique [0002] At present, because polydimethylsiloxane materials have excellent properties such as high and low temperature resistance, aging resistance, electrical insulation, and physiological inertia, they are widely used in aerospace, electronics, transportation, construction, chemical, textile, medical and other industries. . However, as a special silicone material, polymethylphenylsiloxane, due to the introduction of phenyl in the structural unit, the material has high temperature resistance, radiation resistance, refractive index, damping, and compatibility with traditional organic materials. Performance and other aspects are superior to polydimethylsiloxane, and it has increasingly become an important new type of silicone polymer material in the national economy. Among...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/16C08G77/06
Inventor 胡应乾邬继荣来国桥胡承刚张国栋蒋剑雄
Owner HANGZHOU NORMAL UNIVERSITY
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