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Preparation method for hexamethylenediphenyl trisiloxane

A technology of hexamethyldiphenyltrisiloxane and hexamethyldisiloxane is applied in the field of synthesizing organosilicon compounds, and can solve the problem of low yield, difficult hexamethyldiphenyltrisiloxane, It is difficult to scale and other problems to achieve the effect of high yield and easy observation of experimental results.

Active Publication Date: 2018-05-08
GUANGDONG INST OF RARE METALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Usually, diphenyldichlorosilane or diphenyldimethoxysilane, hexamethyldisiloxane, and water are used as raw materials to undergo hydrolysis and condensation under the action of a catalyst to generate phenylpolysiloxanes with different degrees of polymerization. alkane mixture containing 2~4% of hexamethyldiphenyltrisiloxane with a single degree of polymerization, but the yield is low
In the above water phase reaction system, the hydrolysis rate of diphenyldichlorosilane or diphenyldimethoxysilane and the end-capping rate of hexamethyldisiloxane have a large difference, and two reactions will inevitably occur. Phenyldichlorosilane or diphenyldimethoxysilane self-hydrolysis condensation reaction, and it is difficult to form a large amount of hexamethyldiphenyltrisiloxane with a single degree of polymerization with the end-capping agent, so in order to obtain a large amount of Hexamethyldiphenyltrisiloxane, which is difficult to scale up by aqueous phase hydrolysis and high temperature distillation

Method used

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  • Preparation method for hexamethylenediphenyl trisiloxane
  • Preparation method for hexamethylenediphenyl trisiloxane

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 432g of n-heptane to a 2L dry four-neck flask equipped with a thermometer, a constant pressure dropping funnel, a stirrer, and a condenser, weigh 216g of diphenylsilanediol, 21.6g of a strong acid cationic resin (trade name LDX-604 ) into the flask to form a mixed dispersion. Slowly add 216g of hexamethyldisiloxane dropwise through a constant pressure dropping funnel for 1 hour. After the dropwise addition, raise the temperature to 70°C and continue stirring for 2 hours. After reaching room temperature, filter out the strongly acidic cationic resin, distill the filtrate under reduced pressure, and intercept the fraction at 172°C / 18mmHg to obtain a colorless transparent liquid, which is hexamethyldiphenyltrisiloxane. Weighing 331g, the yield is 91.94%, and the chromatographic detection content is 99.76%.

Embodiment 2

[0029] Add 648g of n-heptane to a 2L dry four-neck flask equipped with a thermometer, a constant pressure dropping funnel, a stirrer, and a condenser, weigh 216g of diphenylsilanediol, 32.4g of a strong acid cationic resin (trade name LDX-604 ) into the flask to form a mixed dispersion. Slowly add 260g of hexamethyldisiloxane dropwise through the constant pressure dropping funnel for 1 hour. After the dropwise addition, raise the temperature to 50°C and continue stirring for 3 hours. After reaching room temperature, filter out the strongly acidic cationic resin, distill the filtrate under reduced pressure, and intercept the fraction at 172°C / 18mmHg to obtain a colorless transparent liquid, which is hexamethyldiphenyltrisiloxane. Weighing 326g, the yield is 90.56%, and the chromatographic detection content is 99.56%.

Embodiment 3

[0031] Add 864g of n-heptane to a 2L dry four-neck flask equipped with a thermometer, a constant pressure dropping funnel, a stirrer, and a condenser, weigh 216g of diphenylsilanediol, and 43.2g of a strongly acidic cationic resin (trade name LDX-604 ) into the flask to form a mixed dispersion. Slowly add 324g of hexamethyldisiloxane dropwise through the constant pressure dropping funnel for 2 hours. After the dropwise addition, raise the temperature to 60°C and continue stirring for 2 hours. After reaching room temperature, filter out the strongly acidic cationic resin, distill the filtrate under reduced pressure, and intercept the fraction at 172°C / 18mmHg to obtain a colorless transparent liquid, which is hexamethyldiphenyltrisiloxane. Weighing 333g, the yield is 92.50%, and the chromatographic detection content is 99.61%.

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Abstract

The invention belongs to the technical field of synthesis of organosilicon compounds, and discloses a preparation method for hexamethylenediphenyl trisiloxane. The preparation method comprises the following steps: dropwise adding hexamethyldisiloxane into a mixed dispersing liquid of diphenyl silanediol, n-heptane and a solid acid catalyst with stirring at room temperature; after the hexamethyldisiloxane is added dropwise, rising the temperature to 50 to 70 DEG C, continuously stirring for 2 to 4 hours, cooling to room temperature, filtering to remove the solid acid catalyst, rectifyinging thefiltrate under reduced pressure, and intercepting the fraction at 172 DEG / 18mmHg to obtain the hexamethylenediphenyl trisiloxane. According to the preparation method, an anhydrous system is adopted for reacting; diphenyldimethoxysilane is prevented from performing hydrolytic condensation easily to generate a polymer in a water system. The invention provides the preparation method for the hexamethylenediphenyl trisiloxane, which is simple in process, stable in quality and high in yield.

Description

technical field [0001] The invention belongs to the technical field of synthesizing organosilicon compounds, and in particular relates to a preparation method of hexamethyldiphenyltrisiloxane. Background technique [0002] Hexamethyldiphenyltrisiloxane belongs to the category of phenyl silicone oil. It is a special structure of phenyl silicone oil with the smallest degree of polymerization, that is, the degree of polymerization is 1. It also has the properties of phenyl silicone oil, and can be used as diluent, dispersant, co-solvent, medium oil, etc. for polymer materials, coatings, paints, daily chemicals and other products. [0003] Described hexamethyldiphenyltrisiloxane structural formula is as follows: [0004] [0005] Appearance is colorless and transparent liquid, refractive index (25°C): 1.493, boiling point: 172°C / 18mmHg. [0006] Hexamethyldiphenyltrisiloxane is an important silicone product, which can be used as end-capping agent, diluent and dispersant for...

Claims

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Application Information

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IPC IPC(8): C07F7/08
CPCC07F7/0874
Inventor 朱淮军戴子林
Owner GUANGDONG INST OF RARE METALS
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