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Preparation method for octaphenylcyclotetrasiloxane

A technology of octaphenylcyclotetrasiloxane and diphenylsilanediol, which is applied in the field of synthesizing organosilicon compounds, can solve problems such as difficult separation and recovery, pollution, and inability to recycle, and achieves mild temperature and high yield , Avoid the effect of the introduction of chloride ions

Active Publication Date: 2017-07-21
广东省科学院产业技术育成中心
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method can obtain octaphenylcyclotetrasiloxane under relatively mild conditions, but a large amount of mixed solvent of methanol and acetone is produced by-product, and the mixed solvent cannot be recycled, because as methanol continues to increase, it will inhibit dimethyl Hydrolysis of oxydiphenylsilane, resulting in decreased yield
Moreover, the boiling points of methanol and acetone are very close, so it is difficult to separate and recover, resulting in a large amount of solvent waste and pollution

Method used

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  • Preparation method for octaphenylcyclotetrasiloxane
  • Preparation method for octaphenylcyclotetrasiloxane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Add 1000g of diphenylsilanediol with a mass percentage of 99.5% and 1000g of methanol into a 5L three-necked flask, stir until completely dissolved, add 0.02g of sodium hydroxide, heat the solution to 60°C, reflux for 4h; cool to room temperature, Stand still for 5 hours to fully crystallize octaphenylcyclotetrasiloxane, then filter with a 500-mesh filter cloth, centrifuge the filter cake at a speed of 2000 rpm for 30 minutes, and spin dry it at -0.099MPa and 40°C After 4 hours, the water and methanol adsorbed on the surface were removed to obtain dry needle-shaped crystals, namely octaphenylcyclotetrasiloxane, weighing 889g, yield 97.48%, content detected by liquid chromatography 99.3%, melting point 203°C.

Embodiment 2

[0028] Add 1000g of diphenylsilanediol with a mass percentage of 99.5% and 2000g of methanol into a 5L three-necked flask, stir until completely dissolved, add 0.3g of sodium hydroxide, heat the solution to 62°C, reflux for 5h; cool to room temperature, Stand still for 6 hours to fully crystallize octaphenylcyclotetrasiloxane, then filter with 600-mesh filter cloth, centrifuge the filter cake at 1800 rpm for 40 minutes, and spin-dry it at -0.098MPa and 50°C After 4 hours, the water and methanol adsorbed on the surface were removed to obtain dry needle-shaped crystals, namely octaphenylcyclotetrasiloxane, weighing 896g, yield 98.24%, liquid chromatography detection content 99.5%, melting point 203°C.

Embodiment 3

[0030] Add 1000g of diphenylsilanediol with a mass percentage of 99.8% and 3000g of methanol into a 5L three-necked flask, stir until completely dissolved, add 2g of potassium hydroxide, heat the solution to 64°C, reflux for 6h; cool to room temperature, Stand still for 8 hours to fully crystallize octaphenylcyclotetrasiloxane, then filter with 800-mesh filter cloth, centrifuge the filter cake at 1600 rpm for 45 minutes, and spin-dry it at -0.095MPa and 60°C After 5 hours, the water and methanol adsorbed on the surface were removed to obtain dry needle-shaped crystals, namely octaphenylcyclotetrasiloxane, weighing 892g, yield 97.81%, liquid chromatography detection content 99.7%, melting point 203°C.

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Abstract

The invention discloses a preparation method for octaphenylcyclotetrasiloxane, belonging to the field of synthesis of organo silicon compounds. The preparation method comprises the following steps: adding diphenylsilanediol and methanol in a certain mass ratio into a reaction container and carrying out stirring until diphenylsilanediol and methanol are totally dissolved; then adding an alkaline catalyst; carrying out heating to 60 to 65 DEG C and carrying out reflux for 4 to 6 h; then carrying out cooling to room temperature and standing for 5 to 8 h; and successively carrying out filtering and drying so as to obtain the acicular crystal octaphenylcyclotetrasiloxane. According to the invention, diphenylsilanediol free of chlorine is used as a raw material and introduction of chloride ions is avoided, so reaction temperature is mild, crystallization is carried out at normal temperature and the crystal is easy to filter and separate; solvents are recyclable and pose no influence to reaction effect; and the preparation method for octaphenylcyclotetrasiloxane is simple in process, and prepared octaphenylcyclotetrasiloxane has stable quality and high yield.

Description

technical field [0001] The invention belongs to the field of synthesizing organosilicon compounds, and in particular relates to a method for preparing high-purity octaphenylcyclotetrasiloxane by a crystallization method. Background technique [0002] Octaphenylcyclotetrasiloxane is an important organic silicon intermediate, which can be used to synthesize pharmaceutical intermediates, phenyl silicone oil, phenyl silicone resin, phenyl silicone rubber, etc.; it can also be used as polyurethane resin, epoxy resin , modified intermediates of acrylic resin, PP, PET, PE, etc., endowing new products with high and low temperature resistance, radiation resistance, aging resistance and other properties. [0003] Described octaphenyl cyclotetrasiloxane structural formula is: [0004] [0005] Appearance is white needle crystal, melting point is 203°C, boiling point is 334°C. [0006] The prior art synthesizes octaphenylcyclotetrasiloxane using diphenyldichlorosilane as a raw mate...

Claims

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Application Information

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IPC IPC(8): C07F7/21
CPCC07F7/21
Inventor 朱淮军陈维洪汪涛张旻李向阳
Owner 广东省科学院产业技术育成中心
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