Preparation method of methylphenyldialkoxysilane

A methylphenyl dialkoxysilane and a purpose technology, applied in the field of preparing methylphenyl dialkoxysilane, can solve the problem of low selectivity of the target product, low conversion rate of the target product, and increase the selection of the target product The effect of simplifying the post-processing process, being easy to control, and shortening the reaction time

Active Publication Date: 2012-02-15
CHINA BLUESTAR CHENGRAND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The present invention overcomes the disadvantages of long reaction period, low selectivity of the target product and low conversion rate of the target product existing in the original sodium condensation method, adopts ultrasonic wave to promote the reaction, and can shorten the reaction time; by increasing the amount of methyl triethoxy The ratio of the amount of base silane raw materials, on the one hand, it plays the role of solvent, o

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] 80.1g MeSi(OEt) 3 and 6.9 g of metallic sodium were added into a three-necked flask equipped with an ultrasonic generator, an electromagnetic stirrer, a reflux condenser, and a thermometer, and the temperature was raised to 100° C. under stirring. Start the stirring and ultrasonic generator. At this temperature, gradually drop 16.9g of chlorobenzene into the three-necked flask within 0.5h. The dropping speed keeps the temperature of the material below 145°C. After the dropping, keep stirring and ultrasonic irradiation for 3h. Stop the ultrasound, and cool the material in the three-necked bottle to 3 The material was neutralized to neutral, and the solid residue was removed by filtration to obtain a crude product, which was analyzed by gas chromatography, which contained MeSi(OEt) 3 48g, the recovery rate is 89.9%; containing MePhSi(OEt) 2 25.3 g, 80.03% yield (vs sodium).

Embodiment 2

[0045] 160g MeSi(OEt) 3 and 6.9 g of metallic sodium were added into a three-necked flask equipped with an ultrasonic generator, an electromagnetic stirrer, a reflux condenser, and a thermometer, and the temperature was raised to 100° C. under stirring. Start the stirring and the ultrasonic generator. At this temperature, gradually drop 20.2g of chlorobenzene into the three-necked flask within 0.5h. The dropping speed keeps the temperature of the material below 137°C, and then keep it for 3h after the dropping. Stop the ultrasound, and cool the material in the three-necked bottle to 3 The material was neutralized to neutral, and the solid residue was removed by filtration to obtain a crude product, which was analyzed by gas chromatography, which contained MeSi(OEt) 3 127.9g, the recovery rate is 95.9%; containing MePhSi(OEt) 2 27.1 g, yield (vs sodium) 86.03%.

Embodiment 3

[0047] 81.6g MeSi(OMe) 3 and 6.9 g of metallic sodium were added into a three-necked flask equipped with an ultrasonic generator, an electromagnetic stirrer, a reflux condenser, and a thermometer, and the temperature was raised to 90° C. under stirring. Start the ultrasound, and at this temperature, gradually drop 18.56g of chlorobenzene into the three-necked flask within 0.5h. The dropping speed keeps the temperature of the material below 105°C, and then keep it for another 2h after the dropping. Stop the ultrasound, and cool the material in the three-neck flask to 3 The material is neutralized to neutral, and the solid residue is removed by filtration to obtain a crude product, which is analyzed by gas chromatography, which contains MeSi(OMe) 3 53.8g, recovery rate 87.9%; containing MePhSi(OMe) 2 22.2 g, 81.3% yield (vs sodium).

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Abstract

The invention discloses a method for preparing methylphenyldialkoxysilane under ultrasonic assistance through the sodium condensation method by using excess MeSi(OR)3 and chlorobenzene. The target product is prepared from the following raw materials: MeSi(OR)3, PhCl and Na, wherein the molar ratio of MeSi(OR)3 to PhCl to Na is (3-6): (1-1.2):2, wherein R in the formula of MeSi(OR)3 is Me or Et; and the purity of the product is not less than 99%. The method is characterized in that the raw materials are fewer in type, too many side reactions can be avoided, the operational program and post-treatment process are simplified, ultrasonic irradiation is introduced to improve the dispersion of microscopic materials on the surface of sodium sand in the reaction system, thus the reaction can be performed more smoothly and safer, the reaction time can be greatly shortened, the reaction efficiency can be increased and the selectivity to the target product is high.

Description

Technical field [0001] The present invention involves a preparation method of a methane alkaneoxyxane, especially the use of excess MESI (or) under ultrasound auxiliary conditions 3 The method of reducing the sodium chlorine to prepare methane alkaneoxyxane. Background technique [0002] In the polysilicine material, when the main chain silicon atom with benzyl, it can give it excellent high and low temperature resistance, high energy radiation and damping vibration reduction performance.Patients, improve the discount rate of polysilicide.When a polysilicide containing phenyl -containing is matched with the discount rate of the selected filler, transparent materials can be obtained. [0003] In the organic silicon synthetic material industry, phenyl silicon monomer is another type of important basic raw materials except methyl silicon monomer. Its dosage is second only to methyl silicon monomer and is synthetic phenyl silicon oil and benzene siliconBasic monomers of rubber and be...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 潘涛唐小斗
Owner CHINA BLUESTAR CHENGRAND CO LTD
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