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One-step synthesizing cyclohexyl methyl dimethoxy silane without solvent

A technology of cyclohexylmethyldimethoxysilane and methyltrimethoxysilane, which is applied in the field of chemical raw materials, can solve problems such as harsh production and reaction conditions, high pressure requirements, and high risk, and achieve simple synthesis reaction operations Ease of operation, small equipment load and reasonable process

Inactive Publication Date: 2004-09-29
RES & DESIGN INST WUHAN CHEM COLLEGE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest advantage of the improvement of the above process is that the yield is high, and the raw materials are easy to get and cheap, but the production and reaction conditions are harsh, the pressure requirement is high, and the risk is relatively high.

Method used

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  • One-step synthesizing cyclohexyl methyl dimethoxy silane without solvent
  • One-step synthesizing cyclohexyl methyl dimethoxy silane without solvent
  • One-step synthesizing cyclohexyl methyl dimethoxy silane without solvent

Examples

Experimental program
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Effect test

example 1

[0041] In a 250ml glass round bottom flask with reflux condenser, thermometer, stirrer, heater and balance feeder, under N 2 Add 12 grams of fresh magnesium powder, 56 grams of methyltrimethoxysilane, 5 grams of chlorocyclohexane and 0.2 gram of iodine under protection, and heat to keep the material under stable reflux. After reflux for 30 minutes, start to drop the remaining 41 grams of chlorocyclohexane. Cyclohexane was added completely in about 1 hour. After adding, keep warm for 30 minutes to end the reaction. The analysis results of the reaction solution showed that the conversion rate of cyclohexylmethyldimethoxysilane was 90.3% (calculated as silane), and the yield of cyclohexylmethyldimethoxysilane was 91.4%.

example 2

[0043] In a 500ml four-neck glass round bottom flask with a reflux condenser, thermometer, stirrer, heater and balance feeder, under N 2 Under protection, add 37 grams of fresh magnesium powder, 152 grams of methyltrimethoxysilane, 12 grams of chlorocyclohexane and 0.6 gram of potassium iodide, heat to keep the material under stable reflux, and after 30 minutes of reflux, start to add the remaining 138 grams of chlorine Substituting cyclohexane, use the time of about 1.5 hours to add all of them. After adding, keep warm for 30 minutes to end the reaction. The analysis results of the reaction solution showed that the conversion rate of cyclohexylmethyldimethoxysilane was 89.2% (calculated as silane), and the yield of cyclohexylmethyldimethoxysilane was 91.5%.

example 3

[0045] In a 500ml four-neck glass round bottom flask with a reflux condenser, a thermometer, a stirrer, a heater and a balance feeder, under N 2Under protection, add 37 grams of fresh magnesium powder, 152 grams of methyltrimethoxysilane, 12 grams of chlorocyclohexane and 0.6 gram of iodine and potassium iodide mixture (potassium iodide accounts for 20-60%), heat to keep the material stable reflux, reflux After 30 minutes, start to add the remaining 138 grams of chlorocyclohexane dropwise, and use the time of about 1.5 hours to add all of it. After adding, keep warm for 30 minutes to end the reaction. The analysis results of the reaction solution showed that the conversion rate of cyclohexylmethyldimethoxysilane was 91.5% (calculated as silane), and the yield of cyclohexylmethyldimethoxysilane was 93.1%.

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Abstract

The solvent-free one-step process of synthesizing cyclohexyl methyl dimethoxy silane with methyl dimethoxy silane, cyclohexane halide and magnesium powder in the molar ratio of 1 to 1 to 1-1.5 as material includes compounding material; mixing and heating methyl dimethoxy silane, magnesium powder and catalyst in the amount of 0.1-0.5 % of methyl dimethoxy silane under the protection of N2 and through stirring; dropping slowly 5-15 % of cyclohexane halide; refluxing the materials inside the reactor for 30-40 min while maintaining the temperature; dropping the residual cyclohexane halide; maintaining the temperature for one other 30-40 min; and cooling, filtering and rectifying the filtrate to obtain cyclohexyl methyl dimethoxy silane product. The present invention has the advantages of reasonable, simple and practical process, high yield and high conversion rate, etc.

Description

technical field [0001] The invention relates to the field of chemical raw materials, in particular to a solvent-free one-step method for synthesizing cyclohexylmethyldimethoxysilane. Background technique [0002] Cyclohexylmethyldimethoxysilane [C 6 h 11 CH 3 Si(OCH 3 ) 2 ], referred to as CMMS, also known as Dornor-C in industry. As a polypropylene production aid - electron donor, it plays a very important role in production and can improve the isotacticity of polypropylene products. Its synthesis process route mainly has three categories: organoalkali metal method, hydrosilylation method, Grignard reagent method. Among them, the Grignard reagent method and the hydrosilylation method are more, and they are all synthesized by a two-step method with a solvent. [0003] In organosilicon chemistry, the synthesis method of Grignard reagent is very important. For a long time, scholars have discussed in detail the activity of organic groups on silicon atoms and halogens in ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/08C07F7/18
Inventor 陈发德胡海平黄绪棚熊福胜董家庆
Owner RES & DESIGN INST WUHAN CHEM COLLEGE
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