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Preparation method for allyl silane

A technology of allyl silane and alkyl, which is applied in the field of polymer synthesis, can solve problems such as unfavorable safety application, high production cost, and potential safety hazards, and achieve the effects of reducing costs, reducing equipment load, and avoiding production hazards

Inactive Publication Date: 2017-06-13
MAOMING XINLONG TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the steps in the existing Grignard method are cumbersome, not conducive to operation, and the production cost is high. In addition, organic solvents need to be used, so that there are great potential safety hazards in the production process, which is not conducive to safe application to large-scale industrial production. middle

Method used

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  • Preparation method for allyl silane
  • Preparation method for allyl silane

Examples

Experimental program
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Effect test

Embodiment 1

[0031] In a 250ml four-neck glass round bottom flask equipped with a reflux condenser, thermometer, stirrer, heater and balance feeder, under nitrogen protection, add 15 grams of magnesium chips, 25 grams of chloropropene, and 65 grams of methyl trimethoxy base silane and 0.2 g of iodine, heated to reflux for 4.5 hours, began to drop the remaining 20 g of chloropropene, and added them all in one hour. After adding, keep warm for 30 minutes to end the reaction. The analysis result of the reaction liquid showed that the yield of methyldiallylmethoxysilane was 89.55%.

Embodiment 2

[0033] In a 250ml four-neck glass round-bottomed flask equipped with a reflux condenser, thermometer, stirrer, heater and balance feeder, under nitrogen protection, add 23 grams of magnesium chips, 35 grams of chloropropene, and 110 grams of methyltrimethoxy base silane and 0.55 g of potassium iodide, heated to reflux for 4.5 hours, began to drop the remaining 30 g of chloropropene, and added them all in one hour. After adding, keep warm for 30 minutes to end the reaction. The analysis result of the reaction liquid showed that the yield of methallyldimethoxysilane was 92.75%.

Embodiment 3

[0035] In a 250ml four-neck glass round bottom flask equipped with a reflux condenser, thermometer, stirrer, heater and balance feeder, under nitrogen protection, add 10 grams of magnesium chips, 21 grams of chloropropene, 50 grams of dimethyl di Methoxysilane and a mixture of 0.6 g of iodine and potassium iodide (potassium iodide accounts for 30-55%) were heated to reflux for 5 hours, and the remaining 10 g of chloropropene was added dropwise, and the addition was completed within one hour. After adding, keep warm for 30 minutes to end the reaction. The analysis result of the reaction liquid showed that the yield of dimethylallylmethoxysilane was 91.51%.

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Abstract

The invention provides a preparation method for allyl silane. The structure general formula of the allyl silane is disclosed in formula (I), wherein R, R' and R'' are the same or different, at least one hydrolytic activity group is kept, and R, R' and R'' are respectively and independently selected from alkoxyl groups, halogen, alkyl groups, unsaturated alkyl groups or aryl groups. The preparation method comprises the following steps: S1: under a nitrogen atmosphere, mixing and heating R<1>R<2>R<3>SiR<4>, magnesium chips and a catalyst; S2: in a mixed solution of the S1, adding a certain quantity of halopropene to react; S3: enabling a reactant in S2 to react for 4-6 hours at a backflow temperature; S4: adding residual halopropene, continuously reacting, keeping the temperature for 30-50 minutes, and after reaction is finished, filtering and purifying to obtain the allyl silane. According to the preparation method provided by the invention, inflammable and explosive solvent does not need to be used for participating in the reaction, production risks are avoided, technical steps are greatly simplified, cost is lowered, a target product is synthesized at the lowest production cost, meanwhile, the product can be easily obtained, and a reaction yield is high.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and more specifically relates to a preparation method of monoallylsilane. Background technique [0002] The Grignard reaction has a history of more than 100 years. All chemists in the world who are engaged in chemical synthesis are inseparable from the research work of the Grignard reaction in their own research fields, and the Grignard reagent is a traditional Reagents commonly used in organic synthesis are widely used in the field of organic synthesis and play an important role, and various types of compounds can be prepared through it. There are many new reports on the preparation and application of Grignard reagents every year, and the research on the special properties of Grignard reagents is also deepening. Therefore, the rational and appropriate use of Grignard reagents is an indispensable condition in the field of organic synthesis. [0003] The technique of synthesizing organo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18
CPCC07F7/1804C07F7/1876
Inventor 杨晖宇
Owner MAOMING XINLONG TECH
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