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A kind of synthetic method of diisopropyl chlorosilane

A technology of diisopropyl chlorosilane and synthesis method, which is applied in chemical instruments and methods, compounds of elements of Group 4/14 of the periodic table, organic chemistry, etc. Problems such as the supply of kilograms and above, which are not conducive to industrial scale-up production, achieve the effect of reasonable selection and easy operation.

Active Publication Date: 2016-04-06
内蒙古佳瑞米精细化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] There are not many methods reported in the literature on the synthesis of diisopropylchlorosilane. The literature and patents use ether as a solvent. Commercial diisopropylchlorosilane is also packaged in a few grams or tens of grams, and there is no one above the kilogram level. supply
[0006] Disadvantages: The yield is 44.2%, and the reaction uses ether as a solvent, which is not conducive to industrial scale-up production
[0010] Disadvantages: The yield is 76.5%, and the reaction uses ether as a solvent, which is also not conducive to industrial scale-up production

Method used

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  • A kind of synthetic method of diisopropyl chlorosilane
  • A kind of synthetic method of diisopropyl chlorosilane
  • A kind of synthetic method of diisopropyl chlorosilane

Examples

Experimental program
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Effect test

Embodiment 1

[0024] to N 2 Add 5.10 g (0.21 mol) of magnesium chips and 15 mL of tetrahydrofuran into a 500 mL four-necked flask under protection, and add 2-chloropropane (16.81 g, 0.214 mol) into the constant dropping funnel. Quickly add about 4 mL of 2-chloropropane (about one-fifth of the total 2-chloropropane) dropwise into a 500 mL four-necked flask through a constant dropping funnel, and dilute the remaining 2-chloropropane with 90 mL of tetrahydrofuran. Heat to 40-65°C to initiate the reaction. After initiation, add the remaining 2-chloropropane solution in tetrahydrofuran dropwise, and keep the temperature at 40-65°C. After the dropwise addition, keep warm at 40-65°C for 0.5-1h, then cool to 20-30°C. A mixed solution of 13.68g (0.1mol) trichlorosilane and 41.04g n-hexane was added dropwise, the system exothermed violently and produced a large amount of white solid, the temperature was controlled at 20-30°C. After dropping, react for 0.5-1h, filter with suction, wash the filter ca...

Embodiment 2

[0026] to N 2 Add 5.10 g (0.21 mol) of magnesium chips and 15 mL of tetrahydrofuran into a 500 mL four-necked flask under protection, and add 2-chloropropane (16.81 g, 0.214 mol) into the constant dropping funnel. Quickly add about 4 mL of 2-chloropropane (about one-fifth of the total 2-chloropropane) dropwise into a 500 mL four-necked flask through a constant dropping funnel, and dilute the remaining 2-chloropropane with 90 mL of tetrahydrofuran. Heat to 40-65°C to initiate the reaction. After initiation, add the remaining 2-chloropropane solution in tetrahydrofuran dropwise, and keep the temperature at 40-65°C. After the dropwise addition, keep warm at 40-65°C for 0.5-1h, then cool to 20-30°C. A mixed solution of 13.68g (0.1mol) trichlorosilane and 41.04g n-hexane was added dropwise, the system exothermed violently and a large amount of white solids were produced, the temperature was controlled at 10-20°C. After dropping, react for 0.5-1h, filter with suction, wash the fil...

Embodiment 3

[0028] to N 2 Add 5.10 g (0.21 mol) of magnesium chips and 15 mL of tetrahydrofuran into a 500 mL four-necked flask under protection, and add 2-chloropropane (16.81 g, 0.214 mol) into the constant dropping funnel. Quickly add about 4 mL of 2-chloropropane (about one-fifth of the total 2-chloropropane) dropwise into a 500 mL four-necked flask through a constant dropping funnel, and dilute the remaining 2-chloropropane with 90 mL of tetrahydrofuran. Heat to 40-65°C to initiate the reaction. After initiation, add the remaining 2-chloropropane solution in tetrahydrofuran dropwise, and keep the temperature at 40-65°C. After the dropwise addition, keep warm at 40-65°C for 0.5-1h, then cool to 20-30°C. A mixed solution of 13.68g (0.1mol) of trichlorosilane and 41.04g of n-hexane was added dropwise, the system exothermed violently and a large amount of white solids were produced, and the temperature was controlled at 0-10°C. After dropping, react for 0.5-1h, filter with suction, was...

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Abstract

The invention relates to a synthetic method of diisopropyl chlorosilane, and belongs to the field of chemical synthesis of organic silicon halide in organic chemistry. According to the synthetic method, magnesium chips and part of tetrahydrofuran are added into a four-neck flask equipped with a mechanical stirrer, a thermometer, a reflux condensing tube and a constant-pressure dropwise adding funnel under the protection of N2 and heated to the temperature of 40-65 DEG C for initiation reaction; after initiation, a residual mixed solution of 2-chloropropane and tetrahydrofura is dropwise added at the temperature of 40-65 DEG C; after dropwise adding, the mixture reacts at the temperature of 40-65 DEG C for 0.5-3.0 h and then is cooled to subzero 10-30 DEG C; a mixed solution of trichlorosilane and n-hexane is dropwise added, a system releases heat violently and produces a large quantity of white solids; and after dropwise adding, the mixture reacts for 0.5-3.0 h and finishes the reaction, suction filtration is performed, a filter cake is washed with n-hexane, filtrates are combined, most of solvents are concentrated, rectification is performed, cut fraction at the temperature of 110-140 DEG C is collected and serves as a product, the yield is 50%-75%, and the purity is 95.0%-99.0%. According to the synthetic method, the technical route is reasonable, simple and convenient to select and easy to operate.

Description

technical field [0001] The invention belongs to the field of chemical synthesis of organohalogenated silicon in organic chemistry, and relates to the synthesis technique of preparing organohalosilane compounds by Grignard reagent method. Background technique [0002] There are not many methods reported in the literature on the synthesis of diisopropylchlorosilane. The literature and patents use ether as a solvent. Commercial diisopropylchlorosilane is also packaged in a few grams or tens of grams, and there is no one above the kilogram level. supply. Reported synthesis methods mainly include: [0003] 1) [0004] [0005] Reference: Organometallics, 29(15), 3281-3288; 2010 [0006] Disadvantages: The yield is 44.2%, and the reaction uses ether as a solvent, which is not conducive to industrial scale-up production. [0007] 2) [0008] [0009] References: Tetrahedron, 44(13), 3761-3770; 1988. [0010] Disadvantages: The yield is 76.5%, and ether is used as solven...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/12
Inventor 王荣良杨书慧董永侠陈素红
Owner 内蒙古佳瑞米精细化工有限公司
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