Preparation method of diethyldimethoxysilane

A technology of diethyldimethoxysilane and ethyltrimethoxysilane, which is applied in the field of synthesis of the compound diethyldimethoxysilane, and can solve problems such as by-products and difficulties of triethylmethoxysilane , to achieve the effects of improved controllability, good selectivity, and mild reaction conditions

Active Publication Date: 2015-04-22
山东宝龙达新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, during the sodium condensation reaction, if the reaction process is not properly controlled, triethylmethoxysilane may also be produced as a by-product
The atmospheric boiling point of diethyldimethoxysilane is 130°C (Emeleus, H. J. Journal of the Chemical Society 1947, P1592-1594), and the atmospheric boiling point of triethylmethoxysilane is 141°C (Mironov, I. V.; Zhurnal Obshchei Khimii 1981, V51(12), P2700-2704), the boiling points of the two are relatively close, and there are certain difficulties in separation and purification by rectification

Method used

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  • Preparation method of diethyldimethoxysilane

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Experimental program
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Embodiment 1

[0022] In a dry 250mL four-necked flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistor, add 20g (0.2171 mol) of toluene, 119.8g (0.7973 mol) of ethyltrimethoxysilane, and add 12.7 g (0.5524 mol) freshly cut sodium flakes, heat up to 109°C, and beat the sodium flakes into sodium sand; within 3.5 hours, add 29.5g (0.2707 mol) bromoethane into the reaction system through the bottom tube to control the reaction The temperature is between 107~111°C. After the dropwise addition, continue to react under reflux for 3.5h. After cooling to 18.4°C, slowly add 5.0mL (0.0857 mol) ethanol to neutralize the excess metallic sodium; then mix 8.7g ( 0.0674 mol) dimethyl dichlorosilane was added dropwise to the mixture within 1.5h to neutralize the generated sodium alkoxide; after the dropwise addition was completed, the reaction was continued at this temperature for 3h. Then the reaction mixture was suction-filtered under reduced pressure to obtain 98.8 g ...

Embodiment 2

[0024]In a dry 500mL four-neck flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistor, add 20g (0.2171 mol) of toluene, 159.8g (1.0636 mol) of ethyltrimethoxysilane, and add 12.0 g of g (0.5220 mol) freshly cut sodium flakes, heated up to 103°C, and beat the sodium flakes into sodium sand; within 2.5 hours, add 29.8g (0.2734mol) bromoethane into the reaction system through the bottom tube to control the reaction The temperature is between 101~105°C. After the dropwise addition, continue the reaction under reflux for 2.5h. After cooling to 38°C, slowly add 4.0mL (0.0685 mol) ethanol to neutralize the excess metallic sodium; then mix 7.8g ( 0.0604 mol) dimethyl dichlorosilane was added dropwise to the mixture within 2.5h to neutralize the generated sodium alkoxide; after the dropwise addition was completed, the reaction was continued at this temperature for 2h. Then the reaction mixture was suction-filtered under reduced pressure to obtain 10...

Embodiment 3

[0026] In a dry 500mL four-necked flask equipped with a reflux condenser, a mechanical stirrer and a Pt-100 platinum resistance, add 199.6g (1.3285 mol) of ethyltrimethoxysilane, and add 12.4g (0.5394 mol) of freshly cut The sodium flakes were heated up to 103 °C, and the sodium flakes were beaten into sodium sand; within 2.5 hours, 29.1 g (0.2671 mol) of bromoethane was added to the reaction system through the bottom tube, and the reaction temperature was controlled between 107 and 111 °C After the dropwise addition, continue to react under reflux for 5 h. After cooling to 40°C, slowly add 6.0 mL (0.1028 mol) of ethanol to neutralize the excess metal sodium; then add 20.0 g (0.1550 mol) of dimethyl di Chlorosilane was added dropwise to the mixture within 3.5h to neutralize the generated sodium alkoxide; after the dropwise addition was completed, the reaction was continued at this temperature for 1h. Then the reaction mixture was suction-filtered under reduced pressure to obta...

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Abstract

The invention relates to the field of organic chemistry and provides a preparation method of diethyldimethoxysilane. The preparation method solves the problem that alcoholysis method-based synthesis of diethyldimethoxysilane has defects in safety and cost. The preparation method comprises that the diethyldimethoxysilane is synthesized from ethyltrimethoxysilane and bromoethane as raw materials by a sodium condensation method. The preparation method improves reaction controllability, allows mild reaction conditions, has simple processes, realizes good selectivity of diethyldimethoxysilane in a synthesized mixture, has a high yield and is suitable for large-scale industrial production.

Description

technical field [0001] The invention relates to the field of organic chemistry, in particular to a method for synthesizing a compound diethyldimethoxysilane containing silicon elements. Background technique [0002] Diethyldimethoxysilane is an important synthetic monomer. Its properties are relatively active. It is used to synthesize organosilicon intermediates and high molecular polymers. It can also be used as a structure control agent for silicone rubber. As an excellent external electron donor in the catalytic system of synthetic polypropylene (PP), it improves the overall performance of PP while improving the activity and stereoselectivity of the catalyst. [0003] Field, Leslie D et al (Field, Leslie D.; Messerle, Barbara A.; Rehr, Manuela; Soler, Linnea P.; Hambley, Trevor W. Catationic Iridium (I) Complexes as Catalysts for the Alcoholysis of Silanes. Organometallics, 2003, 22(12): 2387-2395) with diethylsilane (Et 2 SiH 2 ) and methanol as raw materials, [Ir(BPM...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18
Inventor 伍川武侠董红蒋剑雄曹健程大海
Owner 山东宝龙达新材料有限公司
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