Reaction system and synthetic method for producing chloropropyl triethoxy silicane continuously

A technology of chloropropyltriethoxysilane and chloropropyltrichlorosilane, which is applied in the field of reaction devices for synthesizing chloropropyltriethoxysilane, can solve the problem of containing more hydrogen chloride, long synthesis reaction cycle, and production cost Advanced problems, to achieve the effect of low production cost, short reaction cycle and easy operation

Inactive Publication Date: 2007-12-26
HARBIN INST OF TECH
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  • Abstract
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Problems solved by technology

[0005] The purpose of the present invention is to provide a continuous production of chloropropyl triethoxysilane in order to solve the problems of long synthesis reaction cycle, high energy cons

Method used

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  • Reaction system and synthetic method for producing chloropropyl triethoxy silicane continuously

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specific Embodiment approach 1

[0010] Specific embodiment one: (referring to Fig. 1) the reaction system of this embodiment consists of chloropropyl trichlorosilane storage tank 1, ethanol storage tank 2, esterification reactor 5, safety valve 6, pressure gauge 7, agitator 8, First heat exchanger 9, thermocouple 10, heater and temperature controller 11, temperature control resistance wire 12, primary product storage tank 13, second heat exchanger 14, stripping tower 15, third heat exchanger 16, Outlet valve 17, sampling valve 18, the first ceramic pump 19 and the second ceramic pump 20 for air extraction; port is communicated, the liquid outlet at the bottom of the ethanol storage tank 2 is communicated with the liquid inlet of the second heat exchanger 14, and the gas outlet of the second heat exchanger 14 is communicated with the air inlet of the stripping tower 15 bottom, and the gas stripping tower 15 The air outlet at the top communicates with the air inlet of the third heat exchanger 16, the air outle...

specific Embodiment approach 2

[0011] Embodiment 2: The packing in this embodiment is ceramic Pall ring packing, Raschig ring, ceramic saddle ring packing or saddle packing. Other structures and connection methods are the same as those in the first embodiment.

specific Embodiment approach 3

[0012] Specific embodiment three: this embodiment adopts the reaction system in specific embodiment one to synthesize chloropropyl triethoxysilane, and the synthetic method is as follows: the purity is 99% chloropropyl trichlorosilane and dehydrated alcohol by 1: 3.15 Feed at a molar ratio of ~3.3, the reaction pressure is maintained between -0.03 ~ -0.09MPa, the reaction cycle is 3 ~ 3.5h, add absolute ethanol continuously during the reaction cycle, and the reaction temperature increases from 25°C with the addition of absolute ethanol The temperature is raised to 50°C; during the reaction, chloropropyltrichlorosilane is directly added to the esterification reactor 5, and the absolute ethanol is heated to 90-115°C through the second heat exchanger 14 and then enters the stripping tower 15, and the initial product After the mass transfer and heat transfer, the top of the stripper 15 enters the esterification reactor 5 through the third heat exchanger 16 to undergo an esterificat...

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Abstract

This invention relates to reaction system and synthesis method for continuously producing chloropropyl triethoxy silane by esterification reaction. This invention solves the problems of long synthesis period, high energy consumption, high production cost and high HCl content in the crude product faced by the present chloropropyl triethoxy silane synthesis reaction. The liquid outlet at the bottom of the ethanol storage tank of the reaction system is through connected with the liquid inlet of the second heat exchanger. The gas outlet of the second heat exchanger is through connected with the gas inlet at the lower part of the stripping column. The gas outlet at the top of the stripping column is through connected with the gas inlet of the third heat exchanger. The gas outlet of the third heat exchanger is through connected with the gas inlet of the first ceramic suction pump. The liquid out of the third heat exchanger is through connected with the liquid inlet of the esterification reactor. This invention has such advantages as simple apparatus structure, easy operation and low space occupation.

Description

technical field [0001] The invention relates to a reaction device and a synthesis method for synthesizing chloropropyltriethoxysilane. Background technique [0002] The traditional synthetic route of chloropropyltriethoxysilane is esterification reaction between chloropropyltrichlorosilane and ethanol at 80-100°C and 0.03MPa. The reaction formula is: [0003] ClCH 2 CH 2 CH 2 SiCl 3 +CH 3 CH 2 OH→ClCH 2 CH 2 CH 2 Si(OCH 2 CH 3 ) 3 +HCl [0004] Ethanol is added in batches, and the reaction time is about 6 hours. After the reaction, it is refluxed at 0.03 MPa for about 3 hours, and the total reaction time is about 10 hours or more. Finally, the crude product is neutralized by the neutralizing agent sodium ethoxide, and then put into a rectification tower for rectification to obtain chloropropyltriethoxysilane. The main disadvantage of the traditional process is that the esterification reaction is carried out under the process conditions of constant temperature ...

Claims

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Application Information

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IPC IPC(8): C07F7/18
Inventor 张磊杨春晖张巨生
Owner HARBIN INST OF TECH
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