CN110563754B - A alcoholysis reaction system for producing chloromethyl triethoxysilane - Google Patents

A alcoholysis reaction system for producing chloromethyl triethoxysilane Download PDF

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CN110563754B
CN110563754B CN201910715455.4A CN201910715455A CN110563754B CN 110563754 B CN110563754 B CN 110563754B CN 201910715455 A CN201910715455 A CN 201910715455A CN 110563754 B CN110563754 B CN 110563754B
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alcoholysis reaction
pipe
ethanol
reaction tower
alcoholysis
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CN110563754A (en
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刘寒迁
杜启明
李进红
张明义
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Qianjiang Yisheng New Material Co ltd
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    • C07ORGANIC CHEMISTRY
    • C07FACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
    • C07F7/00Compounds containing elements of Groups 4 or 14 of the Periodic Table
    • C07F7/02Silicon compounds
    • C07F7/08Compounds having one or more C—Si linkages
    • C07F7/18Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
    • C07F7/1804Compounds having Si-O-C linkages
    • C07F7/1872Preparation; Treatments not provided for in C07F7/20
    • C07F7/188Preparation; Treatments not provided for in C07F7/20 by reactions involving the formation of Si-O linkages
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The invention relates to the technical field of silane coupling agent production, and discloses an alcoholysis reaction system for producing chloromethyl triethoxysilane, which comprises: the alcoholysis reaction tower is communicated with the upper part of the reaction kettle, a mixed feeding pipe and a vaporization feeding pipe are arranged on the alcoholysis reaction tower, a tail gas outlet pipe is arranged at the top of the alcoholysis reaction tower and connected with a multi-stage condensation mechanism, condensate of the multi-stage condensation mechanism is introduced into the alcoholysis reaction tower through a condensation recovery pipe, uncondensed gas of the multi-stage condensation mechanism enters a tail gas acid removal absorption tower through an acid removal pipeline, and the reaction kettle is connected with a discharging pipe. The invention improves the purity of the product chloromethyl triethoxysilane, and has high productivity and high production efficiency.

Description

A alcoholysis reaction system for producing chloromethyl triethoxysilane
Technical Field
The invention relates to the technical field of production of silane coupling agents, in particular to an alcoholysis reaction system for producing chloromethyl triethoxysilane.
Background
In recent years, organosilicon products have become indispensable chemical materials for developing, producing and improving living environment, and the demand of the organosilicon products is also multiplied. Chloromethyl triethoxy silane ClCH 2 Si(OCH 2 CH 3 ) 3 Reacting with diethylamine to generate diethylamine methyl triethoxysilane, commonly known as ND-22, which is an important silane coupling agent in chemical products.
Chloromethyltrichlorosilane (ClCH) is generally used in the prior art 2 SiCl 3 ) And (3) preparing chloromethyl triethoxysilane by an ethanol alcoholysis method. This method produces a large amount of hydrogen chloride (HCl) as a by-product during the reaction. HCl in chloromethyltriethoxysilane ClCH 2 Si(OCH 2 CH 3 ) 3 If the solubility of the product is extremely high and the product cannot be discharged in time, the main reaction is not facilitated, and the yield and the quality of the product are seriously influenced.
Disclosure of Invention
The invention aims to provide a continuous production alcoholysis reaction system for producing chloromethyl triethoxysilane, which has the advantages of high separation efficiency of hydrogen chloride and chloromethyl triethoxysilane, high yield of chloromethyl triethoxysilane and high purity of more than 90%.
The technical purpose of the invention is realized by the following technical scheme: an alcoholysis reaction system for producing chloromethyl triethoxysilane, comprising: the alcoholysis reaction tower is communicated with the upper part of the reaction kettle, a mixed feeding pipe and a vaporization feeding pipe are arranged on the alcoholysis reaction tower, a tail gas outlet pipe is arranged at the top of the alcoholysis reaction tower and connected with a multi-stage condensation mechanism, condensate of the multi-stage condensation mechanism is introduced into the alcoholysis reaction tower through a condensation recovery pipe, uncondensed gas of the multi-stage condensation mechanism enters a tail gas acid removal absorption tower through an acid removal pipeline, and the reaction kettle is connected with a discharging pipe.
By adopting the technical scheme, the height of the alcoholysis reaction tower is about 10-20 m, the chloromethyl trichlorosilane can carry out alcoholysis reaction with ethanol in the alcoholysis reaction tower to generate a product chloromethyl triethoxysilane and gaseous hydrogen chloride, the boiling point of the product chloromethyl triethoxysilane is high, and the temperature of the alcoholysis reaction tower is slightly higher than that of the ethanol, so that on one hand, vaporized ethanol introduced from the lower part can blow away hydrogen chloride gas from the product chloromethyl triethoxysilane, the product chloromethyl triethoxysilane is sent to a multistage condensation mechanism for treatment, and finally, the product chloromethyl triethoxysilane enters a tail gas acid removal absorption tower through an acid removal pipeline for treatment, and on the other hand, the reaction rate of the alcoholysis reaction is accelerated; multistage condensation mechanism can circulate ethanol condensation and let in reaction and vaporization separation hydrogen chloride in the alcoholysis reaction tower, constantly separates out hydrogen chloride from chloromethyl triethoxysilane, improves chloromethyl triethoxysilane's purity.
As a further configuration of the invention: the device also comprises a pre-reactor, wherein a chlorine feeding pipe and a first ethanol feeding pipe are arranged on the pre-reactor, and a discharge port of the pre-reactor is connected with a mixed feeding pipe.
By adopting the technical scheme, the chloromethyl trichlorosilane and the ethanol can be premixed and reacted firstly, so that the subsequent reaction degree and reaction speed are improved.
As a further configuration of the invention: the top end of the pre-reactor is connected with the tail gas eduction tube.
By adopting the technical scheme, a part of the byproduct hydrogen chloride can be led out for treatment, the amount of the byproduct entering the alcoholysis reaction tower is reduced, the product purity is improved, and the cost consumed by separation is reduced.
As a further configuration of the invention: the device also comprises a reboiler, wherein one end of the reboiler is connected with a second ethanol feeding pipe, and the other end of the reboiler is connected with the vaporization feeding pipe.
By adopting the technical scheme, the reboiler generates a large amount of vaporized ethanol with higher temperature, the vaporized ethanol with higher temperature enters from the lower part of the alcoholysis reaction tower and rapidly rises, the generated hydrogen chloride is rapidly carried away from the alcoholysis reaction tower, and the separation efficiency is high.
As a further configuration of the invention: still include the product circulating pipe, product circulating pipe one end passes through the discharge gate of hydraulic pump connection reation kettle, and the other end links to each other with the alcoholysis reaction tower.
By adopting the technical scheme, the reflux product in the alcoholysis reaction tower comprises chloromethyl triethoxysilane and unreacted chloromethyl trichlorosilane, the product is subjected to circular reaction, the chloromethyl trichlorosilane in the product can be fully reacted, and the content of the chloromethyl triethoxysilane in the product is improved.
As a further setting of the invention: the multistage condensation mechanism comprises a first-stage condenser, a second-stage condenser, a third-stage condenser, a first-stage condensing tank, a second-stage condensing tank, a third-stage condensing tank and a gas pipeline, wherein the gas pipeline is sequentially connected with the first-stage condenser, the first-stage condensing tank, the second-stage condenser, the second-stage condensing tank, the third-stage condenser, the third-stage condensing tank and an acid removal pipeline, and condensate of the first-stage condensing tank, the second-stage condensing tank and the third-stage condensing tank is introduced into the alcoholysis reaction tower through a condensation recovery pipe.
By adopting the technical scheme, the condenser only condenses and recovers the ethanol, the hydrogen chloride gas is finally introduced into the tail gas acid removal absorption tower to be absorbed, and the multistage condenser and the multistage condensing tank are adopted, so that the separation degree of the hydrogen chloride gas and the ethanol can be improved, the purity of the hydrogen chloride which finally enters the tail gas acid removal absorption tower to be recovered is improved, and the content of the hydrogen chloride which enters the alcoholysis reaction tower is also reduced.
As a further configuration of the invention: the discharge port of the reaction kettle is also connected with a neutralization kettle through a pipeline, and a magnesium powder tank is arranged on the neutralization feed port of the neutralization kettle.
By adopting the technical scheme, the product discharged from the reaction kettle is finally neutralized and absorbed by the dissolved hydrogen chloride in the neutralization tank, and finally the dissolved hydrogen chloride in the product chloromethyl triethoxysilane is thoroughly removed by crystallization, separation and other modes, so that the purity of the product chloromethyl triethoxysilane is ensured.
As a further configuration of the invention: the mixed feeding pipe and the product circulating pipe are both connected with the upper part of the alcoholysis reaction tower, and the first ethanol feeding pipe is connected with the lower part of the alcoholysis reaction tower.
As a further configuration of the invention: and introducing the chloromethyl trichlorosilane and ethanol into the alcoholysis reaction system in a weight ratio of 1: 0.5-0.7.
As a further configuration of the invention: the weight ratio of ethanol flowing through the first ethanol feed pipe to ethanol flowing through the second ethanol feed pipe is 2: 1.
The invention has the beneficial effects that: when chloromethyl triethoxysilane is produced, chloromethyl trichlorosilane is fed into the pre-reactor through a chlorine feeding pipe, a part of ethanol enters the pre-reactor through a first ethanol feeding pipe to react with the chloromethyl trichlorosilane spontaneously and violently, a reaction product enters the alcoholysis reaction tower from the upper part, and the other part of ethanol enters the alcoholysis reaction tower from the lower part after being vaporized through a reboiler through a second ethanol feeding pipe.
The method is characterized in that the monochloromethyltrichlorosilane and ethanol spontaneously carry out alcoholysis reaction at normal temperature and normal pressure, the reaction is violent, the product generates chloromethyltriethoxysilane and hydrogen chloride gas, the solubility of the hydrogen chloride in the chloromethyltriethoxysilane is higher, and therefore the generated hydrogen chloride needs to be separated from the chloromethyltriethoxysilane in time during the alcoholysis reaction. According to the invention, chloromethyl trichlorosilane and ethanol are firstly added into a pre-reactor to be mixed and preliminarily pre-reacted, then the mixture enters an alcoholysis reaction tower to be fully reacted, hydrogen chloride gas generated by the reaction is timely taken away by the ethanol vaporized in a reboiler and enters a tail gas pipeline II, then the ethanol is condensed and recycled by a multistage condenser and is put into the alcoholysis reaction tower to be vaporized and separated from hydrogen chloride, the hydrogen chloride gas in the multistage condenser is not condensed, and the hydrogen chloride gas is introduced into a tail gas acid absorption tower to be recycled.
The product chloromethyl triethoxysilane that produces in the alcoholysis reaction tower and the incomplete reaction chloromethyl trichlorosilane enter reation kettle, and then convey to the upper portion of alcoholysis reaction tower and continue abundant reaction with ethanol through the hydraulic pump, constantly reduce the content of chloromethyl trichlorosilane in the product, combine ethanol vaporization to take away the continuous cycle separation effect of hydrogen chloride finally, constantly purify product chloromethyl triethoxysilane, make the purity of the ejection of compact product reach 90% finally.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an embodiment of an alcoholysis reaction system for producing chloromethyltriethoxysilane according to the present invention.
In the figure, 1, an alcoholysis reaction tower, 2, a reaction kettle, 3, a mixed feeding pipe, 4, a vaporization feeding pipe, 5, a tail gas discharge pipe, 6, a multi-stage condensation mechanism, 7, a condensation recovery pipe, 8, an acid removal pipeline, 9, a discharge pipe, 10, a pre-reactor, 11, a chlorine feeding pipe, 12, a first ethanol feeding pipe, 13, a reboiler, 14, a second ethanol feeding pipe, 15, a product circulating pipe, 16, a hydraulic pump, 17, a first-stage condenser, 18, a second-stage condenser, 19, a third-stage condenser, 20, a first-stage condensing tank, 21, a second-stage condensing tank, 22, a third-stage condensing tank, 23, a gas pipeline, 24, a neutralization kettle, 25 and a magnesium powder tank.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the accompanying drawings and specific embodiments. It is to be understood that the described embodiments are merely a few embodiments of the invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments of the present invention without any inventive step, are within the scope of the present invention.
Referring to fig. 1, the present invention provides an alcoholysis reaction system for producing chloromethyltriethoxysilane, comprising: an alcoholysis reaction tower 1, wherein the alcoholysis reaction tower 1 is communicated with the upper part of a reaction kettle 2, the upper part of the alcoholysis reaction tower 1 is provided with a mixed feed pipe 3, the lower part of the alcoholysis reaction tower 1 is provided with a vaporization feed pipe 4, a chlorine feed pipe 11 and a first ethanol feed pipe 12 are arranged on a pre-reactor 10, the discharge port of the pre-reactor 10 is connected with the mixed feed pipe 3, one end of a reboiler 13 is connected with a second ethanol feed pipe 14, the other end of the reboiler is connected with the vaporization feed pipe 4, the top of the alcoholysis reaction tower 1 is provided with a tail gas outlet pipe 5, the tail gas outlet pipe 5 is connected with a multi-stage condensation mechanism 6, condensate of the multi-stage condensation mechanism 6 is introduced into the alcoholysis reaction tower 1 through a condensation recovery pipe 7, uncondensed gas of the multi-stage condensation mechanism 6 enters a tail gas deacidification absorption tower through an acid removal pipeline 8, the bottom of the reaction kettle 2 is provided with a discharge port, one end of a product circulation pipe 15 is connected with the discharge port of the reaction kettle 2 through a hydraulic pump 16, the other end is connected with the upper part of the alcoholysis reaction tower 1.
Specifically, the top end of the pre-reactor 10 is connected with the tail gas outlet pipe 5.
Specifically, multistage condensing mechanism 6 includes one-level condenser 17, second grade condenser 18, tertiary condenser 19, one-level condensate tank 20, second grade condensate tank 21, tertiary condensate tank 22 and gas pipeline 23, gas pipeline 23 has connected gradually one-level condenser 17, one-level condensate tank 20, second grade condenser 18, second grade condensate tank 21, tertiary condenser 19, tertiary condensate tank 22 and deacidification pipeline 8, the condensate of one-level condensate tank 20, second grade condensate tank 21 and tertiary condensate tank 22 lets in alcoholysis reaction tower 1 through condensation recovery pipe 7.
Specifically, the discharge port of the reaction kettle 2 is further connected with a neutralization kettle 24 through a pipeline, and a neutralization feed port of the neutralization kettle 24 is provided with a magnesium powder tank 25.
Specifically, the weight ratio of the chloromethyl trichlorosilane to the ethanol introduced into the alcoholysis reaction system is 1: 0.5-0.7, and the weight ratio of the ethanol flowing through the first ethanol feeding pipe 12 to the ethanol flowing through the second ethanol feeding pipe 14 is 2: 1. The raw materials are adopted according to the proportion and have sufficient reaction and high reaction rate.
During the production of chloromethyltriethoxysilane, chloromethyltrichlorosilane enters the pre-reactor 10 through a chlorine inlet pipe 11, a portion of ethanol enters the pre-reactor 10 through a first ethanol inlet pipe 12 to undergo a spontaneous violent reaction with chloromethyltrichlorosilane, the reaction product enters the alcoholysis reaction tower 1 from the upper part, and the other portion of ethanol enters the alcoholysis reaction tower 1 from the lower part after being vaporized through a reboiler 13 through a second ethanol inlet pipe 14.
The method is characterized in that the monochloromethyltrichlorosilane and ethanol spontaneously carry out alcoholysis reaction at normal temperature and normal pressure, the reaction is violent, the product generates chloromethyltriethoxysilane and hydrogen chloride gas, the solubility of the hydrogen chloride in the chloromethyltriethoxysilane is higher, and therefore the generated hydrogen chloride needs to be separated from the chloromethyltriethoxysilane in time during the alcoholysis reaction. According to the invention, chloromethyl trichlorosilane and ethanol firstly enter a pre-reactor 10 to be mixed and preliminarily pre-reacted, then enter an alcoholysis reaction tower 1 to be fully reacted, hydrogen chloride gas generated by the reaction is timely taken away by the ethanol vaporized in a reboiler 13 and enters a tail gas pipeline II, then the ethanol is condensed and recycled by a multistage condenser 6 and is put into the alcoholysis reaction tower 1 to be vaporized and separated from hydrogen chloride, the hydrogen chloride gas in the multistage condenser 6 is not condensed, and the hydrogen chloride gas is introduced into a tail gas acid absorption tower to be recycled.
The product chloromethyl triethoxysilane and incomplete reacted chloromethyl trichlorosilane generated in the alcoholysis reaction tower 1 enter the reaction kettle 2, and are conveyed to the upper part of the alcoholysis reaction tower 1 through the hydraulic pump 16 to continuously and fully react with ethanol, the content of the chloromethyl trichlorosilane in the product is continuously reduced, the continuous cyclic separation effect of hydrogen chloride is finally taken away by combining ethanol vaporization, the product chloromethyl triethoxysilane is continuously purified, and the purity of the discharged product is finally 90%.
The above description is only for the purpose of describing the preferred embodiments of the present invention, and is not intended to limit the scope of the present invention, and any variations and modifications made by those skilled in the art based on the above disclosure are within the scope of the appended claims.

Claims (4)

1. An alcoholysis reaction method for producing chloromethyl triethoxysilane is characterized in that: the device comprises an alcoholysis reaction tower (1), wherein the alcoholysis reaction tower (1) is communicated with the upper part of a reaction kettle (2), a mixed feeding pipe (3) and a vaporization feeding pipe (4) are arranged on the alcoholysis reaction tower (1), a tail gas discharge pipe (5) is arranged at the top of the alcoholysis reaction tower (1), the tail gas discharge pipe (5) is connected with a multi-stage condensation mechanism (6), condensate of the multi-stage condensation mechanism (6) is introduced into the alcoholysis reaction tower (1) through a condensation recovery pipe (7), uncondensed gas of the multi-stage condensation mechanism (6) enters a tail gas acid removal absorption tower through an acid removal pipeline (8), the reaction kettle (2) is connected with a discharge pipe (9), the device also comprises a pre-reactor (10), a chlorine feeding pipe (11) and a first ethanol feeding pipe (12) are arranged on the pre-reactor (10), and a discharge hole of the pre-reactor (10) is connected with the mixed feeding pipe (3), the pre-reactor (10) top is connected with tail gas contact tube (5), still including reboiler (13), second diethanol inlet pipe (14) is connected to reboiler (13) one end, and the other end is connected vaporization inlet pipe (4), still includes product circulating pipe (15), the discharge gate of reation kettle (2) is passed through hydraulic pump (16) to product circulating pipe (15) one end, and the other end links to each other with alcoholysis reaction tower (1), and multistage condensation mechanism (6) include one-level condenser (17), second grade condenser (18), tertiary condenser (19), one-level condensing tank (20), second grade condensing tank (21), tertiary condensing tank (22) and gas pipeline (23), gas pipeline (23) are connected with one-level condenser (17), one-level condensing tank (20), second grade condenser (18), second grade condensing tank (21), tertiary condenser (19) in proper order, Tertiary condensate tank (22) and deacidification pipeline (8), the lower part that alcoholysis reaction tower (1) was let in through condensation recovery tube (7) to the condensate of one-level condensate tank (20), second grade condensate tank (21) and tertiary condensate tank (22), the upper portion of alcoholysis reaction tower (1) is all connected to mixed inlet pipe (3), product circulating pipe (15), and the lower part of alcoholysis reaction tower (1) is connected in first ethanol inlet pipe (12), along vertical direction, product circulating pipe (15) are located the below of mixing inlet pipe (3), product circulating pipe (15) are located the top of condensation recovery tube (7).
2. An alcoholysis reaction process for the production of chloromethyltriethoxysilane as recited in claim 1, wherein: the discharge hole of the reaction kettle (2) is also connected with a neutralization kettle (24) through a pipeline, and a magnesium powder tank (25) is arranged on the neutralization feed hole of the neutralization kettle (24).
3. An alcoholysis reaction process for the production of chloromethyltriethoxysilane as recited in claim 1, wherein: the weight ratio of the chloromethyl trichlorosilane to the ethanol in the alcoholysis reaction is 1: 0.5-0.7.
4. An alcoholysis reaction process for the production of chloromethyltriethoxysilane as recited in claim 1, wherein: the weight ratio of ethanol flowing through the first ethanol feed pipe (12) to ethanol flowing through the second ethanol feed pipe (14) is 2: 1.
CN201910715455.4A 2019-08-05 2019-08-05 A alcoholysis reaction system for producing chloromethyl triethoxysilane Active CN110563754B (en)

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CN113372559B (en) * 2021-06-21 2023-09-15 福建立亚化学有限公司 Method and device for producing liquid polycarbosilane precursor material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101362776A (en) * 2008-08-25 2009-02-11 淄博市临淄齐泉工贸有限公司 Continuous production method of propyl trialkoxysilane
CN102924504A (en) * 2012-11-20 2013-02-13 江西晨光新材料有限公司 Preparation method of propyl trimethoxy silane
CN109320541A (en) * 2018-11-13 2019-02-12 江西宏柏新材料股份有限公司 The method of tower acid binding agent method continuous production cyanoethyl triethoxysilane

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101362776A (en) * 2008-08-25 2009-02-11 淄博市临淄齐泉工贸有限公司 Continuous production method of propyl trialkoxysilane
CN102924504A (en) * 2012-11-20 2013-02-13 江西晨光新材料有限公司 Preparation method of propyl trimethoxy silane
CN109320541A (en) * 2018-11-13 2019-02-12 江西宏柏新材料股份有限公司 The method of tower acid binding agent method continuous production cyanoethyl triethoxysilane

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Denomination of invention: A alcoholysis reaction system for producing chloromethyltriethoxysilane

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