CN215277266U - Vinyl trichlorosilane semicontinuous synthesizer - Google Patents
Vinyl trichlorosilane semicontinuous synthesizer Download PDFInfo
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- CN215277266U CN215277266U CN202121314837.5U CN202121314837U CN215277266U CN 215277266 U CN215277266 U CN 215277266U CN 202121314837 U CN202121314837 U CN 202121314837U CN 215277266 U CN215277266 U CN 215277266U
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Abstract
The utility model provides a vinyl trichlorosilane semicontinuous synthesizer, including reation kettle and reaction tube, reation kettle is used for heating the mixed liquid of solvent and catalyst constitution to reaction temperature, the top of reaction tube respectively with reation kettle bottom, acetylene source and trichlorosilane silicon source link to each other, its end stretches into in the reation kettle, acetylene gas, trichlorosilane gas, and partly in the reation kettle is heated to reaction temperature's mixed liquid and gets into in the reation kettle, acetylene and trichlorosilane in the reation kettle react under the effect of catalyst, the reaction product vinyl trichlorosilane of formation escapes to the reation kettle in, simultaneously mixed liquid in the reation kettle gets into reation kettle. Because acetylene has light specific gravity and is diffused quickly, the acetylene enters the reaction tube more firstly than trichlorosilane, and the acetylene in the solvent is ensured to be far excessive, so that trichlorosilane is more easily and completely consumed, byproducts generated by the reaction of trichlorosilane and vinyl trichlorosilane are reduced, and the yield of the product vinyl trichlorosilane is ensured.
Description
Technical Field
The utility model particularly relates to a vinyl trichlorosilane semicontinuous synthesizer.
Background
Vinyl silane is an organic compound of formula C14H30O6S, which has wide application, such as being used as a vinyl silane coupling agent mainly for plastic reinforcement and being widely applied to manufacturing silane crosslinked polyethylene wires, insulating and sheathing materials; the glass fiber and the inorganic siliceous filler are also suitable for being impregnated to improve and enhance the infiltration and bonding performance of the resin and the glass fiber; in addition, the coating is copolymerized with various monomers, can be prepared into special coatings, and is suitable for coating protection of parts and planes of national defense advanced products such as aerospace, radio communication, radars, electronic components and the like.
At present, most of vinyl trichlorosilane adopts an intermittent kettle type reaction synthesis kettle, and in the reaction, the yield of the vinyl trichlorosilane is low because the generated product vinyl trichlorosilane is easy to react with raw material trichlorosilane to generate a byproduct bis-trichlorosilane ethane.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the technical problem that to the above-mentioned not enough that exists among the prior art, provide a vinyl trichlorosilane semicontinuous synthesizer that reduces the accessory substance and generate, improve productivity.
Solve the utility model discloses the technical scheme that technical problem adopted is:
the utility model provides a vinyl trichlorosilane semicontinuous synthesizer, include: a reaction kettle and a reaction tube.
The reaction kettle is used for heating mixed liquid consisting of the solvent and the catalyst in the kettle to a reaction temperature.
The initial end of the reaction tube is respectively connected with the bottom of the reaction kettle, the acetylene source and the trichlorosilane silicon source, and the tail end of the reaction tube extends into the reaction kettle.
Acetylene gas, trichlorosilane gas and a part of mixed liquid in the reaction kettle heated to the reaction temperature enter a reaction tube, the acetylene and the trichlorosilane in the reaction tube react under the action of a catalyst, a generated reaction product vinyl trichlorosilane escapes into the reaction kettle, and meanwhile the mixed liquid in the reaction tube enters the reaction kettle.
Optionally, the reaction tube comprises a reaction primary tube, a reaction end tube, and a multi-stage reaction bypass tube connected between the reaction primary tube and the reaction end tube; the initial end of the reaction initial tube is respectively connected with the bottom of the reaction kettle, the acetylene source and the trichlorosilane silicon source, and the tail end of the reaction final tube extends into the reaction kettle.
The reaction by-pass pipe is provided with a by-pass valve and a sampling port, when the synthesizer works, the by-pass valve on one stage of the reaction by-pass pipe is opened, and the other by-pass valves are disconnected, so that a reaction initial pipe section connected with the bottom of the reaction kettle, the reaction by-pass pipe with the opened by-pass valve and a reaction final pipe section connected with the top of the reaction kettle are communicated to form a reaction channel.
Optionally, a shunt valve is arranged on the reaction primary pipe section between two adjacent reaction bypass pipes.
Optionally, a condenser is also included.
The condenser is connected with the top of the reaction kettle and is used for condensing gas phase substances escaping from the reaction kettle to obtain liquid vinyltrichlorosilane.
Optionally, the device further comprises a collecting tank, wherein the collecting tank is connected with the condenser and is used for collecting the liquid vinyltrichlorosilane condensed by the condenser.
Optionally, the system further comprises a circulating pump, wherein the circulating pump is arranged on the reaction tube and is used for circulating the mixed liquid consisting of the solvent and the catalyst between the bottom and the top of the reaction kettle.
Optionally, still include acetylene feed pipe, acetylene flowmeter and acetylene feed valve, the acetylene feed pipe is connected between acetylene source and reaction tube, acetylene flowmeter and acetylene feed valve all locate on the acetylene feed pipe.
Optionally, the system further comprises a trichlorosilane feeding pipe, a trichlorosilane flow meter and a trichlorosilane feeding valve, wherein the trichlorosilane feeding pipe is connected between the trichlorosilane silicon source and the reaction pipe, and the trichlorosilane flow meter and the trichlorosilane feeding valve are both arranged on the trichlorosilane feeding pipe.
Optionally, the system further comprises a mixed liquid flow meter, wherein the mixed liquid flow meter is arranged on a reaction initial pipe section between the circulating pump and the first-stage reaction bypass pipe and is used for detecting the flow of the mixed liquid entering the reaction pipe.
The utility model discloses in, heat the mixture of solvent and catalyst to reaction temperature through reation kettle, mix with raw materials acetylene and trichlorosilane in its input reaction tube again, and under reaction temperature and catalytic action, raw materials acetylene and trichlorosilane reaction generate product vinyl trichlorosilane, because acetylene specific gravity is light, the diffusion is fast, it is more advanced than trichlorosilane and goes into in the reaction tube, can guarantee that the acetylene in the solvent is far away excessive, contact with trichlorosilane and react, thereby it is complete with trichlorosilane consumption more easily, with the two trichlorosilane ethane of accessory substance that reduces trichlorosilane and vinyl trichlorosilane reaction and generate, guarantee product vinyl trichlorosilane's yield.
In addition, the mixture of the solvent and the catalyst is continuously circulated from the bottom of the reaction kettle to the top of the reaction kettle through the reaction tube, so that the semi-continuous reaction is ensured.
Drawings
Fig. 1 is a schematic structural diagram of a vinyl trichlorosilane semicontinuous synthesis apparatus provided in embodiment 1 of the present invention.
Detailed Description
In the following, the technical solutions in the present invention will be described clearly and completely with reference to the accompanying drawings, and obviously, the described embodiments are some, not all embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by a person of ordinary skill in the art without creative efforts belong to the scope of the present invention.
In the description of the present invention, it should be noted that the indication of orientation or positional relationship such as "up" is based on the orientation or positional relationship shown in the drawings, and is only for convenience and simplicity of description, and does not indicate or imply that the indicated device or element must be provided with a specific orientation, constructed and operated in a specific orientation, and thus should not be construed as limiting the present invention.
In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "connected," "disposed," "mounted," "fixed," and the like are to be construed broadly, e.g., as being fixedly connected, detachably connected, or integrally connected; either directly or indirectly through intervening media, or may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood in specific cases for those skilled in the art.
The utility model provides a vinyl trichlorosilane semicontinuous synthesizer, include: a reaction kettle and a reaction tube.
The reaction kettle is used for heating mixed liquid consisting of the solvent and the catalyst in the kettle to a reaction temperature.
The initial end of the reaction tube is respectively connected with the bottom of the reaction kettle, the acetylene source and the trichlorosilane silicon source, and the tail end of the reaction tube extends into the reaction kettle.
Acetylene gas, trichlorosilane gas and a part of mixed liquid in the reaction kettle heated to the reaction temperature enter a reaction tube, the acetylene and the trichlorosilane in the reaction tube react under the action of a catalyst, a generated reaction product vinyl trichlorosilane escapes into the reaction kettle, and meanwhile the mixed liquid in the reaction tube enters the reaction kettle.
Example 1:
as shown in fig. 1, the present embodiment provides a vinyl trichlorosilane semi-continuous synthesis apparatus, comprising: reaction vessel 1 and reaction tube 13.
The reaction kettle 1 is used for heating the mixed liquid consisting of the solvent and the catalyst in the kettle to the reaction temperature.
The initial end of the reaction tube 13 is connected with the bottom of the reaction kettle 1, the acetylene source and the trichlorosilane silicon source respectively, and the tail end thereof extends into the reaction kettle 1.
Acetylene gas, trichlorosilane gas and a part of mixed liquid heated to a reaction temperature in the reaction kettle 1 enter the reaction tube 13, acetylene and trichlorosilane in the reaction tube 13 react under the action of a catalyst, a generated reaction product vinyl trichlorosilane escapes into the reaction kettle 1, and the mixed liquid in the reaction tube 13 enters the reaction kettle 1.
Therefore, the mixture of the solvent and the catalyst is heated to the reaction temperature through the reaction kettle 1, then the mixture is input into the reaction tube 13 to be mixed with the raw material acetylene and the trichlorosilane, and under the reaction temperature and the action of the catalyst, the raw material acetylene and the trichlorosilane react to generate the product of the vinyl trichlorosilane, and the product of the vinyl trichlorosilane enters the reaction tube 13 earlier than the trichlorosilane due to the fact that the acetylene has light specific gravity and is diffused fast, the acetylene in the solvent can be ensured to be far excessive and to be in contact with the trichlorosilane for reaction, and therefore the trichlorosilane can be consumed completely more easily, the byproduct of the double trichlorosilane ethane generated by the reaction of the trichlorosilane and the vinyl trichlorosilane is reduced, and the yield of the product of the vinyl trichlorosilane is ensured.
In addition, the mixture of the solvent and the catalyst is continuously circulated from the bottom of the reaction vessel 1 to the top of the reaction vessel 1 through the reaction tube 13, thereby ensuring the semi-continuous reaction.
In this embodiment, the reaction tube 13 includes a primary reaction tube 131, a secondary reaction tube 132, and a multistage reaction bypass tube 133 connected between the primary reaction tube 131 and the secondary reaction tube 132; the initial end of the initial reaction tube 131 is connected to the bottom of the reaction vessel 1, the acetylene source and the trichlorosilane source, respectively, and the end of the final reaction tube 132 extends into the reaction vessel 1.
The reaction bypass pipe 133 is provided with a bypass valve 12 and a sampling port 11, and when the synthesis apparatus is in operation, the bypass valve 12 of one stage of the reaction bypass pipe 133 is opened, and the remaining bypass valves 12 are opened, so that the reaction initial pipe section connected to the bottom of the reaction vessel 1, the reaction bypass pipe 133 with the opened bypass valve 12 and the reaction final pipe section connected to the top of the reaction vessel 1 are communicated to form a reaction channel.
At present, most of experimental devices for synthesizing the vinyl trichlorosilane, such as CN211411975U, can only simulate the production process conditions of a kettle type vinyl silane process, and experimental verification is carried out, so that the reaction condition cannot be known in time in the reaction process, and the optimal residence time of the vinyl trichlorosilane reaction at a certain temperature can be obtained.
In this embodiment, the reaction tube has a plurality of channels formed by the bypasses, each bypass has a sampling port, so that the reaction conditions of the channels in different stages can be obtained through step-by-step test and sampling analysis, if the components contain trichlorosilane, the next-stage channel test is continued until no trichlorosilane exists, and the reaction time of acetylene and trichlorosilane can be calculated through the flow data, the tube diameter and the tube length of the mixed liquid formed by the solvent and the catalyst in the reaction tube.
In this embodiment, the flow divider valve 10 is provided on the section of the primary reaction pipe 131 between two adjacent reaction bypass pipes 133. The diverter valve 10 ensures that the gas-liquid mixture does not enter other bypasses. As in the third stage channel test, the diverter valve 10 between the first two stages, and the diverter valve 10 between the second three stages are opened, and the remaining diverter valves 10 are opened, thereby ensuring that the gas-liquid mixture substantially all enters the third stage reaction by-pass tube 133.
The solvent and the catalyst are filled in the reaction kettle 1, the solvent and the catalyst are heated to the reaction temperature through a heating jacket of the reaction kettle 1, and are pumped into the reaction tube 13 through the circulating pump 2 and then heated in the process of contacting with the raw materials of acetylene and trichlorosilane, so that the reaction temperature is reached. And the length of the reaction pipe 12 is adjusted by controlling a bypass valve 12 and a flow dividing valve 10 on a reaction pipe 13 connected with the outlet of the pump, so as to test the reaction time required by trichlorosilane with a certain flow rate.
In this embodiment, a condenser 15 is also included.
The condenser 15 is connected with the top of the reaction kettle 1 and is used for condensing gas phase substances escaping from the reaction kettle 1 to obtain liquid vinyltrichlorosilane. Since a small amount of solvent is vaporized at the heating temperature of the reaction vessel 1 and a mixed gas phase is formed with vinyltrichlorosilane generated by the reaction and escapes, condensation is required to separate the two.
In this embodiment, the apparatus further comprises a collecting tank 16, and the collecting tank 16 is connected to the condenser 15 and is used for collecting the liquid vinyltrichlorosilane condensed by the condenser 15.
The reaction kettle 1 is provided with a thermometer and a pressure gauge, the upper part of the reaction kettle 1 is connected with a tail gas pipeline 14, the tail gas pipeline 14 is connected with a condenser 15, the condenser 15 is connected with a collecting tank 16, a reaction product and a part of solvent in the reaction kettle 1 enter the tail gas pipeline 14 through heating and vaporization, then the reaction product is condensed through the condenser 15, and the reaction product is liquefied and enters the collecting tank 16.
In this embodiment, the reactor further comprises a circulation pump 2, wherein the circulation pump 2 is arranged on the reaction tube 13 and is used for circulating a mixed solution composed of the solvent and the catalyst between the bottom and the top of the reaction kettle 1.
In this embodiment, still include acetylene feed pipe 3, acetylene flowmeter 4 and acetylene feed valve 7, acetylene feed pipe 3 is connected between acetylene source and reaction tube 13, and acetylene flowmeter 4 and acetylene feed valve 7 are all located on acetylene feed pipe 3.
In this embodiment, the apparatus further includes a trichlorosilane feeding pipe 5, a trichlorosilane flow meter 6, and a trichlorosilane feeding valve 8, the trichlorosilane feeding pipe 5 is connected between a trichlorosilane silicon source and the reaction pipe 13, and the trichlorosilane flow meter 6 and the trichlorosilane feeding valve 8 are both disposed on the trichlorosilane feeding pipe 5.
In this embodiment, the system further includes a mixed liquid flow meter 9, and the mixed liquid flow meter 9 is disposed on the section of the primary reaction pipe 131 between the circulation pump 2 and the first-stage reaction bypass pipe 133, and is configured to detect a flow rate of the mixed liquid entering the reaction pipe 13.
The acetylene and trichlorosilane flowmeter accurately measures the feeding amount of acetylene and trichlorosilane, and ensures the accurate proportioning of materials. The flow velocity of the mixed liquid in the reaction tube can be accurately calculated through the mixed liquid flowmeter. Through the step-by-step channel test, the reaction time required by trichlorosilane with a certain flow can be calculated according to the pipe diameter and the pipe length of the reaction pipe 13.
The procedure for synthesizing vinyltrichlorosilane by the semicontinuous synthesis device in the embodiment is as follows:
adding solvent chlorobenzene and catalyst (preferably) into a reaction kettle 1, introducing condensed water into a condenser 15, starting a circulating pump 2, closing all flow dividing valves 10, opening a bypass valve 12 on a first-stage reaction bypass pipe 133, enabling the chlorobenzene and the catalyst to enter the reaction kettle 1 for circulation through a channel formed by communicating a reaction initial pipe section connected with the bottom of the reaction kettle 1, the first-stage reaction bypass pipe 133 and a reaction final pipe section connected with the top of the reaction kettle 1, increasing the temperature of the reaction kettle 1, heating to 90 ℃, then opening an acetylene feed valve 7 to introduce acetylene gas, opening a trichlorosilane feed valve 8 after circulating for 30min, starting the reaction, sampling through a sampling port 11 on the first-stage reaction bypass pipe 133, and detecting the component condition in the sample gas. If the component contains trichlorosilane, closing a bypass valve 12 on a first-stage reaction bypass pipe 133, opening a bypass valve 12 on a second-stage reaction bypass pipe 133, and opening a flow dividing valve 10 on a reaction initial pipe section between the first-stage reaction bypass pipe 133 and the second-stage reaction bypass pipe 133, so that a gas-liquid mixture consisting of raw materials, chlorobenzene and a catalyst enters a reaction kettle 1 through a channel formed by communicating a reaction initial pipe section connected with the bottom of the reaction kettle 1, the second-stage reaction bypass pipe 133 and a reaction final pipe section connected with the top of the reaction kettle 1 for circulation, so as to increase reaction time, and so on until no trichlorosilane exists, calculating the reaction time of acetylene and trichlorosilane at 90 ℃ through flow data detected by a mixed liquid flow meter 9, the pipe diameter of a reaction pipe 13 and the pipe length.
Wherein, the reaction bypass pipe 133 closest to the reaction vessel 1 is the first-stage reaction bypass pipe 133, and the passage formed by communicating the reaction bypass pipe 133 with the initial reaction pipe section and the final reaction pipe section is the shortest, and the longer the passage formed by communicating the reaction bypass pipe 133 with the initial reaction pipe section and the final reaction pipe section is, the farther away from the reaction vessel 1, the longer the reaction time is.
It is to be understood that the above embodiments are merely exemplary embodiments that have been employed to illustrate the principles of the present invention, and that the present invention is not limited thereto. It will be apparent to those skilled in the art that various modifications and improvements can be made without departing from the spirit and substance of the invention, and these modifications and improvements are also considered to be within the scope of the invention.
Claims (9)
1. A vinyl trichlorosilane semicontinuous synthesis device is characterized by comprising: a reaction kettle (1) and a reaction tube (13),
the reaction kettle (1) is used for heating mixed liquid consisting of solvent and catalyst in the kettle to reaction temperature,
the initial end of the reaction tube (13) is respectively connected with the bottom of the reaction kettle (1), the acetylene source and the trichlorosilane silicon source, the tail end of the reaction tube extends into the reaction kettle (1),
acetylene gas, trichlorosilane gas and a part of mixed liquid heated to a reaction temperature in the reaction kettle (1) enter the reaction tube (13), acetylene and trichlorosilane in the reaction tube (13) react under the action of a catalyst, a generated reaction product vinyl trichlorosilane escapes into the reaction kettle (1), and meanwhile the mixed liquid in the reaction tube (13) enters the reaction kettle (1).
2. The apparatus for the semi-continuous synthesis of vinyltrichlorosilane according to claim 1,
the reaction tube (13) comprises a primary reaction tube (131), a final reaction tube (132), and a multistage reaction bypass tube (133) connected between the primary reaction tube (131) and the final reaction tube (132); the initial end of the reaction initial tube (131) is respectively connected with the bottom of the reaction kettle (1), the acetylene source and the trichlorosilane source, the tail end of the reaction final tube (132) extends into the reaction kettle (1),
the reaction bypass pipe (133) is provided with a bypass valve (12) and a sampling port (11), when the synthesis device works, the bypass valve (12) on the first-stage reaction bypass pipe (133) is opened, and the rest bypass valves (12) are disconnected, so that a reaction primary pipe (131) connected with the bottom of the reaction kettle (1), the reaction bypass pipe (133) opened by the bypass valve (12) and a reaction final pipe (132) connected with the top of the reaction kettle (1) are communicated to form a reaction channel.
3. The apparatus for the semi-continuous synthesis of vinyltrichlorosilane according to claim 2, wherein a splitter valve (10) is provided on a section of the primary reaction pipe (131) between two adjacent bypass reaction pipes (133).
4. The vinyltrichlorosilane semi-continuous synthesis apparatus according to any one of claims 1 to 3, further comprising a condenser (15),
the condenser (15) is connected with the top of the reaction kettle (1) and is used for condensing gas phase substances escaping from the reaction kettle (1) to obtain liquid vinyltrichlorosilane.
5. The apparatus for the semi-continuous synthesis of vinyltrichlorosilane according to claim 4, further comprising a collection tank (16), wherein the collection tank (16) is connected to the condenser (15) and is used for collecting the liquid vinyltrichlorosilane condensed by the condenser (15).
6. The apparatus for the semi-continuous synthesis of vinyltrichlorosilane according to any one of claims 1 to 3, further comprising a circulation pump (2), wherein the circulation pump (2) is disposed on the reaction tube (13) and is used for circulating a mixed solution of the solvent and the catalyst between the bottom and the top of the reaction vessel (1).
7. The vinyltrichlorosilane semi-continuous synthesis apparatus according to any one of claims 1 to 3, further comprising an acetylene feeding pipe (3), an acetylene flow meter (4) and an acetylene feeding valve (7), wherein the acetylene feeding pipe (3) is connected between an acetylene source and the reaction pipe (13), and the acetylene flow meter (4) and the acetylene feeding valve (7) are both arranged on the acetylene feeding pipe (3).
8. The vinyl trichlorosilane semi-continuous synthesis device according to any one of claims 1 to 3, further comprising a trichlorosilane feeding pipe (5), a trichlorosilane flow meter (6) and a trichlorosilane feeding valve (8), wherein the trichlorosilane feeding pipe (5) is connected between a trichlorosilane silicon source and the reaction pipe (13), and the trichlorosilane flow meter (6) and the trichlorosilane feeding valve (8) are both arranged on the trichlorosilane feeding pipe (5).
9. The vinyltrichlorosilane semi-continuous synthesis apparatus according to claim 2 or 3, further comprising a mixed liquid flow meter (9), wherein the mixed liquid flow meter (9) is arranged on the section of the primary reaction pipe (131) between the circulating pump (2) and the first-stage reaction bypass pipe (133) and is used for detecting the flow of the mixed liquid entering the reaction pipe (13).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202121314837.5U CN215277266U (en) | 2021-06-11 | 2021-06-11 | Vinyl trichlorosilane semicontinuous synthesizer |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202121314837.5U CN215277266U (en) | 2021-06-11 | 2021-06-11 | Vinyl trichlorosilane semicontinuous synthesizer |
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| CN215277266U true CN215277266U (en) | 2021-12-24 |
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| CN202121314837.5U Active CN215277266U (en) | 2021-06-11 | 2021-06-11 | Vinyl trichlorosilane semicontinuous synthesizer |
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