CN210915887U - Methyl chlorosilane synthesis equipment - Google Patents
Methyl chlorosilane synthesis equipment Download PDFInfo
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- CN210915887U CN210915887U CN201921621683.7U CN201921621683U CN210915887U CN 210915887 U CN210915887 U CN 210915887U CN 201921621683 U CN201921621683 U CN 201921621683U CN 210915887 U CN210915887 U CN 210915887U
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Abstract
The application discloses methyl chlorosilane synthesis equipment. The methyl chlorosilane synthesis equipment comprises: the device comprises a fluidized bed reactor, a water washing tower and a filter arranged between the fluidized bed reactor and the water washing tower. Because set up the filter between fluidized bed reactor and washing tower, can so for, when letting in a large amount of nitrogen gas in fluidized bed reactor, nitrogen gas blows reaction raw materials such as silica flour and trace methyl chlorosilane to washing tower when, need flow through the filter to intercept and recycle silica flour through the filter.
Description
Technical Field
The application relates to the technical field of organic silicon chemistry, in particular to methyl chlorosilane synthesis equipment.
Background
Methyl chlorosilane is a support in the field of organosilicon chemistry, wherein most organosilicon products are prepared by processing polymethyl siloxane prepared by hydrolyzing methyl chlorosilane, a regulator, a cross-linking agent, an end capping agent and the like. Methylchlorosilane is usually synthesized by batch operation, and after the equipment for synthesizing methylchlorosilane is continuously operated for a period of time, the equipment needs to be shut down, so that a catalyst is added or the equipment needs to be overhauled.
The structural schematic diagram of the current methylchlorosilane synthesis plant is shown in fig. 1, and comprises a fluidized bed reactor 11 and a water washing tower 12. During the shutdown process of the synthesis equipment, a large amount of nitrogen is introduced into the fluidized bed reactor 11, so that the remaining methylchlorosilane, reaction raw materials and the like are directly blown into the water washing tower 12 through the introduced large amount of nitrogen, and the shutdown mode usually causes a large amount of waste of the remaining reaction raw materials such as silicon powder and the like.
SUMMERY OF THE UTILITY MODEL
The embodiment of the application provides methyl chlorosilane synthesis equipment, which is used for solving the problem of large waste of reaction raw materials such as residual silicon powder in the prior art.
The embodiment of the application provides methyl chlorosilane synthesis equipment, which comprises: the device comprises a fluidized bed reactor, a water washing tower and a filter arranged between the fluidized bed reactor and the water washing tower.
Preferably, the synthesizing apparatus further comprises: at least one surge tank disposed between the fluidized bed reactor and the filter.
Preferably, the inflow pipes of the buffer tanks are connected in an eccentric connection manner.
Preferably, the number of the buffer tanks is 1.
Preferably, the connecting pipeline of the buffer tank and the fluidized bed reactor comprises a first valve.
Preferably, the synthesizing apparatus further comprises: a recovery system coupled to the fluidized bed reactor.
Preferably, the pipeline connecting the recovery system and the fluidized bed reactor comprises a second valve.
Preferably, the synthesizing apparatus further comprises: a nitrogen supply system connected to the fluidized bed reactor.
The embodiment of the application provides methyl chlorosilane synthesis equipment, which comprises: fluidized bed reactor, water wash tower and set up in fluidized bed reactor with at least one buffer tank between the water wash tower.
Preferably, the inflow pipes of the buffer tanks are connected in an eccentric connection manner.
The embodiment of the application adopts at least one technical scheme which can achieve the following beneficial effects:
the method is characterized in that nitrogen is introduced into the fluidized bed reactor at a first feeding speed and is used for feeding a mixed material flow in the fluidized bed reactor into a recovery system, and methyl chloride and methyl chlorosilane monomers are recovered through the recovery system, so that waste of reaction raw materials and products is saved; in addition, a buffer tank and/or a filter are arranged between the fluidized bed reactor and the water washing tower, so that when a large amount of nitrogen is introduced into the fluidized bed reactor, part of reaction raw materials such as silicon powder and the like are blown to the water washing tower by the nitrogen, the reaction raw materials need to flow through the buffer tank and/or the filter, the silicon powder is intercepted by the buffer tank and/or the filter and recycled, and the reaction raw materials are further saved.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
FIG. 1 is a schematic diagram of a specific structure of a methylchlorosilane synthesis apparatus in the prior art;
fig. 2 is a schematic structural diagram of a methylchlorosilane synthesis apparatus provided in an embodiment of the present application;
FIG. 3 is a schematic diagram of another methyl chlorosilane synthesis apparatus according to an embodiment of the present disclosure;
fig. 4 is a schematic specific flowchart of a parking method according to an embodiment of the present application.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be described in detail and completely with reference to the following specific embodiments of the present application and the accompanying drawings. It should be apparent that the described embodiments are only some of the embodiments of the present application, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The technical solutions provided by the embodiments of the present application are described in detail below with reference to the accompanying drawings.
As described above, in the conventional methylchlorosilane synthesis apparatus, a large amount of nitrogen gas is introduced into the fluidized bed reactor of the synthesis apparatus during shutdown (i.e., stoppage of the apparatus), so that a mixture including methylchlorosilane and reaction raw materials is blown into the water-washing tower, but such shutdown causes a large amount of waste of the remaining reaction raw materials such as silicon powder.
Based on this, the embodiment of the present application provides a methylchlorosilane synthesis apparatus, which can be used to solve the above problems. As shown in fig. 2, the synthesizing apparatus 20 includes: a fluidized bed reactor 21, a water washing tower 22, and a filter 24. The filter 24 is disposed between the fluidized bed reactor 21 and the water washing tower 22, so that when a large amount of nitrogen is introduced into the fluidized bed reactor 21, the nitrogen blows reaction raw materials such as methyl chlorosilane and silicon powder to the water washing tower, and the reaction raw materials such as silicon powder need to flow through the filter 24, and the reaction raw materials are filtered and recycled through the filter 24, so that waste of residual reaction raw materials such as silicon powder can be reduced.
In addition, the synthesis apparatus 20 may further include at least one buffer tank 23, and each buffer tank 23 is disposed between the fluidized bed reactor 21 and the filter 24. Through the added buffer tanks 23, on one hand, when the nitrogen flow rate is too large, the buffer tanks 23 can buffer the nitrogen flow rate, so that the nitrogen flow rate is reduced, and the filter 24 and the water washing tower 22 are prevented from being washed by the too large nitrogen flow rate, and the safety of equipment is prevented from being influenced; on the other hand, by adding these buffer tanks 23, when the nitrogen flow rate is reduced in each buffer tank 23, part of the reaction raw material such as silicon powder is naturally deposited by gravity and can be recovered and utilized. Of course, a first valve 27 may be provided in the connecting pipe between the first buffer tank 23 adjacent to the fluidized bed reactor 21 and the fluidized bed reactor 21, and the nitrogen gas carrying the mixture is controlled to enter the water-washing column by opening or closing the first valve 27, and the flow rate thereof may also be controlled by the first valve 27.
It should be noted that, for each buffer tank 23, the pipeline into which the nitrogen gas flow of each buffer tank 23 flows may be connected in an eccentric connection manner, so that the nitrogen gas flowing into each buffer tank 23 may generate a cyclone inside, thereby further reducing the flow rate of the nitrogen gas flow, preventing the flushing of the filter 24 and the water washing tower 22, and forming more reaction raw material sedimentation in each buffer tank 23.
In general, the larger the number of buffer tanks 23, the better the buffering effect on the flow rate of the nitrogen gas stream and the more the reaction raw material sedimentation can be formed, but on the other hand, the more buffer tanks 23 are added, the corresponding cost increase is also caused, and therefore the number of buffer tanks 23 can be determined in accordance with the specific situation. For example, the number may be 1, 2, or other numbers.
In practical applications, the synthesis apparatus 20 may further include a recycling system 29, and the recycling system 29 may be used to recycle a portion of the remaining reaction raw materials, the remaining reaction products, and the like. The recovery system 29 is connected to the fluidized-bed reactor 21, and a second valve 28 may be provided in a pipe connecting the recovery system 29 and the fluidized-bed reactor 21 to control the post-treatment process.
The synthesis apparatus 20 may further include a nitrogen supply system 26, the nitrogen supply system 26 is connected to the fluidized-bed reactor 21, and nitrogen may be introduced into the fluidized-bed reactor 21 through the nitrogen supply system 26. In addition, in order to facilitate control of the process of introducing nitrogen, a third valve 25 may be added to the connection pipe of the nitrogen supply system 26 and the fluidized-bed reactor 21. When the third valve 25 is opened, nitrogen is fed into the fluidized-bed reactor 21, and when the third valve 25 is closed, the feeding of nitrogen is stopped, although the feeding rate of nitrogen can also be adjusted by adjusting the magnitude of opening of the third valve 25.
The embodiment of the application also can provide methyl chlorosilane synthesis equipment. As shown in fig. 3, the synthesizing apparatus 30 includes: a fluidized bed reactor 31, a water scrubber 32 and at least one buffer tank 33, wherein each buffer tank 33 is arranged between the fluidized bed reactor 31 and the water scrubber 32. Compared to the synthesizing apparatus 20 in the above embodiment, the synthesizing apparatus 30 in this embodiment replaces the filter 24 in the synthesizing apparatus 20 with at least one buffer tank 33, and the other parts may be the same as the synthesizing apparatus 20. The flow rate of nitrogen is reduced by these buffer tanks 33, so that the residual reaction raw materials such as silicon powder are naturally settled by gravity, which is convenient for recycling and reduces the waste.
Also, the inflow pipes of the nitrogen gas flows in the respective buffer tanks 33 may be connected in an eccentric connection manner, so that the nitrogen gas flowing therein generates a cyclone inside, thereby further reducing the flow rate thereof, preventing the washing of the water washing tower 32, and causing more reaction raw material sedimentation in the respective buffer tanks 33. In addition, a valve may be provided in the middle of the connection pipe connecting the first buffer tank 33 adjacent to the fluidized-bed reactor 31 and the fluidized-bed reactor 31.
When the number of the buffer tanks 33 is determined, the determination can be made in combination with the actual situation by comprehensively considering the problems of cost, sedimentation effect, prevention of washing of the water washing tower 32, and the like. For example, the number of buffer tanks 33 may be 1, 2 or other and number in general.
The above is an explanation of the structure of the synthesizing apparatus provided in the embodiment of the present application, and for the convenience of understanding, the explanation may be made herein with reference to a specific example. In this example, the synthesis equipment includes fluidized bed reactor, buffer tank, filter and washing tower, and wherein the buffer tank is connected with fluidized bed reactor, and the filter is connected with the buffer tank, and the washing tower is connected with the filter, and the quantity of buffer tank is 1 to be provided with first valve between buffer tank and the fluidized bed reactor. In addition, the synthesis equipment also comprises a recovery system and a nitrogen supply system, wherein a connecting pipeline between the recovery system and the fluidized bed reactor comprises a second valve, and a connecting pipeline between the nitrogen supply system and the fluidized bed reactor comprises a third valve. The parking method of the synthesis device can be explained by using the example, and as shown in fig. 3, the parking method comprises the following specific steps:
step S41: when shutdown is required, the reaction temperature in the fluidized bed reactor is lowered.
In practical applications, after the synthesis equipment is operated for a period of time, such as half a year, shutdown maintenance, or addition of a catalyst and the like are usually required, and at this time, the reaction temperature in the fluidized bed reactor can be reduced, specifically, the reaction temperature in the fluidized bed reactor can be reduced by reducing the temperature of the heat transfer oil.
Step S42: and when the reaction temperature of the fluidized bed reactor is lower than the preset temperature, stopping adding the reaction raw materials into the fluidized bed reactor.
When the reaction temperature in the fluidized bed reactor is lowered, the reaction temperature can be monitored, and when the reaction temperature is lower than a preset temperature, the reaction raw materials are stopped being added into the fluidized bed reactor. The specific value of the preset temperature can be determined according to the temperature required by the methylchlorosilane synthesis reaction, for example, the temperature required by the methylchlorosilane synthesis reaction is usually 240 ℃ to 250 ℃, and the specific value of the preset temperature needs to be lower than 240 ℃ because the synthesis reaction needs to be stopped during the parking process. In particular, the specific value of the preset temperature can be set to be less than or equal to 220 ℃, for example, the preset temperature is set to be 180-220 ℃. For example, the preset temperature is 180 ℃, 185 ℃, 190 ℃, 200 ℃, 210 ℃, 215 ℃, 220 ℃ or other temperatures between 180 ℃ and 220 ℃.
When the reaction temperature of the fluidized bed reactor is lower than the preset temperature, which indicates that the synthesis reaction in the fluidized bed reactor is inhibited due to the excessively low temperature, the reaction raw materials can be stopped from being added into the fluidized bed reactor by closing the feeding valve. For example, the reaction raw materials for the methylchlorosilane synthesis reaction generally include silicon powder and methyl chloride, and the addition of silicon powder and methyl chloride to the fluidized bed reactor can be stopped by closing the respective feed valves.
Step S43: and opening the third valve and the second valve, closing the first valve, and introducing nitrogen into the fluidized bed reactor at a first feeding speed for blowing the residual mixture in the fluidized bed reactor into a recovery system.
After the remaining mixture is blown into the recovery system, part of the remaining reaction raw material and the remaining methylchlorosilane monomer and the like can be recovered by the recovery system, thereby reducing waste of the reaction product and the reaction raw material. For example, the remaining methyl chloride and methyl chlorosilane monomers can be recovered by a recovery system.
In practical applications, after the feeding valve is closed to stop adding the reaction raw materials into the fluidized bed reactor, the actual feeding speed of the reaction raw materials is rapidly reduced because a part of the reaction raw materials still remain in the pipeline. Can be reduced to less than or equal to 500Nm in the feed of methyl chloride3And when the reaction time is over/h, opening a third valve, introducing nitrogen into the fluidized bed reactor at a first feeding speed, opening a second valve, and closing the first valve, so that the residual mixture (residual reaction raw materials, methyl chlorosilane and the like) in the fluidized bed reactor is blown into a recovery system, and part of the residual reaction raw materials and residual methyl chlorosilane monomers are recovered through the recovery system.
It is noted that the first feed rate may be 100-200Nm3H, e.g. 100Nm3/h、120Nm3/h、150Nm3/h、170Nm3/h、190Nm3/h、200Nm3/h or between 100 and 200Nm3Other values between/h.
Step S44: and when the preset conditions are met, closing the second valve and opening the first valve, and introducing nitrogen into the fluidized bed reactor at a second feeding speed which is greater than the first feeding speed, wherein the nitrogen is used for enabling the residual mixture in the fluidized bed reactor to flow through the buffer tank and the filter and blow to the inside of the water washing tower.
Communication between the recovery system and the fluidized bed reactor is cut off by closing the second valve.
Because the second feeding speed is higher than the first feeding speed, part of reaction raw materials, residual trace methyl chlorosilane and the like can be quickly blown out by introducing nitrogen into the fluidized bed reactor at the second feeding speed. Wherein, the time of introducing nitrogen into the fluidized bed reactor at the second feeding speed can be 2-3 hours, and the temperature in the fluidized bed reactor can be further reduced to be below 100 ℃ after introducing nitrogen into the fluidized bed reactor at the second feeding speed for 2-3 hours.
When the preset conditions are met, the residual reaction raw materials, methyl chlorosilane and the like in the fluidized bed reactor are generally reflected to be basically blown out by the introduced nitrogen, and at the moment, the nitrogen can be introduced into the fluidized bed reactor at a second feeding speed which is greater than the first feeding speed. Wherein the second feed rate may be 1800-2000Nm3H, e.g. 1800Nm3/h、1850Nm3/h、1900Nm3/h、1950Nm3/h、2000Nm3/h or between 1800 and 2000Nm3Other values between/h.
The predetermined condition may be determined to be satisfied when a time, for example, a time when nitrogen is introduced into the fluidized bed reactor at the first feed rate exceeds a predetermined time. According to practical circumstances, after the nitrogen gas is generally introduced into the fluidized bed reactor at the first feed rate for more than 5 hours, the remaining reaction raw materials, methylchlorosilanes, etc. in the fluidized bed reactor are substantially blown off by the introduced nitrogen gas, and therefore the preset time may be set to be greater than or equal to 5 hours. The preset time is set to 5-8 hours, such as 5 hours, 6 hours, 8 hours, or other values between 5-8 hours.
In addition, in practical application, sampling detection can be performed on the mixture blown into the water washing tower, the content of the reaction raw materials, the methylchlorosilane and the like in the mixture is measured, and when the measured content is lower than a preset content, the residual reaction raw materials, the methylchlorosilane and the like in the fluidized bed reactor can be considered to be blown out by the introduced nitrogen basically, and at this time, the preset condition can also be considered to be met. Wherein, the size of the preset content can be set according to the actual situation.
By adopting the stopping method provided by the embodiment of the application, the nitrogen is additionally introduced into the fluidized bed reactor at the first feeding speed for blowing the mixture in the fluidized bed reactor into the recovery system, so that residual reaction raw materials such as methyl chloride and residual methyl chlorosilane monomers can be recovered through the recovery system, and the waste of the reaction raw materials and products is reduced. The synthesis equipment comprises a fluidized bed reactor, a buffer tank, a filter and a washing tower, wherein the buffer tank is connected with the fluidized bed reactor, the filter is connected with the buffer tank, and the washing tower is connected with the filter. And when the preset conditions are met, nitrogen is introduced at a second feeding speed which is higher than the first feeding speed, and the residual reaction raw materials, residual trace methyl chlorosilane and the like flow through the buffer tank and the filter and are blown to the water washing tower, so that the reaction raw materials such as silicon powder and the like can be filtered or naturally settled out for recycling, and the problems in the prior art are solved. And because the silicon powder is filtered, nitrogen and trace methyl chlorosilane are mainly fed into the water washing tower, the silicon powder can be used as reaction raw materials, and the reaction raw materials are further saved.
The above are merely examples of the present application and are not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (10)
1. A methyl chlorosilane synthesizing device is characterized by comprising: the device comprises a fluidized bed reactor (21), a water washing tower (22) and a filter (24) arranged between the fluidized bed reactor (21) and the water washing tower (22).
2. The synthesis apparatus of claim 1, wherein the synthesis apparatus further comprises: at least one buffer tank (23) disposed between the fluidized bed reactor (21) and the filter (24).
3. A synthesis plant according to claim 2, characterized in that the inflow conduits of the buffer tanks (23) are connected in an eccentric connection.
4. A synthesis plant according to claim 2, characterized in that the number of buffer tanks (23) is 1.
5. A synthesis plant according to claim 4, characterized in that the connection piping of the buffer tank (23) to the fluidized bed reactor (21) comprises a first valve (27).
6. The synthesis apparatus of claim 1, wherein the synthesis apparatus further comprises: a recovery system (29) connected to the fluidized bed reactor (21).
7. A synthesis plant according to claim 6, characterized in that the connection piping of the recovery system (29) to the fluidized-bed reactor (21) comprises a second valve (28).
8. The synthesis apparatus of claim 1, wherein the synthesis apparatus further comprises: a nitrogen supply system (26) connected to the fluidized bed reactor (21).
9. A methyl chlorosilane synthesizing device is characterized by comprising: fluidized bed reactor, water wash tower and set up in fluidized bed reactor with at least one buffer tank between the water wash tower.
10. The synthesis apparatus according to claim 9, wherein the inflow pipes of the buffer tanks are connected in an eccentric connection.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114272857A (en) * | 2021-12-31 | 2022-04-05 | 合盛硅业股份有限公司 | Method and system for replacing synthetic organic silicon monomer raw material |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114272857A (en) * | 2021-12-31 | 2022-04-05 | 合盛硅业股份有限公司 | Method and system for replacing synthetic organic silicon monomer raw material |
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