CN210449120U - Circulating microchannel chlorination reaction device - Google Patents
Circulating microchannel chlorination reaction device Download PDFInfo
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- CN210449120U CN210449120U CN201920925052.8U CN201920925052U CN210449120U CN 210449120 U CN210449120 U CN 210449120U CN 201920925052 U CN201920925052 U CN 201920925052U CN 210449120 U CN210449120 U CN 210449120U
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Abstract
The application discloses a circulating microchannel chlorination reaction device, which comprises a microreactor, a reaction liquid storage tank and a residual chlorine recovery system, wherein a liquid inlet of the microreactor is connected with a reaction raw material liquid storage tank through a pipeline; the liquid outlet of the micro-reactor is connected with the liquid inlet at the top of the reaction liquid storage tank through a pipeline, a gas-liquid mixed product in the micro-reactor is introduced into the reaction liquid storage tank for gas-liquid separation, the gas-liquid separation is carried out to obtain a liquid product and a gas product containing byproduct hydrogen chloride and unreacted chlorine completely, the liquid product is discharged from the liquid outlet at the bottom of the reaction liquid storage tank, the gas product is discharged from the gas outlet at the top of the reaction liquid storage tank, and the gas product is subjected to chlorine recovery through a residual chlorine recovery system. The process device realizes the effective recycling and reusing of the micro-channel reaction on residual chlorine which is not completely reacted in the chlorination reaction, and can effectively improve the raw material chlorination yield.
Description
Technical Field
The utility model relates to a circulation formula microchannel chlorination reaction unit.
Background
The micro-reactor capable of realizing continuous production of micro liquid holdup has the advantages of enhanced mass and heat transfer process, good safety and controllability, easy amplification and the like, and has good application in reactions with strong heat release and higher dangerousness. With the application and development of the micro-reaction industry, the micro-reaction device still has the following problems: (1) the reaction is incomplete, and the effect of one-time reaction is poor; (2) the temperature control in the process is difficult; (3) the post-treatment step is complicated and a batch treatment or the like is still required. Therefore, the improvement space is still large in process and equipment.
Meanwhile, for general chlorination reaction, chlorine usually needs to be greatly excessive relative to reactants, and unreacted chlorine directly enters the tail gas treatment device, so that on one hand, a large amount of residual chlorine is lost, the utilization rate of chlorine is low, and on the other hand, the load and energy consumption of the tail gas treatment device are greatly increased, and resource waste is caused.
Disclosure of Invention
To the above-mentioned technical problem that prior art exists, the utility model aims to provide a circulating microchannel chlorination reaction unit of characteristics such as reasonable in design, reaction effect are good, raw materials utilization rate is high, tail gas treatment load is low.
The circulating microchannel chlorination reaction device is characterized by comprising a microreactor, a reaction liquid storage tank and a residual chlorine recovery system, wherein a liquid inlet of the microreactor is connected with a reaction raw material liquid storage tank through a pipeline; the liquid outlet of the microreactor is connected with the liquid inlet at the top of the reaction liquid storage tank through a pipeline, a gas-liquid mixed product in the microreactor is introduced into the reaction liquid storage tank for gas-liquid separation, the gas-liquid separation is carried out to obtain a liquid product and a gas product containing byproduct hydrogen chloride and unreacted chlorine completely, the liquid product is discharged from the liquid outlet at the bottom of the reaction liquid storage tank, the gas product is discharged from the gas outlet at the top of the reaction liquid storage tank, and the gas product is subjected to chlorine recovery through a residual chlorine recovery system.
The circulating microchannel chlorination reaction device is characterized in that the residual chlorine recovery system comprises a residual chlorine scrubbing tower and a scrubbing pump, a liquid outlet at the bottom of the residual chlorine scrubbing tower is connected with a liquid inlet of the scrubbing pump through a pipeline, a liquid outlet pipe of the scrubbing pump is divided into two paths, one path of the two paths of the liquid outlet pipe is used for discharging hydrochloric acid byproducts formed by absorbing hydrogen chloride, the other path of the liquid outlet pipe is connected with a liquid inlet at the upper part of the residual chlorine scrubbing tower, and a tap water feeding pipe is further arranged at the upper part of the residual chlorine scrubbing tower; and a gas inlet at the lower part of the residual chlorine scrubbing tower is connected with a gas outlet at the top of the reaction liquid storage tank through a pipeline, and chlorine discharged from the gas outlet at the top of the residual chlorine scrubbing tower is introduced into the microreactor to carry out chlorination reaction.
The circulating microchannel chlorination reaction device is characterized in that the residual chlorine recovery system further comprises a drying box, a compressor and a chlorine buffer tank which are sequentially connected through pipelines, and an air outlet at the top of the residual chlorine scrubbing tower is connected with a second path of air inlet pipe of the microreactor through the drying box, the compressor and the chlorine buffer tank through pipelines.
The circulating microchannel chlorination reaction device is characterized by further comprising a reaction liquid circulating pump, wherein a liquid outlet at the bottom of the reaction liquid storage tank is connected with a liquid inlet of the reaction liquid circulating pump through a pipeline, a liquid outlet pipe of the reaction liquid circulating pump is divided into two paths, a chlorination reaction product is discharged all the way, and the other path is connected to a pipeline between a liquid inlet of the microreactor and a reaction raw material liquid storage tank.
The basic principle of the technology is as follows: the traditional micro-reaction technology and the chlorine gas recovery technology are re-integrated, the traditional micro-reaction technology is improved through a novel and reasonable process integration design, multiple chlorination is realized by adopting circulating feeding, and the chlorine gas is recycled by adopting residual chlorine recovery. Thereby achieving the purposes of full reaction of materials and high utilization rate of raw materials.
The utility model discloses circulation formula microchannel chlorination reaction unit compares with current chlorination technique has following characteristics:
(1) the traditional chlorination reaction technology mostly adopts an intermittent kettle type reaction, the reaction is violent in heat release, the operation period is long, the technology adopts a micro-reactor for continuous chlorination, the risk of chlorination reaction is effectively reduced, the operation is simplified, and the reaction is controllable.
(2) Traditional microchannel reaction technique directly squeezes into the reaction unit with the reaction raw materials and reacts the back direct processing reaction liquid, and the reaction yield is low, and this technique transports again to the feed end after separating reaction liquid gas-liquid, can realize many times reaction, and the degree of depth reaction can be realized to single microreactor, adopts the mode of material circulation reaction simultaneously, can effectively improve the reaction yield, improves the rate of equipment utilization of reactor, reduces disposable equipment investment cost, and the benefit is obvious.
(3) Chlorine usually is far away from the reactant in the chlorination, and unreacted chlorine and hydrogen chloride directly get into tail gas processing apparatus after the reaction, and chlorine loss is big, and tail gas treatment load is big, and this technique is through the processing of spraying to reaction tail gas, detach the hydrogen chloride in the tail gas, and the chlorine recycle that has not reacted has effectively improved the utilization ratio of chlorine, has reduced tail gas emission to can realize the by-product hydrochloric acid.
(4) The technology improves the utilization rate of reactant atoms, improves the reaction yield, reduces the emission of chlorine, and belongs to the green chemical technology. The process device of the utility model realizes that the microchannel reaction is applied to the effective recovery and reuse of the residual chlorine which is not completely reacted in the chlorination reaction, thereby improving the use efficiency of the chlorine; the chlorination liquid is circularly conveyed back to the raw material feeding pipeline, so that multistage chlorination can be carried out, and the raw material chlorination yield can be effectively improved.
Drawings
FIG. 1 is a schematic structural view of a circulating microchannel chlorination reactor of the present invention;
in the figure: the method comprises the following steps of 1-a microreactor, 2-a reaction liquid storage tank, 3-a reaction liquid circulating pump, 4-a residual chlorine scrubbing tower, 5-a scrubbing pump, 6-a drying box, 7-a compressor, 8-a chlorine buffer tank and a reaction raw material liquid storage tank.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b): compare FIG. 1
A circulating microchannel chlorination reaction device comprises a microreactor 1, a reaction liquid storage tank 2 and a residual chlorine recovery system, wherein a liquid inlet of the microreactor 1 is connected with a reaction raw material liquid storage tank a through a pipeline, a gas inlet pipe of the microreactor 1 is divided into two paths, a first path of gas inlet pipe of the microreactor 1 is filled with a chlorine raw material, and a second path of gas inlet pipe of the microreactor 1 is filled with chlorine obtained by recovery of the residual chlorine recovery system; the liquid outlet of the microreactor 1 is connected with the liquid inlet at the top of the reaction liquid storage tank 2 through a pipeline, a gas-liquid mixed product in the microreactor 1 is introduced into the reaction liquid storage tank 2 for gas-liquid separation, the gas-liquid separation is carried out to obtain a liquid product and a gas product containing by-product hydrogen chloride and unreacted chlorine, the liquid product is discharged from the liquid outlet at the bottom of the reaction liquid storage tank 2, the gas product is discharged from the gas outlet at the top of the reaction liquid storage tank 2, and the gas product is subjected to chlorine recovery through a residual chlorine recovery system.
The residual chlorine recovery system comprises a residual chlorine scrubbing tower 4, a scrubbing pump 5, a drying box 6, a compressor 7 and a chlorine buffer tank 8 which are sequentially connected through pipelines, wherein a liquid outlet at the bottom of the residual chlorine scrubbing tower 4 is connected with a liquid inlet of the scrubbing pump 5 through a pipeline, a liquid outlet pipe of the scrubbing pump 5 is divided into two paths, one path of the liquid outlet pipe is used for discharging hydrochloric acid byproducts formed by absorbing hydrogen chloride, the other path of the liquid outlet pipe is connected to a liquid inlet at the upper part of the residual chlorine scrubbing tower 4, and a tap water feeding pipe is further arranged at the upper part of the residual chlorine scrubbing; the air inlet at the lower part of the residual chlorine scrubbing tower 4 is connected with the air outlet at the top of the reaction liquid storage tank 2 through a pipeline, the air outlet at the top of the residual chlorine scrubbing tower 4 is connected with the second path of air inlet pipe of the microreactor 1 through a drying box 6, a compressor 7 and a chlorine buffer tank 8 through a pipeline, and chlorine discharged from the air outlet at the top of the residual chlorine scrubbing tower 4 is introduced into the microreactor 1 to perform chlorination reaction.
In order to promote chlorination's effect, the utility model discloses still include reaction liquid circulating pump 3, the liquid outlet of 2 bottoms of reaction liquid storage tanks is connected by the pipeline with reaction liquid circulating pump 3's inlet, and reaction liquid circulating pump 3's drain pipe divide into two the tunnel, and discharge chlorination reaction product all the way, another way is connected to on the inlet of microreactor 1 and the pipeline between the raw materials liquid storage tank a of reaction.
Utilize the utility model discloses a when the structure carries out chlorination reaction, the working process is:
a reaction material inlet of the microreactor 1 is divided into a gas phase inlet and a liquid phase inlet, chlorine is used as a gas material, and a reaction liquid raw material is used as a liquid material and enters the microreactor to carry out chlorination reaction. A material outlet of the microreactor 1 is connected with the reaction liquid storage tank 2 through a pipeline, and the chlorination reactant, the byproduct hydrogen chloride and the unreacted chlorine gas are subjected to gas-liquid separation in the reaction liquid storage tank 2. The liquid outlet at the bottom of the reaction liquid storage tank 2 is connected with the reaction liquid circulating pump 3 through a pipeline, the outlet of the reaction liquid circulating pump 3 is divided into two streams of materials, one stream is taken out as a product after complete chlorination, the other stream is taken as a product which is not completely chlorinated and is conveyed to the raw material inlet of the microreactor 1 for secondary chlorination reaction, and the progress of the chlorination reaction is controlled by regulating and controlling the flow rate ratio of the two streams of materials at the outlet of the reaction liquid circulating pump 3.
The gas phase outlet of the reaction liquid storage tank 2 is connected with the gas phase inlet of the residual chlorine scrubber 4 through a pipeline, and the gas phase contains byproduct hydrogen chloride and unreacted chlorine. Tap water is added into a tower kettle of a residual chlorine gas washing tower 4, a liquid outlet at the bottom of the residual chlorine gas washing tower 4 is connected with a gas washing pump 5 through a pipeline, an outlet of the gas washing pump 5 is connected with a spray opening at the upper part of a packing section of the residual chlorine gas washing tower 4 through a pipeline, the tap water is circulated through the gas washing pump 5 to spray and clean reaction gas phase entering the residual chlorine gas washing tower 4, hydrogen chloride is absorbed by spray water to form hydrochloric acid solution, and the hydrochloric acid solution is extracted through an outlet of the gas washing pump 5 after reaching a certain concentration and serves as byproduct hydrochloric acid; the residual chlorine enters the drying box 6 through the outlet at the top of the residual chlorine scrubbing tower 4 to be dried and dewatered, the outlet of the drying box 6 is connected with the compressor 7 through a pipeline, the residual chlorine enters the chlorine buffer tank 8 through compression, the outlet of the chlorine buffer tank 8 is connected with the gas phase inlet of the microreactor 1 through a pipeline, and the buffered residual chlorine enters the microreactor 1 to be reused.
The utility model discloses a processing and manufacturing of circulation type microchannel chlorination reaction device is very simple and convenient, and the processing and manufacturing equipment shown according to the instruction attached drawing can.
The utility model discloses an use and to realize single micro-reactor multistage reaction, reduce the equipment investment, retrieve the chlorine residue, improved the utilization ratio of chlorine, have good economic benefits.
Compared with the prior traditional microchannel reaction technology, the utility model can effectively reduce the chlorine loss caused by the direct treatment of the unreacted chlorine in the chlorination reaction, improve the utilization rate of chlorine atoms and reduce the energy consumption and the device load of tail gas treatment; meanwhile, a material circulation reaction mode is adopted, so that the reaction yield can be effectively improved, the equipment utilization rate of the reactor is improved, the one-time equipment investment cost is reduced, and the benefit is obvious.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (4)
1. A circulating microchannel chlorination reaction device is characterized by comprising a microreactor (1), a reaction liquid storage tank (2) and a residual chlorine recovery system, wherein a liquid inlet of the microreactor (1) is connected with a reaction raw material liquid storage tank (a) through a pipeline, a gas inlet pipe of the microreactor (1) is divided into two paths, a chlorine raw material is introduced into the first path of gas inlet pipe, and chlorine obtained by recovery of the residual chlorine recovery system is introduced into the second path of gas inlet pipe; the liquid outlet of the microreactor (1) is connected with the liquid inlet at the top of the reaction liquid storage tank (2) through a pipeline, a gas-liquid mixed product in the microreactor (1) is introduced into the reaction liquid storage tank (2) for gas-liquid separation, the gas-liquid separation is carried out to obtain a liquid product and a gas product containing byproduct hydrogen chloride and unreacted chlorine, the liquid product is discharged from the liquid outlet at the bottom of the reaction liquid storage tank (2), the gas product is discharged from the gas outlet at the top of the reaction liquid storage tank (2), and the gas product is subjected to chlorine recovery through a residual chlorine recovery system.
2. The circulating microchannel chlorination reaction device of claim 1, wherein the residual chlorine recovery system comprises a residual chlorine scrubbing tower (4) and a scrubbing pump (5), a liquid outlet at the bottom of the residual chlorine scrubbing tower (4) is connected with a liquid inlet of the scrubbing pump (5) through a pipeline, a liquid outlet pipe of the scrubbing pump (5) is divided into two paths, one path of the liquid outlet pipe discharges hydrochloric acid byproducts formed by absorbing hydrogen chloride, the other path of the liquid outlet pipe is connected with a liquid inlet at the upper part of the residual chlorine scrubbing tower (4), and a tap water feeding pipe is further arranged at the upper part of the residual chlorine scrubbing tower (4); the gas inlet at the lower part of the residual chlorine scrubbing tower (4) is connected with the gas outlet at the top of the reaction liquid storage tank (2) through a pipeline, and chlorine gas discharged from the gas outlet at the top of the residual chlorine scrubbing tower (4) is introduced into the microreactor (1) for chlorination reaction.
3. The circulating microchannel chlorination reaction device of claim 2, wherein the residual chlorine recovery system further comprises a drying box (6), a compressor (7) and a chlorine buffer tank (8) which are sequentially connected by a pipeline, and an air outlet at the top of the residual chlorine scrubbing tower (4) is connected with the second air inlet pipe of the microreactor (1) through the drying box (6), the compressor (7) and the chlorine buffer tank (8) by a pipeline.
4. The circulating microchannel chlorination reaction device of claim 1, further comprising a reaction liquid circulating pump (3), wherein a liquid outlet at the bottom of the reaction liquid storage tank (2) is connected with a liquid inlet of the reaction liquid circulating pump (3) through a pipeline, a liquid outlet pipe of the reaction liquid circulating pump (3) is divided into two paths, one path is used for discharging chlorination reaction products, and the other path is connected to a pipeline between the liquid inlet of the microreactor (1) and the reaction raw material liquid storage tank (a).
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| CN201920925052.8U CN210449120U (en) | 2019-06-19 | 2019-06-19 | Circulating microchannel chlorination reaction device |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115634642A (en) * | 2021-07-19 | 2023-01-24 | 河北大景大搪化工设备有限公司 | Chlorinated fatty acid methyl ester reaction tower and preparation device formed by same |
| CN116393048A (en) * | 2023-06-07 | 2023-07-07 | 山东金城医药化工有限公司 | Continuous production system and production method of ethyl 4-chloro-2-methoxyiminoacetoacetate |
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2019
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115634642A (en) * | 2021-07-19 | 2023-01-24 | 河北大景大搪化工设备有限公司 | Chlorinated fatty acid methyl ester reaction tower and preparation device formed by same |
| CN116393048A (en) * | 2023-06-07 | 2023-07-07 | 山东金城医药化工有限公司 | Continuous production system and production method of ethyl 4-chloro-2-methoxyiminoacetoacetate |
| CN116393048B (en) * | 2023-06-07 | 2023-09-12 | 山东金城医药化工有限公司 | Continuous production system and production method of ethyl 4-chloro-2-methoxyiminoacetoacetate |
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