CN110947348A - Micro-channel continuous ozone oxidation device - Google Patents
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Abstract
The invention relates to the technical field of gas-liquid oxidation, in particular to a microchannel continuous ozone oxidation device, wherein an oxygen gas cylinder, an ozone generator, an ozone supercharger and a first feeding port of an ozonization micro-reactor in an ozone oxidation system are sequentially connected in series, a substrate solution storage tank, a first metering pump and a second feeding port of the ozonization micro-reactor are sequentially connected in series, a discharge port of the ozonization micro-reactor, a gas-liquid separation tank and an oxide storage tank are sequentially connected in series, a quenching system is provided with a quenching micro-reactor and a quenching agent storage tank, the oxide storage tank, the quenching micro-reactor and a product storage tank are sequentially connected in series, a detection system is provided with an ozone analyzer, and an output end of the ozone generator and a tail gas output port of the. The invention can safely and effectively improve the ozone flux, integrates the ozone oxidation reaction and the quenching reaction, realizes the full continuous process, can greatly avoid side reaction, ensures the safety and improves the reaction efficiency.
Description
Technical Field
The invention relates to the technical field of gas-liquid oxidation, in particular to a micro-channel continuous ozone oxidation device.
Background
Ozone, as a strong oxidizing agent, is widely used in the research fields of medicines, pesticide intermediates and the like because of its high-efficiency cleaning property for oxidizing unsaturated molecules. The organic matter capable of being oxidized by ozone mainly comprises olefins, amines, carbocycles, aromatic compounds and the like, wherein the double bond oxidation capability of the olefin compounds is strongest.
The characteristics and dangers of the ozone oxidation reaction comprise: 1. the ozone has high potential and is easy to cause explosion accidents; 2. the ozone oxidation reaction belongs to a reaction process with high heat release, and the reaction risk is high; 3. in the traditional intermittent gas-liquid reaction, the poor gas-liquid mixing effect causes the low utilization rate of ozone, and the existence of redundant unreacted ozone easily causes safety accidents. Therefore, the research on the intrinsic safety of the ozone oxidation reaction is more and more focused.
The microchannel reactor has the characteristics of high mass transfer rate, good heat exchange efficiency, high safety performance, excellent automatic control performance and the like. For gas-liquid reaction, compared with conventional gas-liquid reaction equipment, the microchannel reactor has the advantages that the contact area of a gas-liquid phase boundary is increased by at least 1-2 orders of magnitude, and the gas-liquid mass transfer and heat exchange are greatly enhanced. The microchannel reactor is adopted to carry out the ozone oxidation reaction, so that the reaction rate can be improved, and the deterioration of intermediate products is avoided, thereby improving the yield.
Sandra et al (org. Process Res. Dev.2009,13, 952-. Claudio et al (org. Process Res. Dev.2012,16, 798-.
The above-mentioned microchannel ozone oxidation device is not comprehensive in terms of precise control of reaction, ozone detection equipment, ozone oxidation and quenching technology, and the adopted microchannel reaction device has difficulty in amplification.
Disclosure of Invention
The invention aims to provide a micro-channel continuous ozone oxidation device which can safely and effectively improve ozone flux, integrates the processes of ozone oxidation reaction and quenching reaction, realizes a full continuous process, can greatly avoid side reaction and improve reaction efficiency.
The purpose of the invention is realized by the following technical scheme:
a microchannel continuous ozone oxidation device comprises an ozone oxidation system, a quenching system, a detection system and a product storage tank, wherein the ozone oxidation system comprises an oxygen gas cylinder, an ozone generator, an ozone supercharger, a substrate solution storage tank, a first metering pump, an ozonization micro-reactor, a gas-liquid separation tank and an oxide storage tank, the oxygen gas cylinder, the ozone generator, the ozone supercharger and a first feeding port of the ozonization micro-reactor are sequentially connected in series, the substrate solution storage tank, the first metering pump and a second feeding port of the ozonization micro-reactor are sequentially connected in series, a discharging port of the ozonization micro-reactor, the gas-liquid separation tank and the oxide storage tank are sequentially connected in series, the quenching system is provided with a quenching micro-reactor and a quenching agent storage tank, the quenching agent storage tank is connected with the quenching micro-reactor, the oxide storage, the detection system comprises an ozone analyzer, an ozone destructor and a tail gas absorption storage tank which are sequentially connected in series, and the output end of the ozone generator and the tail gas output port of the gas-liquid separation tank are respectively connected with the ozone analyzer through pipelines.
And a first heat exchanger is arranged between the first metering pump and the ozonation microreactor, and a second heat exchanger is arranged between the ozonation microreactor and the gas-liquid separation tank.
An oxygen inlet valve is arranged between the oxygen gas bottle and the ozone generator, and an ozone gas storage tank, a pressure gauge, a pressure reducing valve and a first gas mass flow controller are sequentially arranged on a pipeline between the ozone supercharger and the ozonization micro-reactor.
And a pressure sensor, a temperature sensor and a liquid discharge valve are arranged on a pipeline between the first metering pump and the ozonization micro-reactor.
And a pressure sensor, a temperature sensor and a liquid discharge valve are arranged on a pipeline between the ozonation microreactor and the gas-liquid separation tank.
And the nitrogen gas cylinder is connected with the ozonization micro-reactor and the gas-liquid separation tank through a gas path, and a nitrogen gas inlet valve is arranged on the gas path.
The oxide storage tank is connected with a first input port of the quenching microreactor, a second metering pump is arranged between the oxide storage tank and the quenching microreactor, the quenching agent storage tank is connected with a second input port of the quenching microreactor, a third metering pump is arranged between the quenching agent storage tank and the quenching microreactor, and an output port of the quenching microreactor is connected with the product storage tank.
And a pressure sensor, a temperature sensor and a liquid discharge valve are arranged on a pipeline between the quenching agent storage tank and the quenching micro-reactor.
The top of the gas-liquid separation tank is provided with a gas outlet pipeline, a three-way valve A is arranged on a pipeline between the ozone generator and the ozone booster, a test pipeline led out by the three-way valve A is converged on a three-way valve B with the gas outlet pipeline, and the led-out pipeline of the three-way valve B is connected with the ozone analyzer.
And a second gas mass flow controller is arranged on a pipeline between the ozone analyzer and the ozone destructor.
The invention has the advantages and positive effects that:
1. compared with the existing micro-channel ozone oxidation device, the invention can effectively increase the concentration of ozone, thereby improving the concentration of liquid-phase materials and improving the production efficiency, in addition, the invention adopts complete and standard ozone generating equipment, analytical equipment and a destroying device, greatly ensures the safety of the device, uses a complete gas-liquid separation device, ensures the seamless connection of an ozonization process and a quenching process, realizes a full continuous process, reduces the product shelf time, prevents the product from deteriorating, and also improves the yield of the product in the reaction process.
2. Compared with the effect of intermittent equipment, the invention ensures that the safety is improved, and simultaneously the conditions such as reaction temperature, residence time, reaction pressure and the like are accurately controlled by the microchannel continuous device, so that the whole process is accurately controllable, the energy consumption is strictly reduced, the cost is reduced, and the olefin reaction yield is improved to more than 95 percent from 60-80 percent of the intermittent reaction by utilizing the efficient mixing action of the microreactor.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
Wherein, 1 is an ozonization micro-reactor; 2 is an ozone generator; 3 is an ozone supercharger; 4 is a first gas mass flow controller; 5 is a substrate solution storage tank; 6 is a gas-liquid separating tank; 7 is an oxide storage tank; 8 is a first metering pump; 9 is an ozone analyzer; 10 is an ozone destructor; 11 is a tail gas absorption storage tank; 12 is an oxygen cylinder; 13 is a nitrogen gas cylinder; 14 is a quenching micro-reactor; 15 is a quencher storage tank; 16 is a third metering pump; 17 is a product storage tank, 18 is a second metering pump, 19 is a second gas mass flow controller, 20 is a first feeding port, 21 is a second feeding port, 22 is a discharging pipeline, 23 is a three-way valve A, 24 is a testing pipeline, 25 is an air outlet pipeline, 26 is a three-way valve B, 27 is an ozone storage tank, 28 is a first four-way valve, 29 is a second four-way valve, and 30 is a third four-way valve.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
As shown in fig. 1, the present invention comprises an ozone oxidation system, a quenching system, a detection system and a product storage tank 17, wherein the ozone oxidation system comprises an oxygen gas cylinder 12, an ozone generator 2, an ozone supercharger 3, a substrate solution storage tank 5, a first metering pump 8, an ozonization microreactor 1, a gas-liquid separation tank 6 and an oxide storage tank 7, the oxygen gas cylinder 12, the ozone generator 2, the ozone supercharger 3 and a first inlet 20 of the ozonization microreactor 1 are sequentially connected in series, the substrate solution storage tank 5, the first metering pump 8 and a second inlet 21 of the ozonization microreactor 1 are sequentially connected in series, a discharge port of the ozonization microreactor 1, the gas-liquid separation tank 6 and the oxide storage tank 7 are sequentially connected in series, the quenching system is provided with a quenching microreactor 14, and the oxide storage tank 7, the quenching microreactor 14 and the, the detection system is provided with an ozone analyzer 9, and the output end of the ozone generator 2 and the tail gas output port of the gas-liquid separation tank 6 are respectively connected with the ozone analyzer 9 through pipelines. The ozone generator 2, the ozone supercharger 3 and the gas-liquid separation tank 6 are all known technologies in the field and are commercially available products, wherein the ozone supercharger 3 provides power by means of an air pressure pump to compress ozone, and a digital display liquid level meter is arranged on the gas-liquid separation tank 6 and used for observing the height of liquid level in the tank body.
As shown in fig. 1, a first heat exchanger is provided in a pipeline between the first metering pump 8 and the ozonation microreactor 1, and a second heat exchanger is provided in a pipeline between the ozonation microreactor 1 and the gas-liquid separation tank 6. The substrate solution reaches a specified reaction temperature after passing through the first heat exchanger 28, and the output solution of the ozonation microreactor 1 reaches a specified reaction temperature after passing through the second heat exchanger 29. The heat exchanger is well known in the art and is a commercially available product.
Be equipped with the oxygen admission valve of adjustment oxygen air input between oxygen gas cylinder 12 and ozone generator 2, be equipped with ozone gas holder 27, manometer, relief pressure valve and first gas mass flow controller 4 on the pipeline between ozone booster 3 and the ozonization microreactor 1 in proper order, wherein the manometer is used for detecting the atmospheric pressure condition, and the relief pressure valve is used for adjusting admission pressure, and first gas mass flow controller 4 control gas flow, first gas mass flow controller 4 accessible PIC automatic control system adjusts.
The device comprises an ozonization micro-reactor 1, a first metering pump 8, an ozonization micro-reactor 1, a second metering pump 8, a gas-liquid separation tank 6, a first four-way valve 28, a second four-way valve 29, a pressure sensor, a temperature sensor and a liquid discharge valve, wherein the first metering pump 8 is arranged on a pipeline between the first metering pump 8 and the ozonization micro-reactor 1, the second four-way valve is arranged on a pipeline between the ozonization micro-reactor 1 and the gas-liquid separation tank 6, each four-way valve is provided with four interfaces which are respectively a material inlet, a material outlet, a liquid discharge port and an interface connected with the temperature sensor, the first metering pump 8 is used for pumping raw materials into the ozonization micro-reactor at a certain flow rate, the pressure sensor and the temperature sensor detect the liquid.
The top end of the gas-liquid separation tank 6 is provided with a gas outlet pipeline 25, the gas outlet pipeline 25 is provided with a pressure reducing valve for adjusting the gas pressure, and a discharge control valve is arranged on a pipeline between the gas-liquid separation tank 6 and the oxide storage tank 7.
As shown in fig. 1, a nitrogen gas cylinder 13 is connected with the ozonation microreactor 1 and the gas-liquid separation tank 6 through a gas path, so that the whole system forms nitrogen protection, and a nitrogen gas inlet valve for adjusting the nitrogen gas inflow is arranged on the gas path.
As shown in fig. 1, the quenching system includes a quenching microreactor 14, a quencher storage tank 15, a second metering pump 18 and a third metering pump 16, wherein the oxide storage tank 7 is connected to a first input port of the quenching microreactor 14 through a pipeline, the quencher storage tank 15 is connected to a second input port of the quenching microreactor 14 through a pipeline, the second metering pump 18 is disposed on a pipeline between the oxide storage tank 7 and the quenching microreactor 14, the third metering pump 16 is disposed on a pipeline between the quencher storage tank 15 and the quenching microreactor 14, and an output port of the quenching microreactor 14 is connected to the product storage tank 17 through a pipeline. The second metering pump 18 and the third metering pump 16 are used for pumping the ozonized reaction liquid and the quenching agent into the quenching agent microreactor 14 at a certain flow rate, a pressure sensor, a temperature sensor and a liquid discharge valve are arranged on a pipeline between the quenching agent storage tank 15 and the quenching microreactor 14, a third four-way valve 30 is arranged on a pipeline between the quenching agent storage tank 15 and the quenching microreactor 14, and the third four-way valve 30 is provided with four interfaces which are respectively a material inlet, a material outlet, a liquid discharge port and an interface connected with the temperature sensor. The ozonation microreactor 1 and the quench microreactor 14 are microchannel reactors, which are well known in the art.
As shown in fig. 1, a three-way valve a23 is arranged on a pipeline between the ozone generator 2 and the ozone supercharger 3, a test pipeline 24 led out by the three-way valve a23 and an outlet pipeline 25 of the gas-liquid separation tank 6 are converged on a three-way valve B26, and a lead-out pipeline of the three-way valve B26 is connected with the ozone analyzer 9, wherein the test pipeline 24 is connected with the ozone analyzer 9 to test the ozone generating capacity of the ozone generator 2, and the outlet pipeline 25 is connected with the ozone analyzer 9 to measure the residual ozone amount after the reaction.
As shown in fig. 1, the detection system comprises an ozone analyzer 9, an ozone destructor 10 and a tail gas absorption storage tank 11 which are connected in series in sequence, and a second gas mass flow controller 19 is arranged on a pipeline between the ozone analyzer 9 and the ozone destructor 10. The ozone analyzer 9 and the ozone destructor 10 are well known in the art and are commercially available products, wherein the output of the ozone analyzer 9 is provided with a dryer.
The working principle of the invention is as follows:
when the invention works, gas in an oxygen gas bottle 12 and raw material liquid in a substrate solution storage tank 5 enter an ozonization microreactor 1 at a certain flow rate, wherein the substrate solution is adjusted to the reaction temperature by a first heat exchanger 28, two gas-liquid materials enter the ozonization microreactor 1 through different material inlets according to a certain material proportion, then are efficiently mixed in the ozonization microreactor 1 to generate gas-liquid reaction, then under the action of gas separation of a gas-liquid separation tank 6, reaction liquid is obtained and stored in an oxide storage tank 7 to finish the gas-liquid reaction process, the reaction liquid in the oxide storage tank 7 is pumped into a quenching microreactor 14 through a second metering pump 18, a quenching agent is pumped into the quenching microreactor 14 through a third metering pump 16, the quenching agent reaches a specified reaction temperature under the condition of heat exchange of the heat exchanger 30, and the reaction liquid and the quenching agent generate quenching reaction in the quenching microreactor 14, the final product is stored in product tank 17 to complete the quenching process. Finally, qualified products are obtained in the post-treatment processes of extraction, distillation, purification and the like. In addition, the ozone analyzer 9 in the detection system of the invention can test the ozone generating capacity of the ozone generator 2 from the test pipeline 24 on one hand, and measure the residual ozone amount after reaction from the gas outlet pipeline 25 on the other hand, and the equipment system can be adjusted in time according to the test condition, thereby safely and effectively improving the ozone flux.
The invention is further illustrated below by means of a few application examples.
Application example 1
The application example carries out the ozone oxidation reaction of anethole, and comprises the following specific steps:
firstly adjusting a nitrogen gas inlet valve, blowing the whole reaction system by using nitrogen gas to ensure the cleanness of the system, then adjusting an oxygen gas inlet valve to enable oxygen to enter, starting an ozone generator 2 and an ozone supercharger 3, boosting the mixed gas of ozone and oxygen by using the ozone supercharger 3, and simultaneously starting a cold-hot circulation all-in-one machine matched with each heat exchanger to enable each heat exchanger to start preheating.
Preparing an anethole solution with the mass concentration of 10% (the solvent is a mixed solvent of absolute ethyl alcohol and normal hexane in a volume ratio of 1: 4), setting the volume flow of ozone/oxygen mixed gas to be 1L/min through a first gas mass flow controller 4, setting the concentration of ozone generated by an ozone generator 2 to be 120ppm, adjusting the flow rate of a liquid phase substrate to be 5ml/min through a first metering pump 8, carrying out ozonization reaction when the temperature of gas and liquid reaches 0 ℃ after the gas and liquid enter an ozonization microreactor 1 to obtain ozonization reaction liquid with complete reaction, pumping the ozonization reaction liquid and a sodium sulfite solution with the concentration of 15% of a quenching agent into a quenching microreactor 14 according to the molar ratio of 1:1 after gas-liquid separation at the flow rate of 20ml/min (controlled by a second metering pump 18 and a third metering pump 16), carrying out quenching reaction at-10 ℃, finally obtaining the product reaction liquid. The final product anisaldehyde is obtained through the processes of extraction, distillation and purification, the yield is 97 percent, and the purity is 99 percent. The reaction formula of the application example is as follows:
application example 2
The application example performs the ozone oxidation reaction of the cinnamaldehyde, and comprises the following specific steps:
firstly, adjusting a nitrogen gas inlet valve, blowing the whole reaction system by using nitrogen gas to ensure the cleanness of the system, then adjusting an oxygen gas inlet valve, blowing a pipeline by using oxygen gas, starting an ozone generator 2 and an ozone supercharger 3, pressurizing ozone/oxygen mixed gas, and simultaneously starting a cold-hot circulation all-in-one machine matched with each heat exchanger.
Preparing a 10% cinnamaldehyde solution (absolute ethyl alcohol as a solvent), setting the volume flow of an ozone/oxygen mixed gas to be 1L/min, setting the ozone concentration to be 120ppm, adjusting the flow rate of a liquid phase substrate to be 5ml/min, carrying out ozonization reaction when the temperature reaches-10 ℃ after gas and liquid enter an ozonization microreactor 1 to obtain ozonization reaction liquid with complete reaction, carrying out quenching reaction on ozonization reactants subjected to gas-liquid separation and a quenching agent thiourea at-10 ℃ according to the molar ratio of 1:1 and the flow rate of 20ml/min to finally obtain a product reaction liquid. The final product benzaldehyde is obtained through the processes of extraction, distillation and purification, the yield is 98 percent, and the purity is 99 percent. The reaction formula of the application example is as follows:
application example 3
The application example performs an ozone oxidation reaction of cyclohexene, and comprises the following specific steps:
firstly, adjusting a nitrogen gas inlet valve, blowing the whole reaction system by using nitrogen to ensure that the system is clean, then adjusting an oxygen gas inlet valve, blowing a pipeline by using oxygen, starting an ozone generator, pressurizing ozone/oxygen mixed gas, and simultaneously starting a cold-hot circulation all-in-one machine.
Preparing 12.5% cyclohexene solution (solvent is mixed solvent of glacial acetic acid and dichloroethane with volume ratio of 1: 2), setting volume flow of ozone/oxygen gas mixture at 0.5L/min, setting ozone concentration at 120ppm, and adjusting liquid phase substrate flow rate at 10 ml/min. And carrying out ozonization reaction when the temperature of the system reaches 5 ℃ to obtain ozonization reaction liquid with complete reaction. Carrying out gas-liquid separation on the ozonized reactant and a 15% sodium sulfite solution of a quenching agent according to a molar ratio of 1:1, and carrying out quenching reaction at 0 ℃ at flow rates of 20ml/min respectively to finally obtain a product reaction liquid. The final product 1, 6-hexanedial is obtained with the yield of 96 percent and the purity of 99 percent through the processes of extraction, water washing, distillation and reduced pressure distillation. The reaction formula of the application example is as follows:
Claims (10)
1. a microchannel continuous ozone oxidation device is characterized in that: the device comprises an ozone oxidation system, a quenching system, a detection system and a product storage tank (17), wherein the ozone oxidation system comprises an oxygen gas cylinder (12), an ozone generator (2), an ozone supercharger (3), a substrate solution storage tank (5), a first metering pump (8), an ozonization micro-reactor (1), a gas-liquid separation tank (6) and an oxide storage tank (7), the oxygen gas cylinder (12), the ozone generator (2), the ozone supercharger (3) and a first feeding port (20) of the ozonization micro-reactor (1) are sequentially connected in series, the substrate solution storage tank (5), the first metering pump (8) and a second feeding port (21) of the ozonization micro-reactor (1) are sequentially connected in series, a discharge port of the ozonization micro-reactor (1), the gas-liquid separation tank (6) and the oxide storage tank (7) are sequentially connected in series, the quenching system is provided with a quenching micro-reactor (14, and the quenching agent storage tank (15) is connected with the quenching microreactor (14), the oxide storage tank (7), the quenching microreactor (14) and the product storage tank (17) are sequentially connected in series, the detection system comprises an ozone analyzer (9), an ozone destructor (10) and a tail gas absorption storage tank (11) which are sequentially connected in series, and the output end of the ozone generator (2) and the tail gas output port of the gas-liquid separation tank (6) are respectively connected with the ozone analyzer (9) through pipelines.
2. The microchannel continuous ozonation device according to claim 1, wherein: a first heat exchanger is arranged between the first metering pump (8) and the ozonization microreactor (1), and a second heat exchanger is arranged between the ozonization microreactor (1) and the gas-liquid separation tank (6).
3. The microchannel continuous ozonation device according to claim 1, wherein: an oxygen inlet valve is arranged between the oxygen gas bottle (12) and the ozone generator (2), and an ozone gas storage tank (27), a pressure gauge, a pressure reducing valve and a first gas mass flow controller (4) are sequentially arranged on a pipeline between the ozone supercharger (3) and the ozonization microreactor (1).
4. The microchannel continuous ozonation device according to claim 1, wherein: and a pressure sensor, a temperature sensor and a liquid discharge valve are arranged on a pipeline between the first metering pump (8) and the ozonization microreactor (1).
5. The microchannel continuous ozonation device according to claim 1, wherein: and a pressure sensor, a temperature sensor and a liquid discharge valve are arranged on a pipeline between the ozonization microreactor (1) and the gas-liquid separation tank (6).
6. The microchannel continuous ozonation device according to claim 1, wherein: and a nitrogen gas bottle (13) is connected with the ozonization microreactor (1) and the gas-liquid separation tank (6) through a gas path, and a nitrogen gas inlet valve is arranged on the gas path.
7. The microchannel continuous ozonation device according to claim 1, wherein: the oxide storage tank (7) is connected with a first input port of the quenching microreactor (14), a second metering pump (18) is arranged between the oxide storage tank (7) and the quenching microreactor (14), the quenching agent storage tank (15) is connected with a second input port of the quenching microreactor (14), a third metering pump (16) is arranged between the quenching agent storage tank (15) and the quenching microreactor (14), and an output port of the quenching microreactor (14) is connected with the product storage tank (17).
8. The microchannel continuous ozone oxidation device as set forth in claim 1 or 7, wherein: and a pressure sensor, a temperature sensor and a liquid discharge valve are arranged on a pipeline between the quenching agent storage tank (15) and the quenching microreactor (14).
9. The microchannel continuous ozonation device according to claim 1, wherein: the top of gas-liquid separation jar (6) is equipped with gas outlet pipeline (25), be equipped with a three-way valve A (23) on the pipeline between ozone generator (2) and ozone booster (3), and by three-way valve A (23) draw forth a test pipeline (24) with gas outlet pipeline (25) assemble on a three-way valve B (26), three-way valve B (26) draw forth the pipeline with ozone analysis appearance (9) are connected.
10. The microchannel continuous ozonation device according to claim 1 or 9, wherein: and a second gas mass flow controller (19) is arranged on a pipeline between the ozone analyzer (9) and the ozone destructor (10).
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114053971A (en) * | 2021-12-06 | 2022-02-18 | 上海友尹化工科技有限公司 | Continuous ozone oxidation reaction system |
| CN114195099A (en) * | 2021-12-16 | 2022-03-18 | 浙江博瑞电子科技有限公司 | Method for preparing electronic-grade hydrogen fluoride and electronic-grade hydrofluoric acid by in-situ arsenic removal of multi-channel microreactor |
| CN114307891A (en) * | 2020-09-30 | 2022-04-12 | 沈阳化工研究院有限公司 | Device for continuously preparing peroxide and continuously applying peroxide to oxidation reaction |
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| CN114195099B (en) * | 2021-12-16 | 2023-04-28 | 浙江博瑞电子科技有限公司 | Method for preparing electronic grade hydrogen fluoride and electronic grade hydrofluoric acid by in-situ arsenic removal of multichannel microreactor |
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