CN110756134A - System for efficiently producing ethylicin by utilizing microreactor - Google Patents
System for efficiently producing ethylicin by utilizing microreactor Download PDFInfo
- Publication number
- CN110756134A CN110756134A CN201911024524.3A CN201911024524A CN110756134A CN 110756134 A CN110756134 A CN 110756134A CN 201911024524 A CN201911024524 A CN 201911024524A CN 110756134 A CN110756134 A CN 110756134A
- Authority
- CN
- China
- Prior art keywords
- gas
- liquid separation
- microreactor
- storage tank
- separation device
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- OICGFSUWXCJLCO-UHFFFAOYSA-N 1-ethylsulfonylsulfanylethane Chemical compound CCSS(=O)(=O)CC OICGFSUWXCJLCO-UHFFFAOYSA-N 0.000 title claims abstract description 76
- 239000007788 liquid Substances 0.000 claims abstract description 185
- 238000000926 separation method Methods 0.000 claims abstract description 108
- 239000002994 raw material Substances 0.000 claims abstract description 71
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 238000003860 storage Methods 0.000 claims description 88
- 239000000047 product Substances 0.000 claims description 44
- 239000007789 gas Substances 0.000 claims description 41
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 38
- 229910017604 nitric acid Inorganic materials 0.000 claims description 38
- 238000011084 recovery Methods 0.000 claims description 28
- 239000002912 waste gas Substances 0.000 claims description 27
- 230000001590 oxidative effect Effects 0.000 claims description 23
- CETBSQOFQKLHHZ-UHFFFAOYSA-N Diethyl disulfide Chemical compound CCSSCC CETBSQOFQKLHHZ-UHFFFAOYSA-N 0.000 claims description 18
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 16
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 claims description 15
- MWUXSHHQAYIFBG-UHFFFAOYSA-N Nitric oxide Chemical compound O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims description 10
- 229960000583 acetic acid Drugs 0.000 claims description 8
- 239000012362 glacial acetic acid Substances 0.000 claims description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 7
- 239000001301 oxygen Substances 0.000 claims description 7
- 229910052760 oxygen Inorganic materials 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 5
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 239000012071 phase Substances 0.000 description 24
- 238000001816 cooling Methods 0.000 description 5
- 239000012263 liquid product Substances 0.000 description 5
- 239000012530 fluid Substances 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000013589 supplement Substances 0.000 description 2
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/46—Removing components of defined structure
- B01D53/54—Nitrogen compounds
- B01D53/56—Nitrogen oxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/77—Liquid phase processes
- B01D53/78—Liquid phase processes with gas-liquid contact
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/0013—Controlling the temperature of the process
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
- B01J19/002—Avoiding undesirable reactions or side-effects, e.g. avoiding explosions, or improving the yield by suppressing side-reactions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0046—Sequential or parallel reactions, e.g. for the synthesis of polypeptides or polynucleotides; Apparatus and devices for combinatorial chemistry or for making molecular arrays
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C381/00—Compounds containing carbon and sulfur and having functional groups not covered by groups C07C301/00 - C07C337/00
- C07C381/04—Thiosulfonates
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2251/00—Reactants
- B01D2251/50—Inorganic acids
- B01D2251/504—Nitric acid
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Biomedical Technology (AREA)
- Analytical Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a system for efficiently producing ethylicin by using a microreactor, which comprises an ethylicin raw material conveying pipeline, the microreactor, a gas-liquid separation device and a conveying pipeline. The system is designed aiming at the production of ethylicin, can realize high purity and high reaction yield of the produced ethylicin, solves the problem of unsafe local over-high temperature, and improves the production safety.
Description
Technical Field
The invention belongs to the field of chemical systems, and particularly relates to a system for efficiently producing ethylicin by using a microreactor.
Background
In the process of preparing ethylicin by using diethyl disulfide and nitric acid as raw materials, the excessive addition of nitric acid can cause severe oxidation, generate side reaction, reduce yield and be unsafe. Although a plurality of reactions are carried out by using microreactors in the prior art, a microreactor system aiming at the ethylicin and experience which can be used for reference are not provided, and the applicant of the invention develops a system for preparing the ethylicin by using the microreactor through long-term research. The micro-reactor system of the invention is used for preparing ethylicin, and the high efficiency, safety and environmental protection of the preparation of the ethylicin are realized.
Disclosure of Invention
The invention provides a system for preparing ethylicin by using a microreactor, which comprises an ethylicin raw material conveying pipeline, the microreactor, a gas-liquid separation device and a conveying pipeline.
Preferably, in the system for preparing ethylicin by using the microreactor, the gas-liquid separator is a gas-liquid separator or a reaction kettle with a gas-liquid separation function, the gas-liquid separator has a stirring function and/or a heat exchange function, and the reaction kettle has a stirring function and/or a heat exchange function.
Preferably, in the system for preparing ethylicin by using the microreactor, the system further comprises a waste gas recovery subsystem, and the gas-liquid separation device is connected with the waste gas recovery subsystem and used for conveying the gas generated by the gas-liquid separation device into the waste gas recovery subsystem. Preferably, a condenser is arranged between the gas-liquid separation device and the waste gas recovery subsystem.
Preferably, in the above system for preparing ethylicin by using a microreactor, the system is provided with a raw material storage tank, the raw material storage tank comprises a liquid raw material storage tank and a gas raw material storage tank, the liquid raw material storage tank comprises a nitric acid solution storage tank, a glacial acetic acid storage tank and a diethyl disulfide liquid storage tank, the gas raw material storage tank is an oxygen storage tank or an ozone storage tank, the nitric acid solution storage tank and the gas raw material storage tank are collectively referred to as oxidizing raw material storage tanks, the nitric acid solution, the oxygen and the ozone are collectively referred to as oxidizing raw materials, the oxygen and the ozone are collectively referred to as oxidizing gases, and the raw material storage tank is connected with the microreactor.
Preferably, the waste gas recovery subsystem is connected with the nitric acid solution storage tank, and when the waste gas is nitric oxide, the nitric oxide is oxidized into nitric acid solution by the waste gas recovery subsystem and then is input into the nitric acid solution storage tank to be used as the ethylicin raw material; the nitric acid solution storage tank is connected with the gas-liquid separation device, when the reaction continues in the gas-liquid separation device, the nitric acid solution can be input into the gas-liquid separation device through the nitric acid solution storage tank, and preferably, the nitric acid solution is metered through the metering pump before entering the gas-liquid separation device. The gas raw material storage tank is connected with the gas-liquid separation device, in the reaction process of the gas separation device, oxidizing gas can be input into the gas-liquid separation device through the gas raw material storage tank to promote the reaction to proceed, and the gas is metered through the metering pump before entering the gas-liquid separation device.
Preferably, in the system for preparing ethylicin by using the microreactor, the feed pipeline for the ethylicin is provided with a return stop valve.
Preferably, in the system for preparing ethylicin by using the microreactor, a pressurizing device is arranged on the ethylicin raw material conveying pipeline.
Preferably, in the system for preparing ethylicin by using the microreactor, the feed pipeline for the ethylicin is provided with a metering pump.
Preferably, in the system for preparing ethylicin by using the microreactor, a switching device is arranged on the ethylicin raw material conveying pipeline, and the switching device is an automatic switching device and is used for closing the pipeline or opening the pipeline.
Preferably, in the system for preparing ethylicin by using the microreactor, the outlet of the microreactor is provided with a temperature detection device and a pressure detection device for detecting the temperature and the pressure in the microreactor, when the outlet temperature and the outlet pressure are too high, the closing function of a switching device entering a pipeline of the microreactor can be started, and when the temperature or the pressure meets the specified requirements, the pipeline is opened through the switching device.
Preferably, in the system for preparing ethylicin by using the microreactor, the ethylicin raw material conveying pipelines comprise 1 to 3 liquid conveying pipelines which are respectively input into the microreactor.
Preferably, in the system for preparing ethylicin by using the microreactor, the ethylicin raw material conveying pipelines comprise 1-3 liquid conveying pipelines and 1-2 gas conveying pipelines.
Preferably, in the above system for preparing ethylicin by using the microreactor, the ethylicin raw material is a liquid raw material and/or a gas raw material, wherein the gas raw material is oxygen or ozone, and the liquid raw material is a diethyl disulfide solution, a nitric acid solution and glacial acetic acid.
Preferably, in the system for preparing ethylicin by using the microreactor, the gas-liquid separation device has a heat exchange function and a mixing and stirring function.
Preferably, in the system for preparing ethylicin by using the microreactor, the system is further provided with a heat exchanger, the heat exchanger is arranged between the microreactor and the gas-liquid separation device, and a product of the microreactor is input into the heat exchanger through a conveying pipeline and then is input into the gas-liquid separation device through the conveying pipeline.
Preferably, in the system for preparing ethylicin by using the microreactor, the system is further provided with a liquid separation tank, liquid separated by the gas-liquid separation device enters the liquid separation tank through a conveying pipeline to separate an oil phase and a water phase, and the oil phase is the ethylicin product.
Preferably, in the system for preparing ethylicin by using the microreactor, the system is provided with a tubular reactor, and the tubular reactor is connected with the microreactor. Preferably, a heat exchanger is arranged between the micro-reactor and the tubular reactor, a reaction product output by the micro-reactor enters the heat exchanger and then is input into the tubular reactor or is respectively input into a plurality of tubular reactors, one or a plurality of tubular reactors are connected with a gas-liquid separation device, the product is input into the gas-liquid separation device, liquid generated in the gas-liquid separation device enters a liquid separation tank, and an oil phase layer is obtained and is the ethylicin product.
Preferably, in the system for preparing ethylicin by using the microreactors, the system is provided with one microreactor, a circulating reaction is carried out through one microreactor, oxidizing raw materials are added to the microreactors in each circulating reaction, or a plurality of microreactors are arranged, the plurality of microreactors are connected in series, in parallel or in series and in parallel for mixed connection, the ethylicin raw materials or the stage microreactor products enter a gas-liquid separation device for gas-liquid separation after passing through the microreactors, the oxidizing raw materials are added in each microreactor reaction, the microreactor products in the last stage are input into the gas-liquid separation device for gas-liquid separation, and liquid generated in the gas-liquid separation device enters a liquid separation tank to obtain an oil phase layer which is the ethylicin product.
Preferably, in the system for preparing ethylicin by using the microreactors, the system is provided with a plurality of microreactors, the plurality of microreactors are connected in parallel, the plurality of microreactors are respectively connected with the storage tank, and the plurality of microreactors are respectively connected with the gas-liquid separation device.
The method comprises the steps of respectively connecting a plurality of microreactors with a storage tank, respectively obtaining reaction raw materials from the storage tank by each microreactor, then carrying out reaction in the microreactors, respectively connecting each microreactor with a gas-liquid separation device, respectively enabling products obtained by reaction of each microreactor to enter the gas-liquid separation device, wherein ① the products of the plurality of microreactors enter the same gas-liquid separation device, then inputting liquid obtained by the gas-liquid separation device into a liquid separation tank, wherein an oil phase layer obtained by layering of the liquid separation tank is an ethylicin product, ② the products of the plurality of microreactors enter the plurality of gas-liquid separation devices, liquid obtained by the plurality of gas-liquid separation devices respectively enters the liquid separation tank, and an oil phase layer obtained by layering of the liquid separation tank is the ethyli.
Preferably, in the system for preparing ethylicin by using the microreactors, the system is provided with a plurality of microreactors, the plurality of microreactors are connected in series, a gas-liquid separation device is arranged between every two adjacent microreactors, each microreactor is connected with an oxidizing raw material storage tank, and the oxidizing raw material storage tank is a nitric acid solution storage tank or a gas raw material storage tank.
The series-connected microreactors have a sequence, the first microreactor is connected with a storage tank, raw materials are obtained from the storage tank, a product after the reaction is finished is input into a gas-liquid separation device, liquid obtained by the separation of the gas-liquid separation device is input into the second microreactor, but the second microreactor needs to be supplemented with oxidizing raw materials, so the second microreactor is also connected with the oxidizing raw material storage tank, the product after the reaction is finished is input into the gas-liquid separation device again, liquid obtained by the separation of the gas-liquid separation device is input into the third microreactor, and the circulation is carried out in such a way, so each microreactor is connected with the oxidizing raw material storage tank, namely connected with a nitric acid solution storage tank or a. In the case of series connection, the number of microreactors is 3 to 12. And inputting the product of the last microreactor into a gas-liquid separation device, allowing the obtained liquid to enter a liquid separation tank, and layering to obtain an oil phase, namely the ethylicin product.
Preferably, in the system for preparing ethylicin by using the microreactors, the system is provided with a plurality of microreactors, the plurality of microreactors are connected in series and in parallel for mixing, a gas-liquid separation device is arranged between the microreactors connected in series, a product of the last microreactor connected in series is input into the gas-liquid separation device, liquid generated by the gas-liquid separation device is input into the plurality of microreactors, the products of the plurality of microreactors are input into one or more gas-liquid separation devices, liquid generated by the gas-liquid separation device enters a liquid separation tank, an oil phase obtained by layering is an ethylicin product, and the plurality of microreactors are connected with an oxidizing raw material storage tank respectively to supplement oxidizing raw materials.
Namely, after the product of the first micro-reactor is input into the gas-liquid separation device, the product of the gas-liquid separation device sequentially passes through 0-5 micro-reactors and 0-5 gas-liquid separation devices for series reaction, the product of the last micro-reactor connected in series is input into the gas-liquid separation device, the generated liquid is input into a plurality of micro-reactors respectively, the micro-reactors are respectively connected with an oxidizing raw material storage tank to supplement oxidizing raw materials, the products of the micro-reactors are input into one or more gas-liquid separation devices, the liquid product in the one or more gas-liquid separation devices is input into a liquid separation tank, and the oil phase obtained by layering is the ethylicin product.
Preferably, in the system for preparing ethylicin by using the microreactor, the system is provided with the microreactor, a product of the microreactor is input into the gas-liquid separation device, liquid generated by the gas-liquid separation device is respectively input into the microreactor, the oxidizing raw materials are added while the liquid is input into the microreactor again, the reaction product is input into the microreactor again after the liquid is input into the microreactor again for reaction, the circulation is performed in such a way, the reaction raw materials enter the microreactor for reaction for the first time, the total circulation is 1-12 times, the oxidizing raw materials are added when the liquid in the gas-liquid separation device enters the microreactor again each time, after the last circulation reaction, the product of the microreactor is input into the gas-liquid separation device, the liquid generated by the gas-liquid separation device enters the liquid separation tank.
The invention also provides the application of the system, which is characterized in that the system is applied to produce ethylicin safely, efficiently and environmentally.
The invention has the advantages of
1. The system is designed aiming at the production of ethylicin, and can realize high purity and high reaction yield of the ethylicin.
2. The ethylicin production system is simple in configuration, solves the problem of high local temperature and insecurity, and improves the production safety.
3. The system realizes the recovery and the reutilization of the waste gas, and mainly realizes the recovery and the reutilization of the nitric oxide in the waste gas under the condition of adopting nitric acid as an oxidizing substance.
Detailed Description
Example 1
A system for producing ethylicin is provided with a nitric acid storage tank, a diethyl disulfide storage tank and a glacial acetic acid storage tank, wherein the storage tank is connected with a microreactor through a conveying pipeline, a return stop valve, a pressurizing device, a switching device and a meter are arranged on the conveying pipeline, raw materials are input into the microreactor, the microreactor is provided with a cooling device, the microreactor is connected with a gas-liquid separator, a product outlet of the microreactor is provided with a pressure and temperature measuring device, the gas-liquid separator has a stirring function and a temperature adjusting function, reaction products are continuously stirred and react in the gas-liquid separator for 2 hours, the temperature of the gas-liquid separator is maintained at about 80 ℃, gas generated in the gas-liquid separator is connected with a condenser through a conveying pipeline, the condenser is connected with a waste gas recovery subsystem, gas of the condenser is input, the waste gas recovery subsystem is connected with a nitric acid storage tank, nitric acid generated by oxidation of the waste recovery subsystem is input into the nitric acid storage tank, the gas-liquid separator is connected with a liquid separation tank, liquid generated in the gas-liquid separator enters the liquid separation tank, the liquid separation tank separates an oil phase and a water phase, and the oil phase is an ethylicin product.
The pressure and temperature measuring device arranged at the outlet of the micro-reactor is connected with the control device, the control device is connected with the switching device, when the pressure and the temperature of the micro-reactor are overhigh, the control device controls the switching device to close the raw material input, and when the pressure and the temperature are in a control range, the control device controls the switching device to open the raw material input.
The microreactors of the following examples 2 to 5 were each provided with pressure and temperature measuring means, and the starting and stopping of the feed input were controlled by control means.
The gas-liquid separator in the following embodiments 2 to 5 has a stirring function and a temperature adjusting function, the gas generated in the gas-liquid separator is connected to a condenser through a transmission pipeline, the condenser is connected to a waste gas recovery subsystem, the gas of the condenser is input to the waste gas recovery subsystem, the liquid generated by the condensation of the condenser is input to the gas-liquid separator, and the waste gas recovery subsystem is connected to a storage tank.
Example 2
The utility model provides a system for production ethylicin, the system is provided with nitric acid storage tank, diethyl disulfide storage tank, the glacial acetic acid storage tank, the storage tank passes through conveying line and connects the microreactor, be provided with on the conveying line and end valve, pressure device, switching device and counter, input raw materials in to the microreactor, the microreactor is provided with cooling device, the export sets up pressure and temperature measuring device, the microreactor connects the tubular reactor, the tubular reactor connects gas-liquid separator, the gas that produces in the gas-liquid separator passes through condenser input waste gas recovery subsystem, gas-liquid separator connects the branch fluid reservoir, the liquid that produces in the gas-liquid separator gets into the branch fluid reservoir, divide the fluid reservoir to separate oil phase and aqueous phase, the oil phase is the.
Example 3
A system for producing ethylicin is provided with a nitric acid storage tank, a diethyl disulfide storage tank and a glacial acetic acid storage tank, wherein the storage tank is connected with a micro reactor through a conveying pipeline, a return stop valve, a pressurizing device, a switching device and a meter are arranged on the conveying pipeline, raw materials are input into the micro reactors, the micro reactors are provided with a cooling device and are connected with a gas-liquid separator, gas generated in the gas-liquid separator is connected with a waste gas recovery subsystem through a conveying pipeline, the gas-liquid separator is connected with a plurality of micro reactors again to respectively convey liquid products to the micro reactors, meanwhile, the micro reactors (12) are connected with the nitric acid storage tank, nitric acid is input into the micro reactors through the nitric acid storage tank, the products of the micro reactors are input into the gas-liquid separator again, gas generated in the gas-liquid separator enters, separating oil phase and water phase in the separating tank, wherein the oil phase is ethylicin product.
Example 4
A system for producing ethylicin is provided with an ozone storage tank, a diethyl disulfide storage tank and a glacial acetic acid storage tank, wherein the storage tank is connected with a microreactor through a conveying pipeline, a return stop valve, a pressurizing device, a switching device and a meter are arranged on the conveying pipeline, raw materials are input into the microreactor, the microreactor is provided with a cooling device and is connected with a gas-liquid separator, gas generated in the gas-liquid separator is connected with a condenser through a conveying pipeline, liquid generated by the condenser is input into a gas-liquid separator, gas generated by the condenser is input into the ozone storage tank through a compressor, the gas-liquid separator is connected with a 2 nd microreactor, liquid products are conveyed into the microreactor, the microreactor is connected with the ozone storage tank, ozone is input into the microreactor through the ozone storage tank, the products of the microreactor are input into the gas-, the produced liquid enters a 3 rd micro reactor, a liquid product is conveyed to the micro reactor, meanwhile, the micro reactor is connected with an ozone storage tank, ozone is input into the micro reactor through the ozone storage tank, the product of the micro reactor is input into a gas-liquid separator again, gas produced in the gas-liquid separator enters an exhaust gas recovery subsystem, the produced liquid enters a 4 th micro reactor, the circulation is carried out in the way, the product entering the 10 th micro reactor enters the gas-liquid separator, the gas produced in the gas-liquid separator enters the exhaust gas recovery subsystem, the produced liquid enters a liquid separation tank, the liquid separation tank separates an oil phase and a water phase, and the oil phase is an ethylicin product.
Example 5
A system for producing ethylicin is provided with a nitric acid storage tank, a diethyl disulfide storage tank and a glacial acetic acid storage tank, wherein the storage tank is connected with a microreactor through a conveying pipeline, a return stop valve, a pressurizing device, a switching device and a meter are arranged on the conveying pipeline, raw materials are input into the microreactor, the microreactor is provided with a cooling device, the microreactor is connected with a gas-liquid separator, gas generated in the gas-liquid separator is connected with a waste gas recovery subsystem through a conveying pipeline, the gas-liquid separator is connected with the microreactor and used for conveying liquid products to the microreactor, nitric acid is input into the microreactor through the nitric acid storage tank, the products of the microreactor are input into the gas-liquid separator again, gas generated in the gas-liquid separator enters the waste gas recovery subsystem, the generated liquid enters the same microreactor, and (3) inputting the product of the microreactor into the gas-liquid separator again, enabling gas generated in the gas-liquid separator to enter a waste gas recovery subsystem, enabling generated liquid to enter the same microreactor, circulating in the same way until the 5 th cycle, enabling the product of the microreactor to enter the gas-liquid separator, enabling gas generated in the gas-liquid separator to enter the waste gas recovery subsystem, enabling the generated liquid to enter a liquid separation tank, and separating an oil phase and a water phase in the liquid separation tank, wherein the oil phase is an ethylicin product.
Claims (11)
1. A system for preparing ethylicin by using a microreactor comprises a ethylicin raw material conveying pipeline, the microreactor, a gas-liquid separation device and a transmission pipeline, and is characterized in that the ethylicin raw material conveying pipeline is connected with the microreactor and used for conveying the ethylicin raw material into the microreactor, the microreactor is connected with the gas-liquid separation device, a reaction product output by the microreactor is input into the gas-liquid separation device through the transmission pipeline, and liquid generated by the gas-liquid separation device is input into the microreactor again.
2. The system according to claim 1, wherein the gas-liquid separation device is a gas-liquid separator or a reaction kettle with a gas-liquid separation function, the gas-liquid separator has a stirring function and/or a heat exchange function, and the reaction kettle has a stirring function and/or a heat exchange function.
3. The system of claim 1, wherein the system for preparing ethylicin by using the microreactor further comprises a waste gas recovery subsystem, the gas-liquid separation device is connected with the waste gas recovery subsystem, and the gas generated by the gas-liquid separation device is delivered into the waste gas recovery subsystem; preferably, a condenser is arranged between the gas-liquid separation device and the waste gas recovery subsystem.
4. The system according to claim 3, wherein the system is provided with a raw material storage tank, the raw material storage tank comprises a liquid raw material storage tank and a gas raw material storage tank, the liquid raw material storage tank comprises a nitric acid solution storage tank, a glacial acetic acid storage tank and a diethyl disulfide liquid storage tank, the gas raw material storage tank is an oxygen storage tank or an ozone storage tank, the nitric acid solution storage tank and the gas raw material storage tank are collectively called oxidizing raw material storage tanks, the nitric acid solution, the oxygen and the ozone are collectively called oxidizing raw materials, the oxygen and the ozone are collectively called oxidizing gases, the raw material storage tank is connected with a micro-reactor, and/or the raw material storage tank is.
5. The system according to claim 4, wherein the waste gas recovery subsystem is connected with the nitric acid solution storage tank, and when the waste gas is nitric oxide, the nitric oxide is oxidized into the nitric acid solution by the waste gas recovery subsystem and then is input into the nitric acid solution storage tank to be used as the ethylicin raw material; the nitric acid solution storage tank is connected with the gas-liquid separation device, when the reaction continues in the gas-liquid separation device, the nitric acid solution can be input into the gas-liquid separation device through the nitric acid solution storage tank, and preferably, the nitric acid solution is metered through the metering pump before entering the gas-liquid separation device; the gas raw material storage tank is connected with the gas-liquid separation device, in the reaction process of the gas separation device, oxidizing gas can be input into the gas-liquid separation device through the gas raw material storage tank to promote the reaction to proceed, and the gas is metered through the metering pump before entering the gas-liquid separation device.
6. The system of claim 5, wherein the ethylicin raw material conveying pipeline is provided with a check valve, a pressurizing device, a metering pump and a switching device.
7. The system of claim 6, wherein the microreactor outlet is provided with temperature and pressure sensing means for sensing temperature and pressure in the microreactor, wherein the shut-off function of the switching means of the conduit leading into the microreactor can be activated in case of excessive outlet temperature and pressure, and wherein the conduit is opened by the switching means in case of a specified temperature or pressure.
8. The system according to claim 7, wherein a heat exchanger is provided between the microreactor and the gas-liquid separation apparatus, and the product of the microreactor is fed to the heat exchanger through the transfer line and then fed to the gas-liquid separation apparatus through the transfer line.
9. The system of claim 8, wherein the system is further provided with a liquid separation tank, and the liquid separated by the gas-liquid separation device enters the liquid separation tank through a conveying pipeline to separate an oil phase and a water phase, wherein the oil phase is the ethylicin product.
10. The system according to claim 1, wherein in the system for preparing ethylicin by using the microreactor, the system is provided with a tubular reactor, and the tubular reactor is connected with the microreactor; preferably, a heat exchanger is arranged between the micro-reactor and the tubular reactor, a reaction product output by the micro-reactor enters the heat exchanger and then is input into the tubular reactor or is respectively input into a plurality of tubular reactors, one or a plurality of tubular reactors are connected with a gas-liquid separation device, the product is input into the gas-liquid separation device, liquid generated in the gas-liquid separation device enters a liquid separation tank, and an oil phase layer is an ethylicin product.
11. The system according to claim 1, wherein the system for preparing ethylicin by using the microreactors is provided with one microreactor, a circulation reaction is performed by one microreactor, oxidizing raw materials are added to the microreactors in each circulation, or a plurality of microreactors are provided, the plurality of microreactors are connected in series, in parallel or in series and in parallel and in mixed connection, the ethylicin raw materials or the microreactor products in the intermediate stage are input to the gas-liquid separation device for gas-liquid separation after passing through the microreactors, the oxidizing raw materials are added in each reaction of the microreactors, the microreactor products in the last stage are input to the gas-liquid separation device for gas-liquid separation, and liquid generated in the gas-liquid separation device enters the liquid separation tank to obtain the ethylicin product as an oil phase layer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911024524.3A CN110756134B (en) | 2019-10-25 | 2019-10-25 | System for efficiently producing ethylicin by utilizing microreactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201911024524.3A CN110756134B (en) | 2019-10-25 | 2019-10-25 | System for efficiently producing ethylicin by utilizing microreactor |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN110756134A true CN110756134A (en) | 2020-02-07 |
| CN110756134B CN110756134B (en) | 2021-11-05 |
Family
ID=69333741
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201911024524.3A Active CN110756134B (en) | 2019-10-25 | 2019-10-25 | System for efficiently producing ethylicin by utilizing microreactor |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110756134B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114790157A (en) * | 2022-02-28 | 2022-07-26 | 开封大地农化生物科技有限公司 | Method for synthesizing high-content ethylicin |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006257001A (en) * | 2005-03-16 | 2006-09-28 | Mitsubishi Chemicals Corp | Gas-liquid reaction method |
| CN104511264A (en) * | 2015-01-26 | 2015-04-15 | 深圳市一正科技有限公司 | Micro-channel reaction system |
| CN108794307A (en) * | 2018-07-18 | 2018-11-13 | 山东道可化学有限公司 | A kind of micro- reaction system and method for the solvent method synthesis bromo- 3- methylanisoles of 4- |
| CN109467508A (en) * | 2018-11-22 | 2019-03-15 | 四川金象赛瑞化工股份有限公司 | A kind of method of micro passage reaction synthesizing dinitrotoluene |
-
2019
- 2019-10-25 CN CN201911024524.3A patent/CN110756134B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006257001A (en) * | 2005-03-16 | 2006-09-28 | Mitsubishi Chemicals Corp | Gas-liquid reaction method |
| CN104511264A (en) * | 2015-01-26 | 2015-04-15 | 深圳市一正科技有限公司 | Micro-channel reaction system |
| CN108794307A (en) * | 2018-07-18 | 2018-11-13 | 山东道可化学有限公司 | A kind of micro- reaction system and method for the solvent method synthesis bromo- 3- methylanisoles of 4- |
| CN109467508A (en) * | 2018-11-22 | 2019-03-15 | 四川金象赛瑞化工股份有限公司 | A kind of method of micro passage reaction synthesizing dinitrotoluene |
Non-Patent Citations (2)
| Title |
|---|
| 俞金寿: "《化工自动化及仪表》", 28 February 2011, 华东理工大学出版社 * |
| 朱永和: "《农药大典》", 31 October 2006, 中国三峡出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114790157A (en) * | 2022-02-28 | 2022-07-26 | 开封大地农化生物科技有限公司 | Method for synthesizing high-content ethylicin |
Also Published As
| Publication number | Publication date |
|---|---|
| CN110756134B (en) | 2021-11-05 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110756134B (en) | System for efficiently producing ethylicin by utilizing microreactor | |
| CN106517348B (en) | Potassium manganate continuous automatic production process | |
| CN103911194A (en) | Composite type diesel fuel cetane number improver and production process thereof | |
| CN104907008A (en) | Reaction device and method for preparing benzoic acid and benzaldehyde through direct oxidation of methylbenzene | |
| CN113429264B (en) | Continuous production method of 3-chloro-2-methylphenol and device for production thereof | |
| CN106478430B (en) | A kind of triethanolamine continuous production device and technique | |
| CN108479653B (en) | Integral microchannels reaction unit and the method for preparing two-(2- chloroethyl) di-phosphate esters using the device | |
| CN104447362B (en) | Autoclave continuously hydrogen adding prepares the reaction system and method for para-aminophenol | |
| CN102875342B (en) | Continuous flow method for preparing benzaldehyde from benzyl dichloride through hydrolysis | |
| CN103864626A (en) | Device and process for producing 4-aminodiphenylamine by catalytic hydrogenation | |
| CN212142558U (en) | Continuous production system | |
| CN109180461A (en) | A kind of method that micro-reacting tcchnology prepares butyric acid | |
| CN111359560B (en) | Micro-reaction system for synthesizing trans-2-hexenal | |
| CN109776330B (en) | Method for preparing 1,2, 4-butanetriol trinitrate by using microchannel reactor | |
| CN203568999U (en) | Reaction separation system and device for preparing polyoxymethylene dimethyl ethers | |
| CN209109181U (en) | Diazinon cyclization reaction device | |
| CN203558989U (en) | Extraction system for polyoxymethylene dimethyl ether preparation device | |
| CN105218492A (en) | Supergravity reactor is utilized to produce device and the production method of furfuryl alcohol | |
| CN216678191U (en) | Quick alkali washing system for industrial device | |
| CN210543427U (en) | Hot water circulating device for vinyl chloride production | |
| CN221222999U (en) | Heptane heating device for PVC mixed dewatering device | |
| CN215138442U (en) | Membrane separation device for isomeride alkane gas | |
| CN217120288U (en) | Continuous preparation production system for acyl chloride products | |
| CN217856060U (en) | Dicyclopentadiene hydrogenation process reaction device | |
| CN205295195U (en) | Utilize device of super -gravity reactor production furfuryl alcohol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right | ||
| PE01 | Entry into force of the registration of the contract for pledge of patent right |
Denomination of invention: A system for efficient production of ethyl allicin using microreactors Effective date of registration: 20231020 Granted publication date: 20211105 Pledgee: Industrial Bank Co.,Ltd. Haikou Branch Pledgor: HAINAN ZHENGYE ZHONGNONG HIGH TECHNOLOGY Co.,Ltd. Registration number: Y2023980062064 |
|
| CP03 | Change of name, title or address | ||
| CP03 | Change of name, title or address |
Address after: Fuchang Village, Laocheng Development Zone, Chengmai County, Hainan Province, 571923 Patentee after: Hainan Zhengye Biotechnology Co.,Ltd. Address before: 571924 Fuchang village, Laocheng Development Zone, Chengmai County, Hainan Province Patentee before: HAINAN ZHENGYE ZHONGNONG HIGH TECHNOLOGY Co.,Ltd. |