CN219232302U - Ozonization reaction device - Google Patents
Ozonization reaction device Download PDFInfo
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- CN219232302U CN219232302U CN202220166288.XU CN202220166288U CN219232302U CN 219232302 U CN219232302 U CN 219232302U CN 202220166288 U CN202220166288 U CN 202220166288U CN 219232302 U CN219232302 U CN 219232302U
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Abstract
The utility model discloses an ozonization reaction device, which has a circulation loop structure, and comprises the following components in sequence: a reactor, a circulating assembly, a buffer separation tank, a heat exchanger, a product outlet, a raw material inlet and the like. The ozonization reaction device of the utility model aims at the ozonization reaction process with high activity and high heat release, and effectively solves various problems of low-pressure ozone addition, full dispersion and heat release of the reaction by the design of an external circulation type reaction system. The device controls the ozone adding speed by adjusting the liquid phase circulation amount, thereby controlling the ozonization reaction progress and the reaction heat release speed, and finally obtaining the target product with high yield. The utility model is based on an industrial reactor, and has the advantages of simple structure, easy operation and low processing and manufacturing cost; the whole device can run continuously or intermittently, and is safe and reliable.
Description
Technical Field
The utility model relates to the technical field of multiphase oxidation reaction, in particular to an ozonization reaction device which has high dispersity on ozone-containing gas and can be efficiently and controllably removed in time.
Background
Ozone acts as a strong oxidizing agent and organic substances that can be oxidized include olefins, amines, carbocycles, aromatic compounds, and the like. Compared with other oxidants, ozone has the advantages of strong oxidizing ability, high reaction speed and the like; after the reaction is finished, ozone is automatically decomposed, no residue exists, and no pollution is caused to the environment. Therefore, the ozone is widely applied to the fields of wastewater treatment, disinfection, chemical synthesis and the like.
Meanwhile, the high potential of ozone also leads to the characteristics of high heat release and easy explosion of the ozonization reaction. In the traditional bubbling stirring kettle, the low ozone utilization rate is caused by poor gas-liquid mixing effect, unreacted ozone is aggregated, and once flammable and explosive organic solvents are encountered, explosion is easily caused; moreover, the bubbling stirring kettle has limited heat transfer efficiency, and when the ozone concentration is high and the reaction heat release is fast, the heat in the system can not be removed in time by jacket heat exchange, and the reaction operation has great danger.
CN110947348A applies a microchannel reactor to a continuous ozonation process; a tube-type ozonization continuous reaction apparatus is described in CN202516541U et al; the U.S. P2 Science company has also developed ozonation continuous tubular flow technology and has been successfully used for olefin ozonation. The holding capacity of the device in the processes is smaller, the specific heat exchange surface area is sufficient, and the safety problem of the bubbling stirring kettle is effectively solved. However, these reaction facilities have a fine and complex core structure, and the characteristic dimensions are usually in the order of millimeters, and the manufacturing requirements and the manufacturing costs are high. In addition, the pressure drop of the equipment is large, the inlet pressure is higher, the outlet pressure (about 0.3 MPa) of the main stream ozone generating equipment is not easy to match with the main stream ozone generating equipment, and special pressurizing equipment is often required to be additionally arranged.
There is a need to develop an ozonation reactor that is simpler in structure, easier to manufacture and more efficient in reaction.
Disclosure of Invention
The utility model provides a novel ozonization reaction device, which continuously circulates reaction materials out of a reactor through a circulation loop to carry out intensified heat exchange; meanwhile, the negative suction effect generated by the circulating component ensures the continuous addition of ozone; the whole device can control the ozonization reaction process by adjusting the circulation quantity.
The technical scheme of the utility model is as follows:
a novel ozonation reaction apparatus having a circulation loop structure, comprising, in order:
the reactor is used for mixing liquid-phase raw materials and ozone gas-liquid to generate ozonization reaction, the reactor is provided with a tail gas outlet for discharging tail gas through a pipeline, and an overflow outlet is arranged on the side wall of the reactor close to the top of the reactor and used for overflowing liquid-phase materials out of the reactor;
the circulating assembly is used for sucking ozone at a negative pressure and mixing the ozone with liquid-phase materials comprising fresh raw materials and circulating materials and introducing the mixture into the reactor, and comprises an ozone inlet for introducing ozone;
the buffer separation tank is connected with an overflow outlet of the reactor through a pipeline, receives liquid phase materials subjected to reaction in the reactor and performs gas-liquid phase separation, and is connected to a pipeline of the tail gas outlet of the reactor through a pipeline to discharge tail gas;
the heat exchanger is connected with the buffer separation tank through a pipeline, receives part of the reacted liquid phase material from the buffer separation tank, controls the temperature of the material through heat exchange, and is connected with the circulating assembly through a pipeline to re-convey part of the reacted liquid phase material into the reactor;
a product outlet arranged on a pipeline between the buffer separation tank and the heat exchanger for outputting a part of liquid-phase material product;
and a raw material inlet is arranged on a pipeline between the heat exchanger and the circulating assembly and is used for supplementing liquid phase raw material.
Preferably, the reactor is externally provided with a heat exchange jacket or internally provided with heat exchange means to enhance control of the reaction temperature.
Preferably, the heat exchange member is a coil or the like.
Preferably, a catalyst bed layer is arranged in the reactor, and a solid phase catalyst is filled and fixed for catalyzing ozone catalytic reaction; an inner member for enhancing gas-liquid mixing can also be arranged.
Preferably, the inner member includes, but is not limited to, a stirrer.
Preferably, the circulation assembly includes, but is not limited to, a combination of a venturi ejector and a liquid phase pump, or a separate gas-liquid mixing pump.
Preferably, the liquid phase pump or the gas-liquid mixing pump is a continuously variable pump.
Preferably, the number of the circulating components is one or more according to the needs of the ozonization reaction, and the circulating components are installed at the bottom, the lower part or the middle part of the reactor so as to supplement ozone and liquid phase materials into the reactor.
Preferably, the ozonation reaction apparatus does not include the buffer separation tank.
Preferably, the heat exchangers include, but are not limited to, tubular heat exchangers and the like, and the number of the heat exchangers can be 1 group or multiple groups according to the reaction heat exchange requirement.
Preferably, a pressure regulating valve can be arranged on the pipeline of the tail gas outlet, and the pressure of the reaction system is controlled by regulating the tail gas discharging speed.
Advantageous effects
The ozonization reaction device of the utility model aims at the ozonization reaction process with high activity and high heat release, and effectively solves various problems of low-pressure ozone addition, full dispersion and heat release of the reaction by the design of an external circulation type reaction system. The device controls the ozone adding speed by adjusting the liquid phase circulation amount, thereby controlling the ozonization reaction progress and the reaction heat release speed, and finally obtaining the target product with high yield. The utility model is based on an industrial reactor, and has the advantages of simple structure, easy operation and low processing and manufacturing cost; the whole device can run continuously or intermittently, and is safe and reliable.
Drawings
FIG. 1 is a schematic structural view of an ozonization reaction apparatus according to the present utility model.
Reference numerals
1-reactor, 2-circulation assembly, 3-buffer separation tank, 4-heat exchanger, 5-raw material inlet, 6-ozone inlet, 7-overflow outlet, 8-tail gas outlet and 9-product outlet.
Detailed Description
Hereinafter, specific embodiments of the present utility model will be described in detail with reference to the accompanying drawings, but not limiting the utility model.
It should be understood that various modifications may be made to the embodiments disclosed herein. Therefore, the following description should not be taken as limiting, but merely as exemplification of the embodiments. Other modifications within the scope and spirit of this disclosure will occur to persons of ordinary skill in the art.
The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments of the disclosure and, together with a general description of the disclosure given above and the detailed description of the embodiments given below, serve to explain the principles of the disclosure.
These and other characteristics of the utility model will become apparent from the following description of a preferred form of embodiment, given as a non-limiting example, with reference to the accompanying drawings.
It is also to be understood that, although the utility model has been described with reference to some specific examples, a person skilled in the art will certainly be able to achieve many other equivalent forms of the utility model, having the characteristics as set forth in the claims and hence all coming within the field of protection defined thereby.
The above and other aspects, features and advantages of the present disclosure will become more apparent in light of the following detailed description when taken in conjunction with the accompanying drawings.
The specification may use the word "in one embodiment," "in another embodiment," "in yet another embodiment," or "in other embodiments," which may each refer to one or more of the same or different embodiments in accordance with the disclosure.
The structure of the ozonization reaction apparatus of the present utility model, which has a circulation loop structure, is specifically described below with reference to fig. 1, which sequentially includes:
the reactor 1 is used for mixing liquid-phase raw materials and ozone gas-liquid to generate ozonization reaction, the reactor 1 is provided with a tail gas outlet for discharging tail gas through a pipeline, and an overflow outlet is arranged on the side wall of the reactor 1 close to the top of the reactor 1 and used for overflowing liquid-phase materials out of the reactor 1;
a circulation assembly 2 for sucking ozone at a negative pressure and mixing with liquid phase materials including fresh raw materials and circulating materials and introducing the mixture into the reactor 1, wherein the circulation assembly 2 comprises an ozone inlet 6 for introducing ozone;
a buffer separation tank 3 connected to an overflow outlet 7 of the reactor 1 through a pipeline, receiving the liquid phase material reacted in the reactor 1 and performing gas-liquid phase separation, the buffer separation tank 3 being connected to a pipeline of the tail gas outlet 8 of the reactor 1 through a pipeline, and discharging tail gas;
and a heat exchanger 4 connected with the buffer separation tank 3 through a pipeline, receiving part of the reacted liquid phase material from the buffer separation tank 3, and controlling the temperature of the material through heat exchange. The heat exchanger 4 is connected with the circulating assembly 2 through a pipeline and is used for conveying part of the liquid phase material after the reaction to the reactor 1 again;
a product outlet 9, which is arranged on a pipeline between the buffer separation tank 3 and the heat exchanger 4, and is used for outputting partial liquid phase material products;
a feed inlet 5, provided in the line between the heat exchanger 4 and the circulation module 2, for feeding in liquid phase feed.
Preferably, the reactor 1 is externally provided with a heat exchange jacket or internally provided with heat exchange means to enhance control of the reaction temperature.
Preferably, the heat exchange member is a coil or the like.
Preferably, a catalyst bed layer is arranged in the reactor 1, and a solid phase catalyst is filled and fixed for catalyzing ozone catalytic reaction; an inner member for enhancing gas-liquid mixing can also be arranged.
Preferably, the inner member includes, but is not limited to, a stirrer.
Preferably, the circulation module package 2 is a transport device with negative pressure suction and sufficient dispersion for the ozone gas added, including but not limited to a venturi jet and liquid phase pump combination, or a gas-liquid mixing pump; the negative pressure generated by the circulating assembly is only required to be lower than the outlet pressure of the ozone generating device, and is not required to be lower than the atmospheric pressure. Wherein the liquid phase pump or the gas-liquid mixing pump is a stepless speed change pump.
Preferably, the number of the circulating components 2 is one or more according to the needs of the ozonization reaction, and the circulating components 2 are installed at the bottom, the lower part or the middle part of the reactor 1 so as to supplement the ozone and the liquid phase material into the reactor 1.
Preferably, the ozonation reaction apparatus does not include the buffer separation tank 3 according to the specific case of the ozonation reaction. When the ozonization reaction device does not comprise the buffer separation tank 3, the tail gas in the ozonization reaction device is directly discharged through the tail gas outlet 8, the overflow outlet is directly connected with the product outlet 9 and the heat exchanger 4, and the amount of liquid phase material flowing out of the product outlet 9 and the amount flowing into the heat exchanger 4 are regulated through valves.
Preferably, the heat exchangers 4 include, but are not limited to, tubular heat exchangers, etc., and the number of the heat exchangers can be 1 group or multiple groups according to the reaction heat exchange requirement. The temperature of the circulating material is controlled by the heat exchanger 4 and then mixed with fresh raw material and fed into the reactor by a pump in the circulating assembly.
Preferably, a pressure regulating valve can be installed on the pipeline of the tail gas outlet 8, and the pressure of the reaction system is controlled by regulating the tail gas discharging speed.
In particular, the ozonation apparatus according to the present utility model may be operated intermittently or continuously.
The specific operation of the ozonization reaction apparatus of the present utility model is described below with reference to fig. 1:
1) Closing the ozone inlet 6 of the ozonization device before reaction, opening the circulation assembly 2, and introducing fresh raw materials into the reactor from the raw material inlet 5 through the circulation assembly 2 until the reactor 1, the buffer separation tank 3, the heat exchanger 4, the circulation pipeline 2 and connecting pipelines between the raw materials are filled with enough raw materials; then closing the raw material inlet 5, circulating the material by the ozonization device, and opening the heat exchanger 4 until the material reaches a preset temperature;
2) After the operation of the step 1) is stable, opening the ozone inlet 6, continuously adding ozone, and carrying out ozonization reaction in the reactor 1;
3) Adjusting the circulation flow of the ozonization device, and controlling the adding speed of ozone; simultaneously adjusting a pressure regulating valve on a pipeline of the tail gas outlet 8 to control the pressure of the ozonization device; monitoring the reaction temperature, and adjusting the heat exchanger 4 to control the temperature of the reaction materials;
4) After monitoring the reaction, collecting the product from the product outlet 9;
5) If the reaction needs to run continuously, after the reaction state of the step 3) is basically stable, slowly opening the raw material inlet 5, controlling the raw material adding speed, monitoring the reaction condition, and slowly opening the product outlet 9; under the condition that the output product meets the requirement, the raw material adding speed, the product outflow speed, the circulating flow and the like are adjusted and controlled, and the reaction process is gradually optimized.
Example 1
1) Closing an ozone inlet 6 of the ozonization device before reaction, opening a liquid phase pump in the circulating assembly 2, and in the embodiment, the circulating assembly 2 adopts a combination of a venturi ejector and the liquid phase pump, and after raw materials cyclohexene, solvent methanol and methylene dichloride are mixed, pumping the raw materials into the reactor 1 through the circulating assembly 2 liquid phase pump from the raw material inlet 5 until the reactor 1, a buffer separation tank 3, a heat exchanger 4, a circulating pipeline 2 and connecting pipelines among the raw materials are filled with enough raw materials, and 1000g cyclohexene, 5000g methanol and 4000g methylene dichloride are filled in total; then closing the raw material inlet 5, circulating the material by the whole ozonization device, and starting the heat exchanger 4 until the temperature of the material is reduced to about-10 ℃;
2) After the operation of the step 1) is stable, an ozone inlet 6 of the ozonization device is opened, ozone is continuously added into the reactor 1 to carry out ozonization reaction, and the specification of an ozone generator is 100g/h;
3) Adjusting the circulation flow to control the ozone adding speed; simultaneously adjusting a pressure regulating valve on a pipeline of the tail gas outlet 8, and controlling the pressure of the ozonization device to be not more than 0.3MPa; the heat exchanger 4 is regulated to control the temperature of the reaction materials to be 10-20 ℃;
4) After about 7 hours, the reaction is completed, crude products are collected from the product outlet 9, then the solvent is distilled off under reduced pressure, and formic acid and hydrogen peroxide are added for reaction, and 1708g of adipic acid product is finally obtained.
Compared with the kettle type reaction process, the ozonization device can effectively control the reaction heat release, and the reaction temperature is increased from 0 ℃ to 20 ℃, the reaction time is reduced from 10 hours to about 7 hours, and the yield of the final product adipic acid is increased from 92% to about 96%, so that the ozonization device improves the ozone utilization efficiency, and safely and effectively controls the ozonization reaction process.
The above embodiments are only exemplary embodiments of the present utility model and are not intended to limit the present utility model, the scope of which is defined by the claims. Various modifications and equivalent arrangements of this utility model will occur to those skilled in the art, and are intended to be within the spirit and scope of the utility model.
Claims (10)
1. An ozonation reaction apparatus having a circulation loop structure, comprising, in order:
the reactor is used for mixing liquid-phase raw materials and ozone gas-liquid to generate ozonization reaction, the reactor is provided with a tail gas outlet for discharging tail gas through a pipeline, and an overflow outlet is arranged on the side wall of the reactor close to the top of the reactor and used for overflowing liquid-phase materials out of the reactor;
the circulating assembly is used for sucking ozone at a negative pressure and mixing the ozone with liquid-phase materials comprising fresh raw materials and circulating materials and introducing the mixture into the reactor, and comprises an ozone inlet for introducing ozone;
the buffer separation tank is connected with an overflow outlet of the reactor through a pipeline, receives liquid phase materials subjected to reaction in the reactor and performs gas-liquid phase separation, and is connected to a pipeline of the tail gas outlet of the reactor through a pipeline to discharge tail gas;
the heat exchanger is connected with the buffer separation tank through a pipeline, receives part of the reacted liquid phase material from the buffer separation tank, controls the temperature of the material through heat exchange, and is connected with the circulating assembly through a pipeline to re-convey part of the reacted liquid phase material into the reactor;
a product outlet arranged on a pipeline between the buffer separation tank and the heat exchanger for outputting a part of liquid-phase material product;
and a raw material inlet is arranged on a pipeline between the heat exchanger and the circulating assembly and is used for supplementing liquid phase raw material.
2. The ozonation reaction apparatus of claim 1, wherein the reactor is externally provided with a heat exchange jacket or internally provided with heat exchange means to enhance control of reaction temperature.
3. The ozonation reaction apparatus of claim 2, wherein the heat exchange member is a coil.
4. The ozonization reaction apparatus according to claim 1, wherein a catalyst bed layer is provided inside the reactor, filled with a solid phase catalyst and fixed for catalyzing an ozone catalytic reaction; or an inner member for enhancing gas-liquid mixing is provided, wherein the inner member comprises a stirrer.
5. The ozonation reaction apparatus of claim 1, wherein the circulation assembly comprises a combination of a venturi jet and a liquid phase pump, or is a separate gas-liquid mixing pump.
6. The ozonation reaction apparatus of claim 5, wherein the liquid phase pump or the gas-liquid mixing pump is a continuously variable pump.
7. The ozonation reaction apparatus of claim 1, wherein the number of circulation assemblies is one or more, and the circulation assemblies are installed at a bottom, a lower portion, or a middle portion of the reactor so as to supplement the reactor with ozone and liquid phase materials.
8. The ozonation reaction apparatus of claim 1, wherein the ozonation reaction apparatus does not comprise the buffer separation tank.
9. The ozonation reaction apparatus of claim 1, wherein the heat exchanger comprises a tube array heat exchanger, the number of heat exchangers being 1 or more groups.
10. The ozonization reaction apparatus according to claim 1, wherein a pressure regulating valve is installed on the line of the off-gas outlet, and the pressure of the reaction system is controlled by regulating the off-gas discharge rate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220166288.XU CN219232302U (en) | 2022-01-21 | 2022-01-21 | Ozonization reaction device |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220166288.XU CN219232302U (en) | 2022-01-21 | 2022-01-21 | Ozonization reaction device |
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| CN219232302U true CN219232302U (en) | 2023-06-23 |
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| CN202220166288.XU Active CN219232302U (en) | 2022-01-21 | 2022-01-21 | Ozonization reaction device |
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