CN111760544B - Continuous plug flow swirling flow reaction device - Google Patents
Continuous plug flow swirling flow reaction device Download PDFInfo
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- CN111760544B CN111760544B CN202010639648.9A CN202010639648A CN111760544B CN 111760544 B CN111760544 B CN 111760544B CN 202010639648 A CN202010639648 A CN 202010639648A CN 111760544 B CN111760544 B CN 111760544B
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- 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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2415—Tubular reactors
- B01J19/242—Tubular reactors in series
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- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J19/0006—Controlling or regulating processes
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- 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
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- 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
- B01J19/0053—Details of the reactor
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- 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
- B01J19/0053—Details of the reactor
- B01J19/006—Baffles
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- 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
- B01J19/24—Stationary reactors without moving elements inside
- B01J19/2405—Stationary reactors without moving elements inside provoking a turbulent flow of the reactants, such as in cyclones, or having a high Reynolds-number
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/16—Halides of ammonium
- C01C1/162—Ammonium fluoride
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/14—Purification
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D5/00—Sulfates or sulfites of sodium, potassium or alkali metals in general
- C01D5/16—Purification
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00076—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements inside the reactor
- B01J2219/00081—Tubes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/00074—Controlling the temperature by indirect heating or cooling employing heat exchange fluids
- B01J2219/00087—Controlling the temperature by indirect heating or cooling employing heat exchange fluids with heat exchange elements outside the reactor
- B01J2219/00092—Tubes
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- 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
- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00051—Controlling the temperature
- B01J2219/0015—Controlling the temperature by thermal insulation means
- B01J2219/00155—Controlling the temperature by thermal insulation means using insulating materials or refractories
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
- B01J2219/00049—Controlling or regulating processes
- B01J2219/00164—Controlling or regulating processes controlling the flow
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a continuous plug flow swirling flow reaction device, a nitration reaction device, an ammonium fluoride production device and a sodium sulfate and sodium chloride separation system. The continuous plug flow swirling flow reaction device of the invention comprises: the input end of the reaction module is used for inputting materials, and the output end of the reaction module is used for outputting a product after reaction; the piston device is connected in parallel with the reaction module, one end of the piston device is communicated with the input end of the reaction module, and the other end of the piston device is communicated with the output end of the piston device and is used for providing push-pull power for the piston to enable the materials to flow and fully mix and react; and the heat exchange module is arranged in the reaction module and used for adjusting the reaction temperature in the reaction module. The invention has compact volume, greatly saves the occupied area, and is simple, reliable and easy to maintain; meanwhile, the process time is greatly shortened, the efficiency is higher, and the control is easy.
Description
Technical Field
The invention relates to the technical fields of material heat exchange, mixing, reaction synthesis and crystallization, in particular to a continuous plug flow swirling flow reaction device, a nitration reaction device, an ammonium fluoride production device and a sodium sulfate and sodium chloride separation system.
Background
At present, the main equipment for mixing, reacting and crystallizing traditional materials is a reaction kettle, and the purposes of material mixing, reacting and crystallizing are achieved by stirring the reaction kettle and heating or cooling a jacket of the reaction kettle. In practice, the flowing state of materials in the traditional reaction kettle is a laminar flow state, mass transfer is very uneven, and a heating or cooling temperature curve cannot be accurately controlled.
The reaction kettle used for mixing, reacting and crystallizing the traditional materials has the following defects:
1. the materials can only be batched and processed, and continuous metering production can not be realized.
2. The mass transfer of the materials in the reaction kettle is poor, and the treatment rate is low.
3. Aiming at the reaction synthesis of high-temperature, high-pressure and dangerous materials, the equipment cost of the reaction kettle is high, and the operation environment is dangerous.
4. Aiming at the mixed reaction of multiple materials including gas phase, solid phase and the like, a special stirring and homogenizing mechanism is required to be arranged on a reaction kettle, so that the equipment of a basic reaction unit is complicated.
5. The product process line is matched with more reaction kettles, so that a material production process system is complicated and has large occupied space, and a special in-place cleaning system is required to be configured, so that the investment of production equipment, the operation cost and the labor cost are high.
Disclosure of Invention
According to an embodiment of the present invention, there is provided a continuous plug flow swirling flow reaction apparatus including:
the input end of the reaction module is used for inputting materials, and the output end of the reaction module is used for outputting a product after reaction;
the piston device is connected in parallel with the reaction module, one end of the piston device is communicated with the input end of the reaction module, and the other end of the piston device is communicated with the output end of the piston device and is used for providing push-pull power for the piston to enable the materials to flow and fully mix and react;
and the heat exchange module is arranged in the reaction module and used for adjusting the reaction temperature in the reaction module.
Further, the reaction module comprises: the input end of the first reaction tube in series inputs materials and is communicated with one end of the piston device, and the output end of the last reaction tube in series outputs a product after reaction and is communicated with the other end of the piston device.
Further, the reaction tube comprises:
a tube body;
the reaction core body is fixedly arranged in the pipe body;
the material inlet is arranged on the pipe body and is used for inputting materials;
the material outlet is arranged on the pipe body and is used for outputting materials or outputting reacted products;
the heat preservation layer wraps the outer surface of the pipe body.
Further, the reaction tube further comprises: and the process analysis interface is arranged on the tube body and is used for observing and process analyzing the reaction in the reaction tube.
Further, the method further comprises the following steps: and the sensor is arranged at the process analysis interface and is used for collecting reaction data and states in the reaction tube.
Further, the reaction core comprises:
the vibrating plates are arranged in the pipe body in parallel, and divide the inside of the pipe body into a plurality of sections along the radial direction of the pipe body;
a plurality of oscillating plate fixing rods, each oscillating plate fixing rod penetrates through and fixes a plurality of oscillating plates along the radial direction of the pipe body;
and the pair of tube plates are respectively arranged at two ends of the tube body.
Further, the heat exchange module comprises: and the heat exchange modules are all or partially connected in series, each heat exchange module is arranged in the reaction tube and used for circulating heat exchange media, and the serial direction of the heat exchange modules is the same as the serial direction of the reaction tube.
Further, the heat exchange module includes:
the heat exchange pipes penetrate through the oscillating plates along the radial direction of the pipe body, and two ends of each heat exchange pipe respectively penetrate through a pair of pipe plates;
the pair of end socket assemblies are respectively connected to the outer sides of the pair of tube plates, and are respectively communicated with the two ends of each heat exchange tube.
Further, the head assembly comprises: the heat exchange device comprises a seal head and a seal head connecting pipe, wherein the seal head is used for communicating a heat exchange pipe, and the seal head connecting pipe is used for inputting or outputting a heat exchange medium.
Further, each oscillating plate is provided with a plurality of through holes, and the through holes are respectively used for penetrating the oscillating plate fixing rod and the heat exchange tube and for material circulation.
According to still another embodiment of the present invention, there is provided a nitration reaction apparatus including any one of the continuous plug flow swirling flow reaction apparatuses described above, further including: and the separation filter circuit is connected with the piston device and the reaction module in parallel, and two ends of the separation filter circuit are respectively communicated with two ends of the piston device.
Further, the separation filtration circuit comprises: and the two ends of the separation filter are respectively communicated with the two ends of the piston device through pipelines and are used for carrying out solid-liquid separation on the products after reaction in the reaction module, collecting solid products and recycling waste acid into the reaction module.
According to still another embodiment of the present invention, there is provided an ammonium fluoride production apparatus including any one of the continuous plug flow swirling flow reaction apparatuses described above, further including: and the ammonium fluoride separation and filtration loop is connected with the piston device and the reaction module in parallel, and two ends of the ammonium fluoride separation and filtration loop are respectively communicated with two ends of the piston device.
Further, the ammonium fluoride separation filtration circuit comprises: and the two ends of the ammonium fluoride separation filter are respectively communicated with the two ends of the piston device through pipelines and are used for carrying out solid-liquid separation on the products after reaction in the reaction module, collecting solid products and recycling waste acid into the reaction module.
According to still another embodiment of the present invention, there is provided a sodium sulfate and sodium chloride separation system comprising a sodium chloride separation device and a sodium sulfate separation device in series;
the sodium chloride separation device comprises any one of the continuous plug flow swirling flow reaction devices and a sodium chloride separation filter, wherein the input end of the sodium chloride separation filter is connected with the output end of a reaction module of the continuous plug flow swirling flow reaction device, and the sodium chloride separation filter is used for carrying out solid-liquid separation on a product reacted in the reaction module, collecting solid sodium chloride and recycling salt water into the sodium sulfate separation device;
the sodium sulfate separation device comprises another continuous plug flow swirling flow reaction device and a sodium sulfate separation filter, wherein the input end of a reaction module of the other continuous plug flow swirling flow reaction device is connected with the output end of the sodium chloride separation filter, the output end of a reaction module of the other continuous plug flow swirling flow reaction device is connected with the input end of the sodium sulfate separation filter, and the sodium sulfate separation filter is used for carrying out solid-liquid separation on a product, collecting solid sodium sulfate and discharging salt water.
The continuous plug flow swirling flow reaction device provided by the embodiment of the invention has the advantages of compact volume, large occupied area saving, simplicity, reliability and easiness in maintenance; meanwhile, the process time is greatly shortened, the efficiency is higher, and the control is easy.
It is to be understood that both the foregoing general description and the following detailed description are exemplary and are intended to provide further explanation of the technology claimed.
Drawings
FIG. 1 is a schematic diagram of a continuous plug flow swirling flow reaction apparatus according to an embodiment of the present invention;
FIG. 2 is a schematic structural view of the reaction module and the heat exchange module of FIG. 1;
FIG. 3 is a schematic view of the housing of FIG. 2;
FIG. 4 is an internal schematic view of FIG. 2;
FIG. 5 is a schematic diagram of the oscillating plate of FIG. 1;
FIG. 6 is a schematic diagram of the material flow pattern of a continuous plug flow swirling flow reaction device according to an embodiment of the present invention;
FIG. 7 is a schematic diagram of a continuous plug flow swirling flow reaction apparatus according to an embodiment of the present invention applied to bio-enzyme protein synthesis production;
FIG. 8 is a schematic view showing the construction of a nitration reaction apparatus according to an embodiment of the present invention;
FIG. 9 is a schematic view showing the construction of an apparatus for producing ammonium fluoride according to an embodiment of the present invention;
fig. 10 is a schematic diagram of a separation system for sodium sulfate and sodium chloride according to an embodiment of the present invention.
Detailed Description
The preferred embodiments of the present invention will be described in detail below with reference to the attached drawings, which further illustrate the present invention.
Firstly, a continuous plug flow swirling flow reaction device according to an embodiment of the present invention will be described with reference to fig. 1 to 7, and is used for chemical reactions, and has a wide application scenario.
As shown in fig. 1, the continuous plug flow swirling flow reaction device of the embodiment of the present invention has a reaction module 1, a plug device 2 and a heat exchange module 3.
Specifically, as shown in fig. 1, the input end of the reaction module 1 inputs materials, and the output end of the reaction module 1 outputs a reacted product, which has: the input end of the first reaction tube 11 in series inputs materials and is communicated with one end of the piston device 2, and the output end of the last reaction tube 11 in series outputs a product after reaction and is communicated with the other end of the piston device 2, so that the volume is compact, the occupied area is greatly saved, and the device is simple, reliable and easy to maintain.
Further, as shown in fig. 2 to 4, the reaction tube 11 comprises: the reaction device comprises a tube body 111, a reaction core 112, a material inlet 113, a material outlet 114 and a heat preservation layer 115, wherein the reaction core 112 is fixedly arranged inside the tube body 111; a material inlet 113 is provided on the pipe body 111 for inputting material; a material outlet 114 is provided on the tube 111 for outputting material or outputting reacted product; the heat preservation layer 115 wraps the outer surface of the tube 111.
Further, as shown in fig. 1 to 3, the reaction tube 11 further comprises: a process analysis interface 116, the process analysis interface 116 being provided on the tube body 111 for observing and process analyzing the reaction in the reaction tube 11. In this embodiment, the continuous plug flow swirling flow reaction apparatus of the embodiment of the present invention further has a sensor 4, where the sensor 4 is disposed at the process analysis interface 116, and uses a process analysis technology to collect reaction data and status in the reaction tube 11, for example: the data of the raw materials, the intermediates and the final products are convenient for knowing the influence mode of the process variables on the basis of physical, chemical and biological systems, and provide opportunities for detecting unknown intermediates, mechanisms and endpoints, and can be adopted in the processes of research, development, amplification production and process control.
Further, as shown in fig. 2 and 4, the reaction core 112 includes: a plurality of oscillating plates 1121, a plurality of oscillating plate fixing rods 1122, and a pair of tube plates 1123. The oscillating plates 1121 are arranged in parallel inside the tube 111, and the oscillating plates 1121 divide the inside of the tube 111 into a plurality of sections along the radial direction of the tube 111, so that a plurality of small reaction kettles connected in series are formed among the oscillating plates 1121; each oscillating plate fixing rod 1122 penetrates and fixes a plurality of oscillating plates 1121 along the radial direction of the pipe body 111; a pair of tube plates 1123 are provided at both ends of the tube body 111, respectively.
Specifically, as shown in fig. 1, the piston device 2 is connected in parallel with the reaction module 1, one end of the piston device 2 is communicated with the input end of the reaction module 1, and the other end of the piston device 2 is communicated with the output end of the piston device 2, so as to provide push-pull power for the piston to enable the materials to flow and be fully mixed and reacted.
Specifically, as shown in fig. 1, 2, and 4, a heat exchange module 3 is provided in the reaction module 1 for adjusting the reaction temperature in the reaction module 1, and has: the heat exchange modules 31 are all or partially connected in series, each heat exchange module 31 is arranged in the reaction tube 11, the heat exchange modules 31 are used for circulating heat exchange media, the serial direction of the heat exchange modules 31 is the same as the serial direction of the reaction tube 11, and the volume is further compact, and the heat exchange module is simple, reliable and easy to maintain. In this embodiment, when all the heat exchange modules 31 are connected in series, the same heat exchange medium is used; when a plurality of heat exchange modules 31 are partially connected in series, the mutually connected parts adopt the same heat exchange medium, and different heat exchange mediums are adopted according to the needs, so as to achieve better heat exchange effect.
Further, as shown in fig. 1, 2 and 4, the heat exchange module 31 includes: a plurality of heat exchange tubes 311 and a pair of head assemblies 312.
As shown in fig. 1, 2 and 4, the plurality of heat exchange tubes 311 pass through the plurality of oscillation plates 1121 along the radial direction of the tube body 111, and two ends of each heat exchange tube 311 respectively pass through the pair of tube plates 1123, so that a plurality of parallel small reaction kettles are formed between any two oscillation plates 1121 due to the division of the heat exchange tubes 311, a plurality of serial small reaction kettles are formed between the plurality of oscillation plates 1121, and active mixing of the piston device 2 is performed, as shown in fig. 6, so that material fluid fully reacts in a piston flow and vortex flow mode at the reaction core 112, the piston flow effect is equivalent to series connection of a plurality of continuous kettle reactors, the mixing times and the mass transfer rate are all higher than those of 1-2 orders of magnitude of large kettle reactors, the fluid dispersion coefficient is small, the residence time is wide for 10s-10h, the downstream reaction is also possible, the process time is greatly shortened, the efficiency is higher, and the control is easy.
As shown in fig. 1, 2 and 4, a pair of head assemblies 312 are respectively connected to the outer sides of a pair of tube plates 1123, and the pair of head assemblies 312 are respectively communicated with both ends of each heat exchange tube 311, in this embodiment, the head assemblies 312 have: a seal head 3121 and a seal head connection pipe 3122, wherein the seal head 3121 is used for communicating the heat exchange tube 311, and the seal head connection pipe 3122 is used for inputting or outputting a heat exchange medium. When materials accompanied with exothermic or endothermic reactions are produced, the formation of hot spots or cold spots can be prevented by properly controlling the reactions, the heat exchange coefficient between the materials and the heat exchange medium in the heat exchange tube 311 is effectively improved by the flow of the materials in the form of plug flow and vortex flow at the reaction core 112, the temperature gradient problem can be solved by precisely controlling the temperature, and various types of heating or cooling curves can be realized by flexibly setting temperature areas through the isolation, series connection and parallel connection of the heat exchange medium flow channels.
Further, as shown in fig. 5, each oscillating plate 1121 is provided with a plurality of through holes 11211, and the plurality of through holes 11211 are respectively used for penetrating the oscillating plate fixing rod 1122 and the heat exchange tube 311, and for material circulation.
When in operation, as shown in fig. 7, taking a biological enzyme protein synthesis production process as an example, three materials enter a cavity formed by a tube body 111, a tube plate 1123, a vibrating plate 1121, a vibrating plate fixing rod 1122 and a heat exchange tube 311 from a material inlet 113, and reciprocate at a through hole on the vibrating plate 1121 in the cavity, so as to finish the processes of mixing, heat exchange, reaction, crystallization and the like, and are discharged through a material outlet 114, wherein a heat exchange medium enters the heat exchange tube 311 through a sealing head 3121 and a sealing head connecting tube 3122, flows out through the sealing head 3121 and the sealing head connecting tube 3122 at the other end of the reaction core 112, and completes the heat exchange process.
As above, in the continuous plug flow swirling flow reaction device according to the embodiment of the invention, the volume is compact, the occupied area is greatly saved, and the device is simple, reliable and easy to maintain; meanwhile, the process time is greatly shortened, the efficiency is higher, and the control is easy.
The continuous plug flow swirling flow reaction device according to the embodiment of the invention is described above with reference to fig. 1 to 7. Further, the present invention can also be applied to a nitration reaction apparatus.
As shown in FIG. 8, the nitration reaction apparatus according to the embodiment of the present invention has the continuous plug flow swirling flow reaction apparatus according to the above embodiment, and further comprises: and a separation filter circuit 5 connected in parallel with the piston device 2 and the reaction module 1, and two ends of the separation filter circuit are respectively communicated with two ends of the piston device 2. In this embodiment, the working principle of the continuous plug flow swirling flow reaction device is the same as that of the continuous plug flow swirling flow reaction device in the embodiment of the present invention, and will not be described here again.
Further, as shown in fig. 8, the separation filter circuit 5 includes: the separation filter 51 has two ends respectively connected to two ends of the piston device 2 via pipes, and is used for solid-liquid separation of the reacted product in the reaction module 1.
As shown in figure 8, the nitration reaction is a reaction process of introducing nitro into organic molecules, the nitration is a strong exothermic reaction, the heat release is concentrated, when the device works, mixed acid and benzene are sent into a continuous plug flow vortex flow reaction device to complete heat exchange and reaction synthesis of materials, and temperature and pressure parameters in the heat exchange and reaction synthesis process of the materials are monitored by a sensor 4 to realize control. After the reaction, solid-liquid separation is performed by the separation filter 51, nitrobenzene separated from the solids is collected by the collecting tank, and waste acid is recycled into the reaction module 1.
A nitration reaction apparatus according to an embodiment of the present invention is described above with reference to fig. 8. Further, the present invention can also be applied to an ammonium fluoride production apparatus.
As shown in fig. 9, the ammonium fluoride production apparatus according to the embodiment of the present invention includes the continuous plug flow swirling flow reaction apparatus according to the above embodiment, further including: and the ammonium fluoride separation and filtration loop 6 is connected with the piston device 2 and the reaction module 1 in parallel, and two ends of the ammonium fluoride separation and filtration loop are respectively communicated with two ends of the piston device 2. In this embodiment, the working principle of the continuous plug flow swirling flow reaction device is the same as that of the continuous plug flow swirling flow reaction device in the embodiment of the present invention, and will not be described here again.
Further, as shown in fig. 9, the ammonium fluoride separation filter circuit 6 includes: the two ends of the ammonium fluoride separation filter 61 are respectively communicated with the two ends of the piston device 2 through pipelines, and are used for carrying out solid-liquid separation on the products after reaction in the reaction module 1.
When in operation, as shown in fig. 9, the material HF and ammonia gas are input into the continuous plug flow swirling flow reaction device, after heat exchange and reaction synthesis, the temperature, pressure and PH parameters in the heat exchange and reaction synthesis process of the material are monitored by the sensor 4 to realize control, and in this embodiment, the continuous plug flow swirling flow reaction device adopts two heat exchange mediums to exchange heat for the material. After the reaction, solid-liquid separation is performed by an ammonium fluoride separation filter 61, and the separated ammonium fluoride crystals are collected by a collecting tank, and the waste acid is recycled into the reaction module 1.
An apparatus for producing ammonium fluoride according to an embodiment of the present invention is described above with reference to fig. 9. Further, the invention can also be applied to a sodium sulfate and sodium chloride separation system.
As shown in fig. 10, the sodium sulfate and sodium chloride separation system of the embodiment of the present invention has a sodium chloride separation device 7 and a sodium sulfate separation device 8 connected in series;
the sodium chloride separation device 7 comprises the continuous plug flow swirling flow reaction device and the sodium chloride separation filter 71 of the above embodiments, and the input end of the sodium chloride separation filter 71 is connected with the output end of the reaction module 1 of the continuous plug flow swirling flow reaction device.
The sodium sulfate separation device 8 comprises another continuous plug flow swirling flow reaction device and a sodium sulfate separation filter 81 of the above embodiments, wherein the input end of the reaction module 1 of the other continuous plug flow swirling flow reaction device is connected with the output end of the sodium chloride separation filter 71, and the output end of the reaction module 1 of the other continuous plug flow swirling flow reaction device is connected with the input end of the sodium sulfate separation filter 81.
When the device works, as shown in fig. 10, sodium chloride and sodium sulfate supersaturated liquid are input into a continuous plug flow swirling flow reaction device of a sodium chloride separation device 7, after the reaction, products after the reaction in a reaction module 1 are subjected to solid-liquid separation by a sodium chloride separation filter 71, solid sodium chloride is collected, brine is input into a sodium sulfate separation device 8, then the products are subjected to solid-liquid separation by a sodium sulfate separation filter 81 after the reaction by the continuous plug flow swirling flow reaction device of the sodium sulfate separation device 8, and the solid sodium sulfate is collected and the brine is discharged.
The continuous plug flow swirling flow reaction device according to the embodiment of the invention is described above with reference to fig. 1 to 10, and has compact volume, greatly saves occupied area, and is simple, reliable and easy to maintain; meanwhile, the process time is greatly shortened, the efficiency is higher, and the control is easy.
It should be noted that in this specification the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation, an element defined by the phrase "comprising … …" does not exclude the presence of additional identical elements in a process, method, article, or apparatus that comprises an element.
While the present invention has been described in detail through the foregoing description of the preferred embodiment, it should be understood that the foregoing description is not to be considered as limiting the invention. Many modifications and substitutions of the present invention will become apparent to those of ordinary skill in the art upon reading the foregoing. Accordingly, the scope of the invention should be limited only by the attached claims.
Claims (9)
1. A continuous plug flow swirling flow reaction device, comprising:
the input end of the reaction module is used for inputting materials, and the output end of the reaction module is used for outputting a product after reaction;
the piston device is connected with the reaction module in parallel, one end of the piston device is communicated with the input end of the reaction module, and the other end of the piston device is communicated with the output end of the piston device and is used for providing piston push-pull power to enable materials to flow and fully mix and react;
the heat exchange module is arranged in the reaction module and used for adjusting the reaction temperature in the reaction module;
the reaction module comprises a plurality of reaction tubes which are connected in series, wherein the input end of the first reaction tube in series inputs materials and is communicated with one end of the piston device, and the output end of the last reaction tube in series outputs a product after reaction and is communicated with the other end of the piston device;
the reaction tube may comprise a tube having a cross-section,
a tube body;
the reaction core body is fixedly arranged in the pipe body;
the material inlet is arranged on the pipe body and is used for inputting materials;
the material outlet is arranged on the pipe body and is used for outputting materials or outputting reacted products;
the heat preservation layer is wrapped on the outer surface of the pipe body;
the reaction core may comprise a polymer material that,
the vibrating plates are arranged in the pipe body in parallel, and divide the inside of the pipe body into a plurality of sections along the radial direction of the pipe body;
the vibration plate fixing rods penetrate through and fix the vibration plates along the radial direction of the pipe body;
the pair of tube plates are respectively arranged at two ends of the tube body;
the heat exchange module comprises a plurality of heat exchange modules which are all or partially connected in series, each heat exchange module is arranged in the reaction tube, the heat exchange modules are used for circulating heat exchange media, and the serial direction of the heat exchange modules is the same as the serial direction of the reaction tube;
the heat exchange module comprises a heat exchange module body and a heat exchange module body,
the heat exchange tubes penetrate through the oscillating plates along the radial direction of the tube body, and the two ends of each heat exchange tube penetrate through the pair of tube plates respectively;
the pair of end socket assemblies are respectively connected to the outer sides of the pair of tube plates and are respectively communicated with the two ends of each heat exchange tube;
each oscillating plate is provided with a plurality of through holes, and the through holes are respectively used for penetrating the oscillating plate fixing rod and the heat exchange tube and for material circulation.
2. The continuous plug flow swirling flow reaction device according to claim 1, wherein the reaction tube further comprises: and the process analysis interface is arranged on the tube body and is used for observing and process analyzing the reaction in the reaction tube.
3. The continuous plug flow swirling flow reaction device according to claim 2, further comprising: and the sensor is arranged at the process analysis interface and is used for collecting reaction data and states in the reaction tube.
4. The continuous plug flow swirling flow reaction device according to claim 1, wherein the head assembly comprises: the heat exchange device comprises a seal head and a seal head connecting pipe, wherein the seal head is used for being communicated with the heat exchange pipe, and the seal head connecting pipe is used for inputting or outputting a heat exchange medium.
5. A nitration reaction apparatus, comprising the continuous plug flow swirling flow reaction apparatus according to any one of claims 1 to 4, further comprising: and the separation filter circuit is connected with the piston device and the reaction module in parallel, and two ends of the separation filter circuit are respectively communicated with two ends of the piston device.
6. The nitration reaction apparatus of claim 5, wherein the separation filtration circuit comprises: and the two ends of the separation filter are respectively communicated with the two ends of the piston device through pipelines and are used for carrying out solid-liquid separation on the products after reaction in the reaction module, collecting solid products and recycling waste acid into the reaction module.
7. An ammonium fluoride production apparatus comprising the continuous plug flow swirling flow reaction apparatus according to any one of claims 1 to 4, further comprising: and the ammonium fluoride separation and filtration loop is connected with the piston device and the reaction module in parallel, and two ends of the ammonium fluoride separation and filtration loop are respectively communicated with two ends of the piston device.
8. The ammonium fluoride production plant of claim 7, wherein the ammonium fluoride separation filter circuit comprises: and the two ends of the ammonium fluoride separation filter are respectively communicated with the two ends of the piston device through pipelines and are used for carrying out solid-liquid separation on the products after reaction in the reaction module, collecting solid products and recycling waste acid into the reaction module.
9. The sodium sulfate and sodium chloride separation system is characterized by comprising a sodium chloride separation device and a sodium sulfate separation device which are connected in series;
the sodium chloride separation device comprises the continuous plug flow swirling flow reaction device and a sodium chloride separation filter according to any one of claims 1-4, wherein the input end of the sodium chloride separation filter is connected with the output end of a reaction module of the continuous plug flow swirling flow reaction device, and the sodium chloride separation filter is used for carrying out solid-liquid separation on a product reacted in the reaction module, collecting solid sodium chloride and recycling brine into the sodium sulfate separation device;
the sodium sulfate separation device comprises another continuous plug flow swirling flow reaction device and a sodium sulfate separation filter according to any one of claims 1-4, wherein the input end of a reaction module of the other continuous plug flow swirling flow reaction device is connected with the output end of the sodium chloride separation filter, the output end of the reaction module of the other continuous plug flow swirling flow reaction device is connected with the input end of the sodium sulfate separation filter, and the sodium sulfate separation filter is used for carrying out solid-liquid separation on a product, collecting solid sodium sulfate and discharging brine.
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