CN116408020A - Microreactor suitable for two liquid phase raw materials rapid reaction generates solid phase product - Google Patents
Microreactor suitable for two liquid phase raw materials rapid reaction generates solid phase product Download PDFInfo
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- CN116408020A CN116408020A CN202111672864.4A CN202111672864A CN116408020A CN 116408020 A CN116408020 A CN 116408020A CN 202111672864 A CN202111672864 A CN 202111672864A CN 116408020 A CN116408020 A CN 116408020A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 43
- 239000002994 raw material Substances 0.000 title claims abstract description 43
- 239000007791 liquid phase Substances 0.000 title claims abstract description 33
- 239000007790 solid phase Substances 0.000 title claims abstract description 33
- 238000007599 discharging Methods 0.000 claims abstract description 22
- 238000002156 mixing Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 230000002708 enhancing effect Effects 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 13
- 230000008569 process Effects 0.000 abstract description 12
- 239000002245 particle Substances 0.000 abstract description 9
- 238000009826 distribution Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 36
- 239000007788 liquid Substances 0.000 description 8
- 239000002002 slurry Substances 0.000 description 8
- 239000006185 dispersion Substances 0.000 description 6
- 238000010992 reflux Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 3
- 230000009471 action Effects 0.000 description 3
- 239000012895 dilution Substances 0.000 description 3
- 238000010790 dilution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000012295 chemical reaction liquid Substances 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000006399 behavior Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
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- 238000009792 diffusion process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
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- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 238000010008 shearing Methods 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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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
- B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
-
- 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
- B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
Abstract
The invention discloses a micro-reactor suitable for the rapid reaction of two liquid phase raw materials to generate a solid phase product, which is characterized by comprising the following components: the reactor comprises a reactor body, wherein a first distributor and a second distributor are arranged in the reactor body from top to bottom, the reactor body is divided into an upper chamber, a middle chamber and a lower chamber, a first feeding hole is formed in the top of the reactor body, a first discharging hole is formed in the bottom of the reactor body, a second feeding hole is formed in one side of the side wall of the chamber located at the lowest position, a second discharging hole is formed in the other side of the side wall of the chamber, the second feeding hole is higher than the second discharging hole, and the second discharging hole is communicated with the middle chamber through a circulating pipeline. The product produced by the reactor has small particle size and narrow particle size distribution range, so that the technical process is more stable in the industrial use process, and the operation control is simple and easy to implement; the product has good repeatability and stable quality.
Description
Technical Field
The invention relates to the technical field of chemical reactors, in particular to a micro-reactor suitable for rapid reaction of two liquid-phase raw materials to generate a solid-phase product.
Background
The industrial production of the solid phase product generated by the rapid reaction of the two liquid phase raw materials adopts a large-scale stirring kettle, but the mixing time of the large-scale stirring kettle is in the second level, the mixing scale is in the millimeter level, and the mixing scale is not matched with the rapid reaction; the shearing force is small, the agglomeration phenomenon of the produced solid product particles is obvious, and the material diffusion speed in the agglomeration is slow, so that the concentration of reactant slurry in a reaction kettle is not easy to be uniform quickly, the local supersaturation degree is easy to be low, and the particle size of the product is large and the particle size distribution is wide; the unstable technological process is easy to cause, and the operation control difficulty is increased; the product quality is easy to have larger fluctuation.
Micro-dispersion technology uses micro-structural elements as cores, enhances mixing, dispersion and transmission by reducing the dispersion scale of the system in a micrometer or submillimeter limited space, and improves the controllability and efficiency of the process. With the reduction of the dispersion scale, the controllability of the fluid in the microstructure equipment is enhanced, the rapid mixing can be achieved in milliseconds, the reaction speed is adapted, and the concentration of the product slurry can be rapidly and uniformly achieved. Therefore, the invention discloses a micro-reactor which adopts micro-dispersion technology and is suitable for the rapid reaction of two liquid-phase raw materials to generate solid-phase products.
Disclosure of Invention
The invention aims to provide a micro-reactor suitable for the rapid reaction of two liquid-phase raw materials to generate a solid-phase product, so as to solve the problems of inaccurate control of a reaction process and poor controllability of process operation when the rapid reaction of the two liquid-phase raw materials to generate the solid-phase product is performed by a large-scale stirring kettle in the prior art.
To achieve the above object, the present invention provides a microreactor suitable for rapid reaction of two liquid phase raw materials to form a solid phase product, comprising: the reactor comprises a reactor body, wherein a first distributor and a second distributor are arranged in the reactor body from top to bottom, the reactor body is divided into an upper chamber, a middle chamber and a lower chamber, a first feeding hole is formed in the top of the reactor body, a first discharging hole is formed in the bottom of the reactor body, a second feeding hole is formed in one side of the side wall of the chamber located at the lowest position, a second discharging hole is formed in the other side of the side wall of the chamber, the second feeding hole is higher than the second discharging hole, and the second discharging hole is communicated with the middle chamber through a circulating pipeline.
The invention relates to a microreactor suitable for rapid reaction of two liquid phase raw materials to generate a solid phase product, wherein a first feed inlet is connected with a feed pipeline and a flowmeter.
The micro-reactor is suitable for the rapid reaction of two liquid phase raw materials to generate a solid phase product, and a pump and a flowmeter are arranged on the circulating pipeline.
The microreactor suitable for the rapid reaction of two liquid phase raw materials to generate a solid phase product is characterized in that a third distributor is arranged at the second feed inlet and is externally connected with a feed pipeline and a flowmeter.
The microreactor suitable for the rapid reaction of two liquid phase raw materials to generate a solid phase product is characterized in that the reactor body is internally provided with a straight cylinder, and the inner diameter of the reactor body is 5-20 cm.
The vertical distance between the second feeding port and the second discharging port is more than or equal to 5cm.
The microreactor is suitable for the rapid reaction of two liquid-phase raw materials to generate a solid-phase product, and the distributor is of a circular disc-shaped pore flow structure.
The micro-reactor is suitable for the rapid reaction of two liquid phase raw materials to generate a solid phase product, and the pore diameters of the upper pores of the first distributor and the second distributor are 10-1500 mu m.
The micro-reactor is suitable for the rapid reaction of two liquid phase raw materials to generate a solid phase product, and the aperture of the third distributor is 0.1-1000 mu m.
The microreactor suitable for the rapid reaction of two liquid phase raw materials to generate a solid phase product is characterized in that the inner wall of the middle chamber is provided with a member for enhancing the mixing strength.
The microreactor is suitable for the rapid reaction of two liquid-phase raw materials to generate a solid-phase product, and the distributor is connected with the reactor body in a sealing way through a flange.
The micro-reactor is suitable for the rapid reaction of two liquid phase raw materials to generate a solid phase product, and the inner wall of the reactor body and the distributor are made of stainless steel.
The invention has the beneficial effects that:
the invention designs a micro-reactor aiming at the reaction of two liquid-phase raw materials to quickly generate a solid-phase product.
The reactor body comprises two distributors and three chambers, wherein the upper chamber and the middle chamber are dilution units, and the lower chamber is a reaction unit. The reactor is suitable for the process of fast reaction of two liquid phase materials to produce solid phase product and is also suitable for industrial product production. The micro-dispersion technology is combined during design, the scale of raw material liquid drops is reduced, one raw material is dispersed into the other raw material in the form of micro-liquid drop groups to form a uniformly dispersed mixed form, and the supersaturation degree of the system is effectively regulated and controlled in the micron scale range, so that the nucleation and growth behaviors of particles are regulated and controlled at micron scale points, the mass transfer efficiency of the reaction process is improved, the defect of a large-scale stirring kettle in the mass transfer aspect is effectively overcome, the particle size of produced product particles is small, the particle size distribution range is narrow, the technological process is more stable in the industrial use process, and the operation control is simple and easy to implement; the product has good repeatability and stable quality. Therefore, the micro-reactor is suitable for the process of rapidly reacting two liquid-phase raw materials to generate a solid-phase product and is also suitable for the use in the industrial scale production of the product.
Drawings
FIG. 1 is a schematic diagram of a microreactor for rapidly reacting two liquid phase raw materials to form a solid phase product according to the present invention;
FIG. 2 shows the preparation of gamma-Al using the apparatus of the present invention 2 O 3 Key technological parameter change condition in industrial experiment process and preparation of gamma-Al by using traditional method 2 O 3 And comparing the key process parameter change conditions with the graphs.
Wherein, the reference numerals:
1. 5, 7 flowmeter
2. First distributor
3. Second distributor
4. 6 pump
8. Third distributor
9. Reaction kettle
Detailed Description
The present invention will be specifically described below by way of examples. It is noted herein that the following examples are given solely for the purpose of illustration and are not to be construed as limiting the scope of the invention, as many insubstantial modifications and variations of the invention will become apparent to those skilled in the art in light of the above disclosure.
As shown in figure 1, the microreactor suitable for the rapid reaction of two liquid phase raw materials to generate a solid phase product comprises a reactor body, wherein a first distributor 2 and a second distributor 3 are arranged in the reactor body from top to bottom to divide the reactor body into an upper chamber, a middle chamber and a lower chamber, an upper chamber is formed between the top of the reactor body and the first distributor 2, a middle chamber is formed between the first distributor 2 and the second distributor 3, a lower chamber is formed between the second distributor 3 and the bottom of the reactor body, the upper chamber and the middle chamber are dilution units, and the lower chamber is a reaction unit. The top of the reactor body is provided with a first feed inlet for introducing a liquid material into the reactor, the bottom of the reactor body is provided with a first discharge outlet for discharging the reacted material out of the reactor into a reaction kettle 9, and the first feed inlet is connected with a feed pipeline and a flowmeter 1. The side wall of one side of the lower chamber is provided with a second feeding hole, the second feeding hole is externally connected with a feeding pipeline, a pump 6 and a flowmeter 7, the side wall of the other side is provided with a second discharging hole, the position of the second feeding hole on the side wall is higher than that of the second discharging hole, another reaction liquid enters the lower chamber through the second feeding hole and reacts with materials from the first feeding hole, a membrane structure fitting and a third distributor 8 are further arranged at the second feeding hole, the second discharging hole is communicated with the middle chamber through a circulating pipeline, the circulating pipeline is provided with the pump 4 and the flowmeter 5, and the reaction liquid of the lower chamber returns to the middle chamber through the circulating pipeline.
The upper chamber, the middle chamber and the lower chamber are all straight cylinders, and the inner diameters are the same and are 5-20 cm.
The vertical distance between the second feeding hole and the second discharging hole is more than or equal to 5cm. The ratio of the flow rate of the reflux liquid pumped out from the lower chamber to the flow rate of the raw material entering the lower chamber (comprising the raw material entering through the first feeding port and the raw material entering through the second feeding port) is 5-15.
The distributor is of a disc-shaped hole flow structure, and the apertures of the holes on the first distributor and the second distributor are 10-1500 mu m; the aperture of the third distributor is 0.1-1000 mu m, and the distributor and the reactor body are connected in a sealing way through a flange.
The inner wall of the middle chamber is provided with a member for enhancing the mixing strength, and the inner wall of the reactor body and the distributor are made of stainless steel.
Example 1
A microreactor device suitable for the rapid reaction of two liquid-phase raw materials to generate a solid-phase product is provided with two circular disk-shaped hole flow type distributors, wherein the diameter of each hole is 1000 mu m. The micro-reactor is divided into three chambers from top to bottom by two distributors, wherein the upper two chambers are dilution units, the lowest chamber is a reaction unit, the sections of the three chambers are circular, the diameters of the three chambers are 15cm, a member for enhancing the mixing strength is arranged in the middle chamber, and the chambers are connected in a sealing way by a flange at the position where the distributors are arranged; the top of the upper chamber is provided with a feed inlet, and is externally connected with a feed pipe and a flowmeter; a feeding hole is formed in one side wall of the middle chamber, a return pipe and a flowmeter are externally connected with the wall of the middle chamber, and the other end of the return pipe is connected with a discharging hole of the lower chamber; a feed inlet is arranged on one side wall of the lower chamber, a membrane structure fitting is arranged at the feed inlet, a feed pipe and a flowmeter are externally connected, a discharge port is arranged on the opposite side wall, a return pipe and a flowmeter are externally connected, the other end of the return pipe is connected with the feed inlet of the middle chamber, and the other discharge port is arranged below the return pipe; one of the two raw material liquids flows into the microreactor from the feed inlet of the upper chamber after passing through the flowmeter, and flows into the middle chamber after passing through the distributor; the raw material liquid and the circulating liquid pumped out from the lower chamber flow into the lower chamber through the distributor after being intensively mixed in the middle chamber; the other raw material is input into the feeding pipe through the flowmeter through the action of the pump, flows into the microreactor from the feeding hole of the lower chamber through the distributor with the diameter of 100 mu m, reacts with the slurry from the middle chamber, part of the reacted slurry flows out of the microreactor from the discharging hole which is positioned 15cm below the feeding hole of the lower chamber through the reflux pipe through the flowmeter through the action of the pump, the ratio of the flow rate of circulating liquid input into the reflux pipe to the flow rate of the raw material entering the lower chamber is 10, and the other part flows out of the microreactor from the discharging hole below the lower chamber and flows into the reaction kettle. The materials of each chamber and the internal distributor of the microreactor are stainless steel.
Example 2
Using the microreactor of example 1, a prepared sodium metaaluminate solution at a concentration of 8.48g/L was introduced into the lower chamber of the microreactor at a flow rate of 205.36L/h; 3.27g/L of aluminum salt solution is prepared, the solution enters the upper chamber of the micro-reactor at the flow rate of 939.27L/h, passes through the upper chamber and enters the middle chamber, and thenMixing the mixture with sodium metaaluminate solution in the lower chamber at 55.0 deg.c to reflux one part of the mixed liquid in the lower chamber to the middle chamber and one part to flow out of the reactor to obtain gamma-Al 2O3 precursor suspension to prepare gamma-Al 2 O 3 . The ratio of the reflux stream to the stream entering the intermediate chamber from the upper chamber was 5. The pH value of the product slurry is monitored during the preparation process, and specific data are shown in FIG. 2.
Comparative example
The raw materials in example 2 are used, but a mechanical stirring kettle type reactor consisting of a stirrer and a kettle body is used for heterogeneous reaction, and a parallel flow dripping mode is adopted, namely two raw materials are dripped into a reaction kettle at the same time, are mixed under the action of the stirrer, and react in the process to prepare gamma-Al 2 O 3 The pH of the product slurry during the preparation process was also monitored and the specific data is shown in fig. 2.
The pH value of the product slurry is gamma-Al 2 O 3 A critical influencing factor of the product quality, the size of the pH fluctuation has a significant influence on the repeatability of the product properties and the stability of the quality. As can be seen from FIG. 2, the pH of the slurry of the product obtained from the microreactor process was significantly less fluctuated and smoother than that obtained from the conventional stirred tank reactor.
Of course, the present invention is capable of other various embodiments and its several details are capable of modification and variation in light of the present invention by one skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (12)
1. A microreactor adapted for rapid reaction of two liquid phase materials to form a solid phase product, comprising: the reactor comprises a reactor body, wherein a first distributor and a second distributor are arranged in the reactor body from top to bottom, the reactor body is divided into an upper chamber, a middle chamber and a lower chamber, a first feeding hole is formed in the top of the reactor body, a first discharging hole is formed in the bottom of the reactor body, a second feeding hole is formed in one side of the side wall of the chamber located at the lowest position, a second discharging hole is formed in the other side of the side wall of the chamber, the second feeding hole is higher than the second discharging hole, and the second discharging hole is communicated with the middle chamber through a circulating pipeline.
2. The microreactor of claim 1, wherein the first feed port is connected to a feed line and a flow meter.
3. The microreactor for rapid reaction of two liquid phase raw materials to solid phase product according to claim 1, wherein a pump and a flowmeter are arranged on the circulating pipeline.
4. The microreactor for rapid reaction of two liquid phase raw materials to solid phase product according to claim 1, wherein the second feeding port is provided with a third distributor, and is externally connected with a feeding pipeline and a flowmeter.
5. The microreactor for rapid reaction of two liquid phase raw materials to solid phase product according to claim 1, wherein the reactor body is a straight cylinder with an inner diameter of 5-20 cm.
6. The microreactor for rapid reaction of two liquid phase raw materials to solid phase product according to claim 1, wherein the vertical distance between the second feeding port and the second discharging port is 5cm or more.
7. The microreactor of claim 1 or 4, wherein the distributor has a disk-shaped pore-flow structure.
8. The microreactor for rapid reaction of two liquid phase raw materials to solid phase product according to claim 7, wherein the pore diameters of the pores on the first distributor and the second distributor are 10-1500 μm.
9. The microreactor for rapid reaction of two liquid phase raw materials to solid phase product according to claim 7, wherein the pore size of the third distributor is 0.1-1000 μm.
10. The microreactor for rapid reaction of two liquid phase raw materials to solid phase product according to claim 1, wherein the inner wall of the intermediate chamber is provided with a member for enhancing mixing strength.
11. The microreactor of claim 1 or 4, wherein the distributor is in sealed connection with the reactor body by a flange.
12. The microreactor of claim 1 or 4, wherein the inner wall of the reactor body and the distributor are made of stainless steel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111672864.4A CN116408020A (en) | 2021-12-31 | 2021-12-31 | Microreactor suitable for two liquid phase raw materials rapid reaction generates solid phase product |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111672864.4A CN116408020A (en) | 2021-12-31 | 2021-12-31 | Microreactor suitable for two liquid phase raw materials rapid reaction generates solid phase product |
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| Publication Number | Publication Date |
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| CN116408020A true CN116408020A (en) | 2023-07-11 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111672864.4A Pending CN116408020A (en) | 2021-12-31 | 2021-12-31 | Microreactor suitable for two liquid phase raw materials rapid reaction generates solid phase product |
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| Country | Link |
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| CN (1) | CN116408020A (en) |
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2021
- 2021-12-31 CN CN202111672864.4A patent/CN116408020A/en active Pending
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