CN111434606A - Micro mixer and preparation method of hollow carbon spheres for lithium battery material - Google Patents
Micro mixer and preparation method of hollow carbon spheres for lithium battery material Download PDFInfo
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- CN111434606A CN111434606A CN201910034766.4A CN201910034766A CN111434606A CN 111434606 A CN111434606 A CN 111434606A CN 201910034766 A CN201910034766 A CN 201910034766A CN 111434606 A CN111434606 A CN 111434606A
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- spring type
- type pipeline
- fluid
- rotating spring
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 26
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 12
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 12
- 239000000463 material Substances 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title abstract description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 33
- 239000012530 fluid Substances 0.000 claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 24
- 238000002347 injection Methods 0.000 claims abstract description 22
- 239000007924 injection Substances 0.000 claims abstract description 22
- GHMLBKRAJCXXBS-UHFFFAOYSA-N resorcinol Chemical compound OC1=CC=CC(O)=C1 GHMLBKRAJCXXBS-UHFFFAOYSA-N 0.000 claims abstract description 22
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 230000000903 blocking effect Effects 0.000 claims abstract description 19
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 10
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000004140 cleaning Methods 0.000 claims abstract description 5
- 239000011259 mixed solution Substances 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 239000004005 microsphere Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 10
- 238000012643 polycondensation polymerization Methods 0.000 claims description 5
- 238000003475 lamination Methods 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 3
- 239000012780 transparent material Substances 0.000 claims description 3
- 230000004888 barrier function Effects 0.000 claims 3
- 230000001678 irradiating effect Effects 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 description 5
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002086 nanomaterial Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- 239000010426 asphalt Substances 0.000 description 2
- 238000009792 diffusion process Methods 0.000 description 2
- 239000003822 epoxy resin Substances 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 239000005011 phenolic resin Substances 0.000 description 2
- 229920001568 phenolic resin Polymers 0.000 description 2
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
- 239000004926 polymethyl methacrylate Substances 0.000 description 2
- 230000005514 two-phase flow Effects 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 239000004793 Polystyrene Substances 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 229920002472 Starch Polymers 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- GELKBWJHTRAYNV-UHFFFAOYSA-K lithium iron phosphate Chemical compound [Li+].[Fe+2].[O-]P([O-])([O-])=O GELKBWJHTRAYNV-UHFFFAOYSA-K 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000001509 sodium citrate Substances 0.000 description 1
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 description 1
- 239000008107 starch Substances 0.000 description 1
- 235000019698 starch Nutrition 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/05—Preparation or purification of carbon not covered by groups C01B32/15, C01B32/20, C01B32/25, C01B32/30
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
- B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
- B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
- B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
- B01F25/4331—Mixers with bended, curved, coiled, wounded mixing tubes or comprising elements for bending the flow
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
- B01F25/40—Static mixers
- B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
- B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
- B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
- B01F25/4334—Mixers with a converging cross-section
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F33/00—Other mixers; Mixing plants; Combinations of mixers
- B01F33/30—Micromixers
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Dispersion Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a micro mixer which comprises a rotary spring type pipeline, wherein two liquid injection pipes are arranged at the inlet of the rotary spring type pipeline, and a plurality of blocking structural members are arranged on the inner wall of the rotary spring type pipeline. A preparation method of hollow carbon spheres for a lithium battery material comprises the steps of dissolving silicon dioxide microspheres in a mixed solution to obtain a fluid A; mixing resorcinol and formaldehyde and dissolving in water to obtain a fluid B; respectively injecting the fluid A and the fluid B into the rotating spring type pipeline through two liquid injection pipes; an ultraviolet emission source is arranged at an outlet of the rotating spring type pipeline, and resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotating spring type pipeline are promoted to be condensed by ultraviolet irradiation to form gel; sintering the gel to obtain a sintered sample; and cleaning the sintered sample, and removing silicon dioxide to obtain the hollow carbon spheres. The size of the micro mixer is shortened, the mixing time is reduced, and the mixing uniformity of the multiphase flow is improved.
Description
Technical Field
The invention relates to the field of lithium batteries, in particular to a micro mixer and a preparation method of hollow carbon spheres for a lithium battery material.
Background
The preparation process of the material in the lithium battery industry needs to uniformly mix all phase substances so as to obtain the nano material with uniform size, a micro mixer is usually used in the mixing process, at present, the commonly used micro mixer adopts a parallel lamination mixer to mix two-phase flow or multi-phase flow in the horizontal direction, the two-phase flow or the multi-phase flow is in parallel flow at the initial stage of mixing, and the multi-phase flow can only be subjected to micro mixing through molecular diffusion due to the fact that a micro channel structure does not have a special blocking structure, and the condition of uneven mixing exists.
Disclosure of Invention
The technical problem to be solved by the invention is to provide a micro mixer and a preparation method of hollow carbon spheres for lithium battery materials, so as to overcome the defects in the prior art.
The technical scheme for solving the technical problems is as follows: a micro mixer comprises a rotary spring type pipeline, at least two liquid injection pipes communicated with an inlet of the rotary spring type pipeline are arranged at the inlet of the rotary spring type pipeline, and a plurality of blocking structural members are arranged on the inner wall of the rotary spring type pipeline.
The invention has the beneficial effects that: through the rotating spring type pipeline and the blocking structural parts additionally arranged in the pipeline, the turbulent flow condition of fluid in the pipeline can be further improved, the size of a micro mixer is shortened, the mixing time is shortened, and the mixing uniformity of multiphase flow is improved.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, hinder the structure and include first hindrance board and second and hinder the board, first hindrance board and second hinder the board and stagger arrangement from top to bottom, and have the interval in the extending direction of swivel spring formula pipeline.
Further, the projection of the first hindering plate in the hindering structure part along the extending direction of the rotating spring type pipeline does not intersect with the projection of the second hindering plate along the extending direction of the rotating spring type pipeline.
Further, the interval between first hindrance board and the second in hindering the structure is 50um-500 um.
Further, the inner diameter of the rotating spring type pipeline is 50-500 μm.
Furthermore, the inlet structure of the liquid injection pipe is a longitudinal lamination type.
Adopt above-mentioned further beneficial effect to do: can effectively utilize the density difference of the molecular diffusion.
Furthermore, the rotating spring type pipeline and all the liquid injection pipes form a U-shaped, Y-shaped, T-shaped or mixed structure together.
Furthermore, the rotating spring type pipeline is made of transparent materials.
Further, the rotating spring type pipeline is made of glass.
Adopt above-mentioned further beneficial effect to do: facilitating observation of the mixing process.
A preparation method of hollow carbon spheres for a lithium battery material comprises the following steps:
s100, dissolving the silicon dioxide microspheres in the mixed solution to obtain a fluid A for later use;
s200, mixing resorcinol and formaldehyde and dissolving in water to obtain a fluid B for later use;
s300, injecting the fluid A and the fluid B into the rotating spring type pipeline through two liquid injection pipes at the same speed respectively;
s400, arranging an ultraviolet emission source at an outlet of the rotary spring type pipeline, and performing ultraviolet irradiation to promote condensation polymerization of resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotary spring type pipeline to form gel;
s500, sintering the gel to obtain a sintered sample;
s600, cleaning the sintered sample, and removing silicon dioxide to obtain the hollow carbon sphere.
Adopt above-mentioned further beneficial effect to do: is beneficial to synthesizing hollow carbon spheres with uniform size.
Drawings
FIG. 1 is a schematic structural diagram of a micro mixer according to the present invention;
FIG. 2 is a schematic view of a partial structure of the coil spring type pipe of the present invention;
FIG. 3 is a cross-sectional view of FIG. 2;
FIG. 4 is a TEM image of hollow carbon spheres prepared according to the present invention;
FIG. 5 is an SEM image of hollow carbon spheres prepared according to the present invention;
FIG. 6 is a Raman image of hollow carbon spheres prepared according to the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
As shown in figures 1, 2 and 3, the micromixer comprises a rotating spring type pipeline 1, at least two liquid injection pipes 2 communicated with the inlet of the rotating spring type pipeline 1 are arranged at the inlet of the rotating spring type pipeline 1, in the invention, only two fluids are required to be injected when the micromixer is used for preparing the hollow carbon spheres in the later period, therefore, the number of the liquid injection pipes 2 can be only two, and the number of the liquid injection pipes 2 can be three, four, five, six and the like under different conditions, and in addition, a plurality of obstruction structural members 110 are arranged on the inner wall of the rotating spring type pipeline 1. The coil spring type pipe 1 is made of transparent material, such as glass.
The two liquid injection pipes 2 are connected with the rotating spring type pipeline 1 to form a U shape, certainly a Y shape or a T shape, the inner diameters of the rotating spring type pipeline 1 and the liquid injection pipes 2 are 50-500 μm, and specifically can be 50um, 80um, 100um, 150um, 170um, 210um, 260um or 300 um.
The blocking structure 110 comprises a first blocking plate 111 and a second blocking plate 112, the first blocking plate 111 and the second blocking plate 112 are arranged in a staggered manner up and down, and are spaced in the extending direction of the rotary spring type pipeline 1, and the projection of the first blocking plate 111 in the extending direction of the rotary spring type pipeline 1 in the blocking structure 110 does not intersect with the projection of the second blocking plate 112 in the extending direction of the rotary spring type pipeline 1, as shown in fig. 3; the interval between the first hindering plate 111 and the second hindering plate 112 in the same hindering structure 110 is 50um-500um, specifically can be 50um, 80um, 100um, 150um, 170um, 210um, 260um or 300 um.
The inlet structure of the liquid injection pipe 2 is a longitudinal lamination type.
The micro mixer pipeline can also be arranged in a slotted structure in the flat plate.
As shown in fig. 4, 5 and 6, a method for preparing hollow carbon spheres for a lithium battery material using the micromixer includes the steps of:
s100, dissolving the silicon dioxide microspheres in the mixed solution to obtain a fluid A for later use;
s200, mixing resorcinol and formaldehyde and dissolving in water to obtain a fluid B for later use;
s300, injecting the fluid A and the fluid B into the rotary spring type pipeline 1 through the two liquid injection pipes 2 at the same speed respectively;
s400, arranging an ultraviolet emission source at an outlet of the rotary spring type pipeline 1, and performing ultraviolet irradiation to promote condensation polymerization of resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotary spring type pipeline 1 to form gel;
s500, sintering the gel to obtain a sintered sample;
s600, cleaning the sintered sample, and removing silicon dioxide to obtain the hollow carbon sphere.
Application example:
a method for preparing hollow carbon spheres for a lithium battery material by using the micromixer comprises the following steps:
s100, dissolving 1.2g of silica microspheres prepared by a template method in 30ml of mixed solution to obtain a fluid A for later use;
s200, mixing resorcinol and formaldehyde according to a molar ratio of 1:2, and dissolving the mixture obtained after mixing in water to form a water sample with a solute content of 10% to obtain a fluid B for later use;
s300, respectively injecting the fluid A and the fluid B into the rotary spring type pipeline 1 through two liquid injection pipes 2 by using a syringe pump at the same speed, wherein the inner diameters of the two liquid injection pipes 2 and the rotary spring type pipeline 1 are 100 mu m, the injection speed is 0.1-10mm/S, actually 0.1mm/S, 0.8mm/S, 1mm/S, 2.6mm/S, 3.5mm/S, 5.8mm/S, 7.5mm/S, 9mm/S or 10mm/S, and good mixing is achieved through the rotary spring type pipeline 1 according to the characteristics of the fluid A and the fluid B and the inner diameters of the liquid injection pipes 2 and the rotary spring type pipeline 1, wherein the injection speed is preferably 1 mm/S;
s400, arranging an ultraviolet emission source at an outlet of the rotary spring type pipeline 1, and performing ultraviolet irradiation to promote condensation polymerization of resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotary spring type pipeline 1 to form gel;
s500, sintering the gel at 1500 ℃ to obtain a sintered sample;
s600, cleaning the sintered sample by using hydrofluoric acid, and removing silicon dioxide to obtain the hollow carbon sphere.
Micro-mixing and coupling with a gel method can prepare solid carbon spheres;
in the gel method, the gel can be organic matters such as resorcinol and formaldehyde which can be subjected to dehydration or alcohol loss condensation polymerization so as to synthesize carbon sources such as phenolic resin and epoxy resin.
Solid carbon spheres can be prepared by coupling micro-mixing with a hydrothermal method;
in the hydrothermal method, the carbon source can be petroleum asphalt, coal asphalt, sucrose, glucose, starch, cellulose, sodium citrate, phenolic resin, epoxy resin and other organic carbon sources.
Micro-mixing and template method coupling can prepare hollow carbon spheres;
the template can be an organic template such as Polystyrene (PS), polymethyl methacrylate (PMMA) and the like, or an inorganic template such as SiO2, MnO and the like.
Micro-mixing may be coupled with vapor deposition.
Can be used for the carbon coating process of the anode nano material;
the nano material comprises lithium iron phosphate, metal oxide, metal sulfide and other lithium battery anode materials.
Fluid: can be gas, liquid or gas-liquid-solid two-phase mixture.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. The micro mixer is characterized by comprising a rotating spring type pipeline (1), wherein at least two liquid injection pipes (2) communicated with an inlet of the rotating spring type pipeline (1) are arranged at the inlet of the rotating spring type pipeline (1), and a plurality of blocking structural members (110) are arranged on the inner wall of the rotating spring type pipeline (1).
2. A micromixer according to claim 1, characterized in that said blocking structure (110) comprises a first (111) and a second (112) blocking plate, said first (111) and second (112) blocking plates being staggered one above the other and spaced in the direction of extension of said rotating spring duct (1).
3. A micromixer according to claim 2, characterized in that the projection of the first blocking plate (111) in the blocking structure (110) in the direction of extension of the coil spring duct (1) does not intersect the projection of the second blocking plate (112) in the direction of extension of the coil spring duct (1).
4. A micromixer according to claim 3, characterized in that the distance between the first barrier plate (111) and the second barrier plate (112) in the barrier structure (110) is 50-500 um.
5. Micromixer according to claim 4, characterized in that the internal diameter of the rotating spring-loaded conduit (1) is 50-500 μm.
6. A micromixer according to claim 1, characterized in that the inlet structure of the injection pipe (2) is of the longitudinal lamination type.
7. The micromixer according to claim 1, characterized in that said coil spring type pipe (1) and all said injection pipes (2) together form a U-shaped, Y-shaped, T-shaped or a hybrid structure thereof.
8. Micromixer according to any of claims 1 to 7, characterized in that the rotating spring-type duct (1) is made of transparent material.
9. Micromixer according to claim 8, characterized in that the rotating spring-type pipe (1) is made of glass.
10. A method for preparing hollow carbon spheres for lithium battery materials, characterized in that a micromixer according to any one of claims 1 to 9 is used, the method comprising the following steps:
s100, dissolving the silicon dioxide microspheres in the mixed solution to obtain a fluid A for later use;
s200, mixing resorcinol and formaldehyde and dissolving in water to obtain a fluid B for later use;
s300, injecting the fluid A and the fluid B into the rotary spring type pipeline (1) through two liquid injection pipes (2) at the same speed respectively;
s400, arranging an ultraviolet emission source at an outlet of the rotary spring type pipeline (1), and irradiating by ultraviolet light to promote condensation polymerization of resorcinol and formaldehyde in the mixed liquid flowing through the outlet of the rotary spring type pipeline (1) to form gel;
s500, sintering the gel to obtain a sintered sample;
s600, cleaning the sintered sample, and removing silicon dioxide to obtain the hollow carbon sphere.
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Cited By (1)
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CN113499744A (en) * | 2021-07-07 | 2021-10-15 | 山东泰和水处理科技股份有限公司 | Micro-channel reactor manufactured based on 3D printer technology |
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Application publication date: 20200721 |