CN113213551A - Battery-grade cobalt carbonate crystal form reaction process - Google Patents
Battery-grade cobalt carbonate crystal form reaction process Download PDFInfo
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- CN113213551A CN113213551A CN202110550888.6A CN202110550888A CN113213551A CN 113213551 A CN113213551 A CN 113213551A CN 202110550888 A CN202110550888 A CN 202110550888A CN 113213551 A CN113213551 A CN 113213551A
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- 238000006243 chemical reaction Methods 0.000 title claims abstract description 58
- 239000013078 crystal Substances 0.000 title claims abstract description 47
- 229910021446 cobalt carbonate Inorganic materials 0.000 title claims abstract description 23
- ZOTKGJBKKKVBJZ-UHFFFAOYSA-L cobalt(2+);carbonate Chemical compound [Co+2].[O-]C([O-])=O ZOTKGJBKKKVBJZ-UHFFFAOYSA-L 0.000 title claims abstract description 23
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims abstract description 21
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims abstract description 20
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims abstract description 20
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 20
- 239000000463 material Substances 0.000 claims abstract description 19
- 239000007788 liquid Substances 0.000 claims abstract description 15
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 14
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 14
- 230000005415 magnetization Effects 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 6
- 238000005086 pumping Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 230000002035 prolonged effect Effects 0.000 description 4
- 239000012295 chemical reaction liquid Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 229910000428 cobalt oxide Inorganic materials 0.000 description 2
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 2
- 239000003337 fertilizer Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 229910000361 cobalt sulfate Inorganic materials 0.000 description 1
- 229940044175 cobalt sulfate Drugs 0.000 description 1
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 description 1
- 239000003086 colorant Substances 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- GEMHFKXPOCTAIP-UHFFFAOYSA-N n,n-dimethyl-n'-phenylcarbamimidoyl chloride Chemical compound CN(C)C(Cl)=NC1=CC=CC=C1 GEMHFKXPOCTAIP-UHFFFAOYSA-N 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000007774 positive electrode material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011573 trace mineral Substances 0.000 description 1
- 235000013619 trace mineral Nutrition 0.000 description 1
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/06—Carbonates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Battery Electrode And Active Subsutance (AREA)
Abstract
The invention relates to a battery-grade cobalt carbonate crystal form reaction process, which comprises the following steps: introducing a cobalt chloride solution, an ammonium bicarbonate solution and an ammonia water solution into a microchannel reactor for uniform mixing reaction, allowing the mixed liquid after the sufficient reaction to automatically flow into a parallel high-efficiency pipeline mixer for positive and negative sufficient reaction, allowing the materials to rapidly and initially solidify into a crystal form, allowing the crystal form to gradually increase to a certain parameter through a magnetization reactor, allowing the crystal form to increase to a product standard crystal form through a crystal form stirring kettle, pumping into a centrifugal machine for centrifugal treatment, and conveying the centrifuged dry materials into a pyrometallurgical shop through a belt to prepare a finished product. The battery-grade cobalt carbonate crystal form reaction process provided by the invention can ensure that the materials are uniformly mixed, and has the advantages of high crystal form initial setting speed, high continuous feeding efficiency, no material loss and the like.
Description
Technical Field
The invention belongs to the technical field of cobalt carbonate preparation, and particularly relates to a battery-grade cobalt carbonate crystal form reaction process.
Background
The cobalt carbonate is mainly used for preparing cobalt chloride, cobalt sulfate, cobalt oxide, metal cobalt and cobalt naphthenate. Also can be used for preparing color-changing pigment, glass pigment, ceramic, feed microelement additive and microelement fertilizer. The cobalt oxide is used as a raw material for manufacturing a lithium battery positive electrode material. The ceramic industry is used as a colorant for cobalt salt manufacture and for the coloring of porcelain. Is used as a mineral dressing agent in the mining industry. The organic industry is used to make catalysts, camouflage coatings and chemical temperature indicators. Is used as trace element fertilizer in agriculture. As analytical reagents in analytical chemistry.
The existing traditional cobalt carbonate preparation process often has the problems of uneven material mixing, longer whole reaction period and serious material loss.
Disclosure of Invention
In order to solve the problems in the background art, the invention provides a battery-grade cobalt carbonate crystal form reaction process, which comprises the following steps:
the method comprises the steps of introducing a cobalt chloride solution, an ammonium bicarbonate solution and an ammonia water solution into a microchannel reactor for uniform mixing reaction, allowing the mixed liquid after the sufficient reaction to automatically flow into a high-efficiency pipeline mixer for positive and negative sufficient reaction, allowing the materials to rapidly and initially solidify into a crystal form, allowing the crystal form to gradually increase to a certain parameter through a magnetization reactor, allowing the crystal form to enter a crystal form stirring kettle, allowing the crystal form to increase to a product standard crystal form, pumping into a centrifuge for centrifugal treatment, and conveying the centrifuged dry materials into a pyrometallurgical workshop through a belt to prepare a finished product.
As a further illustration of the invention, the cobalt chloride solution is obtained by dissolving cobalt chloride in a proper amount of water, and the ammonium bicarbonate solution is obtained by dissolving ammonium bicarbonate in a proper amount of water.
As a further explanation of the invention, the cobalt chloride solution, the ammonium bicarbonate solution and the ammonia water solution are firstly pumped into a microchannel reactor simultaneously according to different proportions through a metering pump for uniform mixing reaction.
As a further description of the present invention, the microchannel reactor includes a first header pipe, a second header pipe, a third header pipe, a fourth header pipe, and a plurality of four-way branch pipes, where the first header pipe, the second header pipe, the third header pipe, and the fourth header pipe are arranged in parallel, and the four-way branch pipes are uniformly distributed along the length direction of the first header pipe, the second header pipe, the third header pipe, and the fourth header pipe, four ports of the four-way branch pipes are respectively communicated with the first header pipe, the second header pipe, the third header pipe, and the fourth header pipe, interfaces of the first header pipe, the second header pipe, and the fourth header pipe are liquid inlets of the microchannel reactor, and an interface of the third header pipe is a liquid outlet of the microchannel reactor.
As a further description of the present invention, the cobalt chloride solution, the ammonium bicarbonate solution, and the ammonia water solution are respectively introduced into the first header pipe, the second header pipe, and the fourth header pipe.
As a further explanation of the present invention, the high-efficiency pipeline mixer is a parallel high-efficiency pipeline mixer.
As a further description of the present invention, the reacted liquid flowing out of the microchannel reactor is respectively introduced into a plurality of high efficiency pipeline mixers for sufficient reaction, and then the reaction liquid flowing out of the high efficiency pipeline mixers is merged and introduced into the magnetization reactor.
Compared with the prior art, the invention has the following beneficial technical effects:
the battery-grade cobalt carbonate crystal form reaction process provided by the invention can ensure that the materials are uniformly mixed, and has the advantages of high crystal form initial setting speed, high continuous feeding efficiency, no material loss and the like.
The battery-grade cobalt carbonate crystal form reaction process provided by the invention adopts the microchannel reactor to carry out sufficient reaction between materials, not only greatly simplifies the process flow, but also greatly shortens the reaction time, improves the effect of the whole process flow, and more importantly, the microchannel reaction principle adopted by the invention can ensure that reactants are in sufficient contact with each other because the microchannel reactor divides the cobalt chloride solution, the ammonium bicarbonate solution and the ammonia water solution into a large number of fine branches and then forms mutual contact reaction by utilizing the mutual contact reaction after the two branches are crossed and converged, namely, the cobalt chloride solution, the ammonium bicarbonate solution and the ammonia water solution are divided into a large number of fine branches to form multiple multi-stage contact reactions, so that the contact time of the two solutions is fully prolonged, in addition, the arrangement of a large number of branch pipelines can also ensure that some branch pipelines are blocked due to the existence of reaction residues, the rest normal branch pipelines can still be utilized to continue the microchannel reaction, and the service life of the whole microchannel reactor is prolonged.
Drawings
FIG. 1 is a schematic diagram of a crystal reaction process of battery grade cobalt carbonate provided by the present invention;
fig. 2 is a schematic view of a microchannel reactor in a battery-grade cobalt carbonate crystal reaction process provided by the invention.
Description of the reference numerals
4-microchannel reactor; 401-a first manifold; 402-a first leg; 403-a second manifold; 404-a second manifold; 405-a third leg; 406-a third manifold; 407-a fourth manifold; 408-fourth branch.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are conventionally placed in use, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal", "vertical" and the like do not imply that the components are required to be absolutely horizontal or pendant, but rather may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless otherwise explicitly specified or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may, for example, be fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The technical solution of the present invention will be explained with reference to specific embodiments.
As shown in fig. 1, a battery-grade cobalt carbonate crystal form reaction process is provided, which comprises the following steps:
the method comprises the steps of introducing a cobalt chloride solution, an ammonium bicarbonate solution and an ammonia water solution into a microchannel reactor for uniform mixing reaction, allowing the mixed liquid after the sufficient reaction to automatically flow into a high-efficiency pipeline mixer for positive and negative sufficient reaction, allowing the materials to rapidly and initially solidify into a crystal form, allowing the crystal form to gradually increase to a certain parameter through a magnetization reactor, allowing the crystal form to enter a crystal form stirring kettle, allowing the crystal form to increase to a product standard crystal form, pumping into a centrifuge for centrifugal treatment, and conveying the centrifuged dry materials into a pyrometallurgical workshop through a belt to prepare a finished product.
The cobalt chloride solution is obtained by dissolving cobalt chloride in a proper amount of water, and the ammonium bicarbonate solution is obtained by dissolving ammonium bicarbonate in a proper amount of water.
In order to ensure that the three reaction raw materials are introduced into the microchannel reactor according to corresponding reaction proportions, the cobalt chloride solution, the ammonium bicarbonate solution and the ammonia water solution are firstly pumped into the microchannel reactor through a metering pump according to different proportions to be uniformly mixed and reacted.
Specifically, as shown in fig. 2, the microchannel reactor includes a first header pipe, a second header pipe, a third header pipe, and a plurality of four-way branch pipes (a four-way branch pipe is composed of three parts, i.e., a first branch pipe 402, a second branch pipe 404, a third branch pipe 405, and a fourth branch pipe 408), the first header pipe, the second header pipe, the third header pipe, and the fourth header pipe are arranged in parallel, the four-way branch pipes are uniformly distributed along the length direction of the first header pipe, the second header pipe, the third header pipe, and the fourth header pipe, four ports of the four-way branch pipe are respectively communicated with the first header pipe, the second header pipe, the third header pipe, and the fourth header pipe, that is, the first branch pipe 402 is communicated with the first header pipe 401, the second branch pipe 404 is communicated with the second header pipe 403, the third branch pipe 405 is communicated with the first header pipe 406, and the fourth branch pipe 408 is communicated with the fourth header pipe 407, the interfaces of the first header pipe, the second header pipe and the fourth header pipe are liquid inlets of the microchannel reactor 4, and the interface of the third header pipe is a liquid outlet of the microchannel reactor 4.
When the microchannel reactor is used, a cobalt chloride solution, an ammonium bicarbonate solution and an ammonia solution are respectively introduced into a first main pipe 401, a second main pipe 403 and a fourth main pipe 407, the third main pipe 406 is externally connected with a subsequent reaction treatment container, at this time, each reaction solution in the first main pipe 401, the second main pipe 403 and the fourth main pipe 407 is divided into countless fine branches and then introduced into different first branch pipes 402, second branch pipes 404 and fourth branch pipes 408, and the reaction solution in the communicated first branch pipes 402, second branch pipes 404 and fourth branch pipes 408 forms a contact reaction and then is merged into the third branch pipes 405, and finally is merged into the first main pipe 406 to be led out.
The battery-grade cobalt carbonate crystal form reaction process provided by the invention adopts the microchannel reactor to carry out sufficient reaction between materials, not only greatly simplifies the process flow, but also greatly shortens the reaction time, improves the effect of the whole process flow, and more importantly, the microchannel reaction principle adopted by the invention can ensure that reactants are in sufficient contact with each other because the microchannel reactor divides the cobalt chloride solution, the ammonium bicarbonate solution and the ammonia water solution into a large number of fine branches and then forms mutual contact reaction by utilizing the mutual contact reaction after the two branches are crossed and converged, namely, the cobalt chloride solution, the ammonium bicarbonate solution and the ammonia water solution are divided into a large number of fine branches to form multiple multi-stage contact reactions, so that the contact time of the two solutions is fully prolonged, in addition, the arrangement of a large number of branch pipelines can also ensure that some branch pipelines are blocked due to the existence of reaction residues, the rest normal branch pipelines can still be utilized to continue the microchannel reaction, and the service life of the whole microchannel reactor is prolonged.
The high-efficiency pipeline mixer is preferably a parallel high-efficiency pipeline mixer; respectively introducing reacted liquid flowing out of the microchannel reactor into a plurality of high-efficiency pipeline mixers for full reaction, converging reaction liquid flowing out of the high-efficiency pipeline mixers, and introducing the converged reaction liquid into the magnetization reactor; the use of the parallel high-efficiency pipeline mixer can divide the reacted liquid flowing out of the microchannel reactor into a plurality of strands of fluid solutions for full reaction, so that the materials can be rapidly and fully initially solidified into a crystal form.
The battery-grade cobalt carbonate crystal form reaction process provided by the invention can ensure that the materials are uniformly mixed, and has the advantages of high crystal form initial setting speed, high continuous feeding efficiency, no material loss and the like.
The embodiments given above are preferable examples for implementing the present invention, and the present invention is not limited to the above-described embodiments. Any non-essential addition and replacement made by the technical characteristics of the technical scheme of the invention by a person skilled in the art belong to the protection scope of the invention.
Claims (7)
1. A battery-grade cobalt carbonate crystal form reaction process is characterized by comprising the following steps:
the method comprises the steps of introducing a cobalt chloride solution, an ammonium bicarbonate solution and an ammonia water solution into a microchannel reactor for uniform mixing reaction, allowing the mixed liquid after the sufficient reaction to automatically flow into a high-efficiency pipeline mixer for positive and negative sufficient reaction, allowing the materials to rapidly and initially solidify into a crystal form, allowing the crystal form to gradually increase to a certain parameter through a magnetization reactor, allowing the crystal form to enter a crystal form stirring kettle, allowing the crystal form to increase to a product standard crystal form, pumping into a centrifuge for centrifugal treatment, and conveying the centrifuged dry materials into a pyrometallurgical workshop through a belt to prepare a finished product.
2. The battery-grade cobalt carbonate crystal form reaction process according to claim 1, wherein the cobalt chloride solution is obtained by dissolving cobalt chloride in a proper amount of water, and the ammonium bicarbonate solution is obtained by dissolving ammonium bicarbonate in a proper amount of water.
3. The battery-grade cobalt carbonate crystal form reaction process according to claim 1, wherein the cobalt chloride solution, the ammonium bicarbonate solution and the ammonia water solution are firstly pumped into a microchannel reactor through a metering pump according to different proportions to be uniformly mixed and reacted.
4. The battery-grade cobalt carbonate crystal form reaction process of claim 1, wherein the microchannel reactor comprises a first header pipe, a second header pipe, a third header pipe, a fourth header pipe and a plurality of four-way branch pipes, the first header pipe, the second header pipe, the third header pipe and the fourth header pipe are arranged in parallel, the four-way branch pipes are uniformly distributed along the length direction of the first header pipe, the second header pipe, the third header pipe and the fourth header pipe, four ports of the four-way branch pipes are respectively communicated with the first header pipe, the second header pipe, the third header pipe and the fourth header pipe, the interfaces of the first header pipe, the second header pipe and the fourth header pipe are liquid inlet ports of the microchannel reactor, and the interface of the third header pipe is a liquid outlet port of the microchannel reactor.
5. The battery-grade cobalt carbonate crystal form reaction process of claim 4, wherein the cobalt chloride solution, the ammonium bicarbonate solution and the ammonia water solution are respectively introduced into the first header pipe, the second header pipe and the fourth header pipe.
6. The battery-grade cobalt carbonate crystal form reaction process according to claim 1, wherein the high-efficiency pipeline mixer is a parallel high-efficiency pipeline mixer.
7. The battery-grade cobalt carbonate crystal form reaction process according to claim 6, wherein the reacted liquid flowing out of the microchannel reactor is respectively introduced into a plurality of high-efficiency pipeline mixers for full reaction, and then the reacted liquid flowing out of the high-efficiency pipeline mixers is merged and introduced into the magnetization reactor.
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| CN106882833A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of method that high-purity basic copper carbonate is prepared in micro passage reaction |
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| CN112197518A (en) * | 2020-09-09 | 2021-01-08 | 厦门钨业股份有限公司 | System and method for continuously drying battery-grade cobalt carbonate |
| CN112573703A (en) * | 2020-12-09 | 2021-03-30 | 陕西金禹科技发展有限公司 | Method and device for treating arsenic-containing wastewater through microchannel reaction |
-
2021
- 2021-05-19 CN CN202110550888.6A patent/CN113213551B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106549153A (en) * | 2015-09-16 | 2017-03-29 | 中国科学院大连化学物理研究所 | A kind of hollow hexagonal shape hydroxy cobalt oxide nano material and preparation method thereof |
| CN106882833A (en) * | 2015-12-15 | 2017-06-23 | 中国科学院大连化学物理研究所 | A kind of method that high-purity basic copper carbonate is prepared in micro passage reaction |
| CN107834046A (en) * | 2017-11-07 | 2018-03-23 | 衢州市鼎盛化工科技有限公司 | The preparation method and its consersion unit of ternary material precursor |
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