CN114230456A - Synthesis process of cobalt acetate - Google Patents
Synthesis process of cobalt acetate Download PDFInfo
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- CN114230456A CN114230456A CN202111596731.3A CN202111596731A CN114230456A CN 114230456 A CN114230456 A CN 114230456A CN 202111596731 A CN202111596731 A CN 202111596731A CN 114230456 A CN114230456 A CN 114230456A
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- 229940011182 cobalt acetate Drugs 0.000 title claims abstract description 37
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 22
- 230000015572 biosynthetic process Effects 0.000 title claims abstract description 16
- 238000003786 synthesis reaction Methods 0.000 title claims abstract description 16
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 63
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 52
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000007864 aqueous solution Substances 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000001816 cooling Methods 0.000 claims abstract description 13
- ZJRWDIJRKKXMNW-UHFFFAOYSA-N carbonic acid;cobalt Chemical compound [Co].OC(O)=O ZJRWDIJRKKXMNW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 238000007873 sieving Methods 0.000 claims abstract description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000001257 hydrogen Substances 0.000 claims abstract description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 5
- 238000002425 crystallisation Methods 0.000 claims abstract description 3
- 230000008025 crystallization Effects 0.000 claims abstract description 3
- 230000008020 evaporation Effects 0.000 claims abstract 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 24
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 16
- 239000004094 surface-active agent Substances 0.000 claims description 16
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 12
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 238000007792 addition Methods 0.000 claims description 12
- OZAIFHULBGXAKX-UHFFFAOYSA-N 2-(2-cyanopropan-2-yldiazenyl)-2-methylpropanenitrile Chemical compound N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 claims description 10
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 10
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 10
- 239000001099 ammonium carbonate Substances 0.000 claims description 10
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 9
- GMSCBRSQMRDRCD-UHFFFAOYSA-N dodecyl 2-methylprop-2-enoate Chemical compound CCCCCCCCCCCCOC(=O)C(C)=C GMSCBRSQMRDRCD-UHFFFAOYSA-N 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N hexane Substances CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 229910017052 cobalt Inorganic materials 0.000 abstract description 8
- 239000010941 cobalt Substances 0.000 abstract description 8
- 239000002184 metal Substances 0.000 abstract description 5
- 229910052751 metal Inorganic materials 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- 238000007086 side reaction Methods 0.000 abstract description 2
- 239000007800 oxidant agent Substances 0.000 abstract 1
- 230000001590 oxidative effect Effects 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 6
- 239000012535 impurity Substances 0.000 description 6
- 229910052759 nickel Inorganic materials 0.000 description 5
- 239000013078 crystal Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/41—Preparation of salts of carboxylic acids
- C07C51/412—Preparation of salts of carboxylic acids by conversion of the acids, their salts, esters or anhydrides with the same carboxylic acid part
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a synthesis process of cobalt acetate, belonging to the technical field of catalyst synthesis and comprising the following steps: reducing the cobalt carbonate powder in a hydrogen atmosphere at 480-500 ℃ for 2h to obtain cobalt powder; adding acetic acid and 50% water into a reaction kettle, adding cobalt powder in three batches, adding hydrogen peroxide and residual water after the addition is finished, controlling the reaction temperature to be 60-90 ℃ and the pressure to be 0.3-0.4MPa, staying for 3-6min, filtering to obtain a cobalt acetate aqueous solution, and performing evaporation concentration, cooling crystallization and sieving to obtain cobalt acetate. Preparing cobalt acetate by directly reacting metal cobalt with acetic acid and hydrogen peroxide; the metal cobalt contact reaction has the advantages of low mass transfer speed and aggravated side reaction, the reaction contact efficiency is improved through the prepared cobalt powder, the acetic acid is added firstly, then the oxidant is added, the utilization rate of the hydrogen peroxide is improved, and the consumption of raw materials is reduced.
Description
Technical Field
The invention belongs to the technical field of catalyst synthesis, and particularly relates to a synthesis process of cobalt acetate.
Background
Cobalt acetate is the most important catalyst in the preparation of terephthalic acid by liquid-phase oxidation of paraxylene, and the early used technology in the synthesis of cobalt acetate generally adopts a nitric acid method to produce cobalt acetate crystals, and the cobalt acetate crystals are dissolved when used. The method is improved, namely nitric acid and acetic acid mixed acid is adopted to react with metal cobalt, and the cobalt acetate crystal is produced through concentration, crystallization, impurity removal and the like, but the process still has many defects, such as environmental pollution, low reaction efficiency, large consumption of raw materials and energy, reduced activity of cobalt in the later stage of reaction, high impurity content in the product and the like.
Disclosure of Invention
In order to solve the technical problems mentioned in the background technology, the invention provides a synthesis process of cobalt acetate.
The purpose of the invention can be realized by the following technical scheme:
a synthesis process of cobalt acetate comprises the following steps:
adding acetic acid and 50% water into a reaction kettle, adding cobalt powder in three batches, adding hydrogen peroxide and residual water after the addition is finished, controlling the reaction temperature to be 60-90 ℃ and the pressure to be 0.3-0.4MPa, staying for 3-6min, filtering, adding a small amount of hydrogen peroxide to remove impurities and activate to obtain a cobalt acetate aqueous solution, and then evaporating, concentrating, cooling, crystallizing and sieving to obtain the cobalt acetate.
Further, the molar ratio of the acetic acid, the hydrogen peroxide and the water is 1: 1: 20-30.
Further, the dosage ratio of the added cobalt powder in three batches is 1: 2: 3; the interval time is 1 min; the molar ratio of the total amount of cobalt powder to the amount of acetic acid is 1: 2-2.1.
Further, the cobalt powder is prepared by the following steps:
step S11, adding an aqueous solution of cobalt chloride and an aqueous solution of ammonium bicarbonate into a high-pressure reaction kettle, then adding a surfactant, stirring for 30min after adding, then heating to 200 ℃, keeping the temperature for 12h, reducing the pressure to normal pressure, cooling to room temperature, filtering, washing a filter cake with distilled water and absolute ethyl alcohol, and after washing, drying for 12h at 80 ℃ to obtain cobalt carbonate powder;
step S12, reducing the cobalt carbonate powder in a hydrogen atmosphere at 480-500 ℃ for 2 h; and introducing nitrogen to passivate the cobalt powder in the cooling stage.
Further, in step S11, the mass fraction of the cobalt chloride aqueous solution is 10% and the mass fraction of the ammonium bicarbonate aqueous solution is 30%; the molar ratio of the cobalt chloride to the ammonium bicarbonate is 1: 3; the volume ratio of the cobalt chloride aqueous solution to the surfactant is 1: 3.
further, the surfactant is prepared by the following steps:
mixing azodiisobutyronitrile, toluene, N-vinyl pyrrolidone and lauryl methacrylate, stirring and reacting for 24 hours at the temperature of 70 ℃ under the protection of nitrogen, adding methanol acidified by hydrochloric acid after the reaction is finished, stopping the reaction, mixing the obtained reaction liquid with N-hexane, filtering, drying in vacuum at 40 ℃ to constant weight, and mixing with ethylene glycol according to the proportion of 1 g: 100mL of the surfactant was mixed to obtain a surfactant. The N-vinyl pyrrolidone is matched with lauryl methacrylate, and the addition of the surfactant enables the reaction to have better dispersity and to be easily removed in the post-treatment process.
Further, azobisisobutyronitrile, toluene, N-vinyl pyrrolidone and lauryl methacrylate were used in a ratio of 50 mg: 20mL of: 1-2 g: 0.5 g.
The invention has the beneficial effects that:
in the hydrogen peroxide process, the utilization rate of hydrogen peroxide is critical to the reaction yield; in the traditional process, the cobalt acetate is prepared by directly reacting the metal cobalt with acetic acid and hydrogen peroxide, the metal cobalt is in contact reaction, the mass transfer speed is low, and the side reaction is intensified.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
Preparing cobalt powder:
mixing azodiisobutyronitrile, toluene, N-vinyl pyrrolidone and lauryl methacrylate, stirring and reacting for 24 hours at the temperature of 70 ℃ under the protection of nitrogen, adding methanol acidified by hydrochloric acid after the reaction is finished, stopping the reaction, mixing the obtained reaction liquid with N-hexane, filtering, drying in vacuum at 40 ℃ to constant weight, and mixing with ethylene glycol according to the proportion of 1 g: mixing 100mL to obtain a surfactant; wherein the dosage ratio of azodiisobutyronitrile, toluene, N-vinyl pyrrolidone and lauryl methacrylate is 50 mg: 20mL of: 1 g: 0.5 g;
adding a cobalt chloride aqueous solution and an ammonia hydrogen carbonate aqueous solution into a high-pressure reaction kettle, then adding a surfactant, stirring for 30min after the addition is finished, and then heating to 200 ℃ under the pressure of 3 MPa; keeping the temperature for 12 hours, reducing the pressure to normal pressure, cooling to room temperature, filtering, washing a filter cake with distilled water and absolute ethyl alcohol, and drying at 80 ℃ for 12 hours after washing to obtain cobalt carbonate powder; wherein the mass fraction of the cobalt chloride aqueous solution is 10 percent, and the mass fraction of the ammonium bicarbonate aqueous solution is 30 percent; the molar ratio of the cobalt chloride to the ammonium bicarbonate is 1: 3; the volume ratio of the cobalt chloride aqueous solution to the surfactant is 1: 3.
reducing cobalt carbonate powder in a hydrogen atmosphere at 480 ℃ for 2 h; and introducing nitrogen to passivate the cobalt powder in the cooling stage.
Example 2
Preparing cobalt powder:
mixing azodiisobutyronitrile, toluene, N-vinyl pyrrolidone and lauryl methacrylate, stirring and reacting for 24 hours at the temperature of 70 ℃ under the protection of nitrogen, adding methanol acidified by hydrochloric acid after the reaction is finished, stopping the reaction, mixing the obtained reaction liquid with N-hexane, filtering, drying in vacuum at 40 ℃ to constant weight, and mixing with ethylene glycol according to the proportion of 1 g: mixing 100mL to obtain a surfactant; wherein the dosage ratio of azodiisobutyronitrile, toluene, N-vinyl pyrrolidone and lauryl methacrylate is 50 mg: 20mL of: 1 g: 0.5 g;
adding a cobalt chloride aqueous solution and an ammonia hydrogen carbonate aqueous solution into a high-pressure reaction kettle, then adding a surfactant, stirring for 30min after the addition is finished, and then heating to 200 ℃ under the pressure of 3 MPa; keeping the temperature for 12 hours, reducing the pressure to normal pressure, cooling to room temperature, filtering, washing a filter cake with distilled water and absolute ethyl alcohol, and drying at 80 ℃ for 12 hours after washing to obtain cobalt carbonate powder; wherein the mass fraction of the cobalt chloride aqueous solution is 10 percent, and the mass fraction of the ammonium bicarbonate aqueous solution is 30 percent; the molar ratio of the cobalt chloride to the ammonium bicarbonate is 1: 3; the volume ratio of the cobalt chloride aqueous solution to the surfactant is 1: 3.
reducing the cobalt carbonate powder in a hydrogen atmosphere at the reduction temperature of 500 ℃ for 2 h; and introducing nitrogen to passivate the cobalt powder in the cooling stage.
Example 3
A synthesis process of cobalt acetate comprises the following steps:
adding acetic acid and 50% of water into a reaction kettle, adding the cobalt powder prepared in the embodiment 1 in three batches, adding hydrogen peroxide and residual water after the addition is finished, controlling the reaction temperature to be 60 ℃ and the pressure to be 0.3MPa, staying for 3min, filtering, adding a small amount of hydrogen peroxide to remove impurities and activate to obtain a cobalt acetate aqueous solution, and then evaporating, concentrating, cooling, crystallizing and sieving to obtain cobalt acetate. Wherein the molar ratio of the acetic acid to the hydrogen peroxide to the water is 1: 1: 20. the dosage ratio of the added cobalt powder in three batches is 1: 2: 3; the interval time is 1 min; the molar ratio of the total amount of cobalt powder to the amount of acetic acid is 1: 2. the cobalt acetate aqueous solution does not contain nickel, and the utilization rate of the hydrogen peroxide is 100 percent.
Example 4
A synthesis process of cobalt acetate comprises the following steps:
adding acetic acid and 50% of water into a reaction kettle, adding the cobalt powder prepared in the example 1 in three batches, adding hydrogen peroxide and residual water after the addition is finished, controlling the reaction temperature to be 70 ℃ and the pressure to be 0.3MPa, staying for 5min, filtering, adding a small amount of hydrogen peroxide to remove impurities and activate to obtain a cobalt acetate aqueous solution, and then evaporating, concentrating, cooling, crystallizing and sieving to obtain cobalt acetate. Wherein the molar ratio of the acetic acid to the hydrogen peroxide to the water is 1: 1: 25. the dosage ratio of the added cobalt powder in three batches is 1: 2: 3; the interval time is 1 min; the molar ratio of the total amount of cobalt powder to the amount of acetic acid is 1: 2. the cobalt acetate aqueous solution does not contain nickel; the utilization rate of the hydrogen peroxide is 100 percent
Example 5
A synthesis process of cobalt acetate comprises the following steps:
adding acetic acid and 50% of water into a reaction kettle, adding the cobalt powder prepared in the embodiment 1 in three batches, adding hydrogen peroxide and residual water after the addition is finished, controlling the reaction temperature to be 90 ℃ and the pressure to be 0.4MPa, staying for 6min, filtering, adding a small amount of hydrogen peroxide to remove impurities and activate to obtain a cobalt acetate aqueous solution, and then evaporating, concentrating, cooling, crystallizing and sieving to obtain cobalt acetate. Wherein the molar ratio of the acetic acid to the hydrogen peroxide to the water is 1: 1: 30. the dosage ratio of the added cobalt powder in three batches is 1: 2: 3; the interval time is 1 min; the molar ratio of the total amount of cobalt powder to the amount of acetic acid is 1: 2.1. the cobalt acetate aqueous solution does not contain nickel; the utilization of hydrogen peroxide was 100%.
Comparative example 1
The cobalt powder in example 4 was changed to industrial cobalt without any treatment and batch addition, and the remaining raw materials and preparation process remained unchanged. The nickel content in the cobalt acetate aqueous solution meets the national standard GB 1290-77; the utilization rate of the hydrogen peroxide is 95 percent
Comparative example 2
The cobalt powder in the example 4 is changed into industrial cobalt, no treatment is carried out, no batch addition is carried out, and the molar ratio of the acetic acid, the hydrogen peroxide and the water is 1: 1: 10, the rest raw materials and the preparation process are kept unchanged. The nickel content in the cobalt acetate aqueous solution meets the national standard GB1290-77, and the utilization rate of the hydrogen peroxide is 93 percent.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing is illustrative and explanatory only and is not intended to be exhaustive or to limit the invention to the precise embodiments described, and various modifications, additions, and substitutions may be made by those skilled in the art without departing from the scope of the invention or exceeding the scope of the claims.
Claims (7)
1. The synthesis process of cobalt acetate is characterized by comprising the following steps:
reducing the cobalt carbonate powder in a hydrogen atmosphere at 480-500 ℃ for 2h to obtain cobalt powder;
adding acetic acid and 50% water into a reaction kettle, adding cobalt powder in three batches, adding hydrogen peroxide and residual water after the addition is finished, controlling the reaction temperature to be 60-90 ℃ and the pressure to be 0.3-0.4MPa, staying for 3-6min, filtering to obtain a cobalt acetate aqueous solution, and performing evaporation concentration, cooling crystallization and sieving to obtain cobalt acetate.
2. The synthesis process of cobalt acetate according to claim 1, wherein the molar ratio of the acetic acid, the hydrogen peroxide and the water is 1: 1: 20-30.
3. The synthesis process of cobalt acetate according to claim 1, wherein the dosage ratio of the added cobalt powder in three batches is 1: 2: 3; the interval time is 1 min; the molar ratio of the total amount of cobalt powder to the amount of acetic acid is 1: 2-2.1.
4. The process of claim 1, wherein the cobalt carbonate powder is prepared by the steps of:
adding an aqueous solution of cobalt chloride and an aqueous solution of ammonium bicarbonate into a reaction kettle, then adding a surfactant, stirring for 30min after the addition is finished, then heating to 200 ℃, preserving heat for 12h, cooling to room temperature, filtering, washing a filter cake with distilled water and absolute ethyl alcohol, and drying for 12h at 80 ℃ after the washing is finished to obtain cobalt carbonate powder.
5. The synthesis process of cobalt acetate according to claim 4, characterized in that the mass fraction of the cobalt chloride aqueous solution is 10% and the mass fraction of the ammonium bicarbonate aqueous solution is 30%; the molar ratio of the cobalt chloride to the ammonium bicarbonate is 1: 3; the volume ratio of the cobalt chloride aqueous solution to the surfactant is 1: 3.
6. the process of claim 4, wherein the surfactant is prepared by the steps of:
mixing azodiisobutyronitrile, toluene, N-vinyl pyrrolidone and lauryl methacrylate, stirring and reacting for 24 hours at the temperature of 70 ℃ under the protection of nitrogen, mixing the obtained reaction liquid with N-hexane after the reaction is finished, filtering, drying in vacuum at 40 ℃ to constant weight, and then mixing with ethylene glycol to obtain the surfactant.
7. The process of claim 6, wherein the ratio of the amounts of azobisisobutyronitrile, toluene, N-vinyl pyrrolidone and lauryl methacrylate is 50 mg: 20mL of: 1-2 g: 0.5 g.
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| CN202111596731.3A CN114230456A (en) | 2021-12-24 | 2021-12-24 | Synthesis process of cobalt acetate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092343A (en) * | 2007-07-19 | 2007-12-26 | 江苏大康实业有限公司 | Method for preparing cobalt acetate |
| CN103071807A (en) * | 2012-11-21 | 2013-05-01 | 四川大学 | Preparation method of ultra-fine spherical cobalt powder |
| CN106799499A (en) * | 2016-11-28 | 2017-06-06 | 格林美股份有限公司 | A kind of preparation method of spherical cobalt powder |
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2021
- 2021-12-24 CN CN202111596731.3A patent/CN114230456A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101092343A (en) * | 2007-07-19 | 2007-12-26 | 江苏大康实业有限公司 | Method for preparing cobalt acetate |
| CN103071807A (en) * | 2012-11-21 | 2013-05-01 | 四川大学 | Preparation method of ultra-fine spherical cobalt powder |
| CN106799499A (en) * | 2016-11-28 | 2017-06-06 | 格林美股份有限公司 | A kind of preparation method of spherical cobalt powder |
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