CN111498913A - Preparation method and application of cobaltosic oxide nanoparticles - Google Patents
Preparation method and application of cobaltosic oxide nanoparticles Download PDFInfo
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- CN111498913A CN111498913A CN202010400268.XA CN202010400268A CN111498913A CN 111498913 A CN111498913 A CN 111498913A CN 202010400268 A CN202010400268 A CN 202010400268A CN 111498913 A CN111498913 A CN 111498913A
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- cobaltosic oxide
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- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(2+);cobalt(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000002105 nanoparticle Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 claims abstract description 46
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000004310 lactic acid Substances 0.000 claims abstract description 23
- 235000014655 lactic acid Nutrition 0.000 claims abstract description 23
- 238000006243 chemical reaction Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000004471 Glycine Substances 0.000 claims abstract description 14
- 150000001868 cobalt Chemical class 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 12
- 239000012265 solid product Substances 0.000 claims abstract description 12
- 238000001354 calcination Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 9
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 9
- 150000001720 carbohydrates Chemical class 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 7
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 230000008020 evaporation Effects 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000005303 weighing Methods 0.000 claims abstract description 6
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 4
- 239000000203 mixture Substances 0.000 description 9
- 239000003054 catalyst Substances 0.000 description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- SRBFZHDQGSBBOR-IOVATXLUSA-N D-xylopyranose Chemical compound O[C@@H]1COC(O)[C@H](O)[C@H]1O SRBFZHDQGSBBOR-IOVATXLUSA-N 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 229920002678 cellulose Polymers 0.000 description 5
- 239000001913 cellulose Substances 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 3
- 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 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- PYMYPHUHKUWMLA-UHFFFAOYSA-N arabinose Natural products OCC(O)C(O)C(O)C=O PYMYPHUHKUWMLA-UHFFFAOYSA-N 0.000 description 3
- SRBFZHDQGSBBOR-UHFFFAOYSA-N beta-D-Pyranose-Lyxose Natural products OC1COC(O)C(O)C1O SRBFZHDQGSBBOR-UHFFFAOYSA-N 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 238000007789 sealing Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229920002488 Hemicellulose Polymers 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- NBBJYMSMWIIQGU-UHFFFAOYSA-N Propionic aldehyde Chemical compound CCC=O NBBJYMSMWIIQGU-UHFFFAOYSA-N 0.000 description 2
- 229920002522 Wood fibre Polymers 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- HYBBIBNJHNGZAN-UHFFFAOYSA-N furfural Chemical compound O=CC1=CC=CO1 HYBBIBNJHNGZAN-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012827 research and development Methods 0.000 description 2
- 239000002025 wood fiber Substances 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- NOEGNKMFWQHSLB-UHFFFAOYSA-N 5-hydroxymethylfurfural Chemical compound OCC1=CC=C(C=O)O1 NOEGNKMFWQHSLB-UHFFFAOYSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 235000011054 acetic acid Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 229910001413 alkali metal ion Inorganic materials 0.000 description 1
- 238000010352 biotechnological method Methods 0.000 description 1
- ZTQSAGDEMFDKMZ-UHFFFAOYSA-N butyric aldehyde Natural products CCCC=O ZTQSAGDEMFDKMZ-UHFFFAOYSA-N 0.000 description 1
- 235000014633 carbohydrates Nutrition 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012084 conversion product Substances 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 235000019253 formic acid Nutrition 0.000 description 1
- RJGBSYZFOCAGQY-UHFFFAOYSA-N hydroxymethylfurfural Natural products COC1=CC=C(C=O)O1 RJGBSYZFOCAGQY-UHFFFAOYSA-N 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- TWNIBLMWSKIRAT-VFUOTHLCSA-N levoglucosan Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@H]2CO[C@@H]1O2 TWNIBLMWSKIRAT-VFUOTHLCSA-N 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 150000002772 monosaccharides Chemical class 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 239000011949 solid catalyst Substances 0.000 description 1
- 235000000346 sugar Nutrition 0.000 description 1
- 150000008163 sugars Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910001428 transition metal ion Inorganic materials 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G51/00—Compounds of cobalt
- C01G51/04—Oxides; Hydroxides
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/75—Cobalt
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a preparation method and application of cobaltosic oxide nanoparticles. The method comprises the following steps: (1) respectively weighing a certain amount of glycine and cobalt salt, adding the glycine and cobalt salt into a beaker filled with deionized water, and stirring to dissolve the glycine and cobalt salt; (2) heating the mixed solution obtained in the step (1), wherein the mixed solution becomes sticky along with the evaporation of water, and continuously heating until the liquid is violently combusted to generate a large amount of gas and a foamy solid product; (3) and (3) placing the foamy solid product obtained in the step (2) into a muffle furnace, and calcining to obtain the cobaltosic oxide nano-particles. The cobaltosic oxide nano-particles obtained by the invention have higher activity in catalyzing the hydrothermal conversion of saccharides into lactic acid.
Description
Technical Field
The invention relates to a preparation method and application of cobaltosic oxide nanoparticles, and belongs to the field of catalyst preparation and catalysis research.
Background
In recent years, nanoscience and technology has attracted much attention in many fields such as catalysis, medicine, environmental protection, energy, and the like, and has become one of the most active fields of international research and development. The nano particles have small size and large specific surface area, the bonding state and the electronic state of the surface are different from those of the interior of the nano particles, and the coordination of surface atoms is incomplete, so that the active sites on the surface of the nano particles are increased, and the nano particles have basic conditions as catalysts. At present, the catalytic reaction by using the nano particles can directly use the nano particles such as silver, aluminum oxide, iron oxide and the like as catalysts in organic synthesis reaction, so that the reaction efficiency can be greatly improved; the catalytic reaction also shows selectivity, for example, the oxidation reaction of propionaldehyde by using silicon carrier nickel catalyst shows that when the nickel grain size is below 5nm, the selectivity is sharply changed, the aldehyde decomposition is controlled, and the selectivity of producing alcohol is sharply increased.
With the concern of global energy, the instability of fossil resources and the greenhouse effect, people are turning to the research road of renewable resources more and more. Lignocellulosic feedstocks are receiving increasing attention from experts in various countries as one of the most abundant renewable resources in the world. The wood fiber raw material mainly comprises three major components of cellulose, hemicellulose and lignin, wherein the cellulose and the hemicellulose can be hydrothermally converted into small molecule chemicals, such as monosaccharide, formic acid, acetic acid, lactic acid, furfural, hydroxymethyl furfural and the like. Lactic acid is a chemical product which can be prepared from biomass raw materials, is a platform compound with high potential and multiple functions, and is widely applied to industries such as food, medicine, cosmetics and the like. Lactic acid can be produced by fermentation of various sources of sugars with lactic acid bacteria. However, biotechnological methods show some disadvantages, such as: lower time/space yields, higher enzyme costs, more saline waste water produced and difficult purification, management requirements and microbial pool supervision. More and more people are turning to the production of lactic acid by chemical conversion of biomass.
Under the condition of no catalysis, the distribution range of the hydrothermal conversion products of the lignocellulose raw material is wide, the yield of the lactic acid is low, the later separation and purification cost is high, and the economical efficiency of the hydrothermal conversion of the lignocellulose into the lactic acid is poor. The addition of a proper catalyst can obviously improve the reaction rate of the hydrothermal conversion of the wood fiber raw material into the lactic acid and obviously change the selectivity of the reaction, and the selection of the catalyst has a decisive effect on the economy of realizing the conversion and utilization of the biomass. When homogeneous acid, alkali and transition metal ions are used for catalysis, although the catalytic effect is obvious, the catalyst is difficult to recover and is easy to cause environmental pollution. More and more researchers have therefore focused on solid catalysts for the catalytic conversion of lignocellulose. The metal oxide has the advantages of high stability, easy preparation and the like, and is often used as a carrier of active species such as noble metals, however, the yield of the transition metal oxide is not ideal in the aspect of catalyzing saccharides to prepare lactic acid. Therefore, research and development of a catalyst capable of efficiently catalyzing saccharides to prepare lactic acid is of great significance for the production of lactic acid.
Disclosure of Invention
The invention develops a preparation method of cobaltosic oxide nano particles and applies the cobaltosic oxide nano particles to catalyzing carbohydrate hydrothermal conversion to prepare lactic acid. The catalyst has high activity, and can convert various saccharides into lactic acid with high selectivity.
The technical scheme of the invention is as follows:
a preparation method of cobaltosic oxide nanoparticles comprises the following steps:
(1) respectively weighing a certain amount of glycine and cobalt salt, adding the glycine and cobalt salt into a beaker filled with deionized water, and stirring to dissolve the glycine and cobalt salt;
(2) heating the mixed solution obtained in the step (1), wherein the mixed solution becomes sticky along with the evaporation of water, and continuously heating until the liquid is violently combusted to generate a large amount of gas and a foamy solid product;
(3) and (3) placing the foamy solid product obtained in the step (2) into a muffle furnace, and calcining to obtain the cobaltosic oxide nano-particles. The molar ratio of the glycine to the cobalt salt in the step (1) is 1: 1-4: 1.
And (3) the cobalt salt in the step (2) is cobalt nitrate.
In the step (3), the calcining temperature is 600-800 ℃, and the calcining time is 1-3 h.
The invention also comprises the application of the cobaltosic oxide nanoparticles in catalyzing the hydrothermal conversion of saccharides into lactic acid.
The invention has the advantages that:
(1) the preparation method of the cobaltosic oxide nano-particles is simple, simple and convenient to operate, uniform in particle dispersion and easy to realize large-scale production.
(2) The cobaltosic oxide nano-particles prepared by the method can obtain high-yield lactic acid in the process of catalyzing hydro-thermal conversion of saccharides.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1:
(1) 0.05mol of glycine and 0.05mol of Co (NO) were weighed out3)2·6H2O, then simultaneously adding the mixture into a beaker filled with deionized water of 20m L, and stirring the mixture to dissolve the mixture;
(2) heating the mixed solution obtained in the step (1), wherein the mixed solution becomes sticky along with the evaporation of water, and continuously heating the liquid for violent combustion to generate a large amount of gas and a foamy solid product;
(3) placing the foamy solid product obtained in the step (2) in a muffle furnace, heating to 600 ℃, and calcining for 2h to obtain cobaltosic oxide nanoparticles;
(4) weighing 1.0g of glucose and 0.05g of cobaltosic oxide nanoparticles, placing the glucose and the cobaltosic oxide nanoparticles in a high-temperature high-pressure reaction kettle, adding 50m L of deionized water, sealing the kettle body, introducing nitrogen to replace air in the kettle, heating the kettle body to 220 ℃ to react for 10min, measuring the lactic acid content in liquid by using a high performance liquid chromatograph after the reaction is finished, and calculating the molar yield of the lactic acid to be 46.1 mol% (relative to the molar amount of the glucose).
Example 2:
(1) 0.10mol of glycine and 0.05mol of Co (NO) were weighed out3)2·6H2O, then simultaneously adding the mixture into a beaker filled with deionized water of 20m L, and stirring the mixture to dissolve the mixture;
(2) heating the mixed solution obtained in the step (1), wherein the mixed solution becomes sticky along with the evaporation of water, and continuously heating the liquid for violent combustion to generate a large amount of gas and a foamy solid product;
(3) and (3) placing the foamy solid product obtained in the step (2) into a muffle furnace, heating to 800 ℃, and calcining for 2h to obtain the cobaltosic oxide nano-particles.
(4) Weighing 1.0g of xylose and 0.05g of cobaltosic oxide nanoparticles, placing the xylose and the cobaltosic oxide nanoparticles in a high-temperature high-pressure reaction kettle, adding 50m L of deionized water, sealing the kettle body, introducing nitrogen to replace air in the kettle, heating the kettle body to 200 ℃, reacting for 10min, measuring the lactic acid content in liquid by using a high performance liquid chromatograph after the reaction is finished, and calculating the lactic acid molar yield to be 72.1 mol% (relative to the molar amount of the xylose).
Example 3:
(1) 0.20mol of glycine and 0.05mol of Co (NO) were weighed out3)2·6H2O, then simultaneously adding the mixture into a beaker filled with deionized water of 20m L, and stirring the mixture to dissolve the mixture;
(2) heating the mixed solution obtained in the step (1), wherein the mixed solution becomes sticky along with the evaporation of water, and continuously heating the liquid for violent combustion to generate a large amount of gas and a foamy solid product;
(3) and (3) placing the foamy solid product obtained in the step (2) into a muffle furnace, heating to 700 ℃, and calcining for 2h to obtain the cobaltosic oxide nano-particles.
(4) Weighing 1.0g of cellulose and 0.05g of cobaltosic oxide nanoparticles, placing the cellulose and the cobaltosic oxide nanoparticles in a high-temperature high-pressure reaction kettle, adding 50m L of deionized water, sealing the kettle body, introducing nitrogen to replace air in the kettle, heating the kettle body to 240 ℃, reacting for 10min, measuring the lactic acid content in liquid by using a high performance liquid chromatograph after the reaction is finished, and calculating the molar yield of the lactic acid to be 47.5 mol% (relative to the molar amount of a cellulose anhydroglucose unit).
The above embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and the scope of the present invention is defined by the claims. Various modifications and equivalents may be made by those skilled in the art within the spirit and scope of the present invention, and such modifications and equivalents should also be considered as falling within the scope of the present invention.
Claims (5)
1. A preparation method of cobaltosic oxide nanoparticles is characterized in that the preparation method of the cobaltosic oxide nanoparticles at least comprises the following steps:
(1) respectively weighing a certain amount of glycine and cobalt salt, adding the glycine and cobalt salt into a beaker filled with deionized water, and stirring to dissolve the glycine and cobalt salt;
(2) heating the mixed solution obtained in the step (1), wherein the mixed solution becomes sticky along with the evaporation of water, and continuously heating until the liquid is violently combusted to generate a large amount of gas and a foamy solid product;
(3) and (3) placing the foamy solid product obtained in the step (2) into a muffle furnace, and calcining to obtain the cobaltosic oxide nano-particles.
2. The method for preparing cobaltosic oxide nanoparticles as claimed in claim 1, wherein the molar ratio of glycine to cobalt salt in step (1) is 1:1 to 4: 1.
3. The method for preparing cobaltosic oxide nanoparticles as claimed in claim 1, wherein the cobalt salt in step (1) is cobalt nitrate.
4. The method for preparing cobaltosic oxide nanoparticles as claimed in claim 1, wherein the calcination temperature in step (3) is 600-800 ℃ and the calcination time is 1-3 h.
5. The method for preparing cobaltosic oxide nanoparticles according to claim 1, wherein the prepared cobaltosic oxide nanoparticles are used for catalyzing saccharides to prepare lactic acid through hydrothermal conversion.
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| CN202010400268.XA CN111498913A (en) | 2020-05-12 | 2020-05-12 | Preparation method and application of cobaltosic oxide nanoparticles |
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2020
- 2020-05-12 CN CN202010400268.XA patent/CN111498913A/en active Pending
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| US20050142058A1 (en) * | 2003-12-30 | 2005-06-30 | Industrial Technology Research Institute | Low temperature process for preparing tricobalt tetraoxide |
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