CN115010594A - Preparation method of charcoal-shaped manganese oxalate crystals - Google Patents
Preparation method of charcoal-shaped manganese oxalate crystals Download PDFInfo
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- CN115010594A CN115010594A CN202210035399.1A CN202210035399A CN115010594A CN 115010594 A CN115010594 A CN 115010594A CN 202210035399 A CN202210035399 A CN 202210035399A CN 115010594 A CN115010594 A CN 115010594A
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- manganese
- oxalate
- charcoal
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- crystals
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- RGVLTEMOWXGQOS-UHFFFAOYSA-L manganese(2+);oxalate Chemical compound [Mn+2].[O-]C(=O)C([O-])=O RGVLTEMOWXGQOS-UHFFFAOYSA-L 0.000 title claims abstract description 29
- 239000013078 crystal Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 19
- 239000003610 charcoal Substances 0.000 claims abstract description 18
- 238000003756 stirring Methods 0.000 claims abstract description 16
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000001035 drying Methods 0.000 claims abstract description 11
- 150000002696 manganese Chemical class 0.000 claims abstract description 11
- 229940039748 oxalate Drugs 0.000 claims abstract description 11
- 230000032683 aging Effects 0.000 claims abstract description 9
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 9
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 claims abstract description 7
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical group [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 claims abstract description 7
- 229940039790 sodium oxalate Drugs 0.000 claims abstract description 7
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims abstract description 5
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical group Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims abstract description 5
- IRXRGVFLQOSHOH-UHFFFAOYSA-L dipotassium;oxalate Chemical compound [K+].[K+].[O-]C(=O)C([O-])=O IRXRGVFLQOSHOH-UHFFFAOYSA-L 0.000 claims abstract description 5
- 229940071125 manganese acetate Drugs 0.000 claims abstract description 5
- 229940099607 manganese chloride Drugs 0.000 claims abstract description 5
- 235000002867 manganese chloride Nutrition 0.000 claims abstract description 5
- 239000011565 manganese chloride Substances 0.000 claims abstract description 5
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims abstract description 5
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002245 particle Substances 0.000 abstract description 10
- 238000005406 washing Methods 0.000 abstract description 7
- 229910010272 inorganic material Inorganic materials 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 239000011147 inorganic material Substances 0.000 abstract description 2
- 238000002156 mixing Methods 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 10
- HDJUVFZHZGPHCQ-UHFFFAOYSA-L manganese(2+);oxalate;dihydrate Chemical compound O.O.[Mn+2].[O-]C(=O)C([O-])=O HDJUVFZHZGPHCQ-UHFFFAOYSA-L 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 239000011259 mixed solution Substances 0.000 description 5
- 229910052573 porcelain Inorganic materials 0.000 description 5
- 238000000967 suction filtration Methods 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 3
- 229910052748 manganese Inorganic materials 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000008204 material by function Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000014509 gene expression Effects 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 230000005389 magnetism Effects 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000005556 structure-activity relationship Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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Classifications
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- 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
- C07—ORGANIC CHEMISTRY
- C07B—GENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
- C07B2200/00—Indexing scheme relating to specific properties of organic compounds
- C07B2200/13—Crystalline forms, e.g. polymorphs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to the field of inorganic material preparation, and particularly relates to a preparation method of charcoal type manganese oxalate crystals, which comprises the steps of uniformly stirring and mixing manganese salt and soluble oxalate, aging for 10-36 hours at 40-70 ℃, washing, filtering and drying to obtain hydrated manganese oxalate crystals; the manganese salt is manganese chloride, manganese acetate or manganese nitrate; the soluble oxalate is sodium oxalate, potassium oxalate or ammonium oxalate; the molar ratio of the manganese salt to the soluble oxalate is 1: 0.2-4. The method has the advantages of simple process, low cost, easy operation and higher yield of the target product, and the obtained manganese oxalate has the particle size of 2-5 mu m and the length of 10-20 mu m.
Description
Technical Field
The invention belongs to the field of inorganic material preparation, and particularly relates to a preparation method of charcoal type manganese oxalate crystals.
Background
The preparation of functional materials has become an indispensable technical means in modern science and technology, and the research on the performance related to the preparation has also been paid attention by researchers. The physical and chemical properties of the micro-nano functional material are related to factors such as the crystal form, the microstructure and the like of the micro-nano functional material. Effective synthesis and preparation of functional materials, and economic and reasonable preparation routes are becoming more important. The preparation method of the precise functional crystal material is beneficial to recognizing and controlling the nucleation and growth of the crystal at the atomic and molecular level and is beneficial to researching the structure-activity relationship between the crystalline structure of the material and the physicochemical property of the material. Manganese oxalate dihydrate is an important inorganic compound and is widely applied to the fields of purification, catalysis, electrochemistry, magnetism and the like. And is also one of the raw materials for preparing other manganese-containing compounds.
Disclosure of Invention
The invention aims to provide a preparation method of charcoal type manganese oxalate crystals, which has the advantages of simple process, mild conditions, high purity of target products, high yield and low cost, and manganese oxalate dihydrate can be used as an inorganic manganese source compound.
In order to solve the technical problem, the invention is realized as follows:
a method for preparing manganese oxalate crystals with charcoal morphology comprises the steps of uniformly stirring and mixing manganese salt and soluble oxalate, aging for 10-36 hours at 40-70 ℃, washing, filtering and drying to obtain hydrated manganese oxalate crystals.
As a preferred scheme, the manganese salt is manganese chloride, manganese acetate or manganese nitrate; the soluble oxalate is sodium oxalate, potassium oxalate or ammonium oxalate.
Further, the molar ratio of the manganese salt to the soluble oxalate is 1: 0.2-4.
Furthermore, the concentration of the manganese salt substance is 0.02-2 mol/L.
Furthermore, the concentration of the oxalate substance is 0.02-2 mol/L.
Furthermore, the stirring speed is 50-100 rpm, and the stirring time is 10-60 minutes.
Furthermore, the aging temperature is 40-70 ℃, the humidity is 50-70%, and the reaction time is 10-36 hours.
Furthermore, the drying time is 1-4 hours, and the drying temperature is 70-90 ℃.
The invention has the following characteristics:
(1) the method has the advantages of simple process, low cost, easy operation, high purity of the target product under mild conditions (temperature of 40-70 ℃ and humidity of 50-70%), and high yield of 93-98%.
(2) The XRD pattern of the obtained product has no obvious impurity peak, and the crystallinity is high. The surface of the particles in the SEM picture of the obtained product is smooth and has no obvious impurity particles, the particle size of the obtained manganese oxalate is 2-5 mu m, the length is 10-20 mu m, and the particle size can be controlled by adjusting the raw materials and the proportion thereof.
(3) The obtained manganese oxalate dihydrate is in a charcoal type in regular shape, and can be used as a chemical reagent, a manganese source material, a detergent and the like.
Drawings
The invention is further described with reference to the following figures and detailed description. The scope of the invention is not limited to the following expressions.
Fig. 1 is an XRD pattern of the manganese oxalate particles prepared in example 1.
Fig. 2 is an SEM photograph of the manganese oxalate particles prepared in example 2.
Fig. 3 is an SEM photograph of the manganese oxalate particles prepared in example 3.
Fig. 4 is an SEM photograph of the manganese oxalate particles prepared in example 4.
Fig. 5 is an SEM photograph of the manganese oxalate particles prepared in example 5.
Detailed Description
Example 1
A method for preparing a manganese oxalate crystal with a charcoal morphology comprises the steps of slowly dropwise adding a manganese chloride solution with the concentration of 0.05 mol/L into a sodium oxalate solution with the concentration of 0.05 mol/L at room temperature, enabling the molar ratio of manganese chloride to sodium oxalate to be 1:1, stirring at a stirring speed of 60 r/min to react for 50 minutes to obtain a mixed solution, standing and aging at a constant temperature of 50 ℃ and a constant humidity of 60% for 10 hours, carrying out suction filtration and water washing on the obtained mixture for three times, transferring the obtained mixture into a porcelain dish, drying in an oven at 80 ℃ for 4 hours to obtain manganese oxalate dihydrate, wherein the yield is 93%.
Example 2
A method for preparing a manganese oxalate crystal with a charcoal morphology comprises the steps of slowly dropwise adding a 0.05 mol/L manganese nitrate solution into a 0.05 mol/L sodium oxalate solution at room temperature, wherein the molar ratio of manganese nitrate to sodium oxalate is 1:1, stirring at a stirring speed of 60 r/min to react for 60 min to obtain a mixed solution, standing and aging at a constant temperature of 50 ℃ and a constant humidity of 60% for 10 h, carrying out suction filtration and water washing on the obtained mixture for three times, transferring the obtained mixture into a porcelain dish, drying in an oven at a temperature of 80 ℃ for 4 h to obtain manganese oxalate dihydrate, wherein the yield is 96%.
Example 3
A method for preparing a manganese oxalate crystal with a charcoal morphology comprises the steps of slowly dropwise adding a manganese nitrate solution with the concentration of 0.05 mol/L into an ammonium oxalate solution with the concentration of 0.05 mol/L at room temperature, enabling the molar ratio of manganese nitrate to ammonium oxalate to be 1:1, stirring at the stirring speed of 60 revolutions/minute to react for 60 minutes to obtain a mixed solution, standing and aging at the constant temperature of 60 ℃ and the constant humidity of 60% for 10 hours, carrying out suction filtration and water washing on the obtained mixture for three times, transferring the obtained mixture into a porcelain dish, and drying in an oven at the temperature of 80 ℃ for 4 hours to obtain manganese oxalate dihydrate with the yield of 98%.
Example 4
A method for preparing a manganese oxalate crystal with a charcoal morphology comprises the steps of slowly dropwise adding a manganese acetate solution with the concentration of 0.05 mol/L into an ammonium oxalate solution with the concentration of 0.05 mol/L at room temperature, enabling the molar ratio of manganese acetate to ammonium oxalate to be 1:1, stirring at a stirring speed of 60 r/min to react for 60 minutes to obtain a mixed solution, standing and aging at the constant temperature of 60 ℃ and the constant humidity of 60% for 10 hours, carrying out suction filtration and water washing on the obtained mixture for three times, transferring the obtained mixture into a porcelain dish, drying in an oven at the temperature of 80 ℃ for 4 hours to obtain manganese oxalate dihydrate, wherein the yield is 96%.
Example 5
A method for preparing a manganese oxalate crystal with a charcoal morphology comprises the steps of slowly dropwise adding a manganese nitrate solution with the concentration of 0.05 mol/L into a potassium oxalate solution with the concentration of 0.05 mol/L at room temperature, enabling the molar ratio of manganese nitrate to potassium oxalate to be 1:1, stirring at a stirring speed of 70 r/min to react for 60 min to obtain a mixed solution, standing and aging at the constant temperature of 60 ℃ and the constant humidity of 70% for 10 h, carrying out suction filtration and water washing on the obtained mixture for three times, transferring the washed mixture into a porcelain dish, and drying in an oven at 70 ℃ for 4 h to obtain a manganese oxalate dihydrate with the yield of 95%.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. A method for preparing manganese oxalate crystals with charcoal morphology is characterized by comprising the following steps: the manganese salt and the soluble oxalate are stirred and mixed uniformly, aged for 10-36 hours at the temperature of 40-70 ℃, and washed, filtered and dried to obtain the hydrated manganese oxalate crystal.
2. The method for preparing manganese oxalate crystals with charcoal morphology according to claim 1, wherein: the manganese salt is manganese chloride, manganese acetate or manganese nitrate; the soluble oxalate is sodium oxalate, potassium oxalate or ammonium oxalate.
3. The method for preparing manganese oxalate crystals with charcoal morphology according to claim 2, wherein: the molar ratio of the manganese salt to the soluble oxalate is 1: 0.2-4.
4. The method for preparing the manganese oxalate crystals with charcoal morphology according to claim 3, wherein: the concentration of the manganese salt is 0.02-2 mol/L.
5. The method for preparing manganese oxalate crystals with charcoal morphology according to claim 4, wherein: the concentration of the oxalate is 0.02-2 mol/L.
6. The method for preparing manganese oxalate crystals with charcoal morphology according to claim 5, wherein: the stirring speed is 50-100 rpm, and the stirring time is 10-60 minutes.
7. The method for preparing the manganese oxalate crystals with charcoal morphology according to claim 6, wherein: the aging temperature is 40-70 ℃, the humidity is 50-70%, and the reaction time is 10-36 hours.
8. The method for preparing the manganese oxalate crystals with charcoal morphology according to claim 7, wherein: the drying time is 1-4 hours, and the drying temperature is 70-90 ℃.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210035399.1A CN115010594A (en) | 2022-01-13 | 2022-01-13 | Preparation method of charcoal-shaped manganese oxalate crystals |
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| CN202210035399.1A CN115010594A (en) | 2022-01-13 | 2022-01-13 | Preparation method of charcoal-shaped manganese oxalate crystals |
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| CN202210035399.1A Pending CN115010594A (en) | 2022-01-13 | 2022-01-13 | Preparation method of charcoal-shaped manganese oxalate crystals |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320952A (en) * | 2011-07-27 | 2012-01-18 | 渤海大学 | Preparation method of barium oxalate hydrate microcrystal with firewood morphology |
| CN103539097A (en) * | 2013-10-30 | 2014-01-29 | 渤海大学 | Preparation method of multi-shape alkaline manganese phosphate microcrystal |
-
2022
- 2022-01-13 CN CN202210035399.1A patent/CN115010594A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320952A (en) * | 2011-07-27 | 2012-01-18 | 渤海大学 | Preparation method of barium oxalate hydrate microcrystal with firewood morphology |
| CN103539097A (en) * | 2013-10-30 | 2014-01-29 | 渤海大学 | Preparation method of multi-shape alkaline manganese phosphate microcrystal |
Non-Patent Citations (2)
| Title |
|---|
| 丁延敏: "锰基复合负极材料的制备及储锂性能研究", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
| 刘瑞瑞: "锰氧化物多孔材料的制备与电化学性能表征", 《中国优秀硕士学位论文全文数据库工程科技Ⅰ辑》 * |
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Application publication date: 20220906 |
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