CN102942471A - Preparation method of oxalate - Google Patents
Preparation method of oxalate Download PDFInfo
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- CN102942471A CN102942471A CN2012104787924A CN201210478792A CN102942471A CN 102942471 A CN102942471 A CN 102942471A CN 2012104787924 A CN2012104787924 A CN 2012104787924A CN 201210478792 A CN201210478792 A CN 201210478792A CN 102942471 A CN102942471 A CN 102942471A
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Abstract
The invention discloses a preparation method of oxalate and relates to the technical field of preparation methods of the oxalate. The method includes the following steps: (1) adding one mole part of metal salt into a first organic solvent, stirring for 10-20min to mix evenly and obtain a metal salt organic solvent, adding 0.5-1.5 mole parts of oxalic acid into a second organic solvent, and stirring for 10-20min to mix evenly and obtain an oxalic acid organic solvent; (2) cooling the metal salt organic solvent and the oxalic acid organic solvent to a temperature ranging from-40DEG C to-80DEG C; (3) mixing the metal salt organic solvent and the oxalic acid organic solvent, stirring for 10-20min to obtain a mixed solution; and (4) stopping cooling, naturally warming the mixed solution, and evenly precipitating the oxalate precipitation. The method is simple in process, easy to operate, suitable for mass production and capable of preparing the oxalate with high purity, small particle diameters and even distribution.
Description
Technical field
The present invention relates to the oxalate preparing technical field, relate in particular to a kind of method of utilizing the precipitator method to prepare oxalate.
Background technology
Ferrox is as one of raw material for preparing the Olivine-type Cathode Material in Li-ion Batteries iron lithium phosphate, and its purity and particle diameter have important impact, wherein Fe to the performance of battery
3+Existence have a strong impact on the charge-discharge performance of battery.The synthetic main chemical precipitation method that adopts of prior art mesoxalic acid ferrous iron is mixed divalent iron salt solution with oxalic acid or oxalate solution, the processing parameter realization by controlling building-up process is to the control of Ferrox particle diameter and pattern thereof.Because the crystalline structure of most metals oxalate is more similar, easily forms the more uniform eutectic throw out of particulate, created good prerequisite for reducing rear generation metal alloy, be the important method of producing the high-test metal wedding agent.Oxalate precipitation-thermal decomposition method is as one of important method for preparing metal simple-substance and oxide powder material thereof, and its advantage is: the one, and heat decomposition temperature is low, purity is high, cost is low.The 2nd, can utilize thermal decomposition product the presoma pattern to be had the characteristics of " inheritance ", in the preparation of oxalate, regulate and control its granule-morphology and granularity, and then prepare metal simple-substance and the oxide powder material thereof that satisfies particular requirement.Someone has obtained very wide ferromegnetism and the ferrimagnetism mixed oxide of component distribution by heat treated co-precipitation Co-Fe, Fe-Ni, Zn-Fe, Mn-Fe oxalate.
At present, the industrial method for preparing oxalate mainly adopts metal-salt such as vitriol, nitrate, muriate etc. to mix with oxalic acid or oxalate solution, generates precipitation.Its reaction equation is as follows:
M
2++C
2O
4 2-+nH
2O=M?C
2O
4·nH
2O?↓
The method Main Problems is: no matter adopt which kind of feed way, all be difficult to guarantee that degree of supersaturation is even in the reaction system, therefore, in the precipitation generative process, can not control effectively to steps such as nucleation, growth, reunions, so that particle is thick and size-grade distribution is wide, have a strong impact on its application performance.
The kind that foreign ion exists in oxalate and the compound grass hydrochlorate and content are very large on the impact of synthetic product property; Particle diameter and distribution thereof are another important factors that affects product property on the other hand, ultramicron has the not available property of ordinary particle, have (1) small-size effect, (2) surface and interface effect, (3) quantum size effect etc. such as nanoparticle, and produce some property at aspects such as thermal characteristic, optical characteristics and chemical property thus, more much lower than conventional powder such as the sintering temperature of nanoparticle; Absorb etc. the broadband of visible light is strong.
In the liquid phase synthetic chemistry on basis, the solubility product of target product is the key factor that affects the synthetic product performance take the precipitator method.In one-component product synthetic, how direct precipitation method no matter order of addition(of ingredients), feed rate is regulated and control, and is difficult to guarantee that the degree of supersaturation of solution is consistent, and there is local overrich phenomenon all the time in whole process, finally causes particle size were to distribute wide.In coprecipitation process, because each component solubility product there are differences, easily form double team type composite precipitation, different components distributes in product and has larger difference, has a strong impact on the cycling processability of product.
Summary of the invention
Technical problem to be solved by this invention is: the deficiency for prior art exists, the method for preparing oxalate is provided, and simple process of the present invention, easy to operate is suitable for scale operation, can prepare that purity is high, grain diameter is little and equally distributed oxalate.
For solving the problems of the technologies described above, technical scheme of the present invention is:
Prepare the method for oxalate, may further comprise the steps:
Metal-salt and the 0.5-1.5 molar part oxalic acid that (1) 1 molar part can be dissolved in organic solvent join respectively in the organic solvent, stir respectively to mix in 10-20 minute, obtain metal-salt organic solution and oxalic acid organic solution;
(2) described metal-salt organic solution and oxalic acid organic solution are cooled to-40 ℃ to-80 ℃;
(3) the metal-salt organic solution that step (2) is obtained and oxalic acid organic solution are mixed, and stir 10-20 minute, get mixing solutions;
(4) stop cooling, described mixing solutions is heated up naturally, evenly separate out oxalate precipitation.
As a kind of scheme, one or more in acetate, nitrate or the muriate that the described metal-salt that can be dissolved in organic solvent is iron, cobalt, nickel, copper, zinc, manganese.
As further scheme, the described metal-salt that can be dissolved in organic solvent is one or more in iron protochloride, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, nickelous nitrate, cupric chloride, zinc chloride and the manganese acetate.
As a kind of scheme, described organic solvent comprises alcohols or organic solvent of ketone.
As further scheme, described alcohols or organic solvent of ketone comprise one or more in dehydrated alcohol, methyl alcohol and the acetone.
As a kind of scheme, in the described step (1), the amount of substance concentration of described metal-salt organic solution is 0.04-0.1mol/L.
As a kind of scheme, in the described step (1), the amount of substance concentration of described oxalic acid organic solution is 0.04-0.1mol/L.
As a kind of scheme, in the described step (1), the amount of substance concentration of described metal-salt organic solution is identical with the amount of substance concentration of oxalic acid organic solution.
As a kind of scheme, 1 molar part metal-salt is joined respectively in the identical organic solvent of volume with 0.5-1.5 molar part oxalic acid.
As a kind of scheme, in the described step (3), with the ethanol/liquid nitrogen bath below-80 ℃ described metal-salt organic solution and oxalic acid organic solution are cooled to-80 ℃.
Owing to having adopted technique scheme, the invention has the beneficial effects as follows:
The present invention at first prepares the organic solution of metal-salt and oxalic acid, then metal-salt organic solution and oxalic acid organic solution are cooled to-40 ℃ to-80 ℃ and mixing, since under-40 ℃ to-80 ℃ cold condition metal-salt organic solution and oxalic acid organic solution can form homogeneous solution and not oxalic salt precipitate, solution system is more stable like this.By improving gradually the temperature of solution system, oxalate precipitation is evenly separated out from solution gradually.Rate of change by control solution system temperature can obtain the target product that has different-grain diameter and be evenly distributed.The oxalate precipitation of preparation has the advantages that particle diameter is little, be evenly distributed like this.Owing to being deposited in solubility product in the organic solvent much smaller than its solubility product in water, the solubility product of each component has levelling effect, thereby when preparation composite salt material, adopt organic solvent to make solvent can to obtain easily equally distributed composite salt, thereby reach simplification preparation technology, reduce the purpose of cost.
Embodiment
Below in conjunction with embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Prepare the method for Ferrox, may further comprise the steps:
(1) 198.83 gram iron protochlorides is added in the 20.00L dehydrated alcohol, stirs and mixed in 10 minutes, get iron protochloride organic solution; 45.02 gram oxalic acid are added in the 10.00L dehydrated alcohol, stir and mixed in 10 minutes, get oxalic acid organic solution;
(2) iron protochloride organic solution and oxalic acid organic solution are cooled to-40 ℃;
(3) iron protochloride organic solution and oxalic acid organic solution are mixed, stirred 10 minutes, get mixing solutions;
(4) stop cooling, mixing solutions is heated up naturally, evenly separate out the Ferrox precipitation.Detect to get product purity 99.1wt%, particle diameter 95nm.
Embodiment 2
Prepare the method for cobalt oxalate, may further comprise the steps:
(1) 291.05 gram Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKESs is added in the 16.67L dehydrated alcohol, stirs and mixed in 12 minutes, get Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES organic solution; 63.03 gram oxalic acid are added in the 11.67L dehydrated alcohol, stir and mixed in 12 minutes, get oxalic acid organic solution;
(2) Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES organic solution and oxalic acid organic solution are cooled to-50 ℃;
(3) Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES organic solution and oxalic acid organic solution are mixed, stirred 12 minutes, get mixing solutions;
(4) stop cooling, mixing solutions is heated up naturally, evenly separate out cobalt oxalate precipitation.Detect to get product purity 99.3wt%, particle diameter 97nm.
Embodiment 3
Prepare the method for nickelous oxalate, may further comprise the steps:
(1) 290.81 gram nickelous nitrates is added in the 14.29L methyl alcohol, stirs and mixed in 13 minutes, get nickelous nitrate organic solution; 81.04 gram oxalic acid are added in the 12.86L methyl alcohol, stir and mixed in 13 minutes, get oxalic acid organic solution;
(2) nickelous nitrate organic solution and oxalic acid organic solution are cooled to-55 ℃;
(3) nickelous nitrate organic solution and oxalic acid organic solution are mixed, stirred 13 minutes, get mixing solutions;
(4) stop cooling, mixing solutions is heated up naturally, evenly separate out the nickelous oxalate precipitation.Detect to get product purity 99.4wt%, particle diameter 96nm.
Embodiment 4
Prepare the method for cupric oxalate, may further comprise the steps:
(1) 170.48 gram cupric chlorides is added in the 12.50L methyl alcohol, stirs and mixed in 15 minutes, get cupric chloride organic solution; 90.04 gram oxalic acid are added in the 12.50L methyl alcohol, stir and mixed in 15 minutes, get oxalic acid organic solution;
(2) cupric chloride organic solution and oxalic acid organic solution are cooled to-60 ℃;
(3) cupric chloride organic solution and oxalic acid organic solution are mixed, stirred 15 minutes, get mixing solutions;
(4) stop cooling, mixing solutions is heated up naturally, evenly separate out the cupric oxalate precipitation.Detect to get product purity 99.2wt%, particle diameter 99nm.
Embodiment 5
Prepare the method for zinc oxalate, may further comprise the steps:
(1) 136.32 gram zinc chloride is added in the 11.11L acetone, stirs and mixed in 16 minutes, get zinc chloride organic solution; 99.04 gram oxalic acid are added in the 12.22L acetone, stir and mixed in 16 minutes, get oxalic acid organic solution;
(2) with-80 ℃ of ethanol/liquid nitrogen baths zinc chloride organic solution and oxalic acid organic solution are cooled to-65 ℃;
(3) zinc chloride organic solution and oxalic acid organic solution are mixed, stirred 16 minutes, get mixing solutions;
(4) stop cooling, mixing solutions is heated up naturally, evenly separate out the zinc oxalate precipitation.Detect to get product purity 99.6wt%, particle diameter 100nm.
Embodiment 6
Prepare the method for manganous oxalate, may further comprise the steps:
(1) 245.09 gram manganese acetates is added in the 10.00L acetone, stirs and mixed in 17 minutes, get manganese acetate organic solution; 108.05 gram oxalic acid are added in the 12.00L acetone, stir and mixed in 17 minutes, get oxalic acid organic solution;
(2) with-80 ℃ of ethanol/liquid nitrogen baths manganese acetate organic solution and oxalic acid organic solution are cooled to-70 ℃;
(3) manganese acetate organic solution and oxalic acid organic solution are mixed, stirred 17 minutes, get mixing solutions;
(4) stop cooling, mixing solutions is heated up naturally, evenly separate out the manganous oxalate precipitation.Detect to get product purity 99.5wt%, particle diameter 101nm.
Embodiment 7
Prepare the method for Ferrox and cobalt oxalate, may further comprise the steps:
(1) 99.42 iron protochlorides and 145.53 gram Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKESs are added in the 10.00L dehydrated alcohol, stir and mixed in 18 minutes, get iron protochloride and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES organic solution; 117.05 gram oxalic acid are added in the 13.00L dehydrated alcohol, stir and mixed in 18 minutes, get oxalic acid organic solution;
(2) iron protochloride and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES organic solution and oxalic acid organic solution are cooled to-75 ℃;
(3) with iron protochloride and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES organic solution and the mixing of oxalic acid organic solution, stirred 18 minutes, get mixing solutions;
(4) stop cooling, mixing solutions is heated up naturally, evenly separate out Ferrox and cobalt oxalate precipitation.Detect to get product purity 99.1wt%, particle diameter 103nm.
Embodiment 8
Prepare the method for nickelous oxalate and cobalt oxalate, may further comprise the steps:
(1) 145.41 gram nickelous nitrates and 145.53 gram Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKESs are added in the 10.00L methyl alcohol, stir and mixed in 20 minutes, get nickelous nitrate and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES organic solution; 135.06 gram oxalic acid are added in the 15.00L methyl alcohol, stir and mixed in 20 minutes, get oxalic acid organic solution;
(2) nickelous nitrate and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES organic solution and oxalic acid organic solution are cooled to-80 ℃;
(3) with nickelous nitrate and Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES organic solution and the mixing of oxalic acid organic solution, stirred 20 minutes, get mixing solutions;
(4) stop cooling, mixing solutions is heated up naturally, evenly separate out nickelous oxalate and cobalt oxalate precipitation.Detect to get product purity 99.0wt%, particle diameter 104nm.
Claims (10)
1. prepare the method for oxalate, it is characterized in that, may further comprise the steps:
Metal-salt and the 0.5-1.5 molar part oxalic acid that (1) 1 molar part can be dissolved in organic solvent join respectively in the organic solvent, stir respectively to mix in 10-20 minute, obtain metal-salt organic solution and oxalic acid organic solution;
(2) described metal-salt organic solution and oxalic acid organic solution are cooled to-40 ℃ to-80 ℃;
(3) the metal-salt organic solution that step (2) is obtained and oxalic acid organic solution are mixed, and stir 10-20 minute, get mixing solutions;
(4) stop cooling, described mixing solutions is heated up naturally, evenly separate out oxalate precipitation.
2. the method for preparing oxalate as claimed in claim 1 is characterized in that: one or more in acetate, nitrate or the muriate that the described metal-salt that can be dissolved in organic solvent is iron, cobalt, nickel, copper, zinc, manganese.
3. the method for preparing oxalate as claimed in claim 2, it is characterized in that: the described metal-salt that can be dissolved in organic solvent is one or more in iron protochloride, Jing Ti/Bao Pian COBALT NITRATE CRYSTALS/FLAKES, nickelous nitrate, cupric chloride, zinc chloride and the manganese acetate.
4. the method for preparing oxalate as claimed in claim 1, it is characterized in that: described organic solvent comprises alcohols or organic solvent of ketone.
5. the method for preparing oxalate as claimed in claim 4, it is characterized in that: described alcohols or organic solvent of ketone comprise one or more in dehydrated alcohol, methyl alcohol and the acetone.
6. the method for preparing oxalate as claimed in claim 1, it is characterized in that: in the described step (1), the amount of substance concentration of described metal-salt organic solution is 0.04-0.1mol/L.
7. the method for preparing oxalate as claimed in claim 1, it is characterized in that: in the described step (1), the amount of substance concentration of described oxalic acid organic solution is 0.04-0.1mol/L.
8. the method for preparing oxalate as claimed in claim 1, it is characterized in that: in the described step (1), the amount of substance concentration of described metal-salt organic solution is identical with the amount of substance concentration of oxalic acid organic solution.
9. the method for preparing oxalate as claimed in claim 1 is characterized in that: 1 molar part metal-salt is joined respectively in the identical organic solvent of volume with 0.5-1.5 molar part oxalic acid.
10. the method for preparing oxalate as claimed in claim 1 is characterized in that: in the described step (3), with the ethanol/liquid nitrogen bath below-80 ℃ described metal-salt organic solution and oxalic acid organic solution are cooled to-80 ℃.
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Cited By (7)
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|---|---|---|---|---|
| CN104649888A (en) * | 2014-08-27 | 2015-05-27 | 江西理工大学 | Preparation method of large-particle neodymium oxalate |
| CN105085238A (en) * | 2015-08-22 | 2015-11-25 | 李亚丰 | Zirconium oxalate crystal and preparation method thereof |
| CN105859542A (en) * | 2016-06-15 | 2016-08-17 | 湖北百杰瑞新材料股份有限公司 | Preparing method for high-purity lithium oxalate |
| CN108069851A (en) * | 2017-12-28 | 2018-05-25 | 甘肃有色冶金职业技术学院 | A kind of method that no ammonia oxalic acid precipitation prepares cobalt oxalate |
| CN110357777A (en) * | 2019-06-27 | 2019-10-22 | 黄冈师范学院 | A kind of synthetic method of high-purity oxalic acid ferrous iron |
| CN113264821A (en) * | 2021-04-29 | 2021-08-17 | 广东邦普循环科技有限公司 | Recovery method and application of lithium iron phosphate waste |
| WO2023040406A1 (en) * | 2021-09-16 | 2023-03-23 | 昆明理工大学 | Preparation method for metal oxalate lithium ion battery negative electrode material with ordered three-dimensional skeleton structure |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104649888A (en) * | 2014-08-27 | 2015-05-27 | 江西理工大学 | Preparation method of large-particle neodymium oxalate |
| CN105085238A (en) * | 2015-08-22 | 2015-11-25 | 李亚丰 | Zirconium oxalate crystal and preparation method thereof |
| CN105085238B (en) * | 2015-08-22 | 2017-02-01 | 李亚丰 | Zirconium oxalate crystal and preparation method thereof |
| CN105859542A (en) * | 2016-06-15 | 2016-08-17 | 湖北百杰瑞新材料股份有限公司 | Preparing method for high-purity lithium oxalate |
| CN108069851A (en) * | 2017-12-28 | 2018-05-25 | 甘肃有色冶金职业技术学院 | A kind of method that no ammonia oxalic acid precipitation prepares cobalt oxalate |
| CN110357777A (en) * | 2019-06-27 | 2019-10-22 | 黄冈师范学院 | A kind of synthetic method of high-purity oxalic acid ferrous iron |
| CN110357777B (en) * | 2019-06-27 | 2022-02-01 | 黄冈师范学院 | Synthetic method of high-purity ferrous oxalate |
| CN113264821A (en) * | 2021-04-29 | 2021-08-17 | 广东邦普循环科技有限公司 | Recovery method and application of lithium iron phosphate waste |
| CN113264821B (en) * | 2021-04-29 | 2023-05-05 | 广东邦普循环科技有限公司 | Recovery method and application of lithium iron phosphate waste |
| WO2023040406A1 (en) * | 2021-09-16 | 2023-03-23 | 昆明理工大学 | Preparation method for metal oxalate lithium ion battery negative electrode material with ordered three-dimensional skeleton structure |
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