CN102557916A - Preparation method of special battery-grade ferrous oxalate for lithium iron phosphate - Google Patents
Preparation method of special battery-grade ferrous oxalate for lithium iron phosphate Download PDFInfo
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- CN102557916A CN102557916A CN2011103965027A CN201110396502A CN102557916A CN 102557916 A CN102557916 A CN 102557916A CN 2011103965027 A CN2011103965027 A CN 2011103965027A CN 201110396502 A CN201110396502 A CN 201110396502A CN 102557916 A CN102557916 A CN 102557916A
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Abstract
The invention discloses a preparation method of special battery-grade ferrous oxalate for lithium iron phosphate, and the method comprises the following steps of: A) removing impurities, adding pure water, stirring, adding solid ferrite, rising the temperature to 80-100 DEG C, adding reduced ferrous powder, stirring for 1-3 hours at a constant temperature, controlling the pH between 2 and 4, and carrying out filter pressing; B) filtering a ferrite solution, and eliminating ferrous powder and purities; C) adding filtrate into a main reaction kettle after the ferrite solution is clear, adding solid oxalate dehydrate to carry out precipitation reaction at the temperature of 30-60 DEG C after filter pressing, and rising the temperature to the constant temperature of 70-100 DEGC after reaction is performed for 10-60 minutes, wherein the charging time is 5-6 minutes; D) stirring a reaction solution, and carrying out heat preservation for 2-4 hours for aging; E) separating ferrous oxalate by virtue of a centrifugal machine; and F) rinsing and drying separated ferrous oxalate to obtain ferrous oxalate products. The preparation method of the special battery-grade ferrous oxalate for the lithium iron phosphate, which is disclosed by the invention, has the advantages of simple and practical process, low production cost and environmental friendliness, and can be used for further synthetizing the small-granular battery-grade ferrous oxalate in one step, wherein the granularity is less than 5mu m and the purity is larger than 99.55%.
Description
Technical field
The present invention relates to a kind of preparation method of Ferrox, particularly relate to a kind of preparation method of iron lithium phosphate reserve battery level iron oxalate.
Background technology
Ferrox molecular formula FeC
2O
42H
2O, existing Ferrox working method mainly contains three major types: 1, make battery level iron oxalate with oxalate solution and ferrous iron solution reaction, its technology shortcoming is that particle is thicker, just can obtain the product of 3-5 μ m after must pulverizing.Make the product of 3-5 μ m if think a step, then need adding assistant.2, make battery level iron oxalate with oxalic acid solution and ferrous iron solution reaction, its technology shortcoming is that particle is thicker, just can obtain the product of 3-5 μ m after must pulverizing.Make the product of 3-5 μ m if think a step, then need adding assistant.3, make battery level iron oxalate with oxalic acid solid and ferrous iron solution reaction.Patent CN200710165366.4 uses is exactly the oxalic acid solid or contains solid oxalic acid and the ferrous iron solution reaction makes product, but it need add organism such as polyoxyethylene glycol and xitix as tensio-active agent.More than these three kinds of modes be not that technology is in the past complicated, need add other organism exactly, the battery level iron oxalate particle of manufacturing is bigger, purity is not high, and production cost is than higher.
Summary of the invention
The present invention accomplishes in order to solve deficiency of the prior art, the purpose of this invention is to provide that a kind of features simple and practical process, production cost are low, more environmental protection, can make that size ratio is less through the production technique such as concentration and temperature of reaction that control adds oxalic acid dihydrate solid speed, ferrous salt, purity is than the preparation method of higher iron lithium phosphate reserve battery level iron oxalate.
The preparation method of a kind of iron lithium phosphate reserve battery level iron oxalate of the present invention comprises following technical process:
A. in the removal of impurities still, add pure water, start to stir, and be that 0.5～5: 1 amount according to pure water adds the ferrous salt solid according to solvent and solute weight ratio; Begin heating, after water temperature rises to 80～100 ℃, add reduced iron powder with ferrous salt solid weight ratio 0.5～3%; Constant temperature stirred 1～3 hour; Control its reacted pH=2～4, obtain ferrous salt solution, the beginning press filtration;
B. with the ferrous salt solution of A generating step through one group of automatic pressurize closed type chamber-type press filter, filtering metal impurity, nonmetallic impurity and remove excessive reduced iron powder obtain purified ferrous salt solution simultaneously;
C. after the ferrous salt filtrating of B step is limpid, open the pressure filter liquid-outlet valve, ferrous salt filtrating is squeezed in the main reaction still fast; After press filtration was accomplished, temperature was controlled at 30～60 ℃, ℃; Get the oxalic acid dihydrate solid of 1.001～1.05 times of amounts of mole number of said ferrous salt; Begin to add the oxalic acid dihydrate solid, the reinforced time is 5～60min, rises to 70～100 ℃ of isothermal reactions to temperature of reaction again after reaction 10～60min;
D. the reaction solution that obtains in the C step is fully stirred, and be incubated 2～4h and carry out ageing, obtain the Ferrox slurry;
E. separate the Ferrox in the Ferrox slurry through whizzer, rotating speed is 30～100 commentaries on classics/min, centrifugation time 20～60min;
F. the Ferrox after will separating obtains the Ferrox finished product through washing after the oven dry.
The preparation method of a kind of iron lithium phosphate reserve battery level iron oxalate of the present invention can also be:
Said ferrous salt is a kind of in iron protochloride, ferrous sulfate and the Iron nitrate.
After water temperature rises to 95 ± 5 ℃ in the said A step, add reduced iron powder.
Said strainer is plate filter or accurate filter.
Filter cloth space in the said E step in the whizzer is 0.1～5 μ m.
The ferrous purity of oxalic acid dihydrate is greater than 99.5%.
The preparation method of a kind of iron lithium phosphate reserve battery level iron oxalate of the present invention is through above-mentioned steps, in terms of existing technologies; Its advantage that has is because the step that adopts is fairly simple, promptly utilizes to add reduced iron powder in the ferrous salt solution and fully react, and reduces the spent acid amount; Improve concentration and filtration and obtain the higher Ferrox of purity, reactivity improves greatly, directly obtains the Ferrox particle of 3-5 μ m; Product mesoxalic acid ferrous content all >=99.5%; And the ferrous salt that utilizes trade waste makes trade waste obtain recycle as basic raw material used in the present invention, improves the quality of environment greatly; Reduce production costs, realize recycling economy and be that green economy all is able to the win-win situation that develops.
Embodiment
Face preparing method's further explain of a kind of iron lithium phosphate reserve battery level iron oxalate of the present invention down.
The preparation method of a kind of iron lithium phosphate reserve battery level iron oxalate of the present invention,
Comprise following technical process:
A. in the removal of impurities still, add pure water, start to stir, and be that 0.5～5: 1 amount according to pure water adds the ferrous salt solid according to solvent and solute weight ratio; Begin heating, after water temperature rises to 80～100 ℃, add reduced iron powder with ferrous salt solid weight ratio 0.5～3%; Constant temperature stirred 1～3 hour; Control its reacted pH=2～4, obtain ferrous salt solution, the beginning press filtration;
B. (sky, Shanghai founds pressure filter ltd through one group of automatic pressurize closed type chamber-type press filter with the ferrous salt solution of A generating step; Model is XAMY40/800-UK); Simultaneously filtering metal impurity, nonmetallic impurity and remove excessive reduced iron powder obtain purified ferrous salt solution;
C. after the ferrous salt filtrating of B step is limpid, open the pressure filter liquid-outlet valve, ferrous salt filtrating is squeezed in the main reaction still fast; After press filtration is accomplished; Temperature is controlled at 30～60 ℃, gets the oxalic acid dihydrate solid of 1.001～1.05 times of amounts of mole number of said ferrous salt, begins to add the oxalic acid dihydrate solid; The reinforced time is 5～60min, rises to 70～100 ℃ of isothermal reactions to temperature of reaction again after reaction 10～60min;
D. the reaction solution that obtains in the C step is fully stirred, and be incubated 2～4h and carry out ageing, obtain the Ferrox slurry;
E. separate the Ferrox in the Ferrox slurry through whizzer, rotating speed is 30～100 commentaries on classics/min, centrifugation time 20～60min;
F. the Ferrox after will separating obtains the Ferrox finished product through washing after the oven dry.
Because adopt above-mentioned steps to make iron lithium phosphate reserve battery level iron oxalate, the step of employing is fairly simple, promptly utilize to add reduced iron powder in the ferrous salt solution and carry out preliminary removal of impurities; Fully reaction reduces the spent acid amount, improves concentration and filters and obtain the higher Ferrox of purity; Reactivity improves greatly; Directly obtain the Ferrox particle of 3-5 μ m, product mesoxalic acid ferrous content all >=99.5%, and the ferrous salt that utilizes trade waste is as basic raw material used in the present invention; Make trade waste obtain recycle; Improve the quality of environment greatly, reduce production costs, realize recycling economy and be that green economy all is able to the win-win situation that develops.
The preparation method of a kind of iron lithium phosphate reserve battery level iron oxalate of the present invention specifically can also be that said ferrous salt is a kind of in iron protochloride, ferrous sulfate and the Iron nitrate.Certainly can also adopt other ferrous salt, the advantage of selecting these several kinds of ferrous salts for use is that these several kinds of ferrous salts are relatively more conventional, and price comparison is cheap, and these several kinds of ferrous salts derive from Iron And Steel Plant, titanium powder plant etc.Can also be after water temperature rises to 95 ± 5 ℃ in the above A step of basis of technical scheme in front, to add reduced iron powder.The better effects if of removal of impurities like this.In addition, said strainer is that one group of automatic pressurize closed type chamber-type press filter can be that the model that the upright pressure filter ltd in sky, Shanghai sells is the pressure filter of XAMY40/800-UK.
Embodiment 1:
A. in the removal of impurities still, add the 175kg pure water, start and stir, and add 350kg iron protochloride (solvent and solute weight ratio is 0.5: 1); Begin heating, make water temperature rise to 90 ℃ after, add reduced iron powder 1.75kg; Control its reacted pH=2.5; Constant temperature stirred 3 hours, obtained solution of ferrous chloride, the beginning press filtration;
B. with the ferrous salt solution of A generating step through one group of automatic pressurize closed type chamber-type press filter (model is XAMY40/800-UK), filter simultaneously and remove metallic impurity, nonmetallic impurity and excessive reduced iron powder, obtain purified ferrous salt solution;
C. after the iron protochloride filtrating of B step is limpid, open the pressure filter liquid-outlet valve, occlusion pressure filter reverse flow valve is squeezed into iron protochloride filtrating in the main reaction still fast; After press filtration is accomplished, add oxalic acid dihydrate solid 211.8kg (according to 1.001 times of the mole numbers of ferrous salt), and do not add any dispersion agent; The reinforced time is 10min, adds after the material, and be under 40 ℃ in temperature; Reaction 30min rises to 70 ℃ to temperature of reaction afterwards again;
D. reaction solution in the C step is fully stirred, and obtain the Ferrox slurry after 3 hours in insulation under 70 ℃;
E. separate the Ferrox in the Ferrox slurry through whizzer (the filter cloth space in the whizzer is 0.1 μ m), rotating speed is 100 commentaries on classics/min, centrifugation time 30min;
F. the Ferrox after will separating is through washing, and obtaining purity after the oven dry is 99.5%, once synthetic granularity is 1.5 μ m Ferrox finished products.
Embodiment 2:
A. in the removal of impurities still, add the 700kg pure water, start and stir, and add 350kg iron protochloride (solvent and solute weight ratio is 2: 1); Begin heating, make water temperature rise to 95 ℃ after, add reduced iron powder 4.5kg; Control its reacted pH=3, constant temperature stirred 2 hours, obtained solution of ferrous chloride;
B. with the ferrous salt solution of A generating step through one group of automatic pressurize closed type chamber-type press filter (model is XAMY40/800-UK), filter simultaneously and remove metallic impurity, nonmetallic impurity and excessive reduced iron powder, obtain purified ferrous salt solution;
C. after the iron protochloride filtrating of B step is limpid, open the pressure filter liquid-outlet valve, occlusion pressure filter reverse flow valve is squeezed into iron protochloride filtrating in the main reaction still fast; After press filtration is accomplished, disposablely to pour oxalic acid dihydrate solid 232.68Kg (according to 1.05 times of the mole numbers of ferrous salt) into, and do not add any dispersion agent, the reinforced time is 60min, is under 50 ℃ in temperature, reaction 30min rises to 100 ℃ to temperature of reaction afterwards again;
D. the reaction solution in the C step is fully stirred, and obtain the Ferrox slurry after 2 hours in insulation under 100 ℃;
E. separate the Ferrox in the Ferrox slurry through supercentrifuge (the filter cloth space in the whizzer is 1.5 μ m), rotating speed is 30 commentaries on classics/min, centrifugation time 60min;
F. the Ferrox after will separating is through washing, and obtaining purity after the oven dry is 99.7%, once synthetic granularity is 4.3 μ m Ferrox finished products.
Embodiment 3:
A. in the removal of impurities still, add the 1750kg pure water, start and stir, and add 350kg iron protochloride (solvent and solute weight ratio is 5: 1); Begin heating, make water temperature rise to 97 ℃ after, add reduced iron powder 10.5kg; Control its reacted pH=4, constant temperature stirred 1 hour, obtained solution of ferrous chloride;
B. with the ferrous salt solution of A generating step through one group of automatic pressurize closed type chamber-type press filter (model is XAMY40/800-UK), filter simultaneously and remove metallic impurity, nonmetallic impurity and excessive reduced iron powder, obtain purified ferrous salt solution;
C. after the iron protochloride filtrating of B step is limpid, open the pressure filter liquid-outlet valve, occlusion pressure filter reverse flow valve is squeezed into iron protochloride filtrating in the main reaction still fast; After press filtration is accomplished, to pour oxalic acid dihydrate solid 223.8kg (according to 1.01 times of the mole numbers of ferrous salt) into, and do not add any dispersion agent, the reinforced time is 45min, is under 60 ℃ in temperature, reaction 60min rises to 90 ℃ to temperature of reaction afterwards again;
D. reaction solution in the C step is fully stirred, and obtain the Ferrox slurry after 2.5 hours in insulation under 90 ℃;
E. separate the Ferrox in the Ferrox slurry through supercentrifuge (the filter cloth space in the whizzer is 5 μ m), rotating speed is 80 commentaries on classics/min, centrifugation time 40min;
F. the Ferrox after will separating obtains the ferrous purity 99.6% of oxalic acid dihydrate through washing after the oven dry, once synthetic granularity is at D
50The Ferrox finished product of=4.5 μ m.
Embodiment 4:
A. in the removal of impurities still, add the 1050kg pure water, start and stir, and add 350kg iron protochloride (solvent and solute weight ratio is 3: 1); Begin heating, make water temperature rise to 93 ℃ after, add reduced iron powder 7kg; Control its reacted pH=3.5, constant temperature stirred 1.5 hours, obtained solution of ferrous chloride;
B. with the ferrous salt solution of A generating step through one group of automatic pressurize closed type chamber-type press filter (model is XAMY40/800-UK), filter simultaneously and remove metallic impurity, nonmetallic impurity and excessive reduced iron powder, obtain purified ferrous salt solution;
C. after the iron protochloride filtrating of B step is limpid, open the pressure filter liquid-outlet valve, occlusion pressure filter reverse flow valve is squeezed into iron protochloride filtrating in the main reaction still fast; After press filtration is accomplished, to pour oxalic acid dihydrate solid 222.7kg (according to 1.005 times of the mole numbers of ferrous salt) into, and do not add any dispersion agent, the reinforced time is 25min, is under 55 ℃ in temperature, reaction 55min rises to 85 ℃ to temperature of reaction afterwards again;
D. reaction solution in the C step is fully stirred, and obtain the Ferrox slurry after 2 hours in insulation under 85 ℃;
E. separate the Ferrox in the Ferrox slurry through supercentrifuge (the filter cloth space in the whizzer is 2 μ m), rotating speed is 50 commentaries on classics/min, centrifugation time 30min;
F. the Ferrox after will separating obtains the ferrous purity 99.6% of oxalic acid dihydrate through washing after the oven dry, once synthetic granularity is at D
50The Ferrox finished product of=3.5 μ m.
The ferrous technical target of the product of case study on implementation mesoxalic acid is following:
Can find out through preparation method of the present invention by last table; The Ferrox finished product that can directly obtain granularity is 3-5 μ m, purity is high; The ferrous salt that utilizes trade waste makes trade waste obtain recycle as basic raw material used in the present invention, improves the quality of environment greatly; Reduce production costs, realize recycling economy and be that green economy all is able to the win-win situation that develops.
Above-mentionedly only several kinds of specific embodiments among the present invention are explained; But can not be as protection scope of the present invention; Every equivalence variation of having done according to the design spirit among the present invention or modification or equal proportion are amplified or are dwindled etc., all should think to fall into protection scope of the present invention.
Claims (5)
1. the preparation method of an iron lithium phosphate reserve battery level iron oxalate is characterized in that: comprise following technical process:
A. in the removal of impurities still, add pure water, start to stir, and be that 0.5～5: 1 amount according to pure water adds the ferrous salt solid according to solvent and solute weight ratio; Begin heating, after water temperature rises to 80～100 ℃, add reduced iron powder with ferrous salt solid weight ratio 0.5～3%; Constant temperature stirred 1～3 hour; Control its reacted pH=2～4, obtain ferrous salt solution, the beginning press filtration;
B. with the ferrous salt solution of A generating step through one group of automatic pressurize closed type chamber-type press filter, filtering metal impurity, nonmetallic impurity and remove excessive reduced iron powder obtain purified ferrous salt solution simultaneously;
C. after the ferrous salt filtrating of B step is limpid, open the pressure filter liquid-outlet valve, ferrous salt filtrating is squeezed in the main reaction still fast; After press filtration is accomplished; Temperature is controlled at 30～60 ℃, gets the oxalic acid dihydrate solid of 1.001～1.05 times of amounts of mole number of said ferrous salt, begins to add the oxalic acid dihydrate solid; The reinforced time is 5～60min, rises to 70～100 ℃ of isothermal reactions to temperature of reaction again after reaction 10～60min;
D. the reaction solution that obtains in the C step is fully stirred, and be incubated 2～4h and carry out ageing, obtain the Ferrox slurry;
E. separate the Ferrox in the Ferrox slurry through whizzer, said centrifuge speed is 30～100 commentaries on classics/min, and the spinning time is 20～60min;
F. the Ferrox after will separating obtains the Ferrox finished product through washing after the oven dry.
2. the preparation method of a kind of iron lithium phosphate reserve battery level iron oxalate according to claim 1 is characterized in that: described ferrous salt is a kind of in iron protochloride, ferrous sulfate and the Iron nitrate;
3. the preparation method of a kind of iron lithium phosphate reserve battery level iron oxalate according to claim 1 and 2 is characterized in that: after water temperature rises to 95 ± 5 ℃ in the said A step, add reduced iron powder.
4. the preparation method of a kind of iron lithium phosphate reserve battery level iron oxalate according to claim 1 and 2 is characterized in that: the filter cloth space in the said E step in the whizzer is 0.1～5 μ m.
5. the preparation method of a kind of iron lithium phosphate reserve battery level iron oxalate according to claim 1 and 2 is characterized in that: the ferrous purity of oxalic acid dihydrate is greater than 99.5%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104030915A (en) * | 2014-06-11 | 2014-09-10 | 湖南海利株洲精细化工有限公司 | Clean preparation method of high-purity ultrafine ferrous 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 |
| CN114649517A (en) * | 2022-03-13 | 2022-06-21 | 江苏乐能电池股份有限公司 | Preparation method of nanoscale carbon composite lithium manganese iron phosphate cathode material for lithium ion battery |
| CN115784873A (en) * | 2022-12-07 | 2023-03-14 | 深圳市环保科技集团股份有限公司 | Method for preparing ferrous oxalate by using stainless steel pickling waste liquid |
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| CN101142138A (en) * | 2005-03-18 | 2008-03-12 | 南方化学股份公司 | Cyclic process for wet-chemically producing lithium metal phosphates |
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| CN101948379A (en) * | 2010-09-01 | 2011-01-19 | 中国科学院宁波材料技术与工程研究所 | Method for preparing battery-level ferrous oxalate |
| CN102225890A (en) * | 2011-04-30 | 2011-10-26 | 湖北浩元材料科技有限公司 | Method for preparing battery-level ferrous oxalate for production of lithium iron phosphate material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104030915A (en) * | 2014-06-11 | 2014-09-10 | 湖南海利株洲精细化工有限公司 | Clean preparation method of high-purity ultrafine ferrous 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 |
| CN114649517A (en) * | 2022-03-13 | 2022-06-21 | 江苏乐能电池股份有限公司 | Preparation method of nanoscale carbon composite lithium manganese iron phosphate cathode material for lithium ion battery |
| CN115784873A (en) * | 2022-12-07 | 2023-03-14 | 深圳市环保科技集团股份有限公司 | Method for preparing ferrous oxalate by using stainless steel pickling waste liquid |
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Address after: No. 608 Nanyuan Road, High tech Industrial Park, Xinyu City, Jiangxi Province, 338015 Patentee after: Jiangxi Ganfeng Lithium Industry Group Co.,Ltd. Address before: No. 608 Nanyuan Road, High tech Industrial Park, Xinyu City, Jiangxi Province, 338015 Patentee before: JIANGXI GANFENG LITHIUM Co.,Ltd. |
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