CN102557916B - 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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- CN102557916B CN102557916B CN201110396502.7A CN201110396502A CN102557916B CN 102557916 B CN102557916 B CN 102557916B CN 201110396502 A CN201110396502 A CN 201110396502A CN 102557916 B CN102557916 B CN 102557916B
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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 special battery-grade ferrous oxalate for lithium iron phosphate.
Background technology
Ferrox molecular formula FeC
2o
42H
2o, existing Ferrox production method mainly contains three major types: 1, by oxalate solution, react and make battery level iron oxalate with ferrous iron solution, its technique shortcoming is that particle is thicker, after must pulverizing, just can obtain the product of 3-5 μ m.If think that a step makes the product of 3-5 μ m, needs adding assistant.2, with oxalic acid solution, react and make battery level iron oxalate with ferrous iron solution, its technique shortcoming is that particle is thicker, after must pulverizing, just can obtain the product of 3-5 μ m.If think that a step makes the product of 3-5 μ m, needs adding assistant.3, with oxalic acid solid, react and make battery level iron oxalate with ferrous iron solution.What patent CN200710165366.4 used is exactly that oxalic acid solid or the oxalic acid that contains solid react and make product with ferrous iron solution, but it need to add the organism such as polyoxyethylene glycol and xitix as tensio-active agent.These three kinds of modes are not that technique is complicated in the past above, need exactly to add other organism, and the battery level iron oxalate particle of manufacture is larger, and purity is not high, and production cost is higher.
Summary of the invention
The present invention completes in order to solve deficiency of the prior art, the object of this invention is to provide that a kind of features simple and practical process, production cost are low, more environmental protection, can by control, add the production technique such as the speed of oxalic acid dihydrate solid, the concentration of ferrous salt and temperature of reaction to make the preparation method of the special battery-grade ferrous oxalate for lithium iron phosphate that granularity is smaller, purity is higher.
The preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate of the present invention, comprises following technical process:
A. in removal of impurities still, add pure water, start and stir, and be according to the amount of pure water to add ferrous salt solid at 0.5～5: 1 according to solvent and solute weight ratio, start heating, water temperature rises to after 80～100 ℃, adds the reduced iron powder with the weight ratio 0.5～3% of ferrous salt solid, constant temperature stirs 1～3 hour, control its reacted pH=2～4, obtain ferrous salt solution, start press filtration;
B. ferrous salt solution A step being produced is by one group of automatic pressure-maintaining closed type chamber-type press filter, and filtering metal impurity, nonmetallic impurity and remove excessive reduced iron powder, obtain pure ferrous salt solution simultaneously;
C. after the ferrous salt filtrate of B step is limpid, open pressure filter liquid-outlet valve, ferrous salt filtrate is squeezed in main reaction still fast; After press filtration completes, temperature is controlled at 30～60 ℃, ℃, get the oxalic acid dihydrate solid of 1.001～1.05 times of amounts of mole number of described ferrous salt, start to add oxalic acid dihydrate solid, feed time is 5～60min, after reaction 10～60min, again temperature of reaction is risen to 70～100 ℃ of isothermal reactions;
D. the reaction solution obtaining in C step is fully stirred, and be incubated 2～4h and carry out ageing, obtain Ferrox slurry;
E. by the Ferrox in the separated Ferrox slurry of whizzer, rotating speed is 30～100 turn/min, centrifugation time 20～60min;
F. by the Ferrox process washing after separation, after oven dry, obtain Ferrox finished product.
The preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate of the present invention can also be:
Described ferrous salt is a kind of in iron protochloride, ferrous sulfate and Iron nitrate.
In described A step, water temperature rises to after 95 ± 5 ℃, adds reduced iron powder.
Described strainer is plate filter or accurate filter.
Filter cloth space in described E step in whizzer is 0.1～5 μ m.
Ferrous oxalate dihydrate purity is greater than 99.5%.
The preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate of the present invention, pass through above-mentioned steps, in terms of existing technologies, its advantage having is because the step adopting is fairly simple, utilizing in ferrous salt solution adds reduced iron powder fully to react, reduce spent acid amount, improve concentration filtration and obtain the Ferrox that purity is higher, reactivity improves greatly, directly obtain the Ferrox particle of 3-5 μ m, product mesoxalic acid ferrous content all >=99.5%, and utilize the ferrous salt of trade waste as basic raw material used in the present invention, make trade waste obtain recycle, greatly improve the quality of environment, reduce production costs, realize recycling economy and be the win-win situation that green economy is all developed.
Embodiment
Below the preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate of the present invention is further described.
The preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate of the present invention,
Comprise following technical process:
A. in removal of impurities still, add pure water, start and stir, and be according to the amount of pure water to add ferrous salt solid at 0.5～5: 1 according to solvent and solute weight ratio, start heating, water temperature rises to after 80～100 ℃, adds the reduced iron powder with the weight ratio 0.5～3% of ferrous salt solid, constant temperature stirs 1～3 hour, control its reacted pH=2～4, obtain ferrous salt solution, start press filtration;
B. ferrous salt solution A step being produced is by one group of automatic pressure-maintaining closed type chamber-type press filter (Shanghai Tian Li pressure filter company limited, model is XAMY40/800-UK), simultaneously filtering metal impurity, nonmetallic impurity and remove excessive reduced iron powder, obtain pure ferrous salt solution;
C. after the ferrous salt filtrate of B step is limpid, open pressure filter liquid-outlet valve, ferrous salt filtrate is squeezed in main reaction still fast; After press filtration completes, temperature is controlled at 30～60 ℃, gets the oxalic acid dihydrate solid of 1.001～1.05 times of amounts of mole number of described ferrous salt, starts to add oxalic acid dihydrate solid, feed time is 5～60min, after reaction 10～60min, again temperature of reaction is risen to 70～100 ℃ of isothermal reactions;
D. the reaction solution obtaining in C step is fully stirred, and be incubated 2～4h and carry out ageing, obtain Ferrox slurry;
E. by the Ferrox in the separated Ferrox slurry of whizzer, rotating speed is 30～100 turn/min, centrifugation time 20～60min;
F. by the Ferrox process washing after separation, after oven dry, obtain Ferrox finished product.
Owing to adopting above-mentioned steps, manufacture iron lithium phosphate special battery-grade ferrous oxalate, the step adopting is fairly simple, utilizing in ferrous salt solution adds reduced iron powder to carry out preliminary removal of impurities, fully reaction, reduce spent acid amount, improve concentration filtration and obtain the Ferrox that purity is higher, reactivity improves greatly, directly obtain the Ferrox particle of 3-5 μ m, product mesoxalic acid ferrous content all >=99.5%, and utilize the ferrous salt of trade waste as basic raw material used in the present invention, make trade waste obtain recycle, greatly improve the quality of environment, reduce production costs, realize recycling economy and be the win-win situation that green economy is all developed.
The preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate of the present invention can also be specifically that described ferrous salt is a kind of in iron protochloride, ferrous sulfate and Iron nitrate.Certainly can also adopt other ferrous salt, the advantage of selecting these several ferrous salts is that these several ferrous salts are more conventional, and price comparison is cheap, and these several ferrous salts derive from Steel Plant, titanium powder plant etc.Can also be that in the above the A step of basis of the technical scheme above, water temperature rises to after 95 ± 5 ℃, add reduced iron powder.The better effects if of removal of impurities like this.In addition, described strainer is that one group of automatic pressure-maintaining closed type chamber-type press filter can be the pressure filter that model that Shanghai Tian Li pressure filter company limited sells is XAMY40/800-UK.
Embodiment 1:
A. in removal of impurities still, add 175kg pure water, start and stir, and add 350kg iron protochloride (solvent and solute weight ratio is 0.5: 1), start heating, water temperature is risen to after 90 ℃, add reduced iron powder 1.75kg, control its reacted pH=2.5, constant temperature stirs 3 hours, obtains solution of ferrous chloride, starts press filtration;
B. ferrous salt solution A step being produced, by one group of automatic pressure-maintaining closed type chamber-type press filter (model is XAMY40/800-UK), filters and removes metallic impurity, nonmetallic impurity and excessive reduced iron powder simultaneously, obtains pure ferrous salt solution;
C. after the iron protochloride filtrate of B step is limpid, open pressure filter liquid-outlet valve, close pressure filter reverse flow valve, iron protochloride filtrate is squeezed in main reaction still fast; After press filtration completes, 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, feed time is 10min, after adding material, in temperature, is at 40 ℃, reaction 30min, rises to 70 ℃ temperature of reaction afterwards again;
D. reaction solution in C step is fully stirred, and obtain Ferrox slurry be incubated 3 hours at 70 ℃ after;
E. by the Ferrox in the separated Ferrox slurry of whizzer (the filter cloth space in whizzer is 0.1 μ m), rotating speed is 100 turn/min, centrifugation time 30min;
F. by Ferrox after separation through washing, after oven dry, obtain purity and be 99.5%, single sintering granularity is 1.5 μ m Ferrox finished products.
Embodiment 2:
A. in removal of impurities still, add 700kg pure water, start and stir, and add 350kg iron protochloride (solvent and solute weight ratio is 2: 1), start heating, water temperature is risen to after 95 ℃, add reduced iron powder 4.5kg, control its reacted pH=3, constant temperature stirs 2 hours, obtains solution of ferrous chloride;
B. ferrous salt solution A step being produced, by one group of automatic pressure-maintaining closed type chamber-type press filter (model is XAMY40/800-UK), filters and removes metallic impurity, nonmetallic impurity and excessive reduced iron powder simultaneously, obtains pure ferrous salt solution;
C. after the iron protochloride filtrate of B step is limpid, open pressure filter liquid-outlet valve, close pressure filter reverse flow valve, iron protochloride filtrate is squeezed in main reaction still fast; After press filtration completes, disposablely 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, feed time is 60min, in temperature, be at 50 ℃, reaction 30min, rises to 100 ℃ temperature of reaction afterwards again;
D. the reaction solution in C step is fully stirred, and obtain Ferrox slurry be incubated 2 hours at 100 ℃ after;
E. by the Ferrox in the separated Ferrox slurry of supercentrifuge (the filter cloth space in whizzer is 1.5 μ m), rotating speed is 30 turn/min, centrifugation time 60min;
F. by Ferrox after separation through washing, after oven dry, obtain purity and be 99.7%, single sintering granularity is 4.3 μ m Ferrox finished products.
Embodiment 3:
A. in removal of impurities still, add 1750kg pure water, start and stir, and add 350kg iron protochloride (solvent and solute weight ratio is 5: 1), start heating, water temperature is risen to after 97 ℃, add reduced iron powder 10.5kg, control its reacted pH=4, constant temperature stirs 1 hour, obtains solution of ferrous chloride;
B. ferrous salt solution A step being produced, by one group of automatic pressure-maintaining closed type chamber-type press filter (model is XAMY40/800-UK), filters and removes metallic impurity, nonmetallic impurity and excessive reduced iron powder simultaneously, obtains pure ferrous salt solution;
C. after the iron protochloride filtrate of B step is limpid, open pressure filter liquid-outlet valve, close pressure filter reverse flow valve, iron protochloride filtrate is squeezed in main reaction still fast; After press filtration completes, 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, feed time is 45min, in temperature, is at 60 ℃, reaction 60min, rises to 90 ℃ temperature of reaction afterwards again;
D. reaction solution in C step is fully stirred, and obtain Ferrox slurry be incubated 2.5 hours at 90 ℃ after;
E. by the Ferrox in the separated Ferrox slurry of supercentrifuge (the filter cloth space in whizzer is 5 μ m), rotating speed is 80 turn/min, centrifugation time 40min;
F. by the Ferrox process washing after separation, obtain ferrous oxalate dihydrate purity 99.6% after oven dry, single sintering granularity is at D
50the Ferrox finished product of=4.5 μ m.
Embodiment 4:
A. in removal of impurities still, add 1050kg pure water, start and stir, and add 350kg iron protochloride (solvent and solute weight ratio is 3: 1), start heating, water temperature is risen to after 93 ℃, add reduced iron powder 7kg, control its reacted pH=3.5, constant temperature stirs 1.5 hours, obtains solution of ferrous chloride;
B. ferrous salt solution A step being produced, by one group of automatic pressure-maintaining closed type chamber-type press filter (model is XAMY40/800-UK), filters and removes metallic impurity, nonmetallic impurity and excessive reduced iron powder simultaneously, obtains pure ferrous salt solution;
C. after the iron protochloride filtrate of B step is limpid, open pressure filter liquid-outlet valve, close pressure filter reverse flow valve, iron protochloride filtrate is squeezed in main reaction still fast; After press filtration completes, 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, feed time is 25min, in temperature, is at 55 ℃, reaction 55min, rises to 85 ℃ temperature of reaction afterwards again;
D. reaction solution in C step is fully stirred, and obtain Ferrox slurry be incubated 2 hours at 85 ℃ after;
E. by the Ferrox in the separated Ferrox slurry of supercentrifuge (the filter cloth space in whizzer is 2 μ m), rotating speed is 50 turn/min, centrifugation time 30min;
F. by the Ferrox process washing after separation, obtain ferrous oxalate dihydrate purity 99.6% after oven dry, single sintering 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 as follows:
As can be seen from the above table by preparation method of the present invention, the Ferrox finished product that can directly obtain granularity is 3-5 μ m, purity is high, utilize the ferrous salt of trade waste as basic raw material used in the present invention, make trade waste obtain recycle, greatly improve the quality of environment, reduce production costs, realize recycling economy and be the win-win situation that green economy is all developed.
Above-mentionedly only several specific embodiments in the present invention are illustrated; but can not be as protection scope of the present invention; every equivalence variation of having done according to the design spirit in the present invention or modification or equal proportion zoom in or out etc., all should think and fall into protection scope of the present invention.
Claims (5)
1. a preparation method for special battery-grade ferrous oxalate for lithium iron phosphate, is characterized in that: comprise following technical process:
A. in removal of impurities still, add pure water, start and stir, and be that 0.5～5:1 adds ferrous salt solid according to the amount of pure water according to solvent and solute weight ratio, start heating, water temperature rises to after 80～100 ℃, adds the reduced iron powder with the weight ratio 0.5～3% of ferrous salt solid, constant temperature stirs 1～3 hour, control its reacted pH=2～4, obtain ferrous salt solution, start press filtration;
B. ferrous salt solution A step being produced is by one group of automatic pressure-maintaining closed type chamber-type press filter, and filtering metal impurity, nonmetallic impurity and remove excessive reduced iron powder, obtain pure ferrous salt solution simultaneously;
C. after the ferrous salt filtrate of B step is limpid, open pressure filter liquid-outlet valve, ferrous salt filtrate is squeezed in main reaction still fast; After press filtration completes, temperature is controlled at 30～60 ℃, gets the oxalic acid dihydrate solid of 1.001～1.05 times of amounts of mole number of described ferrous salt, starts to add oxalic acid dihydrate solid, feed time is 5～60min, after reaction 10～60min, again temperature of reaction is risen to 70～100 ℃ of isothermal reactions;
D. the reaction solution obtaining in C step is fully stirred, and be incubated 2～4h and carry out ageing, obtain Ferrox slurry;
E. by the Ferrox in the separated Ferrox slurry of whizzer, described centrifuge speed is 30～100 turn/min, and the centrifugation time is 20～60min;
F. by the Ferrox process washing after separation, after oven dry, obtain Ferrox finished product.
2. the preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate according to claim 1, is characterized in that: described ferrous salt is a kind of in iron protochloride, ferrous sulfate and Iron nitrate.
3. the preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate according to claim 1 and 2, is characterized in that: in described A step, water temperature rises to after 95 ± 5 ℃, adds reduced iron powder.
4. the preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate according to claim 1 and 2, is characterized in that: the filter cloth space in described E step in whizzer is 0.1～5 μ m.
5. the preparation method of a kind of special battery-grade ferrous oxalate for lithium iron phosphate according to claim 1 and 2, is characterized in that: Ferrox purity is greater than 99.5%.
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| CN104030915B (en) * | 2014-06-11 | 2016-04-27 | 湖南海利株洲精细化工有限公司 | A kind of clean method for preparing of high-purity super fine Ferrox |
| 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 |
| CN116253302A (en) * | 2022-12-27 | 2023-06-13 | 衢州华友钴新材料有限公司 | Method and system for recovering lithium iron phosphate |
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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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| 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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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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