CN109368612B - Method for preparing battery-grade iron phosphate by using iron phosphate production wastewater and iron phosphate prepared by method - Google Patents
Method for preparing battery-grade iron phosphate by using iron phosphate production wastewater and iron phosphate prepared by method Download PDFInfo
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Abstract
The invention discloses a method for preparing battery-grade iron phosphate by using iron phosphate production wastewater and iron phosphate prepared by the method. The preparation method comprises the following steps: adding water to dilute a mixed solution of ammonium sulfate and monoammonium phosphate in the iron phosphate production wastewater treatment system to obtain a phosphorus source; preparing ferric phosphate dihydrate; washing the molten phosphate dihydrate until the conductivity is less than or equal to 200 us/cm; and (3) carrying out flash evaporation drying on the ferric phosphate dihydrate filter cake, and calcining to obtain the battery-grade ferric phosphate. According to the method, the iron phosphate wastewater with specific monoammonium phosphate and ammonium sulfate contents is used as a phosphorus source, and is subjected to redox reaction with an iron source, an oxidant and the like under specific conditions to prepare the battery-grade iron phosphate by calcination, so that the problem of phosphate radical treatment of an iron phosphate wastewater treatment system is solved, the energy consumption of iron phosphate wastewater treatment is reduced, the reutilization of phosphorus resources in the wastewater is realized, the impurity content of the prepared battery-grade iron phosphate sample is lower than 50ppm, the yield is as high as 95-99%, the production cost of the iron phosphate can be greatly reduced, and the economic benefit is high.
Description
Technical Field
The invention relates to the technical field of new energy materials, and particularly relates to a method for preparing battery-grade iron phosphate by using iron phosphate production wastewater and iron phosphate prepared by the method.
Background
At present, phosphate solution is mainly used as a phosphorus source in the iron phosphate production process on the market, in order to better perform crystal form conversion, the phosphorus is usually 5-15% excessive in the preparation process, and for better washing away sulfate radicals in the product, washing water containing phosphate radicals is adopted, so that the iron phosphate production wastewater contains a large amount of sulfate radicals, ammonium radicals, phosphate radicals and trace other impurity ions. The main process flow of the current mainstream iron phosphate wastewater treatment process is as follows: and adding ammonia water into the iron phosphate production wastewater to adjust the pH value to 6-6.5, so that iron ions, nickel ions, chromium ions and manganese ions in the iron phosphate production wastewater respectively form hydroxide or phosphate precipitates. And then removing the precipitate by plate-and-frame filtration, transferring the filtered ferric phosphate wastewater to a membrane treatment system, and performing first-stage, second-stage and third-stage reverse osmosis concentration. And the concentrated iron phosphate wastewater enters MVR for evaporative crystallization, so that phosphate radicals, sulfate radicals and ammonium radicals in the iron phosphate wastewater are continuously concentrated, the pH value is reduced to 2.5-3.5, and ammonium sulfate with the concentration higher than the saturation is continuously separated out. And then carrying out solid-liquid separation by centrifugation, drying the solid to obtain an ammonium sulfate product with the content of 99.5%, and finally circulating the filtrate back to the MVR for re-evaporation. Since the solubility of monoammonium phosphate is lower than that of ammonium sulfate, in order to ensure the production of ammonium sulfate by-product with a purity of 99.5%, it is necessary to "concentrate" the concentration of monoammonium phosphate in the wastewater as soon as it exceeds saturation, namely: and transferring the mixed solution of the quickly saturated monoammonium phosphate and the ammonium sulfate to untreated iron phosphate sewage for retreatment, or discharging the sewage to a sedimentation tank, adding calcium hydroxide for dephosphorization, and then returning to the MVR for evaporative crystallization. However, discharging the mixed solution of monoammonium phosphate and ammonium sulfate with high concentration to a sewage tank for wastewater treatment again not only increases the energy consumption of wastewater, but also leads to the continuous enrichment of phosphate radicals and the more frequent and more frequent discharge of phosphate radicals along with the increase of the wastewater treatment capacity, thus the problem cannot be fundamentally solved. In addition, calcium hydroxide is used for phosphorus removal, and the generated calcium phosphate byproduct has low additional value and can only be treated as solid waste at low price. The prior art CN201710856857.7 discloses a method for recycling mother liquor in the production process of iron phosphate, wherein phosphorus resources and nitrogen resources in the iron phosphate mother liquor are recycled. The phosphorus source in the method for recycling the phosphorus resource is iron phosphate mother liquor, namely ammonium phosphate and phosphoric acid, although the method improves the utilization rate of phosphorus, ammonium sulfate is generated in the production process, and the problem of continuous enrichment of phosphate radical still exists in the process of treating the production wastewater, so that the recycling method still does not solve the problem of 'concentration discharge'.
Therefore, the preparation method of the battery-grade iron phosphate is of great significance in order to fundamentally solve the 'concentration discharge' problem and improve the added value of the by-product in the wastewater generated in the iron phosphate production.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a method for preparing battery-grade iron phosphate by using iron phosphate production wastewater.
Another object of the present invention is to provide iron phosphate prepared by the method of the present invention.
The above purpose of the invention is realized by the following technical scheme:
a method for preparing battery-grade iron phosphate by using iron phosphate production wastewater comprises the following steps:
s1, preparing a phosphorus source: diluting a mixed solution of ammonium sulfate and monoammonium phosphate in an iron phosphate production wastewater treatment system with water to obtain a phosphorus source, wherein the phosphorus source comprises 5-6% by mass of phosphorus, 7-8% by mass of sulfur and 10-12% by mass of ammonium radicals;
s2, preparing ferric phosphate dihydrate: and (3) mixing the phosphorus source, an iron source, a precipitator and an oxidant in the S1 to perform an oxidation reaction to obtain ferric phosphate dihydrate slurry, wherein the iron source is a solution containing ferrous ions, the reaction pH is 1.8-3.0, the reaction temperature is 80-100 ℃, and the ratio of Fe: p: the molar ratio of the oxidant is 0.99-1.03: 1-1.10: 0.6 to 0.9;
s3, impurity removal: washing the ferric phosphate dihydrate in the S2 until the conductivity is less than or equal to 200us/cm to obtain a ferric phosphate dihydrate filter cake; preferably, the water content of the ferric phosphate dihydrate is 30-40%;
s4, calcining: and calcining the ferric phosphate dihydrate filter cake in S3 to obtain battery-grade ferric phosphate, wherein the calcining temperature is 600-700 ℃.
In the iron phosphate production wastewater treatment process, the mixed solution of monoammonium phosphate and ammonium sulfate in the MVR concentration discharge system has the characteristic of high concentration, wherein the mass content of phosphorus is 10-12%, the mass content of sulfur is 14-16%, and the mass content of ammonium radicals is 20-24%. When a mixed solution of monoammonium phosphate and ammonium sulfate with high concentration is directly used as a phosphorus source, the reaction rate is high, and the control of the product morphology is not facilitated, so that a mixed solution of monoammonium phosphate and ammonium sulfate with low concentration is prepared. When the concentrations of monoammonium phosphate and ammonium sulfate are too low, the concentration discharge frequency of MVR is increased, the sewage treatment efficiency of MVR is affected, the load of sewage treatment is increased, and the solid content of reaction slurry is too low, the yield of a single kettle is too low, and the production efficiency is affected. Therefore, the inventor discovers through a large number of experiments that when the phosphorus source is diluted by adding water, the mass fraction of phosphorus in the phosphorus source is 5-6%, the mass fraction of sulfur in the phosphorus source is 7-8%, and the mass fraction of ammonium radicals in the phosphorus source is 10-12%, the morphology of the product is easy to control, and the prepared product has good quality and does not influence the production efficiency.
Wherein the precipitating agent is preferably ammonia and/or urea.
The water content of the dihydrate ferric phosphate filter cake obtained after washing in the S3 is preferably 30-40%.
Preferably, in the phosphorus source in S1, the mass fraction of phosphorus is 5.5%, the mass fraction of sulfur is 7.5%, and the mass fraction of ammonium radicals is 11%.
Preferably, the reaction pH in S2 is 2.0-2.4. When the reaction pH value is too low, the dihydrate ferric phosphate can not be completely reacted and precipitated, the yield is low, the utilization rate of phosphorus resources in the wastewater is low, and the waste is serious. The pH value of the reaction is higher, ferric hydroxide impurities can be generated in the reaction process, and the ferric hydroxide impurities have fine particles, are easy to adsorb a large amount of impurities and are not beneficial to the quality of products.
Preferably, the reaction time in S2 is 2-6 h. Too long a reaction time will affect the production efficiency and the productivity. The reaction time is too short, the nucleation rate of the ferric phosphate dihydrate in the reaction process is too high, the particles are fine, the specific surface area is large, a large amount of impurities are easily adsorbed, and the impurity content of the product is easily out of standard.
Preferably, the mass fraction of iron in the iron source in S2 is 5-6%. The iron mass fraction is too high, the nucleation rate of the dihydrate ferric phosphate in the reaction process is too high, the particles are fine, the specific surface area is large, a large amount of impurities are easily adsorbed, and the impurity content of the product is higher. The mass fraction of iron is low, the single kettle productivity is low, and the production efficiency is influenced.
Preferably, the iron source in S2 is a ferrous sulfate solution.
Preferably, the oxidant in S2 is peroxyacetic acid and/or hydrogen peroxide.
Preferably, the water washing in S3 is pure water washing. The pure water washing is adopted to reduce the content of impurities such as sulfate radical in the finished iron phosphate product, and the purpose of controlling the conductivity to be less than or equal to 200us/cm is to control the content of the impurities in the finished iron phosphate product.
The filter cake of ferric phosphate dihydrate obtained in step S3 of the present invention is subjected to extrusion treatment.
Preferably, the temperature rise rate in S4 is 1-5 ℃/min. The temperature rising rate is too fast, which is not beneficial to the water vapor discharge in the anhydrous ferric phosphate sintering process and influences the impurity content of the product, when the temperature rising rate is too high, the temperature rising time of the product is too short, the water vapor brought by removing two crystal water from the ferric phosphate dihydrate in the calcining process is not discharged in time, the removed crystal water can take away part of impurities, if the water vapor is not discharged smoothly, the water vapor stays in the product, and the impurity content of the product is higher. Too low a temperature rise rate may affect production efficiency.
More preferably, the temperature rise rate in S4 is 2-3 ℃/min. In the invention, the filter cake of the ferric phosphate dihydrate obtained in the step S4 is calcined after being subjected to flash evaporation and drying treatment.
An iron phosphate prepared by the method of the present invention is also within the scope of the present invention. The battery-grade iron phosphate obtained by the preparation method has the impurity standard that Ca is less than or equal to 50ppm, Mg is less than or equal to 50ppm, Na is less than or equal to 100ppm, K is less than or equal to 100ppm, Cu is less than or equal to 50ppm, Zn is less than or equal to 50ppm, and Ni is less than or equal to 50ppm, and the content of ions such as zinc, nickel, potassium and copper in the battery-grade iron phosphate is less than or equal to 50ppm, and the impurity content is low, so that the quality requirement of the battery-grade iron phosphate is met.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a method for preparing battery-grade iron phosphate by using iron phosphate production wastewater, which is characterized in that the iron phosphate wastewater with specific contents of monoammonium phosphate and ammonium sulfate is used as a phosphorus source, and is subjected to redox reaction with an iron source, an oxidant and the like under specific conditions to calcine and prepare the battery-grade iron phosphate, so that the problem of treatment of phosphate radicals which are continuously enriched in an iron phosphate wastewater treatment system is fundamentally solved, the energy consumption of iron phosphate wastewater treatment is reduced, the reutilization of phosphorus resources in wastewater is realized, the impurity content of a prepared battery-grade iron phosphate sample is lower than 50ppm, the yield is as high as 95-99%, the recycling of the phosphorus resources is realized, the production cost of the iron phosphate can be greatly reduced, and the economic benefit is higher.
Detailed Description
In order to more clearly and completely describe the technical scheme of the invention, the invention is further described in detail by the specific embodiments, and it should be understood that the specific embodiments described herein are only used for explaining the invention, and are not used for limiting the invention, and various changes can be made within the scope defined by the claims of the invention.
Example 1
A method for preparing battery-grade iron phosphate by using iron phosphate production wastewater comprises the following steps:
s1, preparing a phosphorus source: diluting a mixed solution of ammonium sulfate and monoammonium phosphate in a wastewater treatment system for producing iron phosphate with water to obtain a phosphorus source, wherein the mass fraction of phosphorus in the phosphorus source is 5%, the mass fraction of sulfur is 7%, and the mass fraction of ammonium radicals is 10%;
s2, preparing ferric phosphate dihydrate: mixing a phosphorus source, an iron source, an oxidant and a precipitator in S1 to perform an oxidation reaction to obtain ferric phosphate dihydrate, wherein the iron source is a ferrous sulfate solution, the mass fraction of iron in the ferrous sulfate solution is 5.5%, the oxidant is hydrogen peroxide, the precipitator is ammonia water, the reaction pH is 1.8, the reaction temperature is 80 ℃, the reaction time is 4h, and the Fe: p: the molar ratio of the oxidant is 0.99:1: 0.6;
s3, impurity removal: washing the ferric phosphate dihydrate in the S2 until the conductivity is less than or equal to 200us/cm, and extruding to obtain a ferric phosphate dihydrate filter cake with the water content of 30%;
s4, calcining: and (3) flash-evaporating and drying the ferric phosphate dihydrate filter cake in the S3, and calcining to obtain the battery-grade ferric phosphate, wherein the calcining temperature is 650 ℃, and the heating rate is 1 ℃/min.
Example 2
The method for preparing battery-grade iron phosphate by using the wastewater from the iron phosphate production is basically the same as that in example 1, except that the mass fraction of phosphorus in S1 is 6%, the mass fraction of sulfur is 8%, the mass fraction of ammonium radicals is 12%, the iron source is ferrous sulfate, and the mass fraction of iron is 6%.
Example 3
A method for preparing battery-grade iron phosphate by using iron phosphate production wastewater, which is basically the same as that in example 1, is characterized in that the mass fraction of phosphorus in S1 is 6.5%, the mass fraction of sulfur is 7.5%, and the mass fraction of ammonium radicals is 11%.
Example 4
A method for preparing battery-grade iron phosphate from iron phosphate production wastewater, which is substantially the same as in example 1, except that an oxidant for the oxidation reaction in S2 is peracetic acid, and Fe: p: the molar ratio of the oxidizing agent is 1:1.05: 0.7.
Example 5
A method for preparing battery grade iron phosphate from iron phosphate production wastewater, which is substantially the same as in example 1, except that the reaction pH in S2 is 3.0.
Example 6
A method for preparing battery grade iron phosphate from iron phosphate production wastewater, which is substantially the same as in example 1, except that the reaction pH in S2 is 2.4.
Example 7
A method for preparing battery grade iron phosphate from iron phosphate production wastewater, which is substantially the same as in example 1, except that the reaction pH in S2 is 2.0.
Example 8
A method for preparing battery-grade iron phosphate from iron phosphate production wastewater, which is substantially the same as in example 1, except that the temperature rise rate in S4 is 5 ℃/min.
Example 9
A method for preparing battery-grade iron phosphate from iron phosphate production wastewater, which is substantially the same as in example 1, except that the temperature rise rate in S4 is 2 ℃/min.
Example 10
A method for preparing battery-grade iron phosphate from iron phosphate production wastewater, which is substantially the same as in example 1, except that the temperature rise rate in S4 is 3 ℃/min.
Comparative example 1
A method for preparing battery-grade iron phosphate by using iron phosphate production wastewater, which is basically the same as that in example 1, is characterized in that the mass fraction of phosphorus in S1 is 4%, the mass fraction of sulfur is 6%, and the mass fraction of ammonium radicals is 9%.
Comparative example 2
A method for preparing battery-grade iron phosphate by using iron phosphate production wastewater, which is basically the same as that in example 1, is characterized in that the mass fraction of phosphorus in S1 is 7%, the mass fraction of sulfur is 9%, and the mass fraction of ammonium radicals is 13%.
Comparative example 3
A method for preparing battery grade iron phosphate from iron phosphate production wastewater, which is substantially the same as in example 1, except that the conductivity of iron phosphate dihydrate in S3 is washed with water to 280 us/cm.
Comparative examples 4 to 11
A method for preparing battery-grade iron phosphate by using iron phosphate production wastewater, which is basically the same as the embodiment 1, and the specific difference process conditions are shown in table 1.
Wherein, in table 1, a is the reaction pH in S2, B is the reaction temperature in S2, C is Fe: p: the molar ratio of the oxidant, D, is the calcination temperature in S4, DEG C.
TABLE 1
| Item | A | B | C | D |
| Comparative example 4 | 1 | 80 | 0.99:1:0.6 | 650 |
| Comparative example 5 | 4 | 80 | 1:1.05:0.7 | 650 |
| Comparative example 6 | 1.8 | 70 | 1:1.05:0.7 | 650 |
| Comparative example 7 | 1.8 | 110 | 0.99:1:0.6 | 600 |
| Comparative example 8 | 1.8 | 100 | 0.8:1:0.9 | 700 |
| Comparative example 9 | 1.8 | 80 | 1.5:0.9:0.5 | 650 |
| Comparative example 10 | 1.8 | 80 | 0.99:1:0.6 | 500 |
| Comparative example 11 | 1.8 | 80 | 1:1.05:0.7 | 800 |
Results detection and evaluation
The yields of battery grade iron phosphate as described in the examples and comparative examples were calculated as yield per actual product weight per theoretical product weight per batch and are shown in table 2.
TABLE 2
The battery-grade iron phosphate requires that Ca is less than or equal to 50ppm, Mg is less than or equal to 50ppm, Na is less than or equal to 100ppm, K is less than or equal to 100ppm, Cu is less than or equal to 50ppm, Zn is less than or equal to 50ppm, and Ni is less than or equal to 50 ppm. The impurity content of the battery grade iron phosphate samples in the examples and the comparative examples is detected, wherein the detection method comprises the following steps: inductively coupled plasma emission spectrometry, the detecting instrument is: ICP-OES, the detection results are shown in Table 3.
TABLE 3
According to the invention, monoammonium phosphate and ammonium sulfate are used for replacing high-purity phosphate, so that repeated evaporative crystallization of the iron phosphate wastewater can be avoided, energy consumed by repeated crystallization is saved, the recycling of phosphorus resources in the wastewater is realized, and the additional value of the phosphorus resources in the iron phosphate wastewater is improved. Fundamentally solves the 'concentration discharge' problem of iron phosphate wastewater treatment. When the annual output of the industrial production of the iron phosphate is 5000 tons, about 300 tons of phosphorus are enriched in the production wastewater, and by adopting the preparation method, about 300 ten thousand of production cost can be saved, the production cost of the iron phosphate is reduced, and higher economic benefit and environmental protection benefit are achieved.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. It will be understood by those skilled in the art that various other changes and modifications may be made in the above-described embodiments, and it is not necessary, nor is it intended to be exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.
Claims (10)
1. A method for preparing battery-grade iron phosphate by using iron phosphate production wastewater is characterized by comprising the following steps:
s1, preparing a phosphorus source: diluting a mixed solution of ammonium sulfate and monoammonium phosphate in an iron phosphate production wastewater treatment system with water to obtain a phosphorus source, wherein the phosphorus source comprises 5-6% by mass of phosphorus, 7-8% by mass of sulfur and 10-12% by mass of ammonium radicals;
s2, preparing ferric phosphate dihydrate: and (3) mixing the phosphorus source, an iron source, a precipitator and an oxidant in the S1 to perform an oxidation reaction to obtain ferric phosphate dihydrate slurry, wherein the iron source is a solution containing ferrous ions, the reaction pH is 1.8-3.0, the reaction temperature is 80-100 ℃, and the ratio of Fe: p: the molar ratio of the oxidant is 0.99-1.03: 1-1.10: 0.6 to 0.9;
s3, impurity removal: washing the ferric phosphate dihydrate in the S2 until the conductivity is less than or equal to 200us/cm to obtain a ferric phosphate dihydrate filter cake;
s4, calcining: and calcining the ferric phosphate dihydrate filter cake in S3 to obtain battery-grade ferric phosphate, wherein the calcining temperature is 600-700 ℃.
2. The method of claim 1, wherein the phosphorus source in S1 comprises 5.5% by weight phosphorus, 7.5% by weight sulfur, and 11% by weight ammonium groups.
3. The method according to claim 1, wherein the reaction pH in S2 is 2.0 to 2.4.
4. The method according to claim 1, wherein the reaction time in S2 is 2-6 h.
5. The method according to claim 1, wherein the mass fraction of iron in the iron source in S2 is 5-6%.
6. The method of claim 1, wherein the iron source in S2 is a ferrous sulfate solution.
7. The method of claim 1, wherein the oxidant in S2 is peracetic acid and/or hydrogen peroxide.
8. The method according to claim 1, wherein the temperature increase rate of the calcination in S4 is 1 to 5 ℃/min.
9. The method according to claim 8, wherein the temperature increase rate in S4 is 2-3 ℃/min.
10. Iron phosphate prepared by the method of any one of claims 1 to 9.
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| CN109809382B (en) * | 2019-03-28 | 2020-12-11 | 衢州华友钴新材料有限公司 | Method for synthesizing iron phosphate by using waste phosphate generated by precipitating trace heavy metals |
| CN110255520A (en) * | 2019-05-17 | 2019-09-20 | 江苏亨利锂电新材料有限公司 | A kind of method that phosphoric acid prepares battery-grade iron phosphate in extraction industrial wastewater |
| CN110540185A (en) * | 2019-09-17 | 2019-12-06 | 襄阳泽东新能源发展有限公司 | synthesis process of battery-grade iron phosphate |
| CN112624077A (en) * | 2020-12-15 | 2021-04-09 | 广东邦普循环科技有限公司 | Battery-grade iron phosphate and preparation method and application thereof |
| CN113072048B (en) * | 2021-04-09 | 2022-10-04 | 湖北虹润高科新材料有限公司 | Sewage treatment and slag recycling process for producing iron phosphate by sodium method |
| CN113104827B (en) * | 2021-04-25 | 2022-04-29 | 湖北云翔聚能新能源科技有限公司 | Method for preparing battery-grade anhydrous iron phosphate from industrial ammonium phosphate clear solution or industrial ammonium phosphate mother solution |
| CN113636684B (en) * | 2021-08-23 | 2023-04-18 | 江苏贞一环保科技股份有限公司 | Iron phosphate wastewater treatment system and treatment method thereof |
| CN113772647B (en) * | 2021-09-09 | 2023-03-21 | 四川龙蟒磷化工有限公司 | High-purity iron phosphate and method for preparing high-purity iron phosphate by adopting multistage purification method |
| CN114506831B (en) * | 2022-02-22 | 2022-11-08 | 四川大学 | Method for preparing battery-grade anhydrous iron phosphate by using liquid crude monoammonium phosphate |
| CN115448272B (en) * | 2022-09-26 | 2024-02-02 | 深圳永清水务有限责任公司 | Recycling treatment process of aging mother liquor in iron phosphate production process |
| CN115477293B (en) * | 2022-10-11 | 2023-09-08 | 湖北虹润高科新材料有限公司 | Preparation method of anhydrous ferric phosphate with low impurity and high specific surface area |
| CN116902946B (en) * | 2023-09-14 | 2023-11-14 | 北京林立新能源有限公司 | Method for preparing ferric phosphate from iron black |
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| CN107445139B (en) * | 2017-09-21 | 2019-10-29 | 中南大学 | The circulation utilization method of mother liquor in a kind of ferric phosphate production process |
| CN108183234B (en) * | 2018-01-05 | 2020-10-20 | 乳源东阳光磁性材料有限公司 | Preparation method of lithium iron phosphate/carbon composite material |
| CN108439361B (en) * | 2018-04-09 | 2020-08-04 | 杭州电子科技大学 | Preparation method of spherical nano iron phosphate |
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