CN110590034A - Process treatment method for lithium iron wastewater of lithium battery anode material - Google Patents
Process treatment method for lithium iron wastewater of lithium battery anode material Download PDFInfo
- Publication number
- CN110590034A CN110590034A CN201910184136.5A CN201910184136A CN110590034A CN 110590034 A CN110590034 A CN 110590034A CN 201910184136 A CN201910184136 A CN 201910184136A CN 110590034 A CN110590034 A CN 110590034A
- Authority
- CN
- China
- Prior art keywords
- water
- wastewater
- lithium iron
- concentration
- treatment method
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/28—Ammonium phosphates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C05—FERTILISERS; MANUFACTURE THEREOF
- C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
- C05F7/00—Fertilisers from waste water, sewage sludge, sea slime, ooze or similar masses
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/14—Maintenance of water treatment installations
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Water Supply & Treatment (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Fertilizers (AREA)
Abstract
The invention discloses a process treatment method for lithium iron wastewater of a lithium battery anode material, which comprises the following steps: filtering the lithium iron phosphate industrial wastewater by a plate frame to remove the residual lithium iron phosphate, mixing the obtained filtrate with the secondary mother liquor of the MVR system of the iron phosphate wastewater, and adding H2O2Removing COD, adjusting the pH value of the mixed solution, and forming hydroxide precipitates from metal ions in the mixed solution through two-step precipitation; removing the precipitate of the treatment liquid by a plate-and-frame filter press, and then allowing the treatment liquid to enter a TUF tubular microfiltration system to remove organic matters or large-particle colloidal substances and the like in pores of a tubular microfiltration membrane tube; the TUF tube test microfiltration produced water enters an MVR machine through a secondary concentration RO device to be evaporated so as to produce ammonium sulfate and ammonium dihydrogen phosphate; second stageFresh water produced by the concentration RO device is purified by the terminal RO device and then is used for the production of the workshop. The process treatment method has stable process operation, high added value of products and zero discharge of sewage.
Description
Technical Field
The invention relates to the technical field of industrial wastewater treatment, and particularly relates to a purification treatment method for lithium iron phosphate production wastewater.
Background
The lithium iron chemical wastewater is chemical mother liquor wastewater generated in the process of preparing a new energy battery precursor material lithium iron phosphate, a lithium iron phosphate precursor can generate a large amount of acidic wastewater (pH is less than 2) in the washing and separating processes, and the wastewater pollution factors are mainly high-concentration ammonia nitrogen and phosphate and also contain pollutants such as sulfate. If the treatment is carried out by an alkali-adding ammonia distillation method, a large amount of alkali is consumed, so that the cost is overhigh; if a calcium method is adopted to adjust the pH value, on one hand, ardealite which is difficult to utilize is generated, on the other hand, the subsequent ammonia stripping tower or ammonia distilling tower is blocked due to high calcium content because further stripping or steam stripping is needed based on high ammonia nitrogen, the subsequent treatment difficulty is increased easily, unnecessary treatment problems are caused, the cost is increased, and the economic benefit is poor. In addition to the above, the research on the treatment of the wastewater in the prior art mainly aims at the removal of ammonia nitrogen and does not record the research on the deep treatment of phosphate radical and sulfate radical ions, the wastewater after deamination still contains sulfate radical and phosphate radical ions, and the direct discharge not only pollutes the environment but also wastes phosphorus and sulfur resources. Therefore, the inventor develops a new process for realizing full-component resource recycling of the lithium iron phosphate production wastewater on the basis of the existing research on the treatment of the lithium iron phosphate production wastewater, the process has the advantages of low cost, stable treatment effect, realization of zero wastewater discharge, high market value of the obtained product and good economic benefit. In addition, the phosphorus and nitrogen containing industrial wastewater is treated by removing nitrogen and phosphorus components in a water body by a biological method to meet the requirement of purifying water quality, but the growth and propagation conditions of biological bacteria need to control a plurality of process conditions, so that the difficulty of long-term stable operation of biological sludge treatment is increased, simultaneously sludge bottom mud belongs to strict control waste, and the complicated subsequent treatment means and high treatment cost of the sludge are adverse factors limiting the application of the biological method process.
At present, a wastewater treatment method which has stable technology and high product added value and is highly in accordance with the national environmental protection policy and has the lowest environmental risk is urgently needed to be found.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a process treatment method for treating the lithium iron industrial wastewater, which has the advantages of stable production and operation, 100% recovery of nitrogen and phosphorus, environmental protection, high efficiency and zero sewage discharge. Particularly, according to the waste water component characteristics and the specific component content state, the pH value of the mixture is 3-4 after the mixture of the frame filtration → the lithium iron waste water filtrate and the secondary mother liquor is mixed, and H is added2O2With Fe in the wastewaterThe method comprises the steps of removing COD through the catalytic action enhanced oxidation reaction generated by impurity ions such as Mn → one-step precipitation → plate frame filtration → two-step precipitation → slurry is subjected to pipe trial microfiltration → plate frame filtration → RO system → mechanical evaporation, and replaces the traditional treatment process, so that phosphorus and nitrogen resources in the wastewater are recycled by 100%, and fresh water produced by the RO system is recycled to a workshop to realize zero-emission wastewater treatment in the true sense.
In order to achieve the purpose, the invention adopts the following technical scheme:
a process treatment method of lithium iron industrial wastewater comprises the following steps:
(1) lifting the lithium iron phosphate production wastewater to a collection water tank by a pump, and then starting a feed pump to a plate-and-frame filter press to remove undissolved-solid lithium iron phosphate residual materials in water slurry;
(2) mixing the filtrate with the secondary mother liquor of the MVR system of the ferric phosphate wastewater, and adding H2O2Removing COD in the mixed solution, and discharging the mixed solution into a mother solution recovery water tank after the concentration of the COD is reduced to 80-100 mg/L;
(3) pumping the treated mixed solution to a mixing reaction tank, adding ammonia water to adjust the pH value to be 4.8-5.2, and stirring to react to obtain Fe in the wastewater3＋Ion formation Fe (OH)3Precipitating, and removing after plate-and-frame filter pressing; adjusting the pH value of the one-step precipitation filtrate to be within the range of 8.5-9.0 by adding ammonia through a pipeline mixer, enabling the formed slurry pump to enter a tube-test microfiltration water supply tank, starting a feed pump to a plate-and-frame filter press to perform two-step precipitation when the slurry concentration in the water supply tank reaches 20-25%, mainly removing Ca, Mg and Mn in the wastewater by forming hydroxide precipitation through the two-step precipitation, adsorbing and wrapping a certain amount of phosphorus and nitrogen salts in the formed two-step precipitation filter mud, drying the two-step precipitation filter mud, then selling the two-step precipitation filter mud as a compound fertilizer raw material, and recycling the filtrate into the water;
(4) the slurry in the water supply tank enters a TUF tube for micro-filtration by a booster pump, the water inlet pressure is 0.5MPa, the water outlet pressure is 0.05MPa, and chemical cleaning (5 percent H) is started after physical back washing for 15 seconds2O2+3%H2SO4) Circularly cleaning for 2h, soaking for 12h, and removing the pores of the microfiltration membrane tube in the tube testOrganic substances or large-particle colloidal substances of (2);
(5) concentrating the TUF tube-test microfiltration produced water by a secondary concentration RO device until the conductivity reaches 120000-130000 mu s, and then mechanically evaporating the concentrated water in an MVR to produce industrial superior ammonium sulfate and qualified ammonium dihydrogen phosphate; and the fresh water produced by the secondary concentration RO device is purified by the terminal RO device to obtain pure water for the production and use of the workshop.
The invention has the following beneficial effects:
1. after filter mud obtained by pretreating lithium iron phosphate wastewater by using a plate-and-frame filter press is dried, the content of P2O5 is up to 50-52%, and the lithium iron phosphate wastewater can be sold as an agricultural phosphate fertilizer raw material; the pH value of the mixed filtrate (pH value of 7-8) and the secondary mother liquor (pH value of 2-3) is 3-4, and metal impurities such as Fe, Mn and the like in the secondary mother liquor generate catalytic action under acidic condition, so that H is strengthened2O2The oxidation of the catalyst is helpful for reducing COD in the filtrate to 80-100 mg/L;
2. after the wastewater is treated by the one-step precipitation and the two-step precipitation processes, metal impurity ions of iron, manganese, calcium and magnesium in the wastewater are removed by more than 99 percent, so that water quality guarantee is provided for the subsequent tube test microfiltration device to produce water to enter an RO system and an MVR system; meanwhile, after the sludge generated by precipitation is dried by a paddle dryer, a certain amount of phosphorus and nitrogen salts are adsorbed and coated, so that the sludge can be sold as a high-value compound fertilizer raw material;
3. the water yield reaches 75-85% under the normal operation condition of the tube test microfiltration device, the water yield conductivity is 40000-50000 mu s, the water yield can be concentrated by a secondary concentration RO device until the conductivity reaches 120000-130000 mu s, and then the water yield is subjected to MVR mechanical evaporation to produce industrial superior ammonium sulfate and qualified ammonium dihydrogen phosphate, so that the product added value of byproducts is greatly improved;
4. the conductivity of the pure water produced after the fresh water produced by the secondary concentration RO device is purified by the terminal RO device is less than 10 mus, and the pH value of 6-7 completely meets the water quality requirement for workshop production, so that the comprehensive utilization of waste resources, the closed circulation of water and the zero emission of wastewater are realized.
Detailed Description
The advantages and features of the present invention will become more apparent from the following description of the embodiments of the invention given by way of example. These examples are illustrative only and do not limit the scope of the present invention in any way. It will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention, and that such changes and modifications may be made without departing from the spirit and scope of the invention.
Example 1
The treatment process of the lithium iron industrial wastewater comprises the following steps:
(1) removing undissolved-solid lithium iron phosphate residue in water slurry from the lithium iron wastewater by a plate-and-frame filter press, drying the produced filter mud, and then drying the dried filter mud to obtain P2O5The content is up to 50.5 percent, the product can be sold as agricultural phosphate fertilizer raw material, the filtrate and the secondary mother liquor are mixed and stirred evenly, and then H accounting for 5 percent of the total amount of the waste water is added2O2COD which is oxidized and removed with the concentration of 1250mg/L is reduced to 98mg/L and is discharged into a mother liquor recovery water tank. Pumping the wastewater into a mixing reaction tank, adding ammonia to adjust the pH value to 4.9, and stirring to react to obtain Fe in the wastewater3＋Formation of Fe (OH)3Removing the precipitate, press-filtering with plate-frame filter press, treating the filter press water in the subsequent process, spirally conveying the formed one-step precipitate filter mud to a blade dryer for treatment, wherein the obtained one-step precipitate drying material has N content of 7.5 percent and P content2O5Content 42.8%, H2The O content is 4.7%.
(2) Adjusting the pH value of the one-step precipitation filtrate to 8.6 by adding ammonia through a pipeline mixer, pumping the formed slurry into a tube-test microfiltration water supply tank, starting a feed pump to a plate-and-frame filter press when the slurry concentration in the water supply tank reaches 22%, mainly removing Ca, Mg and Mn in wastewater by forming hydroxide precipitates through two-step precipitation, wherein the removal rates of the hydroxide precipitates reach more than 99%, and feeding the formed two-step precipitation filter mud into a paddle dryer for drying to obtain a two-step precipitation drying material with the N content of 8.3% and the P content of 8.3% respectively2O5Content 43.5%, H2The O content is 5.0 percent, and the filtrate is recycled to the water tank for cycle concentration.
(3) The slurry in the water supply tank enters a TUF tube for micro-filtration by a booster pump, the water inlet pressure is 0.5MPa, the water outlet pressure is 0.04MPa, the water yield reaches 81 percent, and the water yield is attenuated to 75 percentThe water production function of the tube-test microfiltration can be recovered by physical backwashing for 15 seconds after the water production, and if the physical backwashing can not achieve the expected effect after long-time operation, chemical cleaning is started (5% H)2O2+3%H2SO4) Circularly cleaning for 2h, soaking for 12h, removing organic matters or large-particle colloidal substances and the like in pores of the tube test microfiltration membrane tube, and recovering the designed water yield of the tube test microfiltration.
(4) TUF tube test micro-filtration produces water conductance at 45600 mus, can concentrate through second grade concentration RO device to the conductance reaches 125000 mus, then gets into MVR mechanical evaporation and can produce industry superior quality article ammonium sulfate and qualification product ammonium dihydrogen phosphate, the product added value of very big improvement by-product.
(5) The fresh water produced by the secondary concentration RO device is purified by the terminal RO device to obtain pure water for workshop production and use, thus realizing the purposes of comprehensive utilization of material resources, closed cycle of water and zero discharge of waste water.
Example 2
The treatment process of the phosphate industrial wastewater comprises the following steps:
(1) removing undissolved-solid lithium iron phosphate residue in water slurry from the lithium iron wastewater by a plate-and-frame filter press, drying the produced filter mud, and then drying the dried filter mud to obtain P2O5The content is as high as 51.3 percent, the product can be sold as agricultural phosphate fertilizer raw material, the filtrate and the secondary mother liquor are mixed and stirred evenly, and then H accounting for 5 percent of the total amount of the waste water is added2O2COD with 1350mg/L concentration removed by oxidation is reduced to 100mg/L and discharged into a mother liquor recovery water tank. Pumping the wastewater into a mixing reaction tank, adding ammonia to adjust the pH value to 5.1, and stirring to react to obtain Fe in the wastewater3＋Formation of Fe (OH)3Removing the precipitate, press-filtering with plate-frame filter press, treating the filter-pressing water in the subsequent process, spirally conveying the formed one-step precipitate filter mud to a blade dryer for treatment, wherein the obtained one-step precipitate drying material has 8.3% of N and P2O5Content 41.8%, H2The O content is 5.2%.
(2) Adjusting pH value of the filtrate obtained by the first-step precipitation to 8.8 by adding ammonia through a pipeline mixer, pumping the formed slurry into a tube-test microfiltration water supply tank, starting a feed pump to a plate-and-frame filter press when the concentration of the slurry in the water supply tank reaches 21.8%, and performing the second-step precipitation mainlyRemoving Ca, Mg and Mn in the wastewater to form hydroxide precipitates, wherein the removal rate reaches more than 99 percent, the formed two-step precipitate filter mud enters a paddle dryer to be dried to obtain a two-step precipitate drying material with the N content of 7.9 percent and the P content of 7.9 percent2O5Content 40.5%, H2The O content is 4.6 percent, and the filtrate is recycled to the water tank for cycle concentration.
(3) The slurry in the water supply tank enters a TUF tube for micro-filtration by a booster pump, the water inlet pressure is 0.5MPa, the water outlet pressure is 0.05MPa, the water yield reaches 78.5 percent, the water yield is attenuated to be below 75 percent, the water production function of the tube micro-filtration can be recovered by physical back-washing for 15 seconds, and if the physical back-washing can not reach the expected effect after long-time operation, chemical cleaning is started (5 percent H is used for carrying out micro-filtration), and the water quality of the water is improved2O2+3%H2SO4) Circularly cleaning for 2h, soaking for 12h, removing organic matters or large-particle colloidal substances and the like in pores of the tube test microfiltration membrane tube, and recovering the designed water yield of the tube test microfiltration.
(4) TUF tube test micro-filtration produces water conductance at 43800 mus, can concentrate to the conductance reaches 116000 mus through second grade concentration RO device, then gets into MVR mechanical evaporation and can produce industry superior product ammonium sulfate and qualification product ammonium dihydrogen phosphate, the product added value of very big improvement by-product.
(5) The fresh water produced by the secondary concentration RO device is purified by the terminal RO device to obtain pure water for workshop production and use, thus realizing the purposes of comprehensive utilization of material resources, closed cycle of water and zero discharge of waste water.
Example 3
The treatment process of the phosphate industrial wastewater comprises the following steps:
(1) removing undissolved-solid lithium iron phosphate residue in water slurry from the lithium iron wastewater by a plate-and-frame filter press, drying the produced filter mud, and then drying the dried filter mud to obtain P2O5The content is as high as 51.9 percent, the product can be sold as an agricultural phosphate fertilizer raw material, the filtrate and the secondary mother liquor are mixed and stirred evenly, and then H accounting for 5 percent of the total amount of the wastewater is added2O2COD removed by oxidation at a concentration of 1330mg/L is reduced to 85mg/L and discharged into a mother liquor recovery water tank. Pumping the wastewater into a mixing reaction tank, adding ammonia to adjust the pH value to 5.2, and stirring to react to obtain Fe in the wastewater3＋Formation of Fe (OH)3Removing the precipitate, press-filtering with plate-frame filter press, treating the filter press water in the subsequent process, spirally conveying the formed one-step precipitate filter mud to a blade dryer for treatment, wherein the obtained one-step precipitate drying material has N content of 7.1 percent and P content2O5Content 40.9%, H2The O content is 4.7%.
(2) Adjusting pH value of the filtrate obtained by the first-step precipitation to 9.0 by adding ammonia through a pipeline mixer, pumping the formed slurry into a tube-test microfiltration water supply tank, starting a feed pump to a plate-and-frame filter press when the slurry concentration in the water supply tank reaches 20.3%, removing Ca, Mg and Mn in the wastewater by forming hydroxide precipitates by the second-step precipitation, wherein the removal rates of the hydroxide precipitates reach more than 99%, and drying the formed second-step precipitation filter mud in a blade dryer to obtain a second-step precipitation drying material with the N content of 8.8%, and the P content of the drying material2O5Content 42.4%, H2The O content is 4.9 percent, and the filtrate is recycled to the water tank for cycle concentration.
(3) The slurry in the water supply tank enters a TUF pipe for micro-filtration by a booster pump, the water inlet pressure is 0.5MPa, the water outlet pressure is 0.04MPa, the water production rate reaches 82 percent, the water production rate is attenuated to be below 75 percent, the water production function of the pipe micro-filtration can be recovered by physical back-washing for 15 seconds, and if the physical back-washing cannot reach the expected effect after long-time operation, chemical cleaning is started (5 percent H)2O2+3%H2SO4) Circularly cleaning for 2h, soaking for 12h, removing organic matters or large-particle colloidal substances and the like in pores of the tube test microfiltration membrane tube, and recovering the designed water yield of the tube test microfiltration.
(4) TUF pipe examination microfiltration produces water conductance at 44700 mus, can concentrate through second grade concentration RO device to the conductance reaches 135000 mus, then gets into MVR mechanical evaporation and can produce industry quality product ammonium sulfate and qualification product ammonium dihydrogen phosphate, the product added value of very big improvement by-product.
(5) The fresh water produced by the secondary concentration RO device is purified by the terminal RO device to obtain pure water for workshop production and use, thus realizing the purposes of comprehensive utilization of material resources, closed cycle of water and zero discharge of waste water.
Claims (6)
1. A technical treatment method for lithium iron wastewater of a lithium battery anode material is characterized by comprising the following stepsThe method comprises the following steps: (1) lifting the lithium iron phosphate production wastewater to a collection water tank by a pump, then starting a feed pump to a plate-and-frame filter press to remove impurities in water slurry to obtain filter mud, and carrying out heat treatment on the filter mud to obtain an agricultural phosphate fertilizer raw material; (2) mixing the filtrate with the secondary mother liquor of the MVR system of the ferric phosphate wastewater, and adding H2O2Removing COD in the mixed solution; (3) lifting the treated mixed liquor to a mixing reaction tank by a pump, adding ammonia water to adjust the pH value to form a one-step precipitate, adding the one-step precipitate filtrate to a tubular microfiltration water supply tank by a slurry pump formed by adding ammonia water to adjust the pH value by a pipeline mixer, starting a feed pump to a plate-and-frame filter press to remove the two-step precipitate after the slurry reaches a certain concentration, and recovering the filtrate to the water tank for cyclic concentration; (4) the slurry in the water supply tank enters a TUF pipe for micro-filtration test through a booster pump, the produced water enters an RO system, and the chemical yield is improved by adopting a physical back-washing and chemical cleaning process; (5) the water produced by the TUF tube-test microfiltration passes through a secondary concentration RO device, and the concentrated water enters MVR mechanical evaporation to produce industrial superior ammonium sulfate and qualified ammonium dihydrogen phosphate; and the fresh water produced by the secondary concentration RO device is purified by the terminal RO device to obtain pure water for the production and use of the workshop.
2. The process treatment method for the lithium iron wastewater of the lithium battery positive electrode material according to claim 1, characterized by comprising the following steps: and (2) carrying out heat treatment on the filter mud obtained in the step (1) to obtain an agricultural phosphate fertilizer raw material.
3. The process treatment method for the lithium iron wastewater of the lithium battery positive electrode material according to claim 1, characterized by comprising the following steps: mixing the filtrate obtained in the step (2) with secondary mother liquor of the phosphorus-iron wastewater MVR system in a ratio of 1:1, and adding H2O2The concentration is 30 percent, and the adding ratio is once adding according to 5 percent of the total amount of the mixed solution.
4. The process treatment method for the lithium iron wastewater of the lithium battery positive electrode material according to claim 1, characterized by comprising the following steps: adding ammonia water into the mixed reaction tank in the step (3), and controlling the pH value of the solution to be 4.8-5.2 to form a one-step precipitate; and adding ammonia water into the one-step precipitation filter to control the pH value of the filtrate to be 8.5-9.0, controlling the concentration of slurry in the water supply tank to be 20-25%, and starting a feed pump to a plate-and-frame filter press to remove the two-step precipitate.
5. The process treatment method for the lithium iron wastewater of the lithium battery positive electrode material according to claim 1, characterized by comprising the following steps: the water inlet pressure in the step (4) is set to be 0.5MPa, the water outlet pressure is set to be 0.05MPa, and chemical cleaning (5% H) is started after physical backwashing is carried out for 15 seconds2O2+3%H2SO4) Circularly cleaning for 2h, and soaking for 12 h.
6. The process treatment method for the lithium iron wastewater of the lithium battery positive electrode material according to claim 1, characterized by comprising the following steps: conducting conductance of TUF tube test microfiltration produced water at 40000-50000 mu s, concentrating the water by a secondary concentration RO device until the conductance reaches 120000-130000 mu s, and then mechanically evaporating the water by MVR to produce industrial superior ammonium sulfate and qualified ammonium dihydrogen phosphate; and the fresh water produced by the secondary concentration RO device is purified by the terminal RO device to obtain pure water for the production and use of the workshop.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910184136.5A CN110590034A (en) | 2019-03-12 | 2019-03-12 | Process treatment method for lithium iron wastewater of lithium battery anode material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910184136.5A CN110590034A (en) | 2019-03-12 | 2019-03-12 | Process treatment method for lithium iron wastewater of lithium battery anode material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110590034A true CN110590034A (en) | 2019-12-20 |
Family
ID=68852446
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201910184136.5A Pending CN110590034A (en) | 2019-03-12 | 2019-03-12 | Process treatment method for lithium iron wastewater of lithium battery anode material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110590034A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453911A (en) * | 2020-04-30 | 2020-07-28 | 成都思达能环保设备有限公司 | Treatment method and system of ternary precursor washing water |
| CN113233672A (en) * | 2020-12-31 | 2021-08-10 | 四川思达能环保科技有限公司 | Treatment process for anode material wastewater |
| CN115124178A (en) * | 2022-07-21 | 2022-09-30 | 江苏卓博环保科技有限公司 | Recycling treatment device and method for wastewater generated in iron phosphate production by ammonia process |
| CN115448534A (en) * | 2022-09-05 | 2022-12-09 | 湖北朗润环保科技有限公司 | Treatment method and system for lithium iron phosphate wastewater |
| CN116655140A (en) * | 2023-04-13 | 2023-08-29 | 湖北朗润环保科技有限公司 | Lithium iron phosphate cleaning wastewater recovery and treatment method and system |
| WO2025065149A1 (en) * | 2023-09-25 | 2025-04-03 | 屏南时代新材料技术有限公司 | Recovery system and recovery method for lithium-iron-phosphate precursor slurry iron-discharge sewage |
Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010058048A (en) * | 2008-09-03 | 2010-03-18 | Tohoku Koeki Kk | Method for treating fluorine-containing wastewater using titanium oxide and metatitanic acid |
| CN101948197A (en) * | 2010-09-27 | 2011-01-19 | 中国环境科学研究院 | Method for treating high-concentration phosphonomycin pharmaceutical wastewater and reclaiming phosphorus |
| CN102173519A (en) * | 2011-03-18 | 2011-09-07 | 太仓华辰净化设备有限公司 | Membrane integration technology based process for treating wastewater containing inorganic phosphorous |
| CN104628206A (en) * | 2015-02-11 | 2015-05-20 | 北京赛科康仑环保科技有限公司 | Recycling technique of lithium iron phosphate production wastewater |
| CN104628217A (en) * | 2013-11-12 | 2015-05-20 | 天津卡特化工技术有限公司 | Method for recovery treatment of waste-and-old lithium battery electrolyte and treatment of electrolyte wastewater |
| CN206692499U (en) * | 2017-02-09 | 2017-12-01 | 杭州上拓环境科技股份有限公司 | A kind of processing system of ferric phosphate production waste water |
| CN108147566A (en) * | 2017-12-22 | 2018-06-12 | 上海第二工业大学 | A method for catalytically degrading organic wastewater using waste lithium-ion battery cathode materials |
| CN108675529A (en) * | 2018-04-20 | 2018-10-19 | 深圳市华虹清源环保科技有限公司 | A method of the phosphatic waste water of processing |
| CN108675568A (en) * | 2018-07-13 | 2018-10-19 | 苏州爱源环境工程技术服务有限公司 | A kind of Lithium Battery Industry waste water purification system |
| CN109207730A (en) * | 2018-09-19 | 2019-01-15 | 中国科学院青海盐湖研究所 | A kind of method and system recycling lithium from waste lithium iron phosphate battery |
-
2019
- 2019-03-12 CN CN201910184136.5A patent/CN110590034A/en active Pending
Patent Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010058048A (en) * | 2008-09-03 | 2010-03-18 | Tohoku Koeki Kk | Method for treating fluorine-containing wastewater using titanium oxide and metatitanic acid |
| CN101948197A (en) * | 2010-09-27 | 2011-01-19 | 中国环境科学研究院 | Method for treating high-concentration phosphonomycin pharmaceutical wastewater and reclaiming phosphorus |
| CN102173519A (en) * | 2011-03-18 | 2011-09-07 | 太仓华辰净化设备有限公司 | Membrane integration technology based process for treating wastewater containing inorganic phosphorous |
| CN104628217A (en) * | 2013-11-12 | 2015-05-20 | 天津卡特化工技术有限公司 | Method for recovery treatment of waste-and-old lithium battery electrolyte and treatment of electrolyte wastewater |
| CN104628206A (en) * | 2015-02-11 | 2015-05-20 | 北京赛科康仑环保科技有限公司 | Recycling technique of lithium iron phosphate production wastewater |
| CN206692499U (en) * | 2017-02-09 | 2017-12-01 | 杭州上拓环境科技股份有限公司 | A kind of processing system of ferric phosphate production waste water |
| CN108147566A (en) * | 2017-12-22 | 2018-06-12 | 上海第二工业大学 | A method for catalytically degrading organic wastewater using waste lithium-ion battery cathode materials |
| CN108675529A (en) * | 2018-04-20 | 2018-10-19 | 深圳市华虹清源环保科技有限公司 | A method of the phosphatic waste water of processing |
| CN108675568A (en) * | 2018-07-13 | 2018-10-19 | 苏州爱源环境工程技术服务有限公司 | A kind of Lithium Battery Industry waste water purification system |
| CN109207730A (en) * | 2018-09-19 | 2019-01-15 | 中国科学院青海盐湖研究所 | A kind of method and system recycling lithium from waste lithium iron phosphate battery |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111453911A (en) * | 2020-04-30 | 2020-07-28 | 成都思达能环保设备有限公司 | Treatment method and system of ternary precursor washing water |
| CN113233672A (en) * | 2020-12-31 | 2021-08-10 | 四川思达能环保科技有限公司 | Treatment process for anode material wastewater |
| CN115124178A (en) * | 2022-07-21 | 2022-09-30 | 江苏卓博环保科技有限公司 | Recycling treatment device and method for wastewater generated in iron phosphate production by ammonia process |
| CN115124178B (en) * | 2022-07-21 | 2024-06-11 | 江苏卓博环保科技有限公司 | Recycling treatment device and method for wastewater from ammonia ferric phosphate production |
| CN115448534A (en) * | 2022-09-05 | 2022-12-09 | 湖北朗润环保科技有限公司 | Treatment method and system for lithium iron phosphate wastewater |
| CN116655140A (en) * | 2023-04-13 | 2023-08-29 | 湖北朗润环保科技有限公司 | Lithium iron phosphate cleaning wastewater recovery and treatment method and system |
| WO2025065149A1 (en) * | 2023-09-25 | 2025-04-03 | 屏南时代新材料技术有限公司 | Recovery system and recovery method for lithium-iron-phosphate precursor slurry iron-discharge sewage |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110590034A (en) | Process treatment method for lithium iron wastewater of lithium battery anode material | |
| CN101555053B (en) | A composite coagulant and treatment method that can be used to treat rare earth high-concentration ammonia nitrogen wastewater and recover industrial-grade ammonium chloride | |
| CN108455680B (en) | Environment-friendly resource utilization method of steel pickling waste liquid | |
| CN110589788A (en) | Method for recycling wastewater in battery-grade iron phosphate synthesis process | |
| CN106495404A (en) | A kind of processing method of the high salinity cupric organic wastewater of highly acidity | |
| CN110877945A (en) | Treatment method of high-salt high-organic matter industrial wastewater | |
| CN217709144U (en) | Ferric phosphate effluent disposal system | |
| CN108675529A (en) | A method of the phosphatic waste water of processing | |
| CN101428933A (en) | Biological agent cooperated hydrolyzation-blowing off treatment process for nickel-ammonia wastewater | |
| CN111995155A (en) | Method for recycling ammoniacal nitrogen-containing acidic wastewater | |
| CN116462347A (en) | Treatment method of iron phosphate production wastewater | |
| CN111807589A (en) | Method for recycling high-grade ammonium chloride from high-ammonia nitrogen wastewater in coal chemical industry | |
| CN108793558B (en) | Method for treating wastewater generated in activated carbon production by phosphoric acid activation method | |
| CN101428887B (en) | Treatment for nickel-ammonia wastewater with aeration-hydrolyzing process | |
| CN108569812B (en) | Treatment system and treatment method for wastewater containing low-concentration sulfuric acid | |
| CN108892302B (en) | Comprehensive treatment method for prochloraz production wastewater | |
| CN110563218A (en) | method for recovering phosphorus resource from chemical nickel waste liquid | |
| CN107416863B (en) | Method for preparing industrial-grade ammonium salt from wastewater generated in iron phosphate production | |
| CN105217864A (en) | The treatment process of two cyanogen front-end volatiles waste water in Disperse Blue-60 production process | |
| CN105110515B (en) | A kind of processing method of DSD acid waste water | |
| CN216918911U (en) | Treatment system for zero discharge and recycling of lithium iron phosphate production wastewater | |
| CN107265730A (en) | Chemical nickel waste liquid waste water treatment process and equipment | |
| CN111470677A (en) | Method for producing ionic membrane caustic soda by using high-salt organic wastewater generated in epoxy chloropropane production process | |
| CN217809125U (en) | Automatic processing system of quick-acting denitrogenation resin regeneration waste liquid of control | |
| CN111115661A (en) | Nitric acid wastewater treatment system and method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20191220 |