CN115490385A - Waste liquid treatment system and process - Google Patents
Waste liquid treatment system and process Download PDFInfo
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- CN115490385A CN115490385A CN202211354604.7A CN202211354604A CN115490385A CN 115490385 A CN115490385 A CN 115490385A CN 202211354604 A CN202211354604 A CN 202211354604A CN 115490385 A CN115490385 A CN 115490385A
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- 239000007788 liquid Substances 0.000 title claims abstract description 64
- 239000002699 waste material Substances 0.000 title claims abstract description 64
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000004821 distillation Methods 0.000 claims abstract description 58
- 229910052751 metal Inorganic materials 0.000 claims abstract description 45
- 239000002184 metal Substances 0.000 claims abstract description 45
- 150000003839 salts Chemical class 0.000 claims abstract description 41
- 238000011084 recovery Methods 0.000 claims abstract description 31
- 238000001179 sorption measurement Methods 0.000 claims abstract description 19
- 239000006260 foam Substances 0.000 claims abstract description 18
- 229920005989 resin Polymers 0.000 claims abstract description 15
- 239000011347 resin Substances 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims abstract description 9
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000013078 crystal Substances 0.000 claims description 19
- 238000000926 separation method Methods 0.000 claims description 12
- 239000004094 surface-active agent Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000002243 precursor Substances 0.000 claims description 8
- 238000001514 detection method Methods 0.000 claims description 7
- 239000012266 salt solution Substances 0.000 claims description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 claims description 3
- 238000002360 preparation method Methods 0.000 claims description 3
- 229910001415 sodium ion Inorganic materials 0.000 claims description 3
- LIFHMKCDDVTICL-UHFFFAOYSA-N 6-(chloromethyl)phenanthridine Chemical compound C1=CC=C2C(CCl)=NC3=CC=CC=C3C2=C1 LIFHMKCDDVTICL-UHFFFAOYSA-N 0.000 claims description 2
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 239000002952 polymeric resin Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- 229940083542 sodium Drugs 0.000 claims description 2
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 claims description 2
- -1 sodium laureth carboxylate Chemical class 0.000 claims description 2
- 229920003002 synthetic resin Polymers 0.000 claims description 2
- 239000010808 liquid waste Substances 0.000 claims 3
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 229910021645 metal ion Inorganic materials 0.000 abstract description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 4
- 239000011572 manganese Substances 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 238000009833 condensation Methods 0.000 description 3
- 230000005494 condensation Effects 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 230000002194 synthesizing effect Effects 0.000 description 2
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- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 150000001844 chromium Chemical class 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 150000001868 cobalt Chemical class 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
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- 150000002290 germanium Chemical class 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 150000002505 iron Chemical class 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 150000002696 manganese Chemical class 0.000 description 1
- 150000002815 nickel Chemical class 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Images
Classifications
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- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
-
- 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
- C02F1/048—Purification of waste water by 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
- C02F1/20—Treatment of water, waste water, or sewage by degassing, i.e. liberation of dissolved gases
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/16—Nitrogen compounds, e.g. ammonia
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention belongs to the technical field of lithium ion battery sewage treatment, and discloses a waste liquid treatment system and a waste liquid treatment process. Including waste liquid pond, foam separator, polarity adsorption resin device, negative pressure rotary distillation device, gas recovery condensing equipment and metal salt recovery unit, waste liquid pond, foam separator, polarity adsorption resin, negative pressure rotary distillation device communicate in proper order, the material discharge port that negative pressure rotary distillation device is connected including setting up the gas outlet who is connected with gas recovery condensing equipment and is connected with metal salt recovery unit. The waste liquid treatment system and the process can be widely applied to waste water treatment in different synthetic processes. Effectively removes organic matters, and can recycle ammonia gas and metal ions in the organic matters, thereby further reducing the process cost and improving the environmental protection performance.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery sewage treatment, relates to a waste liquid treatment system and a process, and particularly relates to a waste liquid treatment system and a process in a ternary cathode material precursor preparation process.
Background
The ternary material as the anode material of the lithium ion battery has gained wide attention and research due to the high energy and high stability. The ternary material generates a large amount of waste liquid in the preparation process, and if the ternary material is directly discharged, the ternary material can cause serious harm to the environment, so that the reasonable and effective treatment of the waste liquid becomes an important subject at present.
The ternary material is prepared through coprecipitation to synthesize precursor and subsequent calcination. However, in the process of synthesizing the precursor, due to the addition of the additive and the ammonia water, the generated waste liquid is difficult to separate and treat, and meanwhile, the waste liquid contains a large amount of metal ions, which causes great harm to the environment.
Disclosure of Invention
In view of the above problems in the prior art, an object of the present invention is to provide a waste liquid treatment system, which can be widely applied to wastewater treatment in different synthesis processes, effectively remove organic matters, recycle ammonia gas and metal ions therein, reduce process cost, and improve environmental protection performance.
The invention also aims to provide a waste liquid treatment process.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the utility model provides a waste liquid treatment system, includes waste liquid pond, foam separator, well polarity adsorption resin device, negative pressure rotary distillation device, gas recovery condensing equipment and metal salt recovery unit, waste liquid pond, foam separator, well polarity adsorption resin, negative pressure rotary distillation device communicate in proper order, the material discharge port that negative pressure rotary distillation device is connected including setting up the gas outlet who is connected with gas recovery condensing equipment and is connected with metal salt recovery unit.
Further, an exhaust valve and a pressure gauge are arranged in the foam separator; and a thermometer and a concentration detection assembly are arranged in the negative pressure rotary distillation device.
The invention also discloses a waste liquid treatment process, and the waste liquid treatment system comprises the following steps:
(1) Introducing the waste liquid in the waste liquid pool into a foam separator for bubble separation, and removing organic matters and carbon sources in the waste liquid;
(2) Introducing the waste liquid subjected to the bubble separation into a medium-polarity adsorption resin device, further adsorbing the residual organic matters, trace doped metal sources and large-size sodium ions in the waste liquid, and then introducing the waste liquid into a negative-pressure rotary distillation device;
(3) The method comprises the following steps of (1) carrying out gradient negative pressure rotary distillation on waste liquid in a negative pressure rotary distillation device, specifically:
rotary distilling at 40-50 ℃ for 1-5 h;
rotary distilling at 60-80 ℃ for 1-5h;
rotary distilling at 90-110 ℃ for 1-5h;
gas generated in the distillation process is treated by a gas recovery condensing device, and metal salt crystals are obtained after gradient negative pressure rotary distillation and are treated by a metal salt recovery device.
Further, the waste liquid is the waste liquid in the process of synthesizing the ternary precursor, the main components are nickel salt, cobalt salt, manganese salt, ammonia water and sodium salt, the secondary components are organic additives such as aniline, polyaniline, citric acid and PVP, carbon sources such as glucose, sucrose and graphene, and trace doped metal sources such as chromium salt, magnesium salt, aluminum salt, germanium salt and iron salt.
Further, the gas added into the foam separator is air, and in the process of bubble adsorption separation, the surfactant is added into the waste liquid, wherein the surfactant is one or more of ammonium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium laureth carboxylate and triethanolamine lauryl sulfate.
Further preferably, the mass ratio of the waste liquid to the surfactant is 1:0.01 to 0.05.
Further preferably, the flow velocity of air bubbles in the bubble adsorption separation process is 3 to 6 cm/s.
Further, the medium-polarity adsorption resin device comprises one or more of gel type resin, polyacrylate type polymer resin and epoxy resin.
Further, the gradient negative pressure rotary distillation specifically comprises:
rotary distilling at 40-50 ℃ for 1-5 h; detecting the concentration of the solution in a negative pressure rotary distillation device until the concentration of the metal salt solution is 1 to 2mol/L;
heating the distillation device to 60-80 ℃, and then continuously carrying out rotary distillation for 1-5h; collecting ammonia gas and water vapor into a recovery device, and detecting the concentration of a solution in a negative pressure rotary distillation device until the concentration of a metal salt solution is 2 to 4mol/L;
and (3) continuously heating the distillation device to the temperature of 90-110 ℃, carrying out rotary distillation for 1-5 h, volatilizing all water vapor, condensing the water vapor to a recovery device until the water in the negative pressure rotary distillation device is completely evaporated, and obtaining metal salt crystals in the negative pressure rotary distillation device.
Furthermore, in a metal salt recovery processing device, the Ni content, the Co content and the Mn content in the obtained metal salt crystal are detected, and one or more of Ni salt, co salt and Mn salt are supplemented according to the proportion to be used as raw materials for preparing the precursor.
Compared with the prior art, the invention has the beneficial effects that:
(1) The waste liquid treatment system and the process can be widely applied to waste water treatment in different synthetic processes. Effectively removes organic matters, and can recycle ammonia gas and metal ions in the organic matters, thereby further reducing the process cost and improving the environmental protection performance.
(2) The invention creatively absorbs most of organic matters by combining the bubble adsorption separation with the surfactant foaming activation technology, and the surfactant foams in a large amount in the solution, thereby effectively absorbing the organic matters in the waste liquid.
(3) The method adopts a gradient negative pressure rotary distillation technology, can effectively remove ammonia gas through sectional distillation, can furthest retain valuable metal ions, improves the purification efficiency, ensures the high purity of metal salt crystals, and supplements related metal salts according to the proportion after detecting the contents of Ni, co and Mn in the metal salt crystals, thereby being used as the raw material for preparing the precursor.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the principles of the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic view of the structure of a waste liquid treatment system according to the present invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
As shown in fig. 1, the present embodiment discloses a device comprising a waste liquid pool, a foam separator, a medium-polarity adsorption resin device, a negative pressure rotary distillation device, a gas recovery condensing device and a metal salt recovery device, wherein the waste liquid pool, the foam separator, the medium-polarity adsorption resin device and the negative pressure rotary distillation device are sequentially communicated, and the negative pressure rotary distillation device comprises a gas outlet connected with the gas recovery condensing device and a material outlet connected with the metal salt recovery device. An exhaust valve and a pressure gauge are arranged in the foam separator; and a thermometer and a concentration detection assembly are arranged in the negative pressure rotary distillation device.
Example 2
The present embodiment provides a waste liquid treatment process using the waste liquid treatment system in embodiment 1, including the following steps:
(1) Introducing the waste liquid in the waste liquid pool into a foam separator for bubble separation, and removing organic matters and carbon sources in the waste liquid; the gas added into the foam separator is air, and in the bubble adsorption separation process, the surfactant is added into the waste liquid, wherein the surfactant is ammonium dodecyl sulfate; the mass ratio of the waste liquid to the surfactant is 1:0.02, wherein the flow rate of the added air bubbles is 4 cm/s;
(2) The waste liquid after the bubble separation enters a medium-polarity adsorption resin device to further adsorb residual organic matters, trace doped metal sources and large-size sodium ions in the waste liquid, and then enters a negative-pressure rotary distillation device;
(3) The method comprises the following steps of (1) carrying out gradient negative pressure rotary distillation on waste liquid in a negative pressure rotary distillation device, specifically:
performing rotary distillation at 50 ℃ for 2h to obtain a metal salt solution with the concentration of 2mol/L, and collecting gas, namely ammonia gas, by using a gas recovery and condensation device after distillation;
performing rotary distillation at 80 ℃ for 1h to obtain a metal salt solution with the concentration of 3 mol/L, and directly discharging the gas collected by a gas recovery and condensation device after distillation, wherein the gas is water vapor;
performing rotary distillation at 100 ℃ for 2h to obtain high-purity metal salt crystals, wherein the purity of the metal salt crystals is 99.4% through detection, and the mass of the dried metal salt crystals is 65.9g; the gas collected by the gas recovery and condensation device after distillation is water vapor and is directly discharged, and the obtained metal salt crystals are introduced into the metal salt recovery device;
(4) And after detecting Ni, co and Mn in the obtained high-purity metal salt crystal, supplementing related metal salts according to a proportion, and taking the metal salts as raw materials for preparing a precursor to form a cycle.
Comparative example 1
Comparative example 1 is substantially identical to example 2, except that no surfactant is added in step (1). After the waste liquid is recycled and treated, the metal salt crystal is subjected to relevant detection. The purity of the metal salt crystal is 93.5% by detection, and the dried mass of the metal salt crystal is 66.7 g.
Comparative example 2
The comparative example 1 is substantially the same as the example 2, except that the step (3) is a one-step negative pressure rotary distillation without adopting the gradient negative pressure rotary distillation, the distillation temperature is 100 ℃, and the distillation time is 4 hours. Finally, the metal salt crystal is prepared by recovery. The purity of the metal salt crystal is 99.5% through detection, and the dried mass of the metal salt crystal is 60.2 g.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (9)
1. The utility model provides a waste liquid treatment system, its characterized in that, includes waste liquid pond, foam separator, polarity adsorption resin device, negative pressure rotary distillation device, gas recovery condensing equipment and metal salt recovery unit, waste liquid pond, foam separator, polarity adsorption resin, negative pressure rotary distillation device communicate in proper order, negative pressure rotary distillation device is including setting up the gas outlet who is connected with gas recovery condensing equipment and the material discharge port who is connected with metal salt recovery unit.
2. The liquid waste treatment system of claim 1, wherein a gas vent valve and a pressure gauge are provided in the foam separator; and a thermometer and a concentration detection assembly are arranged in the negative pressure rotary distillation device.
3. A waste liquid treatment process using the waste liquid treatment system according to claim 1 or 2, comprising the steps of:
(1) Introducing the waste liquid in the waste liquid pool into a foam separator for bubble separation, and removing organic matters and carbon sources in the waste liquid;
(2) Introducing the waste liquid subjected to the bubble separation into a medium-polarity adsorption resin device, further adsorbing the residual organic matters, trace doped metal sources and large-size sodium ions in the waste liquid, and then introducing the waste liquid into a negative-pressure rotary distillation device;
(3) The method comprises the following steps of (1) carrying out gradient negative pressure rotary distillation on waste liquid in a negative pressure rotary distillation device, specifically:
rotary distilling at 40-50 ℃ for 1-5 h;
rotary distilling at 60-80 ℃ for 1-5h;
rotary distilling at 90-110 ℃ for 1-5h;
gas generated in the distillation process is treated by a gas recovery condensing device, and metal salt crystals are obtained after gradient negative pressure rotary distillation and are treated by a metal salt recovery device.
4. The waste liquid treatment process according to claim 3, wherein the gas added into the foam separator is air, and a surfactant is added into the waste liquid in the bubble adsorption separation process, wherein the surfactant is one or more of ammonium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium laureth carboxylate and triethanolamine lauryl sulfate.
5. The liquid waste treatment process according to claim 4, wherein the mass ratio of the liquid waste to the surfactant is 1:0.01 to 0.05.
6. The waste liquid treatment process according to claim 4, wherein the flow rate of air bubbles is 3 to 6 cm/s in the bubble adsorption separation process.
7. The waste liquid treatment process according to claim 3, wherein the medium-polarity adsorption resin device comprises one or more of gel-type resin, polyacrylate-type polymer resin and epoxy resin.
8. The waste liquid treatment process according to claim 3, wherein the gradient negative pressure rotary distillation is specifically:
rotary distilling at 40-50 ℃ for 1-5 h; detecting the concentration of the solution in a negative pressure rotary distillation device until the concentration of the metal salt solution is 1 to 2mol/L;
heating the distillation device to 60-80 ℃, and then continuously carrying out rotary distillation for 1-5h; collecting ammonia and water vapor into a recovery device, and detecting the concentration of a solution in a negative pressure rotary distillation device until the concentration of a metal salt solution is 2-4 mol/L;
and (3) continuously heating the distillation device to the temperature of 90-110 ℃, carrying out rotary distillation for 1-5 h, volatilizing all water vapor, condensing the water vapor to a recovery device until the water in the negative pressure rotary distillation device is completely evaporated, and obtaining metal salt crystals in the negative pressure rotary distillation device.
9. The process of claim 3, wherein in the metal salt recovery processing device, the Ni content, co content and Mn content in the obtained metal salt crystal are detected, and one or more of Ni salt, co salt and Mn salt are supplemented according to the proportion to be used as raw materials for precursor preparation.
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