CN115490385B - Waste liquid treatment system and process - Google Patents
Waste liquid treatment system and process Download PDFInfo
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- CN115490385B CN115490385B CN202211354604.7A CN202211354604A CN115490385B CN 115490385 B CN115490385 B CN 115490385B CN 202211354604 A CN202211354604 A CN 202211354604A CN 115490385 B CN115490385 B CN 115490385B
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- 239000007788 liquid Substances 0.000 title claims abstract description 71
- 239000002699 waste material Substances 0.000 title claims abstract description 71
- 238000000034 method Methods 0.000 title claims abstract description 29
- 238000004821 distillation Methods 0.000 claims abstract description 56
- 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 42
- 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
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 10
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 5
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 5
- 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
- 239000002243 precursor Substances 0.000 claims description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 6
- 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
- 229910021645 metal ion Inorganic materials 0.000 abstract description 5
- 238000004065 wastewater treatment Methods 0.000 abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 229910021529 ammonia Inorganic materials 0.000 abstract description 3
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 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
- 238000001035 drying Methods 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
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 1
- 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
- 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
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 150000002290 germanium Chemical class 0.000 description 1
- 239000008103 glucose Substances 0.000 description 1
- 229910021389 graphene Inorganic materials 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
- 230000000717 retained effect Effects 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
Classifications
-
- 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
Landscapes
- 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. The device comprises 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 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. The waste liquid treatment system and the waste liquid treatment process can be widely applied to waste water treatment in different synthesis processes. Effectively removes organic matters, and can recycle ammonia 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 waste liquid treatment process, and in particular relates to a waste liquid treatment system and a waste liquid treatment process in a ternary cathode material precursor preparation process.
Background
The ternary material is widely paid attention to and researched as a lithium ion battery anode material due to 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 waste liquid is reasonably and effectively treated, and the ternary material becomes an important subject at present.
The ternary material is synthesized by adopting a coprecipitation method to synthesize a precursor and then later calcining. However, in the process of synthesizing the precursor, the generated waste liquid is difficult to separate and treat due to the addition of the additive and the ammonia water, and meanwhile, the waste liquid contains a large amount of metal ions, which causes great harm to the environment.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a waste liquid treatment system which can be widely applied to waste water treatment in different synthesis processes, effectively remove organic matters, recycle ammonia and metal ions in the waste water treatment system, reduce the process cost and improve the environmental protection performance.
Another object of the present invention is to provide a waste liquid treatment process.
In order to achieve the above 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, negative pressure rotary distillation device is including setting up the gas outlet and the material discharge port of being connected with metal salt recovery unit who is connected with gas recovery condensing equipment.
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, which uses the waste liquid treatment system and comprises the following steps:
(1) Introducing 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 after bubble separation into a medium-polarity adsorption resin device, further adsorbing the residual organic matters, the trace doped metal sources and the large-size sodium ions in the waste liquid, and then introducing into a negative pressure rotary distillation device;
(3) The waste liquid is subjected to gradient negative pressure rotary distillation in a negative pressure rotary distillation device, and specifically comprises the following steps:
rotary distillation is carried out for 1-5 h at the temperature of 40-50 ℃;
rotating and distilling for 1-5 h at the temperature of 60-80 ℃;
rotary distillation is carried out for 1-5 h at the temperature of 90-110 ℃;
and (3) treating the gas generated in the distillation process by a gas recovery condensing device, carrying out gradient negative pressure rotary distillation to obtain metal salt crystals, and treating by a metal salt recovery device.
Further, the waste liquid is waste liquid in the ternary precursor synthesis process, and mainly comprises nickel salt, cobalt salt, manganese salt, ammonia water, sodium salt, and the secondary components comprise organic additives such as aniline, polyaniline, citric acid, PVP and the like, carbon sources such as glucose, sucrose, graphene and the like, and trace doped metal sources such as chromium salt, magnesium salt, aluminum salt, germanium salt, ferric salt and the like.
Further, 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 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, in the bubble adsorption separation process, the air bubble flow rate is 3-6 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 the following steps:
rotary distillation is carried out for 1-5 h at the temperature of 40-50 ℃; detecting the concentration of the solution in the negative pressure rotary distillation device until the concentration of the metal salt solution is 1-2 mol/L;
heating the distillation device to 60-80 ℃, and continuously performing rotary distillation for 1-5 h; 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 2-4 mol/L;
and continuously heating the distillation device to the temperature of 90-110 ℃, carrying out rotary distillation for 1-5 h, fully volatilizing the water vapor, condensing the water vapor to the recovery device until the water in the negative pressure rotary distillation device is completely evaporated, and obtaining the metal salt crystal in the negative pressure rotary distillation device.
Further, 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 preparing the precursor.
Compared with the prior art, the invention has the beneficial effects that:
(1) The waste liquid treatment system and the waste liquid treatment process can be widely applied to waste water treatment in different synthesis processes. Effectively removes organic matters, and can recycle ammonia and metal ions in the organic matters, thereby further reducing the process cost and improving the environmental protection performance.
(2) The invention creatively adsorbs most of organic matters by combining the bubble adsorption separation and surfactant foaming activation technology, and the surfactant foams a large amount of in the solution, so that the organic matters in the waste liquid can be effectively adsorbed.
(3) According to the invention, a gradient negative pressure rotary distillation technology is adopted, ammonia gas can be effectively removed through sectional distillation, valuable metal ions can be retained to the maximum extent, the purification efficiency is improved, the high purity of metal salt crystals is ensured, and then relevant metal salts are supplemented according to proportion after the content of Ni, co and Mn is detected, so that the metal salt crystals are used as raw materials for preparing precursors.
Drawings
The accompanying drawings are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate the invention and together with the embodiments of the invention, serve to explain the invention. In the drawings:
FIG. 1 is a schematic diagram of a waste liquid treatment system according to the present invention.
Detailed Description
The present invention will be described more fully hereinafter with reference to the accompanying drawings, in which preferred embodiments are shown, for the purpose of illustrating the invention, but the scope of the invention is not limited to the specific embodiments shown.
Unless defined otherwise, all technical and scientific terms 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 be limiting of the scope of the present invention.
Unless otherwise specifically indicated, the various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or may be prepared by existing methods.
Example 1
As shown in fig. 1, this embodiment discloses including 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, negative pressure rotary distillation device is including setting up the gas outlet and the material discharge port of being connected with metal salt recovery unit that are connected with gas recovery condensing equipment. 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
This embodiment provides a waste liquid treatment process using the waste liquid treatment system of embodiment 1, comprising the steps of:
(1) Introducing 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, a 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, and organic matters, trace doped metal sources and large-size sodium ions remained in the waste liquid are further adsorbed, and then enter a negative pressure rotary distillation device;
(3) The waste liquid is subjected to gradient negative pressure rotary distillation in a negative pressure rotary distillation device, and specifically comprises the following steps:
rotating and distilling for 2 hours at 50 ℃ to obtain the concentration of the metal salt solution of 2mol/L, and collecting gas into ammonia gas by a gas recovery condensing device after distillation;
rotating and distilling for 1h at 80 ℃ to obtain metal salt solution with the concentration of 3 mol/L, and collecting gas as water vapor by a gas recovery condensing device after distillation and directly discharging;
rotating and distilling for 2 hours at the temperature of 100 ℃ to obtain high-purity metal salt crystals, wherein the purity of the metal salt crystals is 99.4 percent through detection, and the mass of the metal salt crystals after drying is 65.9g; the gas is collected by the gas recovery condensing device after distillation to be water vapor, and is directly discharged, and the obtained metal salt crystals are introduced into the metal salt recovery device;
(4) After Ni, co and Mn in the obtained high-purity metal salt crystal are detected, relevant metal salts are supplemented according to the proportion, and the metal salt is used as raw materials for preparing precursors to form circulation.
Comparative example 1
This comparative example 1 is substantially identical to example 2 except that no surfactant is added in step (1). And after the recovery treatment of the waste liquid, carrying out relevant detection on the metal salt crystals. The purity of the metal salt crystal is 93.5% through detection, and the quality of the metal salt crystal after drying is 66.7. 66.7 g.
Comparative example 2
This comparative example 1 was substantially identical to example 2 except that the step (3) was a one-step negative pressure rotary distillation at 100℃for 4 hours without using a gradient negative pressure rotary distillation. Finally recovering and preparing metal salt crystals. The purity of the metal salt crystal is 99.5 percent, and the mass of the metal salt crystal after drying is 60.2 and g.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (7)
1. The waste liquid treatment process is characterized by using a waste liquid treatment system, wherein the waste liquid treatment system comprises 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, the waste liquid pool, the foam separator, the medium-polarity adsorption resin 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;
the method comprises the following steps:
(1) Introducing 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, wherein the waste liquid is waste liquid in the ternary precursor synthesis process; the gas added into the foam separator is air, and a surfactant is added into the waste liquid in the bubble adsorption separation process;
(2) Introducing the waste liquid after bubble separation into a medium-polarity adsorption resin device, further adsorbing the residual organic matters, the trace doped metal sources and the large-size sodium ions in the waste liquid, and then introducing into a negative pressure rotary distillation device;
(3) The waste liquid is subjected to gradient negative pressure rotary distillation in a negative pressure rotary distillation device, and specifically comprises the following steps:
rotary distillation is carried out for 1-5 h at the temperature of 40-50 ℃; detecting the concentration of the solution in the negative pressure rotary distillation device until the concentration of the metal salt solution is 1-2 mol/L;
heating the distillation device to 60-80 ℃, and continuously performing rotary distillation for 1-5 h; 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 2-4 mol/L;
continuously heating the distillation device to 90-110 ℃, performing rotary distillation for 1-5 h, completely volatilizing water vapor, condensing 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;
and (3) treating the gas generated in the distillation process by a gas recovery condensing device, carrying out gradient negative pressure rotary distillation to obtain metal salt crystals, and treating by a metal salt recovery device.
2. The waste liquid treatment process according to claim 1, wherein an exhaust 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. The waste liquid treatment process according to claim 1, wherein the surfactant is one or more of ammonium dodecyl sulfate, sodium dodecyl benzene sulfonate, sodium laureth carboxylate, and triethanolamine lauryl sulfate.
4. The waste liquid treatment process according to claim 1, wherein the mass ratio of the waste liquid to the surfactant is 1:0.01 to 0.05.
5. The waste liquid treatment process according to claim 1, wherein the flow rate of air bubbles is 3 to 6 cm/s in the bubble adsorption separation process.
6. The waste liquid treatment process according to claim 1, wherein the medium-polarity adsorption resin device comprises one or more of gel-type resin, polyacrylate-type polymer resin, and epoxy resin.
7. The waste liquid treatment process according to claim 1, wherein in the metal salt recovery treatment device, the Ni content, co content, mn content in the obtained metal salt crystal is detected, and one or more of Ni salt, co salt, mn salt are supplemented in proportion as raw materials for precursor preparation.
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