WO2024199529A1 - 锂电生产中nmp的回收方法及回收系统 - Google Patents

锂电生产中nmp的回收方法及回收系统 Download PDF

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Publication number
WO2024199529A1
WO2024199529A1 PCT/CN2024/085365 CN2024085365W WO2024199529A1 WO 2024199529 A1 WO2024199529 A1 WO 2024199529A1 CN 2024085365 W CN2024085365 W CN 2024085365W WO 2024199529 A1 WO2024199529 A1 WO 2024199529A1
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nmp
gas
liquid
primary
stage
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French (fr)
Inventor
康小兵
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Svolt Energy Technology Co Ltd
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Svolt Energy Technology Co Ltd
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Priority to US18/995,720 priority Critical patent/US20260048358A1/en
Priority to EP24778314.5A priority patent/EP4556095A4/en
Publication of WO2024199529A1 publication Critical patent/WO2024199529A1/zh
Anticipated expiration legal-status Critical
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/06—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with moving adsorbents, e.g. rotating beds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1487—Removing organic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/96—Regeneration, reactivation or recycling of reactants
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/058—Construction or manufacture
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/106—Silica or silicates
    • B01D2253/108—Zeolites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
    • B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2258/00—Sources of waste gases
    • B01D2258/02—Other waste gases
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • 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
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries
    • 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
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/84—Recycling of batteries or fuel cells

Definitions

  • the present disclosure relates to the technical field of lithium battery production, and in particular to a method for recovering NMP in lithium battery production.
  • the present disclosure also relates to a recovery system for implementing the method for recovering NMP in lithium battery production.
  • pole piece coating is an essential process. During the coating process, a large amount of NMP gas will be volatilized. Its chemical name is N-methylpyrrolidone, the chemical formula is CH9NO, and the molecular weight is 99.1. Due to cost considerations, in lithium battery production, the NMP waste gas generated by coating is generally recovered and purified to form NMP finished liquid that can be directly used in coating operations.
  • the recovery rate of NMP in NMP waste gas is low, the purity of the recovered NMP finished liquid is about 80%, and the heat recovery efficiency of NMP waste gas is also low, resulting in problems of heat energy waste and high energy consumption, which in turn leads to increased manufacturing costs and difficulty in meeting environmental protection requirements.
  • the present disclosure aims to propose a method for recovering NMP in lithium battery production, so as to recover and purify NMP waste gas while improving the heat recovery rate.
  • a method for recovering NMP in lithium battery production comprises the following steps:
  • the NMP recovery liquid is subjected to a multi-stage dehydration treatment to remove the dehydrated light component and extract the dehydrated heavy component;
  • the primary NMP reflux gas obtained after the primary NMP gas is adsorbed by the zeolite rotor, and the secondary NMP reflux gas obtained after the dehydrated light components and the distilled light components are condensed, are refluxed to the coating machine after heat exchange with the NMP exhaust gas, and the NMP exhaust gas after cooling is subjected to multi-stage condensation treatment.
  • the multi-stage condensation process in S1 includes a primary condensation process and a secondary condensation process; the cooling medium of the primary condensation process and the secondary condensation process can be cooling water and/or chilled water.
  • the method further comprises the following steps: mixing the desorbed secondary NMP gas obtained in S2 with the NMP waste gas in S1, and then absorbing the gas by the absorption liquid after the multi-stage condensation treatment and the zeolite wheel treatment.
  • the method further comprises the following steps: after the primary NMP reflux gas and the secondary NMP reflux gas are heat exchanged with the NMP waste gas, a tertiary NMP waste liquid formed by preliminary condensation of the NMP waste gas is obtained, and the tertiary NMP waste liquid is merged into the NMP recovery liquid.
  • the absorption liquid includes at least one of the NMP recovery liquid and pure water.
  • the absorption liquid includes a primary absorption liquid and a secondary absorption liquid
  • the NMP concentration in the primary absorption liquid is between 1% and 5%
  • the NMP concentration in the secondary absorption liquid is between 30% and 80%.
  • the multi-stage dehydration treatment includes a primary dehydration treatment and a secondary dehydration treatment; after the NMP recovery liquid is subjected to the primary dehydration treatment, the primary light component is removed and the primary heavy component is produced, and then the primary heavy component is subjected to a secondary dehydration treatment, and the secondary light component is removed to produce the dehydrated heavy component, and the primary light component and the secondary light component constitute the dehydrated light component.
  • the primary light component is condensed to remove waste water and produce a primary light component gas
  • the secondary light component is condensed to produce a secondary light component liquid and a secondary light component gas containing NMP, respectively; wherein the secondary light component liquid is transported to a distillation process, and the secondary NMP reflux gas includes the primary light component gas and the secondary light component gas.
  • the secondary NMP reflux gas is obtained after the dehydrated light component and the distillation light component are condensed, the following steps are also included: the distillation light component is first condensed, and then heat exchanged with the NMP recovery liquid to obtain the distillation light component gas and the NMP finished liquid, wherein the secondary NMP reflux gas includes the distillation light component gas.
  • the NMP concentration in the NMP recovery liquid subjected to the multi-stage dehydration treatment is between 30% and 80%.
  • the NMP concentration in the primary NMP gas is between 150 and 200 ppm; and/or the NMP content of the exhaust gas that meets the standards is not higher than 25 mg/m3, and the exhaust gas that meets the standards accounts for 5 to 10% by weight of the NMP exhaust gas.
  • the present disclosure has the following advantages:
  • the method for recovering NMP in lithium battery production disclosed in the present invention is to obtain a primary NMP reflux gas after adsorption of the primary NMP gas by a zeolite rotor, and obtain a secondary NMP reflux gas after condensation treatment of dehydrated light components and distilled light components, and both are refluxed to the coating machine after heat exchange with NMP waste gas, so that heat recovery of NMP waste gas can be achieved, and the heat recovery utilization rate can be improved, and the overall energy consumption of the equipment can be reduced.
  • the NMP waste gas after the NMP waste gas is sequentially subjected to heat exchange treatment, multi-stage condensation treatment, zeolite rotor treatment, multi-stage dehydration treatment and distillation treatment, the NMP waste gas can be effectively recovered and purified, and the obtained NMP finished liquid can be directly used in the coating process, thereby improving the utilization rate of NMP and being conducive to reducing costs and energy conservation and environmental protection.
  • the present disclosure also proposes a NMP recovery system in lithium battery production, comprising the NMP recovery device, a first dehydration and distillation device, a second dehydration and distillation device, an NMP distillation device and an NMP finished product storage tank which are sequentially connected and arranged, and the NMP recovery device comprises a heat exchange device, a condensation device, an NMP absorption device and an NMP recovery tank;
  • the heat exchange device includes a first heat exchange channel and a second heat exchange channel capable of realizing heat exchange, one end of the first heat exchange channel is connected to the exhaust port of the coater, and the other end is respectively connected to the air inlet of the condensing device and the NMP recovery tank, one end of the second heat exchange channel is connected to the air supply port of the coater, and the other end is respectively connected to the NMP absorption device, the first dehydration and distillation equipment, the second dehydration and distillation equipment and the gas extraction port of the NMP distillation equipment;
  • the condensing device has an exhaust port connected to the NMP absorption device and a liquid discharge port connected to the NMP recovery tank, and the NMP absorption device is connected to the first dehydration distillation equipment through the NMP recovery tank.
  • the NMP absorption device includes a zeolite rotor connected to the exhaust port, and an absorption tower connected to the desorption end of the zeolite rotor, and the absorption tower is connected to the NMP recovery tank.
  • a raw material preheater is connected between the NMP recovery tank and the first dehydration distillation equipment, and the raw material preheater is also connected between the third top condenser and the third reflux tank in the NMP distillation equipment.
  • the first dehydration distillation equipment includes a first dehydration tower connected to the NMP recovery tank, a first reboiler and a first top condenser connected to the first dehydration tower, and a first reflux tank, a first vacuum buffer tank and a first vacuum unit connected in sequence downstream of the first top condenser, and a wastewater storage tank is also connected to the discharge port of the first reflux tank.
  • FIG1 is an overall flow chart of a method for recovering NMP in lithium battery production according to an embodiment of the present invention
  • FIG2 is a schematic diagram of the structure of a system for recovering NMP in lithium battery production according to an embodiment of the present invention
  • FIG3 is a schematic diagram of the structure of the NMP recovery device according to an embodiment of the present invention.
  • FIG4 is a schematic structural diagram of a first dehydration distillation device according to an embodiment of the present invention.
  • FIG5 is a schematic structural diagram of a second dehydration distillation device according to an embodiment of the present invention.
  • FIG6 is a schematic diagram of the structure of the NMP distillation equipment according to an embodiment of the present invention.
  • NMP recovery equipment 2. First dehydration and distillation equipment; 3. Second dehydration and distillation equipment; 4. NMP distillation equipment; 5. NMP finished product storage tank; 6. Return air pipeline; 7. Coating machine; 8. Recovery storage tank; 9. Residual liquid receiving tank; 10. Wastewater storage tank;
  • first dehydration tower 201, first dehydration tower; 202, first reboiler; 203, first top condenser; 204, first reflux tank; 205, first vacuum buffer tank; 206, first vacuum unit;
  • distillation tower 402. third reboiler; 403. third top condenser; 404. third reflux tank; 405. third vacuum buffer tank; 406. third vacuum unit; 407. raw material preheater.
  • connection should be understood in a broad sense.
  • it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be internal communication between two elements.
  • connection can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be an indirect connection through an intermediate medium, or it can be internal communication between two elements.
  • the present embodiment relates to a method for recovering NMP in lithium battery production, which can realize the recovery of heat from NMP waste gas, improve the heat recovery utilization rate, and reduce the overall energy consumption of the equipment. At the same time, it can also effectively recover and purify NMP waste gas to improve the utilization rate of NMP and reduce costs.
  • the method for recovering NMP in lithium battery production of this embodiment comprises the following steps:
  • the NMP recovery liquid is subjected to multi-stage dehydration treatment to remove the dehydrated light component and extract the dehydrated heavy component.
  • the multi-stage condensation treatment in S1 includes a primary condensation treatment and a secondary condensation treatment, and the cooling medium of the primary condensation treatment and the secondary condensation treatment can both be cooling water or chilled water.
  • the cooling medium for the primary condensation treatment in this embodiment is preferably cooling water
  • the cooling medium for the secondary condensation treatment is preferably chilled water, so as to facilitate the formation of layers during the condensation process of the NMP waste gas and improve the condensation efficiency.
  • the cooling medium for the primary condensation treatment and the secondary condensation treatment in this embodiment can also be set and adjusted accordingly according to actual condensation needs.
  • the cooling medium for the primary condensation treatment and the secondary condensation treatment are both chilled water.
  • the recovery method of this embodiment also includes the following steps: mixing the desorbed secondary NMP gas obtained in S2 with the NMP waste gas in S1, and then absorbing it with an absorption liquid after undergoing multi-stage condensation treatment and zeolite wheel treatment.
  • the secondary NMP gas can be purified so that the secondary NMP gas finally absorbed by the absorption liquid contains a higher concentration of NMP, which is beneficial to improving the absorption efficiency and the efficiency of subsequent purification operations.
  • the recovery method of this embodiment also includes the following steps: after the primary NMP reflux gas and the secondary NMP reflux gas are heat exchanged with the NMP waste gas, a tertiary NMP waste liquid formed by the preliminary condensation of the NMP waste gas is obtained, and the tertiary NMP waste liquid is merged into the NMP recovery liquid.
  • the NMP waste gas undergoes heat exchange with the circulating primary NMP reflux gas and the secondary NMP reflux gas, it is initially condensed and NMP purified, and is beneficial to the subsequent two-stage condensation treatment operation, thereby further improving the condensation efficiency of the NMP waste gas.
  • the absorption liquid includes at least one of NMP recovery liquid and pure water, so that the NMP recovery liquid extracted from the NMP waste gas can be used as the absorption liquid, which can improve the recovery rate of NMP.
  • the absorption liquid includes a primary absorption liquid and a secondary absorption liquid
  • the NMP concentration in the primary absorption liquid is between 1 and 5%
  • the NMP concentration in the secondary absorption liquid is between 30 and 80%, so as to fully absorb the NMP in the secondary NMP gas.
  • the secondary absorption liquid is preferably NMP recovery liquid.
  • the primary absorption liquid may also preferably use pure water to form a better absorption layer and effectively absorb the NMP in the secondary NMP gas.
  • the multi-stage dehydration treatment includes a primary dehydration treatment and a secondary dehydration treatment.
  • the NMP recovered liquid removes the primary light component and extracts the primary heavy component, and then the primary heavy component is subjected to a secondary dehydration treatment, and the secondary light component is removed, and the dehydrated heavy component is extracted, and the primary light component and the secondary light component constitute the dehydrated light component.
  • the primary light component is condensed to remove wastewater and produce the primary light component gas
  • the secondary light component is condensed to produce the secondary light component liquid and the secondary light component gas containing NMP, respectively.
  • the secondary light component liquid is transported to the distillation process, and the secondary NMP reflux gas includes the primary light component gas and the secondary light component gas.
  • the secondary NMP reflux gas when the secondary NMP reflux gas is obtained after the dehydrated light component and the distillation light component are condensed, the following steps are also included: the distillation light component is first condensed, and then heat exchanged with the NMP recovery liquid to obtain the distillation light component gas and the NMP finished liquid, wherein the secondary NMP reflux gas includes the distillation light component gas.
  • the distillation light components are first condensed and heat exchanged with the NMP recovery liquid, which can also improve the heat recovery rate in the entire process and reduce energy consumption.
  • the secondary NMP reflux gas is mainly composed of the primary light component gas, the secondary light component gas and the distillation light component gas, that is, the gas generated in the multi-stage dehydration treatment and the gas generated in the distillation treatment are all together with the gas adsorbed by the zeolite wheel (primary NMP reflux gas), after heat exchange with the NMP exhaust gas, and then re-delivered to the coating machine.
  • the primary NMP reflux gas and the secondary NMP reflux gas contain a small amount of NMP, which is transported to the coating machine for utilization after participating in heat exchange, which can avoid environmental pollution, improve the utilization rate of NMP, and further reduce costs.
  • the light fraction of the distillation after condensation treatment is used for heat exchange with the NMP recovery liquid to further improve the heat recovery rate and reduce the overall energy consumption.
  • the NMP concentration in the NMP recovery liquid subjected to multi-stage dehydration treatment is between 30% and 80%, so as to facilitate the subsequent multi-stage dehydration treatment and distillation treatment and improve the purity of NMP.
  • the NMP recovery liquid can be used as an absorption liquid to absorb NMP in the secondary NMP gas until it reaches between 30% and 80%, and then it is subjected to multi-stage dehydration treatment.
  • the NMP concentration in the NMP recovery liquid is higher than 80%, the concentration of NMP in the NMP recovery liquid can be lowered by using pure water as the primary absorption liquid.
  • the NMP concentration threshold of the NMP recovery liquid in the present embodiment can also be set and adjusted accordingly according to the actual purification requirements.
  • the NMP concentration threshold in the NMP recovery liquid can be specifically set to a specific value such as 40%, 55% or 75%, or can be set to a numerical range such as 40% to 55% or 40% to 75%.
  • the temperature of the NMP exhaust gas discharged from the coater is generally around 110°C
  • the temperature of the primary NMP reflux gas and the secondary NMP reflux gas is generally between 12 and 15°C
  • the temperature of the primary NMP reflux gas and the secondary NMP reflux gas after heat exchange is not less than 70°C, so that the heat exchange efficiency reaches about 70%.
  • the NMP concentration in the dehydrated heavy component of this embodiment is not less than 99%, the water content is less than 200ppm, and the NMP concentration in the NMP finished liquid is ensured to be not less than 99.9%, and the overall distillation process efficiency is not less than 98%.
  • the NMP concentration in the first-stage heavy component is not less than 98.5%.
  • the NMP concentration in the primary NMP gas is between 150 and 200 ppm
  • the waste gas obtained after absorption by the absorption liquid in S2 has an NMP content of no more than 25 mg/m3, which accounts for 5 to 10% of the weight of the NMP waste gas, that is, 90 to 95% of the NMP waste gas participates in the circulation, and the NMP waste gas recovery rate is between 90 and 95%.
  • the recovery method of this embodiment is to obtain a primary NMP reflux gas after the primary NMP gas is adsorbed by a zeolite rotor, and a secondary NMP reflux gas obtained after the dehydrated light component and the distilled light component are condensed, and both are refluxed to the coating machine after heat exchange with the NMP waste gas, so that the heat recovery of the NMP waste gas can be realized, the heat recovery utilization rate can be improved, and the overall energy consumption of the equipment can be reduced.
  • the NMP waste gas after the NMP waste gas is sequentially subjected to heat exchange treatment, multi-stage condensation treatment, zeolite rotor treatment, multi-stage dehydration treatment and distillation treatment, the NMP waste gas can be effectively recovered and purified, and the obtained NMP finished liquid can be directly used in the coating process, which improves the utilization rate of NMP and is conducive to reducing costs and energy conservation and environmental protection.
  • the embodiments of the present disclosure also relate to a NMP recovery system in lithium battery production, which can implement the above-mentioned recovery method, purify NMP from NMP waste gas, fully recover and utilize the heat in the NMP waste gas, reduce the overall energy consumption of the equipment, and has good practicality.
  • the recovery system of this embodiment includes an NMP recovery device 1, a first dehydration distillation device 2, a second dehydration distillation device 3, an NMP distillation device 4 and an NMP finished product storage tank 5 which are sequentially connected and arranged, and the NMP recovery device 1 includes a heat exchange device 101, a condensing device 102, an NMP absorption device 103 and an NMP recovery tank 104.
  • the heat exchange device 101 includes a first heat exchange channel and a second heat exchange channel that can realize heat exchange, one end of the first heat exchange channel is connected to the exhaust port of the coater 7, and the other end is respectively connected to the air inlet of the condensing device 102 and the NMP recovery tank 104, one end of the second heat exchange channel is connected to the air supply port of the coater 7, and the other end is respectively connected to the gas extraction port of the NMP absorption device 103, the first dehydration distillation equipment 2, the second dehydration distillation equipment 3 and the NMP distillation equipment 4.
  • the condensing device 102 has an exhaust port connected to the NMP absorption device 103 and a liquid discharge port connected to the NMP recovery tank 104, and the NMP absorption device 103 is connected to the first dehydration distillation equipment 2 through the NMP recovery tank 104.
  • the NMP absorption device 103 includes a zeolite rotor 105 connected to the exhaust port, and an absorption tower connected to the desorption end of the zeolite rotor 105, and the absorption tower is connected to the NMP recovery tank 104.
  • the desorption end of the zeolite wheel 105 is connected to the absorption tower and the condensation device 102, that is, when the NMP concentration in the desorbed gas does not meet the standard, the gas can be condensed and processed by the zeolite wheel 105 to achieve the purpose of purification.
  • the adsorption end of the zeolite wheel 105 is connected to the heat exchange device 101, so that the adsorbed gas is used as circulating cold air and transported to the coating machine 7 after being heated.
  • the absorption tower of the present embodiment includes an upper tower and a lower tower, the desorption end of the zeolite rotor 105 is connected to the lower tower, and the lower tower is connected to the NMP recovery tank 104 through the reflux port 1031, and the NMP solution in the NMP recovery tank 104 can be used as an absorption liquid to absorb the gas containing NMP entering the lower tower, and when the NMP concentration in the NMP solution in the lower tower reaches 30% to 80%, the solution can be transported to the NMP recovery tank 104.
  • a detection pipeline is further provided between the lower tower and the NMP recovery tank 104, and a concentration detection unit 1032 for detecting the NMP concentration is provided on the detection pipeline, and the concentration detection unit 1032 can adopt a liquid concentration sensor or a liquid concentration detector commonly used by those skilled in the art.
  • the upper tower of this embodiment is also connected to a pure water supply device 1033, so as to facilitate the use of pure water as the absorption liquid of NMP, and cooperate with the lower tower to effectively absorb NMP in the gas after desorption.
  • the condensing device 102 includes a first-level condenser 1021 and a second-level condenser 1022 which are sequentially connected between the heat exchange device 101 and the zeolite wheel 105.
  • the first-level condenser 1021 preferably uses cooling water as the cooling medium
  • the second-level condenser 1022 preferably uses chilled water as the cooling medium to form a hierarchical condensation form to improve the condensation effect.
  • a raw material preheater 407 is connected between the NMP recovery tank 104 and the first dehydration distillation equipment 2, and the raw material preheater 407 is also connected between the third tower top condenser 403 and the third reflux tank 404 in the NMP distillation equipment 4, so that the heat in the distillation process can be recycled and utilized, and the energy consumption of the equipment is further reduced.
  • the first dehydration distillation equipment 2 includes a first dehydration tower 201 connected to the NMP recovery tank 104, a first reboiler 202 and a first top condenser 203 connected to the first dehydration tower 201, and a first reflux tank 204, a first vacuum buffer tank 205 and a first vacuum unit 206 connected in sequence downstream of the first top condenser 203, and the discharge port of the first reflux tank 204 is also connected to a wastewater storage tank 10.
  • the second dehydration distillation equipment 3 comprises a second dehydration tower 301 connected to the first dehydration tower 201, a second reboiler 302 and a second top condenser 303 connected to the second dehydration tower 301, and a second reflux tank 304, a second vacuum buffer tank 205 and a second vacuum unit 206 which are sequentially connected to the downstream of the second top condenser 303, and a recovery storage tank 8 is also connected to the discharge port of the second reflux tank 304.
  • the NMP distillation equipment 4 of this embodiment includes a distillation tower 401 connected to the second dehydration tower 301, a third reboiler 402 and a third top condenser 403 connected to the distillation tower 401, and a third reflux tank 404, a third vacuum buffer tank 405 and a third vacuum unit 406 connected in sequence downstream of the third top condenser 403, and a residual liquid receiving tank 9 is also connected to the discharge port of the third reflux tank 404, and the above-mentioned raw material preheater 407 is also connected between the third top condenser 403 and the third reflux tank 404, and as a further improved form, the distillation tower 401 can also be connected to the recovery tank 8 to facilitate the purification of the liquid NMP in the recovery tank 8.
  • the heat exchange device 101 of this embodiment is also connected to the NMP recovery tank 104, and it can adopt a gas-to-gas heat exchanger commonly used by technicians in this field.
  • the first vacuum unit 206, the second vacuum unit 206, the third vacuum unit 406 and the adsorption end of the zeolite wheel 105 of this embodiment are all connected to the second heat exchange channel through the return air pipeline 6 to facilitate the recovery of heat in the NMP exhaust gas discharged by the coating machine 7.
  • the structures not mentioned in the NMP recovery equipment 1, the first dehydration distillation equipment 2, the second dehydration distillation equipment 3 and the NMP distillation equipment 4 in this embodiment can refer to the related equipment products commonly used by those skilled in the art, such as the first tower top condenser 203, the second tower top condenser 303 and the third tower top condenser 403, which are all provided with a water supply end and a water return end for circulating cooling water, which will not be described in detail here.
  • the recovery system of this embodiment can realize the recovery and purification of NMP waste gas through the cooperation of NMP recovery equipment 1, first dehydration and distillation equipment 2, second dehydration and distillation equipment 3, NMP distillation equipment 4 and NMP finished product storage tank 5, and the obtained NMP finished liquid can be directly applied to the coating process, which improves the utilization rate of NMP, is conducive to reducing costs and energy conservation and environmental protection.
  • a heat exchange device 101 is provided in the NMP recovery equipment 1, which is conducive to the recovery and utilization of heat of NMP waste gas, improves the heat recovery and utilization rate of the equipment, reduces the overall energy consumption of the equipment, and has good practicality.
  • the present invention also describes the recovery method in detail in combination with the recovery system, as follows:
  • the NMP waste gas discharged from the coating machine 7 is preliminarily condensed by the heat exchange device 101, and the NMP waste gas after cooling is obtained and transported to the condensing device 102 for two-stage condensation treatment to obtain a primary NMP waste liquid and a primary NMP gas.
  • the primary NMP waste liquid is transported to the NMP recovery tank 104, and the primary NMP gas is transported to the zeolite rotor 105 and the absorption tower in turn, wherein the secondary NMP gas after desorption from the zeolite rotor 105 is transported to the absorption tower, and the absorption liquid is used to absorb the NMP in the secondary NMP gas, and the obtained secondary NMP waste liquid is also transported to the NMP recovery tank 104.
  • the NMP waste gas discharged from the coater 7 will be initially condensed to form a tertiary NMP waste liquid when passing through the heat exchange device 101, and the tertiary NMP waste liquid is also transported to the NMP recovery tank 104. If the NMP concentration of the NMP recovery liquid in the NMP recovery tank 104 is lower than or higher than the threshold value, the NMP recovery liquid can be used as the lower tower absorption liquid and pure water as the upper tower absorption liquid to adjust the NMP recovery liquid until the NMP concentration reaches the threshold requirement.
  • the recovered liquid that meets the threshold requirement will be transported to the first dehydration and distillation equipment 2 for dehydration and separation treatment, to remove the primary light component and produce the primary heavy component, and then the primary heavy component will be transported to the second dehydration and distillation equipment 3 for secondary dehydration and separation treatment, to remove the secondary light component and produce the dehydrated heavy component, and then the dehydrated heavy component will be transported to the NMP distillation equipment 4 for distillation and separation treatment, and the condensate in the produced distillation light component is the NMP finished liquid.
  • the NMP finished product liquid is transported to the NMP finished product storage tank 5 for coating operation, thereby completing the NMP purification process.
  • the separated liquid is transported to the wastewater storage tank 10 as the tower top wastewater, and discharged after the wastewater treatment, and after the second-level light component is condensed by the second tower top condenser 303, the separated liquid can be transported to the distillation tower 401 together with the dehydrated heavy component for distillation separation treatment, and the removed distillation heavy component is transported to the residual liquid receiving tank 9 as the residual liquid.
  • the primary NMP gas is adsorbed by the zeolite wheel 105 to obtain the primary NMP reflux gas.
  • the gas of the primary light component treated by the first tower top condenser 203, the first reflux tank 204, the first vacuum buffer tank 205 and the first vacuum unit 206, the gas of the secondary light component treated by the second tower top condenser 303, the second reflux tank 304, the second vacuum buffer tank 205 and the second vacuum unit 206, and the gas of the rectification light component treated by the third tower top condenser 403, the third reflux tank 404, the third vacuum buffer tank 405 and the third vacuum unit 406 are merged to form the secondary NMP reflux gas.
  • the primary NMP reflux gas and the secondary NMP reflux gas are refluxed to the coating machine 7 after heat exchange with the NMP exhaust gas, so as to effectively recover and utilize the heat in the NMP exhaust gas, thereby realizing heat recovery of the NMP exhaust gas.
  • the distillation light component flowing into the third reflux tank 404 after being processed by the third tower top condenser 403 is also processed by the raw material preheater 407, which can heat the NMP recovery liquid to improve the dehydration separation effect of the first dehydration tower 201, so as to improve the heat recovery rate of the equipment and reduce the overall energy consumption of the equipment.
  • the gas treated by the absorption tower is discharged as a waste gas that meets the standards.

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Abstract

一种锂电生产中NMP的回收方法及回收系统，锂电生产中NMP的回收方法，其特征在于，包括以下步骤：S1，获取涂布机中排出的NMP废气，多级冷凝处理所述NMP废气，得到一级NMP废液和一级NMP气体；S2，将所述一级NMP气体输送至沸石转轮处进行吸附与脱附处理，得到脱附后的二级NMP气体，再通过吸收液吸收所述二级NMP气体中的NMP，得到二级NMP废液和废气达标气体，并排放所述废气达标气体；S3，将所述一级NMP废液和所述二级NMP废液混合得到NMP回收液后，再对所述NMP回收液进行多级脱水处理，脱除脱水轻组分，采出脱水重组分；S4，对所述脱水重组分进行精馏处理，脱除精馏重组分，采出精馏轻组分，并通过精馏轻组分得到NMP成品液；其中，将所述一级NMP气体经所述沸石转轮吸附后得到的一级NMP回流气体，以及所述脱水轻组分和精馏轻组分经冷凝处理后得到的二级NMP回流气体，均通过与所述NMP废气热交换后，回流至所述涂布机处，而降温后的NMP废气再被进行多级冷凝处理。所述锂电生产中NMP的回收方法能够有效提纯NMP废气，并充分回收利用该NMP废气中的热量。

Description

锂电生产中NMP的回收方法及回收系统
本公开要求在2023年3月30日提交中国专利局、申请号为202310331967.7、专利申请名称为“锂电生产中NMP的回收方法及回收系统”的优先权，其全部内容通过引用结合在本公开中。
技术领域
本公开涉及锂电池生产技术领域，特别涉及一种锂电生产中NMP的回收方法。本公开还涉及用于实施该锂电生产中NMP的回收方法的回收系统。
 背景技术
在锂离子电池的生产过程中，极片涂布是必不可少的工序，在涂布过程中会挥发出大量的NMP气体，其化学名为N-甲基吡咯烷酮，化学式为CH9NO，分子量为99.1。基于成本考虑，在锂电池生产中，一般会通过回收涂布产生的NMP废气，通过提纯处理后形成可直接应用于涂布作业中的NMP成品液。
但是，现有的锂离子电池制造中，对于NMP废气中NMP的回收率较低，回收的NMP成品液的纯度在80%左右，且NMP废气的热量回收效率也较低，存在热能浪费及能耗大的问题，进而导致制造成本上升，且难以满足环保要求。
 发明内容
有鉴于此，本公开旨在提出一种锂电生产中NMP的回收方法，以可回收并提纯NMP废气的同时，提升热量回收利用率。
为达到上述目的，本公开的技术方案是这样实现的：
一种锂电生产中NMP的回收方法，包括以下步骤：
S1，获取涂布机中排出的NMP废气，多级冷凝处理所述NMP废气，得到一级NMP废液和一级NMP气体；
S2，将所述一级NMP气体输送至沸石转轮处进行吸附与脱附处理，得到脱附后的二级NMP气体，再通过吸收液吸收所述二级NMP气体中的NMP，得到二级NMP废液和废气达标气体，并排放所述废气达标气体；
S3，将所述一级NMP废液和所述二级NMP废液混合得到NMP回收液后，再对所述NMP回收液进行多级脱水处理，脱除脱水轻组分，采出脱水重组分；
S4，对所述脱水重组分进行精馏处理，脱除精馏重组分，采出精馏轻组分，并通过精馏轻组分得到NMP成品液；
其中，将所述一级NMP气体经所述沸石转轮吸附后得到的一级NMP回流气体，以及所述脱水轻组分和精馏轻组分经冷凝处理后得到的二级NMP回流气体，均通过与所述NMP废气热交换后，回流至所述涂布机处，而降温后的NMP废气再被进行多级冷凝处理。
进一步的，所述S1中的多级冷凝处理包括一级冷凝处理和二级冷凝处理；所述一级冷凝处理及所述二级冷凝处理的冷却介质均可采用冷却水和/或冷冻水。
进一步的，还包括以下步骤：将所述S2中得到的脱附后的二级NMP气体，与所述S1中的NMP废气混合，并在经过所述多级冷凝处理及所述沸石转轮处理后，再被所述吸收液吸收处理。
进一步的，还包括以下步骤：所述一级NMP回流气体和所述二级NMP回流气体均与所述NMP废气热交换后，还得到由所述NMP废气初步冷凝形成的三级NMP废液，并将所述三级NMP废液汇入所述NMP回收液中。
进一步的，所述吸收液包括所述NMP回收液和纯水中的至少一种。
进一步的，所述吸收液包括一级吸收液和二级吸收液，所述一级吸收液中NMP浓度在1~5%之间，所述二级吸收液中NMP浓度在30~80%之间。
进一步的，所述S3中，所述多级脱水处理包括一级脱水处理和二级脱水处理；所述NMP回收液经所述一级脱水处理后，脱除一级轻组分，采出一级重组分，随后将一级重组分经由二级脱水处理，并脱除二级轻组分，采出所述脱水重组分，且所述一级轻组分和所述二级轻组分构成所述脱水轻组分。
进一步的，对所述一级轻组分冷凝处理，脱除废水，采出一级轻组分气体，并对所述二级轻组分冷凝处理，分别采出含有NMP的二级轻组分液体和二级轻组分气体；其中，所述二级轻组分液体被输送至精馏处理中，所述二级NMP回流气体包括所述一级轻组分气体和所述二级轻组分气体。
进一步的，所述脱水轻组分和精馏轻组分经冷凝处理后得到的二级NMP回流气体时，还包括以下步骤：所述精馏轻组分先经由冷凝处理，再与NMP回收液热交换后，得到精馏轻组分气体和所述NMP成品液，其中，所述二级NMP回流气体包括所述精馏轻组分气体。
进一步的，进行所述多级脱水处理的所述NMP回收液中的NMP浓度在30~80%之间。
进一步的，所述一级NMP气体中NMP浓度在150~200ppm之间；和/或，所述废气达标气体的NMP含量不高于25mg/m³，且所述废气达标气体占所述NMP废气的重量在5~10%。
相对于现有技术，本公开具有以下优势：
本公开所述的锂电生产中NMP的回收方法，通过将一级NMP气体经沸石转轮吸附后得到的一级NMP回流气体 ，以及脱水轻组分和精馏轻组分经冷凝处理后得到的二级NMP回流气体，均通过与NMP废气热交换后，回流至所述涂布机处，可实现NMP废气的热量回收，并提升热量回收利用率，降低设备整体能耗，同时，将NMP废气依次经过热交换处理、多级冷凝处理、沸石转轮处理、多级脱水处理及精馏处理后，可有效回收并提纯NMP废气，且得到的NMP成品液能够直接应用于涂布工序中，提升了NMP的利用率，利于降低成本及节能环保。
本公开同时也提出一种锂电生产中NMP的回收系统，包括依次连通设置的所述NMP回收设备、第一脱水精馏设备、第二脱水精馏设备、NMP精馏设备和NMP成品储存罐，且所述NMP回收设备包括热交换装置、冷凝装置、NMP吸收装置和NMP回收罐；
所述热交换装置包括能够实现热交换的第一换热通道和第二换热通道，所述第一换热通道的一端与涂布机的排风口相连通，另一端分别与所述冷凝装置的进气口和所述NMP回收罐相连，所述第二换热通道的一端与所述涂布机的送风口相连通，另一端分别与所述NMP吸收装置、所述第一脱水精馏设备、所述第二脱水精馏设备和所述NMP精馏设备的气体采出口相连通；
所述冷凝装置中具有与所述NMP吸收装置相连的排气口，以及与所述NMP回收罐相连的排液口，且所述NMP吸收装置通过所述NMP回收罐与所述第一脱水精馏设备相连。
进一步的，所述NMP吸收装置包括与所述排气口连通的沸石转轮，以及与所述沸石转轮的脱附端相连的吸收塔，且所述吸收塔与所述NMP回收罐相连。
进一步的，所述NMP回收罐和所述第一脱水精馏设备之间连接有原料预热器，且所述原料预热器还连接在所述NMP精馏设备中的第三塔顶冷凝器与第三回流罐之间。
进一步的，所述第一脱水精馏设备包括与所述NMP回收罐相连的第一脱水塔，与所述第一脱水塔相连的第一再沸器和第一塔顶冷凝器，以及依次连通在所述第一塔顶冷凝器下游的第一回流罐、第一真空缓冲罐和第一真空机组，并在所述第一回流罐的排液口还连通有废水储存罐。
 附图说明
构成本公开的一部分的附图用来提供对本公开的进一步理解，本公开的示意性实施例及其说明用于解释本公开，并不构成对本公开的不当限定。在附图中：
图1为本发明实施例所述的锂电生产中NMP的回收方法的整体流程图；
图2为本发明实施例所述的锂电生产中NMP的回收系统的结构示意图；
图3为本发明实施例所述的NMP回收设备的结构示意图；
图4为本发明实施例所述的第一脱水精馏设备的结构示意图；
图5为本发明实施例所述的第二脱水精馏设备的结构示意图；
图6为本发明实施例所述的NMP精馏设备的结构示意图；
附图标记说明：
1、NMP回收设备；2、第一脱水精馏设备；3、第二脱水精馏设备；4、NMP精馏设备；5、NMP成品储存罐；6、回风管路；7、涂布机；8、回收储罐；9、残液接收罐；10、废水储存罐；
101、热交换装置；102、冷凝装置；1021、一级冷凝器；1022、二级冷凝器；103、NMP吸收装置；1031、返流口；1032、浓度检测单元；1033、纯水供应装置；104、NMP回收罐；105、沸石转轮；
201、第一脱水塔；202、第一再沸器；203、第一塔顶冷凝器；204、第一回流罐；205、第一真空缓冲罐；206、第一真空机组；
301、第二脱水塔；302、第二再沸器；303、第二塔顶冷凝器；304、第二回流罐；205、第二真空缓冲罐；206、第二真空机组；
401、精馏塔；402、第三再沸器；403、第三塔顶冷凝器；404、第三回流罐；405、第三真空缓冲罐；406、第三真空机组；407、原料预热器。
 具体实施方式
需要说明的是，在不冲突的情况下，本公开中的实施例及实施例中的特征可以相互组合。
在本公开的描述中，除非另有明确的限定，术语“安装”、“相连”、“连接”“连接件”应做广义理解。例如，可以是固定连接，也可以是可拆卸连接，或一体地连接；可以是机械连接，也可以是电连接；可以是直接相连，也可以通过中间媒介间接相连，可以是两个元件内部的连通。对于本领域的普通技术人员而言，可以结合具体情况理解上述术语在本实用新型中的具体含义。 
下面将参考附图并结合实施例来详细说明本公开。
本实施例涉及一种锂电生产中NMP的回收方法，其能够实现对NMP废气热量的回收，并提升热量回收利用率，降低设备整体能耗，同时，也能够有效回收并提纯NMP废气，以提升NMP的利用率，降低成本。
整体设计上，如图1所示的，本实施例的锂电生产中NMP的回收方法，包括以下步骤：
S1，获取涂布机中排出的NMP废气，多级冷凝处理NMP废气，得到一级NMP废液和一级NMP气体。
S2，将一级NMP气体输送至沸石转轮处进行吸附与脱附处理，得到脱附后的二级NMP气体，再通过吸收液吸收二级NMP气体中的NMP，得到二级NMP废液和废气达标气体，并排放废气达标气体。
S3，将一级NMP废液和二级NMP废液混合得到NMP回收液后，再对NMP回收液进行多级脱水处理，脱除脱水轻组分，采出脱水重组分。
S4，对脱水重组分进行精馏处理，脱除精馏重组分，采出精馏轻组分，并通过精馏轻组分得到NMP成品液。
其中，将一级NMP气体经沸石转轮吸附后得到的一级NMP回流气体，以及脱水轻组分和精馏轻组分经冷凝处理后得到的二级NMP回流气体，均通过与NMP废气热交换后，回流至涂布机处，而降温后的NMP废气再被进行多级冷凝处理。
基于上述的整体介绍，本实施例中，作为一种优选的实施形式，S1中的多级冷凝处理包括一级冷凝处理和二级冷凝处理，一级冷凝处理及二级冷凝处理的冷却介质均可采用冷却水或冷冻水。
具体实施时，本实施例一级冷凝处理的冷却介质优选采用冷却水，二级冷凝处理的冷却介质优选采用冷冻水，以利于在NMP废气冷凝过程中形成层级，提升冷凝效率。
当然，本实施例一级冷凝处理及二级冷凝处理的冷却介质除了上述实施形式外，也可根据实际的冷凝需求进行相应的设定与调整，例如一级冷凝处理及二级冷凝处理的冷却介质均采用冷冻水等。
作为一种优选的实施形式，本实施例的回收方法还包括以下步骤：将S2中得到的脱附后的二级NMP气体，与S1中的NMP废气混合，并在经过多级冷凝处理及沸石转轮处理后，再被吸收液吸收处理。
如此，可实现对二级NMP气体进行提纯，使得最终被吸收液吸收的二级NMP气体中含有较高浓度的NMP，利于提升吸收效率，以及后续提纯作业效率。
同样，作为一种优选的实施形式，本实施例的回收方法还包括以下步骤：一级NMP回流气体和二级NMP回流气体均与NMP废气热交换后，还得到由NMP废气初步冷凝形成的三级NMP废液，并将三级NMP废液汇入NMP回收液中。
也即，NMP废气在与循环回流的一级NMP回流气体及二级NMP回流气体发生热交换时，被初步冷凝处理及NMP提纯，且利于后续两级冷凝处理作业，进而进一步地提升对NMP废气的冷凝效率。
本实施例中，作为一种优选的实施形式，吸收液包括NMP回收液和纯水中的至少一种，以便于利用NMP废气提取出的NMP回收液作为吸收液，可提升NMP的回收利用率。
同时，作为一种优选的实施形式，吸收液包括一级吸收液和二级吸收液，一级吸收液中NMP浓度在1~5%之间，二级吸收液中NMP浓度在30~80%之间，以利于充分吸收二级NMP气体中的NMP。
在具体实施时，上述二级吸收液优选采用NMP回收液，上述一级吸收液除了采用NMP浓度在1~5%的溶液外，也可优选采用纯水，以便于形成较优的吸收层级，有效吸收二级NMP气体中的NMP。
此外，出于对NMP提纯需求的考虑，本实施例中，作为一种优选的实施形式，S3中，多级脱水处理包括一级脱水处理和二级脱水处理。NMP回收液经一级脱水处理后，脱除一级轻组分，采出一级重组分，随后将一级重组分经由二级脱水处理，并脱除二级轻组分，采出脱水重组分，且一级轻组分和二级轻组分构成脱水轻组分。
具体而言，作为一种优选的改进形式，本实施例中，对一级轻组分冷凝处理，脱除废水，采出一级轻组分气体，并对二级轻组分冷凝处理，分别采出含有NMP的二级轻组分液体和二级轻组分气体。其中，二级轻组分液体被输送至精馏处理中，二级NMP回流气体包括一级轻组分气体和二级轻组分气体。
为提升热量回收利用率，作为一种优选的改进形式，本实施例中，脱水轻组分和精馏轻组分经冷凝处理后得到的二级NMP回流气体时，还包括以下步骤：精馏轻组分先经由冷凝处理，再与NMP回收液热交换后，得到精馏轻组分气体和NMP成品液，其中，二级NMP回流气体包括精馏轻组分气体。
此处，精馏轻组分先经由冷凝处理与NMP回收液热交换，也可提升整个工艺流程中热量的回收利用率，减少能耗。
需注意的是，本实施例中，二级NMP回流气体主要由一级轻组分气体、二级轻组分气体和精馏轻组分气体组成，也即多级脱水处理中产生的气体，以及精馏处理产生的气体均与沸石转轮吸附后的气体（一级NMP回流气体）一起，经过与NMP废气热交换后，重新输送至涂布机处。
并且，可以理解的是，上述一级NMP回流气体和二级NMP回流气体中含有微量的NMP，其参与热交换后，再被输送至涂布机中进行利用，既可避免环境污染，又可提升NMP利用率，进一步地降低成本。同时，利用冷凝处理后的精馏轻组分，与NMP回收液热交换，可再次提升热量回收率，降低整体能耗。
另外，本实施例中，作为另一种优选的实施形式，进行多级脱水处理的NMP回收液中的NMP浓度在30~80%之间，以利于后续多级脱水处理及精馏处理的开展，并提高NMP纯度。
也即，NMP回收液中的NMP浓度低于30%时，暂不输送至后续工序中，而此时，NMP回收液可作为吸收液吸收二级NMP气体中的NMP，直至达到30~80%之间时，才被进行多级脱水处理，同理，NMP回收液中的NMP浓度高于80%时，可通过一级吸收液为纯水的方式来调低NMP回收液中NMP的浓度。
当然，本实施例NMP回收液的NMP浓度阈值除了设置在30~80%之间外，也可根据实际的提纯需求进行相应的设定与调整，例如，NMP回收液中的NMP浓度阈值具体可设置为40%、55%或75%等具体数值，也可设置为40%~55%或40%~75%等数值范围。
值得提及的是，本实施例中有涂布机排出的NMP废气的温度一般在110℃左右，一级NMP回流气体和二级NMP回流气体的温度一般在12~15℃，且热交换后的一级NMP回流气体及二级NMP回流气体的温度不低于70℃，以使换热效率达70%左右。
同时，通过使用本实施例的回收方法，本实施例的脱水重组分中的NMP浓度不低于99%，含水量小于200ppm，并可确保NMP成品液中的NMP浓度不低于99.9%，整体精馏工序效率不低于98%。其中，一级重组分中的NMP浓度不低于98.5%。
除此之外，通过使用本实施例的回收方法，一级NMP气体中NMP浓度在150~200ppm之间，且S2中经过吸收液吸收后得到的废气达标气体，其NMP含量不高于25mg/m³，其占NMP废气的重量在5~10%，也即90~95%的NMP废气参与循环，也使NMP废气回收率在90~95%之间。
本实施例的回收方法，通过将一级NMP气体经沸石转轮吸附后得到的一级NMP回流气体 ，以及脱水轻组分和精馏轻组分经冷凝处理后得到的二级NMP回流气体，均通过与NMP废气热交换后，回流至所述涂布机处，可实现NMP废气的热量回收，并提升热量回收利用率，降低设备整体能耗，同时，将NMP废气依次经过热交换处理、多级冷凝处理、沸石转轮处理、多级脱水处理及精馏处理后，可有效回收并提纯NMP废气，且得到的NMP成品液能够直接应用于涂布工序中，提升了NMP的利用率，利于降低成本及节能环保。
本公开的实施例也涉及一种锂电生产中NMP的回收系统，其能够实施上述回收方法，从NMP废气中提纯NMP的同时，充分回收及利用NMP废气中的热量，降低设备整体能耗，而具有较好的实用性。
在整体结构上，如图2至图6所示的，本实施例回收系统包括依次连通设置的NMP回收设备1、第一脱水精馏设备2、第二脱水精馏设备3、NMP精馏设备4和NMP成品储存罐5，且NMP回收设备1包括热交换装置101、冷凝装置102、NMP吸收装置103和NMP回收罐104。
其中，热交换装置101包括能够实现热交换的第一换热通道和第二换热通道，第一换热通道的一端与涂布机7的排风口相连通，另一端分别与冷凝装置102的进气口和NMP回收罐104相连，第二换热通道的一端与涂布机7的送风口相连通，另一端分别与NMP吸收装置103、第一脱水精馏设备2、第二脱水精馏设备3和NMP精馏设备4的气体采出口相连通。
冷凝装置102中具有与NMP吸收装置103相连的排气口，以及与NMP回收罐104相连的排液口，且NMP吸收装置103通过NMP回收罐104与第一脱水精馏设备2相连。
具体而言，作为一种优选的实施形式，本实施例中，如图3中所示的，NMP吸收装置103包括与排气口连通的沸石转轮105，以及与沸石转轮105的脱附端相连的吸收塔，且吸收塔与NMP回收罐104相连。
在本实施例中，沸石转轮105的脱附端除了与吸收塔相连外，还与冷凝装置102相连，也即当脱附的气体中NMP浓度不达标时，可对气体在此冷凝处理与沸石转轮105处理已到达提纯的目的。沸石转轮105的吸附端与热交换装置101相连，以便于将吸附后的气体作为循环冷风，在被加热后输送至涂布机7处。
并且，值得提及的是，本实施例的吸收塔包括上塔和下塔，沸石转轮105的脱附端与下塔相连，下塔通过返流口1031连接NMP回收罐104，既可调用NMP回收罐104中的NMP溶液作为吸收液来吸收进入下塔中的含有NMP的气体，也可在下塔中的NMP溶液中NMP浓度达到30%~80%时，将该溶液输送至NMP回收罐104中。
而为了检测下塔溶液中的NMP浓度，本实施例中，作为一种优选的实施形式，在下塔与NMP回收罐104之间还设有检测管路，并检测管路上设有用于检测NMP浓度的浓度检测单元1032，且该浓度检测单元1032可采用本领域技术人员常见的液体浓度传感器或液体浓度检测仪。
同样作为一种优选的实施形式，本实施例的上塔还连接有纯水供应装置1033，以利于采用纯水作为NMP的吸收液，而与下塔配合，有效吸收脱附后的气体中的NMP。
本实施例中，为确保冷凝装置102的冷凝效果，仍如图3所示的，作为一种优选的实施形式，冷凝装置102包括依次连接在热交换装置101和沸石转轮105之间的一级冷凝器1021与二级冷凝器1022，具体实施时，一级冷凝器1021优选采用冷却水作为冷却介质，二级冷凝器1022优选采用冷冻水作为冷却介质，以形成层级递进的冷凝形式，提升冷凝效果。
同时，本实施例中，作为一种优选的实施形式，NMP回收罐104和第一脱水精馏设备2之间连接有原料预热器407，且原料预热器407还连接在NMP精馏设备4中的第三塔顶冷凝器403与第三回流罐404之间，以可回收利用精馏工序中的热量，进一步地降低设备能耗。
此外，仍作为一种优选的实施形式，本实施例中，如图4中所示，第一脱水精馏设备2包括与NMP回收罐104相连的第一脱水塔201，与第一脱水塔201相连的第一再沸器202和第一塔顶冷凝器203，以及依次连通在第一塔顶冷凝器203下游的第一回流罐204、第一真空缓冲罐205和第一真空机组206，并在第一回流罐204的排液口还连通有废水储存罐10。
其次，参见图5中所示的，本实施例中，第二脱水精馏设备3包括与第一脱水塔201相连的第二脱水塔301，与第二脱水塔301相连的第二再沸器302和第二塔顶冷凝器303，以及依次连通在第二塔顶冷凝器303下游的第二回流罐304、第二真空缓冲罐205和第二真空机组206，并在第二回流罐304的排液口还连通有回收储罐8。
与此同时，参见图6所示，本实施例NMP精馏设备4包括与第二脱水塔301相连的精馏塔401，与精馏塔401相连的第三再沸器402和第三塔顶冷凝器403，以及依次连通在第三塔顶冷凝器403下游的第三回流罐404、第三真空缓冲罐405和第三真空机组406，并在第三回流罐404的排液口还连通有残液接收罐9，在第三塔顶冷凝器403与第三回流罐404之间还连通有上述的原料预热器407，且作为进一步的改进形式，精馏塔401还可与回收储罐8相连通，以便于提纯回收储罐8中液体的NMP。
仍需说明的是，本实施例热交换装置101还与NMP回收罐104相连，且其可采用本领域技术人员常见的气气换热器，本实施例的第一真空机组206、第二真空机组206、第三真空机组406和沸石转轮105的吸附端，均通过回风管路6与第二换热通道相连，以便于回收涂布机7排出的NMP废气中的热量。
并且，本实施例NMP回收设备1、第一脱水精馏设备2、第二脱水精馏设备3及NMP精馏设备4中未提及的各结构，均可参照本领域技术人员常见的相关设备产品，例如第一塔顶冷凝器203、第二塔顶冷凝器303和第三塔顶冷凝器403，均设置有供冷却水流通的送水端和回水端，在此不再进行赘述。
本实施例的回收系统，通过NMP回收设备1、第一脱水精馏设备2、第二脱水精馏设备3、NMP精馏设备4和NMP成品储存罐5配合使用，可实现对NMP废气的回收及提纯，且得到的NMP成品液能够直接应用于涂布工序中，提升了NMP的利用率，利于降低成本及节能环保，同时，在NMP回收设备1中设置热交换装置101，利于实现对NMP废气的热量的回收及利用，提升设备的热量回收利用率，降低设备整体能耗，而可具有良好的实用性。
另外，为便于理解锂电生产中NMP的回收方法的实施过程，本发明还结合回收系统对该回收方法进行详细描述，具体如下：
（1）提纯NMP的过程：
首先，通过热交换装置101初步冷凝涂布机7排出的NMP废气，得到并将降温后的NMP废气输送至冷凝装置102处，进行两级冷凝处理，以得到一级NMP废液和一级NMP气体，随后，一级NMP废液被输送至NMP回收罐104中，且一级NMP气体依次被输送至沸石转轮105和吸收塔处，其中，沸石转轮105脱附后的二级NMP气体被输送至吸收塔，并采用吸收液吸收二级NMP气体中的NMP，得到的二级NMP废液也被输送至NMP回收罐104中。
同时，需注意的是，涂布机7排出的NMP废气在经过热交换装置101时会被初步冷凝而形成三级NMP废液，该三级NMP废液也被输送至NMP回收罐104中，且如果NMP回收罐104中NMP回收液的NMP浓度低于或高于阈值，则可利用NMP回收液作为下塔吸收液，纯水作为上塔吸收液的方式，对NMP回收液进行调节，直至NMP浓度达到阈值要求。
其次，达到阈值要求的回收液会被输送至第一脱水精馏设备2进行脱水分离处理，脱除一级轻组分，采出一级重组分，随后将一级重组分输送至第二脱水精馏设备3处进行二次脱水分离处理，脱除二级轻组分，采出脱水重组分，再将脱水重组分输送至NMP精馏设备4处进行精馏分离处理，采出精馏轻组分中的冷凝液即为NMP成品液。
最终将NMP成品液输送至NMP成品储存罐5，以用于涂布作业，由此完成NMP提纯过程。其中，值得提及的是，上述一级轻组分经第一塔顶冷凝器203冷凝处理后，其分离出的液体作为塔顶废水被输送至废水储存罐10处，在进行废水处理后排放，上述二级轻组分经第二塔顶冷凝器303冷凝处理后，其分离出的液体可与脱水重组分一起被输送至精馏塔401中进行精馏分离处理，而脱除的精馏重组分，则作为残液被输送至残液接收罐9。
（2）回收NMP废气热量的过程：
在上述（1）NMP提纯过程中，通过一级NMP气体经沸石转轮105吸附后得到一级NMP回流气体。将一级轻组分经过第一塔顶冷凝器203、第一回流罐204、第一真空缓冲罐205和第一真空机组206处理的气体，与二级轻组分经过第二塔顶冷凝器303、第二回流罐304、第二真空缓冲罐205和第二真空机组206处理的气体，以及精馏轻组分经过第三塔顶冷凝器403、第三回流罐404、第三真空缓冲罐405和第三真空机组406处理的气体，汇流并形成二级NMP回流气体。
其次，将一级NMP回流气体和二级NMP回流气体均通过与NMP废气热交换后，回流至涂布机7处，以有效回收并利用NMP废气中热量，由此，实现NMP废气的热量回收。
且仍需提及的是，在精馏轻组分经过第三塔顶冷凝器403处理后流入第三回流罐404过程中，精馏轻组分还经由原料预热器407处理，该原料预热器407能够实现对NMP回收液的加热，以利于提升第一脱水塔201的脱水分离效果，如此，便可提升设备热量回收利用率，降低设备整体能耗。此外，本实施例中，经由吸收塔处理后的气体，则作为废气达标气体排放。
以上所述仅为本公开的较佳实施例而已，并不用以限制本公开，凡在本公开的精神和原则之内，所作的任何修改、等同替换、改进等，均应包含在本公开的保护范围之内。

Claims (15)

  1. 一种锂电生产中NMP的回收方法，其特征在于，包括以下步骤：
    S1，获取涂布机中排出的NMP废气，多级冷凝处理所述NMP废气，得到一级NMP废液和一级NMP气体；
    S2，将所述一级NMP气体输送至沸石转轮处进行吸附与脱附处理，得到脱附后的二级NMP气体，再通过吸收液吸收所述二级NMP气体中的NMP，得到二级NMP废液和废气达标气体，并排放所述废气达标气体；
    S3，将所述一级NMP废液和所述二级NMP废液混合得到NMP回收液后，再对所述NMP回收液进行多级脱水处理，脱除脱水轻组分，采出脱水重组分；
    S4，对所述脱水重组分进行精馏处理，脱除精馏重组分，采出精馏轻组分，并通过精馏轻组分得到NMP成品液；
    其中，将所述一级NMP气体经所述沸石转轮吸附后得到的一级NMP回流气体，以及所述脱水轻组分和精馏轻组分经冷凝处理后得到的二级NMP回流气体，均通过与所述NMP废气热交换后，回流至所述涂布机处，而降温后的NMP废气再被进行多级冷凝处理。
  2.  根据权利要求1所述的锂电生产中NMP的回收方法，其特征在于：
    所述S1中的多级冷凝处理包括一级冷凝处理和二级冷凝处理；
    所述一级冷凝处理及所述二级冷凝处理的冷却介质均可采用冷却水和/或冷冻水。
  3.  根据权利要求1所述的锂电生产中NMP的回收方法，其特征在于，还包括以下步骤：
    将所述S2中得到的脱附后的二级NMP气体，与所述S1中的NMP废气混合，并在经过所述多级冷凝处理及所述沸石转轮处理后，再被所述吸收液吸收处理。
  4.  根据权利要求1所述的锂电生产中NMP的回收方法，其特征在于，还包括以下步骤：
    所述一级NMP回流气体和所述二级NMP回流气体均与所述NMP废气热交换后，还得到由所述NMP废气初步冷凝形成的三级NMP废液，并将所述三级NMP废液汇入所述NMP回收液中。
  5.  根据权利要求1所述的锂电生产中NMP的回收方法，其特征在于：
    所述吸收液包括所述NMP回收液和纯水中的至少一种。
  6.  根据权利要求1所述的锂电生产中NMP的回收方法，其特征在于：
    所述吸收液包括一级吸收液和二级吸收液，所述一级吸收液中NMP浓度在1~5%之间，所述二级吸收液中NMP浓度在30~80%之间。
  7.  根据权利要求1所述的锂电生产中NMP的回收方法，其特征在于：
    所述S3中，所述多级脱水处理包括一级脱水处理和二级脱水处理；
    所述NMP回收液经所述一级脱水处理后，脱除一级轻组分，采出一级重组分，随后将一级重组分经由二级脱水处理，并脱除二级轻组分，采出所述脱水重组分，且所述一级轻组分和所述二级轻组分构成所述脱水轻组分。
  8.  根据权利要求7所述的锂电生产中NMP的回收方法，其特征在于：
    对所述一级轻组分冷凝处理，脱除废水，采出一级轻组分气体，并对所述二级轻组分冷凝处理，分别采出含有NMP的二级轻组分液体和二级轻组分气体；
    其中，所述二级轻组分液体被输送至精馏处理中，所述二级NMP回流气体包括所述一级轻组分气体和所述二级轻组分气体。
  9.  根据权利要求1所述的锂电生产中NMP的回收方法，其特征在于，所述脱水轻组分和精馏轻组分经冷凝处理后得到的二级NMP回流气体时，还包括以下步骤：
    所述精馏轻组分先经由冷凝处理，再与NMP回收液热交换后，得到精馏轻组分气体和所述NMP成品液，其中，所述二级NMP回流气体包括所述精馏轻组分气体。
  10.  根据权利要求1所述的锂电生产中NMP的回收方法，其特征在于：
    进行所述多级脱水处理的所述NMP回收液中的NMP浓度在30~80%之间。
  11.  根据权利要求1至10中任一项所述的锂电生产中NMP的回收方法，其特征在于：
    所述一级NMP气体中NMP浓度在150~200ppm之间；和/或，
    所述废气达标气体的NMP含量不高于25mg/m³，且所述废气达标气体占所述NMP废气的重量在5~10%。
  12.  一种锂电生产中NMP的回收系统，其特征在于：
    包括依次连通设置的所述NMP回收设备、第一脱水精馏设备、第二脱水精馏设备、NMP精馏设备和NMP成品储存罐，且所述NMP回收设备包括热交换装置、冷凝装置、NMP吸收装置和NMP回收罐；
    所述热交换装置包括能够实现热交换的第一换热通道和第二换热通道，所述第一换热通道的一端与涂布机的排风口相连通，另一端分别与所述冷凝装置的进气口和所述NMP回收罐相连，所述第二换热通道的一端与所述涂布机的送风口相连通，另一端分别与所述NMP吸收装置、所述第一脱水精馏设备、所述第二脱水精馏设备和所述NMP精馏设备的气体采出口相连通；
    所述冷凝装置中具有与所述NMP吸收装置相连的排气口，以及与所述NMP回收罐相连的排液口，且所述NMP吸收装置通过所述NMP回收罐与所述第一脱水精馏设备相连。
  13.  根据权利要求12所述的锂电生产中NMP的回收系统，其特征在于：
    所述NMP吸收装置包括与所述排气口连通的沸石转轮，以及与所述沸石转轮的脱附端相连的吸收塔，且所述吸收塔与所述NMP回收罐相连。
  14.  根据权利要求12所述的锂电生产中NMP的回收系统，其特征在于：
    所述NMP回收罐和所述第一脱水精馏设备之间连接有原料预热器，且所述原料预热器还连接在所述NMP精馏设备中的第三塔顶冷凝器与第三回流罐之间。
  15.  根据权利要求12所述的锂电生产中NMP的回收系统，其特征在于：
    所述第一脱水精馏设备包括与所述NMP回收罐相连的第一脱水塔，与所述第一脱水塔相连的第一再沸器和第一塔顶冷凝器，以及依次连通在所述第一塔顶冷凝器下游的第一回流罐、第一真空缓冲罐和第一真空机组，并在所述第一回流罐的排液口还连通有废水储存罐。
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