CN110416652A - A method of separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings - Google Patents
A method of separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings Download PDFInfo
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- CN110416652A CN110416652A CN201910595031.9A CN201910595031A CN110416652A CN 110416652 A CN110416652 A CN 110416652A CN 201910595031 A CN201910595031 A CN 201910595031A CN 110416652 A CN110416652 A CN 110416652A
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- pvdf
- iron phosphate
- lithium iron
- waste lithium
- phosphate positive
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- 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
- H01M10/54—Reclaiming serviceable parts of waste accumulators
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- 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
Abstract
The method that the present invention relates to a kind of to separate and recover PVDF from waste lithium iron phosphate positive powder acidleach tailings, it is characterized in that, the following steps are included: step 1, with organic solvent by the PVDF selective dissolution in waste lithium iron phosphate positive powder acidleach tailings, PVDF lysate is obtained after solid-liquor separation；PVDF lysate obtained in step 1 is heated, organic dissolution is made to volatilize by step 2, is realized the separation of PVDF and organic solvent, is obtained regenerated PVDF product.The method flow that the present invention separates and recovers PVDF from waste lithium iron phosphate positive powder acidleach tailings is simple, it can be achieved that the high level of PVDF recycles, and process of the present invention cleans, no waste water and exhaust gas discharge.
Description
Technical field
The present invention relates to technical field of resource recovery, more particularly, to one kind from waste lithium iron phosphate positive powder acidleach tailings
The method of middle separation and recovery PVDF.
Background technique
Lithium iron phosphate positive material (abbreviation LFP) is because its raw material sources is abundant, inexpensive, nontoxic, theoretical capacity is high, thermostabilization
Property good and good cycle the advantages that be concerned, be the developing direction of power battery.As lithium iron phosphate dynamic battery makes
The increase of dosage, the disposition of waste lithium iron phosphate battery will become the key link of new energy field.Old and useless battery positive electrode
If cannot get safe handling, huge harm will be generated to environment and public safety.Normal practice is mainly by battery through putting at present
Crust, the metal simple-substance in collector, positive powder and negative electrode powder etc. are recycled after electricity, dismantling.The positive powder recycled after dismantling is main
It is head product containing LiFePO4, pure aluminum and binder PVDF etc., generally also needs that resource just can be achieved by chemical recycling
High level regeneration.
Currently, the recovery method of waste and old waste lithium iron phosphate positive electrode is mainly sulfuric acid leaching technique.Its basic process
It is dissolved in sulfuric acid for applying waste lithium ionic positive electrode, then adjusts pH of leaching solution to alkalinity with sodium carbonate, make in leachate
Iron and phosphorus formed phosphoric acid iron product, lithium ion formed lithium carbonate product.
It is poly- inclined to mainly contain PVDF(for the leaching residue of sulfuric acid leaching technique, i.e. waste lithium iron phosphate positive powder acidleach tailings
Vinyl fluoride) and a small amount of unrecovered LiFePO4, at present without reasonable method of disposal.PVDF is a kind of high-intensitive, corrosion resistant
Substance has both the characteristic of fluororesin and resins for universal use, except with good chemical corrosion resistance, heat-resisting quantity, oxidative resistance,
Outside weatherability, resistance to ray radiation performance, also there are the properties such as piezoelectricity, dielectricity, pyroelectricity, be yield in fluoro-containing plastic
The big product ating the second place, purposes are extremely wide.Therefore, recycle PVDF's from waste lithium iron phosphate positive powder acidleach tailings
It is significant.
Summary of the invention
The present invention devises a kind of method that PVDF is separated and recovered from waste lithium iron phosphate positive powder acidleach tailings, solution
Certainly the technical issues of is that PVDF widely used in waste lithium iron phosphate positive powder acidleach tailings lacks recovery method.
In order to solve above-mentioned technical problem, present invention employs following scheme:
A method of separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings, which is characterized in that including following
Step:
Step 1, with organic solvent by the PVDF selective dissolution in waste lithium iron phosphate positive powder acidleach tailings, solid-liquor separation
PVDF lysate is obtained afterwards；
PVDF lysate obtained in step 1 is heated, organic dissolution is made to volatilize by step 2, realize PVDF with it is organic molten
The separation of agent obtains regenerated PVDF product.
Further, the organic solvent condensate to volatilize in step 2 is formed into condensate liquid, the condensate liquid is as in step 1
Organic solvent be used to dissolve PVDF in waste lithium iron phosphate positive powder acidleach tailings.
Further, the organic solvent in step 1 is N-Methyl pyrrolidone, dimethyl acetamide or N, N- diformazan
The mixture of one or more of base formamide.
Further, the solution temperature of PVDF described in step 1 is room temperature~100 DEG C.
Further, the solution temperature of PVDF described in step 1 is room temperature~100 DEG C.
Further, the heating of PVDF lysate described in step 2 makes 170~250 DEG C of temperature that organic solvent volatilizees.
Further, the heating of PVDF lysate described in step 2 makes 170~250 DEG C of temperature that organic solvent volatilizees.
Further, the heating of PVDF lysate described in step 2 makes 170~250 DEG C of temperature that organic solvent volatilizees.
The method that PVDF is separated and recovered from waste lithium iron phosphate positive powder acidleach tailings has the advantages that
(1) present invention separated and recovered from waste lithium iron phosphate positive powder acidleach tailings PVDF method flow it is simple, it can be achieved that
The wherein high level recycling of PVDF.
(2) purity of product of the invention regeneration PVDF product is greater than 99.5wt%, can reach the requirement of relevant criterion.
(3) process of the present invention cleans, no waste water and exhaust gas discharge.
Detailed description of the invention
Fig. 1: the present invention separates and recovers the process flow chart of PVDF from waste lithium iron phosphate positive powder acidleach tailings.
Specific embodiment
Below with reference to figure, the present invention will be further described:
As shown in Figure 1, a kind of method that PVDF is separated and recovered from waste lithium iron phosphate positive powder acidleach tailings, including walk as follows
It is rapid:
Step 1 obtains waste lithium iron phosphate positive powder acidleach tailings organic solvent selective dissolution PVDF after solid-liquor separation
Obtain PVDF lysate；
Step 2, the PVDF lysate that step 1 is obtained heat, and organic dissolution is made to volatilize, and realize point of PVDF and organic solvent
From, and regeneration PVDF product is made；
Step 3, the organic solvent condensate that will be volatilized in step 2, condensate liquid return step one is for dissolving PVDF.
Embodiment 1
A method of it separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings, includes the following steps:
Step 1, by waste lithium iron phosphate positive powder acidleach tailings N-Methyl pyrrolidone selective dissolution at normal temperature
PVDF obtains PVDF lysate after solid-liquor separation；
PVDF lysate obtained in step 1 is heated up to 250 DEG C, N-Methyl pyrrolidone is made to volatilize by step 2, is realized
The separation of PVDF and N-Methyl pyrrolidone, and regeneration PVDF product is made；
Step 3 condenses the N-Methyl pyrrolidone to volatilize in step 2, and condensate liquid return step one is for dissolving PVDF.
The regeneration PVDF product sampling obtained after the N-Methyl pyrrolidone that volatilizees, analyzing its purity is 99.6%.
Embodiment 2
A method of it separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings, includes the following steps:
Step 1, by waste lithium iron phosphate positive powder acidleach tailings dimethyl acetamide selective dissolution PVDF at 100 DEG C,
PVDF lysate is obtained after solid-liquor separation；
PVDF lysate obtained in step 1 is heated up to 250 DEG C, dimethyl acetamide is made to volatilize by step 2, realizes PVDF
With the separation of dimethyl acetamide, and be made regeneration PVDF product；
Step 3 condenses the dimethyl acetamide volatilized in step 2, and condensate liquid return step one is for dissolving PVDF.
The regeneration PVDF product sampling obtained after dimethyl acetamide of volatilizing, analyzing its purity is 99.5%.
Embodiment 3
A method of it separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings, includes the following steps:
Step 1, by waste lithium iron phosphate positive powder acidleach tailings n,N-Dimethylformamide selective dissolution at 100 DEG C
PVDF obtains PVDF lysate after solid-liquor separation；
PVDF lysate obtained in step 1 is heated up to 170 DEG C, n,N-Dimethylformamide is made to volatilize by step 2, is realized
The separation of PVDF and n,N-Dimethylformamide, and regeneration PVDF product is made；
Step 3 condenses the n,N-Dimethylformamide volatilized in step 2, and condensate liquid return step one is for dissolving PVDF.
The regeneration PVDF product sampling obtained after n,N-Dimethylformamide of volatilizing, analyzing its purity is 99.8%.
Above in conjunction with attached drawing, an exemplary description of the invention, it is clear that realization of the invention is not by aforesaid way
Limitation, as long as use the inventive concept and technical scheme of the present invention carry out various improvement, or it is not improved will be of the invention
Conception and technical scheme directly apply to other occasions, be within the scope of the invention.
Claims (8)
1. it is a kind of from waste lithium iron phosphate positive powder acidleach tailings separate and recover PVDF method, which is characterized in that including with
Lower step:
Step 1, with organic solvent by the PVDF selective dissolution in waste lithium iron phosphate positive powder acidleach tailings, solid-liquor separation
PVDF lysate is obtained afterwards；
PVDF lysate obtained in step 1 is heated, organic dissolution is made to volatilize by step 2, realize PVDF with it is organic molten
The separation of agent obtains regenerated PVDF product.
2. the method for separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings according to claim 1, special
Sign is: the organic solvent condensate to volatilize in step 2 being formed condensate liquid, the condensate liquid is as organic molten in step 1
Agent is used to dissolve the PVDF in waste lithium iron phosphate positive powder acidleach tailings.
3. the method according to claim 1 or claim 2 that PVDF is separated and recovered from waste lithium iron phosphate positive powder acidleach tailings,
Be characterized in that: the organic solvent in step 1 is N-Methyl pyrrolidone, dimethyl acetamide or N, N- dimethyl formyl
The mixture of one or more of amine.
4. the method according to claim 1 or claim 2 that PVDF is separated and recovered from waste lithium iron phosphate positive powder acidleach tailings,
Be characterized in that: the solution temperature of PVDF described in step 1 is room temperature~100 DEG C.
5. the method for separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings according to claim 3, special
Sign is: the solution temperature of PVDF described in step 1 is room temperature~100 DEG C.
6. according to claim 1, any in 2 or 5 described separate and recover from waste lithium iron phosphate positive powder acidleach tailings
The method of PVDF, it is characterised in that: the temperature 170 that the heating of PVDF lysate described in step 2 makes organic solvent volatilize~
250℃。
7. the method for separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings according to claim 3, special
Sign is: the heating of PVDF lysate described in step 2 makes 170~250 DEG C of temperature that organic solvent volatilizees.
8. the method for separating and recovering PVDF from waste lithium iron phosphate positive powder acidleach tailings according to claim 4, special
Sign is: the heating of PVDF lysate described in step 2 makes 170~250 DEG C of temperature that organic solvent volatilizees.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111710932A (en) * | 2020-08-11 | 2020-09-25 | 湖南省正源储能材料与器件研究所 | Method for recovering binder of retired lithium ion battery anode |
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| CN108736086A (en) * | 2017-08-31 | 2018-11-02 | 苏州威星能源科技有限公司 | A kind of recovery method of lithium ion cell positive waste paper |
| CN109713393A (en) * | 2018-12-30 | 2019-05-03 | 沈阳化工研究院有限公司 | A kind of isolated method of lithium battery active material |
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- 2019-07-03 CN CN201910595031.9A patent/CN110416652A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106129513A (en) * | 2016-08-22 | 2016-11-16 | 北京小飞融创新能源科技有限公司 | A kind of recovery method of waste lithium cell |
| CN108736086A (en) * | 2017-08-31 | 2018-11-02 | 苏州威星能源科技有限公司 | A kind of recovery method of lithium ion cell positive waste paper |
| CN109713393A (en) * | 2018-12-30 | 2019-05-03 | 沈阳化工研究院有限公司 | A kind of isolated method of lithium battery active material |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111710932A (en) * | 2020-08-11 | 2020-09-25 | 湖南省正源储能材料与器件研究所 | Method for recovering binder of retired lithium ion battery anode |
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