CN104001371A - Method for recycling waste dust removal filter material - Google Patents
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- CN104001371A CN104001371A CN201410234898.9A CN201410234898A CN104001371A CN 104001371 A CN104001371 A CN 104001371A CN 201410234898 A CN201410234898 A CN 201410234898A CN 104001371 A CN104001371 A CN 104001371A
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Abstract
The invention relates to a method for recycling waste dust removal filter material. The method takes the industrial waste dust removal filter material as precursor, and comprises the steps of preparing filter material-based activated carbon fiber (ACF) with larger specific surface area by carbonization and activation, loading a manganese oxide catalyst onto the filter material-based ACF to enable the filter material-based ACF to be applied to the field of low-temperature denitration catalysis, and combining the filter material-based ACF with polyphenylene sulfite (PPS) dust removal filter material. The prepared MnOx/ACF@PPS filter material not only has a dust removal function, but also has a certain denitration effect; the mechanical property of the obtained composite filter material is hardly influenced. The method provides a good thought for solving the problem of industrial waste material treatment, so that the resource can be recycled.
Description
Technical field
The present invention relates to a kind of recoverying and utilizing method of discarded dedusting filtrate, belong to filtrate preparation field.
Background technology
China is coal-fired big country, and burning of coal will be discharged a large amount of pollutant (toxic gas and dust).What at present China was used for controlling coal fired thermal power plant burning and exhausting soot dust granule is the sack cleaner taking filtrate as core, and due to long high-temperature operation, these filtrates will lose the effect of dedusting gradually because of breakage, thereby become trade waste.The mode of industrial these discarded objects of processing mainly contains two kinds: a kind ofly become gas and solid residue by the mode of waste incineration, to dwindle the space of occupying of these discarded objects; Another kind of is exactly to utilize the mode that is similar to municipal refuse landfill by its concentrated landfill.But these two kinds of modes all can not effectively utilize these resources, also easily cause secondary pollution.
And filtrate is substantially by fibrous, the feasibility of preparing NACF is very high, can also greatly reduce costs.In addition, the absorption property that NACF is become reconciled due to its high specific area, is widely used in gas purification, the fields such as catalytic carrier.In recent years, the research of low-temperature SCR catalyst has become focus.Therefore, discarded dedusting filtrate is prepared into NACF, and makes it as low-temperature denitration catalyst carrier, this support type denitrating catalyst is combined with PPS dedusting filtrate simultaneously, to reaching the double effects of dedusting and denitration, this is a good thinking beyond doubt.
Summary of the invention
The object of the invention is to for the deficiencies in the prior art, a kind of recoverying and utilizing method of discarded dedusting filtrate is provided, to discard dedusting filtrate as presoma, make composite filtering material; Greatly reduce like this cost of composite filtering material, and realized the resource reutilization of discarded dedusting filtrate, for the processing of industrial waste dedusting filtrate provides a good thinking.
The present invention is in order to solve the problems of the technologies described above, and the technical scheme adopting is:
A recoverying and utilizing method for discarded dedusting filtrate taking industrial discarded dedusting filtrate as presoma, makes filtrate based active carbon fiber (ACF) after pretreatment, activation; Then Supported Manganese oxide, makes support type denitrating catalyst; Finally applied, be bonded on PPS dedusting filtrate, made the composite filtering material that has dedusting and denitration function concurrently.
Described discarded dedusting filtrate is the aging product of industrial dedusting aramid fiber Nomex filtrate used, described PPS dedusting filtrate is taking polyphenylene sulfide fibre as raw material, be prepared from through shredding, compound batch mixing, combing, lapping, acupuncture, thermal finalization and the press polish of singing, average pore size is 37 μ m.
The recoverying and utilizing method of described discarded dedusting filtrate, concrete steps are:
(1) pretreatment and the activation of discarded dedusting filtrate: after discarded dedusting filtrate decontamination cleaning up, dry, carry out successively, after carbonization, activation, obtaining filtrate based active carbon fiber under inert gas shielding;
(2) preparation of support type denitrating catalyst: filtrate based active carbon fiber is after salpeter solution is processed, and suction filtration, is neutral by washed with de-ionized water to pH value, dry 12-24 h in baking oven; Get the filtrate based active carbon fiber after acidifying, adopt just wet infusion process to make filtrate based active carbon fiber dipping absorption manganese acetate ethanolic solution; Then filtrate based active carbon fiber is calcined at 250-350 DEG C to 30-120 min, obtained support type denitrating catalyst;
(3) preparation of composite filtering material: support type denitrating catalyst is mixed with to thick fluid with ethanol, then it is coated in to PPS filter material surface equably, then drip ethanol on its surface, then exert pressure and make support type denitrating catalyst enter PPS filtrate inside with ethanol with mould, in baking oven, at 80-110 DEG C, evaporate ethanol, carry out the load capacity of control load type denitrating catalyst on PPS filtrate by applying number of times; Then the adhesive solution that drips saturation capacity on composite filtering material surface, dries 12-24 h, finally in baking oven, at 110 DEG C, dries 12-24 h;
The described carbonization of step (1) is at 700-900 DEG C of carbonization 30-120 min;
Activation described in step (1) is chemical activation method, and in the filtrate after activator and carbonization, the mass ratio of carbon is 4:1, and at 700-900 DEG C of activation 30-120 min, wherein activator is KOH;
In step (2), adopt 30-60 wt% salpeter solution to process 60-120 min to filtrate based active carbon fiber;
Dipping in step (2) is at room temperature flooding 12-24 h; After dipping, in baking oven, be dried 12-24 h;
In step (2), the mass concentration of manganese acetate ethanolic solution is 1-20%; By the load capacity of manganese in the concentration control filtrate of manganese acetate ethanolic solution;
The dimethyl formamide solution that adhesive solution described in step (3) is Kynoar, its mass concentration is 1-5 wt%.
The prepared MnOx/ACF@of the present invention PPS composite filtering material is the ACF that utilizes industrial dedusting waste aramid material used to obtain after carbonization-activation, again through acidifying, metal oxide-loaded, finally combine with PPS filtrate, effectively had concurrently the composite filtering material of dedusting and the double function of denitration; Taking PPS needle punched filter material as matrix, the ACF of high-specific surface area is carrier, Mn oxide is active component, has improved to a great extent dust in industrial tail gas and the discharge amount of pollution of NOx.
Compared with prior art, beneficial effect of the present invention is:
(1) raw material is easy to get, and cost is low, for the aramid fiber filtrate of industrial waste, is conducive to industrialized production;
(2) preparation method's technology maturation of NACF and supported catalyst;
(3) gained intermediate products ACF can be used for the aspects such as environmental protection, chemical industry, medical and catalysis, has wide practical use;
(4) when the composite filtering material of gained is applied to industrial tail gas and processes, both can dedusting, again can denitration;
(5) processing that the preparation thinking of products obtained therefrom is trade waste provides a good thinking, is conducive to the protection of environment.
Brief description of the drawings
The SEM figure of the original polyphenylene sulfide Nomex of Fig. 1 filtrate;
The SEM figure of the MnOx/ACF that Fig. 2 embodiment 1 makes;
The SEM figure of the MnOx/ACF@PPS composite filtering material that Fig. 3 embodiment 1 makes;
Fig. 4 makes tubular type SCR reactor assembly figure by oneself; 1-source of the gas; 2-pressure-reducing valve; 3-mass flowmenter; 4-blender; 5-preheater; 6-catalytic bed; 7-catalytic bed; 8-flue gas analyzer;
The ultimate strength block diagram of broadwise and warp-wise before and after Fig. 5 PPS filtrate load MnOx/ACF catalyst.
Detailed description of the invention
In order to understand better the present invention, further illustrate content of the present invention below in conjunction with embodiment, but content of the present invention is not only confined to the following examples.
The present invention adopts its scanning electron microscope (SEM) photograph of PPS filtrate as shown in Figure 1.
Embodiment 1
(1) will discard the filtrate decontamination of dedusting aramid fiber and clean up, after oven dry, first at inert gas N
2protect lower 800 DEG C of carbonization 60 min, the ratio that is 4:1 with KOH according to alkali carbon mass ratio is at N again
2protect lower 800 DEG C of activation 60 min, obtain specific area up to 2493.049 m
2the aramid fiber filtrate based active carbon fiber (ACF) of/g;
(2) ACF in (1) is processed to 120 min with 30 wt% salpeter solutions, suction filtration, makes its pH value to neutrality by washed with de-ionized water, is dried 12 h in baking oven;
(3) get the ACF after 0.3 g acidifying in (2), prepare the manganese acetate ethanolic solution that 3.0 g mass concentrations are 2.86 % simultaneously, (≈ 0.66 g) to adopt just wet infusion process to make the saturated manganese acetate ethanolic solution of ACF dipping absorption, at room temperature flood after 12-24 h, dry 12-24 h in baking oven, mole load capacity computational methods for manganese are: 0.66 × 2.86% ÷ 245.09 ÷ 0.3 × 12=3.08 ‰;
(4) ACF that is impregnated with manganese acetate dried in (3) is calcined to 30 min at 300 DEG C, can obtain load capacity and be 3.08 ‰ MnOx/ACF low-temperature denitration catalyst; Fig. 2 is the SEM figure of MnOx/ACF;
(5) get MnOx/ACF low-temperature denitration catalyst in (4), be mixed with thick fluid with a small amount of ethanol, then the catalyst of 25 mg is coated in equably to the circular PPS filter material surface that diameter is 3.8 cm by the method applying at every turn, then drip ethanol on its surface, exert pressure and make supported catalyst enter PPS filtrate inside with ethanol with mould, in baking oven, at 80 DEG C, evaporate ethanol, repeat aforesaid operations and make for four times the catalyst of 100 mg enter PPS filtrate inside completely, the load capacity of catalyst on PPS filtrate is 8.8 mg/cm
2;
(6) preparation mass concentration is the dimethyl formamide solution of 1wt% Kynoar, on composite filtering material surface in (5), drip this adhesive solution of saturation capacity, then dry 12h, finally in baking oven, at 110 DEG C, dry 12 h, get final product to obtain cementability MnOx/ACF@PPS composite filtering material; Fig. 3 is the SEM figure of MnOx/ACF@PPS composite filtering material;
The denitration performance of MnOx/ACF@PPS composite filtering material is evaluated in the homemade SCR reactor in laboratory (as shown in Figure 4).Total gas flow rate is 700 ml/min, wherein NO and NH
3volume fraction be 0.05%, O
2volume fraction be 5%, all the other are balanced gas N
2.Through active testing, the denitration efficiency of prepared MnOx/ACF@PPS composite filtering material in the time of 180 DEG C can reach 38.8%; And this composite filtering material has dedusting function.
Embodiment 2
(1) will discard the filtrate decontamination of dedusting aramid fiber and clean up, after oven dry, first at inert gas N
2protect lower 700 DEG C of carbonization 120 min, the ratio that is 4:1 with KOH according to alkali carbon mass ratio is at N again
2protect lower 800 DEG C of activation 60 min, obtain specific area up to 2493.049 m
2the aramid fiber filtrate based active carbon fiber (ACF) of/g;
(2) ACF in (1) is processed to 60 min with 60 wt% salpeter solutions, suction filtration, approaches its pH value by washed with de-ionized water neutral, dry 18 h in baking oven;
(3) get the ACF after 0.3 g acidifying in (2), prepare the manganese acetate ethanolic solution that 3.0 g mass concentrations are 8.38% simultaneously, (≈ 0.66 g) to adopt just wet infusion process to make the saturated manganese acetate ethanolic solution of ACF dipping absorption, at room temperature flood after 18 h, dry 18 h in baking oven, mole load capacity computational methods for manganese are: 0.66 × 83.8 ‰ ÷ 245.09 ÷ 0.3 × 12=9.02 ‰;
(4) ACF that is impregnated with manganese acetate dried in (3) is calcined to 30 min at 300 DEG C, can obtain load capacity and be 9.02 ‰ MnOx/ACF low-temperature denitration catalyst;
(5) get MnOx/ACF low-temperature denitration catalyst in (4), be mixed with thick fluid with a small amount of ethanol, then the catalyst of 25 mg is coated in equably to the circular PPS filter material surface that diameter is 3.8 cm by the method applying at every turn, then drip ethanol on its surface, exert pressure and make supported catalyst enter PPS filtrate inside with ethanol with mould, in baking oven, at 95 DEG C, evaporate ethanol, repeat aforesaid operations and make for four times the catalyst of 100 mg enter PPS filtrate inside completely, the load capacity of catalyst on PPS filtrate is 8.8 mg/cm
2;
(6) preparation mass concentration is the dimethyl formamide solution of 3 wt% Kynoar, on composite filtering material surface in (5), drip this adhesive solution of saturation capacity, then dry 18 h, finally in baking oven, at 110 DEG C, dry 18 h, get final product to obtain cementability MnOx/ACF@PPS composite filtering material;
The denitration performance of MnOx/ACF@PPS composite filtering material is evaluated in the homemade SCR reactor in laboratory; Total gas flow rate is 700 ml/min, wherein NO and NH
3volume fraction be 0.05%, O
2volume fraction be 5%, all the other are balanced gas N
2.Through active testing, the denitration efficiency of prepared MnOx/ACF@PPS composite filtering material in the time of 180 DEG C can reach 51.9%; And this composite filtering material has dedusting function.
Embodiment 3
(1) will discard the filtrate decontamination of dedusting aramid fiber and clean up, after oven dry, first at inert gas N
2protect lower 880 DEG C of carbonization 60 min, the ratio that is 4:1 with KOH according to alkali carbon mass ratio is at N again
2protect lower 900 DEG C of activation 30 min, obtain specific area up to 2493.049 m
2the aramid fiber filtrate based active carbon fiber (ACF) of/g;
(2) ACF in (1) is processed to 120 min with 30 wt% salpeter solutions, suction filtration, approaches its pH value by washed with de-ionized water neutral, dry 24 h in baking oven;
(3) get the ACF after 0.3 g acidifying in (2), prepare the manganese acetate ethanolic solution that 3.0 g mass concentrations are 16.6% simultaneously, (≈ 0.66 g) to adopt just wet infusion process to make the saturated manganese acetate ethanolic solution of ACF dipping absorption, at room temperature flood after 24 h, dry 24 h in baking oven, mole load capacity computational methods for manganese are: 0.66 × 166.9 ‰ ÷ 245.09 ÷ 0.3 × 12=17.97 ‰;
(4) ACF that is impregnated with manganese acetate dried in (3) is calcined to 30 min at 300 DEG C, can obtain load capacity and be 17.97 ‰ MnOx/ACF low-temperature denitration catalyst;
(5) get MnOx/ACF low-temperature denitration catalyst in (4), be mixed with thick fluid with a small amount of ethanol, then the catalyst of 25 mg is coated in equably to the circular PPS filter material surface that diameter is 3.8 cm by the method applying at every turn, then drip ethanol on its surface, exert pressure and make supported catalyst enter PPS filtrate inside with ethanol with mould, in baking oven, at 110 DEG C, evaporate ethanol, repeat aforesaid operations and make for four times the catalyst of 100 mg enter PPS filtrate inside completely, the load capacity of catalyst on PPS filtrate is 8.8 mg/cm
2;
(6) preparation mass concentration is the dimethyl formamide solution of 5 wt% Kynoar, on composite filtering material surface in (5), drip this adhesive solution of saturation capacity, then dry 24 h, finally in baking oven, at 110 DEG C, dry 24 h, get final product to obtain cementability MnOx/ACF@PPS composite filtering material;
The denitration performance of MnOx/ACF@PPS composite filtering material is evaluated in the homemade SCR reactor in laboratory.Total gas flow rate is 700 ml/min, wherein NO and NH
3volume fraction be 0.05%, O
2volume fraction be 5%, all the other are balanced gas N
2.Through active testing, the denitration efficiency of prepared MnOx/ACF@PPS composite filtering material in the time of 180 DEG C can reach 69.5%.
Embodiment 4
(1) will discard the filtrate decontamination of dedusting aramid fiber and clean up, after oven dry, first at inert gas N
2protect lower 880 DEG C of carbonization 60 min, the ratio that is 4:1 with KOH according to alkali carbon mass ratio is at N again
2protect lower 800 DEG C of activation 60 min, obtain specific area up to 2493.049 m
2the aramid fiber filtrate based active carbon fiber (ACF) of/g;
(2) ACF in (1) is processed to 120 min with 30 wt% salpeter solutions, suction filtration, approaches its pH value by washed with de-ionized water neutral, dry 18 h in baking oven;
(3) get the ACF after 0.3 g acidifying in (2), prepare the manganese acetate ethanolic solution that 3.0 g mass concentrations are 166 ‰ simultaneously, (≈ 0.66 g) to adopt just wet infusion process to make the saturated manganese acetate ethanolic solution of ACF dipping absorption, at room temperature flood after 12-24 h, dry 20 h in baking oven, mole load capacity computational methods for manganese are: 0.66 × 166.9 ‰ ÷ 245.09 ÷ 0.3 × 12=17.97 ‰;
(4) ACF that is impregnated with manganese acetate dried in (3) is calcined to 30 min at 300 DEG C, can obtain load capacity and be 17.97 ‰ MnOx/ACF low-temperature denitration catalyst;
(5) get MnOx/ACF low-temperature denitration catalyst in (4), be mixed with thick fluid with a small amount of ethanol, then the catalyst of 25 mg is coated in equably to the circular PPS filter material surface that diameter is 3.8 cm by the method applying at every turn, then drip ethanol on its surface, exert pressure and make supported catalyst enter PPS filtrate inside with ethanol with mould, in baking oven, at 100 DEG C, evaporate ethanol, repeat aforesaid operations and make for eight times the catalyst of 200 mg enter PPS filtrate inside completely, the load capacity of catalyst on PPS filtrate is 17.6 mg/cm
2;
(6) preparation mass concentration is the dimethyl formamide solution of 3wt% Kynoar, on composite filtering material surface in (5), drip this adhesive solution of saturation capacity, then dry 20 h, finally in baking oven, at 110 DEG C, dry 20 h, get final product to obtain cementability MnOx/ACF@PPS composite filtering material;
The denitration performance of MnOx/ACF@PPS composite filtering material (as shown in Figure 4) in the homemade SCR reactor in laboratory is evaluated.Total gas flow rate is 700 ml/min, wherein NO and NH
3volume fraction be 0.05%, O
2volume fraction be 5%, all the other are balanced gas N
2.Through active testing, the denitration efficiency of prepared MnOx/ACF@PPS composite filtering material in the time of 180 DEG C can reach 85.8%;
Contrast by experiment, we find in the time that the molar ratio of Mn oxide and NACF is lower, the MnOx/ACF@PPS composite filtering material of identical load amount only has certain denitration performance, and along with the increase of manganese carbon molar ratio, the NO conversion ratio of composite filtering material is in rising trend.And in the situation that other conditions are identical, along with the increase of load capacity, the denitration efficiency of MnOx/ACF@PPS composite filtering material becomes larger.In addition, from the SEM figure of sample, can find out, between MnOx/ACF and PPS filtrate, have certain combination, illustrate and can make the catalyst difficult drop-off in PPS filtrate inside by the method in this experiment, be conducive to strengthen the denitration stability of composite filtering material.Fig. 5 shows that the carrying method using in this experiment is little on the impact of the ultimate strength of PPS filtrate own, and after load MnOx/ACF catalyst, the broadwise of PPS filtrate and warp-wise ultimate strength all increase to some extent.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (9)
1. a recoverying and utilizing method for discarded dedusting filtrate, is characterized in that: taking industrial discarded dedusting filtrate as presoma, after pretreatment, activation, make filtrate based active carbon fiber; Then Supported Manganese oxide, makes support type denitrating catalyst; Finally applied, be bonded on PPS dedusting filtrate, made the composite filtering material that has dedusting and denitration function concurrently.
2. the recoverying and utilizing method of discarded dedusting filtrate according to claim 1, it is characterized in that: described discarded dedusting filtrate is the aging product of industrial dedusting aramid fiber Nomex filtrate used, described PPS dedusting filtrate is taking polyphenylene sulfide fibre as raw material, be prepared from through shredding, compound batch mixing, combing, lapping, acupuncture, thermal finalization and the press polish of singing, average pore size is 37 μ m.
3. the recoverying and utilizing method of discarded dedusting filtrate according to claim 1, is characterized in that: concrete steps are:
(1) pretreatment and the activation of discarded dedusting filtrate: after discarded dedusting filtrate decontamination cleaning up, dry, carry out successively, after carbonization, activation, obtaining filtrate based active carbon fiber under inert gas shielding;
(2) preparation of support type denitrating catalyst: filtrate based active carbon fiber is after salpeter solution is processed, and suction filtration, is neutral by washed with de-ionized water to pH value, dry 12-24 h in baking oven; Get the filtrate based active carbon fiber after acidifying, adopt just wet infusion process to make filtrate based active carbon fiber dipping absorption manganese acetate ethanolic solution; Then filtrate based active carbon fiber is calcined at 250-350 DEG C to 30-120 min, obtained support type denitrating catalyst;
(3) preparation of composite filtering material: support type denitrating catalyst is mixed with to thick fluid with ethanol, then it is coated in to PPS filter material surface equably, then drip ethanol on its surface, then exert pressure and make support type denitrating catalyst enter PPS filtrate inside with ethanol, in baking oven, at 80-110 DEG C, evaporate ethanol; Then the adhesive solution that drips saturation capacity on composite filtering material surface, dries 12-24 h, finally in baking oven, at 110 DEG C, dries 12-24 h.
4. according to the recoverying and utilizing method of the discarded dedusting filtrate described in claim 3, it is characterized in that: the described carbonization of step (1) is at 700-900 DEG C of carbonization 30-120 min.
5. according to the recoverying and utilizing method of the discarded dedusting filtrate described in claim 3, it is characterized in that: the activation described in step (1) is chemical activation method, in filtrate after activator and carbonization, the mass ratio of carbon is 4:1, and at 700-900 DEG C of activation 30-120 min, wherein activator is KOH.
6. according to the recoverying and utilizing method of the discarded dedusting filtrate described in claim 3, it is characterized in that: in step (2), adopt 30-60 wt% salpeter solution to process 60-120 min to filtrate based active carbon fiber.
7. according to the recoverying and utilizing method of the discarded dedusting filtrate described in claim 3, it is characterized in that: the dipping in step (2) is at room temperature flooding 12-24 h; After dipping, in baking oven, be dried 12-24 h.
8. according to the recoverying and utilizing method of the discarded dedusting filtrate described in claim 3, it is characterized in that: in step (2), the mass concentration of manganese acetate ethanolic solution is 1-20%.
9. according to the recoverying and utilizing method of the discarded dedusting filtrate described in claim 3, it is characterized in that: the dimethyl formamide solution that the adhesive solution described in step (3) is Kynoar, its mass concentration is 1-5 wt%.
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CN104941319B (en) * | 2015-06-19 | 2016-06-29 | 合肥工业大学 | A kind of preparation method of manganio dedusting denitrification integral function filter material |
CN106925034A (en) * | 2017-04-27 | 2017-07-07 | 福州大学 | A kind of preparation method of denitration function polyphenylene sulfide composite filtering material |
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CN104941319B (en) * | 2015-06-19 | 2016-06-29 | 合肥工业大学 | A kind of preparation method of manganio dedusting denitrification integral function filter material |
CN106925034A (en) * | 2017-04-27 | 2017-07-07 | 福州大学 | A kind of preparation method of denitration function polyphenylene sulfide composite filtering material |
CN106925034B (en) * | 2017-04-27 | 2018-12-25 | 福州大学 | A kind of preparation method of denitration function polyphenylene sulfide composite filtering material |
CN110508274A (en) * | 2019-08-12 | 2019-11-29 | 四川大学 | Modification biological charcoal low-temperature denitration catalyst and its application |
CN110508274B (en) * | 2019-08-12 | 2021-07-09 | 四川大学 | Modified biochar low-temperature denitration catalyst and application thereof |
CN111013255A (en) * | 2019-12-31 | 2020-04-17 | 江南大学 | Preparation method of micro/nano fiber aerogel composite filter material |
CN112704960A (en) * | 2020-12-07 | 2021-04-27 | 盐城工学院 | Preparation method of composite filter material |
CN113333027A (en) * | 2021-04-28 | 2021-09-03 | 福州大学 | Cobalt molybdic acid-loaded aramid fiber denitration sulfur-resistant filter material and preparation method thereof |
CN115679108A (en) * | 2022-11-24 | 2023-02-03 | 福州大学 | Method for separating and recovering nickel, cobalt, manganese and lithium from waste ternary lithium batteries |
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