CN108179275A - The recovery method of cadmium nickel in a kind of waste Ni Cd battery - Google Patents
The recovery method of cadmium nickel in a kind of waste Ni Cd battery Download PDFInfo
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- CN108179275A CN108179275A CN201711436821.XA CN201711436821A CN108179275A CN 108179275 A CN108179275 A CN 108179275A CN 201711436821 A CN201711436821 A CN 201711436821A CN 108179275 A CN108179275 A CN 108179275A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B17/00—Obtaining cadmium
- C22B17/04—Obtaining cadmium by wet processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0407—Leaching processes
- C22B23/0415—Leaching processes with acids or salt solutions except ammonium salts solutions
- C22B23/0423—Halogenated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B23/00—Obtaining nickel or cobalt
- C22B23/04—Obtaining nickel or cobalt by wet processes
- C22B23/0453—Treatment or purification of solutions, e.g. obtained by leaching
- C22B23/0461—Treatment or purification of solutions, e.g. obtained by leaching by chemical methods
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
-
- 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 present invention provides a kind of recovery method of cadmium nickel in waste Ni Cd battery, including：Waste Ni Cd battery material is immersed in HCl solution, obtained metal ion mixed liquor adjusts pH value to 4~7, and filtering obtains pretreatment fluid；Pretreatment fluid and citric acid are mixed, reaction obtains reaction solution, adjusts pH value to 8~11, filtering obtains cadmium hydroxide and filtrate；Filtrate and calcium nitrate are mixed, adjust pH value to 9~12, reaction obtains sediment；Sediment and HCl solution are reacted, filtering, obtained filtrate adjusts pH value to 7~12, obtains nickel hydroxide.The reclaimer that the recovery method uses is simple, easy to operate, separates and recovers ni-Cd using different pH value, method is simple, and the rate of recovery and purity are higher.The recovery method material therefor is conventional reagent, of low cost；There is no the toxic reagents such as sulfide in removal process, secondary pollution will not be generated.
Description
Technical field
The present invention relates to a kind of times of cadmium nickel in hydrometallurgy cadmium separation nickel technical field more particularly to waste Ni Cd battery
Receiving method.
Background technology
Due to cadmium nickel battery function admirable, widely used, but contain a large amount of toxic heavy metal cadmium in waste Ni Cd battery
And nickel, be directly entered after environment without processing endanger it is huge.The vegetables of long-term consumption cadmium lead contamination, rice, underground water can cause
Renal tubule injury, rickets and itai-itai etc., short-term Excess free enthalpy cadmium can make one to lead to toxicity pulmonary edema, expiratory dyspnea and urgency
Property kidney failure occur.Excess free enthalpy nickel can lead to the major diseases such as lung cancer, leukaemia, asthma, urinary calculus, nickel and chlorion,
Sulphion, carbonyl combine rear toxicity bigger, can cause central recycle and disordered breathing, make must flesh, brain and kidney occur oedema and
Denaturation.Therefore, waste Ni Cd battery is directly entered environment without processing can endanger biological health.Cadmium, nickel are also industrial normal simultaneously
With metal, there is extensive use in fields such as manufacture alloy, pigment, paint, fluorescent powder, stabilizer for plastics, stainless steel, plating
On the way, and higher price, it does not recycle and causes the wasting of resources.
The method of processing ickel-cadmium cell has hydrometallurgy, pyrometallurgy, biological metallurgy and machinery recycling etc. both at home and abroad at present.
The method that wherein hydrometallurgy uses has：(1) ammonium salt leaching method：First ickel-cadmium cell waste material is roasted, then is divided with ammonium nitrate solution
Grade leaching separation, recycling, the method is at low cost and non-secondary pollution, but its rate of recovery is only 20~30%.(2) vulcanization bed is electrolysed
Method：Using metal copper particle as cathode, make metal ion in cathodic reduction, but because granular cathode manufactures difficulty, can not yet put into industry
Change application.(3) organic reagent extraction：It by cadmium nickel battery waste material Acid leaching, is then extracted with organic reagent, then with water pair
Organic phase containing cadmium carries out back extraction；Nickel is recycled in the form of nickel hydroxide in organic sodium hydroxide that is added to of raffinate.The method
The rate of recovery is but expensive up to more than 99%, is not suitable for industrial applications.(4) sulfurization-precipitation method：By cadmium nickel battery waste material
It is dissolved with acid, being passed through hydrogen sulfide, just cadmium sulfide is precipitated, and concentrating filter liquor, cooling make nickel ion with NiSO4·6H2O crystal is precipitated,
The method separation rate is high and at low cost, but H2S breath malodors, pollution air.
The technologies such as pyrometallurgy, biological metallurgy and machinery recycling are complicated there are equipment, high expensive, and the metal after recycling is pure
Spend the problem of low.Often flow is complicated for existing hydrometallurgic recovery old and useless battery, and reagent expends high.
Invention content
In view of this, the purpose of the present invention is to provide a kind of recovery method of cadmium nickel in waste Ni Cd battery, this method
Simply, and the rate of recovery and purity are higher.
The present invention provides a kind of recovery methods of cadmium nickel in waste Ni Cd battery, include the following steps：
A) waste Ni Cd battery material is immersed in HCl solution, obtained metal ion mixed liquor adjusting pH value to 4~
7, filtering obtains pretreatment fluid；
B) pretreatment fluid and citric acid are mixed, reaction obtains reaction solution, adjusts pH value to 8~11, filtering obtains
To cadmium hydroxide and filtrate；
C) filtrate and calcium nitrate are mixed, adjusts pH value to 9~12, reaction obtains sediment；
D) sediment and HCl solution are reacted, filtering, obtained filtrate adjusts pH value to 7~12, obtains hydroxide
Nickel.
Preferably, the granularity of the waste Ni Cd battery material is 0.5~2mm.
Preferably, the temperature that waste Ni Cd battery material is immersed in HCl solution in the step a) is 40~100 DEG C；
Time is 50~120min.
Preferably, the amount of the total material of cadmium ion and nickel ion and the substance of citric acid in pretreatment fluid in the step b)
Amount ratio be 1:0.8~1.3.
Preferably, the amount ratio of the substance of calcium ion is 1 in the citric acid and calcium nitrate:1~1:10.
Preferably, pH value is adjusted in the step a), step b), step c) and step d) and uses NaOH.
Preferably, in the step a) HCl solution a concentration of 3.0mol/L~6.0mol/L.
Preferably, the pH value of HCl solution is 5~7 in the step d).
Preferably, in the step a) waste Ni Cd battery material by J-AAA280A types waste Ni Cd battery and/or
Type-A-AAA types are discarded ickel-cadmium cell and are made.
The present invention provides a kind of recovery methods of cadmium nickel in waste Ni Cd battery, include the following steps：A) by waste and old cadmium
Nickel-based battery material is immersed in HCl solution, and obtained metal ion mixed liquor adjusts pH value to 4~7, and filtering is pre-processed
Liquid；B) pretreatment fluid and citric acid are mixed, reaction obtains reaction solution, adjusts pH value to 8~11, filtering obtains hydrogen-oxygen
Cadmium and filtrate；C) filtrate and calcium nitrate are mixed, adjusts pH value to 9~12, reaction obtains sediment；D) by the precipitation
Object and HCl solution reaction, filtering, obtained filtrate adjust pH value to 7~12, obtain nickel hydroxide.What the recovery method used
Reclaimer is simple, easy to operate, separates and recovers ni-Cd using different pH value, method is simple, and the rate of recovery and purity are higher.
In addition, the recovery method material therefor is conventional reagent, it is of low cost；There is no the toxic reagents such as sulfide in removal process,
Secondary pollution will not be generated.The experimental results showed that：Nickel purity 95.71~98.26%, nickel recovery 89.14~92.44%；Cadmium
Purity is 98.65~99.07%, and the cadmium rate of recovery is 98.21~98.77%.
Specific embodiment
The present invention provides a kind of recovery methods of cadmium nickel in waste Ni Cd battery, include the following steps：
A) waste Ni Cd battery material is immersed in HCl solution, obtained metal ion mixed liquor adjusting pH value to 4~
7, filtering obtains pretreatment fluid；
B) pretreatment fluid and citric acid are mixed, reaction obtains reaction solution, adjusts pH value to 8~11, filtering obtains
To cadmium hydroxide and filtrate；
C) filtrate and calcium nitrate are mixed, adjusts pH value to 9~12, reaction obtains sediment；
D) sediment and HCl solution are reacted, filtering, obtained filtrate adjusts pH value to 7~12, obtains hydroxide
Nickel.
The reclaimer that the recovery method uses is simple, easy to operate, and ni-Cd, method letter are separated and recovered using different pH value
It is single, and the rate of recovery and purity are higher.In addition, the recovery method material therefor is conventional reagent, it is of low cost；Removal process
In there is no the toxic reagents such as sulfide, secondary pollution will not be generated.
Waste Ni Cd battery material is immersed in HCl solution by the present invention, and obtained metal ion mixed liquor adjusts pH value
To 4~7, filtering obtains pretreatment fluid.The present invention preferably disassembles waste Ni Cd battery, sorting positive and negative electrode material, just
The recyclable waste material rich in ni-Cd metal such as pole leftover pieces is immersed in as waste Ni Cd battery material in HCl solution.It is described useless
The granularity of old ickel-cadmium cell material is preferably 0.5~2mm.In the specific embodiment of the invention, the waste Ni Cd battery material
It is made it is preferred that discarding ickel-cadmium cell by J-AAA280A types waste Ni Cd battery and/or Type-A-AAA types.The HCl solution
Concentration is preferably 3.0mol/L~6.0mol/L.
In the present invention, the temperature that the waste Ni Cd battery material is immersed in HCl solution is preferably 40~100 DEG C；
Time is preferably 50~120min.The present invention carries out waste Ni Cd battery material dipping preferably under conditions of stirring；It is described to stir
The rate mixed is preferably 100r/min~300r/min.
Obtained metal ion mixed liquor is adjusted pH value to 4~7 by the present invention, it is therefore an objective to remove a small amount of iron content, containing indium
Wait impurity.
After obtaining pretreatment fluid, the present invention mixes the pretreatment fluid and citric acid, and reaction obtains reaction solution, adjusts
For pH value to 8~11, filtering obtains cadmium hydroxide and filtrate.The amount and lemon of the total material of cadmium ion and nickel ion in pretreatment fluid
The amount of the substance of lemon acid is than preferably 1:0.8~1.3, more preferably 1:0.9~1.1, most preferably 1:1.Pretreatment fluid and lemon
The mixed reaction solution of citric acid cadmium and citric acid nickel is obtained by the reaction in lemon acid.The present invention is preferably added to NaOH and adjusts pH value to 8~11.
Dry 1~3h, recycling are spare at preferably 40 DEG C~80 DEG C of the cadmium hydroxide being obtained by filtration.
After obtaining filtrate, the present invention mixes filtrate and calcium nitrate, adjusts pH value to 9~12, reaction obtains sediment.
The amount ratio of the substance of calcium ion is preferably 1 in the citric acid and calcium nitrate:1~1:10.Present invention preferably employs NaOH adjustings
PH value is to 9~12.Sediment obtained by the reaction includes nickel hydroxide and calcium citrate.
After obtaining sediment, the present invention reacts the sediment and HCl solution, and filtering, obtained filtrate adjusts pH value
To 7~12, nickel hydroxide is obtained.The present invention preferably reacts sediment and pH value for 5~7 HCl solution.In the present invention,
Sediment and HCl solution are preferably reacted under conditions of stirring；The rate of the stirring is preferably 100r/min~300r/
min.The time of the sediment and HCl solution reaction is preferably 20~60min.Filtering, obtains sediment calcium citrate and filter
Liquid；The calcium citrate reuse.The filtrate adjusts pH value to 7~12, it is preferred to use NaOH adjusts pH value to 7~12.This hair
Bright preferably to be filtered after filtrate adjusting pH value to 7~12, obtained moist precipitate object is dried, and obtains nickel hydroxide.Moist precipitate
The temperature that object is dried is 50 DEG C~90 DEG C；The dry time is 1~3h.
The present invention provides a kind of recovery methods of cadmium nickel in waste Ni Cd battery, include the following steps：A) by waste and old cadmium
Nickel-based battery material is immersed in HCl solution, and obtained metal ion mixed liquor adjusts pH value to 4~7, and filtering is pre-processed
Liquid；B) pretreatment fluid and citric acid are mixed, reaction obtains reaction solution, adjusts pH value to 8~11, filtering obtains hydrogen-oxygen
Cadmium and filtrate；C) filtrate and calcium nitrate are mixed, adjusts pH value to 9~12, reaction obtains sediment；D) by the precipitation
Object and HCl solution reaction, filtering, obtained filtrate adjust pH value to 7~12, obtain nickel hydroxide.What the recovery method used
Reclaimer is simple, easy to operate, separates and recovers ni-Cd using different pH value, method is simple, and the rate of recovery and purity are higher.
In addition, the recovery method material therefor is conventional reagent, it is of low cost；There is no the toxic reagents such as sulfide in removal process,
Secondary pollution will not be generated.The experimental results showed that：Nickel purity 95.71~98.26%, nickel recovery 89.14~92.44%；Cadmium
Purity is 98.65~99.07%, and the cadmium rate of recovery is 98.21~98.77%.
In order to further illustrate the present invention, with reference to embodiment to cadmium in a kind of waste Ni Cd battery provided by the invention
The recovery method of nickel is described in detail, but cannot they be interpreted as limiting the scope of the present invention.
Embodiment 1
The J-AAA280A type waste Ni Cd batteries provided using Fushan City, Guangdong Province battery Industrial Co., Ltd.
(1) it disassembles, sorting positive and negative electrode material, anode leftover pieces etc. are rich in the recyclable waste material of cadmium nickel metal, will recycle
Material fragmentation is into the particle of 1.5mm or so；
(2) particle after crushing is placed in in the solution of the HCl of 5.0mol/L the 150r/min rotating speeds item under the conditions of 80 DEG C
100min is stirred under part, obtains metal ion mixed liquor, wherein nickel content 7.24g/L, leaching rate 96.84%, cadmium content
12.73g/L leaching rate 99.37%.
(3) it adds in NaOH and adjusts pH value to 6, filtering removes the impurity such as a small amount of iron, indium, obtains filtrate；
(4) citric acid 45.47g/L is added into the filtrate that step (3) obtains, stirs, obtains citric acid cadmium and citric acid
Nickel mixed liquor；
(5) it adds in NaOH and adjusts pH value to 10, filtering obtains cadmium hydroxide and filtrate, by cadmium hydroxide in 60 DEG C of conditions
Lower dry 2h, obtains cadmium hydroxide 8.98g；Purity is 99.07%；The cadmium rate of recovery is 98.21%；
(6) calcium nitrate 60.73g/L is added into the filtrate that step (5) obtains, NaOH is added to adjust solution ph to 10.5,
The precipitation (nickel hydroxide+calcium citrate) of generation is collected by filtration；
(7) precipitation being collected into is added in dilute HCl solution that pH value is 6,150r/min rotating speeds are stirred to react
30min, filtering, obtains calcium citrate and filtrate；
(8) filtrate that step (7) obtains adjusts pH value to 9.5 with NaOH, and dry 2h, obtains hydrogen-oxygen under the conditions of 70 DEG C of filtering
Change nickel 5.67g；Purity is 98.26%, nickel recovery 89.14%.
Embodiment 2
The Type-A-AAA type waste Ni Cd batteries provided using Fushan City, Guangdong Province Battery Plant, are grasped according to the following steps
Make：
(1) it disassembles, sorting positive and negative electrode material, anode leftover pieces etc. are rich in the recyclable waste material of cadmium nickel metal, will recycle
Material fragmentation is into the particle of 1.0mm or so；
(2) particle after crushing is placed in in the solution of the HCl of 4.0mol/L the 100r/min rotating speeds item under the conditions of 60 DEG C
110min is stirred under part, obtains metal ion mixed liquor, wherein nickel content 7.87g/L, leaching rate 82.48%, cadmium content
13.35g/L leaching rate 99.24%.
(3) it adds in NaOH and adjusts pH value to 5, filtering removes the impurity such as a small amount of iron, indium, obtains filtrate；
(4) citric acid 48.59g/L is added into the filtrate that step (3) obtains, stirs, obtains citric acid cadmium and citric acid
Nickel mixed liquor；
(5) it adds in NaOH and adjusts pH value to 9.5, filtering obtains cadmium hydroxide and filtrate, by cadmium hydroxide in 50 DEG C of conditions
Lower dry 2.5h, obtains cadmium hydroxide 12.23g；Purity is 98.65%；The cadmium rate of recovery is 98.77%；
(6) calcium nitrate 82.98g/L is added into the filtrate that step (5) obtains, NaOH is added to adjust solution ph to 10, mistake
The precipitation (nickel hydroxide+calcium citrate) generated is collected in filter；
(7) precipitation being collected into is added in dilute HCl solution that pH value is 5,120r/min is stirred to react 50min, mistake
Filter, obtains calcium citrate and filtrate；
(8) filtrate that step (7) obtains adjusts pH value to 10 with NaOH, filter generation be deposited in 60 DEG C under the conditions of it is dry
1.5h obtains nickel hydroxide 8.55g；Purity is 95.71%, nickel recovery 92.44%.
As seen from the above embodiment, the present invention provides a kind of recovery method of cadmium nickel in waste Ni Cd battery, including with
Lower step：A) waste Ni Cd battery material is immersed in HCl solution, obtained metal ion mixed liquor adjusting pH value to 4~
7, filtering obtains pretreatment fluid；B) pretreatment fluid and citric acid are mixed, reaction obtains reaction solution, adjusts pH value to 8
~11, filtering obtains cadmium hydroxide and filtrate；C) filtrate and calcium nitrate are mixed, adjusts pH value to 9~12, reaction is sunk
Starch；D) sediment and HCl solution are reacted, filtering, obtained filtrate adjusts pH value to 7~12, obtains nickel hydroxide.
The reclaimer that the recovery method uses is simple, easy to operate, and ni-Cd is separated and recovered using different pH value, and method is simple, and returns
Yield and purity are higher.In addition, the recovery method material therefor is conventional reagent, it is of low cost；Do not have in removal process
The toxic reagents such as sulfide will not generate secondary pollution.The experimental results showed that：Nickel purity 95.71~98.26%, nickel recovery
89.14~92.44%；Cadmium purity is 98.65~99.07%, and the cadmium rate of recovery is 98.21~98.77%.
The above is only the preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. the recovery method of cadmium nickel, includes the following steps in a kind of waste Ni Cd battery：
A) waste Ni Cd battery material is immersed in HCl solution, obtained metal ion mixed liquor adjusting pH value to 4~7, mistake
Filter, obtains pretreatment fluid；
B) pretreatment fluid and citric acid are mixed, reaction obtains reaction solution, adjusts pH value to 8~11, filtering obtains hydrogen
Cadmium oxide and filtrate；
C) filtrate and calcium nitrate are mixed, adjusts pH value to 9~12, reaction obtains sediment；
D) sediment and HCl solution are reacted, filtering, obtained filtrate adjusts pH value to 7~12, obtains nickel hydroxide.
2. recovery method according to claim 1, which is characterized in that the granularity of the waste Ni Cd battery material is 0.5
~2mm.
3. recovery method according to claim 1, which is characterized in that waste Ni Cd battery material impregnates in the step a)
Temperature in HCl solution is 40~100 DEG C；Time is 50~120min.
4. recovery method according to claim 1, which is characterized in that cadmium ion and nickel in pretreatment fluid in the step b)
The amount of the total material of ion and the amount of the substance of citric acid ratio are 1:0.8~1.3.
5. recovery method according to claim 1, which is characterized in that the substance of calcium ion in the citric acid and calcium nitrate
Amount ratio be 1:1~1:10.
6. recovery method according to claim 1, which is characterized in that the step a), step b), step c) and step d)
Middle adjusting pH value uses NaOH.
7. recovery method according to claim 1, which is characterized in that HCl solution is a concentration of in the step a)
3.0mol/L~6.0mol/L.
8. recovery method according to claim 1, which is characterized in that the pH value of HCl solution is 5~7 in the step d).
9. recovery method according to claim 1, which is characterized in that waste Ni Cd battery material is by J- in the step a)
AAA280A types waste Ni Cd battery and/or Type-A-AAA types are discarded ickel-cadmium cell and are made.
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| CN201711436821.XA CN108179275B (en) | 2017-12-26 | 2017-12-26 | The recovery method of cadmium nickel in a kind of waste Ni Cd battery |
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| CN201711436821.XA CN108179275B (en) | 2017-12-26 | 2017-12-26 | The recovery method of cadmium nickel in a kind of waste Ni Cd battery |
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