CN108486376A - A method of leaching metal in waste lithium ion cell anode material - Google Patents
A method of leaching metal in waste lithium ion cell anode material Download PDFInfo
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- CN108486376A CN108486376A CN201810160141.8A CN201810160141A CN108486376A CN 108486376 A CN108486376 A CN 108486376A CN 201810160141 A CN201810160141 A CN 201810160141A CN 108486376 A CN108486376 A CN 108486376A
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- lithium ion
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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
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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
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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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
- C22B47/00—Obtaining manganese
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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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 present invention relates to a kind of methods of metal in leaching waste lithium ion cell anode material, including：Waste and old lithium ion battery is obtained into positive active material by pretreatment, the positive active material is reacted with the ammonium salt solution containing reducing agent then, is separated by solid-liquid separation after reaction, obtains leachate and filter residue.The method of the present invention, it is simple for process, metal leaching rate is high, and metal selective is high, by control reducing agent in leaching process type and dosage, it can be achieved that manganese metal Selectively leaching, such as when in the positive electrode comprising metals such as Li, Co, Mn, the reducing agent is ammonium sulfite, and when concentration is respectively 0.75mol/L and 1.5mol/L, the leaching rate of Mn is respectively 90% and 4%；Impurity content is low in leachate, and follow-up removal of impurities process cost is low, and leaching process carries out in autoclave, is discharged without toxic gas in operating process, good operational environment.
Description
Technical field
The present invention relates to the comprehensive reutilization fields of waste and old lithium ion battery, waste and old more particularly, to a kind of leaching
The method of metal in anode material for lithium-ion batteries.
Background technology
Lithium ion battery due to it is big with energy density, have extended cycle life, self-discharge rate is low, low stain, memory-less effect
Etc. excellent specific properties, since the advent of the world be widely used in fields such as mobile electronic device, power vehicle, energy storage.According to statistics
Chinese lithium ion battery yield in 2015 reaches 5,600,000,000, however the general 3-6 of lithium battery service life, because end-of-life or its
His a variety of causes and the waste and old lithium ion battery that generates is increasing.Positive material used in current commercialized lithium ion battery
Material is the binary or ternary material that cobalt acid lithium, LiFePO4, LiMn2O4 and nickel cobalt manganese form.Because in waste and old lithium ion battery
It is mishandling to not only result in environmental pollution containing a large amount of Co, Ni, Mn, the non-renewable metal of Li et al., while also resulting in a large amount of
The wasting of resources.Therefore not only meet the requirement of environmental protection to the recycling disposal of lithium ion battery, and can recycling nickel cobalt
The valuable metals resource such as manganese obtains good economic benefit and alleviates exploitation production pressure of the industrial production to primary ore, realizes
The win-win of environmental protection and economic development.
Currently, it is various to the recycling disposal technology type of lithium ion battery both at home and abroad, it is broadly divided into pyrogenic process, wet method, reparation
Regenerate three categories.Thermal process is that simple pretreated battery is put into metallurgical furnace high temperature melting, recycles valuable metal
Method.The villages Ru Jin sage's will discharges to lithium ion old and useless battery, remove shell after, battery core is mixed with coke, lime stone, is thrown
Enter and carry out reduction roasting in roaster, organic compound combustion generates carbon dioxide and other gases, cobalt acid lithium are reduced to metallic cobalt
And lithia, fluorine and P elements are fixed by sediment, aluminium is oxidized to Al2O3Clinker.Wet processing is obtained just after pre-processing
Pole active material carries out wet-leaching, then the technologies such as chemical precipitation, solvent extraction, ion exchange, electrochemistry is used to detach back
The method for receiving valuable metal in leachate.The recycling key of wherein valuable metal is to leach positive active material, leaching
Go out method and is divided into acidleach, alkali leaching and Bioleaching.The reparation of positive electrode is broadly divided into solid-phase synthesis with regeneration
(CN102751549A), four kinds of hydro-thermal method (CN102517448A), coprecipitation and sol-gal process.
For the above prior art, thermal process equipment requirement is high, and alloy purity is low, and subsequent wet metallurgical process still needs to one
Serial purification and impurity removal step.Acidleach is low to metal selective in wet processing, causes impurity content in leachate high, follow-up to clean
Tedious process, and the sour gas and waste water that generate are difficult；Microculture used by Bioleaching is complicated, and at leaching
It is longer to manage the period；Alkali leaching especially ammonia leaching is to metal selective height, but the valuable metals leaching rate such as Co, Ni is low, and leaching process is deposited
It is volatile in ammonium hydroxide, the problems such as operating environment is poor.Positive electrode reparation generally requires that the purity of raw material is higher, impurity with regeneration
It is few, it is applied to the recovery processing of substandard product or corner tailing on production line for manufacturing battery, the technique is for type on the market more
The waste and old lithium ion battery mixed, repairing effect need further to be verified.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of side leaching metal in waste lithium ion cell anode material
Method, this method mix waste and old lithium ion battery by the positive active material that pretreatment obtains with the ammonium salt solution containing reducing agent
It closes, the valuable metal under high-temperature and high-pressure conditions in Selectively leaching positive active material.
To achieve the above object, the present invention uses technical solution below：
A method of metal in waste lithium ion cell anode material is leached, including：Waste and old lithium ion battery is passed through
Pretreatment obtains positive active material, then reacts the positive active material with the ammonium salt solution containing reducing agent,
It is separated by solid-liquid separation after reaction, obtains leachate and filter residue.
In above-mentioned technical proposal, the positive active material is reacted with the ammonium salt solution containing reducing agent,
The metal in waste lithium ion cell anode material, especially Ni, Co, Li et al. metal can be effectively leached, and adjusts reducing agent
Type and dosage can control the leaching rate of metal Mn, to realize Selectively leaching.
Preferably, the liquid-solid ratio of the reaction is 4:1-15:1.Under this liquid-solid ratio, pulp density is moderate, both can guarantee
Effective leaching of valuable metal in positive electrode, and industrial production can be met.
Preferably, the ammonium salt solution is one or more of ammonium carbonate, ammonium chloride, ammonium sulfate, a concentration of 1-6mol/
L, preferably 1-3mol/L.Ammonium carbonate, ammonium chloride and ammonium sulfate are the common ammonium in industrial production and laboratory research ammonium soaking technology
Salt can realize the efficient leaching of valuable metal in positive electrode in the concentration range of 1-6mol/L.
Preferably, the reducing agent is hydrazine hydrate, ammonium sulfite, sodium sulfite, one or more of glucose, described
A concentration of 0.5-2mol/L of the reducing agent in the ammonium salt solution.
The above preferred substance has stronger reproducibility, is often used as reducing agent.Preferred concentration is 0.5-2mol/L.When dense
Degree is less than 0.5mol/L, and reducing agent dosage is too low, cannot valuable metal effectively in induced positive electrode material；When concentration is higher than 2mol/
L, reducing agent dosage is excessively high, and a large amount of reagent is caused to consume.
Preferably, the reaction pressure of the reaction is 0.1-3.0MPa.
The reaction temperature of the reaction is 100-220 DEG C.If being less than 100 DEG C, the leaching of valuable metal in positive electrode
Extracting rate is relatively low；If being higher than 220 DEG C, to the improvement effect unobvious of the leaching rate of valuable metal, and since temperature is excessively high, to anti-
It answers equipment requirement high, increases production cost.
The reaction time of the reaction is 1-4h.
The mixing speed of the reaction is 300-600r/min.
Preferably, the pretreatment include waste and old lithium ion battery electric discharge, dismantling are obtained into positive electrode, then by it is described just
Pole material is thermally treated and crushing and screening obtains the positive active material.
In above-mentioned technical proposal, first waste and old lithium ion battery is discharged, then dismantling obtains positive electrode and shell, cathode
Material, diaphragm, terminal, it is to remove binder etc. that the positive electrode, which is carried out heat treatment, and crushing and screening is in order to by aluminium
Foil and the positive active material separate.
Preferably, the method further includes being washed to the filter residue, and washing reagent is ammonium salt solution, and dosage is to leach
The 10%-15% of liquid product.
Preferably, the method for leaching metal in waste lithium ion cell anode material, includes the following steps：
1) waste and old lithium ion battery is soaked in 24-48h in sodium chloride solution, discharged, hand is carried out after electric discharge
Work is disassembled to obtain the positive electrode；
2) by the positive electrode in 200-350 DEG C of roasting temperature 0.5-2.5h；
3) Mechanical Crushing is carried out to the product that step 2) obtains and sieved, obtain positive active material crude product and aluminium foil；
4) it is living to be obtained into the anode in 500-680 DEG C of temperature lower calcination 0.5-2.5h for the positive active material crude product
Property substance；
5) positive active material is mixed with the ammonium salt solution containing reducing agent, is added in autoclave and carries out instead
It answers；
6) product that step 5) obtains is separated by solid-liquid separation, obtains leachate and filter residue.
Preferably, a concentration of 5-15g/L of sodium chloride solution described in step 1).
Preferably, ammonium salt solution described in step 5) is the ammonium sulfate of a concentration of 3mol/L, and the reducing agent is Asia
Ammonium sulfate.
Preferably, it when in the waste lithium ion cell anode material containing Ni, Co, Mn, Li et al. metal, leaches wherein golden
The method of category, includes the following steps：
1) waste and old lithium ion battery is soaked in 24-48h in sodium chloride solution, discharged, hand is carried out after electric discharge
Work is disassembled to obtain the positive electrode；
2) by the positive electrode in 200-350 DEG C of roasting temperature 0.5-2.5h；
3) Mechanical Crushing is carried out to the product that step 2) obtains and sieved, obtain positive active material crude product and aluminium foil；
4) it is living to be obtained into the anode in 500-680 DEG C of temperature lower calcination 0.5-2.5h for the positive active material crude product
Property substance；
5) positive active material is mixed with the ammonium sulfate containing ammonium sulfite, wherein liquid-solid ratio is 4:1-8:
1, a concentration of 3mol/L of ammonium sulfate, a concentration of 0.5-2mol/L of ammonium sulfite are added in autoclave and carry out instead
It answers；
6) product that step 5) obtains is separated by solid-liquid separation, obtains leachate and filter residue.
The present invention has the advantage that compared with the existing technology：
The method for leaching metal in waste lithium ion cell anode material of the present invention, simple for process, metal leaching rate is high,
And metal selective is high, by control reducing agent in leaching process type and dosage, it can be achieved that manganese metal Selectively leaching,
Such as when in the positive electrode comprising metals such as Li, Co, Mn, the reducing agent is ammonium sulfite, concentration is respectively
When 0.75mol/L and 1.5mol/L, the leaching rate of Mn is respectively 90% and 4%；Impurity content is low in leachate, subsequently removes general labourer
Sequence is at low cost, and leaching process carries out in autoclave, is discharged without toxic gas in operating process, good operational environment.
Description of the drawings
Fig. 1 is the process flow chart of the embodiment of the present invention 1；
Fig. 2 is the XRD analysis figure of positive active material described in the embodiment of the present invention 1；
Fig. 3 is each metal leaching rate in the embodiment of the present invention 1 with the trend chart of reducing agent dosage.
Specific implementation mode
With reference to the accompanying drawings and examples, the specific implementation mode of the present invention is described in further detail.Implement below
Example is merely to illustrate the present invention, is not intended to limit protection scope of the present invention.
Embodiment 1
Present embodiments provide a kind of method leaching metal in waste lithium ion cell anode material, process flow chart
As shown in Figure 1, including the following steps：
1) waste and old lithium ion battery is soaked in 36h in the sodium chloride solution of a concentration of 15g/L to discharge, electric discharge terminates
Dismantling by hand is carried out afterwards obtains positive electrode and shell, negative material, diaphragm, terminal；
2) positive electrode that step 1) obtains is put into 350 DEG C of roasting 2h in Muffle furnace；
3) product that step 2) obtains is crushed using high speed Universal pulverizer, is then obtained just with the sieve screening of 80 mesh
Pole active material crude product and aluminium foil；
4) the positive active material crude product that step 3) obtains is put into 650 DEG C of high-temperature calcination 2h in Muffle furnace, obtains anode
Active material detects its element composition (the results are shown in Table 1) and carries out XRD tests (XRD analysis figure is as shown in Figure 2)；
5) it weighs the positive active material that 67g steps 4) obtain to be added in autoclave, adds the 800mL ammonium sulfate of preparation
With the mixed solution of ammonium sulfite, wherein ammonium sulfate concentrations are 3mol/L, a concentration of 0.75mol/L of ammonium sulfite, setting stirring
Speed is 400r/min, reacts 3h at 200 DEG C；
6) product that step 5) obtains is separated by solid-liquid separation, obtains leachate and filter residue, with a concentration of 3mol/L of 100mL
Ammonium sulfate washing filter residue 3 times, merge cleaning solution and leachate.
The element of 1 positive active material of table forms
As can be seen from Table 1, the positive active material includes content higher Co, Mn, Li, Ni and Cu, Fe etc. one
Secondary element slightly.As shown in Figure 2, main object is mutually LiCoO in the positive active material2、Co3O4And LiMn2O4。
Constituent content in the final gained leachate of detection, calculates the leaching rate of each metal in positive electrode, result is
The leaching rate of Ni, Co, Mn and Li respectively reach 97.67%, 76.88%, 91.91% and 98.01%.
Embodiment 2
Present embodiments provide a kind of method leaching metal in waste lithium ion cell anode material, including following step
Suddenly：
1) waste and old lithium ion battery is soaked in 36h in the sodium chloride solution of a concentration of 15g/L, discharged, electric discharge knot
Dismantling by hand is carried out after beam obtains positive electrode；
2) positive electrode that step 1) obtains is put into 350 DEG C of roasting 2h in Muffle furnace；
3) product that step 2) obtains is crushed using high speed Universal pulverizer, is then obtained just with the sieve screening of 80 mesh
Pole active material crude product and aluminium foil；
4) the positive active material crude product that step 3) obtains is put into 650 DEG C of high-temperature calcination 2h in Muffle furnace, obtains anode
Active material；
5) it weighs the positive active material that 80g steps 4) obtain to be added in autoclave, adds the 800mL ammonium sulfate of preparation
With the mixed solution of ammonium sulfite, wherein ammonium sulfate concentrations are 3mol/L, a concentration of 1.5mol/L of ammonium sulfite, setting stirring speed
Degree is 400r/min, reacts 3h at 200 DEG C；
6) product that step 5) obtains is separated by solid-liquid separation, obtains leachate and filter residue, with a concentration of 3mol/L of 100mL
Ammonium sulfate washing filter residue 4 times, merge cleaning solution and leachate.
Constituent content in the final gained leachate of detection, calculates the leaching rate of each metal in positive electrode, result is
The leaching rate of Ni, Co, Mn and Li respectively reach 96.44%, 88.81%, 4.05% and 97.44%.
Based on embodiment 2, the concentration of ammonium sulfite is adjusted, calculates separately the leaching rate of each metal in positive electrode,
It is as shown in Figure 3 with the variation tendency of reductant concentration that drafting pattern obtains each metal leaching rate.
From the figure 3, it may be seen that the leaching rate of metal Li changes little with reducing agent dosage；The leaching rate of W metal and Co are with also
The increase of former agent dosage and increase, when reductant concentration is higher than after 1mol/L, the leaching rate of Ni and Co tend towards stability, respectively
96% and 88%；The leaching rate of metal Mn with reducing agent dosage increase first increases and then decreases, when reductant concentration is
When 0.75mol/L, leaching rate highest is 92%, and when reductant concentration is 1.5mol/L, leaching rate is minimum, is 4%.Due to
Each metal is different with reductant concentration variation tendency, to realize W metal, Co and the Selectively leaching of Li.
Embodiment 3
It is the ammonium sulfate of a concentration of 5mol/L of 600mL in the present embodiment, remaining is same as Example 1.It detects and counts
Calculate the leaching rate of each metal in final gained leachate, the leaching rate of result Ni, Co, Mn and Li is respectively 86.64%,
65.31%, 85.02% and 91.01%.
Embodiment 4
Ammonium sulfate is substituted for the ammonium chloride solution of a concentration of 3mol/L, remaining and 1 phase of embodiment in the present embodiment
Together.The leaching rate of each metal in final gained leachate is detected and calculates, the leaching rate of result Ni, Co, Mn and Li are respectively
95.90%, 73.89%, 91.33% and 95.61%.
Embodiment 5
Reducing agent is hydrazine hydrate in the present embodiment, remaining is same as Example 1.It detects and calculates in final gained leachate
The leaching rate of the leaching rate of each metal, result Ni, Co, Mn and Li is respectively 95.23%, 75.38%, 88.61% and
92.90%.
Embodiment 6
Reaction temperature is 80 DEG C in the present embodiment, and reaction time 5h, remaining is same as Example 1.It detects and calculates most
Eventually in gained leachate each metal leaching rate, the leaching rate of result Ni, Co, Mn and Li is respectively 72.68%, 45%,
20.40% and 78.45%.
Comparative example 1
This comparative example provides a kind of method leaching metal in waste lithium ion cell anode material with ammonium hydroxide, including following
Step：
1) waste and old lithium ion battery is soaked in 36h in the sodium chloride solution of a concentration of 15g/L, discharged, electric discharge knot
Dismantling by hand is carried out after beam obtains positive electrode；
2) positive electrode that step 1) obtains is put into 350 DEG C of roasting 2h in Muffle furnace；
3) product that step 2) obtains is crushed using high speed Universal pulverizer, is then obtained just with the sieve screening of 80 mesh
Pole active material crude product and aluminium foil；
4) the positive active material crude product that step 3) obtains is put into 650 DEG C of high-temperature calcination 2h in Muffle furnace, obtains anode
Active material detects its element composition；
5) positive active material that 40g steps 4) obtain is weighed, the mixed of 800mL ammonium hydroxide, ammonium sulfate and sodium sulfite is prepared
Solution is closed, wherein ammonia concn is 3mol/L, and ammonium sulfate 1.5mol/L and concentration of sodium sulfite are 0.75mol/L, and reaction is added
It is uniformly mixed in device, sets mixing speed as 400r/min, react 3h at 80 DEG C；
6) product that step 5) obtains is separated by solid-liquid separation, obtains leachate and filter residue.
Constituent content in the final gained leachate of detection, calculates the leaching rate of each metal in positive electrode, result is
The leaching rate of Ni, Co, Mn and Li respectively reach 55%, 38%, 4%, 60%.
By contrast it is found that the method in the embodiment of the present invention makes waste lithium cell compared to traditional ammonium hydroxide leaching method
The leaching rate higher of valuable metal in positive electrode, and operating environment is more preferable.
Finally, the preferred embodiment that these are only the present invention, is not intended to limit the scope of the present invention.It is all this
Within the spirit and principle of invention, any modification, equivalent replacement, improvement and so on should be included in the protection model of the present invention
Within enclosing.
Claims (10)
1. a kind of method leaching metal in waste lithium ion cell anode material, which is characterized in that including：By applying waste lithium ionic
Battery obtains positive active material by pretreatment, then by the positive active material and the ammonium salt solution containing reducing agent into
Row reaction, is separated by solid-liquid separation after reaction, obtains leachate and filter residue.
2. a kind of method leaching metal in waste lithium ion cell anode material according to claim 1, feature exist
In the liquid-solid ratio of the reaction is 4:1-15:1.
3. a kind of method leaching metal in waste lithium ion cell anode material according to claim 1, feature exist
In the ammonium salt solution is one or more, a concentration of 1-6mol/L in ammonium carbonate, ammonium chloride, ammonium sulfate.
4. a kind of method leaching metal in waste lithium ion cell anode material according to claim 1, feature exist
In the reducing agent is one or more in hydrazine hydrate, ammonium sulfite, sodium sulfite, glucose, and the reducing agent is described
A concentration of 0.5-2mol/L in ammonium salt solution.
5. a kind of method leaching metal in waste lithium ion cell anode material according to claim 1, feature exist
In the reaction pressure of the reaction is 0.1-3.0MPa, and reaction temperature is 100-220 DEG C, reaction time 1-4h, mixing speed
For 300-600r/min.
6. a kind of method leaching metal in waste lithium ion cell anode material according to claim 1, feature exist
Include in, the pretreatment waste and old lithium ion battery electric discharge, dismantling are obtained into positive electrode, then by the positive electrode through heat at
Reason and crushing and screening obtain the positive active material.
7. a kind of method leaching metal in waste lithium ion cell anode material according to claim 1, feature exist
In further including being washed to the filter residue, washing reagent is ammonium salt solution, and dosage is the 10%-15% of leachate volume.
8. a kind of method leaching metal in waste lithium ion cell anode material according to claim 1, feature exist
In including the following steps：
1) waste and old lithium ion battery is soaked in 24-48h in sodium chloride solution, discharged, carry out tearing open by hand after electric discharge
Solution obtains the positive electrode；
2) by the positive electrode in 200-350 DEG C of roasting temperature 0.5-2.5h；
3) Mechanical Crushing is carried out to the product that step 2) obtains and sieved, obtain positive active material crude product and aluminium foil；
4) the positive active material crude product is obtained into the positive electrode active material in 500-680 DEG C of temperature lower calcination 0.5-2.5h
Matter；
5) positive active material is mixed with the ammonium salt solution containing reducing agent, is added in autoclave and is reacted；
6) product that step 5) obtains is separated by solid-liquid separation, obtains leachate and filter residue.
9. a kind of method leaching metal in waste lithium ion cell anode material according to claim 8, feature exist
In a concentration of 5-15g/L of sodium chloride solution described in step 1).
10. a kind of method leaching metal in waste lithium ion cell anode material according to claim 8, feature exist
In ammonium salt solution described in step 5) is the ammonium sulfate of a concentration of 3mol/L, and the reducing agent is ammonium sulfite.
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