CN108754179A - A kind of method of oxidation pre-treatment secondary material containing zinc - Google Patents
A kind of method of oxidation pre-treatment secondary material containing zinc Download PDFInfo
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- CN108754179A CN108754179A CN201810604950.3A CN201810604950A CN108754179A CN 108754179 A CN108754179 A CN 108754179A CN 201810604950 A CN201810604950 A CN 201810604950A CN 108754179 A CN108754179 A CN 108754179A
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- material containing
- secondary material
- containing zinc
- zinc
- persulfate
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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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
-
- 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/24—Obtaining zinc otherwise than by distilling with leaching with alkaline solutions, e.g. ammonia
-
- 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/26—Refining solutions containing zinc values, e.g. obtained by leaching zinc ores
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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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Abstract
The invention discloses a kind of methods of oxidation pre-treatment secondary material containing zinc, include the following steps：Before carrying out ammonia leaching to the secondary material containing zinc, oxidation pre-treatment reaction is carried out at least two oxidants are added in secondary material containing zinc, to get pretreated secondary material containing zinc, at least two oxidant includes hydrogen peroxide and persulfate for filtering after the completion of reaction.This method impurity element removal effect is good, do not introduce other impurities ion, zinc loses less, enormously simplifies subsequent purification processing step, solves the problems, such as that the method removal effect of impurity element in existing wet method removing secondary material containing zinc is bad, is readily incorporated foreign ion, also needs to carry out complicated subsequent purification technique.
Description
Technical field
The present invention relates to technical field of wet metallurgy, and in particular to a kind of to contain zinc with the pretreatment of a variety of oxidant co-oxidations
The method of secondary material.
Background technology
Zinc is current one of higher metal of cyclic utilization rate in the world, and secondary zinc resource has become zinc raw materials for production
Important component is counted according to zinc trading company of the U.S. and is shown, the zinc in the whole world 30% is from regeneration zinc resource.Using secondary
Zinc resource ammonia process, which prepares activated zinc oxide, becomes people's increasingly focus of attention, has economic value and social benefit.Secondary oxidation
Zinc is a kind of common secondary zinc resource, contains the impurity elements such as manganese, iron, cadmium, lead in secondary zinc oxide powder, in leaching process
In, some can enter solution to these impurity elements, influence the leaching of zinc, increase subsequent purification burden；In addition, content of iron and manganese
It is the important Con trolling index of subsequent product activated zinc oxide, so needing to remove these impurity.
Currently, it is usually that oxygen is added while zincilate end ammonia soaks that wet method, which removes the impurity element in secondary zinc resource,
Manganese, ferro element in leachate is oxidized to the manganese of high-valence state, iron Precipitation, reached by agent potassium permanganate or bleaching powder etc.
The purpose of removal of impurities.But this method can be caused damages when manganese, iron are precipitated due to the absorption of zinc, and there is medications
Amount is difficult to grasp, and solution ph is not easy to control, and removal effect is undesirable and introduces foreign ion to system when removing ferrimanganic
The shortcomings that, it is likely to result in industrial so-called " returning manganese " phenomenon；In addition, this method oxidation is not thorough, subsequently also need to purify
Technique.And removal of impurities is usually the two sections of displacements of zincification powder after ammonia leaching, then add ammonium persulfate removing impurities by oxidation, this method purification technique
Long, purification burden weight, the addition of ammonium persulfate can also increase the ammonia in solution, increase follow-up recovery ammonia burden.
Chinese publication CN102633295A discloses a kind of Pretreatment Methods of soot containing zinc, and soot containing zinc exists
Calcium hypochlorite or sodium hypochlorite are added before ammonia leaching or hydrogen peroxide carries out oxidation pre-treatment, effectively reduces in zinc ammonia leaching solution
Manganese, iron content, but the pH of its preprocessing process be 9-11, for the zinc-containing dust containing zinc oxide, zinc oxide can dissolve
Into in solution, the loss of zinc is caused, in addition bleaching powder is met high temperature and acutely decomposed, and can set off an explosion, and has corrosivity.
There is research that ammonium persulfate is added in the solution that zincilate end ammonia soaks, the divalent Fe and Mn in solution is distinguished
It is oxidized to ferric ion and tetravalence manganese ion, generates hydroxide hydrate colloid, but colloid is difficult to thoroughly precipitate, removing
Effect is undesirable, subsequently also needs to that activated zinc oxide and activated carbon is added.
Invention content
The main purpose of the present invention is to provide a kind of dual oxidants co-oxidation pre-process the secondary material containing zinc method,
Method removal effect to solve impurity element in existing wet method removing secondary material containing zinc is bad, be readily incorporated impurity from
Son also needs the problems such as subsequent purification technique of progress complexity.
To achieve the goals above, the present invention provides a kind of methods of oxidation pre-treatment secondary material containing zinc, including with
Lower step：To before containing the progress ammonia leaching of zinc secondary material, being joined at least two oxidants are added in secondary material containing zinc
Oxidation pre-treatment reaction is closed, filtering is to get pretreated secondary material containing zinc, at least two oxidant after the completion of reaction
Including hydrogen peroxide and persulfate.
Further, the molar ratio of hydrogen peroxide and persulfate is 3:1-3:9, more preferably 3:6-3:9, most preferably
3:7。
Further, the total concentration of hydrogen peroxide and persulfate in reaction solution and divalent in secondary material containing zinc
Manganese, divalent ferro element total concentration ratio be 5-12, more preferably 9-12, most preferably 11.
Further, the temperature of reaction is 30-80 DEG C, more preferably 60 DEG C -80 DEG C, most preferably 60 DEG C.
Further, the time of reaction is 60-180min, more preferably 120-180min, most preferably 120min.
Further, oxidation pre-treatment reaction carries out in neutral conditions.
Further, secondary material containing zinc is soot containing zinc or secondary zinc oxide powder.
Further, persulfate is potassium peroxydisulfate.
Apply the technical scheme of the present invention, to contain zinc secondary material (such as secondary zinc oxide) carry out ammonia leaching before, first to containing
At least two oxidants (including hydrogen peroxide and persulfate) are added in zinc secondary material and carry out oxidation pre-treatment reaction,
Obtain pretreated secondary material containing zinc.Hydrogen peroxide and potassium peroxydisulfate all have a very strong oxidisability, and hydrogen peroxide can be with
Hydroxyl radical free radical (.OH) is generated, persulfate can generate potentiometric titrations (SO4 -.), hydrogen peroxide is combined with persulfate
It uses, oxidant can be in wider pH range internal oxiditions secondary material containing zinc；Also, hydrogen peroxide is reacted with ferrous ion
Heat release can provide advantage for the activation of persulfate, and persulfate can slow down the decomposition of hydrogen peroxide again.The present invention is logical
The oxidisability for crossing the mutual promoting action enhancing system between two kinds of oxidants, passes through the association between hydrogen peroxide and persulfate
Same-action,.OH and SO4 -.Mutually excitation, forms the stronger system of oxidisability, substantially increases the removing effect to impurity element
Fruit.This method will not introduce other impurities ion, significantly by carrying out oxidation pre-treatment before ammonia soaks in zinc ammonia leaching solution
Shorten subsequent purification processing step.Iron, manganese in one side secondary zinc oxide have been oxidized to high-valence state, avoid in the dipped journey of ammonia
In dissolving, eliminate follow-up iron, manganese removal of impurities process；On the other hand, in preprocessing process, cadmium, lead can be immersed secondary zinc oxide
Go out a part, especially cadmium largely to be leached, greatly reduces follow-up removal of impurities burden, the purity of obtained purified solution
Also higher.
Specific implementation mode
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.Below in conjunction with embodiment, the present invention will be described in detail.
As recorded in background technology, in existing wet method removing secondary material containing zinc there is removing in the method for impurity element
Effect is undesirable, be readily incorporated other impurities, also needs the problems such as subsequent purification technique, and to solve the above-mentioned problems, the application carries
A kind of method of oxidation pre-treatment secondary material containing zinc is supplied.
In a kind of typical embodiment of the application, a kind of side of oxidation pre-treatment secondary material containing zinc is provided
Method includes the following steps：To before containing the progress ammonia leaching of zinc secondary material, being aoxidized at least two are added in secondary material containing zinc
Agent carries out oxidation pre-treatment reaction, and filtering is to get pretreated secondary material containing zinc after the completion of reaction.Wherein, this at least two
Kind oxidant includes hydrogen peroxide and persulfate.
The removing of iron and manganese of secondary material containing zinc in the prior art, the conventional process for reducing cadmium lead content are that ammonia soaks simultaneous oxidation
Zincification powder adds oxidant and removes manganese element except cadmium, iron, lead and other elements after removing of iron and manganese or ammonia leaching.This technique is leached in zinc ammonia
It is easily introduced other impurities ion in liquid, causes product impurity content exceeding index；In addition, the hydroxide precipitation due to ferrimanganic is easily formed
Colloid causes sedimentation filtration difficult, also adds subsequent purification burden, and the removal effect of impurity element is unsatisfactory.
The present invention passes through to before containing the progress ammonia leaching of zinc secondary material, being first added at least two into secondary material containing zinc
Oxidant (including hydrogen peroxide and persulfate) carries out oxidation pre-treatment reaction, obtains the pretreated secondary object containing zinc
Material.All there is very strong oxidisability, hydrogen peroxide can generate hydroxyl radical free radical (.OH), mistake for hydrogen peroxide and persulfate
Sulfate can generate potentiometric titrations (SO4 -.), hydrogen peroxide and persulfate are used in combination, oxidant can be wider
PH range internal oxiditions secondary material containing zinc；Also, hydrogen peroxide and the work that ferrous ion exothermic heat of reaction can be persulfate
Change and advantage is provided, persulfate can slow down the decomposition of hydrogen peroxide again.
The present invention enhances the oxidisability of system by mutual promoting action between two kinds of oxidants, by hydrogen peroxide with
Synergistic effect between persulfate,.OH and SO4 -.Mutually excitation, forms the stronger system of oxidisability, substantially increases pair
The removal effect of impurity element.This method will not be introduced by carrying out oxidation pre-treatment before ammonia soaks in zinc ammonia leaching solution
Other impurities ion substantially reduces subsequent purification processing step.
The present invention pre-processes secondary material containing zinc using hydrogen peroxide and persulfate oxidation, can will contain in zinc secondary material
Bivalent manganese, ferro element be oxidized into value Mn and iron, form hydroxide or hydrate enter in solution, after filtering with
The pretreated separation of secondary material containing zinc, avoids the impurity elements such as manganese, iron from entering zinc ammonia leaching solution.Two kinds oxidizing two
Valence iron, the reaction equation of manganese element are as follows：
2MnO+(S2O8)2-+4H2O=2MnO2+8H++2(SO4)2- (1)
Fe3O4+H2O2+2H+=2Fe3++2H2O (2)
Fe3O4+(S2O8)2-=2Fe3++2(SO4)2- (3)
By verification experimental verification, in the oxidizer system used in the present invention, by the molar ratio of hydrogen peroxide and persulfate
Control is being 3:1-3:9, further preferably 3:6-3:9, most preferably 3:When 7, hydrogen peroxide and mistake can be preferably played
Synergistic effect between two kinds of oxidants of sulfate, it is more preferable to the removal effect of impurity element in secondary material containing zinc.
In order to reach ideal removal effect, and saving raw material as far as possible reduces cost, in the present invention, by hydrogen peroxide
With the ratio control of bivalent manganese, divalent ferro element total concentration in total concentration of the persulfate in reaction solution and secondary material containing zinc
System is in 5-12, and further control is in 9-12, most preferably 11.It is found by repetition test, the dosage of oxidant is controlled upper
Ideal removal effect can not only be reached by stating range, but also can save oxidant, avoid the waste for causing oxidant.
In the present invention, the temperature of oxidation pre-treatment reaction is controlled at 30-80 DEG C, it is more preferably 60 DEG C -80 DEG C, optimal
It is selected as 60 DEG C.At this temperature, it can both reach good removal effect, suitable removal efficiency, and can be to avoid due to temperature
Spending height causes hydrogen peroxide decomposition too fast, and can also reduce energy consumption.
Inventor has found through repetition test, in the use of above-mentioned oxidant composition and ratio, oxidant and the secondary material containing zinc
Under the conditions of amount ratio and reaction temperature, by the time control of reaction in 60-180min, more preferably 120-180min, most preferably
For 120min when, you can to obtain good removal effect, the reaction time continues to extend, removal effect improve unobvious, instead
Treatment effeciency can be reduced.
In the present invention, the close neutrality of the pH for the oxidation system being made of hydrogen peroxide and persulfate, oxidation pre-treatment
Reaction can carry out under conditions of close to neutral.And the pH of existing its preprocessing process of processing method is generally 9-11,
Under alkaline condition, zinc oxide when oxidation pre-treatment in secondary material containing zinc can be dissolved into solution, cause the loss of zinc.This
The processing method of invention is pre-processed under near-neutral sulfite deinking, greatly reduces zinc loss.
Secondary material containing zinc handled by the method for the present invention can be various industrial secondary zinc resources, such as soot containing zinc
With secondary zinc oxide powder etc..Persulfate used in the method for the present invention can be sodium peroxydisulfate, potassium peroxydisulfate etc..
To sum up, the present invention can not introduce other impurities ion, under the premise of avoiding zinc oxide solution loss, have
Effect handles secondary zinc oxide raw material, manganese, iron in reduction zinc ammonia leaching solution, cadmium, lead element content, and reduces the consumption of leaching agent,
Subsequent purification burden is reduced, subsequent purification technique is simplified, is that manganese, iron, cadmium, the lead in the active oxidation zinc product subsequently prepared are miscellaneous
Matter content meets industrial product quality and requires to be ready.
Below in conjunction with specific embodiment, the invention will be further described, but should not be construed as protecting the present invention
The limitation of range.
Secondary zinc oxide dust used in following embodiment contains zinc 50.83%, and Mn 0.15%, Fe 2.84%, Cd are
0.22%, Pb 6.47%, main component are zinc oxide, and zinc oxide is a kind of amphoteric oxide, are insoluble in water or ethyl alcohol, solvable
In acid and highly basic.The present invention is suitable for this raw material, but is not limited only to this raw material.
Embodiment 1：
It takes 25g secondary zinc oxides to carry out oxidation pre-treatment, selects dual oxidants hydrogen peroxide and potassium peroxydisulfate molar concentration rate
Respectively 0,3:6,3:7,3:8.Ferrous iron in oxidant concentration and secondary zinc oxide, manganese element concentration proportion be 11.Reaction temperature
Degree is 60 DEG C, pretreatment time 120min, and reaction system nature pH is 6-7, filter cake is filtered to obtain after pretreatment, filter cake is 90
It is 5 hours dry at DEG C, obtain four groups of pretreated samples.
It takes the pretreated sample of each group ammonia at 30 DEG C to soak 1 hour, filters to obtain zinc ammonia leaching solution, detect each group leachate
The content of middle iron, manganese, cadmium, lead metal impurity element.The results are shown in Table 1：
Each group of data in contrast table 1 is it is found that when the concentration ratio of hydrogen peroxide and potassium peroxydisulfate is 3:When 7, in leachate
Iron, manganese element 0, i.e., iron, manganese element have been not present in leachate, and cadmium, lead element concentration are also relatively small.
Metallic impurity elements content in 1 leachate of table
Embodiment 2：
25g secondary zinc oxides are taken to carry out oxidation pre-treatment, it is 3 to select the molar concentration rate of hydrogen peroxide and potassium peroxydisulfate:7,
Take ferrous iron in oxidant concentration and secondary zinc oxide, the concentration proportion of manganese element is respectively 9,10,10.5,11,12, other steps
It is constant, the content of iron, manganese, cadmium, lead metal impurity element in each group leachate is detected, the results are shown in Table 2：
Metallic impurity elements content in 2 leachate of table
From Table 2, it can be seen that when the concentration proportion increase of ferrous iron, manganese element in the concentration of oxidant and secondary zinc oxide
When to 11, without the presence of iron, manganese element in leachate, cadmium, the concentration of lead element are also relatively small.
Embodiment 3：
25g secondary zinc oxides are taken to carry out oxidation pre-treatment, it is 3 to select the molar concentration rate of hydrogen peroxide and potassium peroxydisulfate:7,
Ferrous iron in oxidant concentration and secondary zinc oxide, manganese element concentration proportion be 11, pretreatment temperature selects 50 DEG C respectively, 60
DEG C, 70 DEG C, other steps are constant, detect the content of iron, manganese, cadmium, lead metal impurity element in each group leachate, as a result such as table 3
It is shown：
As shown in Table 3, when pretreatment temperature increases to 60 DEG C, iron, manganese element content in leachate are 0, are leached molten
Without the presence of iron, manganese element in liquid.
Metallic impurity elements content in 3 leachate of table
Embodiment 4：
25g secondary zinc oxides are taken to carry out oxidation pre-treatment, it is 3 to select the molar concentration rate of hydrogen peroxide and potassium peroxydisulfate:7,
Ferrous iron in oxidant concentration and secondary zinc oxide, manganese element concentration proportion be 11,60 DEG C of pretreatment temperature, pretreatment time point
0,1.5h, 2h, 2.5h are not selected, other steps are constant, detect iron, manganese, cadmium, lead metal impurity element in each group leachate and contain
Amount, the results are shown in Table 4：
Metallic impurity elements content in 4 leachate of table
As shown in Table 4, when pretreatment time increases to 2h, the manganese, iron content in zinc ammonia leaching solution are reduced to 0, have expired
Sufficient industrial requirements, cadmium, lead element content in infusion solution significantly reduce.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, any made by repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of method of oxidation pre-treatment secondary material containing zinc, includes the following steps：It is carried out to the secondary material containing zinc
Before ammonia leaching, oxidation pre-treatment reaction is carried out at least two oxidants are added in secondary material containing zinc, is filtered after the completion of reaction,
Up to pretreated secondary material containing zinc, at least two oxidant includes hydrogen peroxide and persulfate.
2. according to the method described in claim 1, it is characterized in that, the molar ratio of the hydrogen peroxide and persulfate is 3:1-
3:9。
3. according to the method described in claim 2, it is characterized in that, the molar ratio of the hydrogen peroxide and persulfate is 3:7.
4. according to the method described in claim 1, it is characterized in that, the hydrogen peroxide and persulfate are in reaction solution
Bivalent manganese in total concentration and secondary material containing zinc, divalent ferro element total concentration ratio be 5-12.
5. according to the method described in claim 4, it is characterized in that, the hydrogen peroxide and persulfate are in reaction solution
Bivalent manganese in total concentration and secondary material containing zinc, divalent ferro element total concentration ratio be 11.
6. according to the method described in claim 1, it is characterized in that, the temperature of the reaction be 30-80 DEG C, preferably 60 DEG C-
80 DEG C, most preferably 60 DEG C.
7. according to the method described in claim 1, it is characterized in that, the time of the reaction is 60-180min, preferably 120-
180min, most preferably 120min.
8. according to the method described in claim 1, it is characterized in that, oxidation pre-treatment reaction carries out in neutral conditions.
9. according to the method described in claim 1, it is characterized in that, the secondary material containing zinc is soot containing zinc or secondary zinc oxide
Powder.
10. according to the method described in claim 1, it is characterized in that, the persulfate is potassium peroxydisulfate.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114150156A (en) * | 2021-11-30 | 2022-03-08 | 西安建筑科技大学 | Process for extracting zinc from low-grade zinc-containing dust and preparing nano zinc oxide |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114150156A (en) * | 2021-11-30 | 2022-03-08 | 西安建筑科技大学 | Process for extracting zinc from low-grade zinc-containing dust and preparing nano zinc oxide |
| CN114150156B (en) * | 2021-11-30 | 2023-10-13 | 西安建筑科技大学 | Low-grade zinc-containing dust zinc extraction and nano zinc oxide preparation process |
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| Publication number | Publication date |
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| CN108754179B (en) | 2019-12-20 |
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