CN102828032B - Method for producing lithopone by utilizing electrolytic zinc acid leaching slag - Google Patents
Method for producing lithopone by utilizing electrolytic zinc acid leaching slag Download PDFInfo
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- CN102828032B CN102828032B CN201210358075.8A CN201210358075A CN102828032B CN 102828032 B CN102828032 B CN 102828032B CN 201210358075 A CN201210358075 A CN 201210358075A CN 102828032 B CN102828032 B CN 102828032B
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- zinc
- ammonia
- acid leaching
- leaching slag
- sulfide white
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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
Abstract
The invention discloses a method for producing lithopone by utilizing electrolytic zinc acid leaching slag, comprising the following concrete steps of: leaching, carrying out replacement reaction, washing and smashing. By virtue of the steps, zinc is selectively leached by adopting an ammonia-ammonium sulphate method, the replacement reaction is carried out to obtain an nZnS-BaSO4 crystalline solid filter cake, and drying and smashing are carried out to obtain the lithopone product, thus the zinc in the acid leaching slag is effectively recycled and utilized. According to the invention, an ammonia leaching method is taken as an effective treatment technical means on the acid leaching slag, the obtained lithopone product has good quality, sulphate radical required by production is provided by the acid leaching slag, recycling utilization of the acid leaching slag is realized, waste material is changed into things of value, production cost is low, and operation is simple.
Description
Technical field
The present invention relates to the production technique of mineral dye zinc sulfide white, be specifically related to a kind of method utilizing electrolytic zinc acid leaching slag to produce zinc sulfide white.
Background technology
Mineral dye zinc sulfide white also claims lithopone, it is the mixed crystal of zinc sulphide and barium sulfate, there is many uniquenesses and excellent performance, zinc sulfide white product formation series product, as high ZnS type, apparent processing-type, aqueous dispersion type, sun-proof type, color-type etc., play an important role in industrial and agricultural production and daily life.Be mainly used in coating, paint, thermoplastics, thermosetting resin, paper etc., by surface treatment or TiO
2coatedly can replace part rutile.
Current zinc sulfide white is mainly at domestic product, and the production overwhelming majority of domestic zinc sulfide white still uses Traditional Method, and main raw material is secondary zinc oxide, sulfuric acid and barium sulphide (barite and coal obtain through high temperature reduction), uses raw material generally containing zinc 45% ~ 70%.It is be raw material sulfuric acid leaching containing zinc more than 45% zinc baking sand that Traditional Method produces zinc sulfide white flow process, obtain the thick liquid of zinc sulfate, then potassium permanganate oxidation deironing etc. is used, zinc dust precipitation heavy metal again, filtration obtains zinc sulfate refined liquid, replacement(metathesis)reaction is carried out again with barium sulphide, press filtration, calcining, rinsing, dry, pulverize and obtain the dissimilar zinc sulfide white series product of Containing Sulfur zinc more than 30%, whole process is carried out in acid (PH < 7) environment, consume a large amount of sulfuric acid, sulfuric acid has strong corrodibility, require high to production unit, the slag of finally discharging is acid slag, new pollution is brought to environment, and it is high to ingredient requirement, production cost is high, the poor product quality obtained.
In addition, along with the demand of zn cpds and zinc sulfide white product is increasing, the continuous exploitation of China's zinc resource, Mineral resources are increasingly poor, thin, assorted, and comprehensive utilization and environmental requirement improve constantly, and people have begun one's study the recovery and utilization technology of low zinc raw material.So-called low zinc raw material is mainly low-grade zinc oxide ore, but except containing except zinc in low-grade zinc oxide ore, also containing zinc in acid leaching residue.
Current domestic zinc hydrometallurgy mainly adopts the production technique of roasting-leaching-electrodeposition, zinc massfraction general 8 ~ 15% in the acid leaching residue of discharge, have up to 20%, in acid leaching residue, zinc is mainly with ZnFe
2o
4form exists, and in order to reclaim these zinc, treatment process has pyrogenic process and wet method two kinds at present, and pyrogenic process is rotary kiln evaporation method (waelz process) and fuming furnace volatilization method.Wet method has hot acid to leach or high-temperature pressurizing leaches.Pyrogenic attack technical process is long, and maintenance of equipment amount is large, and invest high, Working environment is poor, and need to consume a large amount of fire coals or metallurgical coking coal, benefit is low, and environmental pollution is large.Therefore usual hot acid leaches or high pressure leaching, still there is shortcoming in these methods: 1. consumes a large amount of acid, leaching yield is low, due to containing a large amount of calcium sulfate, the ultrafine particulates such as calcium sulfate are to Zinc oxide particles skinning buffer action, cause electrolytic zinc enterprise acid environment leach difficulty, secondary pickling due to the rate of recovery too low, practical significance is little.If 2. leached, although ZnFe with strong acid
2o
4destroyed, leaching rate increases, but the pressure of iron leaching yield also high (reaching 60%) deironing is large, and need consume more reagent, 3. high-temperature high-pressure apparatus seriously corroded, the investment of equipment complexity is larger; 4. running cost is high, deficiency in economic performance.5. last slag of discharging is acid leaching residue, brings new pollution, have to take solidify & bury, not only contaminate environment to environment, and waste resource.
Therefore the optimal treatment process of acid leaching residue is the Selectively leaching carrying out zinc, makes zinc enter in infusion solution, and zinc recovering utilizes and obtains valuable zn cpds or zinc sulfide white product.
In sum, for the process of electrolytic zinc acid leaching slag, how to overcome traditional pyrogenic process and the shortcoming of wet method, in the material of low zinc content, effectively leach zinc wherein, and obtain zinc sulfide white, become industry technical barrier urgently to be resolved hurrily and unsolved.
Summary of the invention
The object of the invention is to the defect overcoming the existence of above-mentioned prior art, design a kind of method utilizing electrolytic zinc acid leaching slag to produce zinc sulfide white, zinc in acid leaching residue is recycled, under ammonia environment, utilizes the operation of simple possible to produce and obtain zinc sulfide white product.
For achieving the above object, technical scheme of the present invention comprises the steps:
1) leach: the ammonia-ammonia sulfate solution that electrolytic zinc acid leaching slag ammonia concn is 5.5 ~ 7.0mol/L, ammonium sulfate volumetric molar concentration is 0 ~ 1.2mol/L leaches, at temperature is 20 ~ 50 DEG C, leach 3h ~ 9h, the whole immersion liquid of gained is that 60-90g/L is for subsequent processing containing zinc mass concentration;
Leaching reaction equation is:
ZnO +n NH
3·H
2O→［Zn NH
3)n］
2++2OH
-
Zn(OH)
2+ n NH
3→［Zn NH
3)n］
2++2OH
-
Zn +n NH
3+ 2H
2O→［Zn NH
3n］
2++H
2+2OH
-
ZnSO
4 + n NH
3→［Zn(NH
3)n］
2++SO
4 2-
ZnFe
2O
4 +n NH
3+4H
2O→［Zn(NH
3)n］
2++2Fe(OH)
3↓+2OH
-
Zn
2SiO
3 +2n NH
3→ 2［Zn(NH
3)n］
2++ SiO
3 2-
CaSO
4+ 2 NH
3·H
2O → （NH
4）
2SO
4+ Ca(OH)
2↓
Wherein n=1 ~ 4
2) replacement(metathesis)reaction: sulphide dissolves is obtained in distilled water replacement(metathesis)reaction clear liquid, then there is replacement(metathesis)reaction slow being added in whole immersion liquid, obtain zinc sulfide white emulsion, filtering separation, ammoniacal liquor after separation returns leaching, the nZnS-BaSO of separation after adjusting ammonia
4xln filter cake enters subsequent processing;
Reaction equation is:
［Zn(NH
3)n］SO
4+BaS→ZnS ↓+ BaSO
4 ↓+ nNH
3
［Zn(NH
3)n］(OH )
2+ H
2S → ZnS ↓+ 2H
2O + nNH
3
3) washing is pulverized: with distilled water or washing with alcohol nZnS-BaSO
4xln filter cake, the nZnS-BaSO of filtering separation after washing
4xln filter cake carries out drying and crushing, obtains zinc sulfide white product.
In electrolytic zinc acid leaching slag in described leaching step, zinc massfraction is 5% ~ 35%.
Preferred version has: in leaching step, add the Sodium dodecylbenzene sulfonate of 0.05kg ~ 0.1kg in the ammoniacal liquor-ammoniumsulphate soln of every cubic metre, Sodium dodecylbenzene sulfonate reduces solution surface energy.
In leaching step, in the ammoniacal liquor-ammoniumsulphate soln of every cubic metre, add 0.3 ~ 0.5kg Sodium Silicofluoride.Add appropriate silicofluoric acid and receive class ultrafine particulates such as abolishing the calcium hydroxide that generates in calcium sulfate and ammonia react process with tensio-active agent coordination energy to the parcel containing zinc particle, realizing ultrafine particulate delamination floats, thus zinc is exposed, realizes leaching molten.
In leaching step, in the ammoniacal liquor-ammoniumsulphate soln of every cubic metre, add the Dicyanodiamide of 0.5 ~ 1kg, by adding Dicyanodiamide, reducing the volatilization of ammonia in technological process, improving Working environment, reduce the loss waste of ammonia.
Sulfide in described replacement(metathesis)reaction step is barium sulphide, sodium sulphite, ammonium sulfide or hydrogen sulfide.
Preferred technical scheme has, in the zinc sulfide white emulsion of replacement(metathesis)reaction step, add H
2o
2,institute adds H
2o
2massfraction be 10 ~ 33%, make zinc sulfide white emulsion desulfurization (being mainly sulfur hydrogen anion ion or elemental sulfur), slowly add H
2o
2until zinc sulfide white emulsion is water white transparency shape.The sulfate ion obtained can be recycled, again for this production technique.
Chemical equation is: 4H
2o
2+ HS
-+ OH
-→ SO
4 2-+ 5H
2o
3H
2O
2+ S+ 2OH
-→ SO
4 2-+ 4H
2O
Replacement(metathesis)reaction temperature 20 ~ 50 DEG C in described replacement(metathesis)reaction step, stirring velocity is 10 ~ 15m/s, chemical combination time 0.5 ~ 1h.
Advantage of the present invention and beneficial effect are:
First, the technique means that ammonia leaching process effectively processes as acid leaching residue, zinc sulfide white is produced under weakly alkaline (PH=8.5 ~ 10) ammonia environment, the Solubilities of Hydroxides of some metallic impurity such as Ca, Mg, Fe, Al is low, the impurity entered in ammonia-ammonia sulfate Selectively leaching in whole immersion liquid reduces, thus ensures the quality of product; Classical acid legal system for zinc sulfide white because more or less simple substance sulphur and sulphite can be produced in the roasting and reduction process of zinc baking sand, Sodium Sulphide, produce the zinc sulfide white whiteness difference color obtained partially yellow, and this patent replacement(metathesis)reaction is carried out in ammonia solution (alkalescence), by adding H
2o
2oxidation, the product finally obtained is sulfate radical, and desulfurization is quick, thorough, just need not can ensure the whiteness of product through high-temperature calcination; Lower than sulfuric acid leaching to equipment requirements; Solve the problem of environmental pollution that acid leaching residue exists, particularly efficiently solve the environmental pollution of the heavy metals such as zinc in acid leaching residue, copper, lead, cadmium, arsenic and acid ion to the impact of heap dis environment.Realize the recycling of high value metals zinc in acid leaching residue, the acidity realizing soil improves and has the comprehensive advantage of low cost, energy-saving and environmental protection.
The second, the invention provides a large industrialized production technique that production cost is low, efficient, energy-conservation, constant product quality yearly capacity reaches few hundred thousand tonnes of.By ammonia process Selectively leaching zinc, replacement(metathesis)reaction obtains nZnS-BaSO
4xln filter cake, convection drying, pulverizing without high-temperature calcination, obtain zinc sulfide white product.Products obtained therefrom quality is good, and industry is workable.
3rd, in product, the moiety of zinc sulphide and barium sulfate is controlled, can carry out the kind regulating product according to market.
4th, the sulfate radical producing needs used due to the present invention is provided by acid leaching residue itself, and acid leaching residue inside is containing SO
4 2-massfraction be more than 15%, effectively can control the leaching yield (can 70% be reached through the leaching yield of multistage leaching sulfate radical under this ammonia environment) of acid group, acid leaching residue is utilized to make the zinc of zinc sulfide white and zinc sulfide white product prepared by sulfate radical raw material, both recycling was achieved to acid leaching residue, make a silk purse out of a sow's ear, again acid leaching residue acid soil is administered and improved, purified environment.Production cost is low, simple to operate.Replacement(metathesis)reaction is carried out in low-density ammonia gonosome system (metathesis reactant reclaims ammonia solvent), and the nucleus of formation is less, and non-toxic and safe.The ammoniacal liquor that replacement(metathesis)reaction filtering separation obtains returns leaching after adjusting ammonia up to standard, and whole production process is without waste water, and the waste residue of production reaches the general solid waste discharge standard of country and carries out outer row, and meeting national industrial policies, is environmental protection " green " type technique.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is further described.Following examples only for technical scheme of the present invention is clearly described, and can not limit the scope of the invention with this.
Embodiment 1
1. the leaching of electrolytic zinc acid leaching slag: produce 1500ml ammoniacal liquor-ammoniumsulphate soln as ammonia leaching solution, wherein ammonia concn is 5.5mol/L, ammonium sulfate volumetric molar concentration is 0.5mol/L, adds the Dicyanodiamide of the Sodium dodecylbenzene sulfonate of 0.05kg, 0.5kg Sodium Silicofluoride, 0.5kg by every cubic metre of ammonia leaching solution.Get 500 grams of acid leaching residue (its moietys, calculate in mass ratio, containing zinc 11.86%, copper 0.97%, calcium sulfate 28%, cadmium 0.007%, arsenic 0.02%, plumbous 3.74%), join in above-mentioned ammonia-ammonia sulfate immersion liquid and carry out three sections of leachings, each section of leaching time is 3 hours, after solid-liquid separation, obtain the whole immersion liquid (taking away in all the other liquid slags) of 1450ml, zinc leaching rate 90.1%, the whole immersion liquid of gained is containing zinc 80.3g/L; Containing SO
4 2-81.2 g/L.
2. the preparation of zinc sulfide white: get 143.3g barium sulphide (not moisture) and 29.8g sodium sulphite (not moisture) mixing is dissolved in distilled water and obtains replacement(metathesis)reaction liquid, temperature of reaction 25 DEG C, stirring velocity is 13m/s, abundant stirring 30min mixes, then slowly join in the whole immersion liquid of 1000ml, adding massfraction after continuing to stir 30min is 10%H
2o
2desulfurization bleaching, bleaching after filtering separation obtain nZnS-BaSO
4xln filter cake.
Use washing with alcohol nZnS-BaSO
4xln filter cake, filter after washing, filter cake is pulverized after loft drier 105 DEG C of dry 1h, zinc, barium productive rate is detected by atomic absorption, reach 97.6% in zinc, reach 99% in barium, detect by National Standard Method: quality product mark reaches 99.4% with zinc sulphide and barium sulfate summation, ZnS massfraction accounts for 37.7%, and the indices such as tinting strength, oil-absorption(number) of zinc sulfide white exceedes GB GB/T1707-1995 B311 type product.
Embodiment 2
1. the leaching of electrolytic zinc acid leaching slag: produce 1500ml ammoniacal liquor-ammoniumsulphate soln as ammonia leaching solution, wherein ammonia concn is 7.0mol/L, ammonium sulfate volumetric molar concentration is 0.3mol/L, adds the Dicyanodiamide of the Sodium dodecylbenzene sulfonate of 0.1kg, 0.3kg Sodium Silicofluoride, 1kg by every cubic metre of ammonia leaching solution.Get 500 grams of acid leaching residue (its moietys, calculate in mass ratio, containing zinc 8%, copper 1.14%, calcium sulfate 29%, cadmium 0.0086%, arsenic 0.03%, plumbous 1.65%), join in above-mentioned ammonia-ammonia sulfate immersion liquid and carry out three sections of leachings, each section of leaching time is 2 hours, after solid-liquid separation, obtain the whole immersion liquid (taking away in all the other liquid slags) of 1450ml, zinc leaching rate 90.9%; Whole immersion liquid is containing zinc 59.1g/L; Containing SO
4 2-64.2g/L.
2. the preparation of zinc sulfide white: get 113.3g barium sulphide (not moisture) and 18.4g sodium sulphite (not moisture) mixing is dissolved in distilled water and obtains replacement(metathesis)reaction liquid, temperature of reaction 10 DEG C, stirring velocity is 10m/s, abundant stirring 60min mixes, then slowly join in the whole immersion liquid of 1000ml, adding massfraction after continuing to stir 30min is 20%H
2o
2desulfurization bleaching, bleaching after filtering separation obtain nZnS-BaSO
4xln filter cake.
Use washing with alcohol nZnS-BaSO
4xln filter cake, filter after washing, filter cake is pulverized after loft drier 105 DEG C of dry 1h, zinc, barium productive rate is detected by atomic absorption, reach 98.2% in zinc, reach 99.2% in barium, detect by National Standard Method: quality product mark reaches 99.5% with zinc sulphide and barium sulfate summation, ZnS massfraction accounts for 36.4%, and the indices such as tinting strength, oil-absorption(number) of zinc sulfide white exceedes GB GB/T1707-1995 B311 type product.
Embodiment 3
1. the leaching of electrolytic zinc acid leaching slag: produce 1500ml ammoniacal liquor-ammoniumsulphate soln as ammonia leaching solution, wherein ammonia concn is 6.0mol/L, ammonium sulfate volumetric molar concentration is 0.9mol/L, adds the Dicyanodiamide of the Sodium dodecylbenzene sulfonate of 0.075kg, 0.45kg Sodium Silicofluoride, 0.75kg by every cubic metre of ammonia leaching solution.Get 500 grams of acid leaching residue (its moietys, calculate in mass ratio, containing zinc 6.1%, copper 1.37%, calcium sulfate 24%, cadmium 0.0043%, arsenic 0.025%, plumbous 2.84%), join in above-mentioned ammonia-ammonia sulfate immersion liquid and carry out three sections of leachings, each section of leaching time is 2 hours, after solid-liquid separation, obtain the whole immersion liquid (taking away in all the other liquid slags) of 1450ml, zinc leaching rate 90.2%; Whole liquid is containing zinc 66.3g/L; Containing SO
4 2-71.9g/L;
2. the preparation of zinc sulfide white: 126.9g barium sulphide (not moisture) and 20.7g sodium sulphite (not moisture) mixing are dissolved in distilled water and obtain replacement(metathesis)reaction liquid, temperature of reaction 40 DEG C, stirring velocity is 15m/s, abundant stirring 40min mixes, then slowly join in the whole immersion liquid of 1000ml, adding massfraction after continuing to stir 30min is 30%H
2o
2desulfurization bleaching, bleaching after filtering separation obtain nZnS-BaSO
4xln filter cake.
Use washing with alcohol nZnS-BaSO
4xln filter cake, filter after washing, filter cake is pulverized after loft drier 105 DEG C of dry 1h, zinc, barium productive rate is detected by atomic absorption, reach 98.4% in zinc, reach 99% in barium, detect by National Standard Method: quality product mark reaches 99.22% with zinc sulphide and barium sulfate summation, ZnS massfraction accounts for 36.1%, and the indices such as tinting strength, oil-absorption(number) of zinc sulfide white exceedes GB GB/T1707-1995 B311 type product.
Claims (4)
1. utilize electrolytic zinc acid leaching slag to produce a method for zinc sulfide white, it is characterized in that, concrete steps are as follows:
1) leach: the ammonia-ammonia sulfate solution that electrolytic zinc acid leaching slag ammonia concn is 5.5 ~ 7.0mol/L, ammonium sulfate volumetric molar concentration is 0 ~ 1.2mol/L leaches, at temperature is 20 ~ 50 DEG C, leach 3h ~ 9h, the whole immersion liquid of gained is that 60-90g/L is for subsequent processing containing zinc mass concentration;
2), then there is replacement(metathesis)reaction slow being added in whole immersion liquid, obtain zinc sulfide white emulsion, add H in replacement(metathesis)reaction: be dissolved in by barium sulphide in distilled water and obtain replacement(metathesis)reaction clear liquid
2o
2oxidation sweetening, filtering separation, the nZnS-BaSO of separation
4xln filter cake enters subsequent processing;
3) washing is pulverized: with distilled water or washing with alcohol nZnS-BaSO
4xln filter cake, the nZnS-BaSO of filtering separation after washing
4xln filter cake carries out drying and crushing, obtains zinc sulfide white product.
2. utilize electrolytic zinc acid leaching slag to produce the method for zinc sulfide white as claimed in claim 1, it is characterized in that, in leaching step, in the ammonia-ammonia sulfate solution of every cubic metre, add the Sodium dodecylbenzene sulfonate of 0.05kg ~ 0.1kg.
3. utilize electrolytic zinc acid leaching slag to produce the method for zinc sulfide white as claimed in claim 1, it is characterized in that, in leaching step, in the ammonia-ammonia sulfate solution of every cubic metre, add 0.3 ~ 0.5kg Sodium Silicofluoride.
4. utilize electrolytic zinc acid leaching slag to produce the method for zinc sulfide white as claimed in claim 1, it is characterized in that, in leaching step, in the ammonia-ammonia sulfate solution of every cubic metre, add the Dicyanodiamide of 0.5 ~ 1kg.
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|---|---|---|---|---|
| EP0109468A1 (en) * | 1982-11-18 | 1984-05-30 | Extramet | Process for the selective recovery of lead from lead sulphides |
| CN1065685A (en) * | 1992-04-28 | 1992-10-28 | 中南工业大学 | Zinc oxide preparing process by ammonia method |
| CN101538648A (en) * | 2009-03-13 | 2009-09-23 | 昆明理工大学 | Method for activating ammonia leaching for high calcium-magnesium zinc oxide ore |
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| CN101838750A (en) * | 2010-05-17 | 2010-09-22 | 赣州华兴钨制品有限公司 | Method for performing direct acid adjusting closed cycle on ammonium paratungstate crystallization mother liquor |
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2012
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0109468A1 (en) * | 1982-11-18 | 1984-05-30 | Extramet | Process for the selective recovery of lead from lead sulphides |
| CN1065685A (en) * | 1992-04-28 | 1992-10-28 | 中南工业大学 | Zinc oxide preparing process by ammonia method |
| CN101538648A (en) * | 2009-03-13 | 2009-09-23 | 昆明理工大学 | Method for activating ammonia leaching for high calcium-magnesium zinc oxide ore |
Non-Patent Citations (1)
| Title |
|---|
| 含锌废料制备立德粉;张桂文等;《云南化工》;20100430;第37卷(第2期);84-85 * |
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