CN1065685A - Zinc oxide preparing process by ammonia method - Google Patents
Zinc oxide preparing process by ammonia method Download PDFInfo
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- CN1065685A CN1065685A CN 92103230 CN92103230A CN1065685A CN 1065685 A CN1065685 A CN 1065685A CN 92103230 CN92103230 CN 92103230 CN 92103230 A CN92103230 A CN 92103230A CN 1065685 A CN1065685 A CN 1065685A
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- zinc
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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Abstract
The present invention relates to a kind of wet method and directly produce the metallurgy chemical process of high grade zinc oxide.Comprise that ammonia-ammonium complexing agent leaches material containing zinc, Zn thoroughly separated with Fe, Mn that leach liquor carries out once heavy zinc then with the one step removal of impurities of sulfuration method; Liquid carries out the heavy zinc of double salt method secondary again behind the once heavy zinc, and zinc hydroxide is sintered into high grade zinc oxide after cleaning; Liquid returns leaching process behind the heavy zinc of secondary after reformulating.Present method is applicable to the secondary zinc oxide that contains zinc 〉=15%, ironmaking, refining manganese zinc smoke, the roasting material of all kinds of zinc ores and zinc ore concentrate, hydrometallurgy filter residue, hot galvanizing residue, the processing of zinc oxide such as casting zinc dross or zinc hydroxide or metallic zinc material.
Description
Zinc oxide preparing process by ammonia method the present invention relates to the metallurgy chemical process that a kind of wet method is directly produced high grade zinc oxide.It closes steps such as leaching, purification, heavy zinc, the high-quality zinc oxide of output by ammino.
The traditional treatment method of zinc oxide material comprises pyrogenic process and wet method, and wherein wet method is divided into acid system and ammonia process.Contain that the higher zinc oxide material of zinc (for example zinc baking sand) is most of use acidic process, this method is reliable and stable, but it is big to have an energy consumption, purification and impurity removal process complexity, problems such as need equipment anticorrosion; In order to solve the shortcoming of aforesaid method, the trend that adopts ammonia process to handle the high low zinc material of iron content is arranged at present greatly.Reclaim zinc oxide as " from blast furnace gas mud, reclaiming zinc oxide " (" Jiangsu chemical industry ", 1990, № 3) with 25～28% ammonia treatment; " research of ammonium chloride leaching smithsonite " (" inorganic chemicals industry ", 1986, № 6, Fu Wanqun) reach " producing the zinc oxide new technology route " (" Liaoning chemical industry ", 1990, № 5) leach the smithsonite roasting material to produce active zinc flower and grade zinc oxide respectively with denseer ammonium chloride solution; Also there is human volatile salt dissolution method to produce high-purity zinc carbonate abroad, as " production of high-purity zinc carbonate " (" nonferrous smelting ", 1991, № 2).The common issue with that above method exists is that the leach liquor zinc concentration is low, and impurity stripping quantities such as lead, manganese are big, and the removal of impurities burden is heavy, therefore, if will produce the high-purity zinc oxide product, then to ingredient requirement height or removal of impurities process complexity.
The purpose of this invention is to provide a kind of multiple material containing zinc, particularly high ferro can handled and hang down the zinc material, and directly produce the method for high grade zinc oxide.
Solution of the present invention is with sulfur-bearing acid group (SO
2-
4) and a small amount of persulfate (S
2O
2-
8) the ammino mixture leach material containing zinc, after leaching, most lead and whole manganese and iron are stayed in the leached mud, zinc enters leach liquor, enters the metal that a spot of lead of also having of solution and cadmium, copper, nickel, cobalt, silver etc. can form ammonia complex with zinc; Leach liquor sulphur root (S
2-) solution removes impurity elements such as cadmium, copper, lead; Use double salt neutralisation (low ammono-system) then or steam ammonium method (high ammono-system) precipitation zinc hydroxide; Zinc hydroxide is sintered into high grade zinc oxide after cleaning; Add sulfuric acid in the liquid and reduce pH value behind the heavy zinc of secondary, sulfate precipitate zinc ammonium double salt, this double salt return once heavy zinc process and make neutralizing agent; Return leaching process after the heavy zinc liquid of secondary is reformulated and close leaching agent as ammino.
Details are as follows about process and condition:
One, complexing is leached
The principal reaction of complexing leaching process is:
I is a ligancy in the formula, value 1～4.
When zinc leaches, the plumbous difficulty soluble salt that forms, manganese is oxidized to high price manganese and enters and soak slag at a low price:
The complexing leaching agent is formed: contain ammonia 1.5～8.5N, ammonium salt 1.5～8.5N, ammonium persulphate are 0～10% of raw material weight, and leaching liquid-solid ratio is 2～10: 1, and temperature is 0～90 ℃, and the time is 0.5～4h; Leached mud after the filtration washs 3 times with the solution of ammonium salt-containing 3～6N (consumption be complexing dosage 5～40%), washes with water 3～5 times again.Ammonium leacheate and leach liquor merge, and draw in the back and carry out purifying treatment.
Two, scavenging process
Sulphur root (the S that in the leach liquor that contains impurity elements such as Cd, Cu, Pb, adds 2～4 times of theoretical amount
2-) as the scavenging agent removal of impurities:
Purification temperature is 0～60 ℃, and the time is 0.25～4h, and employed vulcanizing agent is NaHS or Na
2S or S
2-Purify slag and wash 3 times with 3～6N ammonium salt solution (consumption be complexing agent 1～5%) earlier, wash with water again 3～5 times; Ammonium salt washing lotion and scavenging solution merge and sink the zinc processing.
Three, once heavy zinc
For the lower scavenging solution of free ammonia, adopt the heavy zinc of neutralisation, (its molecular formula is: ZnSO promptly to use the zinc sulfate ammonium
4(NH
4)
2SO
46H
2O) in the double salt and scavenging solution:
Neutral temperature is 0～90 ℃, and the time is 0.25～6h, the zinc precipitation 1/3～1/2 of scavenging solution.
For the higher scavenging solution of free ammonia, adopt the heavy zinc of ammonia still process method:
The ammonia still process temperature is 80～98 ℃; Boil off 20～60% of scavenging solution.
The zinc hydroxide that two kinds of heavy zinc methods obtain is cleaned (drip washing 6～8 times) with pure water and is sent calcination process.
Four, the heavy zinc of secondary
The zinc liquid that once sinks still contains the zinc of total zinc amount 1/3～1/2, adopts the heavy zinc method of double salt that zinc is precipitated fully, promptly to once adding sulfuric acid reduction pH value to 1.0～4.0 in the heavy zinc liquid, makes zinc generate zinc sulfate, ammonium double salt:
0～80 ℃ of heavy double salt temperature, time 0.25～4h.The zinc sulfate ammonium double salt that is generated can be sent into once the heavy zinc process heavy zinc that neutralizes.
Five, zinc hydroxide calcining
Purified zinc hydroxide is 300～900 ℃ of calcining 0.25～6h down in temperature, obtains high-quality grade zinc oxide:
The present invention and acid system relatively have following outstanding advantage: 1. impurity element leaches and lacks, and removal of impurities is simple, and technical process shortens dramatically; 2. can adapt to the processing of the low zinc material of high ferro; 3. service temperature is low, saves the energy; 4. can directly make high-quality grade zinc oxide; 5. do not need equipment anticorrosion, reduced investment.With general ammonia process relatively, also have tangible advantage: 1. leach liquor zinc concentration height has enlarged capacity of equipment; 2. plumbous the leaching seldom, manganese, iron are leached hardly, removal of impurities easily, process is simplified; 3. can directly make high-quality product; 4. can adopt low ammono-system to handle, operational condition is good; 5. very thorough (Zn＜2g/l), zinc direct yield height of the heavy zinc of double salt method secondary.The present invention is applicable to the secondary zinc oxide that contains zinc 〉=15%, ironmaking, refining manganese zinc smoke, the roasting material of all kinds of zinc ores and zinc ore concentrate, hydrometallurgy filter residue, hot galvanizing residue, the processing of zinc oxide such as casting zinc dross or zinc hydroxide or metallic zinc material.
Description of drawings:
Fig. 1 is a principle flow chart of the present invention.
Embodiment:
1. the Guangxi factory zinc sulfide concentrates boiling roaster electricity flue dust that gathers dust, its composition (%) is:
Zn-65.56，Pb-11.96，Cd-0.97，Cu-0.029，Fe-0.55，Mn-0.39
Employed ammino mixture consists of: ammonia 3.0N, and ammonium sulfate 5.0N, ammonium persulphate are 3% of flue dust, liquid-solid ratio is 6.7: 1, extraction time 2 hours, 20 ℃ of extraction temperatures, it is identical with complexing agent to wash the ammonia composition, and its consumption is 10% of a complexing agent consumption, uses Na
2S makes scavenging agent, presses cadmium in the leach liquor, lead, copper cubage, Na
2The S consumption is 3.0 times of theoretical amount.With the zinc sulfate ammonium double salt that returned last time 60 ℃ down in and scavenging solution 0.5 hour, making wherein, 40～60% zinc precipitates into zinc hydroxide.Zinc hydroxide is cleaned the back and was calcined 2 hours down at 700 ℃, gets pure white high grade zinc oxide, and its composition (%) is: ZnO-99.9%, Pb＜0.003, Cd＜0.00045, Cu＜0.0001, Mn＜0.0001.Reduce once with industrial sulphuric acid in the scope of pH value to 2.5～3 of heavy zinc liquid, be as cold as room temperature, separate double salt; Contain Zn-0.98g/l, (NH in the heavy zinc liquid of secondary
4)
2SO
4-6.15N returns leaching process as the main source of ammonium sulfate.Zinc concentration＞90g/l in the leach liquor; Zinc leaching rate＞95%, the zinc recovery from flue dust to high-quality zinc oxide 〉=93%.
2. Hunan factory zinc boiling roaster flue dust, its composition (%) is:
Zn-47.97, Pb-13.15, Cd-3.32, Cu-0.18, Fe-1.4, Ag-0.006, the employed ammino mixture of S-3.01 consists of: ammonia 4.0N, and ammonium sulfate 3.0N, the ammonium persulphate amount is 2.5% of a fume amount, liquid-solid ratio is 5: 1,, leaches at normal temperatures 2 hours after 1 hour 80 ℃ of activation again, 20 ℃ of extraction temperatures, washing and scavenging process are with example 1, and scavenging solution is heated to 83 ℃, zinc ammonia complex begins to decompose the effusion ammonia, to 94 ℃, distillates 40% of scavenging solution.Calcined 2 hours down at 700 ℃ after the sedimentary zinc hydroxide wash cleanization, get high grade zinc oxide, its composition (%) is: ZnO-99.89, Pb＜0.0015, Cd＜0.0004, Cu＜0.0001, Mn＜0.0001.The rectificated remaining liquid that divides dehydrogenation zinc oxide is transferred with industrial sulphuric acid in the scope of pH value to 2.5～3, is as cold as room temperature, separates double salt; Contain Zn-1.56g/l, (NH in the heavy zinc liquid of secondary
4)
2SO
4-5.5N, this solution can be opened a way, and also can return leaching process.Ammonia recovery is 66.27% in the ammonia still process process, zinc leaching rate 94.5%, zinc total yield＞92%.
3. iron-smelting blast furnace zinc smoke, its composition (%) is:
Zn-17，Fe＞40
Employed ammonia-ammonium complexing agent consists of: ammonia 2.5N, and ammonium sulfate 2.5N, the ammonium persulphate amount is 0.5% of a fume amount, liquid-solid ratio is 2.5: 1, at room temperature leached 2 hours, be that the ammonia-ammonium complexing agent of leaching agent 40% is washed and soaked slag more than 3 times with volume.Make high grade zinc oxide by the method for example 1 then, its composition (%) is: ZnO-99.82, Pb＜0.0002, Cd＜0.0003, Cu＜0.0001, Mn＜0.0001.Zinc leaching rate 80%, zinc total yield 75%.
The rich manganese slag blast furnace dust of pyrogenic process volatilization refining produce secondary zinc oxide, its composition (%) is:
Zn-51.97, Pb-24.56, Cd-0.38, Cu-0.00338, Fe-0.039, Ag-0.011, Mn-0.03, employed ammonia-ammonium complexing agent consists of: ammonia 4.0N, ammonium sulfate 3.0N, the ammonium persulphate amount is 1% of a secondary zinc oxide, liquid-solid ratio is 5: 1,, leached at normal temperatures again 1.5 hours after 1 hour 85 ℃ of activation.Washing and scavenging process are with example 1, and the method for use-case 2 is made high grade zinc oxide, and its composition (%) is: ZnO-99.97, Pb＜0.002, Cd＜0.0003, Cu＜0.0001, Mn＜0.0001.Ammonia recovery is 68.% in the ammonia still process process, zinc leaching rate 94.5%, and zinc total yield＞92%, immersion liquid zinc concentration are 86g/l.
Claims (4)
1, produce the method for high grade zinc oxide, comprise the leaching, purification of material containing zinc, technological processs such as heavy zinc, the heavy zinc of secondary and calcining once, it is characterized in that:
A 〉: the complexing leaching agent that leaching process uses is: contain ammonia 1.5～8.5N, ammonium salt 1.5～8.5N, ammonium persulphate are 0～10% of raw material weight, and leaching liquid-solid ratio is 2～10: 1, and temperature is 0～90 ℃, and the time is 0.5～4h;
B〉purification of leach liquor adopts the sulphur root (S of 2～4 times of theoretical amount
2-) as scavenging agent, purification temperature is 0～60 ℃, the time is 0.25～4h;
C〉once heavy zinc adopts in (i) double salt and heavy zinc method, and neutral temperature is 0～90 ℃, and the time is 0.25～6h, (ii) steams the heavy zinc method of ammonium, and controlled temperature is 80～98 ℃;
D〉in heavy zinc liquid once, add sulfuric acid in the heavy zinc process of secondary and reduce pH value to 1.0～4.0,0～80 ℃ of heavy zinc temperature, time 0.25～4h;
E〉calcining temperature of the zinc hydroxide that obtains of once heavy zinc is 300～900 ℃, the time is 0.25～6h.
2, method according to claim 1 is characterized in that, described vulcanizing agent can be NaHS or Na
2S or H
2S or S
2-
3, method according to claim 1 is characterized in that, described double salt is the zinc sulfate ammonium, and its molecular formula is: ZnSO
4(NH
4)
2SO
46H
2O.
4, method according to claim 1, it is characterized in that, described material containing zinc comprises the secondary zinc oxide that contains zinc 〉=15%, ironmaking, refining manganese zinc smoke, the roasting material of all kinds of zinc ores and zinc ore concentrate, the hydrometallurgy filter residue, hot galvanizing residue, zinc oxide or zinc hydroxide or metallic zinc materials such as casting zinc dross.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92103230 CN1028768C (en) | 1992-04-28 | 1992-04-28 | Method for preparing zinc oxide by ammonia process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92103230 CN1028768C (en) | 1992-04-28 | 1992-04-28 | Method for preparing zinc oxide by ammonia process |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1065685A true CN1065685A (en) | 1992-10-28 |
| CN1028768C CN1028768C (en) | 1995-06-07 |
Family
ID=4940084
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92103230 Expired - Fee Related CN1028768C (en) | 1992-04-28 | 1992-04-28 | Method for preparing zinc oxide by ammonia process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1028768C (en) |
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| CN101891607A (en) * | 2010-07-09 | 2010-11-24 | 深圳市危险废物处理站有限公司 | Production method for synthesizing zinc fumarate feed addictive by using secondary zinc oxide |
| CN102633295A (en) * | 2012-04-26 | 2012-08-15 | 中南大学 | Oxidation pretreatment method of soot containing zinc |
| CN102747226A (en) * | 2012-04-25 | 2012-10-24 | 昆明理工大学 | Method for treating zinc hydrometallurgy waste residue by using alkali ammonium sulfur coupling method |
| CN102828032A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing lithopone by utilizing electrolytic zinc acid leaching slag |
| CN102828035A (en) * | 2012-09-25 | 2012-12-19 | 四川巨宏科技有限公司 | Method for producing high-purity zinc oxide through decarbonization on electrolytic zinc acid leaching slag by adopting ammonia process |
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-
1992
- 1992-04-28 CN CN 92103230 patent/CN1028768C/en not_active Expired - Fee Related
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| CN104178642B (en) * | 2014-08-31 | 2015-12-09 | 中南大学 | A method for separating zinc and iron in zinc leaching slag |
| CN104178642A (en) * | 2014-08-31 | 2014-12-03 | 中南大学 | Method for separating zinc and iron from zinc leaching residues |
| CN104862487A (en) * | 2015-04-21 | 2015-08-26 | 上海交通大学 | High-efficiency resource transformation method of nonferrous metal zinc-smelting fly ash |
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Also Published As
| Publication number | Publication date |
|---|---|
| CN1028768C (en) | 1995-06-07 |
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