CN104232944B - Process for comprehensively recycling indium from ammonia leaching residues and co-producing zinc oxide - Google Patents
Process for comprehensively recycling indium from ammonia leaching residues and co-producing zinc oxide Download PDFInfo
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- CN104232944B CN104232944B CN201410453304.3A CN201410453304A CN104232944B CN 104232944 B CN104232944 B CN 104232944B CN 201410453304 A CN201410453304 A CN 201410453304A CN 104232944 B CN104232944 B CN 104232944B
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Abstract
The invention relates to a process for comprehensively recycling indium form ammonia leaching residues and co-producing zinc oxide. On the basis of the conventional technology, the process structure is regulated and the process flow is optimized, so that two production systems which are originally independent from each other are organically combined. By adopting a method of sharing equipment, combining processes and complementing advantages, metal loss is effectively reduced and wastewater emission can be reduced and even avoided, so that the production cost is effectively lowered. Besides, the process further can be used for obviously increasing the yield of crude indium and zinc oxide, so that the performance of enterprises and the social benefits are improved to the greatest extent.
Description
Technical field
The present invention relates to the production technique of thick indium and zinc oxide, particularly relate to a kind of ammonia leaching residue comprehensive recovery of indium and coproduction zinc oxide technique.
Background technology
Indium belongs to rare metal, and the amount in the earth's crust is considerably less, is about 1 × 10 by mass percentage
-5%, it is that dispersion state is present in various metal ore, does not still find independent indium mineral deposit in the world up to now.The most normal association of indium is in Pb-Zn deposits, and the raw material mainly plumbous roasted dust of zinc of thick indium production at present, Qi Zhongqian, zinc are the master operations that thick indium is produced with being separated of indium.Because lead is insoluble to sulfuric acid, still stay in slag after leaching, it is just fairly simple with being separated of indium, and zinc, indium are all soluble in sulfuric acid, and their separation is very difficult.
Traditional thick indium production technique:
1, thick indium is produced: containing indium low zinc material-→ sulfuric acid leaching-→ iron powder reducing-→ extraction-→ back extraction-→ displacement-→ pressure group-→ founding-→ thick indium product.
Zinc oxide has another name called zinc white, is generally white or micro-fine yellow powders, is made up of amorphous or needle-like small-particle, nontoxic, tasteless, presents faint yellow after high-temperature calcination, and in white after cooling, its fusing point is 1975 DEG C.Zinc oxide is widely used in rubber, plastics, ceramic enamel frit makeing, chemical catalyst, makeup, coating and high-tech product etc. field, it is a kind of important ceramic chemical industry flux raw material, especially architectural pottery Wall or floor tile glaze and soft-paste glaze consumption more, also widely use in art pottery glaze.Zinc oxide is intermediate oxide, is soluble in acid, alkali, ammonium chloride and ammoniacal liquor, and long-term storage is in damp atmosphere, and the carbonic acid gas easily absorbed in air generates zinc subcarbonate, also can by carbon or Carbon monoxide reduction metallic zinc.
Existing zinc oxide production technique is divided into pyrogenic process (be subdivided into not only: direct method and indirect method) and wet method (but also be subdivided into: acid system and ammonia process), two kinds of techniques respectively have relative merits, thermal process is simple, do not have discharge of wastewater, but energy consumption is high, cost is high; Wet method energy consumption is low, cost is low, but has waste water to need process or discharge.
Traditional zinc oxide (wet method) production technique:
2, zinc oxide is produced: secondary zinc oxide-→ sulfuric acid leaching-→ adjust PH=5-→ potassium permanganate one time deironing, manganese-→ zinc dust precipitation-→ potassium permanganate secondary deironing, manganese-→ soda ash sink zinc-→ zinc subcarbonate washing-→ drying-→ calcining-→ zinc oxide cooling-→ finished product crushing packing.
Traditional technology has the following disadvantages in actual production:
1, big for environment pollution: two separate systems, just have two strands independently waste water need process or discharge, the namely environmental pollution of twice.Particularly the raffinate of thick indium production, because processing requirement excess sulfuric acid, wherein not only has multiple heavy non-ferrous metal, and also has excessive acid.Some producer directly discharges, and it has just been well imagined the pollution of water body; Though the discharge after simple neutralization of some producer, does not reach the standard of " qualified discharge " far away, it is also contaminate environment similarly.
2, valuable metal runs off serious: two separate systems, also causes the serious situation that two parts of valuable metals run off.Because zinc, indium all vitriolizations, exist all in the liquid phase, and two systems are all a kind of metals only got wherein, and another kind of metal are in vain with discharging of waste liquid, causes serious waste after leaching.It is estimated, often produce a kg crude indium, zinc metal loss is at about 1 hundred to three hundred kilogram; And often produce one ton of zinc oxide, indium metal runs off at about 50 to one hundred five ten grams.What such production was annual be lost in more than more than 100 ten thousand yuan (calculating by daily output 10 kg crude indium or 10 tons of zinc oxide), and one of the metal of metal also contaminate environment just with discharge of wastewater.
3, require high to starting material: because the loss of valuable metal, so starting material selected in producing all are confined to the scope of " institute's metal content of getting is high, and to give up metal content low ", loss could be reduced like this.Also manufacturer's starting material scope of application is just reduced Just because of this.In other words, the development of manufacturer is namely limited.
4, investment is large, and cost is high: build two separate production systems, and because of without common part equipment, its fixing investment is affirmed relatively high.And the production system that two separate, its production cost forms also correspondingly high.Such as thick indium is produced, its processing requirement excess sulfuric acid, that is drops into superfluous one-tenth and originally adapts to processing requirement.And the sulfuric acid of this part surplus must to come passively and it with lime again in the process of wastewater treatment, which again increases a high production cost.Such contradiction also has many in traditional processing technology.
In addition zinc oxide by ammonia process with its less energy-consumption, low cost, Selectively leaching, wastewater treatment simple and strong adaptability etc. advantage be more and more used widely.But it has weak point too, as leaching yield is low, slag is containing zinc high (generally 12-20%) etc., and its raw material (secondary zinc oxide) is usually rich in indium, and therefore the ammonia leached mud comprehensive recovery of indium of zinc oxide by ammonia process and coproduction zinc oxide are the important supplement of its technique.
Summary of the invention
For the problems referred to above, the invention provides a kind of ammonia leaching residue comprehensive recovery of indium and coproduction zinc oxide technique, it is on the basis of zinc oxide by ammonia process preparation technology, increase thick indium coproduction zinc oxide production line, effectively can not only reduce metal loss, reduce and even stop discharge of wastewater, and then effectively reduce production cost, but also thick indium and zinc oxide output can be significantly improved, enterprise benefit and social benefit to greatest extent.
In order to solve the problem, the present invention has carried out improving to thick indium and zinc oxide joint process and provides following technical process to arrange:
1. ammonia leaching residue is sized mixing with water in aerobic fermentation tank, and join the vitriol oil on request and carry out the slaking of high temperature peracid, the filtrate adding zinc subcarbonate washing and recycling is leached, and the slag delead after press filtration washing reclaims.
2. leach liquor, slag washing liquid in neutralization tank with secondary zinc oxide (containing indium comparatively high and low Pb) neutralization, and heat, drum air, add hydrogen peroxide oxidation hydrolysis deironing, in after press filtration and slag, neutralizer 3., 4. walk process following.
3. a, in and slag through slaking again, leaching, and with iron powder, Fe3+ is reduced to upper extraction tank extraction indium after Fe2+, then after back extraction, removal of impurities, displacement, pressure group and founding obtained thick indium product.
Secondary zinc oxide (containing indium, the high plumbous) neutralization of b, raffinate, heating, drum air, add hydrogen peroxide oxidation hydrolysis deironing after converge to " 4. c " and produce zinc oxide.
4. c, above-mentioned two kinds of neutralizers heat, add ammonium persulphate (or potassium permanganate, Javelle water) deironing, demanganization.
D, add zinc dust precipitation purification.
E, secondary add ammonium persulphate and refine.
F, add bicarbonate of ammonia and sink zinc.
G, reacted zinc subcarbonate are through repeatedly washing, filtering, and washings adverse current uses, press filtration after washing that final stage adds " pure water of condensation ".
H, one filtrate enter ammonium sulfate recovery system, through evaporation, concentrated (MVR), cooling, (ammonium sulfate can for agricultural for crystallization production ammonium sulfate, also can join secondary zinc oxide roasting, reclaim ammonia and sulfuric acid, so also greatly can reduce production cost).
The evaporated liquor that i, condensation are got off and steam condensate can be described as " pure water of condensation ", for final stage washing, can guarantee washing effect.
Other filtrate of j, recovery is for leaching, washing, and having more part can stock.
Zinc subcarbonate drying after k, washing, be sintered into zinc oxide, and cool, packaging final prod after fine grinding.
Concrete, ammonia leaching residue comprehensive recovery of indium of the present invention and coproduction zinc oxide technique comprise the following steps:
1) slaking of ammonia leached mud, leaching: ammonia leaching residue is sized mixing with water in aerobic fermentation tank, in dry slag: the vitriol oil is that the ratio of 1:0.7-1.5 is joined the vitriol oil and carried out the slaking of high temperature peracid and stirring reaction 2 hours, then the filtrate adding zinc subcarbonate washing and recycling is leached, and the slag delead after press filtration washing reclaims;
2) enrichment of indium: leach liquor, slag washing liquid in neutralization tank with in secondary zinc oxide and, in and terminal be PH=5.0, and heat to 80 DEG C, drum air, add hydrogen peroxide oxidation hydrolysis deironing, the add-on of hydrogen peroxide is 3-6 times of iron total amount in solution;
3) indium processed:
A, in and slag through slaking again, leaching, namely in dry slag: the ratio of the vitriol oil=1:0.7-1.5 is joined the vitriol oil and carried out the slaking of high temperature peracid and stirring reaction 2 hours, and the filtrate then adding zinc subcarbonate washing and recycling is leached.And upper extraction tank extraction indium after Fe3+ being reduced to Fe2+ with iron powder, then obtain thick indium product after back extraction, removal of impurities, displacement, pressure group and founding;
B, raffinate secondary zinc oxide neutralize, in and terminal be PH=5.0, heat to 80 DEG C, drum air, add hydrogen peroxide oxidation hydrolysis deironing, the add-on of hydrogen peroxide is 3-6 times of iron total amount in solution;
4) zinc oxide is produced and wastewater treatment:
C, above-mentioned two kinds of neutralizers are heated to 90 DEG C, add ammonium persulphate deironing, demanganization, and the add-on of ammonium persulphate is 8-10 times of ferrimanganic total mass in solution;
D, add zinc dust precipitation purification, zinc powder add-on is 2-5 times of plumbous cadmium total mass in solution;
E, secondary add ammonium persulphate and refine, and the add-on of ammonium persulphate is 8-10 times of ferrimanganic total mass in solution;
F, add bicarbonate of ammonia and sink zinc, until solution Zn content≤1g/L;
G, reacted zinc subcarbonate are through repeatedly washing, filtering, and washings adverse current uses, press filtration after washing that final stage adds " pure water of condensation ";
H, one filtrate enter ammonium sulfate recovery system, produce ammonium sulfate through evaporation, concentrated, cooling, crystallization;
The evaporated liquor that i, condensation are got off and steam condensate can be described as " pure water of condensation ", for final stage washing, can guarantee washing effect;
Other filtrate of j, recovery is for leaching, washing, and having more part can stock;
Zinc subcarbonate drying after k, washing, be sintered into zinc oxide, and cool, packaging final prod after fine grinding.
Compared with prior art, the beneficial effect that the present invention has is:
1., in joint process zinc oxide is produced and is actually the raffinate utilizing thick indium to produce and carries out, and the leaching water of thick indium production is that the wash filtrate utilizing zinc oxide to produce carries out.Material is thus formed " closed cycle " of waste water, reduce wastewater treatment and quantity discharged to greatest extent, even can reach the requirement of " zero release ".Social benefit is very large.
2., the combined recovery of joint process, reduce the loss of valuable metal to greatest extent, and sulfuric acid is not superfluous in the entire system, i.e. " used to make the best ", production cost is reduced greatly.In addition, if pay the ammonium sulfate produced and be used for roasting together with secondary zinc oxide, the consumption of sulfuric acid and bicarbonate of ammonia can also be greatly reduced.Namely the space reducing production cost is larger.
3., this technique adopts the bicarbonate of ammonia of low price to replace soda ash, and not only having reduced costs but also created for the recycle of sulfuric acid and ammonia may.
This technique adjusts process structure, optimization technological process on conventional art basis, production system separate for two scripts organically combined.Take the way that collaborative share, technique are in parallel, have complementary advantages, effectively reduce metal loss, reduce and even stop discharge of wastewater, and then effectively reduce production cost.In addition, this technique can also significantly improve thick indium and zinc oxide output, to greatest extent enterprise benefit and social benefit.
Embodiment
Below in conjunction with embodiment, the present invention is described further, but do not cause any restriction to the present invention.
Embodiment 1
A kind of ammonia leaching residue comprehensive recovery of indium and coproduction zinc oxide technique, it comprises the following steps:
1) slaking of ammonia leached mud, leaching: ammonia leaching residue is sized mixing with water in aerobic fermentation tank, in dry slag: the vitriol oil is that the ratio of 1:0.7-1.5 is joined the vitriol oil and carried out the slaking of high temperature peracid and stirring reaction 2 hours, then the filtrate adding zinc subcarbonate washing and recycling is leached, and the slag delead after press filtration washing reclaims;
2) enrichment of indium: leach liquor, slag washing liquid in neutralization tank with in secondary zinc oxide and, in and terminal be PH=5.0, and heat to 80 DEG C, drum air, add hydrogen peroxide oxidation hydrolysis deironing, the add-on of hydrogen peroxide is 3-6 times of iron total amount in solution;
3) indium processed:
A, in and slag through slaking again, leaching, namely in dry slag: the vitriol oil is that the ratio of 1:0.7-1.5 is joined the vitriol oil and carried out the slaking of high temperature peracid and stirring reaction 2 hours, and the filtrate then adding zinc subcarbonate washing and recycling is leached.And with iron powder Fe
3+be reduced to Fe
2+rear upper extraction tank extraction indium, thicker indium product is obtained after back extraction, removal of impurities, displacement, pressure group and founding;
B, raffinate secondary zinc oxide neutralize, in and terminal be PH=5.0, heat to 80 DEG C, drum air, add hydrogen peroxide oxidation hydrolysis deironing, the add-on of hydrogen peroxide is 3-6 times of iron total amount in solution;
4) zinc oxide is produced and wastewater treatment:
C, above-mentioned two kinds of neutralizers are heated to 90 DEG C, add ammonium persulphate deironing, demanganization, and the add-on of ammonium persulphate is 8-10 times of ferrimanganic total mass in solution;
D, add zinc dust precipitation purification, zinc powder add-on is 2-5 times of plumbous cadmium total mass in solution;
E, secondary add ammonium persulphate and refine, and the add-on of ammonium persulphate is 8-10 times of ferrimanganic total mass in solution;
F, add bicarbonate of ammonia and sink zinc, until solution Zn content≤1g/L;
G, reacted zinc subcarbonate are through repeatedly washing, filtering, and washings adverse current uses, press filtration after washing that final stage adds " pure water of condensation ";
H, one filtrate enter ammonium sulfate recovery system, produce ammonium sulfate through evaporation, concentrated, cooling, crystallization;
The evaporated liquor that i, condensation are got off and steam condensate can be described as " pure water of condensation ", for final stage washing, can guarantee washing effect;
Other filtrate of j, recovery is for leaching, washing, and having more part can stock;
Zinc subcarbonate drying after k, washing, be sintered into zinc oxide, and cool, packaging final prod after fine grinding.
The above embodiment only have expressed one embodiment of the present invention, and it describes comparatively concrete and detailed, but therefore can not be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that for the person of ordinary skill of the art, without departing from the inventive concept of the premise, can also make some distortion and improvement, these all belong to protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with claims.
Claims (1)
1. ammonia leaching residue comprehensive recovery of indium and a coproduction zinc oxide technique, is characterized in that, comprise the following steps:
1) slaking of ammonia leached mud, leaching: ammonia leached mud is sized mixing with water in aerobic fermentation tank, in dry slag: the vitriol oil is that the ratio of 1:0.7-1.5 is joined the vitriol oil and carried out the slaking of high temperature peracid and stirring reaction 2 hours, then the filtrate adding zinc subcarbonate washing and recycling is leached, and the slag delead after press filtration washing reclaims;
2) enrichment of indium: leach liquor, slag washing liquid in neutralization tank with in secondary zinc oxide and, in and terminal be PH=5.0, and heat to 80 DEG C, drum air, add hydrogen peroxide oxidation hydrolysis deironing, the add-on of hydrogen peroxide is 3-6 times of iron total amount in solution;
3) indium processed:
A, in and slag through slaking again, leaching, namely in dry slag: the ratio of the vitriol oil=1:0.7-1.5 is joined the vitriol oil and carried out the slaking of high temperature peracid and stirring reaction 2 hours, and the filtrate then adding zinc subcarbonate washing and recycling is leached, and with iron powder Fe
3+be reduced to Fe
2+rear upper extraction tank extraction indium, thicker indium product is obtained after back extraction, removal of impurities, displacement, pressure group and founding;
B, raffinate secondary zinc oxide neutralize, in and terminal be PH=5.0, heat to 80 DEG C, drum air, add hydrogen peroxide oxidation hydrolysis deironing, the add-on of hydrogen peroxide is 3-6 times of iron total amount in solution;
4) zinc oxide is produced and wastewater treatment:
C, two kinds of neutralizers are heated to 90 DEG C, add ammonium persulphate deironing, demanganization, and the add-on of ammonium persulphate is 8-10 times of ferrimanganic total mass in solution;
D, add zinc dust precipitation purification, zinc powder add-on is 2-5 times of plumbous cadmium total mass in solution;
E, secondary add ammonium persulphate and refine, and the add-on of ammonium persulphate is 8-10 times of ferrimanganic total mass in solution;
F, add bicarbonate of ammonia and sink zinc, until solution Zn content≤1g/L;
G, reacted zinc subcarbonate are through repeatedly washing, filtering, and washings adverse current uses, press filtration after washing that final stage adds " pure water of condensation ";
H, one filtrate enter ammonium sulfate recovery system, produce ammonium sulfate through evaporation, concentrated, cooling, crystallization;
The evaporated liquor that i, condensation are got off and steam condensate are called " pure water of condensation ", for final stage washing, can guarantee washing effect;
Other filtrate of j, recovery, for leaching, washing, has more part and stocks;
Zinc subcarbonate drying after k, washing, be sintered into zinc oxide, and cool, packaging final prod after fine grinding.
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| CN104831077A (en) * | 2015-04-01 | 2015-08-12 | 郴州雄风环保科技有限公司 | Method for extracting and separating indium and tin from indium-containing leaching residues |
| CN106381398A (en) * | 2016-09-30 | 2017-02-08 | 西安建筑科技大学 | Method for recovering indium from indium-contained soot |
| CN106337134A (en) * | 2016-09-30 | 2017-01-18 | 西安建筑科技大学 | Technique for recovering indium from indium-containing soot |
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| EP2082070A1 (en) * | 2006-11-02 | 2009-07-29 | Umicore | Recovery of non-ferrous metals from by-products of the zinc and lead industry using electric smelting with submerged plasma |
| CN101565779B (en) * | 2009-05-18 | 2011-06-08 | 葫芦岛锌业股份有限公司 | Method for producing zinc powder and reclaiming scattered metals indium and germanium by distilling aluminum hard zinc in vacuum |
| CN104017995B (en) * | 2014-06-24 | 2016-01-13 | 株洲冶炼集团股份有限公司 | A kind of from containing the method reclaiming copper-indium-galliun-selenium copper-indium-galliun-selenium waste material |
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Denomination of invention: Process for comprehensively recycling indium from ammonia leaching residues and co-producing zinc oxide Effective date of registration: 20200414 Granted publication date: 20150624 Pledgee: Shaoguan urban rural credit cooperatives Wujiang credit cooperatives Pledgor: SHAOGUAN KAIHONG NANO MATERIAL Co.,Ltd. Registration number: Y2020440000082 |