CN104384171B - The resource recoverying and utilizing method of pyrite cinder - Google Patents
The resource recoverying and utilizing method of pyrite cinder Download PDFInfo
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- CN104384171B CN104384171B CN201410572846.2A CN201410572846A CN104384171B CN 104384171 B CN104384171 B CN 104384171B CN 201410572846 A CN201410572846 A CN 201410572846A CN 104384171 B CN104384171 B CN 104384171B
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Abstract
The resource recoverying and utilizing method of pyrite cinder, is related to inorganic chemical technology field.Its key step：Pyrite cinder is separated into aluminium hydroxide, calcium hydroxide with aqueous suspension, is reacted with carbon dioxide or NaOH, potassium hydroxide in water, separate and recover calcium carbonate or calcium hydroxide and aluminium hydroxide or sodium aluminate, potassium aluminate；Again with ammonium hydrogen carbonate or ammonium sulfate/ammonium chloride or phosphoric acid separated and dissolved magnesia；Again with NaOH or the waste residue of potassium hydroxide treatment di-iron trioxide or/and ferrous oxide, silica and sulphur, separated and dissolved silica and sulphur；Recycling di-iron trioxide or/and ferrous oxide, silicic acid, sylvite or sodium salt and sulphur.The separation and recovery for being applied to pyrite cinder is recycled.
Description
Art：
The present invention relates to the resource recoverying and utilizing method of inorganic chemical technology field, particularly pyrite cinder.
Background technology：
Troilite produces sulfuric acid, and often producing 1 ton of sulfuric acid will produce 0.8-0.9 tons of pyrite cinder (sulfate slag), China
Annual pyrite cinder discharge capacity is up to 3,000,000 tons, and waste residue yield is huge.Because China's troilite is mostly lean ore, sulfate slag
Middle sulfur content is too high, iron oxide and ferrous oxide content are most below 50%, and the impurity content such as silica is too high, so often
The sulfate slag that year directly recycles only has 1,000,000 tons or so, causes the serious wasting of resources, environmental pollution and land seizure
Waste, so from resources conservation, the angle of effectively utilization and environmental protection, waste residue separation and recovery is significant.Troilite is produced
The main component of waste residue of sulfuric acid (sulfate slag) has：Di-iron trioxide is iron oxide and ferrous oxide, accounts for waste residue 20%--60%, sulphur
Ferrous oxide content is less in acid sludge, silica, accounts for waste residue 15%--55%, aluminum oxide, accounts for waste residue 10%, calcium oxide, accounts for
Waste residue 5%, magnesia, accounts for waste residue below 5%, and sulphur (element sulphur), accounts for waste residue 0.5%-2%；In addition with micro copper,
The trace meter simple substance such as lead, zinc, cobalt, gold and silver.In the prior art also without inexpensive, simple efficient real separation and recovery
Method, seriously constrains the development that China's troilite produces sulfuric acid industry, had not only wasted resource but also had compromised environment.Existing point
From technology, chemically reacted with hydrochloric acid or sulfuric acid, this is clearly to talk about stratagems on paper.
Chemically reacted with hydrochloric acid or sulfuric acid, both changed di-iron trioxide, ferrous oxide, aluminum oxide, calcium oxide in waste residue
With the hyle form of magnesia, substantial amounts of hydrochloric acid or sulfuric acid are also consumes, drastically increase waste residue separation costs, while
The water soluble salt mixture for being difficult to separate is generated again；Particularly with sulfuric acid reaction, troilite production sulfuric acid produces waste residue, and is
Separating waste residues again fall sulfuric acid consumption, and pyrite slag amount is too big, lose to come as the sulfuric acid of essential industry raw material
Source.Existing isolation technics also changes into the carbonate of iron, then high temperature reduction is di-iron trioxide or ferrous oxide, chemical former material
The consumption and waste of material are excessive, and energy waste is excessive, and separation costs are too high.Due to technical bottleneck, China's sulfuric acid industry is faced with
Awkward predicament：Produced with troilite, waste residue is difficult to separate and recover；Produced with sulphur (S) ore deposit, resource-constrained, it is impossible to meet China's sulphur
Sour industrial expansion demand.
The content of the invention：
Inventive principle：
According to prior art and knowledge：
1. aluminum oxide, calcium oxide are hydrated into hydrated alumina, calcium hydroxide suspension emulsion respectively；Magnesia is dissolved in ammonium salt
The aqueous solution, di-iron trioxide or/and ferrous oxide, silica and sulphur do not dissolve in ammonium salt aqueous solution, and by magnesia and three oxygen
Change two iron or/and ferrous oxide, silica and sulphur mixture are separated；Sl. sol. calcium hydroxide aqueous solution again can be with carbon dioxide
CO2The lime deposit of reaction generation water-insoluble.Ammonium hydrogen carbonate is the ammonium salt of weak acid and weak base, and the aqueous solution is in alkalescence, carbonic acid
It is very weak acid, ammonium hydrogen carbonate can not can only dissolve magnesia with oxidation reactive magnesium generation magnesium salts, its aqueous solution.
2. silica, sulphur all react with the highly basic NaOH or potassium hydroxide aqueous solution of heat, generate water miscible thing
Matter, thus separate nonreactive di-iron trioxide or/and ferrous oxide.
3. aluminum oxide is amphoteric compound, and heating can react with highly basic NaOH or potassium hydroxide, generate water miscible
Aluminate.Industrial Bayer process, aluminum oxide and highly basic NaOH or the principles of science of potassium hydroxide heating response, reaction equation：
AL2O3+3H2O+2NaOH heating=2NaAL (OH)4,
AL2O3+3H2O+2KOH heating=2KAL (OH)4。
4. copper sulfide does not dissolve in dilute sulfuric acid, removes hydrogen sulfide.
5. NaOH or potassium hydroxide do not react with di-iron trioxide or/and ferrous oxide.
6. sulfur dioxide SO2With hydrosulphuric acid H2S reacts, and generates sulphur S and water.
7. silicic acid is that a class has [SiOx(OH)4-2x]nThe compound of formula, can be by soluble silicate and acid reaction
Produce；
Simple silicic acid such as metasilicic acid H2SiO3, two silicic acid H2Si2O5With orthosilicic acid H4SiO4Deng the inspection in weak solution
Measure；Metasilicic acid can only be condensed into two silicic acid in 0 DEG C or so presence during room temperature, two silicic acid resolve into water and dioxy at 150 DEG C
SiClx；
Soluble silicate, plus any weak acid, can obtain silicic acid；The unimolecule silicic acid of separate out, dissolves in
Water, but it in the solution gradually associate form bimolecular, three molecules, eventually form undissolved polymolecular polymer, gained
Colloid is referred to as " silica sol "；If silicate solution concentration is larger, silicic acid jelly is directly formed after acid adding, obtained after dehydration
Silicic acid gel.
8. ammonium hydrogen carbonate starts to decompose into ammonia, carbon dioxide and water more than 30 DEG C.
9. ammonium chloride, ammonium sulfate with oxidation reactive magnesium ionic equation：
MgO+2NH4 +=Mg2++2NH3↑+H2O.Recyclable magnesium chloride or magnesium sulfate and an ammoniacal liquor (hydration ammonia NH3·H2O water
Solution).
10., according to existing knowledge, iron oxide and/or ferrous oxide are dissolved in acid, and magnesia is also dissolved in acid；Magnesia can
It is magnesium hydroxide to be hydrated, but it is iron hydroxide or ferrous hydroxide that iron oxide or ferrous oxide can not be hydrated, it is seen that magnesia
Chemism and molecular polarity are more much better than than iron oxide or ferrous oxide；And phosphoric acid is middle strong acid or weak acid, it hardly has
Oxidizing, phosphoric acid is proportional with phosphate aqueous solution mass concentration to the dissolving power of metal oxide；Same phosphate aqueous solution matter
Under amount concentration, phosphoric acid is proportional with the chemism of metal oxide and molecular polarity size to the dissolving power of metal oxide,
Polar molecule is dissolved in polar molecule；The liquid SPA of the only mass ratio 80%-85% aqueous solution could dissolve iron oxide and/or
Ferrous oxide；And the phosphate aqueous solution of mass ratio 65%-70% can only then dissolve magnesia, it is impossible to dissolve iron oxide and/or oxygen
Change ferrous；At normal temperatures, in a short time, the phosphate aqueous solution of mass ratio 65%-70% does not chemically react with magnesia；Because of oxygen
Change magnesium water solubility very low, phosphoric acid hardly has oxidisability again, the phosphate aqueous solution of mass ratio 65%-70% is only small 24
When more than long-time place under the conditions of, just with magnesia slow reaction；And the phosphoric acid,diluted aqueous solution in mass ratio below 50%
In, magnesia is immediately disconnected Precipitation；Combined with water because phosphoric acid is soluble in water, water is polar molecule, hydrone separates
And the polar attraction between magnesia molecule and phosphoric acid molecules is destroyed, and magnesia molecule is departed from phosphoric acid molecules, dissociate and gather
Collection precipitation.Magnesia is separated with phosphoric acid and its concentration difference, the hyle form of magnesia can be kept.
11. according to existing knowledge, hydrogen peroxide (hydrogen peroxide) and vulcanization (Asia) iron reaction：
(1).H2O2+FeS2+H2O=H2O+Fe(OH)2+2S；
(2).7H2O2+FeS2=6H2O+FeSO4+H2SO4；
(3).15H2O2+2FeS2=14H2O+Fe2(SO4)3+H2SO4.Vulcanization (Asia) iron can be removed.
Pyrite cinder is divided into aluminum oxide, calcium oxide, magnesia, di-iron trioxide or/and ferrous oxide by the present invention, and
This four part of silica, sulphur；Directly obtain di-iron trioxide or/and ferrous oxide；Again to hydrated alumina, calcium hydroxide,
Magnesia, and the method that thing is separated and recovered respectively and combinations thereof that is converted into of silica, sulphur is core of the invention
Technology is innovation essential features.
Technical scheme：
One, is sulfate slag with enough water immersion pyrite cinders, and is stirred, 30 turns -50 revs/min of rotating speed, mixing time
1-2 hours, the aluminum oxide in sulfate slag, calcium oxide is separately converted to hydrated alumina, calcium hydroxide, and turn into suspension milkiness
Liquid, stands, make di-iron trioxide or/and ferrous oxide, magnesia, silica, sulphur and comprising micro copper, lead, zinc, cobalt,
The trace meter simple substance mixture precipitate and separate immediately of gold and silver；Hydrated alumina, calcium hydroxide suspension emulsion are separated simultaneously；
Two, in hydrated alumina, the calcium hydroxide suspension emulsion of above-mentioned (one) to adding enough carbon dioxide CO2Or
Air, stirring, 50 turns -200 revs/min of rotating speed, 2-8 hour stirring reaction time, standing, make calcium hydroxide be converted into calcium carbonate and
Precipitate and separate immediately, then precipitated from hydrated alumina suspension emulsion or be separated by filtration aluminum oxide, reclaim aluminum oxide, water circulation
Utilize；
Or add enough NaOH or hydrogen-oxygen in hydrated alumina, the calcium hydroxide suspension emulsion to above-mentioned (one)
Change potassium, heating response, makes hydrated alumina change into water miscible sodium aluminate or potassium aluminate water at 1-2 hours stirring reaction time
Solution, stands, and reprecipitation or is separated by filtration recovery calcium hydroxide；Sodium aluminate or the vacuum concentration dehydration of aluminic acid aqueous solutions of potassium is dry
It is dry, reclaim sodium aluminate or potassium aluminate；
Reaction equation：AL2O3+3H2O+2NaOH heating=2NaAL (OH)4,
AL2O3+3H2O+2KOH heating=2KAL (OH)4；
Or enough sulfuric acid neutralization reactions are added in hydrated alumina, the calcium hydroxide suspension emulsion to above-mentioned (one),
Heating response, generates water miscible aluminum sulfate aqueous solution, and vacuum concentration is dehydrated, and separates and recovers aluminum sulfate；Precipitation is divided simultaneously
From sulfuric acid and the gypsum calcium sulfate of calcium hydroxide reaction generation；
Three, are by the di-iron trioxide or/and ferrous oxide of above-mentioned (one), magnesia, silica, sulphur and comprising micro
Copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, below 28 DEG C, add enough ammonium bicarbonate aqueous solutions, and
Stirring, 30 turns -50 revs/min of rotating speed mixing time 1-2 hours, makes magnesia be dissolved in ammonium bicarbonate aqueous solution；Precipitate and separate three
Aoxidize two iron or/and ferrous oxide, silica, sulphur and comprising micro copper, lead, zinc, cobalt, Jin Heyin trace meter simple substance
Mixture；The aqueous solution of ammonium hydrogen carbonate and magnesia is obtained simultaneously；
Again in sealing container, by ammonium hydrogen carbonate and the aqueous solution of magnesia, 35C--60 DEG C is heated to, makes ammonium hydrogen carbonate
Decompose, separate out magnesium oxide precipitation, reclaim magnesia；Ammonia NH is reclaimed with vacuum simultaneously3Or a hydration ammonia (NH3·H2O it is) water-soluble
Liquid, again by ammonia NH below 28 DEG C in sealing container3Or a hydration ammonia (NH3·H2O) aqueous solution and carbon dioxide CO2Water
Solution reaction, obtains ammonium bicarbonate aqueous solution, recycles；
Here, aqueous dissolution di-iron trioxide or/and ferrous oxide, the oxidation of ammonium chloride or ammonium sulfate can also be used
Magnesium, silica, sulphur and comprising the magnesia in micro copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, and
Stirring, 30 turns -50 revs/min of rotating speed, mixing time 1-2 hours, precipitate and separate di-iron trioxide or/and ferrous oxide, titanium dioxide
Silicon, sulphur and comprising micro copper, lead, zinc, cobalt, Jin Heyin trace meter simple substance mixture；Obtain magnesium chloride or sulfuric acid simultaneously
The aqueous solution of magnesium, vacuum concentration is dehydrated, pressure 25pa--100pa, time 8-24 hours, reclaims magnesium chloride or magnesium sulfate；
And reclaim ammoniacal liquor；
Or dissolve di-iron trioxide or/and ferrous oxide, magnesia, two with the phosphate aqueous solution of mass ratio 65%-70%
Silica, sulphur and comprising the magnesia in micro copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, and stir,
30 turns -50 revs/min of rotating speed, mixing time 1-2 hours, precipitate and separate di-iron trioxide or/and ferrous oxide, silica, sulphur
And comprising micro copper, lead, zinc, cobalt, Jin Heyin trace meter simple substance mixture；Obtain the aqueous solution of phosphoric acid and magnesia；
The aqueous solution of phosphoric acid and magnesia is added into water dilution again, phosphoric acid quality ratio makes oxidation below 50% in making phosphate aqueous solution
Magnesium is immediately disconnected Precipitation, reclaims magnesia；The phosphoric acid,diluted aqueous solution by this mass ratio below 50%, is concentrated in vacuo dehydration again
To the phosphate aqueous solution of mass ratio 65%-70%, recycle；
Four, by the di-iron trioxide or/and ferrous oxide of above-mentioned (three), silica, sulphur and comprising micro copper, lead,
Added in zinc, cobalt, the trace meter simple substance mixture of Jin Heyin and react slight excess of hydrogen relative to silica, sulfur chemistry
Sodium oxide molybdena or potassium hydroxide, and suppress sodium metasilicate or potassium silicate hydrolysis, to ensure the high-purity of di-iron trioxide or/and ferrous oxide
Degree；Heating response, stirring reaction, reaction time 2-8 hours；
Reaction equation：SiO2+ 2NaOH heating=Na2SiO3+H2O,
SiO2+ 2KOH heating=K2SiO3+H2O；
3S+6NaOH heating=2Na2S+Na2SO3+3H2O；
3S+6KOH heating=2K2S+K2SO3+3H2O；
Obtain the aqueous solution of sodium metasilicate, vulcanized sodium and sodium sulfite or potassium silicate, potassium sulfide and potassium sulfite；
Simultaneously isolated di-iron trioxide or/and ferrous oxide and comprising micro copper, lead, zinc, cobalt, Jin Heyin it is micro-
Amount metal simple-substance mixture；
Five, are water-soluble by the sodium metasilicate of above-mentioned (four), vulcanized sodium and sodium sulfite or potassium silicate, potassium sulfide and potassium sulfite
Add enough sulfuric acid in liquid, stirring reaction,
Reaction time 0.5-1 hours, reaction equation：
Na2SiO3+H2SO4=H2SiO3+Na2SO4
K2SiO3+H2SO4=H2SiO3+K2SO4
Na2SO3+H2SO4=H2SO3+Na2SO4；H2SO3Typically with SO2Exist with water；
K2SO3+H2SO4=H2SO3+K2SO4；H2SO3Typically with SO2Exist with water；
Na2S+H2SO4=H2S↑+Na2SO4
K2S+H2SO4=H2S↑+K2SO4；
Obtain the aqueous solution of silicic acid, sulfurous acid, hydrosulphuric acid, sodium sulphate or potassium sulfate, sulfurous acid H2SO3Or sulfur dioxide SO2
With hydrosulphuric acid H2Contents of the S in its aqueous solution is little；This step reaction, it is also possible to replace sulfuric acid with hydrochloric acid or nitric acid, because salt
Sour HL or nitric acid HNO3Acidity all than sulfuric acid H2SO4By force, sodium chloride or sodium nitrate or potassium chloride or potassium nitrate and silicon are obtained
Acid, sulfurous acid, hydrosulphuric acid；This step reaction, it is also possible to replace sulfuric acid with the organic acid of the strong acidity such as citric acid, fixedness
The volatile acid of acid generation and weak acid, heating response, and obtain its corresponding Organic Sodium Salt or sylvite and silicic acid, sulfurous acid, hydrogen
Sulfuric acid；This step reaction, it is also possible to replace sulfuric acid with phosphoric acid, the volatile acid of acid generation of fixedness and weak acid, heating response,
Obtain sodium ascorbyl phosphate or potassium phosphate and silicic acid, sulfurous acid, hydrosulphuric acid；
The reacting solution of above-mentioned (five) is precipitated or is separated by filtration silicic acid H by six,2SiO3Hydrate is just (original) silicic acid；
Namely the undissolved polymolecular polymer " silica sol " of water；
The aqueous solution of above-mentioned (six) is added enough copper sulphate CuSO by seven,4, stirring reaction makes hydrogen sulfide H2S reaction lifes
Into copper sulfide CuS precipitations, reaction equation：
CuSO4+H2S=CuS ↓+H2SO4；CuS does not dissolve in dilute sulfuric acid；Precipitate or be separated by filtration copper sulfide CuS；Copper sulphate
CuSO4Do not reacted with sulfurous acid or sulfur dioxide, because weak acid can not generate strong acid；In sodium metasilicate, vulcanized sodium and sodium sulfite
Or the aqueous solution of potassium silicate, potassium sulfide and potassium sulfite with hydrochloric acid or nitric acid reaction when, CuSO here4With H2The sulphur of S reaction generations
Acid, can use enough calcium hydroxide reactions, generation gypsum calcium sulfate to remove and reclaim；Remove 2/3rds sulphur；
Or by the aqueous solution of above-mentioned (six), according to
3S+6NaOH heating=2Na2S+Na2SO3+3H2O,
3S+6KOH heating=2K2S+K2SO3+3H2O react and
Na2SO3+H2SO4=H2SO3+Na2SO4,
K2SO3+H2SO4=H2SO3+K2SO4,
Na2S+H2SO4=H2S+Na2SO4,
K2S+H2SO4=H2S+K2SO4The sulfur dioxide and hydrogen sulfide molecule number or mole ratio for reacting generation are 1: 2 (1 ratio
2), further according to sulfur dioxide SO2With hydrosulphuric acid H2S reacts, by SO2And H2S reactions are converted into sulphur S and water, precipitate or are separated by filtration
Whole sulphur S；Reaction equation：SO2+2H2S=3S+2H2O；In sealing container, stirring reaction or heating stirring are reacted, temperature 25
℃--100℃；Reaction time 0.5-1 hours；The present invention also can first separate sulphur S herein, reprecipitation or be separated by filtration above-mentioned (five)
In the undissolved polymolecular polymer " silica sol " of water；
Eight, are by the sodium sulphate Na of above-mentioned (seven)2SO4Or potassium sulfate K2SO4The aqueous solution, vacuum concentration is dehydrated, pressure
25pa--100pa, time 8-24 hours, reclaims sodium sulphate Na2SO4Or potassium sulfate K2SO4。
The present invention, is not particularly illustrated, and is normal temperature and normal pressure；Produced in convention stir and in standing.Each chemistry is anti-
Answer the thing need be by detection level and calculating.
Due to the imperfect combustion of troilite, di-iron trioxide or/and ferrous oxide and comprising micro copper, lead, zinc,
Also contain about 1% iron sulfide FeS in cobalt, the trace meter simple substance mixture of Jin Heyin2, so using hydrogen peroxide (dioxygen again
Water) reacted with vulcanization (Asia) iron, reaction equation：
(1).7H2O2+FeS2=6H2O+FeSO4+H2SO4；
Or (2) .15H2O2+2FeS2=14H2O+Fe2(SO4)3+H2SO4；Will hydrogen peroxide water dilution needed for reaction, preparation
Into the aqueous solution of 3%--10%；Continuous penetrating contains a small amount of iron sulfide FeS2Di-iron trioxide or/and ferrous oxide and comprising
In micro copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, stirring reaction, 30 turns -50 revs/min of rotating speed, stirring
After time 1-2 hours, appropriate water is added, such as above-mentioned stirring at low speed washs ferrous sulfate and sulfuric acid or ferric sulfate and sulfuric acid；
Separation and recovery ferrous sulfate and sulfuric acid or ferric sulfate and sulphur aqueous acid；Obtain di-iron trioxide or/and ferrous oxide and bag
Containing micro copper, lead, zinc, cobalt, the trace meter simple substance of Jin Heyin mixture.
Beneficial effect：
1. the present invention has greatly saved waste residue stacking soil.
2. the present invention saves and is effectively utilized the natural resources of preciousness.
3. the present invention protects water environment and water resource.
4. the present invention opens the new wide of the raw material such as di-iron trioxide i.e. iron oxide and ferrous oxide, aluminium hydroxide
Raw material sources, saved the energy.
5. present invention safety in production, prevents inflammable, toxic gas discharge.
6. the present invention is simple to operate, and production equipment is simple, small investment of production equipment, and production capacity is big, low production cost；Divide completely
From not producing new waste residue；Each separate substance purity such as di-iron trioxide is all more than 98%；Combined sulfur S in di-iron trioxide
Constituent content does not contain element silicon and elemental sulfur in 0--0.15%, is that the development of the high-end steel alloy of China and stainless steel industry is carried
The technical support for having supplied raw material to produce.
The preferred scheme of technical solution of the present invention：
One, is sulfate slag with enough water immersion pyrite cinders, and is stirred, 30 turns -50 revs/min of rotating speed, mixing time
1-2 hours, the aluminum oxide in sulfate slag, calcium oxide is separately converted to hydrated alumina, calcium hydroxide, and turn into suspension milkiness
Liquid, stands, make di-iron trioxide or/and ferrous oxide, magnesia, silica, sulphur and comprising micro copper, lead, zinc, cobalt,
The trace meter simple substance mixture precipitate and separate immediately of gold and silver；Hydrated alumina, calcium hydroxide suspension emulsion are separated simultaneously；
Two, are heated to enough NaOH is added in hydrated alumina, the calcium hydroxide suspension emulsion of above-mentioned (one)
Reaction, 1-2 hour stirring reaction time, hydrated alumina is changed into water miscible sodium aluminate aqueous solution, standing, reprecipitation or
It is separated by filtration recovery calcium hydroxide；Sodium aluminate aqueous solution vacuum concentration is dehydrated, sodium aluminate is reclaimed；
Reaction equation：AL2O3+3H2O+2NaOH heating=2NaAL (OH)4；
Three, are by the di-iron trioxide or/and ferrous oxide of above-mentioned (one), magnesia, silica, sulphur and comprising micro
Copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, below 28 DEG C, add enough ammonium bicarbonate aqueous solutions, and
Stirring, 30 turns -50 revs/min of rotating speed mixing time 1-2 hours, makes magnesia be dissolved in ammonium bicarbonate aqueous solution；Precipitate and separate three
Aoxidize two iron or/and ferrous oxide, silica, sulphur and comprising micro copper, lead, zinc, cobalt, Jin Heyin trace meter simple substance
Mixture；The aqueous solution of ammonium hydrogen carbonate and magnesia is obtained simultaneously；
Again in sealing container, by ammonium hydrogen carbonate and the aqueous solution of magnesia, 35 DEG C are heated to -- 60 DEG C, make ammonium hydrogen carbonate
Decompose, separate out magnesium oxide precipitation, reclaim magnesia；Ammonia NH is reclaimed with vacuum simultaneously3Or a hydration ammonia (NH3.H2O it is) water-soluble
Liquid, again by ammonia NH below 28 DEG C in sealing container3Or a hydration ammonia (NH3.H2O) aqueous solution and carbon dioxide CO2It is water-soluble
Liquid reacts, and obtains ammonium bicarbonate aqueous solution, recycles；
Four, by the di-iron trioxide or/and ferrous oxide of above-mentioned (three), silica, sulphur and comprising micro copper, lead,
Added in zinc, cobalt, the trace meter simple substance mixture of Jin Heyin and react slight excess of hydrogen relative to silica, sulfur chemistry
Sodium oxide molybdena, and suppress sodium metasilicate hydrolysis, to ensure the high-purity of di-iron trioxide or/and ferrous oxide；Heating response, stirring is anti-
Should, reaction time 2-8 hours；
Reaction equation：SiO2+ 2NaOH heating=Na2SiO3+H2O,
3S+6NaOH heating=2Na2S+Na2SO3+3H2O；
Obtain the aqueous solution of sodium metasilicate, vulcanized sodium and sodium sulfite；
Simultaneously isolated di-iron trioxide or/and ferrous oxide and comprising micro copper, lead, zinc, cobalt, Jin Heyin it is micro-
Amount metal simple-substance mixture；
Five, will add enough sulfuric acid in the aqueous solution of the sodium metasilicate, vulcanized sodium and sodium sulfite of above-mentioned (four), stirring is anti-
Should,
Reaction time 0.5-1 hours, reaction equation：
Na2SiO3+H2SO4=H2SiO3+Na2SO4；
Na2SO3+H2SO4=H2SO3+Na2SO4；H2SO3Typically with SO2Exist with water；
Na2S+H2SO4=H2S+Na2SO4
Obtain the aqueous solution of silicic acid, sulfurous acid, hydrosulphuric acid, sodium sulphate, sulfurous acid H2SO3Or sulfur dioxide SO2And hydrosulphuric acid
H2Contents of the S in its aqueous solution is little；
The reacting solution of above-mentioned (five) is precipitated or is separated by filtration silicic acid H by six,2SiO3Hydrate is just (original) silicic acid；
Namely the undissolved polymolecular polymer " silica sol " of water；
Seven, by the aqueous solution of above-mentioned (six), according to
3S+6NaOH heating=2Na2S+Na2SO3+3H2The reaction of O and
Na2SO3+H2SO4=H2SO3+Na2SO4,
Na2S+H2SO4=H2S+Na2SO4Reaction generation sulfur dioxide and hydrogen sulfide molecular number or mole ratio be 1
: 2, further according to sulfur dioxide SO2With hydrosulphuric acid H2S reacts, by SO2And H2S reactions are converted into sulphur S and water, precipitate or are separated by filtration
Whole sulphur S；Reaction equation：SO2+2H2S=3S+2H2O；In sealing container, stirring reaction or heating stirring are reacted, temperature 25
℃--100℃；Reaction time 0.5-1 hours；
Eight, are by the sodium sulphate Na of above-mentioned (seven)2SO4The aqueous solution, vacuum concentration is dehydrated, pressure 25pa--100pa, when
Between 8-24 hours, reclaim sodium sulphate Na2SO4。
The present invention, is not particularly illustrated, and is normal temperature and normal pressure；Produced in convention stir and in standing.Each chemistry is anti-
Answer the thing need be by detection level and calculating.
Specific embodiment：
Embodiment：
One, is sulfate slag with enough water immersion pyrite cinders, and is stirred, 30 turns -50 revs/min of rotating speed, mixing time
1-2 hours, the aluminum oxide in sulfate slag, calcium oxide is separately converted to hydrated alumina, calcium hydroxide, and turn into suspension milkiness
Liquid, stands, make di-iron trioxide or/and ferrous oxide, magnesia, silica, sulphur and comprising micro copper, lead, zinc, cobalt,
The trace meter simple substance mixture precipitate and separate immediately of gold and silver；Hydrated alumina, calcium hydroxide suspension emulsion are separated simultaneously；
Two, in hydrated alumina, the calcium hydroxide suspension emulsion of above-mentioned (one) to adding enough carbon dioxide CO2Or
Air, stirring, 50 turns -200 revs/min of rotating speed, 2-8 hour stirring reaction time, standing, make calcium hydroxide be converted into calcium carbonate and
Precipitate and separate immediately, then precipitated from hydrated alumina suspension emulsion or be separated by filtration aluminum oxide, reclaim aluminum oxide, water circulation
Utilize；Carbon dioxide not with oxidation reactive aluminum；
Or enough potassium hydroxide is added in hydrated alumina, the calcium hydroxide suspension emulsion to above-mentioned (one), heat
Reaction, 1-2 hour stirring reaction time, hydrated alumina is changed into water miscible aluminic acid aqueous solutions of potassium, standing, reprecipitation or
It is separated by filtration recovery calcium hydroxide；Aluminic acid aqueous solutions of potassium vacuum concentration is dehydrated, potassium aluminate is reclaimed；
Reaction equation：AL2O3+3H2O+2KOH heating=2KAL (OH)4；
Or enough sulfuric acid neutralization reactions are added in hydrated alumina, the calcium hydroxide suspension emulsion to above-mentioned (one),
Heating response, generates water miscible aluminum sulfate aqueous solution, and vacuum concentration is dehydrated, and separates and recovers aluminum sulfate；Precipitation is divided simultaneously
From sulfuric acid and the gypsum calcium sulfate of calcium hydroxide reaction generation；
Three, are by the di-iron trioxide or/and ferrous oxide of above-mentioned (one), magnesia, silica, sulphur and comprising micro
The aqueous solution of copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, the enough ammonium chloride of addition or ammonium sulfate, dissolving
Di-iron trioxide or/and ferrous oxide, magnesia, silica, sulphur and comprising micro copper, lead, zinc, cobalt, Jin Heyin it is micro-
Magnesia in amount metal simple-substance mixture, and stir, 30 turns -50 revs/min of rotating speed, mixing time 1-2 hours, precipitate and separate three
Aoxidize two iron or/and ferrous oxide, silica, sulphur and comprising micro copper, lead, zinc, cobalt, Jin Heyin trace meter simple substance
Mixture；The aqueous solution of magnesium chloride or magnesium sulfate is obtained simultaneously, and vacuum concentration is dehydrated, pressure 25pa--100pa, time 8-
24 hours, reclaim magnesium chloride or magnesium sulfate；And reclaim ammonia or ammoniacal liquor；
Or dissolve di-iron trioxide or/and ferrous oxide, magnesia, two with the phosphate aqueous solution of mass ratio 65%-70%
Silica, sulphur and comprising the magnesia in micro copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, and stir,
30 turns -50 revs/min of rotating speed, mixing time 1-2 hours, precipitate and separate di-iron trioxide or/and ferrous oxide, silica, sulphur
And comprising micro copper, lead, zinc, cobalt, Jin Heyin trace meter simple substance mixture；Obtain the aqueous solution of phosphoric acid and magnesia；
The aqueous solution of phosphoric acid and magnesia is added into water dilution again, phosphoric acid quality ratio makes oxidation below 50% in making phosphate aqueous solution
Magnesium is immediately disconnected Precipitation, reclaims magnesia；The phosphoric acid,diluted aqueous solution by this mass ratio below 50%, is concentrated in vacuo dehydration again
To the phosphate aqueous solution of mass ratio 65%-70%, recycle；
Four, by the di-iron trioxide or/and ferrous oxide of above-mentioned (three), silica, sulphur and comprising micro copper, lead,
Added in zinc, cobalt, the trace meter simple substance mixture of Jin Heyin and react slight excess of hydrogen relative to silica, sulfur chemistry
Potassium oxide, and suppress potassium silicate hydrolysis, to ensure the high-purity of di-iron trioxide or/and ferrous oxide；Heating response, stirring is anti-
Should, reaction time 2-8 hours；
Reaction equation：SiO2+ 2KOH heating=K2SiO3+H2O；
3S+6KOH heating=2K2S+K2SO3+3H2O；
Obtain the aqueous solution of potassium silicate, potassium sulfide and potassium sulfite；
Simultaneously isolated di-iron trioxide or/and ferrous oxide and comprising micro copper, lead, zinc, cobalt, Jin Heyin it is micro-
Amount metal simple-substance mixture；
Five, will add enough sulfuric acid in the aqueous solution of the potassium silicate, potassium sulfide and potassium sulfite of above-mentioned (four), stirring is anti-
Should,
Reaction time 0.5-1 hours, reaction equation：
K2SiO3+H2SO4=H2SiO3+K2SO4,
K2SO3+H2SO4=H2SO3+K2SO4, H2SO3Typically with SO2Exist with water；
K2S+H2SO4=H2S+K2SO4；
Obtain the aqueous solution of silicic acid, sulfurous acid, hydrosulphuric acid, potassium sulfate, sulfurous acid H2SO3Or sulfur dioxide SO2And hydrosulphuric acid
H2Contents of the S in its aqueous solution is little；This step reaction, it is also possible to replace sulfuric acid with hydrochloric acid or nitric acid, because hydrochloric acid HL or nitre
Sour HNO3Acidity all than sulfuric acid H2SO4By force, potassium chloride or potassium nitrate and silicic acid, sulfurous acid, hydrosulphuric acid are obtained；This step reaction,
Sulfuric acid can also be replaced with the organic acid of the strong acidity such as citric acid, the acid generation of fixedness is volatile sour and weaker
Acid, heating response, and obtain its corresponding potassium salt and silicic acid, sulfurous acid, hydrosulphuric acid；This step reaction, it is also possible to use phosphoric acid
Instead of sulfuric acid, the acid of fixedness generates volatile sour and weaker acid, and heating response obtains potassium phosphate and silicic acid, Asia
Sulfuric acid, hydrosulphuric acid；
The reacting solution of above-mentioned (five) is precipitated or is separated by filtration silicic acid H by six,2SiO3Hydrate is just (original) silicic acid；
Namely the undissolved polymolecular polymer " silica sol " of water；
The aqueous solution of above-mentioned (six) is added enough copper sulphate CuSO by seven,4, stirring reaction makes hydrogen sulfide H2S reaction lifes
Into copper sulfide CuS precipitations, reaction equation：
CuSO4+H2S=CuS+H2SO4；CuS does not dissolve in dilute sulfuric acid；Precipitate or be separated by filtration copper sulfide CuS；Copper sulphate
CuSO4Do not reacted with sulfurous acid or sulfur dioxide, because weak acid can not generate strong acid；In potassium silicate, potassium sulfide and potassium sulfite
The aqueous solution with hydrochloric acid or nitric acid reaction when, CuSO here4With H2The sulfuric acid of S reaction generations, can be anti-with enough calcium hydroxide
Should, generation gypsum calcium sulfate is removed and reclaimed；Remove 2/3rds sulphur；
Or by the aqueous solution of above-mentioned (six), according to
3S+6KOH heating=2K2S+K2SO3+3H2O react and
K2SO3+H2SO4=H2SO3+K2SO4,
K2S+H2SO4=H2S+K2SO4The molecular number or mole ratio of the sulfur dioxide and hydrogen sulfide that react generation are 1: 2,
Further according to sulfur dioxide SO2With hydrosulphuric acid H2S reacts, by SO2And H2S reactions are converted into sulphur S and water, precipitate or are separated by filtration and be complete
The sulphur S in portion；Reaction equation：SO2+2H2S=3S+2H2O；In sealing container, stirring reaction or heating stirring are reacted, temperature 25
℃--100℃；Reaction time 0.5-1 hours；The present invention also can first separate sulphur S herein, reprecipitation or be separated by filtration above-mentioned (five)
In the undissolved polymolecular polymer " silica sol " of water；
Eight, are by the potassium sulfate K of above-mentioned (seven)2SO4The aqueous solution, vacuum concentration is dehydrated, pressure 25pa--100pa, time
8-24 hours, reclaim potassium sulfate K2SO4。
To save the length of specification, the embodiment of the present invention is not made the simple obvious repetition for more refining and is gone to live in the household of one's in-laws on getting married
State.
Claims (2)
1. the resource recoverying and utilizing method of pyrite cinder, which is mainly characterized in that：
One, is sulfate slag with enough water immersion pyrite cinders, and is stirred, 30 turns -50 revs/min of rotating speed, and mixing time 1-2 is small
When, the aluminum oxide in sulfate slag, calcium oxide is separately converted to hydrated alumina, calcium hydroxide, and turn into suspension emulsion, it is quiet
Put, make di-iron trioxide or/and ferrous oxide, magnesia, silica, sulphur and comprising micro copper, lead, zinc, cobalt, Jin Heyin
Trace meter simple substance mixture precipitate and separate immediately；Hydrated alumina, calcium hydroxide suspension emulsion are separated simultaneously；
Two, in hydrated alumina, the calcium hydroxide suspension emulsion of above-mentioned (one) to adding enough carbon dioxide CO2Or air,
Stirring, 50 turns -200 revs/min of rotating speed, 2-8 hour stirring reaction time, standing, make calcium hydroxide be converted into calcium carbonate and immediately
Precipitate and separate, then precipitated from hydrated alumina suspension emulsion or be separated by filtration aluminum oxide, reclaim aluminum oxide, water circulation profit
With；
Or add enough NaOH or hydroxide in hydrated alumina, the calcium hydroxide suspension emulsion to above-mentioned (one)
Potassium, heating response, makes that hydrated alumina changes into water miscible sodium aluminate or potassium aluminate is water-soluble at 1-2 hours stirring reaction time
Liquid, stands, and reprecipitation or is separated by filtration recovery calcium hydroxide；Sodium aluminate or aluminic acid aqueous solutions of potassium vacuum concentration are dehydrated,
Reclaim sodium aluminate or potassium aluminate；
Reaction equation：AL2O3+3H2O+2NaOH heating=2NaAL (OH)4,
AL2O3+3H2O+2KOH heating=2KAL (OH)4；
Or enough sulfuric acid neutralization reactions are added in hydrated alumina, the calcium hydroxide suspension emulsion to above-mentioned (one), heat
Reaction, generates water miscible aluminum sulfate aqueous solution, and vacuum concentration is dehydrated, and separates and recovers aluminum sulfate；While precipitate and separate sulphur
The gypsum calcium sulfate that acid is generated with calcium hydroxide reaction；
Three, by the di-iron trioxide or/and ferrous oxide of above-mentioned (one), magnesia, silica, sulphur and comprising micro copper,
Lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, below 28 DEG C, add enough ammonium bicarbonate aqueous solutions, and stir
Mix, 30 turns -50 revs/min of rotating speed mixing time 1-2 hours, makes magnesia be dissolved in ammonium bicarbonate aqueous solution；The oxygen of precipitate and separate three
Change two iron or/and ferrous oxide, silica, sulphur and the trace meter simple substance comprising micro copper, lead, zinc, cobalt, Jin Heyin are mixed
Compound；The aqueous solution of ammonium hydrogen carbonate and magnesia is obtained simultaneously；
Again in sealing container, by ammonium hydrogen carbonate and the aqueous solution of magnesia, 35 DEG C are heated to -- 60 DEG C, make ammonium hydrogen carbonate point
Solution, separates out magnesium oxide precipitation, reclaims magnesia；Ammonia NH is reclaimed with vacuum simultaneously3Or a hydration ammonia NH3·H2The O aqueous solution,
Again by ammonia NH below 28 DEG C in sealing container3Or a hydration ammonia NH3·H2The O aqueous solution and carbon dioxide CO2The aqueous solution is anti-
Should, ammonium bicarbonate aqueous solution is obtained, recycle；
Or with ammonium chloride or the aqueous dissolution di-iron trioxide or/and ferrous oxide, magnesia, silica, sulphur of ammonium sulfate
And comprising the magnesia in micro copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, and stir, 30 turns of rotating speed-
50 revs/min, mixing time 1-2 hours, precipitate and separate di-iron trioxide or/and ferrous oxide, silica, sulphur and comprising micro
Copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin；The aqueous solution of magnesium chloride or magnesium sulfate, vacuum are obtained simultaneously
Thickening is dried, pressure 25pa--100pa, time 8-24 hours, reclaims magnesium chloride or magnesium sulfate；And reclaim ammoniacal liquor；
Or dissolve di-iron trioxide or/and ferrous oxide, magnesia, titanium dioxide with the phosphate aqueous solution of mass ratio 65%-70%
Silicon, sulphur and comprising the magnesia in micro copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin, and stir, rotating speed
30 turns -50 revs/min, mixing time 1-2 hours, precipitate and separate di-iron trioxide or/and ferrous oxide, silica, sulphur and bag
Containing micro copper, lead, zinc, cobalt, Jin Heyin trace meter simple substance mixture；Obtain the aqueous solution of phosphoric acid and magnesia；Again will
Phosphoric acid adds water dilution with the aqueous solution of magnesia, and phosphoric acid quality ratio founds magnesia below 50% in making phosphate aqueous solution
I.e. precipitation and separation is separated out, and reclaims magnesia；The phosphoric acid,diluted aqueous solution by this mass ratio below 50%, is concentrated in vacuo dehydration to matter again
The phosphate aqueous solution than 65%-70% is measured, is recycled；
Four, by the di-iron trioxide or/and ferrous oxide of above-mentioned (three), silica, sulphur and comprising micro copper, lead, zinc,
Added in cobalt, the trace meter simple substance mixture of Jin Heyin and react slight excess of hydrogen-oxygen relative to silica, sulfur chemistry
Change sodium or potassium hydroxide, and suppress sodium metasilicate or potassium silicate hydrolysis, to ensure the high-purity of di-iron trioxide or/and ferrous oxide
Degree；Heating stirring is reacted, reaction time 2-8 hours；
Reaction equation：SiO2+ 2NaOH heating=Na2SiO3+H2O,
SiO2+ 2KOH heating=K2SiO3+H2O；
3S+6NaOH heating=2Na2S+Na2SO3+3H2O；
3S+6KOH heating=2K2S+K2SO3+3H2O；
Obtain the aqueous solution of sodium metasilicate, vulcanized sodium and sodium sulfite or potassium silicate, potassium sulfide and potassium sulfite；
Simultaneously isolated di-iron trioxide or/and ferrous oxide and comprising micro copper, lead, zinc, cobalt, Jin Heyin micro gold
Category simple substance mixture；
Five, are by the aqueous solution of the sodium metasilicate, vulcanized sodium and sodium sulfite or potassium silicate, potassium sulfide and potassium sulfite of above-mentioned (four)
The enough sulfuric acid of addition, stirring reaction,
Reaction time 0.5-1 hours, reaction equation：
Na2SiO3+H2SO4=H2SiO3+Na2SO4
K2SiO3+H2SO4=H2SiO3+K2SO4
Na2SO3+H2SO4=H2SO3+Na2SO4；H2SO3Typically with SO2Exist with water；
K2SO3+H2SO4=H2SO3+K2SO4；H2SO3Typically with SO2Exist with water；
Na2S+H2SO4=H2S+Na2SO4
K2S+H2SO4=H2S+K2SO4；
Obtain the aqueous solution of silicic acid, sulfurous acid, hydrosulphuric acid, sodium sulphate or potassium sulfate, sulfurous acid H2SO3Or sulfur dioxide SO2And hydrogen
Sulfuric acid H2Contents of the S in its aqueous solution is little；This step reaction, it is also possible to replace sulfuric acid with hydrochloric acid or nitric acid, and obtain chlorination
Sodium or sodium nitrate or potassium chloride or potassium nitrate and silicic acid, sulfurous acid, hydrosulphuric acid；This step reaction, it is also possible to replace sulphur with citric acid
Acid, heating response, and obtain its corresponding Organic Sodium Salt or sylvite and silicic acid, sulfurous acid, hydrosulphuric acid；This step reaction, it is also possible to
Replace sulfuric acid with phosphoric acid, heating response obtains sodium ascorbyl phosphate or potassium phosphate and silicic acid, sulfurous acid, hydrosulphuric acid；
6th, by the reacting solution of above-mentioned (five), precipitate or be separated by filtration silicic acid H2SiO3Hydrate is positive silicic acid；Namely water is not
The polymolecular polymer " silica sol " of dissolving；
The aqueous solution of above-mentioned (six) is added enough copper sulphate CuSO by seven,4, stirring reaction makes hydrogen sulfide H2S reaction generation sulphur
Change copper CuS precipitations, reaction equation：
CuSO4+H2S=CuS+H2SO4；Precipitate or be separated by filtration copper sulfide CuS；In sodium metasilicate, vulcanized sodium and sodium sulfite or silicon
When the aqueous solution of sour potassium, potassium sulfide and potassium sulfite is with hydrochloric acid or nitric acid reaction, CuSO here4With H2The sulfuric acid of S reaction generations,
Enough calcium hydroxide reactions, generation gypsum calcium sulfate can be used to remove and reclaim；Remove 2/3rds sulphur；
Or by the aqueous solution of above-mentioned (six), according to
3S+6NaOH heating=2Na2S+Na2SO3+3H2O,
3S+6KOH heating=2K2S+K2SO3+3H2O react and
Na2SO3+H2SO4=H2SO3+Na2SO4,
K2SO3+H2SO4=H2SO3+K2SO4,
Na2S+H2SO4=H2S+Na2SO4,
K2S+H2SO4=H2S+K2SO4The molecular number or mole ratio of the sulfur dioxide and hydrogen sulfide that react generation are 1: 2, then root
According to sulfur dioxide SO2With hydrosulphuric acid H2S reacts, by SO2And H2S reactions are converted into sulphur S and water, precipitate or are separated by filtration and be whole
Sulphur S；Reaction equation：SO2+2H2S=3S+2H2O；In sealing container, stirring reaction or heating stirring are reacted, 25 DEG C of temperature -- and 100
℃；Reaction time 0.5-1 hours；The present invention also can first separate sulphur S herein, and reprecipitation or the water that is separated by filtration in above-mentioned (five) are not
The polymolecular polymer " silica sol " of dissolving；
Eight, are by the sodium sulphate Na of above-mentioned (seven)2SO4Or potassium sulfate K2SO4The aqueous solution, vacuum concentration is dehydrated, pressure 25pa--
100pa, time 8-24 hours, reclaims sodium sulphate Na2SO4Or potassium sulfate K2SO4。
2. the resource recoverying and utilizing method of pyrite cinder according to claim 1, in above-mentioned (four), di-iron trioxide
Or/and ferrous oxide and comprising the pact also contained in micro copper, lead, zinc, cobalt, the trace meter simple substance mixture of Jin Heyin
1% iron sulfide FeS2, its separation method is：
It is that hydrogen peroxide reacts with iron sulfide with hydrogen peroxide, reaction equation：
(1).7H2O2+FeS2=6H2O+FeSO4+H2SO4；
Or (2) .15H2O2+2FeS2=14H2O+Fe2(SO4)3+H2SO4；
Hydrogen peroxide water will be diluted needed for reaction, be configured to the aqueous solution of 3%--10%；Continuous penetrating contains a small amount of iron sulfide
FeS2Di-iron trioxide or/and ferrous oxide and the trace meter simple substance comprising micro copper, lead, zinc, cobalt, Jin Heyin mixing
In thing, stirring reaction, 30 turns -50 revs/min of rotating speed after mixing time 1-2 hours, adds appropriate water, agitator treating sulfuric acid
Ferrous and sulfuric acid or ferric sulfate and sulfuric acid, 30 turns -50 revs/min of rotating speed；Separation and recovery ferrous sulfate and sulfuric acid or ferric sulfate and sulphur
Aqueous acid；Obtain di-iron trioxide or/and ferrous oxide and comprising micro copper, lead, zinc, cobalt, Jin Heyin micro gold
Belong to the mixture of simple substance.
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| CN108706562A (en) * | 2018-08-14 | 2018-10-26 | 武汉轻工大学 | A method of preparing ferric phosphate using pyrite cinder |
| CN109517996B (en) * | 2019-01-07 | 2020-08-07 | 合肥工业大学 | Process for extracting iron in sulfuric acid cinder by aid of enhanced acid leaching method |
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| CN115155620A (en) * | 2022-07-27 | 2022-10-11 | 广西民族大学 | Desulfurization composite catalyst and preparation method and application thereof |
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