CN106222413A - A kind of method of indium strip liquor removing arsenic antimony - Google Patents
A kind of method of indium strip liquor removing arsenic antimony Download PDFInfo
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- CN106222413A CN106222413A CN201610689619.7A CN201610689619A CN106222413A CN 106222413 A CN106222413 A CN 106222413A CN 201610689619 A CN201610689619 A CN 201610689619A CN 106222413 A CN106222413 A CN 106222413A
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- strip liquor
- arsenic
- indium
- antimony
- indium strip
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Metallurgy (AREA)
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- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
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- Inorganic Compounds Of Heavy Metals (AREA)
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Abstract
The method that the present invention relates to a kind of indium strip liquor removing arsenic antimony, regulates acidity including (1)；(2) add ferrous sulfate heptahydrate and hydrogen peroxide, make ferrous sulfate react with the arsenic in indium strip liquor, antimony ion and generate precipitation；(3) steps such as remaining acid are neutralized in solution.The present invention utilizes hydrogen peroxide as ferrous oxidising for ferric iron in indium strip liquor of oxidant, and the trivalent arsenic in indium strip liquor is oxidized to pentavalent arsenic, ferric iron in indium strip liquor is reacted with pentavalent arsenic and generates stable ferrum arsenic co-precipitation thing, hydrogen peroxide as catalyst make ferrous oxidising for ferric iron and with the arsenic in indium strip liquor, antimony ion 45 100 DEG C i.e. react generation precipitation, arsenic antimony removal efficiency be more than 85%.It is co-precipitated remove impurity arsenic antimony than conventional iron arsenic antimony, decreases the consumption of ferrous sulfate, reduce reaction temperature, saved cost.Precipitating rich arsenic antimony slag crystal structure out is good, it is easy to clarifies, filter and separates.
Description
Technical field
The method that the present invention relates to a kind of indium strip liquor removing arsenic antimony.
Background technology
Indium is a kind of meltable dissipated metal of silvery white.Matter is soft, can use fingernail indentation.Ductility is good, without adding during pressure processing
Work hardening phenomenon, can roll into very thin sheet material.Indium self has cold weld, supply indium block to be coated with grease.The chemical of indium
Matter is similar to ferrum.The most oxidizable, red heat can be burnt, and can be dissolved in mineral acid.Not yet find the independent mineral deposit of indium, it with
Trace association is in the mineral such as zinc, stannum.When its content reach 100,000/several, just have commercial production to be worth, be presently mainly from sudden strain of a muscle
Zinc ore extracts.It addition, the waste residue produced from zinc, lead and stannum, the most recyclable indium flue dust.The recovery method of indium is main at present
Have: extraction, reducing process, membrane separation process etc..With having the generation of arsenic, antimony during extraction recovery indium, directly affects
The quality of sponge indium, but conventional iron arsenic antimony co-precipitation remove impurity arsenic antimony, the consumption of ferrous sulfate heptahydrate is very big, and reaction temperature is relatively
Height, relatively costly, and the ferrum arsenic antimony co-precipitation thing stability generated is the highest, arsenic antimony removal efficiency is relatively low.
Summary of the invention
For the deficiencies in the prior art, it is an object of the invention to provide a kind of ferrous sulfate heptahydrate consumption little, reaction temperature
Ferrum arsenic antimony co-precipitation thing stability low, that generate is high, the method for the indium strip liquor removing arsenic antimony that arsenic antimony removal efficiency is high.
For achieving the above object, the present invention provides techniques below scheme:
The method of a kind of indium strip liquor removing arsenic antimony, it is characterised in that comprise the following steps:
(1) in the indium strip liquor containing As1-3g/l, Sb0.5-5g/l, add acid, regulate acidity, control pH=3-5；
(2) add ferrous sulfate heptahydrate and the hydrogen peroxide of 20-50g of 20-100g at every liter of indium strip liquor, make ferrous iron in acid
Property, react under oxidizing atmosphere generation precipitation with the arsenic in indium strip liquor, antimony ion, control solution temperature and be 45-100 DEG C,
Insulation reaction 10-65min；
(3), after reaction terminates, in indium strip liquor, add nertralizer, neutralize remaining acid in solution, control pH=4-6；
(4) solution that step (3) obtains is filtered, if filtrate As ＜ 0.4g/L, Sb ＜ 0.2g/L are then qualified, by it
Send follow-up indium reclaiming clean remove impurity to process, such as filtrate As ＞ 0.4g/L, Sb ＞ 0.2g/L, then to its repeat step (1)-
(3) until qualified.
Preferably, the acid in described step (1) is one or more in hydrochloric acid, sulphuric acid, perchloric acid.
Preferably, described step (2) first should add ferrous sulfate heptahydrate in indium strip liquor and stir 5-15 minute, then add
Enter hydrogen peroxide stirring reaction.
Preferably, the hydrogen peroxide in described step (2) is as ferrous oxidising for trivalent in indium strip liquor of oxidant
Ferrum, and the trivalent arsenic in indium strip liquor is oxidized to pentavalent arsenic so that the ferric iron in indium strip liquor reacts with pentavalent arsenic
Generate ferrum arsenic co-precipitation thing.
Preferably, the hydrogen peroxide in described step (2) as catalyst make ferrous oxidising for ferric iron and with indium back extraction
Arsenic, antimony ion in liquid precipitate the 45-100 DEG C of generation that i.e. reacts.
Preferably, the nertralizer in described step (3) is Caustic soda, and the addition of Caustic soda is that every liter of indium strip liquor adds 5-
The Caustic soda of 50g.
Above-mentioned steps (2) first adds in indium strip liquor ferrous sulfate heptahydrate and forms seven water sulphuric acid Asias of adsorbable impurity
Ferrum colloid, ferrous sulfate heptahydrate colloid can adsorb a small amount of arsenic antimony in indium strip liquor in advance, add hydrogen peroxide afterwards, now
Hydrogen peroxide serves not only as ferrous oxidising for ferric iron by indium strip liquor of oxidant, and by the trivalent arsenic oxygen in indium strip liquor
Turn to pentavalent arsenic, and the hydrogen peroxide added also becomes catalyst so that the ferric iron in indium strip liquor occurs with pentavalent arsenic
Can react at a temperature of relatively low and generate stable ferrum arsenic co-precipitation thing, hydrogen peroxide plays the effect of oxidant and catalyst.
Above-mentioned steps (3) adds nertralizer and not only acts as the effect of remaining acid in indium strip liquor that neutralizes, the most also may be used
So that the iron ion of free state is combined generation ferric hydroxide colloid with hydroxyl, the ferric hydroxide colloid of generation can enter again one
The impurity such as the arsenic antimony in step absorption indium strip liquor.
Indium strip liquor is filtered in (4) by above-mentioned steps, can be by the seven water sulphuric acid having adsorbed arsenic antimony in indium strip liquor
Ferrous colloid, ferrum arsenic co-precipitation thing separate with indium strip liquor, the arsenic antimony being effectively reduced in indium strip liquor.
It is an advantage of the current invention that and utilize hydrogen peroxide as ferrous oxidising for trivalent in indium strip liquor of oxidant
Ferrum, and the trivalent arsenic in indium strip liquor is oxidized to pentavalent arsenic so that the ferric iron in indium strip liquor reacts with pentavalent arsenic
Generating stable ferrum arsenic co-precipitation thing, hydrogen peroxide makes ferrous sulfate heptahydrate and the arsenic in indium strip liquor, antimony ion as catalyst
The 45-100 DEG C of generation precipitation that i.e. reacts, arsenic antimony removal efficiency is more than 85%.It is co-precipitated remove impurity arsenic antimony than conventional iron arsenic antimony,
Decrease the consumption of ferrous sulfate, reduce reaction temperature, saved cost.Precipitating rich arsenic antimony slag crystal structure out is good,
It is prone to clarification, filters and separate.
Detailed description of the invention
The following examples can help those skilled in the art that the present invention is more fully understood, but cannot be with any
Mode limits the present invention.
Embodiment 1
The method of a kind of indium strip liquor removing arsenic antimony, it is characterised in that comprise the following steps:
(1) during certain extraction recovery indium, the indium strip liquor of output is mainly composed of: In53g/L, As1g/L, Sb0.5g/L,
HCl95g/L.Take its 1L, sulfuric acid system, control pH=3；
(2) the first ferrous sulfate heptahydrate at indium strip liquor addition 20g stirs 5 minutes, then adds the dioxygen of 20g at indium strip liquor
Water, makes ferrous iron generate the generation that reacts of ferric iron and the arsenic in indium strip liquor, antimony ion under acid, oxidizing atmosphere heavy
Forming sediment, controlling solution temperature is 45 DEG C, insulation reaction 10min；
(3) after reaction terminates, adding nertralizer Caustic soda in indium strip liquor, every liter of indium strip liquor adds in the Caustic soda of 5g and solution
In remaining acid, control pH=4；
(4) solution that step (3) obtains is filtered, sampled chemical examination, containing In68g/L, As0.08g/L, Sb0.05g/L,
Then follow-up indium reclaiming clean remove impurity is sent to process.Being computed, in indium strip liquor, the removal efficiency of arsenic is 92.00%, taking off of antimony
Except rate is 90.00%, removal efficiency is both greater than 85%.
Embodiment 2
The method of a kind of indium strip liquor removing arsenic antimony, it is characterised in that comprise the following steps:
(1) during certain extraction recovery indium, the indium strip liquor of output is mainly composed of: In53g/L, As3g/L, Sb5g/L,
HCl95g/L.Take its 1L, hydrochloric acid system, control pH=5；
(2) the first ferrous sulfate heptahydrate at indium strip liquor addition 100g stirs 15 minutes, then adds the dioxygen of 50g at indium strip liquor
Water, makes ferrous iron generate the generation that reacts of ferric iron and the arsenic in indium strip liquor, antimony ion under acid, oxidizing atmosphere heavy
Forming sediment, controlling solution temperature is 100 DEG C, insulation reaction 65min；
(3), after reaction terminates, in indium strip liquor, nertralizer Caustic soda is added, with molten in the Caustic soda of every liter of indium strip liquor addition 50g
Remaining acid in liquid, controls pH=6；
(4) solution that step (3) obtains is filtered, sampled chemical examination, containing In65g/L, As0.12g/L, Sb0.10g/L,
Then follow-up indium reclaiming clean remove impurity is sent to process.Being computed, in indium strip liquor, the removal efficiency of arsenic is 96.00%, taking off of antimony
Except rate is 98.00%, removal efficiency is both greater than 85%.
Embodiment 3
The method of a kind of indium strip liquor removing arsenic antimony, it is characterised in that comprise the following steps:
(1) during certain extraction recovery indium, the indium strip liquor of output is mainly composed of: In53g/L, As1.5g/L, Sb2.5g/
L, HCl95g/L.Take its 1L, perchloric acid system, control pH=4；
(2) the first ferrous sulfate heptahydrate at indium strip liquor addition 50g stirs 10 minutes, then adds the dioxygen of 35g at indium strip liquor
Water, makes ferrous iron generate the generation that reacts of ferric iron and the arsenic in indium strip liquor, antimony ion under acid, oxidizing atmosphere heavy
Forming sediment, controlling solution temperature is 75 DEG C, insulation reaction 35min；
(3), after reaction terminates, in indium strip liquor, nertralizer Caustic soda is added, with molten in the Caustic soda of every liter of indium strip liquor addition 35g
Remaining acid in liquid, controls pH=5；
(4) solution that step (3) obtains is filtered, sampled chemical examination, containing In67g/L, As0.11g/L, Sb0.12g/L,
Then follow-up indium reclaiming clean remove impurity is sent to process.Being computed, in indium strip liquor, the removal efficiency of arsenic is 92.67%, taking off of antimony
Except rate is 95.20%, removal efficiency is both greater than 85%.
Comparative example 1
Compared with Example 1, comparative example 1 first hydrogen peroxide at indium strip liquor addition 20g in step (2) stirs 5 minutes, then
Indium strip liquor add 20g ferrous sulfate heptahydrate, control solution temperature be 45 DEG C, insulation reaction 10min, remaining step all with
Embodiment 1 is identical.
The present invention chooses and is mainly composed of: the indium strip liquor of In53g/L, As1.5g/L, Sb2.5g/L, HCl95g/L 50 parts
For object of study, every part of 1L.Being below 5 groups of indium strip liquor removing arsenic antimony tests, often group 10 parts, is contrast test: wherein A, B, C
Group uses the method for the indium strip liquor removing arsenic antimony in embodiment 1-3 respectively, and D group uses the indium strip liquor removing in comparative example 1
The method of arsenic antimony, E group uses the method for conventional iron arsenic antimony co-precipitation remove impurity arsenic antimony, result such as table 1.
Table 1
| Packet | The removal efficiency (%) of arsenic | The removal efficiency (%) of antimony | Ferrous sulfate heptahydrate consumption (g) | Reaction temperature (DEG C) |
| A | 92.12 | 91.00 | 20 | 45 |
| B | 96.34 | 98.17 | 100 | 100 |
| C | 93.09 | 95.41 | 50 | 75 |
| D | 84.11 | 82.35 | 20 | 45 |
| E | 81.26 | 80.58 | 135 | 145 |
It is not difficult to find out from the above and is co-precipitated remove impurity arsenic antimony than conventional iron arsenic antimony, the indium strip liquor removing arsenic that the present invention provides
The method of antimony decreases the consumption of ferrous sulfate, reduces reaction temperature, has saved cost.
Although, the present invention is described in detail the most with a general description of the specific embodiments, but
On the basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Cause
This, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to the scope of protection of present invention.
Claims (6)
1. the method for an indium strip liquor removing arsenic antimony, it is characterised in that comprise the following steps:
(1) in the indium strip liquor containing As1-3g/l, Sb0.5-5g/l, add acid, regulate acidity, control pH=3-5；
(2) add ferrous sulfate heptahydrate and the hydrogen peroxide of 20-50g of 20-100g at every liter of indium strip liquor, make ferrous iron in acid
Property, react under oxidizing atmosphere generation precipitation with the arsenic in indium strip liquor, antimony ion, control solution temperature and be 45-100 DEG C,
Insulation reaction 10-65min；
(3), after reaction terminates, in indium strip liquor, add nertralizer, neutralize remaining acid in solution, control pH=4-6；
(4) solution that step (3) obtains is filtered, if filtrate As ＜ 0.4g/L, Sb ＜ 0.2g/L are then qualified, by it
Send follow-up indium reclaiming clean remove impurity to process, such as filtrate As ＞ 0.4g/L, Sb ＞ 0.2g/L, then to its repeat step (1)-
(3) until qualified.
The method of a kind of indium strip liquor removing arsenic antimony, it is characterised in that the acid in step (1) is salt
One or more in acid, sulphuric acid, perchloric acid.
The method of a kind of indium strip liquor removing arsenic antimony, it is characterised in that should be first at indium in step (2)
Strip liquor adds ferrous sulfate heptahydrate stir 5-15 minute, add hydrogen peroxide stirring reaction.
The method of a kind of indium strip liquor removing arsenic antimony, it is characterised in that the hydrogen peroxide in step (2)
As ferrous oxidising for ferric iron in indium strip liquor of oxidant, and the trivalent arsenic in indium strip liquor is oxidized to pentavalent
Arsenic so that the ferric iron in indium strip liquor and pentavalent arsenic react and generate ferrum arsenic co-precipitation thing.
The method of a kind of indium strip liquor removing arsenic antimony, it is characterised in that the hydrogen peroxide in step (2)
As catalyst make ferrous oxidising for ferric iron and with the arsenic in indium strip liquor, antimony ion the 45-100 DEG C of life that i.e. reacts
Become precipitation.
The method of a kind of indium strip liquor removing arsenic antimony, it is characterised in that the nertralizer in step (3)
Being Caustic soda, the addition of Caustic soda is the Caustic soda that every liter of indium strip liquor adds 5-50g.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106282609A (en) * | 2016-08-29 | 2017-01-04 | 南丹县南方有色金属有限责任公司 | A kind of method of indium strip liquor removing arsenic antimony |
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| CN106282609A (en) * | 2016-08-29 | 2017-01-04 | 南丹县南方有色金属有限责任公司 | A kind of method of indium strip liquor removing arsenic antimony |
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Application publication date: 20161214 |