CN109536716A - Gu arsenic removing method of the arsenic containing Copper Slag - Google Patents
Gu arsenic removing method of the arsenic containing Copper Slag Download PDFInfo
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- CN109536716A CN109536716A CN201811468218.4A CN201811468218A CN109536716A CN 109536716 A CN109536716 A CN 109536716A CN 201811468218 A CN201811468218 A CN 201811468218A CN 109536716 A CN109536716 A CN 109536716A
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- arsenic
- copper
- removing method
- copper slag
- containing copper
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- 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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
-
- 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
- C22B15/00—Obtaining copper
- C22B15/0063—Hydrometallurgy
- C22B15/0084—Treating solutions
- C22B15/0089—Treating solutions by chemical methods
- C22B15/0093—Treating solutions by chemical methods by gases, e.g. hydrogen or hydrogen sulfide
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
-
- 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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- Engineering & Computer Science (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention provides a kind of solid arsenic removing method of the arsenic containing Copper Slag, comprising: mixes solid arsenic in the ratio that solid-liquid mass ratio is 1:5~8 containing Copper Slag and leachate, obtains ore pulp；Sulphur dioxide reduction processing is carried out to gained ore pulp；Then it is filtered, obtains lead skim and filtrate；Gained lead skim enters smelting system and carries out melting, and gained filtrate carries out vulcanization copper-coating, obtains copper ashes and mother liquor；Gained copper ashes enters smelting system and is smelted, and arsenic oxide arsenoxide is precipitated after mother liquid obtained crystallized processing, finally carries out purification processes to the arsenic oxide arsenoxide.Solid arsenic removing method of the arsenic containing Copper Slag provided by the invention is realized from solid arsenic containing efficient dearsenification in Copper Slag, solid arsenic has effectively been recycled containing valuable metals such as copper, lead in Copper Slag, this method energy consumption is small, non-pollutant discharge, has high economic benefit and environmental benefit.
Description
Technical field
The present invention relates to metallurgical technology field, in particular to a kind of solid arsenic removing method of the arsenic containing Copper Slag.
Background technique
The setting form occurred during Copper making, it is raw with the reaction of arsenic by the way that iron powder is added under acid, oxygen pressure condition
Carry out solid arsenic at arsenic acid molysite (scorodite) precipitating being stabilized under the conditions of low acid, copper is leached to liquid phase, thus reach copper,
Arsenic is separated to purpose, and the technique is using relatively broad.Cupric, the lead of generation consolidate arsenic minerals slag containing arsenic 10.56%, cupric 9.14%,
Iron content 7.73%, leaded 15.0%.
Since the slag cupric, lead are higher, there are also very high added values, but after must carrying out dearsenification processing, could obtain
It is enriched with and is utilized with further recycling.Currently, main namely two class of wet process and Fire arsenic removal of the slag arsenic removing method, due to slag
Calorific value itself is not high, for general Fire arsenic removal, needs to configure more fuel, leads to higher cost, low efficiency,
And environmental pollution is serious inherently Fire arsenic removal the drawbacks of.As Chinese patent CN103820587B discloses one kind containing arsenic richness
The method of volatilization dearsenification in scum, wherein using the coke blacking for matching people 4%-8% in rich scum, 750 DEG C -950 DEG C of temperature,
It is passed through under the conditions of the mixed gas of vapor and air, so that the arsenic in iron ore is volatilized, this method can only handle low containing arsenic 1.4%
Arsenic minerals slag, for the slag containing arsenic 10% or more, dearsenification efficiency just seems awkward, and also very to equipment requirement
It is high.In wet method dearsenication, since the slag itself is the product for carrying out solid arsenic under acidity, oxygen pressure condition by wet processing,
So conventional acidic leaching, acts on it less.Such as it is wet to disclose a kind of high symplesite by Chinese patent CN103572041A
The method of method depth dearsenification, this method are 5.64% arsenic iron tcrude ore (FeAs to arsenic is contained2) can achieve 90% or more removing
Rate, but the solid arsenic product of cupric, lead and complicated component for generating under this acid oxygen pressure condition is helpless.Such as
Chinese patent CN107739837A discloses a kind of method of the efficient dearsenification of high arsenic smoke dust of Copper making, is soaked by secondary atmospheric alkali,
It can be by 8% arsenic-removing rate for reaching 90% containing arsenic smoke dust.It may be implemented the removing of arsenic by normal pressure, alkaline pressure of oxygen leaching, but by
Too high in sodium hydroxide cost, although can be by lime causticization recovery section lye, in addition the calcium arsenate generated be
A kind of dangerous waste, and there is presently no good methods of disposal, can only accumulate storage.
Summary of the invention
The present invention provides a kind of solid arsenic removing method of the arsenic containing Copper Slag, the purpose is to solve solid arsenic containing Copper Slag cleaning,
The problem of efficient dearsenification hardly possible.
In order to achieve the above object, technical solution provided by the invention is as follows:
A kind of solid arsenic removing method of the arsenic containing Copper Slag, includes the following steps:
1) solid arsenic is mixed containing Copper Slag and leachate in the ratio that solid-liquid mass ratio is 1:5~8, obtains ore pulp；
Wherein, the leachate is the acid solution containing arsenic, and wherein sulfuric acid concentration is 150~180g/L；
2) sulphur dioxide reduction processing is carried out to ore pulp obtained by step 1)；Then it is filtered, obtains lead skim and filtrate；
3) filtrate obtained by step 2) carries out vulcanization copper-coating, obtains copper ashes and mother liquor；
4) arsenic oxide arsenoxide is precipitated after the mother liquid obtained crystallized processing of step 3), purification processes is carried out to the arsenic oxide arsenoxide.
Further, it includes arsenic, copper, iron and lead element in Copper Slag that step 1) the solid arsenic, which contains,.
Further, step 2) the sulphur dioxide reduction processing is is passed through sulfur dioxide into ore pulp, and is stirred.
Further, the sulphur dioxide reduction processing reaction temperature is 80~90 DEG C, and the reaction time is 1.5~2h.
Further, lead skim obtained by step 2) enters lead smelting system.
Further, step 3) the vulcanization copper-coating specifically: hydrogen sulfide gas is passed through in Xiang Suoshu filtrate, often
30min detects the copper content in first-time filtrate, stops ventilation as copper content < 0.02g/L in filtrate, then be filtered processing.
Further, copper ashes obtained by step 3) enters copper metallurgy industry.
Further, crystallization treatment in step 4) specifically: centrifugal treating is carried out after mother liquor is cooled to 20~30 DEG C, point
Separate out arsenic oxide arsenoxide.
Further, crystallization treatment post mother liquor return step 1 in step 4)) it is used as leachate.
Further, the step 4) purification processes specifically: wash the arsenic oxide arsenoxide isolated, until arsenic oxide arsenoxide
Purity is up to 98% or more；
Wherein, washing gained water lotion return step 1) it is used as leachate.
Above scheme of the invention have it is following the utility model has the advantages that
(1) solid arsenic removing method of the arsenic containing Copper Slag provided by the invention, which is realized from solid arsenic, contains efficient dearsenification in Copper Slag,
The purpose for reaching safe disposal and recycling, be convert arsenic-containing material to the cleaning of arsenic product, recycling one
Effective way；
(2) separating by extraction of solid arsenic removing method of the arsenic containing Copper Slag provided by the invention is up to 85% or more, and entire technique
It shortens and mentions arsenic technological approaches, reduce energy consumption, improve economic benefit；
(3) solid arsenic removing method of the arsenic containing Copper Slag provided by the invention has effectively recycled solid arsenic containing copper, the lead in Copper Slag
Equal valuable metals, the direct yield of copper are 90% or more, and the direct yield of lead reaches 95% or more, has very high economic benefit and ring
Protect benefit；
(4) arsenic removing method of the solid arsenic containing Copper Slag provided by the invention carry out it is self-produced it is self-consuming recycle, energy consumption
It is small, economic benefit is improved, application prospect is had a vast market.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
To keep the technical problem to be solved in the present invention, technical solution and advantage clearer, below in conjunction with attached drawing and tool
Body embodiment is described in detail.
Embodiment 1
(1) take solid arsenic 100g containing Copper Slag (butt), wherein containing As10.56%, Cu9.14%, Fe7.73%,
Pb15.0%, leachate 500g (contain arsenic 12.7g/L), adjust acidity to 150g/L with the concentrated sulfuric acid.Solid arsenic containing Copper Slag and is soaked
Liquid is mixed to join in the beaker of 2L out；
(2) start electric stirring, and access gas-guide tube, be continually fed into SO2Gas is heated up to 80 DEG C, and constant temperature maintenance 1.5 is small
When, it then filters while hot, obtains lead skim and filtrate；
(3) lead skim is sent to lead smelting system, hydrogen sulfide gas is passed through into filtrate, every 30min is detected in first-time filtrate
Copper content, until in filtrate when copper content < 0.02g/L stop ventilation being filtered processing again, obtain copper ashes and mother liquor；
(4) copper ashes is sent to copper metallurgy industry, arsenic oxide arsenoxide is precipitated after the crystallized processing of mother liquor, carried out after being cooled to 20 DEG C from
Heart processing, the arsenic oxide arsenoxide being then demultiplex out washed, until arsenic oxide arsenoxide purity is up to 98% or more.Crystallized processing post mother liquor is made
It is continued to use for leachate.
The removal efficiency that sampling analysis obtains As is 85.2%, and the direct yield of copper is 91.5%, and the direct yield of lead is 96.2%.
Embodiment 2:
(1) take solid arsenic 100g containing Copper Slag (butt), wherein containing As10.56%, Cu9.14%, Fe7.73%,
Pb15.0%, leachate 600g (contain arsenic 12.7g/L), adjust acidity to 160g/L with the concentrated sulfuric acid.Solid arsenic containing Copper Slag and is soaked
Liquid is mixed to join in the beaker of 2L out；
(2) start electric stirring, and access gas-guide tube, be continually fed into SO2Gas is heated up to 85 DEG C, and constant temperature maintenance 1.6 is small
When, it then filters while hot, obtains lead skim and filtrate；
(3) lead skim is sent to lead smelting system, hydrogen sulfide gas is passed through into filtrate, every 30min is detected in first-time filtrate
Copper content, until in filtrate when copper content < 0.02g/L stop ventilation being filtered processing again, obtain copper ashes and mother liquor；
(4) copper ashes is sent to copper metallurgy industry, arsenic oxide arsenoxide is precipitated after the crystallized processing of mother liquor, carried out after being cooled to 25 DEG C from
Heart processing, the arsenic oxide arsenoxide being then demultiplex out washed, until arsenic oxide arsenoxide purity is up to 98% or more.Crystallized processing post mother liquor is made
It is continued to use for leachate.
The removal efficiency that sampling analysis obtains As is 89.5%, and the direct yield of copper is 92.1%, and the direct yield of lead is 97.2%.
Embodiment 3:
(1) take solid arsenic 100g containing Copper Slag (butt), wherein containing As10.56%, Cu9.14%, Fe7.73%,
Pb15.0%, leachate 800g (contain arsenic 12.7g/L), adjust acidity to 160g/L with the concentrated sulfuric acid.Solid arsenic containing Copper Slag and is soaked
Liquid is mixed to join in the beaker of 2L out；
(2) start electric stirring, and access gas-guide tube, be continually fed into SO2Gas is heated up to 90 DEG C, and constant temperature maintenance 1.5 is small
When, it then filters while hot, obtains lead skim and filtrate；
(3) lead skim is sent to lead smelting system, hydrogen sulfide gas is passed through into filtrate, every 30min is detected in first-time filtrate
Copper content, until in filtrate when copper content < 0.02g/L stop ventilation being filtered processing again, obtain copper ashes and mother liquor；
(4) copper ashes is sent to copper metallurgy industry, arsenic oxide arsenoxide is precipitated after the crystallized processing of mother liquor, carried out after being cooled to 30 DEG C from
Heart processing, the arsenic oxide arsenoxide being then demultiplex out washed, until arsenic oxide arsenoxide purity is up to 98% or more.Crystallized processing post mother liquor is made
It is continued to use for leachate.
The removal efficiency that sampling analysis obtains As is 93.3%, and the direct yield of copper is 92.6%, and the direct yield of lead is 97.6%.
Embodiment 4:
(1) take solid arsenic 100g containing Copper Slag (butt), wherein containing As10.56%, Cu9.14%, Fe7.73%,
Pb15.0%, leachate 800g (contain arsenic 12.7g/L), adjust acidity to 180g/L with the concentrated sulfuric acid.Solid arsenic containing Copper Slag and is soaked
Liquid is mixed to join in the beaker of 2L out；
(2) start electric stirring, and access gas-guide tube, be continually fed into SO2Gas is heated up to 90 DEG C, and constant temperature maintenance 2 is small
When, it then filters while hot, obtains lead skim and filtrate；
(3) lead skim is sent to lead smelting system, hydrogen sulfide gas is passed through into filtrate, every 30min is detected in first-time filtrate
Copper content, until in filtrate when copper content < 0.02g/L stop ventilation being filtered processing again, obtain copper ashes and mother liquor；
(4) copper ashes is sent to copper metallurgy industry, arsenic oxide arsenoxide is precipitated after the crystallized processing of mother liquor, carried out after being cooled to 30 DEG C from
Heart processing, the arsenic oxide arsenoxide being then demultiplex out washed, until arsenic oxide arsenoxide purity is up to 98% or more.Crystallized processing post mother liquor is made
It is continued to use for leachate.
The removal efficiency that sampling analysis obtains As is 95.7%, and the direct yield of copper is 93.0%, and the direct yield of lead is 98.1%.
Embodiment 5:
(1) solid arsenic minerals slag 1000Kg (butt) is taken, wherein contain As9.97%, Cu9.02%, Fe7.08%, Pb15.0%,
Circulation fluid 8000Kg (contains As10.2g/L, Cu0.89g/L), adjusts acidity to 180g/L with the concentrated sulfuric acid.Will solid arsenic containing Copper Slag with
Leachate is mixed to join in the beaker of 2L；
(2) from bottom gas-guide tube with 0.2m3/ h speed is continually fed into SO2(liquid) is heated up to 90 DEG C by steam pipe coil,
Constant temperature maintains 2 hours.It is filtered while hot with plate and frame type filter-press, obtains lead skim and filtrate；
(3) lead skim is sent to lead smelting system, hydrogen sulfide gas is passed through into filtrate, every 30min is detected in first-time filtrate
Copper content, until in filtrate when copper content < 0.02g/L stop ventilation being filtered processing again, obtain copper ashes and mother liquor；
(4) copper ashes is sent to copper metallurgy industry, arsenic oxide arsenoxide is precipitated after the crystallized processing of mother liquor, carried out after being cooled to 30 DEG C from
Heart processing, the arsenic oxide arsenoxide being then demultiplex out washed, until arsenic oxide arsenoxide purity is up to 98% or more.Crystallized processing post mother liquor is made
It is continued to use for leachate.
The removal efficiency that sampling analysis obtains As is 94.5%, and the direct yield of copper is 92.3%, and the direct yield of lead is 96.7%.
The above is a preferred embodiment of the present invention, it is noted that for those skilled in the art
For, without departing from the principles of the present invention, it can also make several improvements and retouch, these improvements and modifications
It should be regarded as protection scope of the present invention.
Claims (10)
1. a kind of solid arsenic removing method of the arsenic containing Copper Slag, which comprises the steps of:
1) solid arsenic is mixed containing Copper Slag and leachate in the ratio that solid-liquid mass ratio is 1:5~8, obtains ore pulp；
Wherein, the leachate is the acid solution containing arsenic, and wherein sulfuric acid concentration is 150~180g/L；
2) sulphur dioxide reduction processing is carried out to ore pulp obtained by step 1)；Then it is filtered, obtains lead skim and filtrate；
3) filtrate obtained by step 2) carries out vulcanization copper-coating, obtains copper ashes and mother liquor；
4) arsenic oxide arsenoxide is precipitated after the mother liquid obtained crystallized processing of step 3), purification processes is carried out to the arsenic oxide arsenoxide.
2. consolidating arsenic removing method of the arsenic containing Copper Slag according to claim 1, which is characterized in that step 1) the solid arsenic contains copper mine
It include arsenic, copper, iron and lead element in slag.
3. consolidating arsenic removing method of the arsenic containing Copper Slag according to claim 1, which is characterized in that the step 2) sulfur dioxide is also
Original place reason is stirred to be passed through sulfur dioxide into ore pulp.
4. consolidating arsenic removing method of the arsenic containing Copper Slag according to claim 3, which is characterized in that the sulphur dioxide reduction processing
Reaction temperature is 80~90 DEG C, and the reaction time is 1.5~2h.
5. consolidating arsenic removing method of the arsenic containing Copper Slag according to claim 1, which is characterized in that lead skim obtained by step 2) enters molten
Refining system.
6. consolidating arsenic removing method of the arsenic containing Copper Slag according to claim 1, which is characterized in that step 3) is described to be vulcanized at heavy copper
Reason specifically: hydrogen sulfide gas, the copper content in every 30min detection first-time filtrate, when copper in filtrate are passed through in Xiang Suoshu filtrate
Stop ventilation when content < 0.02g/L, then is filtered processing.
7. consolidating arsenic removing method of the arsenic containing Copper Slag according to claim 1, which is characterized in that copper ashes obtained by step 3) enters smelting
Refining system.
8. consolidating arsenic removing method of the arsenic containing Copper Slag according to claim 1, which is characterized in that crystallization treatment is specific in step 4)
Are as follows: centrifugal treating is carried out after mother liquor is cooled to 20~30 DEG C, isolates arsenic oxide arsenoxide.
9. consolidating arsenic removing method of the arsenic containing Copper Slag according to claim 1, which is characterized in that crystallization treatment stepmother in step 4)
Liquid return step 1) it is used as leachate.
10. consolidating arsenic removing method of the arsenic containing Copper Slag according to claim 1, which is characterized in that the step 4) purification processes
Specifically: the arsenic oxide arsenoxide isolated is washed, until arsenic oxide arsenoxide purity is up to 98% or more；
Wherein, washing gained water lotion return step 1) it is used as leachate.
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| CN201811468218.4A CN109536716A (en) | 2018-12-03 | 2018-12-03 | Gu arsenic removing method of the arsenic containing Copper Slag |
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| CN201811468218.4A CN109536716A (en) | 2018-12-03 | 2018-12-03 | Gu arsenic removing method of the arsenic containing Copper Slag |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114015879A (en) * | 2021-09-28 | 2022-02-08 | 中南大学 | Method for recovering copper by pyrogenic process of arsenic matte |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106636656A (en) * | 2016-09-19 | 2017-05-10 | 昆明理工大学 | Method for recovering valuable metal from copper smelting white smoke |
| CN107385209A (en) * | 2017-07-19 | 2017-11-24 | 中南大学 | A kind of method of white metal synthetical recovery |
-
2018
- 2018-12-03 CN CN201811468218.4A patent/CN109536716A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106636656A (en) * | 2016-09-19 | 2017-05-10 | 昆明理工大学 | Method for recovering valuable metal from copper smelting white smoke |
| CN107385209A (en) * | 2017-07-19 | 2017-11-24 | 中南大学 | A kind of method of white metal synthetical recovery |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114015879A (en) * | 2021-09-28 | 2022-02-08 | 中南大学 | Method for recovering copper by pyrogenic process of arsenic matte |
| CN114015879B (en) * | 2021-09-28 | 2022-12-06 | 中南大学 | Method for recovering copper by pyrogenic process of arsenic matte |
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Application publication date: 20190329 |