CN107739837B - A kind of method of the efficient dearsenification of the high arsenic smoke dust of Copper making - Google Patents
A kind of method of the efficient dearsenification of the high arsenic smoke dust of Copper making Download PDFInfo
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- CN107739837B CN107739837B CN201711055859.2A CN201711055859A CN107739837B CN 107739837 B CN107739837 B CN 107739837B CN 201711055859 A CN201711055859 A CN 201711055859A CN 107739837 B CN107739837 B CN 107739837B
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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
- C22B7/02—Working-up flue dust
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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
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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
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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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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Abstract
The invention discloses a kind of methods of the efficient dearsenification of the high arsenic smoke dust of Copper making, include the following steps: A, arsenic-containing smoke dust is carried out to the leaching of level-one normal pressure alkali, leaching condition are as follows: leached using secondary leachate, control NaOH concentration 40g/L-60g/L；Separation of solid and liquid obtains a leachate and a leached mud；B, a leached mud obtained by step A carries out the leaching of secondary atmospheric alkali, leaching condition are as follows: NaOH concentration 60-80g/L；Separation of solid and liquid obtains secondary leachate and secondary leached mud；C, by a leachate lime causticization obtained by step A, separation of solid and liquid obtains liquid after calcium arsenate and causticization.The present invention is suitable for the processing for the high arsenic-containing smoke dust that Copper making process generates, and arsenic-containing smoke dust dearsenification and valuable element comprehensive reutilization may be implemented, and has the advantages that environmental protection, economic, energy conservation, resource utilization are high.
Description
Technical field
The invention belongs to smelting field of nonferrous metal, and in particular to the method for efficient dearsenification from Copper making cigarette ash.
Background technique
In nature, arsenic is usually with mispickel (FeAsS), arsenic magnetic iron ore (FeAsS2), symplesite (FeAs2), sulphur arsenical copper
Mine (Cu3AsS3), realgar (As2S3), orpiment (As2S3) etc. mineral, be enriched in the non-ferrous metals such as copper, lead, zinc, nickel, cobalt, gold and silver
In ore；In Nonferrous Metallurgical Process, many high arsenic solid materials of output, such as roasting and melting flue dust.These materials are high containing arsenic
Up to 5-50%, also contain a large amount of valuable metal, directly returns and smelt process, lead to the circulative accumulation of arsenic in systems, therefore,
It usually should individually handle dearsenification.About 20000 yuan/ton of open circuit cost of arsenic during Copper making will be led if raw material is high containing arsenic
It causes Copper making anode plate arsenic exceeded, is electrolysed the overload operation of net liquid workshop, arsenic disposes the problems such as difficult, costly, develops arsenic in smelting
It is also inevitable choice that low-cost high-efficiency open circuit in refining systematic procedure, which is trend,.
The flue dust that copper metallurgy industry generates daily is up to 6-8% containing arsenic, and in order to recycle the valuable metals such as copper, the flue dust is general
Directly return to smelting furnace melting.It vouches and learns through arsenic process, which accounts for the total arsenic input amount of smelting furnace
50%, if removing not in time, accumulation of the arsenic in system certainly will be will cause.
The method of processing arsenic-containing smoke dust is mainly two classes at present, first is that fire concentrate, second is that wet separation.Pyrogenic process production
In, mainly using the difference of the oxide of arsenic and other elements oxide boiling point, separate arsenic with other elements.
CN103602835A discloses a kind of displacement reduction method and obtains crude arsenic and needle antimony, and CN103602834A discloses a kind of selective oxygen
Change-reduction obtains the not high As of purity2O3And needle antimony, CN104294053A disclose a kind of side of arsenic-containing smoke dust reduction volatilization arsenic
Method obtains As2O3Purity reaches 97.0% or more.But if containing the metal (such as antimony) close with arsenic element property in flue dust,
The arsenic trioxide purity then obtained is not high.Mainly there are water logging, acidleach, alkali to soak three kinds of techniques, but can only in wet production
The products such as purity not high arsenic trioxide, natrium arsenicum are obtained, and the recycling of valuable metal powder is not made further research.
CN105567983A discloses a kind for the treatment of process of Copper making flue dust water logging-alkali leaching, separates arsenic with metal, the arsenic of preparation produces
Product are at a discount, still higher containing arsenic in leached mud.CN104357668A discloses a kind of waste acid leaching flue dust, electrodeposition dearsenification, acid
Leaching and electrolytic deposition process are easy to produce arsenic hydride.CN105648226A and CN105648227A discloses a kind of oxygen pressure alkali leaching realization arsenic
The method of antimony separation, more thoroughly, but the natrium arsenicum obtained in process is untreated, the valuable gold such as tellurium, antimony for the ratio of arsenic antimony separation
Belong to unrecovered.
There are many dearsenification, the research paper for extracting valuable metal and related patents report from flue dust, but there are valuable elements
Comprehensive recovery is low, and arsenic product market is limited, and there are potential security risks.Therefore, the existing technology has yet to be improved and developed.
Summary of the invention
In view of the deficiencies of the prior art, the present invention is intended to provide a kind of method of the efficient dearsenification of the high arsenic smoke dust of Copper making, is fitted
For the processing for the high arsenic-containing smoke dust that Copper making process generates, arsenic-containing smoke dust dearsenification and valuable element synthetical recovery benefit may be implemented
With having the advantages that environmental protection, economic, energy conservation, resource utilization are high.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of method of the efficient dearsenification of high arsenic smoke dust of Copper making, includes the following steps:
A, arsenic-containing smoke dust is subjected to the leaching of level-one normal pressure alkali, leaching condition are as follows: leached, controlled using secondary leachate
NaOH concentration 40g/L-60g/L；Separation of solid and liquid obtains a leachate and a leached mud；
B, a leached mud obtained by step A carries out the leaching of secondary atmospheric alkali, leaching condition are as follows: NaOH concentration 60-80g/L；Gu
The isolated secondary leachate of liquid and secondary leached mud；
C, by a leachate lime causticization obtained by step A, separation of solid and liquid obtains liquid after calcium arsenate and causticization.
It should be noted that by copper weld pool system is returned after secondary leached mud drying obtained by step B；It is secondary obtained by step B
Leachate is returned to be soaked for level-one normal pressure alkali；Liquid is returned after causticization obtained by step C soaks for secondary atmospheric alkali；Arsenic obtained by step C
Stockpiling after sour calcium is cured.
It should be noted that in step A, leaching condition further include: liquid-solid ratio 3-8:1, temperature: 50 DEG C -90 DEG C, the time
1h-3h。
It should be noted that in step B, leaching condition further include: liquid-solid ratio 5-10:1, -90 DEG C of temperature 60 C, the time
0.5h-2h。
It should be noted that in step C, causticization condition are as follows: with Ca (OH)2Make caustic, the molar ratio by Ca and As is
2-6:1 addition, causticization time are 1h-4h hours, and reaction temperature is 50 DEG C -90 DEG C.
The beneficial effects of the present invention are:
(1) using under the conditions of specific NaOH concentration (pH value), the different leaching characteristic of the elements such as arsenic and copper, lead, zinc, head
It is secondary to propose to control specific whole alkali concentration using second adverse current alkali leaching processing Copper making arsenic-containing smoke dust, realize the efficient leaching of arsenic, and
Effectively inhibit the leaching of the elements such as copper, lead, zinc.
(2) causticization is carried out to alkali immersion liquid, by controlling whole alkali concentration, the operating conditions such as arsenic calcium ratio and heavy arsenic temperature are realized
The generation of the heavy arsenic process products calcium arsenate object of causticization, improves arsenic rate of deposition and arsenic accumulation rate, while promoting the regeneration of NaOH, drops
Low reagent cost.
The present invention realizes the purpose that arsenic is effectively removed from height smelting smoke dust containing arsenical copper, simple process, and reagent consumption saves,
Circulative accumulation of the arsenic in copper metallurgy industry is effectively reduced, business economic and environmental benefit are improved.Process flow is simple, arsenic abjection
Rate effectively reduces As in the cyclic cumulants of system, saves duplication of production cost 90% or more；Using alkali leaching-causticization work
Skill makes alkali regeneration, medicament less investment；And arsenic is made efficiently to open a way with metastable arsenic acid calcium speciation, environmental benefit is obvious.
Detailed description of the invention
Fig. 1 is the flow diagram of the embodiment of the present invention.
Specific embodiment
Below with reference to attached drawing, the invention will be further described, it should be noted that following embodiment is with this technology
Premised on scheme, the detailed implementation method and specific operation process are given, but protection scope of the present invention is not limited to this
Embodiment.
As shown in Figure 1, the process route of the present embodiment is that " two-stage countercurrent leaching arsenic -- leachate causticization regenerates lye and sinks
Shallow lake arsenic -- leached mud returns to melting and recycles copper ", technique mainly includes alkali leaching and causticization.
The embodiment of two-stage countercurrent alkali caustic dip leaching is carried out to arsenic-containing smoke dust are as follows: press NaOH concentration 40g/L-60g/L, liquid is solid
Than 3-8:1, temperature: 50 DEG C -90 DEG C, time 1h-3h condition carries out level-one leaching；Leached mud in liquid-solid ratio 5-10:1,
- 90 DEG C of temperature 60 C, second level leaching is carried out under the conditions of time 0.5h-2h by NaOH concentration 60-80g/L.Two-stage countercurrent, which leaches, to be utilized
The dissolution Leaching Rule difference of the metals such as arsenic and copper, lead, zinc under the conditions of low alkalinity, while leaching arsenic, inhibit copper, lead,
The leaching of the valuable metals such as zinc, realization arsenic and valuable metal efficiently separate.Arsenic leaching solution presses mole mass ratio n into causticizing tank
(Ca): n (As)=2-6:1 adds white lime into alkali immersion liquid, and reaction certain time is sufficiently stirred under specific temperature, and rich arsenic is severe
Slugging open circuit stockpiling, causticization liquid return to alkali leaching.
Embodiment 1:
Cu:20.05%, As:7.38%, Pb:3.04%, Zn:3.86% in handled copper arsenic-containing smoke dust in the present embodiment
Treatment process, effect are as follows:
(1) arsenic-containing smoke dust is carried out level-one normal pressure alkali to soak, NaOH concentration 50g/L, liquid-solid ratio 5:1, temperature: 80 DEG C, the time
2h.Cu:22.78%, As:2.93%, Pb:3.46%, Zn:4.39% in leached mud.
(2) leached mud is subjected to the leaching of secondary atmospheric alkali, liquid-solid ratio 7:1, NaOH concentration 70g/L, 85 DEG C of temperature, the time
1h.Cu:31.79%, As:1.07%, Pb:4.41%, Zn:5.85% in secondary leached mud；Arsenic, copper, lead, zinc leaching rate be
Respectively 90.9%, 0.1%, 8.6% and 4.5%.
(3) leachate of gained carries out causticization, n (Ca): n (As)=3:1, and the causticization time is 2h hours, reaction temperature
It is 70 DEG C.Arsenic rate of deposition is 98.1%, liquid alkaline concentration 48.5g/L after causticization, and alkali regeneration rate is 97%.
Embodiment 2:
Cu:20.05%, As:7.38%, Pb:3.04%, Zn:3.86% in handled copper arsenic-containing smoke dust in the present embodiment
Treatment process, effect are as follows:
(1) arsenic-containing smoke dust is carried out level-one normal pressure alkali to soak, NaOH concentration 40g/L, liquid-solid ratio 8:1, temperature: 90 DEG C, the time
1h.Cu:22.28%, As:3.25%, Pb:3.21%, Zn:4.10% in leached mud.
(2) leached mud is subjected to the leaching of secondary atmospheric alkali, liquid-solid ratio 5:1, NaOH concentration 80g/L, temperature 60 C, time
2h.Cu:31.53%, As:1.11%, Pb:4.35%, Zn:5.61% in secondary leached mud；The leaching rate of arsenic, copper, lead and zinc
To be respectively 90.5%, 0.9%, 9.8% and 8.4%.
(3) leachate of gained carries out causticization, n (Ca): n (As)=2:1, and the causticization time is 4h hours, reaction temperature
It is 90 DEG C.Arsenic rate of deposition is 97.5%, liquid alkaline concentration 34.8g/L after causticization, and alkali regeneration rate is 87%.
Embodiment 3:
Cu:20.05%, As:7.38%, Pb:3.04%, Zn:3.86% in handled copper arsenic-containing smoke dust in the present embodiment
Treatment process, effect are as follows:
(1) arsenic-containing smoke dust is carried out level-one normal pressure alkali to soak, NaOH concentration 60g/L, liquid-solid ratio 3:1, temperature: 50 DEG C, the time
3h.Cu:25.04%, As:3.15%, Pb:3.49%, Zn:4.48% in leached mud.
(2) leached mud is subjected to the leaching of secondary atmospheric alkali, liquid-solid ratio 10:1, NaOH concentration 60g/L, 90 DEG C of temperature, when
Between 0.5h.Cu:32.02%, As:1.20%, Pb:4.47%, Zn:5.71% in secondary leached mud；The leaching of arsenic, copper, lead and zinc
Extracting rate is respectively 90.2%, 0.2%, 8.1% and 7.5%.
(3) leachate of gained carries out causticization, n (Ca): n (As)=6:1, and the causticization time is 1h hours, reaction temperature
It is 50 DEG C.Arsenic rate of deposition is 97.2%, liquid alkaline concentration 50.9g/L after causticization, and alkali regeneration rate is 84.8%.
Embodiment 4:
Cu:15.77%, As:8.20%, Pb:5.36%, Zn:4.01% in handled copper arsenic-containing smoke dust in the present embodiment,
Treatment process, effect are as follows:
(1) arsenic-containing smoke dust is carried out level-one normal pressure alkali to soak, NaOH concentration 50g/L, liquid-solid ratio 5:1, temperature: 80 DEG C, the time
2h.Cu:17.51%, As:2.73%, Pb:5.52%, Zn:4.38% in leached mud.
(2) leached mud is subjected to the leaching of secondary atmospheric alkali, liquid-solid ratio 7:1, NaOH concentration 70g/L, 85 DEG C of temperature, the time
1h.Cu:23.96%, As:1.10%, Pb:7.51%, Zn:5.76% in secondary leached mud；Arsenic, copper, lead, zinc leaching rate be
Respectively 91.2%, 0.2%, 7.9% and 5.6%.
(3) leachate of gained carries out causticization, n (Ca): n (As)=3:1, and the causticization time is 2h hours, reaction temperature
It is 70 DEG C.Arsenic rate of deposition is 98.5%, liquid alkaline concentration 49.2g/L after causticization, and alkali regeneration rate is 98.4%.
Wherein basicity is the principal element for guaranteeing arsenic and separating with valuable metal in the leaching of adverse current alkali, is lower than above-mentioned basicity lower limit
When, arsenic leaches not exclusively, and separating effect is bad, and when being higher than the above-mentioned basicity upper limit, the Elements Leachings rate such as copper, lead, zinc increases, valuable
Metal loss is big, and OH excessive when causticization-It can be adsorbed into calcium arsenate, influence alkali regeneration.
Table 1 show the Contrast on effect of each embodiment.
Table 1
For those skilled in the art, it can be provided various corresponding according to above technical solution and design
Change and modification, and all these change and modification, should be construed as being included within the scope of protection of the claims of the present invention.
Claims (2)
1. a kind of method of the efficient dearsenification of high arsenic smoke dust of Copper making, characterized by the following steps:
A, arsenic-containing smoke dust is subjected to the leaching of level-one normal pressure alkali, leaching condition are as follows: NaOH concentration 40g/L-60g/L, liquid-solid ratio 3-8:1,
Temperature: 50 DEG C -90 DEG C, time 1h-3h；Separation of solid and liquid obtains a leachate and a leached mud；
B, a leached mud obtained by step A carries out the leaching of secondary atmospheric alkali, leaching condition are as follows: liquid-solid ratio 5-10:1, NaOH concentration 60-
80g/L, -90 DEG C of temperature 60 C, time 0.5h-2h；Separation of solid and liquid obtains secondary leachate and secondary leached mud；The secondary leaching of gained
Liquid is returned out soaks for level-one normal pressure alkali；Copper weld pool system is returned after the secondary leached mud of gained is dry；
C, by a leachate lime causticization obtained by step A, separation of solid and liquid obtains liquid after calcium arsenate and causticization, liquid after gained causticization
It returns and is soaked for secondary atmospheric alkali；Stockpiling after gained calcium arsenate is cured.
2. the method for the efficient dearsenification of the high arsenic smoke dust of Copper making according to claim 1, it is characterised in that: in step C, causticization
Condition are as follows: with Ca (OH)2Make caustic, be 2-6:1 addition by the molar ratio of Ca and As, the causticization time is 1h-4h hours, reaction
Temperature is 50 DEG C -90 DEG C.
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| CN108998677A (en) * | 2018-08-28 | 2018-12-14 | 郴州丰越环保科技有限公司 | A kind of method of wet-treating high arsenic smoke dust containing indium |
| CN112553469B (en) * | 2021-02-26 | 2021-05-11 | 中国科学院过程工程研究所 | Method for separating vanadium, tungsten and arsenic from sodium hydroxide waste liquid and application |
| CN113444886B (en) * | 2021-07-21 | 2022-12-06 | 东北大学 | Valuable element leaching and recycling method for copper smelting smoke dust |
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