CN114086002A - Method for efficiently separating arsenic and antimony from high-arsenic smoke dust - Google Patents
Method for efficiently separating arsenic and antimony from high-arsenic smoke dust Download PDFInfo
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- CN114086002A CN114086002A CN202111399810.5A CN202111399810A CN114086002A CN 114086002 A CN114086002 A CN 114086002A CN 202111399810 A CN202111399810 A CN 202111399810A CN 114086002 A CN114086002 A CN 114086002A
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- arsenic
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- 229910052785 arsenic Inorganic materials 0.000 title claims abstract description 91
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 title claims abstract description 59
- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 58
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000000428 dust Substances 0.000 title claims abstract description 36
- 238000000034 method Methods 0.000 title claims abstract description 36
- 239000000779 smoke Substances 0.000 title claims abstract description 36
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000002893 slag Substances 0.000 claims abstract description 17
- 239000003546 flue gas Substances 0.000 claims abstract description 15
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000654 additive Substances 0.000 claims abstract description 12
- 230000000996 additive effect Effects 0.000 claims abstract description 12
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000000463 material Substances 0.000 claims abstract description 9
- 150000001463 antimony compounds Chemical class 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 229940058905 antimony compound for treatment of leishmaniasis and trypanosomiasis Drugs 0.000 claims abstract description 3
- 229910000410 antimony oxide Inorganic materials 0.000 claims abstract description 3
- 238000002156 mixing Methods 0.000 claims abstract description 3
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical class [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims abstract description 3
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 9
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 4
- 239000004744 fabric Substances 0.000 claims description 4
- 239000005751 Copper oxide Substances 0.000 claims description 3
- 229910000431 copper oxide Inorganic materials 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 6
- 238000003723 Smelting Methods 0.000 description 6
- 230000001698 pyrogenic effect Effects 0.000 description 4
- DLISVFCFLGSHAB-UHFFFAOYSA-N antimony arsenic Chemical compound [As].[Sb] DLISVFCFLGSHAB-UHFFFAOYSA-N 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 238000002386 leaching Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000005070 sampling Methods 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- GSYZQGSEKUWOHL-UHFFFAOYSA-N arsenic calcium Chemical compound [Ca].[As] GSYZQGSEKUWOHL-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910000967 As alloy Inorganic materials 0.000 description 1
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 1
- 235000011941 Tilia x europaea Nutrition 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003818 cinder Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 239000004571 lime Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- ZODDGFAZWTZOSI-UHFFFAOYSA-N nitric acid;sulfuric acid Chemical compound O[N+]([O-])=O.OS(O)(=O)=O ZODDGFAZWTZOSI-UHFFFAOYSA-N 0.000 description 1
- 238000009856 non-ferrous metallurgy Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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Classifications
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G28/00—Compounds of arsenic
- C01G28/005—Oxides; Hydroxides; Oxyacids
-
- 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
- C22B30/02—Obtaining antimony
-
- 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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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
A method for efficiently separating arsenic and antimony in high-arsenic smoke dust comprises the following steps: antimony fixation: adding a solid additive into the high-arsenic smoke dust, uniformly mixing, roasting at 300-500 ℃ for 2-6 hours to convert low-valence antimony oxides in the high-arsenic smoke dust into high-valence antimony compounds which are difficult to volatilize, and roasting the generated As2O3Collecting flue gas, and obtaining As after the reaction is finished2O3The temperature of the product and the arsenic-rich and antimony-rich roasting slag is continuously raised to 500-750 ℃ for roasting reaction for 3-6 h, and volatilized As is treated in the process2O3Collecting flue gas, and obtaining As after the reaction is finished2O3Products and secondary materials containing antimony. The invention obtains high-grade As2O3The product, antimony is enriched in the slag, and the effective separation of arsenic and antimony is better realized. The method is simple to operate, easy to realize industrialization and good in application prospect.
Description
Technical Field
The invention belongs to the technical field of non-ferrous metallurgy environmental protection and comprehensive resource recycling, and particularly relates to a method for efficiently separating arsenic and antimony from high-arsenic smoke dust.
Background
Arsenic is a harmful element which pollutes the environment and is also a harmful element in the nonferrous smelting process, often coexists with various nonferrous metal ores, and enters smoke dust in the nonferrous smelting process to form high-arsenic smoke dust. In recent years, along with the expansion of production and capacity expansion of various large nonferrous smelting enterprises, high-grade mineral resources are gradually exhausted, the exploitation and utilization of complex polymetallic minerals and arsenic-containing minerals are increased, a large amount of arsenic, antimony and the like are brought into a production flow, and a large amount of high-arsenic antimony-containing smoke dust is produced. In order to comprehensively recycle valuable metals in the high-arsenic smoke dust and reduce the pollution to the environment, a method for efficiently separating arsenic and antimony is developed, and the problem of arsenic open circuit can be effectively solved.
With the strictness of the national environmental protection policy on the disposal of arsenic-containing materials, the disposal of arsenic-containing hazardous waste materials becomes a technical problem for non-ferrous smelting enterprises. The current open-circuit mode of arsenic mainly comprises the preparation of high-grade metal arsenic and As2O3Arsenic series chemical products, arsenic alloys and the like. However, arsenic and antimony are inThe non-ferrous smelting smoke dust is often present in a form of accompanying, and how to effectively separate arsenic and antimony in the smoke dust to obtain As2O3The product becomes the key to solve the arsenic open circuit problem.
The common arsenic-antimony separation methods at present mainly comprise a pyrogenic process and a wet process. The main treatment means of the pyrogenic process is a vacuum distillation method and a high-temperature volatilization method, both of which utilize the difference of the saturated vapor pressure of the arsenic-antimony compound to realize the effective separation of arsenic and antimony, but the pyrogenic process has higher economic cost, is difficult to popularize and apply industrially and has strict requirements on environmental protection safety measures. The wet process mainly comprises acid leaching, alkali leaching, hydrogen peroxide oxidation and the like, wherein the acid leaching mainly adopts a sulfuric acid-nitric acid system, arsenic is removed in the form of arsenic-calcium slag by adding a certain amount of lime milk after arsenic is oxidized, and the produced arsenic-calcium slag also belongs to 'dangerous waste' slag with high arsenic content and can enter a slag yard for stockpiling after being further treated.
Disclosure of Invention
The invention mainly aims at the problems and the defects of the existing arsenic-antimony separation technical means, and provides a method for efficiently separating arsenic and antimony from high-arsenic smoke dust by a pyrogenic process.
The technical scheme adopted by the invention is as follows.
A method for efficiently separating arsenic and antimony in high-arsenic smoke dust comprises the following steps:
(1) antimony fixation: adding a solid additive into the high-arsenic smoke dust, uniformly mixing, roasting at 300-500 ℃ for 2-6 hours to convert low-valence antimony oxides in the high-arsenic smoke dust into high-valence antimony compounds which are difficult to volatilize, and roasting the generated As2O3Collecting flue gas, and obtaining As after the reaction is finished2O3Products and arsenic-containing antimony-rich roasting residues; the arsenic content in the high-arsenic smoke dust is 30-70 wt.%, and the antimony content is 0.3-1.8 wt.%; the solid additive is MnO2A composite additive in an amount of 30 to 70 wt.%; the addition amount of the additive is 20-40 wt% of the high-arsenic smoke dust;
(2) and (4) volatilizing arsenic: continuously heating the arsenic-containing antimony-rich roasting slag obtained in the step (1) to 500-750 ℃ for roasting reaction for 3-6 h, wherein the volatilized arsenic-containing antimony-rich roasting slag is subjected to roasting reaction in the processAs2O3Collecting flue gas, and obtaining As after the reaction is finished2O3Products and secondary materials containing antimony.
The composite additive is industrial MnO2And one or more of potassium permanganate, copper oxide and hydrogen peroxide.
The volatilized As in the step (1) and the step (2)2O3The flue gas is collected by a cloth bag and a settling chamber.
The invention makes full use of As in low temperature2O3The characteristic that the volatile high-valence antimony compound is difficult to volatilize is that under the action of the high-activity additive, the low-valence antimony in the high-arsenic smoke dust is selectively oxidized into the difficult-to-volatilize high-valence antimony compound, and then the arsenic is further volatilized, so that the high-grade As is obtained2O3The product, antimony is enriched in the slag, and the effective separation of arsenic and antimony is better realized. The method is simple to operate, easy to realize industrialization and good in application prospect.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
As shown in figure 1, the method for efficiently separating arsenic and antimony from high-arsenic smoke dust comprises the following steps:
(1) antimony fixation: 10kg of high-arsenic smoke (with an arsenic content of 63.76% and an antimony content of 0.776%) and 3kg of technical MnO2(MnO270 wt.%), placing in a muffle furnace for roasting at 380 deg.C, reacting for 3h, in which process As is2O3In the flue gas, a cloth bag is adopted to collect dust to As2O3Collecting the flue gas to obtain As2O3Product (As)2O3The content is more than or equal to 99 percent), and arsenic-rich and antimony-rich roasting slag (also called arsenic-removing slag) is obtained after the reaction is finished. Antimony is enriched in the slag, and effective separation of arsenic and antimony is realized.
(2) And (4) volatilizing arsenic: baking arsenic-containing antimony-richThe temperature of the cinder is continuously raised to 650 ℃ in a muffle furnace for reaction for 6h, and the volatilized As is treated in the process2O3Collecting the flue gas by using a cloth bag to collect dust continuously, and obtaining As after the reaction is finished2O3Product (As)2O3Content is more than or equal to 99%) and antimony-containing secondary material. The antimony-containing secondary material can be used as an antimony smelting raw material.
Sampling and detecting prove that after the high-arsenic smoke dust is treated by the process, the volatilization rate of arsenic is about 87 percent, and the arsenic is effectively recovered. The antimony volatility was only 4%.
Example 2
The method for efficiently separating arsenic and antimony from high-arsenic smoke dust comprises the following steps:
(1) antimony fixation: 10kg of high-arsenic smoke (containing 69.73% of arsenic and 0.36% of antimony) and 3kg of industrial MnO21kg of copper oxide (MnO)230 wt.%), placing in a muffle furnace for roasting at 500 deg.C, reacting for 2h, and reacting on As in the process2O3Collecting the flue gas to obtain As2O3Product (As)2O3The content is more than or equal to 99 percent), and arsenic-rich and antimony-rich roasting slag is obtained after the reaction is finished.
(2) And (4) volatilizing arsenic: continuously heating the arsenic-rich and antimony-rich roasting slag to 750 ℃ for reaction for 3 hours, and reacting volatilized As in the process2O3Collecting flue gas, and obtaining As after the reaction is finished2O3Product (As)2O3Content is more than or equal to 99%) and antimony-containing secondary material.
Sampling and detecting prove that after the high-arsenic smoke dust is treated by the process, the arsenic volatilization rate is about 86 percent, and the antimony volatilization rate is about 0.4 percent.
Example 3
The method for efficiently separating arsenic and antimony from high-arsenic smoke dust comprises the following steps:
(1) antimony fixation: 10kg of high-arsenic smoke (containing 31.69% of arsenic and 1.68% of antimony) and 1kg of industrial MnO20.5kg of potassium permanganate and 0.5kg of hydrogen peroxide (MnO)230 wt.%), placing in a muffle furnace for roasting at 300 deg.C for 6h, and reacting on As in the process2O3Collecting the flue gas to obtain As2O3Product (As)2O3The content is more than or equal to 99 percent), and arsenic-rich and antimony-rich roasting slag is obtained after the reaction is finished.
(2) And (4) volatilizing arsenic: the obtained arsenic-rich and antimony-rich roasting slag is continuously heated to 500 ℃ to react for 4 hours, and volatilized As is treated in the process2O3Collecting flue gas, and obtaining As after the reaction is finished2O3Product (As)2O3Content is more than or equal to 99%) and antimony-containing secondary material.
Sampling and detecting prove that after the high-arsenic smoke dust is treated by the process, the volatilization rate of arsenic is about 87 percent, and the volatilization rate of antimony is 0.
The above description is only a few examples of the present invention, and is not intended to limit the present invention. It is to be understood that the present invention is not limited to the above-described embodiments, and various changes and modifications may be made without departing from the scope of the present invention.
Claims (3)
1. A method for efficiently separating arsenic and antimony in high-arsenic smoke dust is characterized by comprising the following steps:
(1) antimony fixation: adding a solid additive into the high-arsenic smoke dust, uniformly mixing, roasting at 300-500 ℃ for 2-6 hours to convert low-valence antimony oxides in the high-arsenic smoke dust into high-valence antimony compounds which are difficult to volatilize, and roasting the generated As2O3Collecting flue gas, and obtaining As after the reaction is finished2O3Products and arsenic-containing antimony-rich roasting residues; the content of arsenic in the high-arsenic smoke dust is 30-70 wt%, and the content of antimony in the high-arsenic smoke dust is 0.3-1.8 wt%; the solid additive is MnO2A composite additive in an amount of 30 to 70 wt.%; the addition amount of the additive is 20-40 wt% of the high-arsenic smoke dust;
(2) and (4) volatilizing arsenic: continuously heating the arsenic-containing antimony-rich roasting slag obtained in the step (1) to 500-750 ℃ for roasting reaction for 3-6 h, wherein the volatilized As is treated in the process2O3Collecting flue gas, and obtaining As after the reaction is finished2O3Products and secondary materials containing antimony.
2. The method for efficiently separating arsenic and antimony in high-arsenic smoke dust according to claim 1, wherein the composite additive is industrial MnO2And one or more of potassium permanganate, copper oxide and hydrogen peroxide.
3. The method for efficiently separating arsenic and antimony from high-arsenic smoke dust according to claim 1 or 2, wherein the As volatilized in the step (1) and the step (2) is collected by using a cloth bag for dust collection2O3Flue gas.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5110353A (en) * | 1987-08-25 | 1992-05-05 | Asarco Incorporated | Process for the recovery and separation of arsenic from antimony |
| CN103602834A (en) * | 2013-11-07 | 2014-02-26 | 昆明理工大学 | Selective oxidation-reduction method for recycling arsenic and antimony from arsenic-antimony smoke |
| CN104789786A (en) * | 2015-04-01 | 2015-07-22 | 郴州雄风环保科技有限公司 | Method for harmlessly treating arsenic-containing waste slag and comprehensively recycling valuable metals in arsenic-containing waste slag |
| US20160237523A1 (en) * | 2013-10-02 | 2016-08-18 | Outotec (Finland) Oy | Method and plant for removing arsenic and/or antimony from flue dusts |
| CN106381396A (en) * | 2016-09-13 | 2017-02-08 | 昆明理工大学 | Method for separating arsenic from antimony as well as recovering antimony through roasting of high arsenic-antimony smoke by solid oxidant |
| CN106702170A (en) * | 2016-12-16 | 2017-05-24 | 昆明理工大学 | Method for separating arsenic and recycling arsenic and antimony through high-arsenic-antimony smoke oxidization-fixation method |
-
2021
- 2021-11-24 CN CN202111399810.5A patent/CN114086002A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5110353A (en) * | 1987-08-25 | 1992-05-05 | Asarco Incorporated | Process for the recovery and separation of arsenic from antimony |
| US20160237523A1 (en) * | 2013-10-02 | 2016-08-18 | Outotec (Finland) Oy | Method and plant for removing arsenic and/or antimony from flue dusts |
| CN103602834A (en) * | 2013-11-07 | 2014-02-26 | 昆明理工大学 | Selective oxidation-reduction method for recycling arsenic and antimony from arsenic-antimony smoke |
| CN104789786A (en) * | 2015-04-01 | 2015-07-22 | 郴州雄风环保科技有限公司 | Method for harmlessly treating arsenic-containing waste slag and comprehensively recycling valuable metals in arsenic-containing waste slag |
| CN106381396A (en) * | 2016-09-13 | 2017-02-08 | 昆明理工大学 | Method for separating arsenic from antimony as well as recovering antimony through roasting of high arsenic-antimony smoke by solid oxidant |
| CN106702170A (en) * | 2016-12-16 | 2017-05-24 | 昆明理工大学 | Method for separating arsenic and recycling arsenic and antimony through high-arsenic-antimony smoke oxidization-fixation method |
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