CN110093510A - A method of the comprehensively recovering valuable metal of flue dust containing arsenical copper - Google Patents
A method of the comprehensively recovering valuable metal of flue dust containing arsenical copper Download PDFInfo
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- CN110093510A CN110093510A CN201910380550.3A CN201910380550A CN110093510A CN 110093510 A CN110093510 A CN 110093510A CN 201910380550 A CN201910380550 A CN 201910380550A CN 110093510 A CN110093510 A CN 110093510A
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- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000002184 metal Substances 0.000 title claims abstract description 27
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 27
- 229910000563 Arsenical copper Inorganic materials 0.000 title 1
- 239000003500 flue dust Substances 0.000 title 1
- 238000002386 leaching Methods 0.000 claims abstract description 124
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 76
- 239000010949 copper Substances 0.000 claims abstract description 68
- 239000002893 slag Substances 0.000 claims abstract description 66
- 229910052802 copper Inorganic materials 0.000 claims abstract description 63
- 229910052785 arsenic Inorganic materials 0.000 claims abstract description 59
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims abstract description 59
- 229910052738 indium Inorganic materials 0.000 claims abstract description 56
- APFVFJFRJDLVQX-UHFFFAOYSA-N indium atom Chemical compound [In] APFVFJFRJDLVQX-UHFFFAOYSA-N 0.000 claims abstract description 56
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910052718 tin Inorganic materials 0.000 claims abstract description 42
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 34
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 33
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 33
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 33
- 239000003517 fume Substances 0.000 claims abstract description 27
- 150000002739 metals Chemical class 0.000 claims abstract description 24
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 24
- 239000011701 zinc Substances 0.000 claims abstract description 24
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000011084 recovery Methods 0.000 claims abstract description 20
- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 19
- 238000005363 electrowinning Methods 0.000 claims abstract description 17
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 12
- 239000001301 oxygen Substances 0.000 claims abstract description 12
- 239000000428 dust Substances 0.000 claims abstract description 11
- 239000000463 material Substances 0.000 claims description 18
- 239000004071 soot Substances 0.000 claims description 14
- 238000004064 recycling Methods 0.000 claims description 11
- JEMGLEPMXOIVNS-UHFFFAOYSA-N arsenic copper Chemical compound [Cu].[As] JEMGLEPMXOIVNS-UHFFFAOYSA-N 0.000 claims description 10
- 238000003723 Smelting Methods 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 7
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 claims description 5
- 229910000365 copper sulfate Inorganic materials 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 239000000779 smoke Substances 0.000 abstract description 10
- GSYZQGSEKUWOHL-UHFFFAOYSA-N arsenic calcium Chemical compound [Ca].[As] GSYZQGSEKUWOHL-UHFFFAOYSA-N 0.000 abstract description 4
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 4
- 229910052791 calcium Inorganic materials 0.000 description 4
- 239000011575 calcium Substances 0.000 description 4
- 238000001354 calcination Methods 0.000 description 3
- KTTMEOWBIWLMSE-UHFFFAOYSA-N diarsenic trioxide Chemical compound O1[As](O2)O[As]3O[As]1O[As]2O3 KTTMEOWBIWLMSE-UHFFFAOYSA-N 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000002920 hazardous waste Substances 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting 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
- 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
- C22B15/0065—Leaching or slurrying
- C22B15/0067—Leaching or slurrying with acids or salts thereof
- C22B15/0071—Leaching or slurrying with acids or salts thereof containing sulfur
-
- 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
- C22B15/0091—Treating solutions by chemical methods by cementation
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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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/20—Obtaining zinc otherwise than by distilling
- C22B19/22—Obtaining zinc otherwise than by distilling with leaching with acids
-
- 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
- C22B19/00—Obtaining zinc or zinc oxide
- C22B19/30—Obtaining zinc or zinc oxide from metallic residues or scraps
-
- 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
- C22B25/00—Obtaining tin
- C22B25/04—Obtaining tin by wet processes
-
- 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
- C22B25/00—Obtaining tin
- C22B25/06—Obtaining tin from scrap, especially tin scrap
-
- 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
-
- 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
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- 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
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25C—PROCESSES FOR THE ELECTROLYTIC PRODUCTION, RECOVERY OR REFINING OF METALS; APPARATUS THEREFOR
- C25C1/00—Electrolytic production, recovery or refining of metals by electrolysis of solutions
- C25C1/16—Electrolytic production, recovery or refining of metals by electrolysis of solutions of zinc, cadmium or mercury
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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
本发明公开了一种含砷铜烟尘综合回收有价金属的方法,包括以下步骤：低温焙烧：将含砷铜烟尘在回转窑中进行低温焙烧，焙烧时得烟尘和焙烧渣，其中烟尘为三氧化二砷，并进一步对烟尘进行收尘处理，即得高品级三氧化二砷；常压酸浸：将得到的焙烧渣采用浓度为150‑200g/L的硫酸进行浸出处理，此时获得含铜浸出液和初级浸出渣；含铜浸出液置换；初级浸出渣氧压酸浸：将初级浸出渣采用氧压酸浸法进行处理，获得含铟浸出液和含铅、锡浸出渣；含铟浸出液置换；硫酸锌溶液的电积处理；将获得的硫酸锌溶液进行电积处理，即可获得电积锌。本发明在运用的过程中有价金属直收率高、流程短且不产生砷钙渣，进而有利于进行运用。
The invention discloses a method for comprehensively recovering valuable metals from arsenic-containing copper fumes, which comprises the following steps: low-temperature roasting: performing low-temperature roasting on arsenic-containing copper fumes in a rotary kiln to obtain fumes and roasting slag, wherein the fumes are arsenic trioxide , and further carry out dust collection treatment on the smoke and dust to obtain high-grade arsenic trioxide; Atmospheric pressure acid leaching: the obtained roasted slag is leached with sulfuric acid with a concentration of 150-200g/L, and the copper-containing leaching solution and primary leaching slag are obtained at this time ; Copper-containing leaching solution replacement; primary leaching slag oxygen pressure acid leaching: the primary leaching slag is treated with oxygen pressure acid leaching to obtain indium-containing leaching solution and lead and tin-containing leaching slag; indium-containing leaching solution replacement; electrowinning of zinc sulfate solution Treatment; the obtained zinc sulfate solution is subjected to electrowinning treatment to obtain electrolytic zinc. During the application process of the present invention, the direct recovery rate of valuable metals is high, the process is short, and no arsenic-calcium slag is generated, which is beneficial to the application.
Description
技术领域technical field
本发明涉及冶金废料综合利用技术领域，尤其涉及一种含砷铜烟尘综合回收有价金属的方法。The invention relates to the technical field of comprehensive utilization of metallurgical waste, in particular to a method for comprehensively recovering valuable metals from arsenic-containing copper dust.
背景技术Background technique
铜火法熔炼过程中，精矿中砷大量挥发进入烟尘，形成含砷铜烟尘。含砷铜烟尘成分复杂，一方面含有铜、铅、锌、锡、铟等有价金属，极具回收价值；另一方面含砷量高，环境潜在性危害大，无害化和资源化利用工艺复杂。砷与烟尘中其他组分的高效分离和无害化处理，适当的有价金属提取技术是铜烟尘，是高砷铜烟尘处理的关键点和难点。During the copper fire smelting process, a large amount of arsenic in the concentrate volatilizes into the fume, forming arsenic-containing copper fume. The composition of arsenic-containing copper dust is complex. On the one hand, it contains valuable metals such as copper, lead, zinc, tin, indium, etc., which is of great recycling value; on the other hand, it contains high arsenic content, which has great potential harm to the environment. The process is complex. The efficient separation and harmless treatment of arsenic and other components in the soot, and the appropriate valuable metal extraction technology is copper fume, which is the key point and difficulty in the treatment of high-arsenic copper fume.
含砷铜烟尘的处理方法主要有火法，湿法和火法—湿法联合处理法：The treatment methods of arsenic-containing copper fume mainly include fire method, wet method and combined fire method and wet method:
1、火法是依据砷易挥发的性质，在高温下，于一定的还原气氛下，将含砷铜烟尘中的砷挥发进入烟尘，砷以低品级三氧化二砷形式回收，有价金属再采用熔融还原—造渣等方法回收。火法处理的缺点是有价金属直收率低，元素分散，三氧化二砷产品质量低。1. The fire method is based on the volatile nature of arsenic. At high temperature and in a certain reducing atmosphere, the arsenic in the arsenic-containing copper fume is volatilized into the soot. The arsenic is recovered in the form of low-grade arsenic trioxide, and the valuable metals are then smelted. — Recycling by slag making and other methods. The disadvantages of pyroprocessing are low direct recovery of valuable metals, dispersion of elements, and low quality of arsenic trioxide products.
2、湿法是以酸、碱、水等为溶剂，将含砷铜烟尘中砷锌铜铟等可溶物质浸入溶液，锡铅等留在渣中富集，砷以砷钙渣的形式除去，锌铜铟等通过分离以硫酸锌、海绵铜、富铟物料等形式回收。湿法处理的缺点是，产生大量砷钙渣危废，难以利用。火法—湿法联合处理法，是首先采用高温还原法将砷锌铟铅等富集浸入烟尘，烟尘再采用湿法浸出回收其中的有价金属。火法—湿法联合处理法的缺点是产生流程长，砷以砷钙渣的形式除去，难以综合利用。为此，我们提出了一种含砷铜烟尘综合回收有价金属的方法。2. The wet method uses acid, alkali, water, etc. as solvents to immerse soluble substances such as arsenic, zinc, copper, and indium in the arsenic-containing copper fume into the solution, tin, lead, etc. are left in the slag for enrichment, and arsenic is removed in the form of arsenic-calcium slag , Zinc, copper, indium, etc. are recovered in the form of zinc sulfate, sponge copper, and indium-rich materials through separation. The disadvantage of wet treatment is that it produces a large amount of hazardous waste of arsenic and calcium slag, which is difficult to utilize. The fire method-wet method combined treatment method is to first use the high-temperature reduction method to enrich and immerse arsenic, zinc, indium, lead, etc. into the soot, and then use the wet method to leaching the soot to recover the valuable metals. The disadvantage of the fire-wet combined treatment method is that the production process is long, and the arsenic is removed in the form of arsenic-calcium slag, which is difficult to comprehensively utilize. To this end, we propose a method for the comprehensive recovery of valuable metals from arsenic-containing copper fumes.
发明内容Contents of the invention
本发明的目的是为了解决现有技术中存在的缺点，而提出的一种含砷铜烟尘综合回收有价金属的方法。The purpose of the present invention is to solve the shortcomings in the prior art, and propose a method for comprehensive recovery of valuable metals from arsenic-containing copper fumes.
为了实现上述目的，本发明采用了如下技术方案：In order to achieve the above object, the present invention adopts the following technical solutions:
一种含砷铜烟尘综合回收有价金属的方法，包括以下步骤：A method for comprehensively recovering valuable metals from arsenic-containing copper fume, comprising the following steps:
A、低温焙烧：将含砷铜烟尘在回转窑中进行低温焙烧，并加入砷铜烟尘总质量的3％-5％的焦粉及砷铜烟尘总质量的1％-10％的氧化铜粉，焙烧时得烟尘和焙烧渣，其中烟尘为三氧化二砷，并进一步对烟尘进行收尘处理，即得高品级三氧化二砷；A. Low-temperature roasting: Low-temperature roasting of arsenic-containing copper dust in a rotary kiln, and adding coke powder of 3%-5% of the total mass of arsenic-copper fume and copper oxide powder of 1%-10% of the total mass of arsenic-copper fume , soot and roasting slag are obtained during roasting, wherein the soot is arsenic trioxide, and the dust is further dust-collected to obtain high-grade arsenic trioxide;
B、常压酸浸：将步骤A中得到的焙烧渣采用浓度为150-200g/L的硫酸进行浸出处理，并控制浸出处理持续120-180min，此时获得含铜浸出液和初级浸出渣；B, normal pressure acid leaching: the roasted slag obtained in the step A is leached by sulfuric acid with a concentration of 150-200g/L, and the leaching treatment is controlled to continue for 120-180min, at this time, the copper-containing leaching solution and the primary leaching slag are obtained;
C、含铜浸出液置换：向步骤B中的含铜浸出液中加入锌粉进行置换，此时能够得到海绵铜和硫酸锌溶液，对硫酸锌进行进一步的过滤，即可实现海绵铜的回收利用；C, replacement of copper-containing leaching solution: adding zinc powder to the copper-containing leaching solution in step B for replacement, at this time, sponge copper and zinc sulfate solution can be obtained, and zinc sulfate is further filtered to realize the recycling of sponge copper;
D、初级浸出渣氧压酸浸：将步骤B中的初级浸出渣采用氧压酸浸法进行处理，并控制浸出温度为200-220℃，硫酸浓度150-200g/L，浸出时间120-180min，此时获得含铟浸出液和含铅、锡浸出渣；D. Oxygen pressure acid leaching of primary leaching slag: process the primary leaching slag in step B by oxygen pressure acid leaching, and control the leaching temperature to 200-220°C, sulfuric acid concentration 150-200g/L, and leaching time 120-180min , at this time, the leaching solution containing indium and the leaching slag containing lead and tin are obtained;
E、含铟浸出液置换：向步骤D中获得的含铟浸出液加入锌粉进行置换，此时能够得到富铟物料和硫酸锌溶液，此时将富铟物料从硫酸锌溶液中过滤分离即可实现富铟物料的回收；E. Replacement of indium-containing leaching solution: add zinc powder to the indium-containing leaching solution obtained in step D for replacement. At this time, an indium-rich material and a zinc sulfate solution can be obtained. At this time, the indium-rich material can be filtered and separated from the zinc sulfate solution. Recycling of indium-rich materials;
F、硫酸锌溶液的电积处理；将步骤C及步骤E中获得的硫酸锌溶液进行电积处理，即可获得电积锌。F. Electrowinning treatment of zinc sulfate solution: electrowinning the zinc sulfate solution obtained in step C and step E to obtain electrowinning zinc.
进一步的，步骤A中含砷铜烟尘的成份为：砷：9％-20％、铜2％-6％、锌12％-20％、铟500-2000g/t、锡3％-8％、铅10％-20％；Further, the composition of arsenic-containing copper dust in step A is: arsenic: 9%-20%, copper 2%-6%, zinc 12%-20%, indium 500-2000g/t, tin 3%-8%, Lead 10%-20%;
进一步的，步骤A中低温焙烧时的温度为300-500℃，焙烧时间持续2-3小时并使焙烧渣中砷的含量降低至1％以下。Further, in step A, the temperature during low-temperature calcination is 300-500° C., and the calcination time lasts 2-3 hours to reduce the content of arsenic in the calcination slag to below 1%.
进一步的，步骤B中的浸出温度为85-100℃，并控制铜和锌的浸出率大于95％。Further, the leaching temperature in step B is 85-100° C., and the leaching rate of copper and zinc is controlled to be greater than 95%.
进一步的，步骤D中铟的浸出率大于99％，且含铅、锡浸出渣中的铟小于100g/t。Further, the leaching rate of indium in step D is greater than 99%, and the indium in the leaching slag containing lead and tin is less than 100g/t.
进一步的，步骤D获得的含铅、锡浸出渣中的铅、锡含量分别富集至20％-35％和10％-18％，此时铅、锡浸出渣可作为锡冶炼原料使用。Further, the contents of lead and tin in the lead-containing and tin leaching slag obtained in step D are respectively enriched to 20%-35% and 10%-18%, at this time, the lead and tin leaching slag can be used as tin smelting raw materials.
本发明提出的一种含砷铜烟尘综合回收有价金属的方法，有益效果在于：本方案通过低温挥发—湿法浸出的方法，使得砷以高品级三氧化二砷形式回收、锌以电积锌的形式回收、铜以海绵铜的形式回收、铟以富铟物料的形式回收、铅、锡以锡冶炼原料的形式回收，其中与火法处理相比：三氧化二砷产品质量高，元素不分散，有价金属直收率高；与湿法处理相比：砷以三氧化二砷产品回收，不产砷钙渣；与火法—湿法联合处理法比：流程短，有价金属直收率高；砷以三氧化二砷产品回收，不产砷钙渣，进而有利于进行运用。The present invention proposes a method for comprehensively recovering valuable metals from arsenic-containing copper fumes. The beneficial effect is that: the solution uses low-temperature volatilization-wet leaching to recover arsenic in the form of high-grade arsenic trioxide and zinc in the form of electrodeposited zinc. Recycling, copper is recovered in the form of sponge copper, indium is recovered in the form of indium-rich materials, lead and tin are recovered in the form of tin smelting raw materials, and compared with pyroprocessing: the product quality of arsenic trioxide is high, the elements are not dispersed, and the valuable metal High direct recovery rate; compared with wet treatment: arsenic is recovered as arsenic trioxide product without producing arsenic-calcium slag; compared with pyro-wet combined treatment method: short process and high direct recovery rate of valuable metals; arsenic is recovered as arsenic trioxide product Recycling does not produce arsenic and calcium slag, which is beneficial to use.
附图说明Description of drawings
图1为本发明提出的一种含砷铜烟尘综合回收有价金属的方法的工艺流程图。Fig. 1 is a process flow diagram of a method for comprehensively recovering valuable metals from arsenic-containing copper fumes proposed by the present invention.
具体实施方式Detailed ways
下面将结合本发明实施例，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention. Apparently, the described embodiments are only some of the embodiments of the present invention, not all of them. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
实施例1Example 1
参照图1，一种含砷铜烟尘综合回收有价金属的方法，包括以下步骤：With reference to Fig. 1, a kind of method for the comprehensive recovery of valuable metals of arsenic-containing copper smoke comprises the following steps:
A、低温焙烧：将成份为：砷：9％-13％、铜2-3％、锌12％-14％、铟500-1000g/t、锡3％-5％、铅10％-13％的含砷铜烟尘在回转窑中进行低温焙烧，低温焙烧时的温度为300-370℃，并加入砷铜烟尘总质量的3％的焦粉及砷铜烟尘总质量的3％的氧化铜粉，焙烧时间持续2小时；焙烧时得烟尘和焙烧渣，其中焙烧渣中砷的含量降低至1％以下，且烟尘为三氧化二砷，并进一步对烟尘进行收尘处理，即得高品级三氧化二砷；A. Low temperature roasting: the ingredients are: arsenic: 9%-13%, copper 2-3%, zinc 12%-14%, indium 500-1000g/t, tin 3%-5%, lead 10%-13% The arsenic-containing copper soot is roasted at low temperature in a rotary kiln, and the temperature during low-temperature roasting is 300-370°C, and 3% of the total mass of the arsenic-copper soot and 3% of the total mass of the arsenic-copper soot are added. Copper oxide powder , the roasting time lasts for 2 hours; smoke dust and roasting slag are obtained during roasting, wherein the content of arsenic in the roasting slag is reduced to below 1%, and the smoke dust is arsenic trioxide, and the dust is further dust-collected to obtain high-grade arsenic trioxide;
B、常压酸浸：将步骤A中得到的焙烧渣采用浓度为150-170g/L的硫酸进行浸出处理，浸出温度为85-90℃，并控制浸出处理持续120-140min，并控制铜和锌的浸出率大于95％，此时获得含铜浸出液和初级浸出渣；B, atmospheric acid leaching: the roasted slag obtained in step A is leached by sulfuric acid with a concentration of 150-170g/L, the leaching temperature is 85-90°C, and the leaching treatment is controlled to continue for 120-140min, and the copper and The leaching rate of zinc is greater than 95%, and at this time, copper-containing leaching solution and primary leaching slag are obtained;
C、含铜浸出液置换：向步骤B中的含铜浸出液中加入锌粉进行置换，此时能够得到海绵铜和硫酸锌溶液，对硫酸锌进行进一步的过滤，即可实现海绵铜的回收利用；C, replacement of copper-containing leaching solution: add zinc powder to the copper-containing leaching solution in step B for replacement, then sponge copper and zinc sulfate solution can be obtained, and zinc sulfate is further filtered to realize the recycling of sponge copper;
D、初级浸出渣氧压酸浸：将步骤B中的初级浸出渣采用氧压酸浸法进行处理，并控制浸出温度为200-210℃，硫酸浓度150-170g/L，浸出时间120-140min，此时获得含铟浸出液和含铅、锡浸出渣，铟的浸出率大于99％，且含铅、锡浸出渣中的铟小于100g/t；D. Oxygen pressure acid leaching of primary leaching slag: process the primary leaching slag in step B by oxygen pressure acid leaching, and control the leaching temperature to 200-210°C, sulfuric acid concentration 150-170g/L, and leaching time 120-140min , at this time, obtain indium-containing leaching solution and lead-containing and tin-containing leaching slag, the leaching rate of indium is greater than 99%, and the indium in the lead-containing and tin-containing leaching slag is less than 100g/t;
E、含铟浸出液置换：向步骤D中获得的含铟浸出液加入锌粉进行置换，此时能够得到富铟物料和硫酸锌溶液，此时将富铟物料从硫酸锌溶液中过滤分离即可实现富铟物料的回收，步骤D获得的含铅、锡浸出渣中的铅、锡含量分别富集至20％-25％和10％-14％，此时铅、锡浸出渣可作为锡冶炼原料使用；E. Replacement of indium-containing leaching solution: add zinc powder to the indium-containing leaching solution obtained in step D for replacement. At this time, an indium-rich material and a zinc sulfate solution can be obtained. At this time, the indium-rich material can be filtered and separated from the zinc sulfate solution. In the recovery of indium-rich materials, the contents of lead and tin in the lead-containing and tin leaching slag obtained in step D are respectively enriched to 20%-25% and 10%-14%, at this time, the lead and tin leaching slag can be used as tin smelting raw materials use;
F、硫酸锌溶液的电积处理；将步骤C及步骤E中获得的硫酸锌溶液进行电积处理，即可获得电积锌。F. Electrowinning treatment of zinc sulfate solution: electrowinning the zinc sulfate solution obtained in step C and step E to obtain electrowinning zinc.
实施例2Example 2
参照图1，一种含砷铜烟尘综合回收有价金属的方法，包括以下步骤：With reference to Fig. 1, a kind of method for the comprehensive recovery of valuable metals of arsenic-containing copper smoke comprises the following steps:
A、低温焙烧：将成份为：砷：13％-17％、铜3-5％、锌14％-17％、铟1000-1500g/t、锡5％-7％、铅13％-17％的含砷铜烟尘在回转窑中进行低温焙烧，低温焙烧时的温度为370-450℃，并加入砷铜烟尘总质量的4％的焦粉及砷铜烟尘总质量的7％的氧化铜粉，焙烧时间持续2.5小时；焙烧时得烟尘和焙烧渣，其中焙烧渣中砷的含量降低至1％以下，且烟尘为三氧化二砷，并进一步对烟尘进行收尘处理，即得高品级三氧化二砷；A. Low temperature roasting: the ingredients are: arsenic: 13%-17%, copper 3-5%, zinc 14%-17%, indium 1000-1500g/t, tin 5%-7%, lead 13%-17% The arsenic-containing copper soot is roasted at low temperature in a rotary kiln, and the temperature during low-temperature roasting is 370-450°C, and 4% of the total mass of the arsenic-copper soot and 7% of the total mass of the arsenic-copper soot are added. Copper oxide powder , the roasting time lasts for 2.5 hours; smoke dust and roasting slag are obtained during roasting, wherein the content of arsenic in the roasting slag is reduced to below 1%, and the smoke dust is arsenic trioxide, and the dust is further dust-collected to obtain high-grade arsenic trioxide;
B、常压酸浸：将步骤A中得到的焙烧渣采用浓度为170-180g/L的硫酸进行浸出处理，浸出温度为90-95℃，并控制浸出处理持续140-160min，并控制铜和锌的浸出率大于95％，此时获得含铜浸出液和初级浸出渣；B, atmospheric acid leaching: the roasted slag obtained in step A is leached by sulfuric acid with a concentration of 170-180g/L, the leaching temperature is 90-95°C, and the leaching treatment is controlled to continue for 140-160min, and the copper and The leaching rate of zinc is greater than 95%, and at this time, copper-containing leaching solution and primary leaching slag are obtained;
C、含铜浸出液置换：向步骤B中的含铜浸出液中加入锌粉进行置换，此时能够得到海绵铜和硫酸锌溶液，对硫酸锌进行进一步的过滤，即可实现海绵铜的回收利用；C, replacement of copper-containing leaching solution: adding zinc powder to the copper-containing leaching solution in step B for replacement, at this time, sponge copper and zinc sulfate solution can be obtained, and zinc sulfate is further filtered to realize the recycling of sponge copper;
D、初级浸出渣氧压酸浸：将步骤B中的初级浸出渣采用氧压酸浸法进行处理，并控制浸出温度为210-215℃，硫酸浓度170-180g/L，浸出时间140-160min，此时获得含铟浸出液和含铅、锡浸出渣，铟的浸出率大于99％，且含铅、锡浸出渣中的铟小于100g/t；D. Oxygen pressure acid leaching of primary leaching slag: process the primary leaching slag in step B by oxygen pressure acid leaching, and control the leaching temperature to 210-215°C, sulfuric acid concentration 170-180g/L, and leaching time 140-160min , at this time, obtain indium-containing leaching solution and lead-containing and tin-containing leaching slag, the leaching rate of indium is greater than 99%, and the indium in the lead-containing and tin-containing leaching slag is less than 100g/t;
E、含铟浸出液置换：向步骤D中获得的含铟浸出液加入锌粉进行置换，此时能够得到富铟物料和硫酸锌溶液，此时将富铟物料从硫酸锌溶液中过滤分离即可实现富铟物料的回收，步骤D获得的含铅、锡浸出渣中的铅、锡含量分别富集至25％-30％和14％-16％，此时铅、锡浸出渣可作为锡冶炼原料使用；E. Replacement of indium-containing leaching solution: add zinc powder to the indium-containing leaching solution obtained in step D for replacement. At this time, an indium-rich material and a zinc sulfate solution can be obtained. At this time, the indium-rich material can be filtered and separated from the zinc sulfate solution. In the recovery of indium-rich materials, the content of lead and tin in the lead-containing and tin leaching slag obtained in step D is enriched to 25%-30% and 14%-16% respectively. At this time, the lead and tin leaching slag can be used as tin smelting raw materials use;
F、硫酸锌溶液的电积处理；将步骤C及步骤E中获得的硫酸锌溶液进行电积处理，即可获得电积锌。F. Electrowinning treatment of zinc sulfate solution: electrowinning the zinc sulfate solution obtained in step C and step E to obtain electrowinning zinc.
实施例3Example 3
参照图1，一种含砷铜烟尘综合回收有价金属的方法，包括以下步骤：With reference to Fig. 1, a kind of method for the comprehensive recovery of valuable metals of arsenic-containing copper smoke comprises the following steps:
A、低温焙烧：将成份为：砷：17％-20％、铜5％-6％、锌17％-20％、铟1500-2000g/t、锡7％-8％、铅17％-20％的含砷铜烟尘在回转窑中进行低温焙烧，低温焙烧时的温度为450-500℃，并加入砷铜烟尘总质量的5％的焦粉及砷铜烟尘总质量的10％的氧化铜粉，焙烧时间持续3小时；焙烧时得烟尘和焙烧渣，其中焙烧渣中砷的含量降低至1％以下，且烟尘为三氧化二砷，并进一步对烟尘进行收尘处理，即得高品级三氧化二砷；A. Low temperature roasting: the ingredients are: arsenic: 17%-20%, copper 5%-6%, zinc 17%-20%, indium 1500-2000g/t, tin 7%-8%, lead 17%-20 % of the arsenic-containing copper dust is roasted at a low temperature in a rotary kiln, and the temperature during low-temperature roasting is 450-500°C, and 5% of the total mass of the arsenic-copper fume and 10% of the total mass of the arsenic-copper fume are added. Copper oxide powder, and the roasting time lasts for 3 hours; smoke and roasted slag are obtained during roasting, wherein the content of arsenic in the roasted slag is reduced to below 1%, and the smoke is arsenic trioxide, and the dust is further dust-collected to obtain high-grade diarsenic trioxide;
B、常压酸浸：将步骤A中得到的焙烧渣采用浓度为180-200g/L的硫酸进行浸出处理，浸出温度为95-100℃，并控制浸出处理持续160-180min，并控制铜和锌的浸出率大于95％，此时获得含铜浸出液和初级浸出渣；B, atmospheric acid leaching: the roasted slag obtained in step A is leached by sulfuric acid with a concentration of 180-200g/L, the leaching temperature is 95-100°C, and the leaching treatment is controlled to continue for 160-180min, and the copper and The leaching rate of zinc is greater than 95%, and at this time, copper-containing leaching solution and primary leaching slag are obtained;
C、含铜浸出液置换：向步骤B中的含铜浸出液中加入锌粉进行置换，此时能够得到海绵铜和硫酸锌溶液，对硫酸锌进行进一步的过滤，即可实现海绵铜的回收利用；C, replacement of copper-containing leaching solution: adding zinc powder to the copper-containing leaching solution in step B for replacement, at this time, sponge copper and zinc sulfate solution can be obtained, and zinc sulfate is further filtered to realize the recycling of sponge copper;
D、初级浸出渣氧压酸浸：将步骤B中的初级浸出渣采用氧压酸浸法进行处理，并控制浸出温度为215-220℃，硫酸浓度180-200g/L，浸出时间160-180min，此时获得含铟浸出液和含铅、锡浸出渣，铟的浸出率大于99％，且含铅、锡浸出渣中的铟小于100g/t；D. Oxygen pressure acid leaching of primary leaching slag: process the primary leaching slag in step B by oxygen pressure acid leaching, and control the leaching temperature to 215-220°C, sulfuric acid concentration 180-200g/L, and leaching time 160-180min , at this time, obtain indium-containing leaching solution and lead-containing and tin-containing leaching slag, the leaching rate of indium is greater than 99%, and the indium in the lead-containing and tin-containing leaching slag is less than 100g/t;
E、含铟浸出液置换：向步骤D中获得的含铟浸出液加入锌粉进行置换，此时能够得到富铟物料和硫酸锌溶液，此时将富铟物料从硫酸锌溶液中过滤分离即可实现富铟物料的回收，步骤D获得的含铅、锡浸出渣中的铅、锡含量分别富集至30％-35％和16％-18％，此时铅、锡浸出渣可作为锡冶炼原料使用；E. Replacement of indium-containing leaching solution: add zinc powder to the indium-containing leaching solution obtained in step D for replacement. At this time, an indium-rich material and a zinc sulfate solution can be obtained. At this time, the indium-rich material can be filtered and separated from the zinc sulfate solution. In the recovery of indium-rich materials, the contents of lead and tin in the lead-containing and tin leaching slag obtained in step D are respectively enriched to 30%-35% and 16%-18%, at this time, the lead and tin leaching slag can be used as tin smelting raw materials use;
F、硫酸锌溶液的电积处理；将步骤C及步骤E中获得的硫酸锌溶液进行电积处理，即可获得电积锌。F. Electrowinning treatment of zinc sulfate solution: electrowinning the zinc sulfate solution obtained in step C and step E to obtain electrowinning zinc.
综上所述：本发明通过低温挥发—湿法浸出的方法，使得砷以高品级三氧化二砷形式回收、锌以电积锌的形式回收、铜以海绵铜的形式回收、铟以富铟物料的形式回收、铅、锡以锡冶炼原料的形式回收，其中与火法处理相比：三氧化二砷产品质量高，元素不分散，有价金属直收率高；与湿法处理相比：砷以三氧化二砷产品回收，不产砷钙渣；与火法—湿法联合处理法比：流程短，有价金属直收率高；砷以三氧化二砷产品回收，不产砷钙渣，进而有利于进行运用。In summary: the present invention recovers arsenic in the form of high-grade arsenic trioxide, zinc in the form of electrodeposited zinc, copper in the form of sponge copper, and indium in the form of indium-rich materials through the low-temperature volatilization-wet leaching method. Recovery, lead and tin are recovered in the form of tin smelting raw materials. Compared with pyroprocessing: the product quality of diarsenic trioxide is high, the elements are not dispersed, and the direct recovery rate of valuable metals is high; compared with wet treatment: arsenic is recovered as diarsenic trioxide product , does not produce arsenic and calcium slag; compared with the pyro-wet combined treatment method: the process is shorter and the direct recovery rate of valuable metals is high; arsenic is recovered as arsenic trioxide without producing arsenic and calcium slag, which is beneficial for utilization.
以上所述，仅为本发明较佳的具体实施方式，但本发明的保护范围并不局限于此，任何熟悉本技术领域的技术人员在本发明揭露的技术范围内，根据本发明的技术方案及其发明构思加以等同替换或改变，都应涵盖在本发明的保护范围之内。The above is only a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto, any person familiar with the technical field within the technical scope disclosed in the present invention, according to the technical solution of the present invention Any equivalent replacement or change of the inventive concepts thereof shall fall within the protection scope of the present invention.
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| CN111363924A (en) * | 2020-04-17 | 2020-07-03 | 铜仁学院 | Method for treating copper-arsenic-containing filter cake |
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| CN113621813A (en) * | 2021-08-18 | 2021-11-09 | 昆明理工大学 | Method for separating and recovering copper and arsenic from zinc hydrometallurgy copper and arsenic slag |
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| CN115369252A (en) * | 2022-08-02 | 2022-11-22 | 云南铜业股份有限公司西南铜业分公司 | Treatment method of copper smelting white smoke dust |
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