CN105385853B - A kind of cupric gives up the processing method of magnesia brick - Google Patents

A kind of cupric gives up the processing method of magnesia brick Download PDF

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Publication number
CN105385853B
CN105385853B CN201510778010.2A CN201510778010A CN105385853B CN 105385853 B CN105385853 B CN 105385853B CN 201510778010 A CN201510778010 A CN 201510778010A CN 105385853 B CN105385853 B CN 105385853B
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Prior art keywords
copper
liquid
heavy copper
leachate
magnesium
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CN105385853A (en
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汪秋雨
肖珲
何强
胡意文
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Jiangxi Copper Industry Technology Research Institute Co Ltd
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Jiangxi Copper Industry Technology Research Institute Co Ltd
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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
    • C22B11/00—Obtaining noble metals
    • C22B11/04—Obtaining noble metals by wet processes
    • C22B11/042—Recovery of noble metals from waste materials
    • C22B11/044—Recovery of noble metals from waste materials from pyrometallurgical residues, e.g. from ashes, dross, flue dust, mud, skim, slag, sludge
    • 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
    • C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
    • C22B26/20—Obtaining alkaline earth metals or magnesium
    • C22B26/22—Obtaining magnesium
    • 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

Abstract

The invention belongs to non-ferrous metallurgy technology field, more particularly to a kind of cupric gives up the processing method of magnesia brick.This method specifically includes following steps：Step（1）Useless magnesia brick is leached with the acid pickle produced during Copper making, is then separated by filtration leachate and leached mud；Step（2）Precipitating reagent or reducing agent are added in cupric leachate, copper is precipitated in the form of insoluble compound or simple substance, heavy copper ashes is collected by filtration；Step（3）Leached mud and the cleaning of heavy copper ashes, drying are returned into the valuable metal such as copper metallurgy industry processing, recycling Cu, Au, Ag；Step（4）Using liquid after heavy copper as raw material, magnesium sulfate or gypsum tailings containing magnesium are prepared, recycles the magnesium in liquid after heavy copper.The treatment of wastes with processes of wastes against one another of the present invention, has the advantages that technique is simple, production cost is low, and equipment investment is few, clean environment firendly, it is easy to accomplish industrialized production.

Description

A kind of cupric gives up the processing method of magnesia brick
Technical field
The invention belongs to non-ferrous metallurgy technology field, more particularly to a kind of cupric gives up the processing method of magnesia brick.
Background technology
Domestic large-scale cupper smelting uses the thermal process of " copper matte regulus melting-the blowing refinement of the matte-refining ", pyrogenic process refining more at present Need to consume substantial amounts of magnesia fire-protecting wall during copper, metallurgy of copper furnace lining in use directly with matte and blister copper Melt contacts, inevitably occur physical-chemical reaction.Refractory material there are about 50% and is etched into smelting in use In golden slag, nubbin is handled when metallurgical furnace is repaired with useless magnesia brick, in these useless refractory brick containing substantial amounts of copper, gold, The valuable metal element such as silver, lead, arsenic, chromium, magnesium.Since content of magnesia is too high (30~80%) in useless magnesia brick, if directly added Enter smelting furnace melting, MgO easily forms MgOSiO2(or 2MgOSiO2) etc. dystectic compound, make the fusing point liter of clinker High, viscosity increase, the increase of Copper in Slag amount, so as to cause the direct yield of copper to reduce；Dystectic clinker easily forms accretion at the same time, The service life of metallurgical furnace body is seriously affected, therefore useless magnesia brick is unsuitable for recycling valuable gold therein by way of pyrometallurgical smelting Belong to element.It is owned by France in " National Hazard gives up according to national environmental protection again due to containing the toxic elements such as As, Cd, Cr in useless magnesia brick Thing " category is, it is specified that enterprise cannot without authorization shift, stacks, topple over, it is necessary to by being handled with danger waste disposal qualification concentration of enterprises, The bargain price of whole nation dangerous waste product brings great environmental protection pressure and economy generally more than 4000 yuan/ton to enterprise at present Pressure.Therefore, set out from open pit mining, environmental improvement, and maximizing the benefits, carry out the comprehensive utilization technique of useless magnesia brick Research significance is great.
The technique of the useless magnesia brick of processing at present mainly includes the method for gravity treatment, flotation, gravity-floatation combination and sulfuric acid leaching.This There are problems with for a little methods：(1) it is difficult to obtain high-grade copper concentrate at the same time and high have using the method for gravity treatment and flotation Valency metal recovery rate, the rate of recovery of copper are generally less than 90%；The content of magnesia is still higher in the concentrate sub-elected, it is difficult to straight Stove is accessed to smelt；Equipment disposably puts into big, technological process length；Floatation process needs to add a variety of organic flotation agent and collecting Agent, a large amount of flotation waste waters containing organic matter can be produced in floatation process, add wastewater treatment capacity.(2) removed using sulfuric acid leaching The magnesia of useless magnesia brick, since the content of magnesia in the magnesia brick that gives up is very high, so needing to expend substantial amounts of acid；(3) sulfuric acid soaks When going out useless magnesia brick, the cupric oxide of part can be leached into liquid phase, and current sulfuric acid leaching technique does not all return this part copper Receipts processing.
The acid waste liquids such as substantial amounts of sulfuric acid, hydrochloric acid, the purified treatment work of these acid waste liquids can be produced during Copper making Need to consume substantial amounts of alkali in skill, spent acid therein is not effectively utilized, and causes the wasting of resources, environmental pollution.
The content of the invention
To solve the above-mentioned problems, the present invention propose it is a kind of overcast, short route, clean environment firendly, resource high-efficiency recycling Cupric gives up the processing method of magnesia brick,
The technical scheme is that：A kind of cupric gives up the processing method of magnesia brick, which first gives up cupric magnesia brick The useless magnesia brick of leaching is mixed with acid pickle, is then separated by filtration leachate and leached mud；Into cupric leachate add precipitating reagent or Reducing agent, copper is precipitated in the form of insoluble compound or simple substance, heavy copper ashes is collected by filtration；Leached mud that step 1 is obtained and The valuable metal such as copper metallurgy industry processing, recycling Cu, Au, Ag is returned in heavy copper ashes cleaning, drying；Using liquid after heavy copper as raw material, system For magnesium sulfate or gypsum tailings containing magnesium, the magnesium after the heavy copper of recycling in liquid.
A kind of above-mentioned cupric gives up the processing method of magnesia brick, specifically includes following steps：
Step 1：By useless magnesia brick powder and acidity (H+Ion solubility) for 0.5mol~5.0mol acid pickle import wet method Reactive tank, controls liquid-solid ratio (L/kg) scope 5:1~20:1st, range of reaction temperature for 20 DEG C~85 DEG C, stirring reaction 0.5~ 4.5 it is small when, be separated by filtration leachate and leached mud after reaction；
Step 2：Step 1 is obtained into leachate and imports wet method reactive tank, adds precipitating reagent, control adds the leaching after precipitating reagent It is 3.0~9.0 to go out liquid PH, and lasting stirring, the copper in leachate is precipitated completely in the form of insoluble compound, acquisition is collected by filtration Heavy copper ashes；
Step 3：The heavy copper ashes that the leached mud and step 2 that step 1 is obtained obtain returns copper metallurgy industry after washing, drying Processing, wherein, the content range of copper is >=13.0% in the leached mud and heavy copper ashes, and the content range of magnesium is≤3.0%；
Step 4：Liquid adds Mg (OH) as raw material after obtaining heavy copper using step 22Or after the heavy copper of MgO controls liquid PH extremely Between 5.0~9.0, by the impurity F e in liquid after heavy copper2+、Fe3+、Al3+Removed in the form of precipitation, after purified heavy copper Liquid condensing crystallizing prepares copper sulphate；Or it is directly added into CaCO to liquid after heavy copper3With Ca (OH)2Liquid PH to 9.0 after the heavy copper of control~ 12.0 prepare gypsum tailings containing magnesium, wherein, after the heavy copper in liquid magnesium content ＜ 3.5%.
Further, the precipitating reagent includes Na2S、NaOH、Mg(OH)2、MgO、Ca(OH)2Etc. one or more therein.
Further, the step 2 can also be：
Step 2：Step 1 is obtained into leachate and imports wet method reactive tank, reducing agent is added, after control adds the precipitation of copper Leachate PH is 3.0~7.0, and lasting stirring, the copper in leachate is precipitated completely in the form of simple substance, is collected by filtration and is sunk Copper ashes；
Further, the reducing agent includes the one or more therein such as iron powder, zinc powder, aluminium powder, hydrazine hydrate, formaldehyde.
Further, the acid pickle is the mixed liquor of one or more of liquid in waste sulfuric acid, waste hydrochloric acid or waste nitric acid liquid.
Invention effect
The present invention proposes to give up the method for magnesia brick with the acid waste liquid Treatment of Copper that Copper making process produces, and realizes in acid pickle The efficient utilization of acid, solves the problems, such as that sulfuric acid leaching technique needs to consume a large amount of technical pure sulfuric acid；The present invention proposes cupric leaching Go out the method for liquid recycling copper, solve the problems, such as that copper recovery is low, realize valuable metal element high efficiente callback, average recovery rate reaches More than 95%, the average recovery rate of particularly copper reaches more than 99%；The present invention proposes that leached mud and heavy copper ashes return Copper making system The method of system processing processing, solves existing high magnesia brick treatment process because of valuable metal elements such as substep recycling Cu, Au, Ag, deposits Complex process, long flow path, big equipment investment the problem of；The present invention is with technological process is short, processing cost is low, equipment investment Less, the advantages that clean environment firendly, cupric is can be achieved with existing waste water treatment process equipment and is given up the processing that magnesia brick gives up.
From the point of view of comprehensive utilization of resources and environmental protection, this method proposes to give up magnesia brick using acid waste liquid Treatment of Copper, The treatment of wastes with processes of wastes against one another, while realize the secondary recovery of resource in the magnesia brick that makes full use of and give up sour in spent acid, reach economic benefit most Bigization and the purpose of environmental improvement, have great economic and social benefit.
Attached drawing and brief description of the drawings
Fig. 1 is the process flow chart of the inventive method.
Embodiment
The embodiment of the present invention is described further with reference to exemplary embodiment, is not therefore sent out this Bright is limited in the range of described exemplary embodiment.
Example 1
It is raw material to take the 2kg cuprics magnesia brick that gives up, and is 1.2mol/L waste sulfuric acids in concentration, liquid-solid ratio 5:1, temperature is 75 DEG C, carry out 2.5 it is small when leaching test, be collected by filtration leached mud after reaction, the content of copper is 17.09% in leached mud, magnesium Content be 1.51%；Add Mg (OH) in cupric leachate2Adjustment solution PH is settled out Cu (OH) to 5.02, wherein liquid after heavy copper The content ＜ 10mg/L of middle copper, are collected by filtration heavy copper ashes；Leached mud and heavy copper ashes are cleaned to neutrality, drying with clear water and return copper smelting The processing of refining system, recycles the valuable metal elements such as copper therein, gold, silver；Liquid adds Mg (OH) after heavy copper2Control the PH in solution To 8.0, the impurity after purification removing is heavy in liquid, condensing crystallizing prepares technical pure magnesium sulfate.Au, Ag are calculated according to result of the test The rate of recovery reach 96.4%, the rate of recovery of copper reaches 99.2%, and magnesium removal efficiency reaches 96.7% in useless magnesia brick.
Example 2
It is raw material to take the 2kg cuprics magnesia brick that gives up, and is 2.5mol/L waste sulfuric acids in concentration, liquid-solid ratio 10:1, temperature is 50 DEG C, carry out 2.0 it is small when leaching test, be collected by filtration leached mud after reaction, the content of copper is 17.93% in leached mud, magnesium Content be 1.28%；Add Na in cupric leachate2S adjusts solution PH and is settled out Cu to 4.02S, wherein copper in liquid after heavy copper Content ＜ 10mg/L, are collected by filtration heavy copper ashes；Leached mud and heavy copper ashes are cleaned to neutrality, drying with clear water and return copper metallurgy industry Processing, recycles the valuable metal elements such as copper therein, gold, silver；Liquid adds Ca (OH) after heavy copper2The PH to 9.0 in solution is controlled, Precipitation prepares gypsum tailings containing magnesium.The rate of recovery that Au, Ag are calculated according to result of the test reaches 95.9%, and the rate of recovery of copper reaches 99.4%, magnesium removal efficiency reaches 97.5% in useless magnesia brick.
Example 3
It is raw material to take the 2kg cuprics magnesia brick that gives up, and is 4.0mol/L waste sulfuric acids in concentration, liquid-solid ratio 15:1, reaction temperature For room temperature, leaching test when reaction 2.0 is small is collected by filtration leached mud after reaction, and the content of copper is in leached mud 18.37%, the content of magnesium is 0.71%；Cupric leachate adjusts solution PH to 5.5, then in plus iron powder be settled out Ni metal, After heavy copper in liquid copper content ＜ 10mg/L, heavy copper ashes is collected by filtration；Leached mud and heavy copper ashes are mixed, cleaned with clear water into Property, drying returns copper metallurgy industry processing, recycles the valuable metal elements such as copper therein, gold, silver；Liquid first adds CaCO after heavy copper3 The PH in solution is controlled to add Ca (OH) afterwards to 6.0 removing impurities2The PH to 10.0 in solution is controlled, precipitation prepares gypsum tailings containing magnesium. The rate of recovery that Au, Ag are calculated according to result of the test reaches 97.1%, and the rate of recovery of copper reaches 99.7%, and magnesium removes in the magnesia brick that gives up Rate reaches 96.9%.

Claims (4)

  1. The cupric magnesia brick that gives up first is mixed with acid pickle the useless magnesium of leaching by the processing method of magnesia brick 1. a kind of cupric gives up, the processing method Brick, is then separated by filtration leachate and leached mud；
    Precipitating reagent or reducing agent are added into cupric leachate, copper is precipitated in the form of insoluble compound or simple substance, filtering is received The heavy copper ashes of collection；Copper metallurgy industry processing is returned in the leached mud that step 1 is obtained and the cleaning of heavy copper ashes, drying, and recycling Cu, Au, Ag have Valency metal；Using liquid after heavy copper as raw material, magnesium sulfate or gypsum tailings containing magnesium are prepared, recycles the magnesium in liquid after heavy copper, its It is characterized in that, specifically includes following steps：
    Step 1：By useless magnesia brick powder and H+The acid pickle that ion solubility is 0.5mol/L ~ 5.0mol/L imports wet method reactive tank, control Liquid-solid ratio scope 5 processed:1~20:When 1 L/kg, range of reaction temperature are 20 DEG C ~ 85 DEG C, stirring reaction 0.5 ~ 4.5 is small, reaction knot Leachate and leached mud are separated by filtration after beam；
    Step 2：Step 1 is obtained into leachate and imports wet method reactive tank, adds precipitating reagent, control adds the leachate after precipitating reagent PH is 3.0 ~ 9.0, and lasting stirring, the copper in leachate is precipitated completely in the form of insoluble compound, is collected by filtration and is sunk Copper ashes；The precipitating reagent includes Na2S、NaOH、Mg(OH)2, MgO or Ca (OH)2In one or more；
    Step 3：The heavy copper ashes that the leached mud and step 2 that step 1 is obtained obtain is returned at copper metallurgy industry after washing, drying Reason, wherein, the content range of copper is >=13.0% in the leached mud and heavy copper ashes, and the content range of magnesium is≤3.0%；
    Step 4：Liquid adds Mg (OH) as raw material after obtaining heavy copper using step 22Or after the heavy copper of MgO controls liquid pH to 5.0 ~ Between 9.0, by the impurity F e in liquid after heavy copper2+、Fe3+、Al3+Removed in the form of precipitation, liquid after purified heavy copper is concentrated Crystallization prepares magnesium sulfate；Or it is directly added into CaCO to liquid after heavy copper3With Ca (OH)2Liquid pH to 9.0 ~ 12.0 makes after the heavy copper of control Standby gypsum tailings containing magnesium, wherein, after the heavy copper in liquid magnesium content ＜ 3.5%.
  2. 2. the method described in a claim 1, it is characterised in that the step 2 can also be：
    Step 2：Step 1 is obtained into leachate and imports wet method reactive tank, adds reducing agent, control adds the leaching after the precipitation of copper Liquid pH is 3.0 ~ 7.0, and lasting stirring, the copper in leachate is precipitated completely in the form of elemental copper, and the heavy copper of acquisition is collected by filtration Slag.
  3. 3. according to the method described in claim 2, it is characterized in that, the reducing agent includes iron powder, zinc powder, aluminium powder, hydrazine hydrate Or the one or more in formaldehyde.
  4. The processing method of magnesia brick 4. a kind of cupric according to claim 1 gives up, it is characterised in that acid pickle for waste sulfuric acid, The mixed liquor of one or more of liquid in waste hydrochloric acid or waste nitric acid liquid.
CN201510778010.2A 2015-11-12 2015-11-12 A kind of cupric gives up the processing method of magnesia brick Active CN105385853B (en)

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Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108330284B (en) * 2018-01-24 2019-09-17 黄冈师范学院 The method of metallic copper is recycled from copper-iron alloy
CN108913912B (en) * 2018-08-01 2020-11-13 济源职业技术学院 Device for recovering copper from waste slag generated in copper smelting
CN114835292A (en) * 2022-04-29 2022-08-02 西部矿业股份有限公司 Wastewater treatment method for recovering copper from copper hydrometallurgy tail water

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CN1948522A (en) * 2006-10-31 2007-04-18 辽宁石油化工大学 Metho of recovering valuable metal in gold silver smelting furance waste lining brick
CN101082080A (en) * 2007-07-04 2007-12-05 葫芦岛锌业股份有限公司 Method for reclaiming metal by copper smelting-furnace magnesia brick lining
CN102925705A (en) * 2012-11-28 2013-02-13 郴州市金贵银业股份有限公司 Method for recovering valuable metals from furnace blocks of silver-refining furnaces
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CN1948522A (en) * 2006-10-31 2007-04-18 辽宁石油化工大学 Metho of recovering valuable metal in gold silver smelting furance waste lining brick
CN101082080A (en) * 2007-07-04 2007-12-05 葫芦岛锌业股份有限公司 Method for reclaiming metal by copper smelting-furnace magnesia brick lining
CN102925705A (en) * 2012-11-28 2013-02-13 郴州市金贵银业股份有限公司 Method for recovering valuable metals from furnace blocks of silver-refining furnaces
CN103468969A (en) * 2013-09-22 2013-12-25 栾晓明 Method for recycling silver and gold from waste brick of smelting furnace liner

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