CN108642288A - A kind of method that magnesian-chrome efractoy is discarded in full element recycling - Google Patents
A kind of method that magnesian-chrome efractoy is discarded in full element recycling Download PDFInfo
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- CN108642288A CN108642288A CN201810501880.9A CN201810501880A CN108642288A CN 108642288 A CN108642288 A CN 108642288A CN 201810501880 A CN201810501880 A CN 201810501880A CN 108642288 A CN108642288 A CN 108642288A
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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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/26—Magnesium halides
- C01F5/30—Chlorides
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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 that magnesian-chrome efractoy is discarded in full element recycling, include the following steps：By discarded magnesian-chrome efractoy comminution to certain fineness, material to be soaked is obtained；Material to be soaked is put into according to the liquid-solid ratio of setting in leaching agent, Leach reaction is stirred, after leaching, is filtered, obtains chromium-rich leached mud and rich magnesium leachate；Chromium-rich leached mud is washed and dried, ferrochrome mineral products are obtained, then cleaning solution is incorporated into rich magnesium leachate；The pH to 7.0~7.5 that caustic-calcined magnesite adjusts leachate is added to rich magnesium leachate, is stirred reaction, after completion of the reaction, is filtered, obtains precipitation and chlorination mother liquid of magnesium；Precipitation is washed and dried, mixed-metal compounds are obtained, then cleaning solution is incorporated into chlorination mother liquid of magnesium；Chlorination mother liquid of magnesium is evaporated crystallization, obtains magnesium chloride product.The method of the present invention is simple, and cost is relatively low, and the rate of recovery is high, realizes the full element of discarded magnesian-chrome efractoy and recycles.
Description
Technical field
The invention belongs to refractory material comprehensive reutilization fields, and in particular to a kind of complete discarded magnesium chromium matter of element recycling is resistance to
The method of fiery material.
Background technology
According to incompletely statistics, China discards magchrome refractory at 4,000,000 tons or more every year.These discarded magnesium chromium at present
Refractory material is difficult processing, and smeltery is generally in order to recycle metal, as metallurgical raw material after a small amount of refractory material is crushed
Auxiliary material is smelted, and landfill disposal is concentrated in most of refractory material stockpiling.Although processing mode cost simple in this way is smaller,
It is but to make valuable metal resource serious waste therein, it is often more important that poisonous and harmful metal therein causes environment very big
Injury, at present country environmental issue is increasingly paid attention to, it is this processing refractory material method be destined to be substituted.
Since half a century, magnesian-chrome efractoy is special because its slag resistance is good, structural stability is strong and calorific intensity is high etc.
Point has been widely used in non-ferrous metallurgy and other pyroprocess industry, and still can be with without other refractory materials
Substitution.But magnesian-chrome efractoy its short life, chemical erosion is serious, and replacement frequency is high；On the other hand, China's magnesium, chromium money
Source shortage, the raw material for producing magnesian-chrome efractoy is nervous, and especially high-grade chromite is in short supply.Therefore, how to realize useless
It is a urgent problem to be solved that magnesium, the chromium resource abandoned in magnesian-chrome efractoy, which recycle,.
Publication No. is " to recycle gold using copper smelting-furnace magnesia brick lining disclosed in the Chinese invention patent application of CN100463983C
" a kind of gold silver smelting furance waste lining brick time disclosed in the method for category " and the Chinese invention patent application that publication No. is CN100554443
The method for receiving valuable metal " is realized using the technological process of sulfuric acid de-magging-alkali leaching lead-nitric acid leaching silver-chloroazotic acid leaching gold
The separation and recycling of Mg, Pb, Ag, Au.But the leaching rate of two methods Mg is not high, and only 75% or so, still have a large amount of
Mg is not recycled effectively；The rate of recovery of Cr is very low, has only recycled a small amount of Cr being present in leachate, has had ignored and largely deposit
It is the recycling and processing of the Cr in de-magging slag；In addition the recycling of Ag, Au are concentrated on, but complex process, acid consumption is higher, pair sets
It is standby corrosion-resistant more demanding.Publication No. is that " one kind passing through gravity treatment-coal disclosed in the Chinese invention patent application of CN106269170A
The method of valuable metal in oily aggregative flotation process integration recycling waste refractory materials ", is made a kind of or few by the method for ore dressing
Several metals of number are effectively recycled, but its comprehensive resource utilization rate is not high, still has a large amount of ore dressing tailings not obtain effective profit
With.Publication No. is " a kind of discarded magchrome refractory flotation of separation disclosed in the Chinese invention patent application of CN107419102A
The method of valuable metal in tailings " is further processed magchrome refractory flotation tailings, flotation tail by the method for chloridizing volatilization
Foreign metal further removes in slag so that final tailings can be used as the raw material of production refractory material, but chlorination is waved
Hair method energy consumption is higher, and the tail gas pollution that volatilizees is serious.
Invention content
The object of the present invention is to provide a kind of simple for process, cost is relatively low, and magnesium chromium is discarded in the high full element recycling of the rate of recovery
The method of fire resistant materials.
A kind of method that magnesian-chrome efractoy is discarded in full element recycling of the present invention, includes the following steps：
1) by discarded magnesian-chrome efractoy comminution to certain fineness, material to be soaked is obtained；
2) material to be soaked in step 1) is put into according to the liquid-solid ratio of setting by HCl and MgCl2The leaching agent of composition
In, it is stirred Leach reaction, after leaching, is filtered, chromium-rich leached mud and rich magnesium leachate are obtained；
3) the chromium-rich leached mud in step 2) is washed and is dried, obtain ferrochrome mineral products, then simultaneously by cleaning solution
Enter in the rich magnesium leachate into step 2)；
4) pH to 7.0~7.5 that caustic-calcined magnesite adjusts leachate is added to the rich magnesium leachate in step 3), is stirred
Reaction, after completion of the reaction, is filtered, and precipitation and chlorination mother liquid of magnesium are obtained；
5) precipitation in step 4) is washed and is dried, obtained mixed-metal compounds, be then incorporated to cleaning solution
Into the chlorination mother liquid of magnesium in step 4)；
6) the chlorination mother liquid of magnesium in step 5) is evaporated crystallization, obtains magnesium chloride product.
In the step 1), the fineness of material to be soaked is to account for 70~80% less than 0.15mm.
In the step 2), a concentration of 5.0~5.5mol/L, MgCl of HCl in leaching agent2A concentration of 1.0~
1.5mol/L；Liquid-solid ratio is (5~6):1,75~85 DEG C, 1.0~1.5h of reaction time of Leach reaction temperature, stirring intensity 400
~500r/min.
In the step 4), it is 0.5~1.0h to be stirred to react the time.
The principle of the present invention：Magnesian-chrome efractoy is one kind in basic refractory, mainly by magnesia and chromium
Made of iron ore and using magnesia as main component, main object is mutually periclase and spinelle.Magnesium in discarded magchrome refractory
Mainly exist in the form of MgO, is easily leached in acid condition into leachate, chromium, iron are mainly with FeCr2O4Spinel structure
Form exist, in acid condition be difficult be leached and stay in leached mud, to realize chromium, iron and the separation of magnesium.
MgO (s)+2HCl (a)=MgCl2(a)+H2O(l)(353.15K,101kPa)
△ G=-13.411kJ/mol
FeCr2O4(s)+8HCl (a)=2CrCl3(a)+FeCl2(a)+4H2O(l)(353.15K,101kPa)
△ G=+104.194kJ/mol
Magchrome refractory under the hot conditions of non-ferrous metal metallurgy, penetrate into its internal foreign metal mostly with simple substance,
The form of oxide and solid solution alloy exists.The wherein simple substance of Sb, the simple substance and its oxide of Pb, Bi, the oxidation of Cu, Ag
Object is easily leached in acid condition into leachate；The AgCl generated in the simple substance of Cu, Ag and reaction high concentration cl from
Complex is formed under the conditions of son also enters leachate, MgCl in leaching agent2Effect be that improve solution chloride ion concentration, from
And promote the leaching of Cu, Ag；As is mainly with Ca3(AsO4)2Form exist, hydrochloric acid is soluble in, to realize foreign metal
With the separation of chromium.
4Sb(s)+12HCl(a)+3O2(g)=4SbCl3(a)+6H2O(l)
Pb (s)+2HCl (a)=PbCl2(a)+H2(g)
PbO (s)+2HCl (a)=PbCl2(a)+H2O(l)
4Bi(s)+12HCl(a)+3O2(g)=4BiCl3(a)+6H2O(l)
Bi2O3(s)+6HCl (a)=2BiCl3(a)+3H2O(l)
CuO (s)+2HCl (a)=CuCl2(a)+H2O(l)
Ag2O (s)+2HCl (a)=2AgCl (s)+H2O(l)
2Cu+4HCl=2H [CuCl2]+H2(g)
2Ag+4HCl=2H [AgCl2]+H2(g)
AgCl (s)+HCl (a)=H [AgCl2](a)
Ca3(AsO4)2(s)+6HCl (a)=3CaCl2(a)+2H3AsO4(a)
Magchrome refractory obtains rich magnesium leachate after Leach reaction, and foreign metal is mainly present in the form of an ion
In leachate, caustic-calcined magnesite, which is added, makes leachate pH gradually rise carry out neutralization precipitation.It is constantly increased to 7.0~7.5 in pH
In the process, Sb3+、Bi3+Ion constantly hydrolysis generates SbOCl, BiOCl precipitation, unstable [AgCl respectively2]-Coordinate ion by
Gradually resolve into AgCl precipitations, AsO4 3-Ion is with Ca3(AsO4)2、Mg3(AsO4)2Etc. forms be precipitated, Cu2+、Pb2+Ion and few
The Cr of amount3+、Fe2+、Fe3+Ion increasingly generates hydroxide precipitation, to realize the separation of foreign metal and magnesium.
Beneficial effects of the present invention：
The present invention passes through lot of experiments, it is determined that the technological process of discarded magnesian-chrome efractoy comprehensive utilization.
To the chromite products C r rate of recovery can reach 92~97%, the Fe rate of recovery and can reach 85~90%, it is true through X-ray diffraction analysis
It is FeCr to have determined its object mutually2O4, wherein Cr2O3Content >=30% can be used as the use of chemical industry grade chromite；Neutralized precipitation obtains
Metallic compound, the metals overall recovery such as Cu, Pb, Bi, Sb, Ag, As can reach 82~88%, and metal content is higher, can
It returns to smelt and further recycle；Magnesium is finally enriched in chlorination mother liquid of magnesium, and Mg leaching rates can reach 85~88%, final Mg
The rate of recovery can reach 155~165%, and MgCl can be obtained through evaporative crystallization2The technical grade magnesium chloride product of content >=45%.
The method of the present invention is simple, and cost is relatively low, realizes discarded magnesian-chrome efractoy whole element and recycles, will endanger
Dangerous waste is transformed into price product, has significant economic value and environmental benefit, while being waste refractory materials synthesis profit
With providing Technical Reference.
Description of the drawings
The process flow chart of Fig. 1 present invention.
The XRD diagram for the ferrochrome mineral products that Fig. 2 embodiment of the present invention 1 obtains.
Specific implementation mode
Embodiment 1
The raw material of use are the discarded furnace lining magnesium chromium firebricks of Hunan smeltery silver converter, wherein being containing Mg
27.58%, Cr 10.06%, Fe 6.97%, the foreign metals total content such as Cu, As, Ag, Sb, Pb, Bi are 21.89%.
It is 70~80% materials to be soaked for being less than 0.15mm at fineness to take the discarded magnesium chromium firebrick, comminution.Formulation components
For 5mol/L HCl and 1.5mol/L MgCl2Mixed solution as leaching agent.Will material be soaked by 5:1 liquid-solid ratio is added
Into leaching agent, 80 DEG C of constant temperature in waters, Leach reaction 1.5h under conditions of stirring intensity 400r/min, after Leach reaction
The obtained washing of chromium-rich leached mud, drying will be filtered, ferrochrome mineral products is obtained, cleaning solution is incorporated to rich magnesium leachate.To rich magnesium
Caustic-calcined magnesite is added in leachate, pH value of solution is gradually adjusted to 7.5, and is allowed to react 0.5h.Precipitation rear filter completely is precipitated
Washing of precipitate, drying are obtained into mixed-metal compounds with chlorination mother liquid of magnesium, cleaning solution is incorporated to chlorination mother liquid of magnesium, is steamed
Hair crystallization obtains magnesium chloride product.Three separately sampled assays of product, the results are shown in Table 1.
The ferrochrome mineral products of acquisition are subjected to XRD analysis, the results are shown in Figure 1, it will be seen from figure 1 that its is main
Characteristic absorption peak is FeCr2O4Characteristic absorption peak, miscellaneous peak is less, illustrate obtain chromite product purity it is higher, impurity compared with
Few, extract technology can effectively realize the separation of magnesium, chromium.
Table 1
As can be seen from Table 1, chromite products C r, Fe grade is respectively 28.44%, 17.97%, Cr, Fe rate of recovery point
Not Wei 94.44%, 86.11%, gained ferrochrome mineral products meet chromite chemical grade industrial requirements.Cu、As、Ag、Sb、Pb、Bi
The equal foreign metals overwhelming majority is enriched in metallic compound, and grade is higher, can return to smelting system and further recycles.
The magnesium chloride product Mg rate of recovery is that 158.74%, Mg grades are 12.16%, total grade≤0.29% of foreign metal, meets industry
Grade magnesium chloride standard.
Embodiment 2
The raw material of use are the discarded furnace lining magnesium chromium firebricks of Hunan Smelter Copper converter, wherein being containing Mg
24.92%, Cr 9.38%, Fe 6.95%, the foreign metals total content such as Cu, As, Ag, Sb, Pb, Bi are 25.26%.
It is 70~80% materials to be soaked for being less than 0.15mm at fineness to take the discarded magnesium chromium firebrick, comminution.Formulation components
For 5mol/L HCl and 1.0mol/L MgCl2Mixed solution as leaching agent.Will material be soaked by 6:1 liquid-solid ratio is added
Into leaching agent, 85 DEG C of constant temperature in waters, Leach reaction 1.0h under conditions of stirring intensity 450r/min.After Leach reaction
The obtained washing of chromium-rich leached mud, drying will be filtered, ferrochrome mineral products are obtained, cleaning solution is incorporated to rich magnesium leachate, will be added suitable
PH value of solution is gradually adjusted to 7.0 by amount caustic-calcined magnesite, and is allowed to react 1.0h.The completely rear suction filtration of precipitation obtains precipitation and magnesium chloride is female
Washing of precipitate, drying are obtained mixed-metal compounds by liquid, and cleaning solution is incorporated to chlorination mother liquid of magnesium, crystallization is evaporated and obtains
Magnesium chloride product.Three separately sampled assays of product, the results are shown in Table 2.
Table 2
As can be seen from Table 2, chromite products C r, Fe grade is respectively 26.84%, 18.67%, Cr, Fe rate of recovery point
Not Wei 95.54%, 89.79%, gained ferrochrome mineral products meet chromite chemical grade industrial requirements.Cu、As、Ag、Sb、Pb、Bi
The equal foreign metals overwhelming majority is enriched in metallic compound, and grade is higher, can return to smelting system and further recycles.
The magnesium chloride product Mg rate of recovery is that 163.97%, Mg grades are 12.38%, total grade≤0.40% of foreign metal, meets industry
Grade magnesium chloride standard.
Claims (8)
1. a kind of method that magnesian-chrome efractoy is discarded in full element recycling, includes the following steps：
1) by discarded magnesian-chrome efractoy comminution to certain fineness, material to be soaked is obtained；
2) material to be soaked in step 1) is put into according to the liquid-solid ratio of setting by HCl and MgCl2In the leaching agent of composition, into
Row leaching is reacted, and after leaching, is filtered, and chromium-rich leached mud and rich magnesium leachate are obtained；
3) the chromium-rich leached mud in step 2) is washed and is dried, obtained ferrochrome mineral products, be then incorporated into cleaning solution
In rich magnesium leachate in step 2)；
4) pH to 7.0~7.5 that caustic-calcined magnesite adjusts leachate is added to the rich magnesium leachate in step 3), is stirred anti-
It answers, after completion of the reaction, is filtered, obtain precipitation and chlorination mother liquid of magnesium；
5) precipitation in step 4) is washed and is dried, obtain mixed-metal compounds, cleaning solution is then incorporated into step
It is rapid 4) in chlorination mother liquid of magnesium in；
6) the chlorination mother liquid of magnesium in step 5) is evaporated crystallization, obtains magnesium chloride product.
2. the method that magnesian-chrome efractoy is discarded in full element recycling according to claim 1, which is characterized in that the step
It is rapid 1) in, the fineness of material to be soaked is to account for 70~80% less than 0.15mm.
3. the method that magnesian-chrome efractoy is discarded in full element recycling according to claim 1, which is characterized in that the step
It is rapid 2) in, a concentration of 5.0~5.5mol/L, MgCl of HCl in leaching agent2A concentration of 1.0~1.5mol/L.
4. the method that magnesian-chrome efractoy is discarded in full element recycling according to claim 1 or 3, which is characterized in that liquid
Gu than being (5~6):1.
5. the method that magnesian-chrome efractoy is discarded in full element recycling according to claim 1 or 3, which is characterized in that institute
It states in step 2), 75~85 DEG C of Leach reaction temperature.
6. the method that magnesian-chrome efractoy is discarded in full element recycling according to claim 1 or 3, which is characterized in that institute
It states in step 2), 1.0~1.5h of reaction time.
7. the method that magnesian-chrome efractoy is discarded in full element recycling according to claim 1 or 3, which is characterized in that institute
It states in step 2), 400~500r/min of stirring intensity.
8. the method that magnesian-chrome efractoy is discarded in full element recycling according to claim 1, which is characterized in that the step
It is rapid 4) in, be stirred to react the time be 0.5~1.0h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112080642A (en) * | 2020-09-25 | 2020-12-15 | 中南大学 | Method for comprehensively recycling desulfurized gypsum slag and waste magnesium-chromium refractory bricks through synergistic treatment |
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| JP2007284727A (en) * | 2006-04-13 | 2007-11-01 | Nippon Steel Corp | Method for recovering chromium from chromium-containing slag |
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| CN101509072A (en) * | 2009-02-18 | 2009-08-19 | 中南大学 | Method for extracting valuable metals from laterite nickel mine with hydrochloric acid full-closed circulation method |
| CA2680729A1 (en) * | 2008-09-25 | 2010-03-25 | Michel Gueguin | Thermal reduction process for the recovery of refractory metal oxides and the production of vanadium-rich iron alloys from mining residues or metallurgical wastes by-produced during the beneficiation and upgrading of titania slags |
| CN107419102A (en) * | 2017-07-19 | 2017-12-01 | 中南大学 | A kind of method for separating valuable metal in discarded magchrome refractory flotation tailings |
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2018
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| CN1085832A (en) * | 1992-10-17 | 1994-04-27 | 曾庆琳 | Chromium leaching slag treatment process |
| JP2007284727A (en) * | 2006-04-13 | 2007-11-01 | Nippon Steel Corp | Method for recovering chromium from chromium-containing slag |
| 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 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112080642A (en) * | 2020-09-25 | 2020-12-15 | 中南大学 | Method for comprehensively recycling desulfurized gypsum slag and waste magnesium-chromium refractory bricks through synergistic treatment |
| CN112080642B (en) * | 2020-09-25 | 2021-08-27 | 中南大学 | Method for comprehensively recycling desulfurized gypsum slag and waste magnesium-chromium refractory bricks through synergistic treatment |
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