CN104718027A - A method for improving selectivity and recovery in the flotation of nickel sulphide ores that contain pyrhotite by exploiting the synergy of multiple depressants - Google Patents

A method for improving selectivity and recovery in the flotation of nickel sulphide ores that contain pyrhotite by exploiting the synergy of multiple depressants Download PDF

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CN104718027A
CN104718027A CN201380030461.7A CN201380030461A CN104718027A CN 104718027 A CN104718027 A CN 104718027A CN 201380030461 A CN201380030461 A CN 201380030461A CN 104718027 A CN104718027 A CN 104718027A
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sulfide
ore
deta
flotation
methods according
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CN104718027B (en
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J·董
M·徐
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Vale SA
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/01—Organic compounds containing nitrogen
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/002—Inorganic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/016—Macromolecular compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/018—Mixtures of inorganic and organic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/02—Froth-flotation processes
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/004—Organic compounds
    • B03D1/012—Organic compounds containing sulfur
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/06—Depressants
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00—Specified materials treated by the flotation agents; specified applications
    • B03D2203/02—Ores
    • 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)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

A method of using the synergy of multiple depressants to improve the depression of iron sulphide without compromising the recovery of the valuable sulphide minerals in the flotation of non-ferrous metal sulphides, while reducing or eliminating the use of environmentally problematic chemicals such as polyamines. The method has significant economic and environmental benefits. The multiple depressants comprise at least one organic polymer, at least one sulphur-containing compound and/or at least one nitrogen-containing organic compound.

Description

In the flotation of the nickel sulfide ores containing magnetic iron ore, selective and method that the is rate of recovery is improved by utilizing the synergy of various inhibitors
This application claims the U.S. Patent application No.61/623 that the title submitted on April 12nd, 2012 is " A Method forImproving Selectivity and Recovery in the Flotation of NickelSulphide Ores that Contain Pyrrhotite by Exploiting the Synergyof Multiple Depressants ", the priority of 459, and at this, it is incorporated to herein in full with it by reference.
Invention field
Present disclosure relates to the method using the combination of inhibitor reagent to carry out selective froth flotation sulfide mineral.
Background of invention
Since twentieth century is early stage, put into practice sulfide mineral flotation.Its industrial significance is familiar with well because can more economic melting and refining from the concentrate of flotation, to provide crude metal.Froth flotation is by utilizing the difference of surface hydrophobic from the method for the valuable mineral of useless rock material Selective Separation.Usually, method for floating is included in underflow material the ore that grinds and pulverize to monomer separation granularity, then regulates (conditioning) it with different reagent in suitable dilution slurries.These reagent comprise trapping agent, inhibitor, foaming agent, modifier etc.Trapping agent makes the surface of required mineral be hydrophobic by physical/chemical adsorption, and this contributes to bubbles attached, and described bubble makes mineral grain float to pulp surface and forms stable foam, collects described stable foam for further process.Inhibitor has and trapping agent opposite effect, by absorption hydrophilic component or by the avtive spot of removing for the absorption of trapping agent, makes the surface of unwanted mineral grain become hydrophilic, thus particle is retained in mine tailing part.Foaming agent contributes to the bubble stablizing suitable dimension in slurry, so as to catch and transfer particle to flotation area.Modifier is generally used for pH and controls.The various schemes of the froth flotation used are usually quite complicated, to make the grade of the valuable mineral of existence and the rate of recovery maximize, and make to have the rock of little commercial value and sulfide mineral give up maximization.
In the processing of the sulfide ore for reclaiming non-ferric rich ore metal, the mineral of handled common value comprise respectively for the pentlandite W metal, Cu, Pb and Zn and capillose, chalcopyrite and vitreous copper and bornite, galena, and zincblende.But, these valuable mineral natively with iron sulfide, namely not there is commercial value and be regarded as the magnetic iron ore of sulfide gangue, pyrite and marcasite and combine.In flotation, selective iron sulfide of giving up significantly can improve the economic worth of concentrate and the SO also reduced in smelting device 2discharge, wherein iron sulfide significantly contributes to these gas dischargings.But giving up of magnetic iron ore is challenging.It not only relates to the abundance of magnetic iron ore in ore, but also relates to the crystal structure (i.e. monocline, six sides or troilite) of magnetic iron ore.In addition, magnetic iron ore closely with other mineral, be mainly combined with pentlandite.Rate of recovery magnetic iron ore Selective depression not being damaged Cu and Ni in floatation process is crucial for producing in industrial mineral processing factory commercial value.
U.S. Patent No. 5,074,993 methods describing flotation sulfide, wherein by using water-soluble polyamines to be suppressed by magnetic iron ore grinding in mineral intermixture of consumption >50g/mt.Water-soluble polyamines is preferably diethylenetriamines (DETA), and also can be selected from and comprise following list: comprise trien, tetren, penten, 2-[(2-aminoethyl) is amino] ethanol, three-(2-aminoethyl) amine, N-lethylenediamine and 1,2 – diaminourea 2-methylpropanes.
U.S. Patent No. 5,411,148 describe and to be separated single-or the improving one's methods of many metallicity sulfide mineral from iron sulfide.The method be included in the inorganic compound flotation of at least one water-soluble sulfur-bearing before adjustment section as in employing as US5,074, the steps necessary before the nitrogenous organic sequestering agent described in 993 regulates further.This water-soluble sulfur-bearing inorganic compound is preferably sodium sulfite (Na 2sO 3), and also optional bin cure compound, dithionate, tetrathionate and sulfur dioxide, its consumption changes to from 50 the drying solid that 600g/mt processes.Nitrogenous organic sequestering agent preferably for the polyethylene polyamine used under enough dose specific flotation feed, such as diethylenetriamines (DETA).Due to the combined effect of the sulfur-containing compound that adds with particular order and organic compounds containing nitrogen, magnetic iron ore is suppressed.
Adopt selective magnetic iron ore to suppress, preceding method is very effective in increase Ni and Cu concentrate grade and the rate of recovery.But, for total (solvable and soluble) Cu and Ni discharged in effluent, use DETA can make the complicated operation of wastewater treatment.DETA is extensive chemical chelating agent, and it and heavy metal ion such as Cu and Ni forms stable complex compound.By raising pH higher than 11 (these usually carry out in wastewater treatment plant), these complex compound sediment can not be made to go out.On the contrary, by polyamines precipitating reagent such as 8702 (can available from Nalco Company, Naperville, IL) add waste water to, precipitate to react with DETA-metal complex and to be formed.But precipitation is very thin particle, and it does not have sedimentation in clarifier, thus make to be difficult to effectively from waste water removing Cu and Ni.In the waste water when using DETA, Cu and Ni of high-load, makes great efforts to determine alternative iron sulfide inhibitor, uses DETA to reduce or eliminate.
Up-to-date patent (U.S. Patent No. 8,221,709) from LignoTech describes and uses hardwood lignosulfonates for being separated the method for rock material from metallicity sulfide ore.This patent specifies the three kinds of hardwood lignosulfonates with different sulphur or sulfonate content and molecular weight obtained from eucalyptus, maple and birch, and in the flotation of the ore slurry ground (it comprises copper sulfide, zinc sulphide or vulcanized lead and iron sulfide) under the NaCN of the dosage of ~ 250-500g/mt adds, compare their performance.Lignosulfonates can be added before or after other reagent and pH regulate.But when only adding ligninsulfonate in commercial run, selective between Cu/Ni sulfide and magnetic iron ore is not improved.
In this meaning, prior art lacks following method: a) in the flotation of the Cu/Ni sulfide mineral be combined with iron sulfide, improve the selective and rate of recovery, and b) reduce or eliminate the problematic polyamines chemicals (such as DETA) of use, to minimize the negative effect to environment.
Summary of the invention
Problem in view of the above and the demand be not met, the invention discloses and utilize the synergy of various inhibitors to improve the suppression of iron sulfide in the flotation of nonferrous metal sulfide and the rate of recovery of not damaging valuable sulfide mineral reduces or eliminates the method using environment-conscious chemicals such as polyamines simultaneously.The method has significant economy and environment benefit.Be included in method for floating process as the slurry of fresh ground or as through pretreatment and the Cu/Ni sulfide ore of the meticulous process intermediates ground and the flotation example of magnetic iron ore.
The essence of this method relates to use various inhibitors, thus utilizes the independent inhibition of often kind of chemicals, and produces synergy to improve the selective and rate of recovery and the use of polyamines is reduced by least 50%, or just eliminates the use of polyamines as possible.The three kinds of chemicals used comprise 1) polyamines, such as DETA; 2) water-soluble sulfur-bearing inorganic compound, such as sodium sulfite; With 3) hardwood lignin sulfonic acid product salt, preferably there is the calcium lignosulfonate of 6kDa molecular weight, 5% sulfonate and 2% sugar, and particularly from the D-912 product of LignoTech.Be used alone these chemicals or a) do not produce sufficient magnetic iron ore suppression, or b) reduce the Cu/Ni rate of recovery, or c) due to the heavy metal of potential high-load, in wastewater treatment plant, causing environmental effluent problems.
Can add respectively simultaneously or (there is no preferred sequence) in order and add three kinds of chemicals, or three kinds of chemicals are pre-blended into single solution with preferred ratio.Similarly, two kinds of components can be pre-blended into single solution with preferred ratio, and add separately the third component to the consumption of change.Inhibitor can be added before or after other flotation reagent.
Each aspect of the present invention promotes the improvement of the non-ferric rich ore metal that selective recovery is combined with iron sulfide.
Each aspect of the present invention promotes the synergy between inhibitor and trapping agent, thus with employing DETA/Na 2sO 3combine the polyamines dosage typically used to compare, allow polyamines (i.e. DETA) dosage to be reduced by least 50%, and do not damage the selective and rate of recovery in floatation process.
Each aspect of the present invention contributes to the discharge of heavy metal and the DETA avoiding the pressure that can cause occurring because forming DETA-metal complex to limit in wastewater treatment plant.
The additional advantage of these aspects of the present invention and a novel feature part are listed in explanation subsequently, and to those skilled in the art, when consulting following content or when by putting into practice the present invention and learning, a part will become more obvious.
Accompanying drawing is sketched
With reference to but be not limited to following accompanying drawing, describe the various illustrative aspects of system and method in detail, wherein:
Fig. 1 is set forth in coarse classifier flotation the curve map only adopting the inefficient magnetic iron ore of D912 to suppress;
Fig. 2 is set forth in coarse classifier flotation to adopt D-912 and Na 2sO 3the curve map that suppresses of effective magnetic iron ore;
Fig. 3 A and 3B sets forth to adopt D-912 and Na for intermediate stream 2sO 3the curve map of the lower rate of recovery;
Fig. 4 A and 4B sets forth to adopt D-912, Na for intermediate stream 2sO 3, the synergistic curve map-dosage that suppresses of magnetic iron ore of DETA and PAX and the impact of order of addition;
Fig. 5 sets forth to adopt D-912, Na for intermediate stream 2sO 3, DETA and PAX the synergistic curve map-from the optimization dosage of factorial design experiment that suppresses of magnetic iron ore;
Fig. 6 A and 6B sets forth to adopt D-912, Na for intermediate stream 2sO 3, and the synergy research of synergistic curve map-come self-optimizing and repeating test that suppresses of the magnetic iron ore of DETA;
Fig. 7 sets forth to adopt D-912, Na 2sO 3, and the impact of order/method of curve map-interpolation reagent that suppresses of the magnetic iron ore of DETA;
Fig. 8 A and 8B is set forth in middling stream (middling stream) to adopt D-912, Na 2sO 3, and DETA magnetic iron ore suppress synergistic curve map; With
Fig. 9 sets forth to adopt D-912, Na 2sO 3, and DETA magnetic iron ore suppress block diagram-reductions concentrate and tailings water in remain DETA, Cu and Ni concentration.
Describe in detail
Following detailed description is never intended to limit the scope of the invention, applicability or structure.More specifically, following explanation is provided for necessity understanding implementing example feature of the present invention.When using the instruction provided herein, those skilled in the art will recognize that the spendable suitable alternative when not extrapolating the scope of the invention.
The invention describes utilize the synergy of various inhibitors come selective floation contain at least one or multiple non-ferric rich ore metal and the sulfide mineral be combined with iron sulfide with the method for the good degree and the rate of recovery that obtain non-ferric rich ore metal values, this iron sulfide forms primarily of magnetic iron ore.By utilizing the synergy using various inhibitors to obtain, the dosage of one of crucial chemicals (i.e. DETA) can significantly reduce, thus alleviates the potential negative effect to environment.The method comprises:
I) in aqueous alkaline slurry, under the existence of trapping agent, foaming agent, pH modifier and the vector gas distributed in the middle of slurry and various inhibitors, sulfide ore is processed, this sulfide ore is the slurry of fresh ground or through pretreatment and the meticulous process intermediates ground, it contains at least one or multiple non-ferric rich ore bacterial attachment (Cu/Ni) and iron sulfide (magnetic iron ore).
Pending slurry contains the iron sulfide of at most ~ 80%.Non-ferric rich ore metal sulfide can be pentlandite and capillose, chalcopyrite and vitreous copper and bornite, galena, and zincblende (they be respectively valuable mineral for Ni, Cu, Pb and Zn).Iron sulfide can be magnetic iron ore, pyrite and marcasite.
Trapping agent can be selected from least one in xanthates and/or ester, dithiophosphates and/or ester, thiocarbamate and/or ester, dithiocar-bamate and/or ester, phosphonodithious acid salt and/or ester, xanthogen formate salt and/or ester, xanthan ester or its mixture.Use amylic potassium xanthate as an example.For the good recovery of rich ore metal, regulate the dosage of trapping agent according to the dosage of inhibitor.
The foaming agent tested is polyglycol ether (F160-13, Flottec), but can also be selected from least one in natural oil, oxyalkyl chain alkane, fatty alcohol, polyglycol ether, polypropylene glycol.Foaming agent is not main factor in the present invention.
The pH modifier tested is the lime of pH 9.5, but can also be soda ash or NaOH.PH scope can be 8-12.
The vector gas used is air.It can also be nitrogen, be rich in the air of nitrogen or rich oxygen containing air or carbon dioxide (rich carbonated air).
After interpolation trapping agent or inhibitor, need regulating step.
Flotation unit can be the standard Denver flotation unit having 2.2L groove and 1200rpm electromotor velocity or have 1.1L groove and 900rpm electromotor velocity.
Ii) various inhibitors contain at least one organic polymer (calcium lignosulfonate from hardwood), at least one sulfur-containing compound and at least one organic compounds containing nitrogen (polyamines) if, compared with being used alone the latter or be combined with a kind of sulfur-containing compound, the latter is present in mixture with less consumption.
Described " organic polymer " is the electronegative watersoluble organic polymer of at least one, and it is selected from by one or more groups formed in lignosulfonates, dextrin, guar gum, cassava, starch or cellulose.Preferably a kind of is the calcium lignosulfonate from hardwood with 6kDa molecular weight and 5% sulfonate and 2% sugar.A kind of such product is from LignoTech " D-912 ", and this is determined by LignoTech patent.
Described " sulfur-containing compound " is at least one water-soluble inorganic sulfur-containing compound, and it is selected from the group be made up of one or more sulfide, sulphite, bisulfites, metabisulfite (meta-bisulphate), dithionate, tetrathionate and sulfur dioxide.Preferred one is sodium sulfite (Na 2sO 3).
Described " organic compounds containing nitrogen " is at least one organic compounds containing nitrogen, it has the configuration be selected from by one or more groups formed had in the polyethylene-polyamines of OCNCCCNCNC and NCCN structure, comprises diethylenetriamines, trien, tetren, penten, ethoxy-DETA, diethanol amine and aminoethyl ethanolamine.Preferred one is diethylenetriamines (DETA).
Iii) add various inhibitors and there is following selection, wherein allow certain regulating time:
Can be added them respectively simultaneously; Or
(without any preferred sequence) can be added them in order, and be with or without adjustment among each other; Or
They can be pre-blended into single solution with predetermined preferred proportion; Or
Two kinds of components can be pre-blended into single solution with predetermined preferred proportion, and optionally add separately the third component with the consumption of change.
Inhibitor can be added before or after trapping agent, and there is certain adjustment.
Iv) polyamines for synergy and minimizing uses, and the dosage of inhibitor will depend on that ore type, grade and its mineralogy form, and therefore should determine by experiment.For tested ore sample, the dosage range of D-912 is 50-150g/t, Na 2sO 3>=100g/t, and DETA is 0-50g/t.Even for intermediate stream, the dosage quoted refers again to the ore ground.DETA dosage keeps low as far as possible and does not damage global selectivity and the rate of recovery, to avoid high-caliber heavy metal in waste water.
V) therefore, trapping agent dosage will be regulated for the metallurgy method optimized, because there is competition between trapping agent and inhibitor.
In preferred embodiments, the present invention relates to and utilize the synergy selective floation of various inhibitors to contain at least one or multiple non-ferric rich ore metal and the method for at least one that is combined of iron sulfide in sulfide ore or multiple sulfide mineral, the method comprises:
I) in aqueous alkaline slurry, under the existence of trapping agent, foaming agent, pH modifier and the vector gas distributed in the middle of described slurry and various inhibitors, sulfide ore is processed, this sulfide ore be fresh ground slurry or through pretreatment and the meticulous process intermediates ground, it contains valuable sulfide mineral described at least one that is combined with at least one iron sulfide mineral, selects this various inhibitors to comprise at least one organic polymer, at least one sulfur-containing compound and/or at least one organic compounds containing nitrogen; With
Ii) carry out froth flotation to be suppressed by iron sulfide, allow the valuable non-iron sulfide of flotation simultaneously.
In another preferred embodiment, the present invention relates to and use the synergy selective floation of various inhibitors to contain at least Ni, Cu, Co, Pt, Pd, Au and Ag rich ore metal and at least Ni/Cu/Co sulfide mineral combined with iron sulfide mineral (it is included at least magnetic iron ore in sulfide ore), the method comprises:
I) in aqueous alkaline slurry, under the existence of trapping agent, foaming agent, pH modifier, the vector gas distributed in the middle of described slurry and various inhibitors, Ni/Cu/Co sulfide ore is processed, this Ni/Cu/Co sulfide ore be fresh ground slurry or through pretreatment and the meticulous process intermediates ground, it contains at least mineral pentlandite and vitreous copper that are combined with at least magnetic iron ore, such as, and this various inhibitors comprises lignin sulfonic acid calcium product (preferred product, D-912), sodium sulfite (Na 2sO 3) and/or DETA; With
Ii) carry out froth flotation to be suppressed by magnetic iron ore, allow the valuable pentlandite of flotation and vitreous copper simultaneously.
Or adding the method for three kinds of inhibitor can comprise: 1) respectively but all simultaneously; With 2) in order and regulate separately.
In addition, inhibitor solution can be added before or after trapping agent.
Polyamines for synergy and minimizing uses, and finds that the dosage of inhibitor depends on that ore type, grade and its mineralogy form, and should therefore determine by experiment.For tested ore sample, the dosage range of D-912 is 50-150g/t, Na 2sO 3>=100g/t, and DETA is 0-50g/t.Even for intermediate stream, the dosage quoted refers again to the ore ground.
Making the magnetic iron ore of often kind of inhibitor acquisition suppress to maximize by adopting under minimum dose, obtaining and (passing through DETA, Na when using various inhibitors 2sO 3with D-912 combination) the collaborative magnetic iron ore that obtains suppresses.More specifically, DETA, Na in iron sulfide suppresses 2sO 3with D-912, there is the function of their uniquenesses.PYRRHOTITE BY FLOTATION has three kinds of mechanism proposed: 1) Cu activation, to promote that trapping agent (xanthates and/or ester) adsorbs; 2) form many-sulphur (poly-sulfur), adhere to for bubble to produce some hydrophobicity sites on Surface of Pyrrhotite; With 3) form the dixanthogen being used for hydrophobicity site.DETA can remove or cover the Cu on iron sulfide 2+activation site, to suppress trapping agent absorption on a surface.By removing at the trapping agent of iron sulfide Adsorption on Surface or many sulphur of formation, Na 2sO 3iron sulfide flotation can be prevented.D-912 is electronegative hydrophilic polymer, and it is by avtive spot (such as Fe (OH) 2+, Ca 2+or Cu 2+) be adsorbed onto iron sulfide on the surface, make its surface be hydrophilic, thus iron sulfide is suppressed.
When single use any one inhibitor, when not damaging rich ore metal recovery rate or causing high-caliber heavy metal in waste water, there is no effective magnetic iron ore and suppress.By using three kinds of different inhibitor simultaneously, create synergy.Advantage can be obtained by each in three kinds of reagent, thus cause making iron sulfide suppress to maximize, make the reduction of the rate of recovery of valuable mineral minimize simultaneously.
Embodiment
Following embodiment is intended to set forth, and never limits the scope of claimed invention, applicability or structure.
In the accompanying drawings, should be noted that and employ shorthand in the axle title of mineral.Comprise symbol: Pn (pentlandite), Cp (chalcopyrite) and Po (magnetic iron ore).
Embodiment 1
The inefficient magnetic iron ore of D-912 is only adopted to suppress
Fig. 1 presents according to U.S. Patent No. 8,221, operation in 709 (LignoTech) only uses hardwood lignin sulfonic acid product salt D-912 as the result of the accumulation rate of recovery of pentlandite and magnetic iron ore in the coarse classifier flotation of the nickel-Copper Ores (containing the 1.5%Ni that has an appointment (3.7% pentlandite), 1.5%Cu (4.3% chalcopyrite) and 21%Fe (19.7% magnetic iron ore) and 72.3% rock (other silicate)) of magnetic iron ore inhibitor process.In this test, when adding 5g/t trapping agent (PAX – amylic potassium xanthate) and 400g/t lime, in rod mill, 1kg ore being milled to and reaching P80 ~ 106 μm.Adopt lime as modifier, carry out incrementally coarse classifier test for 9.5 times at pH.After adding inhibitor and trapping agent respectively, have the adjustment of 2 minutes, and 15ppm foaming agent (F160-13) is in process water.Use the 2.2L Denver flotation cell with 1200rpm rotating shaft, and in flotation, apply the air of 3L/ minute.Concentrate is collected after 0.5,1,2,5,8 and 12 minute.Summarize the chemicals be added in coarse classifier in Table 1 to add.
Only adopt the test of trapping agent (PAX) not show magnetic iron ore to suppress.Adopt DETA/Na 2sO 3test represent acceptable magnetic iron ore suppress and rich ore metal recovery rate.
With use DETA and Na 2sO 3combination (i.e. " benchmark " chemicals) compare, use under the dosage of 25-50g/t hardwood lignin sulfonic acid product salt D-912 as magnetic iron ore inhibitor do not improve magnetic iron ore suppress.With DETA and Na 2sO 3combination compare, under the high D-912 dosage of 250g/t, pentlandite is significantly suppressed, and does not improve the selective of pentlandite/magnetic iron ore.
Embodiment 2
D-912 and Na is adopted for a kind of ore 2sO 3effective magnetic iron ore suppress
Fig. 2 presents the result in the accumulation rate of recovery with pentlandite in the coarse classifier flotation of the identical nickel-Copper Ores used in embodiment 1 and magnetic iron ore, wherein by Na 2sO 3add in coarse classifier with D-912.Grind ore in the same manner as example 1, comprise and add 5g/t trapping agent (PAX) and add 400g/t lime.Work as Na 2sO 3during dosage>=200g/t, observe magnetic iron ore and suppress.The chemicals summarized in table 2 in coarse classifier flotation adds.
Only adopt the test of trapping agent (PAX) not show magnetic iron ore to suppress.Adopt DETA/Na 2sO 3test represent acceptable magnetic iron ore suppress and rich ore metal recovery rate.
Demonstrate and use 200g/t Na 2sO 3dosage itself magnetic iron ore is suppressed to have some effects, but result is not as using benchmark chemicals DETA and Na 2sO 3those acquisition are so good.At employing D-912 and Na 2sO 3test in, work as Na 2sO 3during dosage >100g/t, observe some signs that magnetic iron ore suppresses.Work as Na 2sO 3during dosage>=200g/t and D-912 dosage>=50g/t, adopt D912/Na 2sO 3obtain and benchmark DETA/Na 2sO 3similar pentlandite/magnetic iron ore selectivity curve.The dosage of D-912 is increased to 100g/t and by Na from 25 2sO 3dosage be increased to from 200 the shape (namely the pentlandite rate of recovery declines along with the decline of the magnetic iron ore rate of recovery) that 400g/t does not significantly change pentlandite/magnetic iron ore selectivity curve.
For this raw material, do not need to add DETA, this is preferred for environmental concern.
Embodiment 3
D-912 and Na is adopted for intermediate stream 2s0 3the lower rate of recovery
Fig. 3 A and 3B presents containing 7.6%Cu (21.9% chalcopyrite) respectively, 6.4%Ni (17.3% pentlandite), pentlandite/the magnetic iron ore accumulated in the refiner flotation of the intermediate stream of 37%Fe (39.8% magnetic iron ore) and 21% rock and chalcopyrite/magnetic iron ore optionally result, wherein by Na 2sO 3add in refiner with D-912.This research relates to coarse classifier and refiner float test, and is added in refiner section by inhibitor.10g/t trapping agent (PAX) will be amounted to add in coarse classifier flotation, and collect coarse classifier concentrate lasting 6 minutes.In refiner section, pH 9.5 times with lime as modifier treatment coarse classifier concentrate.After adding inhibitor and trapping agent respectively, there is the adjustment of 2 minutes, and 15ppm foaming agent (F160-13) is in process water.Use the 1.1L Denver flotation cell the air applying 1L/ minute in refiner flotation with 900rpm rotating shaft.After 1.5,3,5 and 16 minutes, collect refiner concentrate.The chemicals summarized in table 3 in refiner flotation adds.
There is 200g/t Na as D-912 dosage>=50g/t 2s0 3time, observe and be selectively improved and be even better than DETA/Na 2s0 3benchmark.But the rate of recovery of chalcopyrite declines ~ 15%.If the dosage of D-912 declines further, the dosage of (≤25g/t) or PAX increases, and so will damage selective.This is unacceptable for industrial production.
Embodiment 4
D-912, DETA, Na is adopted for intermediate stream 2s0 3with the synergy that the magnetic iron ore of PAX suppresses
Fig. 4 A with 4B presents pentlandite/magnetic iron ore from the accumulation of the refiner flotation with the identical intermediate stream used in embodiment 3 and chalcopyrite/magnetic iron ore optionally result respectively.In this embodiment, by DETA and Na 2s0 3add in refiner with D-912, but with as DETA and Na 2s0 3compare when being used as " benchmark " condition a part of together, dosage reduces.This research relates to the coarse classifier and refiner float test that describe in embodiment 3.The chemicals summarized in table 4 in refiner flotation adds.
Fix wherein in the test (T18309, T18310, T18311) of dosage of often kind of chemicals, change the order of adding chemicals.Do not see the marked difference of result.
Change wherein in the test of dosage of inhibitor and trapping agent, selective very good, but the rate of recovery of pentlandite and chalcopyrite is far below target (T18309, T18310, T18311), the rate of recovery of pentlandite and chalcopyrite is acceptable, but selective remarkable decline (T18358, T18360).
Only when reaching the balance between trapping agent and inhibitor (T18359), the selective and rate of recovery is close to " benchmark " result.At D-912, DETA and Na 2s0 3with under the suitable dose of trapping agent (PAX), obtain the good selective and rate of recovery.
Embodiment 5
For intermediate stream for finding synergistic D-912, DETA and Na of suppressing for magnetic iron ore 2s0 3with the factorial design experiment of the optimization dosage of PAX
Fig. 5 presents at maintenance Na 2s0 3dosage fixing while between D-912, DETA and trapping agent (PAX) interactional 2 3the result of factorial design experiment.Result from embodiment 4 shows that the combination of three kinds of chemicals creates synergy as inhibitor, and this allows DETA dose degradation, maintains good selective and rich ore metal recovery rate simultaneously.Meanwhile, find that the dosage of trapping agent plays very important effect.In order to confirm the optimization range of the dosage acting synergistically and determine often kind of chemicals further, when chemicals being added to refiner section, carry out the three factors-secondary (2 of the dosage to PAX, DETA and D-912 3) factor design research.Raw material with describe in embodiment 3 identical.Coarse classifier-refiner flotation circuit with describe in embodiment 3 identical.In all these tests, under the fixed dosage of 200g/t, add Na 2s0 3.Define dosage and the experimental condition of DETA, D-912 and PAX in table 5.
In this experimental design, the standard of selective dose comprises: a) DETA dosage should be less than at DETA/Na 2s0 3the level (i.e. usual 50g/t) used in combination; B) the D-912 dosage due to result display <50g/t is above inoperative, and the upper limit is unknown, therefore extends this dosage to higher level; And c) be presented at pentlandite and chalcopyrite under the PAX dosage of 10-15g/t due to the result of embodiment 5 the rate of recovery be sufficient, thus do not need to reach the dosage more much higher than normal (i.e. 5g/t).
In one group (FD2, FD3, FD5 and FD7) adopting high dose D-912, obtain the high concentrate grade with the low-down pentlandite rate of recovery (20 ~ 50%), this shows that the D-912 level of 150g/t is too high.In another group (FD8 and FD9) adopting high dose PAX and low dosage D-912, the selective decline of pentlandite/magnetic iron ore, thus cause the concentrate grade lower than target.The dosage (FD1) being used in the intermediate point place of this scope creates the result between these limiting values.Can find out under 10g/t PAX, 50g/t D-912 and 15g/t DETA (FD6), obtain good pentlandite/magnetic iron ore selective, and result be close to DETA/Na 20 3those of benchmark.Under these dosage, the chalcopyrite rate of recovery also very good (~ 90%).
Embodiment 6
D-912, DETA and Na is used for the synergy that the magnetic iron ore of intermediate stream suppresses 2s0 3optimization and repeating test
Fig. 6 presents and ought use D-912, DETA and Na together to verify 2s0 3in time, repeatably acts synergistically (it is proven in embodiment 5) and optimizes the dosage of chemicals and the result of the Optimum Experiment carried out and reference test.Coarse classifier-refiner flotation circuit with describe in embodiment 3 identical.Intermediate stream with describe in embodiment 3 identical.The dosage of the chemicals adding refiner to is defined in table 6.Be initial by the condition providing good result (FD6: adopt 15g/tDETA, 50g/t D-912 and 10g/t PAX), as eliminating D-912 (T18558) or DETA (T18560) or Na 2s0 3(T18612), time, pentlandite/magnetic iron ore is selective not as so good when using all chemicals together.
Other repeats with the result optimized all in the identical selective scope of pentlandite/magnetic iron ore, and this shows stable performance.Can find out: a) D-912 dosage is increased to 75g/t and can reduces pentlandite and a little percentage point of the chalcopyrite rate of recovery; B) DETA dosage is changed to 25 from 15, then changing to 35g/t does not affect the rate of recovery and selective, thus preferably lower DETA dosage (15g/t); And c) slightly reduce PAX dosage (namely from 10 to 7.5g/t) result is had no significant effect.
Embodiment 7
Add D-912, DETA and Na 2s0 3the impact of order and method
Fig. 7 presents to evaluate and adds the order of chemicals and the result of method.Intermediate stream with describe in embodiment 3 identical.Identical with embodiment 3 of coarse classifier-refiner flotation circuit, and adopt following condition: 1) under adjustment, add three kinds of chemicals (D-912, DETA and Na simultaneously 2s0 3); 2) Na is added in order 2s0 3, DETA and D-912 and for each time add there is a regulating time; 3) DETA and D-912 is pre-blended into a kind of solution, and it can be used as single agents and Na under adjustment 2s0 3add in slurries; With 4) by DETA, D-912 and Na 2s0 3be pre-blended into a kind of solution, and it can be used as single agents to add in slurries under adjustment.
Summarize chemicals in refiner in table 7 to add and the condition of adding method.
The difference with insignificance of the result adopting the various methods of adding chemicals to obtain, because all results show good selective.The advantage of adding three kinds of chemicals respectively can regulate separately each dosage.Use aqueous premix provides the fairly simple scheme for arranging chemical product holding vessel and transfer line, and when condition is set up completely, this is good.
Embodiment 8
D-912, DETA and Na is adopted for another middling stream 2s0 3magnetic iron ore suppress synergy
Fig. 8 A and 8B presents to be presented in middling stream and adds D-912, Na 2s0 3with the result of DETA on the impact of the suppression of magnetic iron ore.Use the middling raw material containing 1.0%Cu (2.7% chalcopyrite), 2.0%Ni (4.3% pentlandite), 44.6%Fe (65.7% magnetic iron ore) and 27.3% rock, carry out two sections of coarse classifiers-refiner float test.The chemicals summarized in table 8 in coarse classifier and refiner section adds.
Fig. 8 A presents by only inhibitor being added to the result obtained in coarse classifier section.Compared with the situation (T20013) only adopting PAX, add D-912 and cause the significantly reduced magnetic iron ore rate of recovery.By D-912 and Na 2s0 3(T20027) combination is not so good as to use D-912, Na together on the impact that magnetic iron ore suppresses 2s0 3so good with (T20030) during DETA.From adopting the result of test of these three kinds of chemicals comparatively close to DETA/Na 2s0 3benchmark (T20016), but there is much lower DETA interpolation (~ 40%DETA).
Fig. 8 B presents by inhibitor being added to the result obtained in both coarse classifier and refiner section.As use three kinds of chemicals (D-912, DETA and Na 2s0 3) combination time, being added to by enough D-912 in coarse classifier section is most critical.If this dose is not enough high (i.e. <75g/t D-912) in coarse classifier section, so occur that little magnetic iron ore suppresses.When adopting high dose D-912 in coarse classifier section, more D-912 is added to can to improve pentlandite/magnetic iron ore further in refiner section selective.In a word, in the flotation of high magnetic iron ore middling stream, need D-912, DETA, Na of enough dose 2s0 3selective to realize good pentlandite/magnetic iron ore with PAX.
Embodiment 9
By using D-912, DETA and Na 2s0 3combination reduce the residual quantity of DETA, Cu and Ni in process water
Fig. 9 A and 9B set forth to be used in embodiment 5 and 6 qualification new inhibitor mixture respectively on the impact of the quality of concentrate and tailings water.Use the operation described in embodiment 3, carry out two coarse classifiers-refiner float test with on the identical nickel-Copper Ores used in embodiment 1." benchmark " condition of use, adopts 50g/t DETA, 200g/t Na 2s0 3carry out the first test.Use new condition, adopt 50g/t D-912,15g/t DETA and 200g/tNa 2s0 3carry out the second test.Show this two set condition above, result in similar flotation metallurgy.After flotation, collect the concentrate and tailings water from each test, and analyze residual DETA, Cu and Ni.Analysis result is summarized in table 9.Can be clear that and use D-912, DETA and Na 2s0 3new blend obtain DETA, Cu and Ni reduce residual level.
Known different gangue solids has the certain capabilities of stably adsorbing DETA separately.The result verification that provides in table 9 is by using D-912, DETA and Na 2s0 3combination and the DETA dosage of reduction, significantly can reduce the residual quantity of DETA in process water.The DETA of this amount can be adsorbed on gangue solids, and to wastewater treatment plant without any negative effect.

Claims (22)

1., by utilizing the synergy of various inhibitors to improve the selective and rate of recovery of the valuable non-iron sulfide mineral be combined with iron sulfide in the foam flotation method on nonferrous metal sulfide to reduce or eliminate the method using environment-conscious chemicals such as polyamines simultaneously, the method comprises:
I) in aqueous alkaline slurry, under the existence of trapping agent, foaming agent, pH modifier, the vector gas distributed in the middle of slurry and various inhibitors, sulfide ore is processed, this sulfide ore be fresh ground slurry or through pretreatment and the meticulous process intermediates ground, it contains at least one or multiple non-ferric rich ore bacterial attachment and iron sulfide, selects this various inhibitors to comprise at least one organic polymer, at least one sulfur-containing compound and/or at least one organic compounds containing nitrogen; With
I i) carry out froth flotation to be suppressed by iron sulfide, allow the valuable non-iron sulfide of flotation simultaneously.
2. method according to claim 1, wherein said sulfide mineral is pentlandite and capillose, chalcopyrite and vitreous copper and bornite, galena, or zincblende, or at least one in its mixture, it is the ore of fresh ground or pretreated intermediate stream.
3. method according to claim 1, wherein said at least one or multiple non-ferric rich ore metal are selected from the nickel of sulfide mineral, copper, zinc and lead, cobalt, platinum, palladium, gold and silver-colored part.
4. method according to claim 1, wherein said iron sulfide is magnetic iron ore, pyrite and marcasite or its mixture.
5. method according to claim 1, the pH of wherein said aqueous alkaline slurry is about 8 to 12.
6., according to the method for claim 1 and 5, the pH of wherein said aqueous alkaline slurry is 9.5.
7. method according to claim 1, wherein said trapping agent is at least one in xanthates and/or ester, dithiophosphates and/or ester, thiocarbamate and/or ester, dithiocar-bamate and/or ester, phosphonodithious acid salt and/or ester, xanthogen formate salt and/or ester, xanthan ester or its mixture.
8. method according to claim 7, wherein said trapping agent is xanthates and/or ester.
9. method according to claim 1, wherein said vector gas selects free air, nitrogen, be rich in the group of at least one composition in the air of nitrogen or rich oxygen containing air or carbon dioxide (rich carbonated air) or its mixture.
10. method according to claim 9, wherein said vector gas is air.
11. methods according to claim 1, wherein said organic compounds containing nitrogen has at least one organic compounds containing nitrogen be selected from by the configuration of one or more groups formed had in the polyethylene polyamine of OCNCCCNCNC and NCCN structure or its mixture, comprises diethylenetriamines, trien, tetren, penten, ethoxy-DETA, diethanol amine and aminoethyl ethanolamine.
12. methods according to claim 11, wherein said organic compounds containing nitrogen is DETA (diethylenetriamines).
13. methods according to claim 1, wherein said sulfur-containing compound is at least one water-soluble inorganic sulfur-containing compound, and it is selected from the group be made up of one or more sulfide, sulphite, bisulfites, metabisulfite, dithionate, tetrathionate, sulfur dioxide or its mixture.
14. methods according to claim 13, wherein said sulfur-containing compound is sulphite.
15. methods according to claim 1, wherein said organic polymer is the electronegative watersoluble organic polymer of at least one, and it is selected from the group be made up of one or more hardwood lignosulfonates, dextrin, guar gum, cassava, starch or cellulose.
16. methods according to claim 15, wherein said organic polymer has 6kDa molecular weight and containing the calcium lignosulfonate from hardwood of have an appointment 5% sulfonate and about 2% sugar.
17. methods according to claim 1, wherein for often kind of sulfide ore, are determined by experiment the optimization dosage of often kind of inhibitor.
18. methods according to claim 1, if wherein organic compounds containing nitrogen is to be present in mixture than the consumption being used alone it or be combined required consumption few with sulfur-containing compound.
19. methods according to claim 1, wherein can add various inhibitors simultaneously respectively.
20. methods according to claim 1, wherein can add various inhibitors when not having particular order in order.
21. methods according to claim 1, wherein can add various inhibitors with the single solution of the premixed of each component with the preferred proportion determined.
22. methods according to claim 1, wherein can add various inhibitors with the single solution of the premixed of two kinds of components with the preferred proportion determined, and optionally add separately the third component with the consumption of change.
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CN106492993A (en) * 2016-10-30 2017-03-15 长春黄金研究院 Suppress the composite restrainer of particulate silicate gangue
CN107824341A (en) * 2017-10-25 2018-03-23 江西理工大学 One kind improves difficult copper sulfide ore beneficiation and refers to calibration method
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