CN105363564A - Desulfurization reagent for removing pyrrhotite in iron concentrate containing high sulphur by flotation method - Google Patents
Desulfurization reagent for removing pyrrhotite in iron concentrate containing high sulphur by flotation method Download PDFInfo
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- CN105363564A CN105363564A CN201510913937.2A CN201510913937A CN105363564A CN 105363564 A CN105363564 A CN 105363564A CN 201510913937 A CN201510913937 A CN 201510913937A CN 105363564 A CN105363564 A CN 105363564A
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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
- B03D1/018—Mixtures of inorganic and organic compounds
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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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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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
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/04—Frothers
Abstract
The invention relates to a desulfurization reagent for removing pyrrhotite in an iron concentrate containing high sulphur by a flotation method. The desulfurization reagent is characterized in that a flotation agent is prepared by mixing citric acid, tartaric acid, oxalic acid and copper sulfate which are prepared into a, b and c mixed solutions. For magnetic iron concentrate with different pyrrhotite contents, 0 to 50% of mixed solution b and 0 to 50% of mixed solution c are added to the mixed solution a to prepare a floatation desulfurization reagent which can effectively activate the pyrrhotite so as to separate the pyrrhotite and magnetite, and as a result, the optimal desulfurization effect can be achieved. The flotation desulfurization reagent is simple and easy to prepare and use, common tap water and industrial backwater can be used for preparation of desulfurization reagent, and the current problems of low desulfurization and low recovery rate of the iron concentrate containing high sulphur can be solved.
Description
Technical field
The present invention relates to a kind of dressing activator, particularly relating to the desulfurization medicament (hereafter can be described as LJ desulfurization medicament) of magnetic iron ore in a kind of flotation removing iron concentrate containing high sulphur, belonging to ore dressing field.
Background technology
Difficulty selects the sulphur in iron concentrate containing high sulphur mainly to exist with the form of magnetic iron ore, and its desulphurization problem governs the development of iron and steel enterprise for a long time, belongs to the whole common problem faced of industry.All to some extent containing magnetic iron ore in most of iron ore on the ground such as Xinjiang of China, Anhui, Hubei, Jiangsu, Inner Mongol, and sulfur content is higher; In addition, also containing higher sulphur in the iron ore of some external import.Want to make full use of these iron ore resources, must desulfurization process be carried out.But due to the specific susceptibility of magnetic iron ore and magnetic iron ore, proportion all closely, therefore iron ore concentrate desulfurization becomes an industry difficult problem, domesticly at present there is no more ripe technique and can it be separated with magnetic iron ore well with medicament.
CN104069937A discloses the beneficiation method that a kind of iron ore removes magnetic iron ore, adopt fragmentation, ore grinding, classification-weak magnetic separation process obtain TFe grade >=65.0%, inferior fine magnetite concentrate containing S0.5 ~ 1.4%, it is characterized in that: described inferior fine magnetite concentrate is adopted anti-floatingly to roughly select, low-sulfur iron ore concentrate that twice anti-floating selected acquisition contains S<0.15%; The described anti-floating regime of agent roughly selected to feed the dry ore deposit gauge of reverse flotation work is: (1) pH adjusting agent: sulfuric acid 800 ~ 1200g/t; (2) activator: copper sulphate 45 ~ 210g/t; (3) collecting agent: butyl xanthate or Isobutylxanthic acid 200 ~ 650g/t, butyl black powder 140 ~ 250g/t; (4) foaming agent: 2# oil 20 ~ 70g/t; Described anti-floating selected regime of agent to feed the dry ore deposit gauge of reverse flotation work is: (1) primary cleaning 1. collecting agent: butyl black powder 50 ~ 80g/t; 2. foaming agent: 2# oil 30 ~ 50g/t; (2) recleaning 1. collecting agent: butyl black powder 25 ~ 40g/t; 2. foaming agent: 2# oil 20 ~ 40g/t.
CN102886311A discloses a kind of method for floating of platiniferous mineral violarite, the method comprises: platiniferous nickel minerals to adjust agent through adding sulfuric acid, oxalic acid or citric acid, waterglass, calgon or hydroxyethylcellulose do gangue inhibitor, copper sulphate or plumbi nitras make activator, and butyl xanthate does collecting agent, and terpenic oil, kerosene or diesel oil do foaming agent, through stage grinding, stage grading, roughly select flotation, scan flotation and selected operation, achieve the enrichment of platiniferous purple sulphur nickel nickel minerals.But the method is the selective absorption for mineral platinum ore and violarite, and need not simply be diverted to magnetic iron ore in flotation removing iron concentrate containing high sulphur, and in the method, inhibitor is necessary component.
CN102989589A discloses the process that a kind of two step method reclaims downtrod pyrite and magnetic iron ore, and it comprises the following steps: (1) adds acid, makes pH value be less than 10; (2) copper sulphate is added; (3) butyl xanthate is added; (4) foaming agent is added; (5) flotation obtains high iron concentrate; (6) ore pulp after flotation adds acid again, makes pH value be 6-7; (7) copper sulphate is added; (8) butyl xanthate is added; (9) foaming agent is added; (10) flotation obtains low iron concentrate.
CN102974469A discloses a kind of method that sulphur falls in floating sulphur collecting agent and iron ore concentrate flotation, floating sulphur collecting agent is amylic potassium xanthate and the N of 1 ~ 3: 1 by mass ratio, N-sodium oiethyl dithiocarbamate forms, and the method utilizing this floating sulphur collecting agent to make iron ore concentrate flotation fall sulphur adds adjusting agent adjusted to ph in weak magnetic separation iron concentrate pulp.
Containing diacyl bis-thiourea class surfactant in CN101337206A sulfide flotation collector composition; such diacyl bis-thiourea compound is as structural formula (I) or (II), and this collecting agent has high collecting ability to precious metal minerals such as the vulcanized lead mineral of the copper sulfide minerals such as chalcopyrite, activated by copper ions or zinc sulfide mineral, nickel sulfide mineral and gold and silver.
University of Science & Technology, Beijing has all carried out desulfurization research to Anshan Iron, Kunming University of Science and Technology to Yunnan High sulfur iron ore to certain imported Fe ore (sulfur-bearing 2.51%) and Xinjiang iron ore (sulfur-bearing 10.07%), Shenyang Research Institute of Nonferrous Metals for the self-produced iron ore concentrate of Baogang, mine research institute of Ma'an Mountain, find that the main Problems existing of iron ore concentrate desulfurization is: if the sulphur in iron ore concentrate lowers, the iron ore concentrate rate of recovery will inevitably be caused to reduce; In addition, some desulfurization medicament is subject to the restriction of acid-base value, temperature, water quality, uses more complicated.So, no matter from production angle or from environmental angle, all must carry out floatation desulphurization process in early stage to iron ore concentrate, to reduce subsequent smelting cost, improve steel, protection of the environment, enterprise competitiveness.This area is needed badly and is developed that desulfurized effect is good, the iron ore concentrate rate of recovery is high, the adaptable desulfurization medicament of service condition.
Summary of the invention
For solving the problems of the technologies described above, the present inventor, through further investigation and great many of experiments, just effectively can remove magnetic iron ore in iron concentrate containing high sulphur under providing a kind of normal temperature, ensure the desulfurization medicament of the higher iron ore concentrate rate of recovery (can be called " LJ medicament " or " LJ desulfurization medicament ") simultaneously.Further, its preparation uses simple, is applicable to ordinary tap water and the use of industrial backwater, can solves the problem that current iron concentrate containing high sulphur desulfurized effect is poor, the iron ore concentrate rate of recovery is low.
In one aspect of the invention, provide the desulfurization medicament of magnetic iron ore in a kind of flotation removing iron concentrate containing high sulphur, wherein the formula of this desulfurization medicament is: desulfurization pharmacy kit is containing citric acid, tartaric acid, oxalic acid, copper sulphate and water, this desulfurization medicament forms by aqueous citric acid solution, aqueous tartaric acid solution, oxalic acid aqueous solution and copper sulfate solution are composite, and in described aqueous citric acid solution, aqueous tartaric acid solution, oxalic acid aqueous solution, copper sulfate solution, the mass percent concentration of citric acid, tartaric acid, oxalic acid and copper sulphate is 0.5-1.5% independently of one another.
Preferably, in described aqueous citric acid solution, aqueous tartaric acid solution, oxalic acid aqueous solution, copper sulfate solution, the mass percent concentration of citric acid, tartaric acid, oxalic acid and copper sulphate is 1.0%.
Further preferably, above-mentioned compound process can comprise the following steps:
(1) be that x:1 mixes with copper-bath according to mass ratio respectively by aqueous citric acid solution, aqueous tartaric acid solution, oxalic acid aqueous solution, x value is the 1-5 arbitrary value of 1 to 5 (namely from), is mixed with a, b, c tri-parts of mixed solutions stand-by; Preferably, citric acid solution: the mass ratio of copper-bath is 3:1, tartaric acid solution: the mass ratio of copper-bath is 3:1, oxalic acid solution: the mass ratio of copper-bath is 3:1.
(2) in mixed solution a with addition of mixed solution b, c, being 0-50% independently of one another with addition of amount, but is not 0, obtains desulfurization medicament.Be appreciated that described with addition of amount refer to mixed solution b, c respectively with the mass ratio of mixed solution a, preferably, solution a:b:c mass ratio equals 6:1:1.
In an especially preferred embodiment, described desulfurization medicament also comprises following formula (I) based on this desulfurization medicament total weight 0.01-10 % by weight, preferred 0.5-5.0 % by weight or the collecting agent shown in formula (II):
This compound can react obtained by methacrylic acid and oxalamide.
This collecting agent can with treat that Iron Ore Flotation stone produces larger combined surface area, thus be conducive to FLOTATION SEPARATION.Further, due to the special amide structure of described collecting agent, make that there is good selective chelation, special surface of solids effect can be produced on iron ore surface, thus to magnetic iron ore, there is particularly preferred adsorptive selectivity.Such effect is that previously institute was unanticipated.
Quaternary ammonium type collecting agent shown in above-mentioned formula (II) in use demonstrates stronger collecting ability, this is because it produces stronger physics electrostatic attraction and hydrogen bond effect on iron ore surface, its performance is significantly better than common ether amine, ether diamine, long-chain season by collecting agents such as salt (as cetyl quaternary ammonium acetate).
It will be appreciated, of course, that and can not add described collecting agent in this desulfurization medicament, but as mentioned below, in use, after adding above-mentioned desulfurization medicament of the present invention, with addition of collecting agent.In addition, also can use the mixture both it, shown in formula (I) and formula (II), the ratio of collecting agent can be such as 1:5-5:1 (weight).Such collecting agent or its combination do not report in the art or relevant art enlightenment.
In still another aspect of the invention, provide a kind of method preparing above-mentioned desulfurization medicament, the method can comprise the following steps:
(1) citric acid, tartaric acid, oxalic acid, copper sulphate are mixed with water respectively, stirring and dissolving, being mixed with mass percent concentration is four parts of solution for later use of 0.5-1.5% independently of one another;
(2) be x:1, x value with copper-bath according to mass ratio respectively by citric acid in step (1), tartaric acid, oxalic acid solution be 1-5, be mixed with a, b, c tri-parts of mixed solutions stand-by;
(3) in mixed solution a with addition of mixed solution b, c, being 0-50% independently of one another with addition of amount, but is not 0, obtains desulfurization medicament.
Preferably, in step (1), the mass percent concentration of four parts of solution is 1.0%.
In another aspect of the invention, provide the method for magnetic iron ore in a kind of flotation removing iron concentrate containing high sulphur, the method comprises the following steps: in floatation process, after adding above-mentioned desulfurization medicament of the present invention, with addition of collecting agent and/or foaming agent, carry out the flotation of magnetic iron ore in iron concentrate containing high sulphur.Described collecting agent is preferably the collecting agent shown in formula (I) above.
Described collecting agent can be such as butyl xanthate, and described foaming agent can be such as foaming agent No. 2 oil.
Preferably, in described floatation process, point to roughly select, scan and carry out with selected three phases.
Further preferably, scan described in and multiple sub of scanning can also be divided into carry out.Particularly preferably, scan sub described in and be divided into sub one and sub two." one slightly sweeps an essence " now also can be called " a thick essence two is swept ".
Floating to Iron grade 68.12%, under sulfur content 2.15% condition, adopting described " one slightly sweeps an essence " closed circuit technological process, final iron ore concentrate productive rate 88.92%, TFe69.13%, S0.33%, the TFe rate of recovery 90.24%, iron concentrate S18.41%, TFe60.01%, desulfurization degree 86.35%.Such effect is that those skilled in the art can not expect.
The present inventor, through large quantity research and screening, finds desulfurization medicament and the collecting agent by using variable concentrations in floatation process different phase, can obtain particularly preferred effect.Particularly preferably, roughly select the stage: LJ drug concentration is 400, butyl xanthate concentration is 500; Scanning sub one: LJ drug concentration is 200, and butyl xanthate concentration is 200; Scanning sub two: LJ drug concentration is 100, and butyl xanthate concentration is 100; In the selected stage: LJ drug concentration is 200, butyl xanthate concentration is 200; Described concentration unit is g/t, does ore deposit amount re-computation by flotation to ore deposit.Such certain concentration combination is not reported in the prior art, neither those skilled in the art easily expect or simple analysis reasoning or limited test available.By described drug concentration combination of the present invention, Fe rate of recovery % can reach 90.24, desulfurization degree can reach 86.35%, and effect is far superior to the conventional magnetic iron ore sulfur removal technology (such as previously described prior art such as CN104069937A) of this area.
In a detailed description of the invention, the compound method of LJ desulfurization medicament of the present invention can be:
(1) be that 1:99 mixes with running water respectively by citric acid pure for solid analysis, tartaric acid, oxalic acid, copper sulphate according to mass ratio, stir in glass container, be mixed with four parts of solution for later use that mass percent concentration is 1%;
(2) according to the height of magnetic iron ore content, can be that x:1 (x=1 ~ 5) mixes with copper-bath respectively in glass container according to mass ratio by citric acid, tartaric acid, oxalic acid solution in (1), be mixed with a, b, c tri-parts of mixed solutions stand-by;
(3) according to the magnetic separation of iron ore concentrate of different magnetic iron ore content, with addition of mixed solution b, c in mixed solution a, be respectively 0 ~ 50% with addition of amount, total combined amount is 100%;
In floatation process, in ore pulp, first add the LJ medicament of activation, then with addition of collecting agent (xanthate), the foaming agent (No. 2 oil) of routine, the flotation of magnetic iron ore in iron concentrate containing high sulphur can have been carried out.
By said method of the present invention, LJ medicament can be adopted at normal temperatures to carry out activating rear flotation, remove magnetic iron ore in iron concentrate containing high sulphur, water mitigation is not returned by industry, adjustable use amount, remove magnetic iron ore in the iron ore concentrate of different sulfur content, or even sulfur content is up to the magnetic iron ore of more than 3%; After flotation and obtain sulfur content below 0.4%, the iron ore concentrate of the rate of recovery more than 90%, that is, taken into account desulfurization and the rate of recovery in iron ore concentrate, this be very difficult in the prior art realize.
Specific embodiments
Below in conjunction with following examples, the present invention is described in further detail, but embodiments of the present invention are not limited thereto.
Embodiment 1
The Iron grade 68.70% of the high-sulfur magnetic separation of iron ore concentrate of Inner Mongol sulfur-bearing based on magnetic iron ore, sulphur grade 1.66%, the flotation flowsheet of " a thick essence two is swept " is adopted to carry out floatation desulphurization to it, floating agent adds successively according to No. 2, LJ medicament, collecting agent butyl xanthate and foaming agent oil order, selected and the section of scanning dosing once reduces by half, and regime of agent as shown in Tables 1 and 2.
Table 1 flotation LJ reagent combination (solution quality percent concentration is 1%, mixes all in mass ratio)
Table 2 flotation LJ dosing (g/t does ore deposit amount re-computation by flotation to ore deposit)
To above-mentioned flotation flowsheet, control flotation time is the section of roughly selecting 3-10min, and selected section is 2-8min, sweeps one section for 2-6min, sweeps two sections of 1-4min, through " a thick essence two is swept " operation, finally obtains mix sulphur concentrate and mixing iron ore concentrate.Obtained experimental result is as shown in table 3.
Table 3 high-sulfur magnetic iron ore active flotation Desulfurization Test Results
As can be seen from above-mentioned experimental result clearly, by medicament of the present invention, and combination is roughly selected, is scanned and dressing process, to the desulfurization of magnetic iron ore, there is extraordinary removal effect and remove selective, such as iron ore concentrate, sulfur content can be low to moderate 0.18%, and for mix sulphur concentrate, sulfur recovery rate can up to 90.24%.Meanwhile, desulfurized effect and the rate of recovery of smart iron ore concentrate has been taken into account very well.Such effect is all that institute is unanticipated in advance for those skilled in the art.
Embodiment 2
The Iron grade 66.70% of the high-sulfur magnetic separation of iron ore concentrate of Inner Mongol sulfur-bearing based on magnetic iron ore, sulphur grade 2.34%, the flotation flowsheet of " a thick essence two is swept " is adopted to carry out floatation desulphurization to it, floating agent adds successively according to No. 2, LJ medicament, collecting agent butyl xanthate and foaming agent oil order, selected and the section of scanning dosing once reduces by half, and regime of agent is as shown in table 4 and 5.
Table 4 flotation LJ reagent combination (solution quality percent concentration is 1%, mixes all in mass ratio)
Table 5 flotation LJ dosing (g/t does ore deposit amount re-computation by flotation to ore deposit)
To above-mentioned flotation flowsheet, control flotation time is the section of roughly selecting 3-10min, and selected section is 2-8min, sweeps one section for 2-6min, sweeps two sections of 1-4min, through " a thick essence two is swept " operation, finally obtains mix sulphur concentrate and mixing iron ore concentrate.Obtained experimental result is as shown in table 6.
Table 6 high-sulfur magnetic iron ore active flotation Desulfurization Test Results
As can be seen from above-mentioned experimental result clearly, by medicament of the present invention, and combination is roughly selected, is scanned and dressing process, to the desulfurization of magnetic iron ore, there is extraordinary removal effect and remove selective, such as iron ore concentrate, sulfur content can be low to moderate 0.24%, and for mix sulphur concentrate, sulfur recovery rate can up to 90.73%.Meanwhile, desulfurized effect and the rate of recovery of smart iron ore concentrate has been taken into account very well.Such effect is all that institute is unanticipated in advance for those skilled in the art.
The open the present invention of this written description use-case, comprises optimal mode, and also enables those skilled in the art manufacture and use the present invention.Of the present inventionly the scope of granted patent can be defined by the claims, and other example that those skilled in the art expect can be comprised.If other example this has the structural element of the literal language not differing from claims, if or other example this comprises and the equivalent structure element of the literal language of claims without substantial differences, then this other example intention is within the scope of claims.Can not cause under inconsistent degree, be incorporated herein by reference to by all references part of reference herein.
Claims (7)
1. the desulfurization medicament of magnetic iron ore in a flotation removing iron concentrate containing high sulphur, wherein the formula of this desulfurization medicament is: desulfurization pharmacy kit is containing citric acid, tartaric acid, oxalic acid, copper sulphate and water, this desulfurization medicament forms by aqueous citric acid solution, aqueous tartaric acid solution, oxalic acid aqueous solution and copper sulfate solution are composite, and in described aqueous citric acid solution, aqueous tartaric acid solution, oxalic acid aqueous solution, copper sulfate solution, the mass percent concentration of citric acid, tartaric acid, oxalic acid and copper sulphate is 0.5-1.5% independently of one another.
2. desulfurization medicament according to claim 1, in wherein said aqueous citric acid solution, aqueous tartaric acid solution, oxalic acid aqueous solution, copper sulfate solution, the mass percent concentration of citric acid, tartaric acid, oxalic acid and copper sulphate is 1.0%.
3., according to the desulfurization medicament of claim 1 or 2, wherein compound process comprises the following steps:
(1) be that x:1 mixes with copper-bath according to mass ratio respectively by aqueous citric acid solution, aqueous tartaric acid solution, oxalic acid aqueous solution, x value is 1-10, is mixed with a, b, c tri-parts of mixed solutions stand-by;
(2) in mixed solution a with addition of mixed solution b, c, being 0-50% independently of one another with addition of amount, but is not 0, obtains desulfurization medicament.
4. prepare a method for desulfurization medicament as claimed in one of claims 1-3, the method comprises the following steps:
(1) citric acid, tartaric acid, oxalic acid, copper sulphate are mixed with water respectively, stirring and dissolving, being mixed with mass percent concentration is four parts of solution for later use of 0.5-1.5% independently of one another;
(2) be x:1, x value with copper-bath according to mass ratio respectively by citric acid in step (1), tartaric acid, oxalic acid solution be 1-5, be mixed with a, b, c tri-parts of mixed solutions stand-by;
(3) in mixed solution a with addition of mixed solution b, c, being 0-50% independently of one another with addition of amount, but is not 0, obtains desulfurization medicament.
5. method according to claim 4, wherein the mass percent concentration of four parts of solution is 1.0% in step (1).
6. the method for magnetic iron ore in a flotation removing iron concentrate containing high sulphur, the method comprises the following steps: in floatation process, after the desulfurization medicament according to any one of claim 1-3 having added activation or the desulfurization medicament prepared according to any one of claim 4-5 method, with addition of collecting agent and foaming agent, carry out the flotation of magnetic iron ore in iron concentrate containing high sulphur.
7. method according to claim 6, in described floatation process, point to roughly select, scans and carry out with selected three phases.
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| CN106964493A (en) * | 2017-05-03 | 2017-07-21 | 西安建筑科技大学 | The intensifying method of magnetic iron ore floatability and its application in a kind of high calcium water body |
| CN107199120A (en) * | 2017-07-27 | 2017-09-26 | 中钢集团马鞍山矿山研究院有限公司 | A kind of beneficiation method containing magnetic iron ore, the high-sulfur magnetic iron ore of pyrite |
| CN107694748A (en) * | 2017-11-10 | 2018-02-16 | 内蒙古科技大学 | A kind of method of coal desulfurization drop ash |
| CN107777735A (en) * | 2017-09-19 | 2018-03-09 | 西南科技大学 | A kind of method that ammonium nickel sulfate is prepared with nickel sulfide ore normal pressure |
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| CN110624698A (en) * | 2019-08-15 | 2019-12-31 | 葫芦岛八家矿业股份有限公司 | Method for recovering pyrrhotite from magnetic concentrate |
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| CN113019706A (en) * | 2021-03-15 | 2021-06-25 | 中国恩菲工程技术有限公司 | Flotation method for pyrite inhibited by calcium oxide |
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