CN107670846A - A kind of preparation method and applications of black and white tungsten mineral intergrowth flotation collector - Google Patents

A kind of preparation method and applications of black and white tungsten mineral intergrowth flotation collector Download PDF

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Publication number
CN107670846A
CN107670846A CN201710941709.5A CN201710941709A CN107670846A CN 107670846 A CN107670846 A CN 107670846A CN 201710941709 A CN201710941709 A CN 201710941709A CN 107670846 A CN107670846 A CN 107670846A
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China
Prior art keywords
black
white tungsten
flotation
product
mineral intergrowth
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CN201710941709.5A
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Chinese (zh)
Inventor
黄志强
廖春发
刘汝宽
邱廷省
赵奎
何桂春
黄万抚
余新阳
李立清
周贺鹏
冯博
钟地长
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Jiangxi University of Science and Technology
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Jiangxi University of Science and Technology
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Priority to CN201710941709.5A priority Critical patent/CN107670846A/en
Publication of CN107670846A publication Critical patent/CN107670846A/en
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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
    • 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
    • B03D1/025—Froth-flotation processes adapted for the flotation of fines
    • 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
    • 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
    • B03D2203/04—Non-sulfide ores

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The present invention provides a kind of preparation method and applications of black and white tungsten mineral intergrowth flotation collector, belongs to technical field of beneficiation.The preparation method comprises the following steps：(1) by gutter oil, methanol and the concentrated sulfuric acid gutter oil in mass ratio：Methanol：The concentrated sulfuric acid=1.0~1.2：1.1~1.8：0.05~0.09 mixes, and stirring reaction 5~12 hours, obtains product 1 at 60~90 DEG C；(2) by hydroxylamine hydrochloride, water and sodium hydroxide hydroxylamine hydrochloride in mass ratio：Water：Sodium hydroxide=1.0~1.3：6.4~9.3：1.9~2.4 mix, and stirring reaction 1~3 hour, obtains product 2 at 20~30 DEG C；(3) by the product 1 in mass ratio of product 1：Product 2=1.0~1.2：0.28~0.48 adds in product 2, and stirring reaction 4~6 hours, produce collecting agent at 40~60 DEG C.When collecting agent prepared by the present invention is used for flotation black and white tungsten mineral intergrowth, with good, the strong feature of collecting ability of selectivity, black and white tungsten ore synchronization flotation can be realized, the preparation of collecting agent is gutter oil using raw material in the present invention, so technical scheme is all significant to reducing food security threat etc..

Description

A kind of preparation method and applications of black and white tungsten mineral intergrowth flotation collector
Technical field
The present invention relates to technical field of beneficiation, particularly relate to a kind of black and white tungsten mineral intergrowth flotation collector preparation method and It is applied.
Background technology
Tungsten ore is the Dominant Mineral Resources of China, and China in 2011 is just with the tungsten in the reserves production whole world 83% in the whole world 61%.In The utilization of state's tungsten ore make significant contribution for the product supply of world's tungsten ore.In recent years, tungsten ore production in China's is accumulative verifies storage Amount increases year by year, ends for the end of the year 2014, the resource reserve that tungsten has been verified in China is 720.5 ten thousand t.In January, 2016, Jiangxi Fuliang County Zhu Xi tungsten copper ore deposits find out the t of 333+334 class tungstic acids stock number 2,860,000, have refreshed the record of single tungsten deposit reserves again, into For new tungsten deposit the biggest in the world.For a long time, Chinese tungsten ore resource is developed always based on wolframite.But with black tungsten The increasingly depleted of ore resources, the Beneficiation Feed Grade of tungsten ore are in downward trend year by year, the characteristics of tungsten ore resource " poor, thin, miscellaneous, difficult " also by Gradually show, therefore the utilization of black and white tungsten paragenetic mineral resource are just more and more aobvious important.Floatation process is black and white tungsten symbiosis The most important dressing method of ore deposit, at present, the flotation of black and white tungsten mineral intergrowth mainly use fatty acid collecting agent, but conventional fat The shortcomings that acid collector is that poor selectivity, dosage be big, solubility and bad dispersibility at normal temperatures, is often needed in floatation process Heating is carried out to ore pulp and can be only achieved preferable separating effect.Therefore, research and develop new and effective flotation collector for The utilization of black and white tungsten paragenetic mineral resource and the sustainable development of related industries have very great meaning.
The content of the invention
The present invention is directed to collecting agent poor selectivity present in existing black and white tungsten mineral intergrowth flotation, dosage greatly, at normal temperatures Solubility and the problems such as bad dispersibility, there is provided a kind of preparation method and applications of black and white tungsten mineral intergrowth flotation collector.
The preparation method of the black and white tungsten mineral intergrowth flotation collector comprises the following steps：
(1) by gutter oil, methanol and the concentrated sulfuric acid gutter oil in mass ratio：Methanol：The concentrated sulfuric acid=1.0~1.2：1.1~ 1.8：0.05~0.09 mixing, stirring reaction 5~12 hours at 60~90 DEG C, obtains product 1；
(2) by hydroxylamine hydrochloride, water and sodium hydroxide hydroxylamine hydrochloride in mass ratio：Water：Sodium hydroxide=1.0~1.3：6.4 ~9.3：1.9~2.4 mixing, stirring reaction 1~3 hour at 20~30 DEG C, obtain product 2；
(3) by the product 1 in mass ratio of product 1：Product 2=1.0~1.2：0.28~0.48 adds in product 2,40~ Stirring reaction 4~6 hours at 60 DEG C, produce black and white tungsten mineral intergrowth flotation collector.
The process for carrying out black and white tungsten mineral intergrowth flotation using above-mentioned obtained collecting agent is as follows：
First, by raw ore black and white tungsten symbiotic ore ore grinding to monomer dissociation, inhibitor is then added, adds activator, Gained collecting agent again plus in step (3), finally plus foaming agent, collecting is carried out to black and white tungsten mineral intergrowth, wherein, the total dosage of collecting agent For：400~4000g/t.
Wherein, flotation pulp pH value is 8~13, and slurry pH is adjusted by sodium carbonate or sodium hydroxide.
Inhibitor used is waterglass, and the total dosage of waterglass is 500~5000g/t.
Activator used is plumbi nitras, and the total dosage of plumbi nitras is 300~3000g/t.
Foaming agent used is one kind in No. 2 oil or methyl isobutyl carbinol, and the total dosage of foaming agent is 20~200g/t.
When raw ore is sulfur-bearing black and white tungsten mineral intergrowth, after raw ore ore grinding to monomer dissociation, first with butyl xanthate and No. 2 oil Desulfurization flotation is carried out, wherein, the dosage of butyl xanthate is 50~200g/t, and No. 2 oily dosages are 20~100g/t；Then press again The above method carries out flotation to desulfurization mine tailing.
In above-mentioned floatation process, collecting agent used is added using stoste.
The above-mentioned technical proposal of the present invention has the beneficial effect that：
In such scheme, raw material sources extensively, simple production process, good dispersion, slurry temperature it is applied widely, specifically Advantage is as follows：
(1) raw material gutter oil wide material sources, cost is cheap, and production technology can make full use of threatening environment and food security Gutter oil, realize pollution control and comprehensive utilization double effectses；
(2) simple production process, green technique is belonged to, it is easy to accomplish industrialization, have broad application prospects；
(3) collecting agent is selectively good, soluble in water, good dispersion, is affected by temperature small, has at normal temperatures relatively good Separating effect, excellent floatation indicators can be reached.
Embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with specific implementation Example is described in detail.
The present invention is for collecting agent poor selectivity present in existing black and white tungsten mineral intergrowth flotation, dosage is big, in normal temperature Under solubility and the problems such as bad dispersibility, there is provided a kind of preparation method and applications of black and white tungsten mineral intergrowth flotation collector.
Embodiment 1
One example of the preparation method of black and white tungsten mineral intergrowth flotation collector of the present invention, comprises the following steps：
(1) by gutter oil, methanol and the concentrated sulfuric acid gutter oil in mass ratio：Methanol：The concentrated sulfuric acid=1.0：1.1：0.05 mixing, Stirring reaction 5 hours at 60 DEG C, obtain product 1；
(2) by hydroxylamine hydrochloride, water and sodium hydroxide hydroxylamine hydrochloride in mass ratio：Water：Sodium hydroxide=1.0：6.4：It is 1.9 mixed Close, stirring reaction 1 hour at 20 DEG C, obtain product 2；
(3) by the product 1 in mass ratio of product 1：Product 2=1.0：0.28 adds in product 2, the stirring reaction 4 at 40 DEG C Hour, produce black and white tungsten mineral intergrowth flotation collector.
Embodiment 2
Another example of the preparation method of black and white tungsten mineral intergrowth flotation collector of the present invention, including following step Suddenly：
(1) by gutter oil, methanol and the concentrated sulfuric acid gutter oil in mass ratio：Methanol：The concentrated sulfuric acid=1.2：1.8：0.09 mixing, Stirring reaction 12 hours at 90 DEG C, obtain product 1；
(2) by hydroxylamine hydrochloride, water and sodium hydroxide hydroxylamine hydrochloride in mass ratio：Water：Sodium hydroxide=1.3：9.3：It is 2.4 mixed Close, stirring reaction 3 hours at 30 DEG C, obtain product 2；
(3) by the product 1 in mass ratio of product 1：Product 2=1.2：0.48 adds in product 2, and stirring reaction 6 is small at 60 DEG C When, produce black and white tungsten mineral intergrowth flotation collector.
Embodiment 3
The present embodiment is application example of the black and white tungsten mineral intergrowth flotation collector in flotation black and white tungsten mineral intergrowth.
Certain black and white tungsten mineral intergrowth sample ore, raw ore contain WO30.73%, add carbon after ore ore grinding to mineral monomer is dissociated It is 10 that sour sodium, which adjusts slurry pH, then adds waterglass 1400g/t and makees inhibitor, adds plumbi nitras 620g/t and make activator, Obtained collecting agent 560g/t again plus in embodiment 1, finally plus No. 2 oily 45g/t of foaming agent carry out roughing to black and white tungsten mineral intergrowth Flotation, scan and add 230g/t collecting agents, No. 2 oily 25g/t, primary cleaning adds waterglass 800g/t, and recleaning adds water Glass 700g/t.As a result show that ore deposit WO can be being given effectively by black and white tungsten mineral intergrowth efficient flotation separation using above agentia condition3Contain Under the conditions of amount 0.73%, by one roughing once purging selection and selected twice, obtain containing WO353.92%th, the rate of recovery is 70.16% flotation black and white tungsten bulk concentrate.
Embodiment 4
The present embodiment is that another application of the black and white tungsten mineral intergrowth flotation collector in flotation black and white tungsten mineral intergrowth is real Example.
Certain sulfur-bearing black and white tungsten mineral intergrowth sample ore, raw ore contain WO30.42%, it is first after ore ore grinding to mineral monomer is dissociated Desulfurization flotation is first carried out, desulfurization flotation adds butyl xanthate 70g/t, No. 2 oily 55g/t, then adds sodium carbonate and adjusts slurry pH For 10, then add waterglass 800g/t and make inhibitor, add plumbi nitras 740g/t and make activator, then add and made in embodiment 1 The collecting agent 700g/t obtained, finally plus No. 2 oily 36g/t of foaming agent carry out roughing flotation to black and white tungsten mineral intergrowth, scan addition nitre Lead plumbate 210g/t, collecting agent 310g/t, No. 2 oily 16g/t, primary cleaning addition waterglass 600g/t, recleaning add water glass Glass 500g/t.As a result show that ore deposit WO can be being given effectively by black and white tungsten mineral intergrowth efficient flotation separation using above agentia condition3Content Under the conditions of 0.42%, by one roughing once purging selection and selected twice, obtain containing WO348.95%th, the rate of recovery 73.11% Flotation black and white tungsten bulk concentrate.
Described above is the preferred embodiment of the present invention, it is noted that for those skilled in the art For, on the premise of principle of the present invention is not departed from, some improvements and modifications can also be made, these improvements and modifications It should be regarded as protection scope of the present invention.

Claims (7)

  1. A kind of 1. preparation method of black and white tungsten mineral intergrowth flotation collector, it is characterised in that：Comprise the following steps：
    (1) by gutter oil, methanol and the concentrated sulfuric acid gutter oil in mass ratio：Methanol：The concentrated sulfuric acid=1.0~1.2：1.1~1.8： 0.05~0.09 mixing, stirring reaction 5~12 hours at 60~90 DEG C, obtains product 1；
    (2) by hydroxylamine hydrochloride, water and sodium hydroxide hydroxylamine hydrochloride in mass ratio：Water：Sodium hydroxide=1.0~1.3：6.4~ 9.3：1.9~2.4 mixing, stirring reaction 1~3 hour at 20~30 DEG C, obtain product 2；
    (3) by the product 1 in mass ratio of product 1：Product 2=1.0~1.2：0.28~0.48 adds in product 2, at 40~60 DEG C Lower stirring reaction 4~6 hours, produce black and white tungsten mineral intergrowth flotation collector.
  2. 2. the application of black and white tungsten mineral intergrowth flotation collector according to claim 1, it is characterised in that：First, by raw ore Then black and white tungsten symbiotic ore ore grinding adds inhibitor, adds activator, then add gained in step (3) to catch to monomer dissociation Agent is received, finally adds foaming agent, collecting is carried out to black and white tungsten mineral intergrowth, wherein, the total dosage of collecting agent is：400~4000g/t.
  3. 3. the application of black and white tungsten mineral intergrowth flotation collector according to claim 2, it is characterised in that：The flotation pulp PH value is 8~13, and slurry pH is adjusted by sodium carbonate or sodium hydroxide.
  4. 4. the application of black and white tungsten mineral intergrowth flotation collector according to claim 2, it is characterised in that：The inhibitor is Waterglass, the total dosage of waterglass are 500~5000g/t.
  5. 5. the application of black and white tungsten mineral intergrowth flotation collector according to claim 2, it is characterised in that：The activator is Plumbi nitras, the total dosage of plumbi nitras are 300~3000g/t.
  6. 6. the application of black and white tungsten mineral intergrowth flotation collector according to claim 2, it is characterised in that：The foaming agent is One kind in No. 2 oil or methyl isobutyl carbinol, the total dosage of foaming agent are 20~200g/t.
  7. 7. the application of black and white tungsten mineral intergrowth flotation collector according to claim 2, it is characterised in that：When raw ore is sulfur-bearing During black and white tungsten mineral intergrowth, after raw ore ore grinding to monomer dissociation, desulfurization flotation first is carried out with butyl xanthate and No. 2 oil, wherein, fourth The dosage of base xanthate is 50~200g/t, and No. 2 oily dosages are 20~100g/t；Then desulfurization mine tailing is entered according to the method again Row flotation.
CN201710941709.5A 2017-10-11 2017-10-11 A kind of preparation method and applications of black and white tungsten mineral intergrowth flotation collector Withdrawn CN107670846A (en)

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Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4054442A (en) * 1976-02-23 1977-10-18 Union Carbide Corporation Method for recovering scheelite from tungsten ores by flotation
GB2154564A (en) * 1984-02-27 1985-09-11 Amax Inc Extraction of minerals containing tungsten
CN1133265A (en) * 1995-10-23 1996-10-16 北京矿冶研究总院 Beneficiation method for recovering wolframite and scheelite from complex polymetallic ore
CN1600444A (en) * 2004-10-27 2005-03-30 广州有色金属研究院 Mineral dressing method for black and white tungsten minerals
CN102211053A (en) * 2011-05-27 2011-10-12 广州有色金属研究院 Method for separating black and white tungsten bulk flotation rough concentrates
CN105413856A (en) * 2015-12-31 2016-03-23 赣州有色冶金研究所 Mineral separation method and system for recovering wolframite and scheelite in tungsten fine slime
CN107185723A (en) * 2017-07-26 2017-09-22 平顶山华兴浮选工程技术服务有限公司 A kind of low-grade bauxite direct flotation collecting agent and preparation method thereof

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4054442A (en) * 1976-02-23 1977-10-18 Union Carbide Corporation Method for recovering scheelite from tungsten ores by flotation
GB2154564A (en) * 1984-02-27 1985-09-11 Amax Inc Extraction of minerals containing tungsten
CN1133265A (en) * 1995-10-23 1996-10-16 北京矿冶研究总院 Beneficiation method for recovering wolframite and scheelite from complex polymetallic ore
CN1600444A (en) * 2004-10-27 2005-03-30 广州有色金属研究院 Mineral dressing method for black and white tungsten minerals
CN102211053A (en) * 2011-05-27 2011-10-12 广州有色金属研究院 Method for separating black and white tungsten bulk flotation rough concentrates
CN105413856A (en) * 2015-12-31 2016-03-23 赣州有色冶金研究所 Mineral separation method and system for recovering wolframite and scheelite in tungsten fine slime
CN107185723A (en) * 2017-07-26 2017-09-22 平顶山华兴浮选工程技术服务有限公司 A kind of low-grade bauxite direct flotation collecting agent and preparation method thereof

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