CN107520063A - A kind of preparation method and applications of Rare Earth Mine flotation collector - Google Patents

A kind of preparation method and applications of Rare Earth Mine flotation collector Download PDF

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Publication number
CN107520063A
CN107520063A CN201710941687.2A CN201710941687A CN107520063A CN 107520063 A CN107520063 A CN 107520063A CN 201710941687 A CN201710941687 A CN 201710941687A CN 107520063 A CN107520063 A CN 107520063A
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China
Prior art keywords
rare earth
product
earth mine
flotation collector
mass ratio
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CN201710941687.2A
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CN107520063B (en
Inventor
黄志强
廖春发
邱廷省
赵奎
何桂春
黄万抚
余新阳
李立清
周贺鹏
冯博
刘汝宽
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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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/018Mixtures of inorganic and organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/02Collectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION 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
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; specified applications
    • B03D2203/02Ores

Abstract

The present invention provides a kind of preparation method and applications of Rare Earth Mine 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.The Rare Earth Mine efficient flotation separation collecting agent of the present invention, solve existing flotation collector cost height, poor selectivity, not easy to operate in production, cause the technological process of production complicated with rare earth ore concentrate grade, rate of recovery index is undesirable the problem of.

Description

A kind of preparation method and applications of Rare Earth Mine flotation collector
Technical field
The present invention relates to technical field of beneficiation, particularly relates to a kind of preparation method of Rare Earth Mine flotation collector and its answers With.
Background technology
Rare earth is widely distributed in the earth's crust, and species is a lot, and it has been established that, and the mineral containing rare earth just have kind more than 250.But have The mineral for having industrial value only have ten several, including monazite, bastnaesite, parisite, cordylite, silicon beryllium yttrium Ore deposit, nuevite, euxenite, xenotime, fergusonite etc., wherein monazite, bastnaesite and xenotime be it is most important simultaneously And 3 kinds of rare-earth minerals that yield is maximum.China's rare earth resources rich reserves, according to 2010 and the United States Federal's geology in 2014 The data that investigation bureau announces, China rare earth stock number is fifty-five million ton, accounts for 40%~50% or so of world's gross reserves.China is dilute Soil resource is mainly distributed on the ground such as the Inner Mongol, Sichuan, Jiangxi, Guangdong and Guangxi Provinces and Fujian, and wherein Bayan Obo iron content-rare earth mineral deposit is for I State has found out the maximum mineral deposit of stock number, and its stock number accounts for 96% or so of national total amount.In the industrial production, flotation is rare earth Ore deposit sorts the most frequently used also one of most efficient method, and wherein flotation collector is the key factor for influenceing flotation effect.At present, it is dilute Tu Kuang flotation mainly uses hydroximic acid collecting agent, but is that cost is high, selective the shortcomings that conventional hydroximic acid collecting agent With collecting performance is poor, reagent toxicity is high.Therefore, exploitation profit of the new and effective flotation collector for rare-earth ore resource is researched and developed There is very great meaning with the sustainable development with related industries.
The content of the invention
The present invention is for collecting agent cost present in existing Rare Earth Mine flotation is high, selectivity and collecting performance are poor, medicament poison A kind of the problems such as property is high, there is provided preparation method and applications of Rare Earth Mine flotation collector.
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 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 Rare Earth Mine flotation collector.
The process for carrying out Rare Earth Mine flotation using above-mentioned obtained collecting agent is as follows:
First, by raw ore rare earth ore ore grinding to monomer dissociation, inhibitor is then added, then adds gained in step (3) to catch Agent is received, finally adds foaming agent, collecting is carried out to Rare Earth Mine, wherein, the total dosage of collecting agent is:1000~9000g/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 2000~8000g/t.
Foaming agent used is one kind in No. 2 oil or methyl isobutyl carbinol, and the total dosage of foaming agent is 60~600g/t.
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, it is simple production process, good dispersion, environment-friendly, specific 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 cost present in existing Rare Earth Mine flotation is high, selectivity and collecting performance are poor, medicament A kind of the problems such as toxicity is high, there is provided preparation method and applications of Rare Earth Mine flotation collector.
Embodiment 1
One example of the preparation method of Rare Earth Mine 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 Rare Earth Mine flotation collector.
Embodiment 2
Another example of the preparation method of Rare Earth Mine 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=1.2:1.8:0.09 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 Rare Earth Mine flotation collector.
Embodiment 3
The present embodiment is application example of the Rare Earth Mine flotation collector in flotation of rare earth ore deposit.
Certain Rare Earth Mine sample ore, raw ore contain REO 10.18%, and adding sodium carbonate after ore ore grinding to mineral monomer is dissociated adjusts Slurry pH is 8, then adds waterglass 4100g/t and makees inhibitor, then adds obtained collecting agent 3200g/t in embodiment 1, most Afterwards plus No. 2 oily 58g/t of foaming agent carry out roughing flotation to Rare Earth Mine, scan and add 600g/t collecting agents, No. 2 oily 25g/t, once Selected addition waterglass 550g/t, recleaning add waterglass 350g/t.As a result show can have using above agentia condition Effect is by Rare Earth Mine efficient flotation separation, under the conditions of to ore deposit REO contents 10.18%, by one roughing once purging selection and selected twice, It is 90.16% flotation of rare earth concentrate to obtain containing REO 66.92%, the rate of recovery.
Embodiment 4
The present embodiment is another application example of the Rare Earth Mine flotation collector in flotation of rare earth ore deposit.
Certain Rare Earth Mine sample ore, raw ore contain REO 3.68%, and adding sodium carbonate after ore ore grinding to mineral monomer is dissociated adjusts Slurry pH is 9, then adds waterglass 1200g/t and makees inhibitor, then adds obtained collecting agent 1300g/t in embodiment 1, most Afterwards plus No. 2 oily 88g/t of foaming agent carry out roughing flotation to Rare Earth Mine, scan and add waterglass 600g/t, collecting agent 600g/t, 2 Number oily 50g/t, primary cleaning add waterglass 340g/t, and recleaning adds waterglass 120g/t, and triple cleaning adds water glass Glass 120g/t.As a result showing can be effectively by Rare Earth Mine efficient flotation separation, to ore deposit REO contents 3.68% using above agentia condition Under the conditions of, by one roughing once purging selection and triple cleaning, it is that 92.19% flotation is dilute to obtain containing REO 61.04%, the rate of recovery Native 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 (5)

  1. A kind of 1. preparation method of Rare Earth Mine 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, produces Rare Earth Mine flotation collector.
  2. 2. the application of Rare Earth Mine flotation collector according to claim 1, it is characterised in that:First, by raw ore Rare Earth Mine Then stone mill ore deposit adds inhibitor to monomer dissociation, then add gained collecting agent in step (3), finally plus foaming agent, to Rare Earth Mine Collecting is carried out, wherein, the total dosage of collecting agent is:1000~9000g/t.
  3. 3. the application of Rare Earth Mine flotation collector according to claim 2, it is characterised in that:The flotation pulp pH value is 8~13, slurry pH is adjusted by sodium carbonate or sodium hydroxide.
  4. 4. the application of Rare Earth Mine flotation collector according to claim 2, it is characterised in that:The inhibitor is water glass Glass, the total dosage of waterglass are 2000~8000g/t.
  5. 5. the application of Rare Earth Mine flotation collector according to claim 2, it is characterised in that:The foaming agent is No. 2 oil Or one kind in methyl isobutyl carbinol, the total dosage of foaming agent are 60~600g/t.
CN201710941687.2A 2017-10-11 2017-10-11 Preparation method and application of rare earth ore flotation collector Active CN107520063B (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110813541A (en) * 2019-10-24 2020-02-21 商洛学院 Collector combination for flotation of monazite and xenotime from fine-grained seashore placer
CN110813540A (en) * 2019-10-24 2020-02-21 商洛学院 Collecting agent composition for flotation and recovery of monazite from zircon heavy sand
CN110947520A (en) * 2019-10-28 2020-04-03 中国地质科学院矿产综合利用研究所 Collecting agent for reverse flotation of medium-low grade collophanite, preparation method and application
CN110976096A (en) * 2019-11-15 2020-04-10 南华大学 Beneficiation method for rare earth ore

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS55119456A (en) * 1979-03-08 1980-09-13 Dowa Mining Co Ltd Floatation method of bastnaesite
JPS60238173A (en) * 1984-05-12 1985-11-27 Kobe Steel Ltd Flotation of rare earth mineral
CN86100710A (en) * 1986-01-24 1987-08-05 冶金工业部包头稀土研究院 A kind of synthesis technique of rare earth catching agent
CN1114596A (en) * 1994-07-07 1996-01-10 金仲农 Method for preparation of collecting agent of oxidized ore
CN1403204A (en) * 2001-09-11 2003-03-19 上海第二工业大学 RE mineral floating process
CN102500465A (en) * 2011-11-22 2012-06-20 广州有色金属研究院 Benefication method for bastnaesite
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
JPS55119456A (en) * 1979-03-08 1980-09-13 Dowa Mining Co Ltd Floatation method of bastnaesite
JPS60238173A (en) * 1984-05-12 1985-11-27 Kobe Steel Ltd Flotation of rare earth mineral
CN86100710A (en) * 1986-01-24 1987-08-05 冶金工业部包头稀土研究院 A kind of synthesis technique of rare earth catching agent
CN1114596A (en) * 1994-07-07 1996-01-10 金仲农 Method for preparation of collecting agent of oxidized ore
CN1403204A (en) * 2001-09-11 2003-03-19 上海第二工业大学 RE mineral floating process
CN102500465A (en) * 2011-11-22 2012-06-20 广州有色金属研究院 Benefication method for bastnaesite
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

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110813541A (en) * 2019-10-24 2020-02-21 商洛学院 Collector combination for flotation of monazite and xenotime from fine-grained seashore placer
CN110813540A (en) * 2019-10-24 2020-02-21 商洛学院 Collecting agent composition for flotation and recovery of monazite from zircon heavy sand
CN110813540B (en) * 2019-10-24 2021-11-26 商洛学院 Collecting agent composition for flotation and recovery of monazite from zircon heavy sand
CN110947520A (en) * 2019-10-28 2020-04-03 中国地质科学院矿产综合利用研究所 Collecting agent for reverse flotation of medium-low grade collophanite, preparation method and application
CN110976096A (en) * 2019-11-15 2020-04-10 南华大学 Beneficiation method for rare earth ore

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