CN108554644B - A kind of tin-lead soldering collecting agent and preparation method thereof - Google Patents

A kind of tin-lead soldering collecting agent and preparation method thereof Download PDF

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Publication number
CN108554644B
CN108554644B CN201810029322.7A CN201810029322A CN108554644B CN 108554644 B CN108554644 B CN 108554644B CN 201810029322 A CN201810029322 A CN 201810029322A CN 108554644 B CN108554644 B CN 108554644B
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Prior art keywords
collecting agent
tin
lead soldering
agent
parts
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Expired - Fee Related
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CN201810029322.7A
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CN108554644A (en
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刘杰
宫贵臣
韩跃新
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Northeastern University China
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Northeastern University China
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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
    • B03D2203/04Non-sulfide ores

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

Abstract

The invention discloses one kind to be used for tin-lead soldering collecting agent, which is characterized in that is made of main collecting agent, solubilizer and supplementary catching agent;Wherein, the main collecting agent is positive dodecyl phosphonic acid, and the solubilizer is sodium carbonate, and the supplementary catching agent is fatty alcohol.The preparation process of the collecting agent are as follows: mix dodecyl phosphonic acids in mass ratio with sodium carbonate, after the stirring of the mixing speed of 500~1000rad/min is configured to homogeneous solution in 5~10 minutes, the fatty alcohol of certain mass is added, stirs 3~5min, tin-lead soldering combined capturing and collecting agent can be obtained.The present invention has good water solubility, collecting ability is strong, and foam is uniform, and dispersibility is good, the advantages such as easy to use compared with conventional collectors for cassiterite.

Description

A kind of tin-lead soldering collecting agent and preparation method thereof
Technical field
The present invention relates to technical field of mineral processing, more particularly to a kind of tin-lead soldering collecting agent and preparation method thereof.
Background technique
The development of tin-lead soldering collecting agent is always one of the important pushing factor of tin-lead soldering technological progress.It is used for earliest The collecting agent of tin-lead soldering is fatty acid and its soaps, such as oleic acid, but the selectivity of this kind of collecting agent is very poor, cannot be effective Ground is separated by cassiterite from gangue mineral.Later a series of new type collectors for cassiterite is just constantly developed, In include arsine acid collector, this collecting agent is selectively good, once once obtains large-scale industrial application, but due to it Strong toxicity, can cause damages to human health and environment, stop using now;Collecting energy of the alkyl sulfate to cassiterite Power is strong, but its using effect is affected by metal ion in ore pulp, and be suitable for application pH condition in acidic environment, no It is suitble to industrial application;The selectivity of hydroximic acid collecting agent is strong, but collecting ability is insufficient, and dosage is excessive, limits this catch Receive the large-scale application of agent;Alkyl sulfosuccinamate is that a kind of collecting ability is strong, cheap, nontoxic collecting Agent, but the problem of equally exist poor selectivity.It is great that the appearance of phosphonic acid collecting agent really produces the flotation of cassiterite Progress, this kind of collecting agent includes aromatic radical phosphonic acids and alkyl phosphonic acid.Wherein the styryl phosphonic acid in aromatic radical phosphonic acids is most to hold It is easily-synthesized also most efficient phosphonic acid collectors for cassiterite, has industrially obtained large-scale application, but styrene phosphine The optimal use pH value of acid is 4 or so, and the time of sizing mixing needed in use process is long, usually at 1 more than hour.Alkane Short chain phosphonic acids (C in base phosphonic acids5-C7) collecting cassiterite scarce capacity, need to add heavy metal ion (such as plumbi nitras) as activation Agent, this will cause environmental pollution;The alkyl phosphonic acid of long hydrocarbon chain has stronger collecting ability, but its water solubility to cassiterite Deficiency, dispersibility is poor, inconvenient to use.Therefore, it is caught in order to solve the above technical problems, needing to provide the new tin-lead soldering of one kind Receive agent.
Summary of the invention
The object of the present invention is to provide a kind of tin-lead soldering collecting agents and preparation method thereof, are deposited with solving the above-mentioned prior art The problem of, make it have good water solubility, collecting ability is strong, and foam is uniform, and dispersibility is good, it is easy to use the advantages that, with reality The separation of cassiterite and gangue mineral, obtains high-grade cassiterite concentrate in present flotation.
To achieve the above object, the present invention provides following schemes:
The present invention provides a kind of tin-lead soldering collecting agent, it is characterised in that: by main collecting agent, solubilizer and auxiliary collecting Agent composition;Wherein, the main collecting agent is positive dodecyl phosphonic acid, and the solubilizer is sodium carbonate, the supplementary catching agent For fatty alcohol.
Preferably, the fatty alcohol is one of n-butanol, glycerine, n-hexyl alcohol, the tert-butyl alcohol.
Preferably, as mass fraction, 100 parts of the dodecyl phosphonic acids, 50~70 parts of the sodium carbonate, the rouge 100 parts of fat alcohol.
Preferably, slurry pH is first adjusted to 4~10, then in ore pulp when carrying out flotation by tin-lead soldering collecting agent After gangue mineral inhibitor is added, tin-lead soldering collecting agent is added into ore pulp according to certain dosage, after sufficiently being acted on ore pulp, Carry out flotation.
Preferably, the mineral inhibitor is made of carboxymethyl cellulose and sodium metasilicate, by weight, the carboxymethyl 20~200 parts of cellulose, 20~200 parts of the sodium metasilicate.
Preferably, by weight, 100~1000 parts of the tin-lead soldering collecting agent.
The present invention also provides a kind of preparation methods of tin-lead soldering collecting agent, which comprises the steps of: In Under room temperature, dodecyl phosphonic acids is mixed in mass ratio with sodium carbonate, in the mixing speed of 500~1000rad/min After 5~10min of lower stirring is configured to homogeneous solution, the fatty alcohol of certain mass is added, obtains tin-lead soldering after stirring 3~5min Collecting agent.
Preferably, as mass fraction, 100 parts of the dodecyl phosphonic acids, 50~70 parts of the sodium carbonate, the rouge 100 parts of fat alcohol.
The invention discloses following technical effects:
Cassiterite combined capturing and collecting agent preparation of the invention is simple, has good dispersion in ore pulp, foam size distribution uniformly, Collecting ability is strong, stability is good, good water solubility, advantage easy to use, floatation indicators are high and stable.
Detailed description of the invention
Fig. 1 is flotation artificial mixed ore flow diagram of the present invention;
Fig. 2 is Flotation of Cassiterite green ore flow diagram of the present invention.
Specific embodiment
It is clearly and completely described below in conjunction with the technical solution in the embodiment of the present invention, it is clear that described reality Applying example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is general Logical technical staff every other embodiment obtained without making creative work belongs to what the present invention protected Range.
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, With reference to embodiment The present invention is described in further detail.
Embodiment 1
(1) preparation of tin-lead soldering collecting agent
At room temperature, dodecyl phosphonic acids is mixed in mass ratio with sodium carbonate, in 500~1000rad/min Mixing speed under after 5~10min of stirring is configured to homogeneous solution, be added the glycerine of certain mass, stir after 3~5min To tin-lead soldering collecting agent, dodecyl phosphonic acids: sodium carbonate: glycerine=100:50:100.
(2) flotation of artificial mixed ore
The ratio of cassiterite minal, quartzy minal and fluorite minal 1:2:2 in mass ratio is mixed, 50g is taken to mix Mine after being dispersed with stirring composite ore addition agitator, adjusts slurry pH to after 4~10 with sodium hydroxide and sulfuric acid, carboxylic is added Then tin-lead soldering collecting agent 600g/t is added as gangue mineral inhibitor in methylcellulose 80g/t, sodium metasilicate 80g/t, right 50g composite ore carry out flotation, flotation flowsheet as shown in Figure 1, obtain tin grade be 62.14%, the tin rate of recovery be 73.31% tin Stone concentrate.
Embodiment 2
(1) preparation of tin-lead soldering collecting agent
At room temperature, dodecyl phosphonic acids is mixed in mass ratio with sodium carbonate, in 500~1000rad/min Mixing speed under after 5~10min of stirring is configured to homogeneous solution, be added the n-butanol of certain mass, stir after 3~5min To tin-lead soldering collecting agent, dodecyl phosphonic acids: sodium carbonate: n-butanol=100:70:100.
(2) flotation of artificial mixed ore
The ratio of cassiterite minal, quartzy minal and fluorite minal 1:2:2 in mass ratio is mixed, 50g is taken to mix Mine after being dispersed with stirring composite ore addition agitator, adjusts slurry pH to after 4~10 with sodium hydroxide and sulfuric acid, carboxylic is added Then tin-lead soldering collecting agent 600g/t is added as gangue mineral inhibitor in methylcellulose 100g/t, sodium metasilicate 100g/t, Flotation is carried out to 50g composite ore, for flotation flowsheet as shown in Figure 1, obtaining tin grade is 60.88%, the tin rate of recovery is 74.15% Cassiterite concentrate.
Embodiment 3
(1) preparation of tin-lead soldering collecting agent
At room temperature, dodecyl phosphonic acids is mixed in mass ratio with sodium carbonate, in 500~1000rad/min Mixing speed under after 5~10min of stirring is configured to homogeneous solution, be added the n-hexyl alcohol of certain mass, stir after 3~5min To tin-lead soldering collecting agent, dodecyl phosphonic acids: sodium carbonate: n-hexyl alcohol=100:60:100.
(2) flotation of artificial mixed ore
The ratio of cassiterite minal, quartzy minal and fluorite minal 1:2:2 in mass ratio is mixed, 50g is taken to mix Mine after being dispersed with stirring composite ore addition agitator, adjusts slurry pH to after 4~10 with sodium hydroxide and sulfuric acid, carboxylic is added Then tin-lead soldering collecting agent 600g/t is added as gangue mineral inhibitor in methylcellulose 100g/t, sodium metasilicate 100g/t, Flotation is carried out to 50g composite ore, for flotation flowsheet as shown in Figure 1, obtaining tin grade is 61.44%, the tin rate of recovery is 75.35% Cassiterite concentrate.
Embodiment 4
(1) preparation of tin-lead soldering collecting agent
At room temperature, dodecyl phosphonic acids is mixed in mass ratio with sodium carbonate, in 500~1000rad/min Mixing speed under after 5~10min of stirring is configured to homogeneous solution, be added the tert-butyl alcohol of certain mass, stir after 3~5min To tin-lead soldering collecting agent, dodecyl phosphonic acids: sodium carbonate: the tert-butyl alcohol=100:60:100.
(2) flotation of artificial mixed ore
The ratio of cassiterite minal, quartzy minal and fluorite minal 1:2:2 in mass ratio is mixed, 50g is taken to mix Mine after being dispersed with stirring composite ore addition agitator, adjusts slurry pH to after 4~10 with sodium hydroxide and sulfuric acid, carboxylic is added Then tin-lead soldering collecting agent 600g/t is added as gangue mineral inhibitor in methylcellulose 100g/t, sodium metasilicate 100g/t, Flotation is carried out to 50g artificial mixed ore, as shown in Figure 1, obtaining tin grade is 61.83%, the tin rate of recovery is flotation flowsheet 74.50% cassiterite concentrate.
Embodiment 5
(1) preparation of tin-lead soldering collecting agent
At room temperature, dodecyl phosphonic acids is mixed in mass ratio with sodium carbonate, in 500~1000rad/min Mixing speed under after 5~10min of stirring is configured to homogeneous solution, be added the tert-butyl alcohol of certain mass, stir after 3~5min To tin-lead soldering collecting agent, dodecyl phosphonic acids: sodium carbonate: glycerine=100:50:100.
(2) flotation of cassiterite green ore
It chooses Yunnan Province's cassiterite green ore 300g to be added in flotation device, tin grade is 0.38% in raw ore, uses hydroxide Sodium and sulfuric acid adjust slurry pH to after 4~10, sweep two essences according to shown in Fig. 2 one thick three, that chats sequence returns is closed circuit floating Process is selected to carry out flotation.In rougher process, carboxymethyl cellulose 150g/t, sodium metasilicate 150g/t is added and inhibits as gangue mineral Then tin-lead soldering collecting agent 800g/t is added in agent;During scanning, tin-lead soldering collecting agent 400g/t is added;Refining process In, gangue inhibitor carboxymethyl cellulose dosage is 80g/t, the dosage of sodium metasilicate is 80g/t.Carboxymethyl cellulose 80g/ is added T, sodium metasilicate 80g/t is as gangue mineral inhibitor;Obtaining tin grade is 61.83%, the cassiterite essence that the tin rate of recovery is 74.50% Mine.
Embodiment described above is only that preferred embodiment of the invention is described, and is not carried out to the scope of the present invention It limits, without departing from the spirit of the design of the present invention, those of ordinary skill in the art make technical solution of the present invention Various changes and improvements, should all fall into claims of the present invention determine protection scope in.

Claims (2)

1. a kind of tin-lead soldering collecting agent, it is characterised in that: be made of main collecting agent, solubilizer and supplementary catching agent;Wherein, The main collecting agent is positive dodecyl phosphonic acid, and the solubilizer is sodium carbonate, and the supplementary catching agent is fatty alcohol;
The fatty alcohol is one of n-butanol, glycerine, n-hexyl alcohol, the tert-butyl alcohol;
As mass fraction, 100 parts of the dodecyl phosphonic acids, 50~70 parts of the sodium carbonate, 100 parts of the fatty alcohol;
The preparation method of tin-lead soldering collecting agent includes the following steps: at room temperature, by dodecyl phosphonic acids and carbonic acid Sodium mixes in mass ratio, after 5~10min of stirring is configured to homogeneous solution under the mixing speed of 500~1000rad/min, adds Enter the fatty alcohol of certain mass, obtains tin-lead soldering collecting agent after stirring 3~5min.
2. a kind of application of tin-lead soldering collecting agent as described in claim 1: it is characterized in that, when flotation, first by pH values of pulp Value is adjusted to 4~10, and after gangue mineral inhibitor then is added in ore pulp, tin-lead soldering is added into ore pulp according to certain dosage Collecting agent after sufficiently acting on ore pulp, carries out flotation;
Mineral inhibitor is made of carboxymethyl cellulose and sodium metasilicate, by weight, the carboxymethyl cellulose 20~200 Part, 20~200 parts of the sodium metasilicate;
By weight, 100~1000 parts of the tin-lead soldering collecting agent.
CN201810029322.7A 2018-01-12 2018-01-12 A kind of tin-lead soldering collecting agent and preparation method thereof Expired - Fee Related CN108554644B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109174460B (en) * 2018-09-25 2020-11-06 东北大学 Cassiterite flotation method
CN113058749A (en) * 2021-04-06 2021-07-02 昆明理工大学 Depression activating agent for cassiterite flotation and preparation method and application thereof
CN113333173B (en) * 2021-05-13 2022-06-21 西北矿冶研究院 Beneficiation reagent for tin flotation of tin ore and preparation method thereof
CN113275130A (en) * 2021-06-08 2021-08-20 青岛鑫润矿业科技有限公司 Cheaper cassiterite flotation auxiliary collecting agent

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU624652A1 (en) * 1976-06-10 1978-09-25 Предприятие П/Я А-1997 Collector for flotation of tin-containing ores
SU638378A1 (en) * 1977-03-11 1978-12-25 Центральный Научно-Исследовательский Институт Оловянной Промышленности "Цнииолово" Министерства Цветной Металлургии Ссср Collector for flotation cassiterite from ores
CN104549765A (en) * 2014-11-21 2015-04-29 广西大学 Preparation method for cassiterite mineral collector
CN105149107A (en) * 2015-07-13 2015-12-16 中南大学 Application of phosphoric acid ester compound to flotation of calcium-containing minerals
CN105772226A (en) * 2016-03-16 2016-07-20 云南缘矿科技开发有限公司 Flotation activating agent for fine-grain cassiterite and preparing method of flotation activating agent
CN106861919A (en) * 2017-04-28 2017-06-20 中南大学 A kind of tin-lead soldering collecting agent and its application
CN107520062A (en) * 2017-10-11 2017-12-29 江西理工大学 A kind of preparation method and applications of tin fines stone ore flotation collector

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
SU624652A1 (en) * 1976-06-10 1978-09-25 Предприятие П/Я А-1997 Collector for flotation of tin-containing ores
SU638378A1 (en) * 1977-03-11 1978-12-25 Центральный Научно-Исследовательский Институт Оловянной Промышленности "Цнииолово" Министерства Цветной Металлургии Ссср Collector for flotation cassiterite from ores
CN104549765A (en) * 2014-11-21 2015-04-29 广西大学 Preparation method for cassiterite mineral collector
CN105149107A (en) * 2015-07-13 2015-12-16 中南大学 Application of phosphoric acid ester compound to flotation of calcium-containing minerals
CN105772226A (en) * 2016-03-16 2016-07-20 云南缘矿科技开发有限公司 Flotation activating agent for fine-grain cassiterite and preparing method of flotation activating agent
CN106861919A (en) * 2017-04-28 2017-06-20 中南大学 A kind of tin-lead soldering collecting agent and its application
CN107520062A (en) * 2017-10-11 2017-12-29 江西理工大学 A kind of preparation method and applications of tin fines stone ore flotation collector

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