CN112892877A - Method for separating and floating calcite of fluorite and gangue minerals - Google Patents

Method for separating and floating calcite of fluorite and gangue minerals Download PDF

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Publication number
CN112892877A
CN112892877A CN202110057026.XA CN202110057026A CN112892877A CN 112892877 A CN112892877 A CN 112892877A CN 202110057026 A CN202110057026 A CN 202110057026A CN 112892877 A CN112892877 A CN 112892877A
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Prior art keywords
fluorite
flotation
calcite
mineral
ore
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CN202110057026.XA
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Inventor
倪晨权
罗旭彪
任重
刘畅
畅子雯
曾桂生
杨利明
邵鹏辉
熊贞晟
刘廷玺
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Nanchang Hangkong University
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Nanchang Hangkong University
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Priority to CN202110057026.XA priority Critical patent/CN112892877A/en
Publication of CN112892877A publication Critical patent/CN112892877A/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
    • B03D1/02—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
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B1/00—Conditioning for facilitating separation by altering physical properties of the matter to be treated
    • 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
    • B03D1/011—Quaternary ammonium 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
    • 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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  • Manufacture And Refinement Of Metals (AREA)

Abstract

A method for separating and floating calcite of fluorite and gangue minerals relates to a method for separating the calcite of fluorite and gangue minerals. The invention aims to solve the technical problem that the selectivity of the existing fluorite cation collector is poor after the pH value of a flotation system is increased. The method is used for mineral flotation and collection, the recovery rate of fluorite after the pure fluorite mineral is floated can reach 92.31 percent, and the recovery rate of calcite after the pure calcite mineral is floated can reach 18.36 percent; in the manual mixed ore experiment, the recovery rate of fluorite can reach 99.23%, and the grade of fluorite can reach 77.96%. The method has the advantages of high efficiency, high selectivity, simple use process, simple medicament system and good flotation effect.

Description

Method for separating and floating calcite of fluorite and gangue minerals
Technical Field
The invention relates to a method for separating fluorite and gangue mineral calcite.
Background
Fluorite is a strategic mineral, and industrially significant fluorite deposits are distributed around the world. The method of separation of fluorite ore depends on its end use: the separation method of the metallurgical grade fluorite concentrate comprises gravity separation and magnetic separation. Flotation is the main separation method for producing acid-grade fluorite concentrate. Since the crystal lattices of both minerals contain the same Ca2+The preferred flotation of fluorite and calcite presents a number of problems. Due to the similar surface physicochemical properties of the two minerals, the anion collecting agent is difficult to efficiently separate fluorite and calcite due to the low selectivity, and the calcite inhibitor can inhibit the floatation of the fluorite. The traditional calcite and fluorite separation method is complex in reagent and general in separation efficiency.
Compared with the traditional anionic collector sodium oleate, the cationic quaternary ammonium collector has stronger floatation capability on fluorite, but is not easy to select the collector capable of realizing the calcite floatation of fluorite and gangue minerals, and meanwhile, the existing cationic collector has the problem that the selectivity is poor after the pH value of a floatation system is improved. Furthermore, in order to meet the requirement of floatably separating the fluorite and the gangue mineral calcite, the collecting agent with simple use process and simple medicament system is provided more difficultly.
Therefore, the collecting agent has high selectivity, stable high selectivity in flotation under the condition of high pH value, simple and convenient use process and simple medicament system, and has great industrial value for the field of calcite flotation of fluorite and gangue minerals.
Disclosure of Invention
The invention provides a method for separating and floating fluorite and gangue mineral calcite, and aims to solve the technical problem that the selectivity of the existing fluorite cation collector is poor after the pH value of a flotation system is increased.
The method for separating and floating the calcite of fluorite and gangue minerals comprises the following steps:
mixing a mineral sample with water, and then carrying out primary size mixing to obtain primary size; the granularity of the ore sample is 0.038-0.074 mm; the mass ratio of the ore sample to the water is 1 (15-20); the first size mixing mode is stirring, the stirring time is 1-2 min, and the used equipment is a flotation machine; the ore sample is a fluorite ore sample or a calcite ore sample;
adjusting the pH value of the primary slurry obtained in the step one to be 6-11, and then carrying out secondary size mixing to obtain ore pulp; adjusting the pH value of the primary slurry obtained in the first adjusting step by using an HCl aqueous solution and an NaOH aqueous solution; the second slurry mixing mode is stirring, the stirring time is 2-3 min, and the used equipment is a flotation machine;
thirdly, adding a collecting agent into the ore pulp obtained in the second step, uniformly stirring, and then carrying out mineral flotation and foam scraping, wherein the flotation time is 2-5 min, and the used equipment is a flotation machine, so as to obtain concentrate (foam product) and tailings; the dosage of the collecting agent relative to the ore pulp is 0.1 multiplied by 10-4mol/L～2×10-4mol/L；
The preparation method of the collecting agent comprises the following steps: dissolving 1, 6-dibromohexane and dodecyl tertiary amine in ethanol, and then carrying out quaternization reaction to obtain a collecting agent;
the molar ratio of the 1, 6-dibromohexane to the dodecyl tertiary amine is 1 (2-2.5); the dosage of the ethanol is based on the condition that the 1, 6-dibromohexane and the dodecyl tertiary amine can be fully dissolved; the quaternization reaction is carried out under a protective atmosphere; the quaternization reaction is carried out under the condition of oil bath reflux, the oil bath reflux temperature is 70-100 ℃, and the oil bath reflux time is 24-72 hours.
The collecting agent prepared in the third step of the invention has low toxicity and no pollution, has stronger electrostatic adsorption, hydrogen bond adsorption and physical adsorption with fluorite, and has high selectivity for fluorite; the pH range applicable to flotation is wide; and the complex formulation with other collectors is not needed, the use process is simple and convenient, and the medicament system is simple.
Test results show that the method is used for mineral flotation and collection, the recovery rate of fluorite after pure fluorite mineral flotation can reach 92.31%, and the recovery rate of calcite after pure calcite mineral flotation can reach 18.36%; in the manual mixed ore experiment, the recovery rate of fluorite can reach 99.23%, and the grade of fluorite can reach 77.96%. The method has the advantages of high efficiency, high selectivity, simple use process, simple medicament system and good flotation effect.
Detailed Description
The first embodiment is as follows: the embodiment is a method for separating and floating calcite of fluorite and gangue minerals, which is specifically carried out according to the following steps:
mixing a mineral sample with water, and then carrying out primary size mixing to obtain primary size; the granularity of the ore sample is 0.038-0.074 mm; the mass ratio of the ore sample to the water is 1 (15-20); the first size mixing mode is stirring, the stirring time is 1-2 min, and the used equipment is a flotation machine; the ore sample is a fluorite ore sample or a calcite ore sample;
adjusting the pH value of the primary slurry obtained in the step one to be 6-11, and then carrying out secondary size mixing to obtain ore pulp; adjusting the pH value of the primary slurry obtained in the first adjusting step by using an HCl aqueous solution and an NaOH aqueous solution; the second slurry mixing mode is stirring, the stirring time is 2-3 min, and the used equipment is a flotation machine;
thirdly, adding a collecting agent into the ore pulp obtained in the second step, uniformly stirring, and then carrying out mineral flotation and foam scraping, wherein the flotation time is 2-5 min, and the used equipment is a flotation machine, so as to obtain concentrate and tailings; the dosage of the collecting agent relative to the ore pulp is 0.1 multiplied by 10-4mol/L～2×10-4mol/L；
The preparation method of the collecting agent comprises the following steps: dissolving 1, 6-dibromohexane and dodecyl tertiary amine in ethanol, and then carrying out quaternization reaction to obtain a collecting agent;
the molar ratio of the 1, 6-dibromohexane to the dodecyl tertiary amine is 1 (2-2.5); the quaternization reaction is carried out under a protective atmosphere; the quaternization reaction is carried out under the condition of oil bath reflux, the oil bath reflux temperature is 70-100 ℃, and the oil bath reflux time is 24-72 hours.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the stirring speed in the step one is 1702rpm to 1904 rpm. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the flotation machine in the step one is an XFGII-5 type hanging groove flotation machine. The others are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the stirring speed in the second step is 1702-1904 rpm. The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the fourth difference between this embodiment and the specific embodiment is that: and in the third step, adding a collecting agent into the ore pulp obtained in the second step, stirring for 3min, and then performing mineral flotation and foam scraping. The rest is the same as the fourth embodiment.
The invention was verified with the following tests:
test one: the test is a method for separating and floating fluorite, and is specifically carried out according to the following steps:
firstly, mixing 2g of fluorite ore sample and water in a flotation tank, and then carrying out primary size mixing to obtain primary size; the granularity of the ore sample is 0.038-0.074 mm; the mass ratio of the ore sample to the water is 1: 17; the first size mixing mode is stirring, the stirring speed is 1704rpm, the stirring time is 2min, and the used equipment is a flotation machine;
adjusting the pH value of the primary slurry obtained in the step one to be 8, and then carrying out secondary slurry mixing to obtain the ore pulp; adjusting the pH value of the primary slurry obtained in the first adjusting step by using an HCl aqueous solution or an NaOH aqueous solution; the second size mixing mode is stirring, the stirring speed is 1704rpm, the stirring time is 2min, and the used equipment is a flotation machine; the concentration of the HCl aqueous solution is 1mol/L, and the concentration of the NaOH aqueous solution is 1 mol/L;
thirdly, adding a collecting agent into the ore pulp obtained in the second step, stirring for 3min, and then performing mineral flotation and foam scraping, wherein the flotation time is 3min, and the used equipment is a flotation machine, so that concentrate (foam product) and tailings (in-tank product) are obtained; the amount of the collector used relative to the pulp is 10-4mol/L；
The preparation method of the collecting agent comprises the following steps: dissolving 1, 6-dibromohexane and dodecyl tertiary amine in ethanol, and then carrying out quaternization reaction to obtain a collecting agent;
the molar ratio of the 1, 6-dibromohexane to the dodecyl tertiary amine is 1: 2.2; the quaternization reaction is carried out under a protective atmosphere; the quaternization reaction is carried out under the condition of oil bath reflux, the oil bath reflux temperature is 80 ℃, and the oil bath reflux time is 60 hours;
the flotation machine is an XFGII-5 type hanging groove flotation machine.
And respectively putting the concentrate and the tailings into a vacuum drying oven for drying and weighing, and calculating the recovery rate R according to the formula I.
R＝M1/(M1+M2) X 100% of formula I;
in the formula I, R is the recovery rate and the unit is%;
M1is the concentrate mass, with unit g;
M2the mass of the tailings is g.
Calculated fluorite recovery was 92.31%.
And (2) test II: this test differs from the test one in that: in the first step, 2g of calcite sample and water are mixed in a flotation tank and then subjected to first size mixing. The rest is the same as test one.
And respectively putting the concentrate and the tailings into a vacuum drying oven for drying and weighing, and calculating the recovery rate R according to the formula I.
R＝M1/(M1+M2) X 100% of formula I;
in the formula I, R is the recovery rate and the unit is%;
M1is the concentrate mass, with unit g;
M2the mass of the tailings is g.
Calculated calcite recovery was 18.36%.
And (3) test III: this test differs from the test one in that: adjusting the pH value of the primary slurry obtained in the step one to 11 in the step two; the dosage of the collecting agent in the third step is 0.5 multiplied by 10 relative to the ore pulp-4mol/L. The rest is the same as test one.
And respectively putting the concentrate and the tailings into a vacuum drying oven for drying and weighing, and calculating the recovery rate R according to the formula I.
R＝M1/(M1+M2) X 100% of formula I;
in the formula I, R is the recovery rate and the unit is%;
M1is the concentrate mass, with unit g;
M2the mass of the tailings is g.
Calculated fluorite recovery was 94.05%.
And (4) testing: the difference between this test and the second test is that: adjusting the pH value of the primary slurry obtained in the step one to 11 in the step two; the dosage of the collecting agent in the third step is 0.5 multiplied by 10 relative to the ore pulp-4mol/L. The rest was the same as in test two.
And respectively putting the concentrate and the tailings into a vacuum drying oven for drying and weighing, and calculating the recovery rate R according to the formula I.
R＝M1/(M1+M2) X 100% of formula I;
in the formula I, R is the recovery rate and the unit is%;
M1is the concentrate mass, with unit g;
M2the mass of the tailings is g.
Calculated calcite recovery was 39.11%.
And (5) testing: the test is a method for separating and floating fluorite and calcite, and is specifically carried out according to the following steps:
firstly, mixing 1g of fluorite and 1g of calcite sample with water in a flotation tank, and then carrying out primary size mixing to obtain primary size; the granularity of the ore sample is 0.038-0.074 mm; the mass ratio of the ore sample to the water is 1: 17; the first size mixing mode is stirring, the stirring speed is 1704rpm, the stirring time is 2min, and the used equipment is a flotation machine;
adjusting the pH value of the primary slurry obtained in the step one to 7, and then carrying out secondary size mixing to obtain the ore pulp; adjusting the pH value of the primary slurry obtained in the first adjusting step by using an HCl aqueous solution or an NaOH aqueous solution; the second size mixing mode is stirring, the stirring speed is 1704rpm, the stirring time is 2min, and the used equipment is a flotation machine; the concentration of the HCl aqueous solution is 1mol/L, and the concentration of the NaOH aqueous solution is 1 mol/L;
thirdly, adding a collecting agent into the ore pulp obtained in the second step, stirring for 3min, and then performing mineral flotation and foam scraping, wherein the flotation time is 3min, and the used equipment is a flotation machine, so that concentrate (foam product) and tailings (in-tank product) are obtained; the amount of the collector used relative to the pulp is 10-4mol/L；
The preparation method of the trapping agent comprises the following steps: dissolving 1, 6-dibromohexane and dodecyl tertiary amine in ethanol, and performing quaternization reaction to obtain a trapping agent;
the molar ratio of the 1, 6-dibromohexane to the dodecyl tertiary amine is 1: 2.2; the quaternization reaction is carried out under a protective atmosphere; the quaternization reaction is carried out under the condition of oil bath reflux, the oil bath reflux temperature is 80 ℃, and the oil bath reflux time is 60 hours;
the flotation machine is an XFGII-5 type hanging groove flotation machine.
The fluorite grade in the concentrate is 77.96%; the fluorite recovery was 81.21% as calculated according to formula I.
And (6) test six: the difference between this test and test five is: and adjusting the pH value of the primary slurry obtained in the step one to be 11 in the step two. The rest were the same as test five.
The fluorite grade in the concentrate is 76.42 percent; the fluorite recovery was 99.23% as calculated according to formula I.
Test results show that the method is used for mineral flotation and collection, the recovery rate of fluorite after pure fluorite mineral flotation can reach 92.31%, and the recovery rate of calcite after pure calcite mineral flotation can reach 18.36%; in the manual mixed ore experiment, the recovery rate of fluorite can reach 99.23%, and the grade of fluorite can reach 77.96%. The method has the advantages of high efficiency, high selectivity, simple use process, simple medicament system and good flotation effect.

Claims (5)

1. A method for separating and floating calcite which is fluorite and gangue mineral is characterized in that the method for separating and floating the fluorite and the gangue mineral is carried out according to the following steps:
mixing a mineral sample with water, and then carrying out primary size mixing to obtain primary size; the granularity of the ore sample is 0.038-0.074 mm; the mass ratio of the ore sample to the water is 1 (15-20); the first size mixing mode is stirring, the stirring time is 1-2 min, and the used equipment is a flotation machine; the ore sample is a fluorite ore sample or a gangue mineral calcite ore sample;
adjusting the pH value of the primary slurry obtained in the step one to be 6-11, and then carrying out secondary size mixing to obtain ore pulp; adjusting the pH value of the primary slurry obtained in the first adjusting step by using an HCl aqueous solution and an NaOH aqueous solution; the second slurry mixing mode is stirring, the stirring time is 2-3 min, and the used equipment is a flotation machine;
thirdly, adding a collecting agent into the ore pulp obtained in the second step, uniformly stirring, and then carrying out mineral flotation and foam scraping, wherein the flotation time is 2-5 min, and the used equipment is a flotation machine, so as to obtain concentrate and tailings; the dosage of the collecting agent relative to the ore pulp is 0.1 multiplied by 10-4mol/L～2×10-4mol/L；
The preparation method of the collecting agent comprises the following steps: dissolving 1, 6-dibromohexane and dodecyl tertiary amine in ethanol, and then carrying out quaternization reaction to obtain a collecting agent;
the molar ratio of the 1, 6-dibromohexane to the dodecyl tertiary amine is 1 (2-2.5); the quaternization reaction is carried out under a protective atmosphere; the quaternization reaction is carried out under the condition of oil bath reflux, the oil bath reflux temperature is 70-100 ℃, and the oil bath reflux time is 24-72 hours.
2. The process of claim 1, wherein the agitation in step one is at a rate of 1702rpm to 1904 rpm.
3. The process of claim 1, wherein the flotation machine in step one is a hanging trough flotation machine of XFGII-5 type.
4. The process according to claim 1, wherein the agitation in step two is at a rate of 1702rpm to 1904 rpm.
5. The method for separating and floating the calcite which is a fluorite mineral and a gangue mineral according to claim 1, wherein a collecting agent is added into the ore pulp obtained in the second step in the third step, and the ore pulp is stirred for 3min and then subjected to mineral flotation and foam scraping.
CN202110057026.XA 2021-01-15 2021-01-15 Method for separating and floating calcite of fluorite and gangue minerals Pending CN112892877A (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5235102A (en) * 1975-06-06 1977-03-17 American Cyanamid Co Method of selecting ore of nonnsulfide mineral
CN109174465A (en) * 2018-09-14 2019-01-11 武汉工程大学 A kind of quaternary ammonium salt suitable for flotation
CN110773325A (en) * 2019-11-08 2020-02-11 南昌航空大学 Application of amine collecting agent
CN111185307A (en) * 2020-01-13 2020-05-22 南昌航空大学 Application of gemini quaternary ammonium salt collecting agent

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5235102A (en) * 1975-06-06 1977-03-17 American Cyanamid Co Method of selecting ore of nonnsulfide mineral
CN109174465A (en) * 2018-09-14 2019-01-11 武汉工程大学 A kind of quaternary ammonium salt suitable for flotation
CN110773325A (en) * 2019-11-08 2020-02-11 南昌航空大学 Application of amine collecting agent
CN111185307A (en) * 2020-01-13 2020-05-22 南昌航空大学 Application of gemini quaternary ammonium salt collecting agent

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
张泾生等: "《矿用药剂》", vol. 1, 30 November 2008, 冶金工业出版社, pages: 300 - 305 *
杨耀辉等: ""季铵盐类表面活性剂在矿物浮选中应用"", 《矿产保护与利用》, no. 5, 31 December 2011 (2011-12-31), pages 108 - 112 *
钱有军等: ""萤石与方解石、重晶石等盐类矿物浮选分离现状"", 《中国非金属矿工业导刊》, no. 4, 31 August 2014 (2014-08-31), pages 18 - 21 *

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