CN115382660A - Separation method of fluorite-containing lepidolite concentrate - Google Patents

Separation method of fluorite-containing lepidolite concentrate Download PDF

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Publication number
CN115382660A
CN115382660A CN202211054383.1A CN202211054383A CN115382660A CN 115382660 A CN115382660 A CN 115382660A CN 202211054383 A CN202211054383 A CN 202211054383A CN 115382660 A CN115382660 A CN 115382660A
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fluorite
concentrate
lepidolite
concentration
collector
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Inventor
凌石生
尚衍波
朱阳戈
肖巧斌
肖文工
刘书杰
赵晨
贺壮志
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Beikuang Chemical Technology Cangzhou Co ltd
BGRIMM Technology Group Co Ltd
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Beikuang Chemical Technology Cangzhou Co ltd
BGRIMM Technology Group Co Ltd
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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
    • B03B—SEPARATING SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS
    • B03B9/00—General arrangement of separating plant, e.g. flow sheets
    • 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
    • B03D1/012—Organic compounds containing sulfur
    • 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
    • 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
    • B03D2201/00—Specified effects produced by the flotation agents
    • B03D2201/06—Depressants
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Abstract

The invention relates to a separation method of fluorite-containing lepidolite concentrate, which comprises the following steps: adding an inhibitor and a collector A into ore pulp containing fluorite lepidolite concentrate to carry out roughing operation to obtain fluorite rough concentrate and roughed tailings; adding an inhibitor into the fluorite rough concentrate to carry out concentration operation to obtain a fluorite concentrate product; and (3) mixing the rougher tailings, adding a collecting agent B for recleaning to obtain lepidolite rough concentrate and recleaning tailings, and performing blank concentration on the obtained lepidolite rough concentrate to obtain a lepidolite concentrate product. The inhibitor is caustic starch and sodium hydroxide; collecting agent A is sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate; collectors B are dodecylamine and octadecylamine. According to the invention, the fluorite lepidolite is separated by adopting the mixed flotation method, so that the defects of long process flow, multiple types of medicaments, low recovery rate and the like caused by the adoption of the method for inhibiting mica from floating fluorite in the prior art are overcome, and the efficient separation of fluorite lepidolite mixed concentrate resources is realized.

Description

Separation method of fluorite-containing lepidolite concentrate
Technical Field
The invention relates to the field of mineral processing, in particular to a separation method of fluorite-containing lepidolite concentrate.
Background
Fluorite is a national important strategic resource and is a main fluorine raw material. With the gradual depletion of high-grade fluorite ore resources, the use of concomitance (co) type fluorite ore resources brings a schedule, and the flotation process is the most main beneficiation method for fluorite ore.
Lithium is widely applied to the fields of new energy, ceramics, aerospace, medicine, national defense war industry and the like, and lepidolite is one of the most important resources for extracting lithium elements, so that the utilization rate of the lepidolite resources is improved, and the high-quality development of the lithium industry is promoted.
For example, CN104399592a discloses a fluorite flotation process, which comprises the following steps: the method comprises the steps of taking low-grade fluorite ore as a raw material, taking linoleic acid, peanut oil and sodium dodecyl sulfate as collecting agents, sequentially adding sulfuric acid, water glass, hydrofluoric acid and the collecting agents in the selection process, and conducting flotation for three times to obtain flotation fluorite. CN107790290A discloses a beneficiation method for recovering fluorite from scheelite rough concentrate, which comprises the following steps: the method comprises the steps of pre-concentrating the scheelite rough concentrate by using inhibitor water glass, adding collector NAK for rough concentration, and adding inhibitor acidified water glass for ten times of concentration. CN103316773A discloses a fluorite ore flotation method, which comprises the steps of primary roughing, primary scavenging, nine times of fine selection and middling return in sequence; in the flotation process, saponified oleic acid is used as a collecting agent; salinized water glass (15 parts of water glass, 10 parts of sodium hexametaphosphate, 2 parts of tannin extract and 245 parts of water) is used as an inhibitor. CN105289848A discloses a fluorite flotation method, which uses fluorite ore as a raw material, modified oleic acid ionic liquid as a collecting agent, water glass as an inhibitor, sodium carbonate as a pH value regulator and an XFD series flotation machine with the volume of 1.5L for roughing.
The lepidolite is mainly selected by a flotation method, for example, CN111151381A discloses a positive ion temperature sensitive collector for Li with unobvious lepidolite characteristics 2 Flotation of ore with 1.2-1.8% of O content mainly comes from flotation of hole mining lepidolite ore. The temperature-sensitive type collector of the positive ion adopts N-isopropyl acrylamide (NIPAM) and N- [ 3-dimethylamino propyl group]Methacrylamide (DMAPMA) two monomers are copolymerized by a free radical polymerization method, and the molar ratio of the two monomers is 1:5-8:1. The prepared positive ion temperature-sensitive collector has no obvious Li characteristics to lepidolite 2 Flotation of ore with the O content of 1.2-1.8% mainly comes from flotation of hole mining lepidolite ore, and has a good flotation effect.
At present, fluorite and lepidolite are generally recovered respectively in industry, and the method for inhibiting mica by adopting flotation fluorite has the defects of long flow, multiple medicament types and low recovery rate.
Disclosure of Invention
In view of the problems in the prior art, the invention aims to provide a separation method of fluorite-containing lepidolite concentrate, aiming at the mixed concentrate obtained by mixed flotation of fluorite lepidolite, the technical scheme of inhibiting lepidolite by floating fluorite is adopted, so that the efficient separation of fluorite lepidolite mixed concentrate resources is realized, the process is short, the recovery rate is high, and the resource utilization rate of fluorite concentrate and lepidolite concentrate is improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides a separation method of a fluorite-containing lepidolite concentrate, which comprises the following steps:
adding an inhibitor and a collector A into ore pulp containing fluorite lepidolite concentrate to carry out roughing operation to obtain fluorite rough concentrate and roughed tailings;
adding an inhibitor into the fluorite rough concentrate to carry out concentration operation to obtain a fluorite concentrate product;
and (3) mixing the rougher tailings, adding a collecting agent B for recleaning to obtain lepidolite rough concentrate and recleaning tailings, and performing blank concentration on the obtained lepidolite rough concentrate to obtain a lepidolite concentrate product.
The inhibitor consists of caustic starch and sodium hydroxide; the collecting agent A consists of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate; the collector B consists of dodecylamine and octadecylamine.
The invention improves the flotation mode, selects fluorite lepidolite mixed flotation, and separates the obtained bulk concentrate, overcomes the defects of long process flow, multiple medicament types, low recovery rate and the like of fluorite lepidolite mixed concentrate resources caused by respectively recycling fluorite and lepidolite and adopting a method for floating fluorite to inhibit mica in the prior art, and realizes the high-efficiency separation of the fluorite lepidolite mixed concentrate resources.
The invention improves the chemical system of fluorite flotation, and realizes the separation of fluorite concentrate from fluorite lepidolite mixed concentrate by utilizing the combination of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate collector and the combination of inhibitor. The sulfonated oleic acid, the diesel oil and the sodium dodecyl benzene sulfonate are matched, so that the excessive foam can be promoted to be broken to form a secondary enrichment effect, the grade of the rough concentrate is improved, the thickness of a foam layer is adjusted, the foam has a stable state, the stability of flotation operation is facilitated, and the foam can be more stably adsorbed on the surface of fluorite. The combined collecting agent has the characteristics of good selectivity, strong collecting capability, good foam state and the like, and can achieve a good flotation effect by using a small amount in the rough separation process.
The invention is added in the process of fluorite selection operationInhibitor of caustic starch and sodium hydroxide against Al on the surface of lepidolite 3+ And Li + The chemical bonding effect is generated, so that the starch is adsorbed on the surface of the lepidolite, the surface of the mineral is hydrophilized, the inhibiting effect is realized, the flotation separation effect of fluorite, the lepidolite and gangue is improved, and fluorite concentrate with higher grade and recovery rate can be obtained.
According to the invention, the grade of fluorite in the fluorite lepidolite concentrate is obviously higher than that of lepidolite, the grade of fluorite is that the lepidolite grade is more than or equal to 50.
In the invention, the pH value of the ore pulp containing fluorite lepidolite concentrate can be 7-9.
In a preferred embodiment of the present invention, the concentration of the solid phase in the ore slurry containing the fluorite lepidolite concentrate is 20 to 40% by mass, and may be, for example, 20%, 22%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38%, 40%, or the like, but is not limited to the values listed, and other values not listed in the range are also applicable.
In a preferred embodiment of the present invention, the inhibitor may be, for example, 4:1, 4.1.
Preferably, the mass ratio of the sulfonated oleic acid, the diesel oil and the sodium dodecyl benzene sulfonate in the collector a is (4-5): 1:1, which can be, for example, 4.
Preferably, the mass ratio of dodecylamine to octadecylamine in the collector B is (1-1.5): 1, and can be, for example, 1:1, 1.1, 1.2, 1.3.
In a preferred embodiment of the present invention, the amount of the inhibitor added in the roughing step is 10 to 100g/t, and may be, for example, 10g/t, 20g/t, 30g/t, 40g/t, 50g/t, 60g/t, 70g/t, 80g/t, 90g/t or 100g/t, but is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable.
Preferably, the amount of collector a added in the roughing operation is 10 to 50g/t, for example 10g/t, 20g/t, 30g/t, 40g/t or 50g/t, etc., but is not limited to the values listed, and other values not listed in this range are equally applicable.
In a preferred embodiment of the present invention, the roughing operation is performed at least 1 time, for example, 1 time, 2 times, or 3 times, but the roughing operation is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable, and are specifically selected according to actual circumstances.
Preferably, the rougher tailings are subjected to at least 1 scavenging operation, for example, 1 scavenging operation, 2 scavenging operations, or 3 scavenging operations, but the rougher tailings are not limited to the recited values, and other values not recited in the range are also applicable, and are specifically selected according to actual conditions.
Preferably, 5-10g/t of collector a is added to the sweep operation, for example 5g/t, 6g/t, 7g/t, 8g/t, 9g/t or 10g/t etc., but not limited to the values recited, and other values not recited in this range are equally applicable.
Preferably, middlings obtained by the scavenging operation are sequentially returned to the previous operation.
In a preferred embodiment of the present invention, the concentration operation is performed at least 3 times, for example, 3 times, 4 times, or 5 times, but the present invention is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable, and are specifically selected according to actual circumstances.
Preferably, the amount of inhibitor used in the beneficiation process is from 10 to 60g/t, for example, 10g/t, 20g/t, 30g/t, 40g/t, 50g/t, or 60g/t, and the like, but is not limited to the values recited, and other values not recited in this range are equally applicable.
Preferably, the middlings obtained in the concentration operation are sequentially returned to the previous operation.
In a preferred embodiment of the present invention, the pH of the rougher tailings is adjusted to 2 to 5, for example, 2, 2.5, 3, 3.5, 4, 4.5 or 5, but is not limited to the values listed, and other values not listed in this range are also applicable.
Preferably, the amount of collector B added in the reselection is 5-10g/t, such as 5g/t, 6g/t, 7g/t, 8g/t, 9g/t or 10g/t, but not limited to the recited values, and other values not recited in the range are equally applicable.
In the invention, the reselection can be performed for multiple times, such as 1 time, 2 times, 3 times and the like, and the specific selection is performed according to the actual situation.
In a preferred embodiment of the present invention, the recleaning tailings are subjected to at least 1 scavenging, for example, 1 scavenging, 2 scavenging, or 3 scavenging, but the present invention is not limited to the recited values, and other values not recited in the range are also applicable, and are specifically selected according to actual circumstances.
Preferably, 1-5g/t of collector B is added to the sweep, and can be, for example, 1g/t, 2g/t, 3g/t, 4g/t, or 5g/t, and the like, but is not limited to the recited values, and other values not recited within this range are equally applicable.
Preferably, the middlings obtained in the scavenging are sequentially returned to the previous operation.
In a preferred embodiment of the present invention, the blank concentration is performed at least 3 times, for example, 3 times, 4 times, or 5 times, but the blank concentration is not limited to the above-mentioned values, and other values not shown in the above-mentioned range are also applicable, and are specifically selected according to actual circumstances.
Preferably, the middlings obtained by blank concentration are sequentially returned to the previous operation.
As a preferred embodiment of the present invention, the separation method comprises: adding an inhibitor and a collector A into ore pulp containing fluorite lepidolite concentrate to carry out roughing operation to obtain fluorite rough concentrate and roughed tailings; the additive amount of the inhibitor in the roughing operation is 10-100g/t, the additive amount of the collector A in the roughing operation is 10-50g/t, the roughing operation is carried out for at least 1 time, and the roughing tailings are subjected to scavenging operation for at least 1 time; collecting agent A of 5-10g/t is added in the scavenging operation, and middlings obtained in the scavenging operation sequentially return to the previous operation;
adding an inhibitor into the fluorite rough concentrate to carry out concentration operation to obtain a fluorite concentrate product; the concentration operation is carried out for at least 3 times, the addition amount of the inhibitor used in the concentration operation is 10-60g/t, and middlings obtained in the concentration operation sequentially return to the previous operation;
mixing the rougher tailings, adding a collecting agent B for recleaning to obtain lepidolite rough concentrate and recleaning tailings, and carrying out blank concentration on the obtained lepidolite rough concentrate to obtain a lepidolite concentrate product; the size mixing is to adjust the pH value of the roughed tailings to 2-5; the addition amount of the collecting agent B in the re-concentration is 5-10g/t; carrying out scavenging on the recleaning tailings for at least 1 time, adding 1-5g/t of collecting agent B in the scavenging, and returning middlings obtained in the scavenging to the previous operation in sequence; the blank concentration is carried out for at least 3 times, and middlings obtained by the blank concentration are returned to the previous operation in sequence;
the mass concentration of the solid phase in the ore pulp containing the fluorite lepidolite concentrate is 20-40%;
the inhibitor consists of caustic starch and sodium hydroxide, and the weight ratio of the caustic starch to the sodium hydroxide in the inhibitor is (4-5) to 1;
the collector A consists of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate, and the mass ratio of the sulfonated oleic acid to the diesel oil to the sodium dodecyl benzene sulfonate in the collector A is (4-5): 1:1;
the collector B is composed of dodecylamine and octadecylamine, and the mass ratio of the dodecylamine to the octadecylamine in the collector B is (1-1.5): 1.
In the invention, the addition amount g/t of the chemical is that a certain amount of chemical is added for flotation based on the mass t of solids in the fluorite-containing lepidolite concentrate.
Compared with the prior art, the invention has the following beneficial effects:
(1) The method disclosed by the invention is used for separating the mixed concentrate obtained by simultaneously floating and recovering fluorite and lepidolite, has short flow and high recovery rate, overcomes the defects of long flow, multiple types of medicaments, low recovery rate and the like in the process of respectively recovering fluorite and lepidolite in the current industry, and can improve the resource utilization rate of the fluorite lepidolite.
(2) According to the invention, the sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate combined collecting agent are adopted, and the sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate combined collecting agent generate a matching effect, so that the sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate combined collecting agent can be adsorbed on the surface of fluorite more stably. The combined collecting agent has the characteristics of good selectivity, strong collecting capability, good foam state and the like, and can achieve a good flotation effect by using a small amount in the rough separation process.
(3) The inhibitor which is formed by combining caustic starch and sodium hydroxide is added in the fluorite concentration operation process, the inhibitor and the inhibitor are matched, the inhibiting effect on lepidolite and gangue minerals is enhanced, the flotation separation effect of fluorite, lepidolite and gangue is improved, fluorite concentrate with higher grade and recovery rate can be obtained, the grade of the fluorite concentrate is not less than 95.01%, and the recovery rate is not less than 70.09%.
(4) According to the invention, after fluorite flotation, lepidolite is recovered by adopting acid activation and flotation of a combined collecting agent of laurylamine and octadecylamine, so that the lepidolite in fluorite lepidolite mixed concentrate is recovered to the maximum extent, the grade of the lepidolite is not less than 1.33%, and the recovery rate is not less than 50.67%.
Drawings
Figure 1 is a schematic representation of the flotation scheme in example 1 of the present invention.
The present invention is described in further detail below. The following examples are merely illustrative of the present invention and do not represent or limit the scope of the claims, which are defined by the claims.
Detailed Description
To better illustrate the invention and to facilitate the understanding of the technical solutions thereof, typical but non-limiting examples of the invention are as follows:
example 1
CaF-containing mixed concentrate of some fluorite lepidolite 2 95.20％、Li 2 And 1.02 percent of O. The flotation process for fluorite provided by the embodiment adopts a rough scanning and three fine processes, as shown in fig. 1, wherein the first processReturning the middlings subjected to the first secondary concentration and scavenging to rough concentration, and returning the middlings obtained by the second and third secondary concentration to the previous concentration operation in sequence; the lepidolite flotation operation adopts a one-roughing-scavenging-three-fine flow, wherein middlings obtained in the first concentration and scavenging are returned to roughing, and middlings obtained in the second and third concentration are returned to the previous concentration operation in sequence.
Specifically, the flotation is carried out according to the following steps:
(1) Adding water into the fluorite lepidolite mixed concentrate to prepare ore pulp (the pH value is 8) with the mass concentration of 31%, adding an inhibitor into the ore pulp, then adding a collecting agent A to perform primary roughing operation, and obtaining fluorite rough concentrate and roughed tailings after roughing; the inhibitor is a combination of caustic starch and sodium hydroxide, the mass ratio of the caustic starch to the sodium hydroxide is 4:1, and the addition amount of the inhibitor is 80g/t according to the mass of the fluorite lepidolite bulk concentrate; the collecting agent A is a combination of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate, the mass ratio of the sulfonated oleic acid to the diesel oil to the sodium dodecyl benzene sulfonate is 4;
(2) Carrying out primary scavenging operation on the rougher tailings obtained in the step (1); wherein the total adding amount of the collecting agent A in the scavenging process is 7g/t according to the mass of the fluorite lepidolite mixed concentrate, and middlings obtained by scavenging are sequentially returned to the previous operation;
(3) Adding an inhibitor into the fluorite rough concentrate obtained in the step (1) to carry out concentration operation for three times, and obtaining a fluorite concentrate product after the concentration is finished; wherein, the adding amount of the inhibitor is 40g/t, the mass ratio of the caustic starch to the sodium hydroxide is 4:1, and the middlings obtained by concentration are returned to the previous operation in sequence according to the mass of the fluorite lepidolite bulk concentrate.
(4) Adding acid into the scavenged tailings obtained in the step (2) to adjust the pH value of the ore pulp to 4, adding a collecting agent B for recleaning, wherein the collecting agent B is a combination of dodecylamine and octadecylamine, the mass ratio of dodecylamine to octadecylamine is 1:1, and obtaining lepidolite rough concentrate and recleaning tailings after recleaning; according to the mass of the fluorite lepidolite mixed concentrate, the total adding amount of the collecting agent B in the re-concentration process is 10g/t;
(5) And (4) carrying out scavenging operation on the recleaning tailings obtained after the recleaning in the step (4), wherein the total adding amount of the collecting agent B in the scavenging process is 3g/t according to the mass of the fluorite lepidolite mixed concentrate, and returning middlings obtained by scavenging to the previous operation in sequence.
(6) And (5) carrying out three times of blank concentration operation on the lepidolite rough concentrate obtained in the step (4), obtaining a lepidolite concentrate product after the concentration is finished, and returning middlings obtained by the concentration to the previous operation sequentially.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 97.41 percent and the recovery rate is 82.06 percent; lepidolite concentrate containing Li 2 O2.88 percent and recovery rate 50.67 percent.
Example 2
CaF-containing fluorite lepidolite bulk concentrate 2 83.36％、Li 2 0.70 percent of O. The fluorite flotation operation of the flotation process provided by the embodiment adopts a rough sweeping and three-fine flow, wherein middlings obtained in the first concentration and the first sweeping are returned to rough concentration, and middlings obtained in the second and third concentration are returned to the previous concentration operation in sequence; the lepidolite flotation operation adopts a one-roughing one-sweeping three-refining flow, wherein middlings subjected to the first-time concentration and one-sweeping are returned to roughing, and middlings obtained by the second-time concentration and the third-time concentration are returned to the previous concentration operation in sequence.
Specifically, the flotation is carried out according to the following steps:
(1) Adding water into the fluorite lepidolite mixed concentrate to prepare ore pulp (the pH value is 9) with the mass concentration of 28%, adding an inhibitor into the ore pulp, then adding a collecting agent A to perform primary roughing operation, and obtaining fluorite rough concentrate and roughed tailings after roughing; the inhibitor is a combination of caustic starch and sodium hydroxide, the mass ratio of the caustic starch to the sodium hydroxide is 4:1, and the addition amount of the inhibitor is 60g/t according to the mass of the fluorite lepidolite bulk concentrate; the collecting agent A is a combination of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate, the mass ratio of the sulfonated oleic acid to the diesel oil to the sodium dodecyl benzene sulfonate is 4;
(2) Carrying out primary scavenging operation on the rougher tailings obtained in the step (1); wherein the total adding amount of the collecting agent A in the scavenging process is 5g/t according to the mass of the fluorite lepidolite mixed concentrate, and middlings obtained by scavenging are sequentially returned to the previous operation;
(3) Adding an inhibitor into the fluorite rough concentrate obtained in the step (1) to carry out concentration operation for at least three times, and obtaining a fluorite concentrate product after the concentration is finished; wherein, the adding amount of the inhibitor is 35g/t, the mass ratio of the caustic starch to the sodium hydroxide is 4:1, and the middlings obtained by concentration are returned to the previous operation in sequence according to the mass of the fluorite lepidolite bulk concentrate.
(4) Adjusting the pH value of the ore pulp to be 2 by adding acid into the scavenged tailings obtained in the step (2), adding a collecting agent B for recleaning, wherein the collecting agent B is a combination of dodecylamine and octadecylamine, the mass ratio of the dodecylamine to the octadecylamine is 1:1, obtaining lepidolite rough concentrate and recleaning tailings after recleaning is completed, and the total adding amount of the collecting agent B in the recleaning process is 7g/t according to the mass of fluorite lepidolite mixed concentrate;
(5) And (5) carrying out primary scavenging operation on the recleaning tailings obtained after the recleaning in the step (4), wherein the total adding amount of the collecting agent B in the scavenging process is 2g/t according to the mass of the fluorite lepidolite mixed concentrate, and sequentially returning middlings obtained by scavenging to the previous operation.
(6) Carrying out three times of blank concentration operation on the lepidolite rough concentrate obtained in the step (4), and obtaining a lepidolite concentrate product after the concentration is finished; and returning the middlings obtained by concentration to the previous operation in sequence.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 95.01% recovery 70.09%; lepidolite concentrate containing Li 2 O1.33% and recovery 51.19%.
Example 3
CaF-containing fluorite lepidolite bulk concentrate 2 85.80％、Li 2 And 0.74 percent of O. The fluorite flotation operation of the flotation process provided by the embodiment adopts a rough-sweeping-three-fine flow, wherein middlings obtained in the first concentration and sweeping-sweeping are returned to rough concentration, and middlings obtained in the second and third concentration are sequentially returned to the previous concentration operation; the lepidolite flotation operation adopts a rough-sweeping-three-fine flow process, wherein the first concentration and sweepingThe middlings of the first time are returned to rough concentration, and the middlings obtained by the second and third times of concentration are returned to the previous concentration operation in sequence.
Specifically, the flotation is carried out according to the following steps:
(1) Adding water into the fluorite lepidolite mixed concentrate to prepare ore pulp (the pH value is 7) with the mass concentration of 30%, adding an inhibitor into the ore pulp, then adding a collecting agent A to perform primary roughing operation, and obtaining fluorite rough concentrate and roughed tailings after roughing; the inhibitor is a combination of caustic starch and sodium hydroxide, the mass ratio of the caustic starch to the sodium hydroxide is 4:1, and the addition amount of the inhibitor is 50g/t according to the mass of the fluorite lepidolite bulk concentrate; the collecting agent A is a combination of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate, the mass ratio of the sulfonated oleic acid to the diesel oil to the sodium dodecyl benzene sulfonate is 4;
(2) Performing secondary scavenging operation on the rougher tailings obtained in the step (1); wherein the total adding amount of the collecting agent A in the scavenging process is 6g/t according to the mass of the fluorite lepidolite mixed concentrate, and middlings obtained by scavenging are sequentially returned to the previous operation;
(3) Adding an inhibitor into the fluorite rough concentrate obtained in the step (1) to carry out concentration operation for three times, and obtaining a fluorite concentrate product after the concentration is finished; wherein, the adding amount of the inhibitor is 30g/t, the mass ratio of the caustic starch to the sodium hydroxide is 4:1 according to the mass of the fluorite lepidolite mixed concentrate, and the middlings obtained by concentration are returned to the previous operation sequentially.
(4) Adjusting the pH value of the ore pulp to be 5 by adding acid into the scavenged tailings obtained in the step (2), adding a collecting agent B for recleaning, wherein the collecting agent B is a combination of dodecylamine and octadecylamine, the mass ratio of the dodecylamine to the octadecylamine is 1:1, obtaining lepidolite rough concentrate and recleaning tailings after recleaning is completed, and the total adding amount of the collecting agent B in the recleaning process is 8g/t according to the mass of fluorite lepidolite mixed concentrate;
(5) And (5) carrying out primary scavenging operation on the recleaning tailings obtained after the recleaning in the step (4), wherein the total adding amount of the collecting agent B in the scavenging process is 2g/t according to the mass of the fluorite lepidolite mixed concentrate, and sequentially returning middlings obtained by scavenging to the previous operation.
(6) Carrying out three times of blank concentration operation on the lepidolite rough concentrate obtained in the step (4), and obtaining a lepidolite concentrate product after the concentration is finished; and returning the middlings obtained by concentration to the previous operation in sequence.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 95.14 percent, and the recovery rate 72.63 percent; lepidolite concentrate containing Li 2 O1.37% and recovery rate 55.25%.
Comparative example 1
In comparison to example 1, the procedure and conditions were exactly the same as in example 1 except that collector a was replaced with oleic acid. Namely, only oleic acid is used as the collector a, and the total addition amount of the collector a is unchanged.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.01% recovery 82.93%; lepidolite concentrate containing Li 2 O2.58 percent and the recovery rate is 43.11 percent.
Comparative example 2
In comparison to example 1, the procedure and conditions were exactly the same as in example 1 except that collector a was replaced with sulfonated oleic acid. Namely, only sulfonated oleic acid is used as the collector A, and the total addition amount of the collector A is unchanged.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.42 percent and the recovery rate is 82.25 percent; lepidolite concentrate containing Li 2 O2.55 percent and recovery rate 45.61 percent.
Comparative example 3
In comparison to example 1, the procedure and conditions were exactly the same as in example 1 except that collector a was replaced with sodium dodecylbenzenesulfonate. Namely, only sodium dodecyl benzene sulfonate is used as the collector A, and the total addition amount of the collector A is unchanged.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.01% recovery 81.91%; lepidolite concentrate containing Li 2 O2.56% and recovery 44.83%.
Comparative example 4
Compared to example 1, the procedure and conditions were exactly the same as example 1 except that collector a was replaced with sulfonated oleic acid and sodium dodecylbenzenesulfonate (mass ratio of 4:1). Namely, only sulfonated oleic acid and sodium dodecyl benzene sulfonate are selected as the collecting agent A, and the total addition amount of the collecting agent A is unchanged.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.37 percent, and the recovery rate is 82.62 percent; lepidolite concentrate containing Li 2 O2.57% and recovery rate 41.93%.
Comparative example 5
Compared to example 1, the procedure and conditions were exactly the same as example 1 except collector a was replaced with sulfonated oleic acid and diesel oil (mass ratio 4:1). Namely, only sulfonated oleic acid and diesel oil are selected as the collector A, and the total addition amount of the collector A is unchanged.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 97.17% with recovery rate 79.93%; lepidolite concentrate containing Li 2 O2.55% and recovery rate 49.42%.
Comparative example 6
Compared to example 1, the procedure and conditions were exactly the same as example 1 except that collector a was replaced with sodium dodecylbenzenesulfonate and diesel oil (mass ratio 1:1). Namely, only sodium dodecyl sulfate and diesel oil are selected as the collecting agent A, and the total addition amount of the collecting agent A is unchanged.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.85 percent, and the recovery rate 75.85 percent; lepidolite concentrate containing Li 2 O2.15% and recovery 47.54%.
Comparative example 7
Compared with example 1, the procedure and conditions were exactly the same as in example 1 except that the inhibitor was replaced with caustic starch. Namely, only caustic starch is selected as the inhibitor, and the total addition amount of the inhibitor is not changed.
ThroughAnd (3) detecting, wherein the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.92 percent, recovery rate 84.70 percent; lepidolite concentrate containing Li 2 O2.82 percent and recovery rate 41.63 percent.
Comparative example 8
In comparison with example 1, the procedure and conditions were exactly the same as in example 1 except that the inhibitor was replaced with sodium hydroxide. That is, only sodium hydroxide is selected as the inhibitor, and the total addition amount of the inhibitor is not changed.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.06 percent, and the recovery rate is 86.97 percent; lepidolite concentrate containing Li 2 O1.38 percent and recovery rate 16.27 percent.
Comparative example 9
Compared with example 1, the steps and conditions were exactly the same as example 1 except that the inhibitor was replaced with conventional water glass. Namely, only the conventional water glass is selected as the inhibitor, and the total addition amount of the inhibitor is not changed.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.33% with recovery rate 86.16%; lepidolite concentrate containing Li 2 O1.25% and recovery 16.04%.
Comparative example 10
In comparison to example 1, the procedure and conditions were exactly the same as example 1 except that collector B was replaced with octadecylamine. Namely, only octadecylamine is selected as the collector B, and the total addition amount of the collector B in the concentration process is unchanged.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 97.43% with 81.98% recovery; lepidolite concentrate containing Li 2 O2.76 percent and the recovery rate is 48.02 percent.
Comparative example 11
In comparison to example 1, the procedure and conditions were exactly the same as in example 1 except that collector B was replaced with dodecylamine. Namely, the dodecylamine is only selected as the collecting agent B, and the total addition amount of the collecting agent B is not changed in the concentration process.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 97.56% with recovery rate 81.10%; lepidolite concentrate containing Li 2 O2.73% and recovery rate 48.30%.
Comparative example 12
The only comparison with example 1 was that the diesel oil in collector a was replaced by an equal amount of kerosene.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 97.33% with recovery rate 79.81%; lepidolite concentrate containing Li 2 O2.65%, recovery 48.19%.
Comparative example 13
The only comparison with example 1 was to replace the diesel oil in collector a with an equal amount of No. two oil.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.27 percent and the recovery rate is 81.27 percent; lepidolite concentrate containing Li 2 O2.63 percent, and the recovery rate is 45.61 percent.
Comparative example 14
The only comparison with example 1 was to replace the sulfonated oleic acid in collector a with an equivalent amount of oleic acid.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.61 percent, recovery rate 80.35 percent; lepidolite concentrate containing Li 2 O2.61%, recovery 47.93%.
Comparative example 15
The only comparison with example 1 was to replace the sodium dodecylbenzenesulfonate in collector a with an equivalent amount of sodium dodecylsulfate.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.71 percent and the recovery rate is 80.65 percent; lepidolite concentrate containing Li 2 O2.63% and recovery 47.06%.
Comparative example 16
Compared with example 1, the mass ratio of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate in collector a is 2.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 96.14 percent, recovery rate 79.70 percent; lepidolite concentrate containing Li 2 O2.60% and recovery 47.95%.
Comparative example 17
Compared with example 1, the mass ratio of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate in the collector A is 4.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 95.64% with recovery rate 81.65%; lepidolite concentrate containing Li 2 O2.60% and recovery 46.20%.
Comparative example 18
Compared with example 1, the mass ratio of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate in collector a is 4.
Through detection, the finally obtained closed circuit test indexes are as follows: caF-containing fluorite concentrate 2 95.86 percent, and the recovery rate 79.32 percent; lepidolite concentrate containing Li 2 O2.50 percent and recovery rate 48.20 percent.
According to the results of the above examples and comparative examples, the invention improves the flotation mode, selects the technical scheme of fluorite lepidolite mixed flotation and then separates the obtained bulk concentrate, overcomes the defects of long process flow, multiple medicament types, low recovery rate and the like caused by the adoption of the method for inhibiting mica from floating fluorite in the prior art, and realizes efficient separation of fluorite lepidolite bulk concentrate resources.
It is to be noted that the present invention is described by the detailed structural features of the present invention through the above embodiments, but the present invention is not limited to the detailed structural features, that is, it is not meant to imply that the present invention must be implemented by relying on the detailed structural features. It should be understood by those skilled in the art that any modifications of the present invention, equivalent substitutions of selected components of the present invention, additions of auxiliary components, selection of specific modes, etc., are within the scope and disclosure of the present invention.
The preferred embodiments of the present invention have been described in detail, however, the present invention is not limited to the specific details of the above embodiments, and various simple modifications may be made to the technical solution of the present invention within the technical idea of the present invention, and these simple modifications are within the protective scope of the present invention.
It should be noted that the various technical features described in the above embodiments can be combined in any suitable manner without contradiction, and the invention is not described in any way for the possible combinations in order to avoid unnecessary repetition.
In addition, any combination of the various embodiments of the present invention is also possible, and the same should be considered as the disclosure of the present invention as long as it does not depart from the spirit of the present invention.

Claims (10)

1. A separation method of a concentrate containing fluorite lepidolite is characterized by comprising the following steps:
adding an inhibitor and a collector A into ore pulp containing fluorite lepidolite concentrate to carry out roughing operation to obtain fluorite rough concentrate and roughed tailings;
adding an inhibitor into the fluorite rough concentrate to carry out concentration operation to obtain a fluorite concentrate product;
mixing the rougher tailings, adding a collecting agent B for recleaning to obtain lepidolite rough concentrate and recleaning tailings, and performing blank concentration on the obtained lepidolite rough concentrate to obtain a lepidolite concentrate product;
the inhibitor consists of caustic starch and sodium hydroxide; the collecting agent A consists of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate; the collector B consists of dodecylamine and octadecylamine.
2. The separation method according to claim 1, wherein the pulp containing fluorite lepidolite concentrate has a solid phase concentration of 20 to 40% by mass.
3. The separation method of claim 1 or 2, wherein the inhibitor comprises caustic starch and sodium hydroxide in a weight ratio of (4-5): 1;
preferably, the mass ratio of the sulfonated oleic acid to the diesel oil to the sodium dodecyl benzene sulfonate in the collector A is (4-5) 1:1;
preferably, the mass ratio of the dodecylamine to the octadecylamine in the collector B is (1-1.5): 1.
4. The separation method according to any one of claims 1 to 3, wherein the inhibitor is added in the roughing operation in an amount of 10 to 100g/t;
preferably, the addition amount of the collector A in the roughing operation is 10-50g/t.
5. The separation process according to any one of claims 1 to 4, wherein the roughing operation is carried out at least 1 time;
preferably, the rougher tailings are subjected to at least 1 scavenging operation;
preferably, 5-10g/t of collector A is added in the scavenging operation;
preferably, middlings obtained by the scavenging operation are sequentially returned to the previous operation.
6. The separation process according to any one of claims 1 to 5, wherein the concentration operation is carried out at least 3 times;
preferably, the addition amount of the inhibitor used in the concentration operation is 10-60g/t;
preferably, the middlings obtained in the concentration operation are sequentially returned to the previous operation.
7. The separation method of any one of claims 1 to 6, wherein the size mixing is to adjust the pH value of the rougher tailings to 2-5;
preferably, the addition amount of the collector B in the reselection is 5-10g/t.
8. The separation process of any one of claims 1 to 7, wherein the recleaning tailings are subjected to at least 1 sweep;
preferably, 1-5g/t of collector B is added in the sweeping;
preferably, the middlings obtained in the scavenging are sequentially returned to the previous operation.
9. The separation method of any one of claims 1 to 8, wherein the blank concentration is performed at least 3 times;
preferably, the middlings obtained by blank concentration are sequentially returned to the previous operation.
10. The separation method of any one of claims 1 to 9, wherein the separation method comprises:
adding an inhibitor and a collector A into ore pulp containing fluorite lepidolite concentrate to carry out roughing operation to obtain fluorite rough concentrate and roughed tailings; the additive amount of the inhibitor in the roughing operation is 10-100g/t, the additive amount of the collector A in the roughing operation is 10-50g/t, the roughing operation is carried out for at least 1 time, and the roughing tailings are subjected to scavenging operation for at least 1 time; collecting agent A of 5-10g/t is added in the scavenging operation, and middlings obtained in the scavenging operation sequentially return to the previous operation;
adding an inhibitor into the fluorite rough concentrate to carry out concentration operation to obtain a fluorite concentrate product; the concentration operation is carried out for at least 3 times, the addition amount of the inhibitor used in the concentration operation is 10-60g/t, and middlings obtained in the concentration operation are returned to the previous operation in sequence;
mixing the rougher tailings, adding a collecting agent B for recleaning to obtain lepidolite rough concentrate and recleaning tailings, and performing blank concentration on the obtained lepidolite rough concentrate to obtain a lepidolite concentrate product; the size mixing is to adjust the pH value of the roughed tailings to 2-5; the addition amount of the collecting agent B in the re-concentration is 5-10g/t; carrying out scavenging on the recleaning tailings for at least 1 time, adding 1-5g/t of collecting agent B in the scavenging, and returning middlings obtained in the scavenging to the previous operation in sequence; the blank concentration is carried out for at least 3 times, and middlings obtained by the blank concentration are returned to the previous operation in sequence;
the mass concentration of the solid phase in the ore pulp containing the fluorite lepidolite concentrate is 20-40%;
the inhibitor consists of caustic starch and sodium hydroxide, and the weight ratio of the caustic starch to the sodium hydroxide in the inhibitor is (4-5): 1;
the collector A consists of sulfonated oleic acid, diesel oil and sodium dodecyl benzene sulfonate, and the mass ratio of the sulfonated oleic acid to the diesel oil to the sodium dodecyl benzene sulfonate in the collector A is (4-5): 1:1;
the collector B is composed of dodecylamine and octadecylamine, and the mass ratio of the dodecylamine to the octadecylamine in the collector B is (1-1.5): 1.
CN202211054383.1A 2022-08-31 2022-08-31 Separation method of fluorite-containing lepidolite concentrate Pending CN115382660A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116371590A (en) * 2023-06-05 2023-07-04 矿冶科技集团有限公司 Beneficiation method for comprehensively improving indexes of low-grade lepidolite concentrate

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN116371590A (en) * 2023-06-05 2023-07-04 矿冶科技集团有限公司 Beneficiation method for comprehensively improving indexes of low-grade lepidolite concentrate
CN116371590B (en) * 2023-06-05 2023-08-18 矿冶科技集团有限公司 Beneficiation method for comprehensively improving indexes of low-grade lepidolite concentrate

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