CN113019708A - Oxidation flotation separation process for copper-molybdenum bulk concentrate - Google Patents

Oxidation flotation separation process for copper-molybdenum bulk concentrate Download PDF

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Publication number
CN113019708A
CN113019708A CN202110420884.6A CN202110420884A CN113019708A CN 113019708 A CN113019708 A CN 113019708A CN 202110420884 A CN202110420884 A CN 202110420884A CN 113019708 A CN113019708 A CN 113019708A
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China
Prior art keywords
copper
oxidation
molybdenum
flotation
bulk concentrate
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Inventor
宋翔宇
张红涛
翟晓辰
张振
许来福
王文
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Henan Zhengda Minerals Processing And Metallurgy Engineering Technology Co ltd
Zhengzhou University
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Henan Zhengda Minerals Processing And Metallurgy Engineering Technology Co ltd
Zhengzhou University
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Priority to CN202110420884.6A priority Critical patent/CN113019708A/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00—Flotation
    • B03D1/001—Flotation agents
    • B03D1/002—Inorganic 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
    • B03D2201/04—Frothers
    • 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

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

Abstract

The invention relates to the technical field of mineral dressing metallurgy, in particular to an oxidation flotation separation process of copper-molybdenum bulk concentrates. The beneficial effects are that: by using "CaO + O3+ H2O "as oxidation system, at certain ore pulp concentration, through regulating CaO and O3The addition amount of the sulfur-containing mineral slurry is regulated and controlled, the pH value and the oxidation potential of the slurry system are regulated and controlled, the surface oxidation of chalcopyrite minerals is promoted, hydrophilic copper hydroxide and hydrophilic iron hydroxide are generated by copper and iron elements, sulfur is converted into sulfate radicals to enter a solution, and the sulfate radicals react with calcium ions to produce calcium sulfate precipitates so as to promote the dissolution of the sulfur; molybdeniteThe ore has stronger oxidation resistance, and the surface hydrophobicity is basically unchanged. The copper and molybdenum are separated by flotation without adding an inhibitor by utilizing the characteristic that the floatability difference of two minerals is increased after the surface hydrophobicity is changed. The purpose of short-flow, green and low-cost copper-molybdenum separation is realized.

Description

Oxidation flotation separation process for copper-molybdenum bulk concentrate
Technical Field
The invention relates to the technical field of mineral processing metallurgy, in particular to an oxidation flotation separation process of copper-molybdenum bulk concentrates.
Background
Molybdenum resources in China are quite rich, and the reserves of the molybdenum resources in China in 2019 are about 830 ten thousand tons, which account for 46.1 percent of the reserves all over the world. Copper sulfide minerals are associated in most molybdenum ore resources, and because copper sulfide ores and molybdenite have good natural floatability, the copper-molybdenum mixed flotation can obtain high recovery rate and high grade, but the subsequent copper-molybdenum separation is difficult. Therefore, how to efficiently and greenly separate copper and molybdenum is a great technical problem in the field of concentration and metallurgy.
At present, the processes for separating copper-molybdenum bulk concentrates at home and abroad mainly comprise two types: the first type is copper-molybdenum flotation, namely copper sulfide mineral flotation; the second type is molybdenum suppression and copper flotation, namely molybdenite suppression and copper sulfide flotation. Both of these broad classes of processes require the use of inhibitors: the molybdenum-inhibiting copper-floating process mainly adopts dextrin as an inhibitor of molybdenum. The copper inhibitor for copper-floating molybdenum-inhibiting process mainly includes sodium sulfide, sodium hydrosulfide, sodium mercaptoacetate, Nox agents of phosphonox and arsenic Nox, cyanide, etc. Regardless of the process, the bulk concentrate needs to be freed of the flotation reagents remaining on the surface before flotation separation.
At present, the copper and molybdenum floating inhibiting process is a copper and molybdenum separation process adopted by most of domestic and overseas mines. The secondary copper minerals are very difficult to inhibit in the flotation process, so the dosage of the common copper inhibitor in production is generally large, taking the most common sodium sulfide or sodium hydrosulfide as an example, the dosage is basically within the range of 10-50 kg/t concentrate, the high consumption of the inhibitor greatly increases the production cost of enterprises, and the problem of environmental pollution is brought. Therefore, the method becomes a technical problem to be solved urgently for copper-molybdenum mines if the high-efficiency, green and low-cost separation of the copper-molybdenum bulk concentrates is realized.
Disclosure of Invention
In order to solve the problems, the embodiment of the invention provides an oxidation flotation separation process of copper-molybdenum bulk concentrates.
The purpose of the invention is realized as follows:
an oxidation flotation separation process for copper-molybdenum bulk concentrate uses molybdenite and chalcopyrite in strong oxidant ozone (O)3) The surface hydrophobicity difference is shown under the action, and the flotation separation is carried out under the condition of no inhibitor.
Preferably, use is made of "CaO + O3+ H2O "as an oxidation system by controlling O3The addition amount of the copper pyrites promotes the surface oxidation of the chalcopyrite minerals by regulating and controlling the oxidation potential of the ore pulp system.
Preferably, the oxidation flotation separation process of the copper-molybdenum bulk concentrate comprises the following steps:
step one, carrying out pesticide removal treatment on mixed copper-molybdenum concentrate produced in flotation operation by an ultrasonic action and activated carbon adsorption method;
step two, respectively adjusting the copper-molybdenum bulk concentrate after reagent removal to proper concentration and alkalinity by using water and CaO;
step three, the pulp after size mixing enters a series of closed high-efficiency stirring tanks, and ozone O is introduced in a countercurrent manner3Carrying out oxidation treatment;
and step four, after the oxidation treatment is finished, performing flotation operation on the ore pulp, wherein the flotation agent is a combined agent formed by a collecting agent and a foaming agent.
Preferably, in the second step, the concentration of the ore pulp is adjusted to 15-40%.
Preferably, in the second step, the alkalinity is adjusted to be 8-10.
Preferably, in the third step, 2-10 closed efficient stirring tanks are used.
Preferably, ozone O is used in step three, or step three3The amount of the catalyst is controlled to be 0.01 to 5 g/L.h, and the time of the oxidation treatment is 10 to 60 min.
Preferably, in the third step, the residual ozone is treated by the ozone destructor and then is discharged harmlessly.
Preferably, in the fourth step, the collector is kerosene, and the foaming agent is terpineol oil.
The embodiment of the invention has the beneficial effects that: the invention adopts CaO + O3+ H2O as an oxidation system, under a certain ore pulp concentration, the pH value and the oxidation potential of the ore pulp system are regulated and controlled by regulating and controlling the adding amount of CaO and O3, so that the surface oxidation of chalcopyrite minerals is promoted, copper and iron elements in the chalcopyrite generate hydrophilic copper hydroxide and iron hydroxide, sulfur is converted into sulfate radicals to enter a solution, and the sulfate radicals react with calcium ions to produce calcium sulfate precipitates, so that the dissolution of the sulfur is promoted; the molybdenite has strong oxidation resistance, and the surface hydrophobicity is basically unchanged. Therefore, when the surface hydrophobicity of the two minerals is changed, the difference of floatability is increased, so that the separation can be carried out by flotation without adding an inhibitor. The whole process realizes the purposes of short flow, green and low cost copper-molybdenum separation.
Drawings
The invention provides a flow chart of an oxidation flotation separation process of copper-molybdenum bulk concentrates.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. Wherein, the related numerical values, fractions or proportions are quality numerical values, quality fractions or quality proportions if the numerical values, fractions or proportions are not marked.
The pre-oxidation and flotation separation processes in industrial production are continuous processes, and the applied equipment comprises a plurality of closed stirring tanks and flotation units which are connected in series. The laboratory test is a discontinuous process, the pre-oxidation is completed in a small closed stirring tank, and the flotation process is completed in a small hanging tank flotation machine through a simulation closed circuit test. The following examples are all laboratory tests
Example 1
S1, the copper-molybdenum bulk concentrate is an artificial bulk concentrate and is prepared by mixing pure minerals of molybdenite and chalcopyrite according to the mass ratio of 1: 1. The fineness of the bulk concentrate is-0.074 mm 74.82%, and the grades of molybdenum and copper in the bulk concentrate are 29.25% and 16.93%, respectively.
And S2, respectively adjusting the copper-molybdenum bulk concentrate prepared in the step S1 to proper concentration and alkalinity by using water and CaO. The concentration of the ore pulp is adjusted to 30 percent, and the alkalinity is adjusted to pH 9.
And S3, transferring all the ore pulp prepared in the step S2 into a stirring tank, wherein the rotating speed of the stirring tank is 1400rpm, the ozone introducing amount is 0.015 g/L.h, and the oxidation treatment is carried out for 30 minutes.
And S4, transferring the copper-molybdenum mixed ore pulp subjected to oxidation treatment in the step S3 into a flotation tank for flotation separation. The flow structure is 'one coarse and three fine scanning'; the coal oil consumption in the molybdenum roughing operation is 100g/t, and the pine alcohol oil consumption is 20 g/t. The dosage of scavenging medicament is 50g/t of kerosene and 10g/t of pine oil. During the selection, no medicament is added, and the selection is carried out after stirring for 3 minutes.
In the embodiment, the grades of molybdenum and copper in the molybdenum concentrate obtained by the closed-loop test are 57.25% and 0.08% respectively, and the molybdenum recovery rate is 99.87%; the copper and molybdenum grades in the copper concentrate are 34.23 percent and 0.08 percent respectively, and the copper recovery rate is 99.04 percent.
Example 2
In a skarn type copper-molybdenum ore, molybdenum-containing minerals in the ore mainly comprise molybdenite, and copper-containing minerals mainly comprise chalcopyrite, a small amount of chalcocite, copper blue and the like; the gangue minerals are mainly quartz, mica, feldspar, chlorite, etc. After copper-molybdenum bulk flotation and concentration, the molybdenum grade in the copper-molybdenum bulk concentrate is 33.25 percent, and the copper grade is 8.58 percent.
S1, adding water into the copper-molybdenum bulk concentrate obtained by the flotation of the raw ore, mixing the mixture to a concentration of 15-20%, then placing the mixture into an ultrasonic stirring tank for drug removal treatment for 10 minutes, and then carrying out solid-liquid separation; the operation of removing the drug is completed after 2 times of repetition.
S2: and respectively regulating the concentration and the alkalinity of the copper-molybdenum bulk concentrate obtained after the reagent removal to proper values by using water and CaO. The concentration of the ore pulp is adjusted to 30 percent, and the alkalinity is adjusted to pH 9.
And S3, transferring all the ore pulp prepared in the step S2 into a stirring tank, wherein the rotating speed of the stirring tank is 1400rpm, the ozone introducing amount is 0.02 g/L.h, and the oxidation treatment is carried out for 20 minutes.
And S4, transferring the copper-molybdenum mixed ore pulp subjected to oxidation treatment in the step S3 into a flotation tank for flotation separation. The flow structure is 'one coarse, four fine and two sweeps'; the coal oil consumption in the molybdenum roughing operation is 120g/t, and the pine alcohol oil consumption is 30 g/t. The dosage of the scavenging agents of the two sections is 60g/t of kerosene, and the dosage of the pine oil is 15 g/t. During the selection, no medicament is added, and the selection is carried out after stirring for 3 minutes.
In the embodiment, the grades of molybdenum and copper in the molybdenum concentrate obtained by the closed-loop test are 53.02% and 0.41% respectively, and the molybdenum recovery rate is 99.64%; the copper and molybdenum grades in the copper concentrate are 22.90% and 0.32% respectively, and the copper recovery rate is 97.11%.
Example 3
In certain porphyry type copper-molybdenum ore, molybdenum-containing minerals in the ore mainly comprise molybdenite, copper-containing minerals mainly comprise chalcopyrite, a small amount of porphyry and the like; the gangue minerals are mainly quartz, mica, feldspar, illite, etc. After copper-molybdenum bulk flotation and concentration, the molybdenum grade in the copper-molybdenum bulk concentrate is 12.32 percent, and the copper grade is 16.69 percent.
S1, adding water into the copper-molybdenum bulk concentrate obtained by the flotation of the raw ore, mixing the mixture to a concentration of 15-20%, then placing the mixture into an ultrasonic stirring tank for drug removal treatment for 10 minutes, and then carrying out solid-liquid separation; the operation of removing the drug is completed after 2 times of repetition.
S2: and respectively regulating the concentration and the alkalinity of the copper-molybdenum bulk concentrate obtained after the reagent removal to proper values by using water and CaO. The concentration of the ore pulp is adjusted to 30 percent, and the alkalinity is adjusted to pH 9.
And S3, transferring all the ore pulp prepared in the step S2 into a stirring tank, wherein the rotating speed of the stirring tank is 1400rpm, the ozone introducing amount is 0.02 g/L.h, and the oxidation treatment is carried out for 30 minutes.
And S4, transferring the copper-molybdenum mixed ore pulp subjected to oxidation treatment in the step S3 into a flotation tank for flotation separation. The flow structure is 'one coarse, four fine and two sweeps'; the coal oil consumption in the molybdenum roughing operation is 100g/t, and the pine alcohol oil consumption is 30 g/t. The dosage of the scavenging agents in the two sections is 50g/t of kerosene, and the dosage of the pine oil is 15 g/t. 1-4, adding 200g/t, 100g/t and 100g/t of water glass as a dispersing agent, stirring for 2 minutes and then concentrating.
In the embodiment, the grades of molybdenum and copper in the molybdenum concentrate obtained by the closed-loop test are 46.12% and 0.64% respectively, and the molybdenum recovery rate is 99.34%; the copper and molybdenum grades in the copper concentrate are 22.49 percent and 0.11 percent respectively, and the copper recovery rate is 98.98 percent.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the invention.

Claims (9)

1. An oxidation flotation separation process of copper-molybdenum bulk concentrate is characterized in that molybdenite and chalcopyrite are used in strong oxidant ozone (O)3) The surface hydrophobicity difference is shown under the action, and the flotation separation is carried out under the condition of no inhibitor.
2. The process for the separation by oxidative flotation of copper molybdenum bulk concentrate according to claim 1, characterized in that "CaO + O3+ H2O" is used as an oxidation system, and O is controlled3The addition amount of the copper pyrites promotes the surface oxidation of the chalcopyrite minerals by regulating and controlling the oxidation potential of the ore pulp system.
3. The process for the oxidative flotation separation of copper molybdenum bulk concentrate according to claim 1 or 2, characterized by comprising the following steps:
step one, carrying out pesticide removal treatment on mixed copper-molybdenum concentrate produced in flotation operation by an ultrasonic action and activated carbon adsorption method;
step two, respectively adjusting the copper-molybdenum bulk concentrate after reagent removal to proper concentration and alkalinity by using water and CaO;
step three, the pulp after size mixing enters a series of closed high-efficiency stirring tanks, and ozone O is introduced in a countercurrent manner3Carrying out oxidation treatment;
and step four, after the oxidation treatment is finished, performing flotation operation on the ore pulp, wherein the flotation agent is a combined agent formed by a collecting agent and a foaming agent.
4. The oxidation flotation separation process of the copper molybdenum bulk concentrate according to claim 3, characterized in that in the second step, the pulp concentration is adjusted to 15-40%.
5. The oxidation flotation separation process of the copper molybdenum bulk concentrate according to claim 3, wherein in the second step, the alkalinity is adjusted to pH 8-10.
6. The oxidation flotation separation process of the copper molybdenum bulk concentrate according to claim 3, characterized in that in the third step, 2-10 closed high-efficiency stirring tanks are provided.
7. The process of claim 3, wherein in step three, ozone O is added to the copper molybdenum bulk concentrate3The amount of the catalyst is controlled to be 0.01 to 5 g/L.h, and the time of the oxidation treatment is 10 to 60 min.
8. The oxidation flotation separation process of copper molybdenum bulk concentrate according to claim 3, characterized in that in step three, residual ozone is treated by an ozone destructor and then discharged harmlessly.
9. The oxidation flotation separation process of the copper molybdenum bulk concentrate according to claim 3, wherein in the fourth step, the collector is kerosene and the foaming agent is pine oil.
CN202110420884.6A 2021-04-19 2021-04-19 Oxidation flotation separation process for copper-molybdenum bulk concentrate Pending CN113019708A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114054216A (en) * 2021-11-13 2022-02-18 内蒙古拜仁矿业有限公司 Method and equipment for improving separation and flotation concentration of bulk concentrate
CN114247569A (en) * 2021-12-10 2022-03-29 郑州大学 Method for flotation separation of talc and copper sulfide
CN115582210A (en) * 2022-10-12 2023-01-10 中南大学 Copper-nickel flotation separation beneficiation process after removal of reagent from copper-nickel bulk concentrate

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CN108043573A (en) * 2017-11-21 2018-05-18 江西铜业股份有限公司 Copper-molybdenum bulk concentrate magnetic separation-ultrasonic wave reagent removal-FLOTATION SEPARATION ore-dressing technique

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114054216A (en) * 2021-11-13 2022-02-18 内蒙古拜仁矿业有限公司 Method and equipment for improving separation and flotation concentration of bulk concentrate
CN114054216B (en) * 2021-11-13 2023-11-28 内蒙古拜仁矿业有限公司 Method and equipment for improving separation flotation concentration of bulk concentrate
CN114247569A (en) * 2021-12-10 2022-03-29 郑州大学 Method for flotation separation of talc and copper sulfide
CN114247569B (en) * 2021-12-10 2023-09-22 郑州大学 Flotation separation method for talcum and copper sulfide
CN115582210A (en) * 2022-10-12 2023-01-10 中南大学 Copper-nickel flotation separation beneficiation process after removal of reagent from copper-nickel bulk concentrate

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