CN107081220B - Method for improving enrichment effect of molybdenum oxide in scheelite flotation concentrate - Google Patents

Method for improving enrichment effect of molybdenum oxide in scheelite flotation concentrate Download PDF

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CN107081220B
CN107081220B CN201710325108.1A CN201710325108A CN107081220B CN 107081220 B CN107081220 B CN 107081220B CN 201710325108 A CN201710325108 A CN 201710325108A CN 107081220 B CN107081220 B CN 107081220B
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molybdenum
collector
molybdenum oxide
scheelite
flotation
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CN107081220A (en
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宛鹤
杨玮
卜显忠
龙涛
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Xian University of Architecture and Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/004Organic compounds
    • B03D1/008Organic compounds containing oxygen
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/002Inorganic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D1/00Flotation
    • B03D1/001Flotation agents
    • B03D1/018Mixtures of inorganic and organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/007Modifying reagents for adjusting pH or conductivity
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/02Collectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/06Depressants
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2203/00Specified materials treated by the flotation agents; specified applications
    • B03D2203/02Ores

Abstract

The invention provides a method for improving the enrichment effect of molybdenum oxide in scheelite flotation concentrate, which takes molybdenum sulfide flotation tailing slurry as a raw material to float scheelite to obtain the scheelite flotation concentrate enriched with molybdenum oxide, and comprises the following steps: step one, adding a molybdenum oxide modifier, a regulator, a selective inhibitor, a collector and a collector powerful agent into molybdenum sulfide flotation tailing pulp in sequence, and carrying out normal-temperature flotation to obtain tungsten-molybdenum mixed rough concentrate pulp; step two, concentrating the product of the step one; adding a pH regulator, a desiccants, a selective inhibitor, a collector and a collector powerful agent into the product obtained in the step two; step four, diluting the product obtained in the step three, and then performing flotation to obtain scheelite flotation concentrate enriched with molybdenum oxide; according to the invention, the molybdenum oxide modifier is added in the tailing slurry in a targeted manner to modify the surface properties of molybdenum oxide, particularly molybdenum dioxide, molybdenum trioxide and calcium molybdate resources, so that the content of molybdenum oxide in the recycled scheelite is greatly increased.

Description

Method for improving enrichment effect of molybdenum oxide in scheelite flotation concentrate
Technical Field
The invention belongs to the technical field of mineral processing, relates to improvement of molybdenum oxide enrichment effect in scheelite flotation concentrate, and particularly relates to a method for improving the recovery rate of molybdenum oxide in scheelite flotation concentrate when scheelite is recovered from molybdenum sulfide flotation tailings.
Background
Molybdenum is an important rare metal and strategic reserve resource, and plays an extremely important role in the whole national economy and human health. With the continuous expansion of molybdenum resource exploitation and utilization scale, the simple and easy-to-select molybdenum ores are increasingly reduced, the selection proportion of poor, fine and high-oxidation-rate molybdenum ores is gradually increased, and for molybdenum ore dressing, a grinding and floating process using hydrocarbon oil (kerosene and diesel oil) as a collecting agent is generally adopted to recover molybdenite in the ores. The hydrocarbon oil collecting agent can only be applied to the surfaces of molybdenite particles with good natural floatability through physical adsorption, so that the floatability of the molybdenite is improved, the efficient recovery of the molybdenite is realized, and molybdenum oxide in the ore has no collecting capacity, so that the molybdenum oxide resource in the ore is lost along with tailing resources.
The recovery of molybdenum oxide belongs to a worldwide problem, the difficult selection reason is mainly that ① molybdenum oxide is subjected to certain damage to mineral lattices in the surface oxidation ore-forming process, the molybdenum oxide is easy to argillization during ore grinding, and the recovery effect is influenced, ② ore is usually associated with oxysalts of various cations with the same name, the floatability of the oxysalts is similar, and the oxysalts are difficult to separate from gangue minerals with the same name in the molybdenum oxide flotation process, so that the molybdenum oxide concentrate product has low grade, for example, the molybdenite is difficult to separate from scheelite, calcite, fluorite, apatite and the like associated in the ore.
For the tungsten-molybdenum deposit, the mineral processing process flow adopts a preferential flotation flow of firstly selecting molybdenite and floating molybdenum tailings and then selecting scheelite: in the flotation process of the scheelite, a fatty acid collecting agent is usually adopted to obtain rough concentrate containing the scheelite and other calcium minerals, and then a Peterov method is adopted to carry out concentration on the rough concentrate to obtain the scheelite concentrate. Because the fatty acid collecting agent belongs to an oxidized ore collecting agent and has a certain collecting capacity on molybdenum oxide, a small amount of molybdenum oxide is contained in the white tungsten concentrate, but because the molybdenum oxide is not recovered in a targeted manner, a large amount of molybdenum oxide resources are not reasonably recycled in tailings, and the loss and waste of the molybdenum resources are caused.
At present, researches on recovery of scheelite resources and molybdenum oxide resources from molybdenite flotation tailings of tungsten-molybdenum ore deposits have been advanced, industrial production of scheelite resources from molybdenite flotation tailings by Henan Luo-Mo group has been realized, and WO in molybdenum flotation tailings3Under the conditions that the grade is 0.07-0.1% and the molybdenum grade is about 0.025%, oleic acid soap is used as a collecting agent, and WO is obtained through one-time rough separation3Heating and concentrating the rough tungsten-molybdenum concentrate with the grade of about 1.6 percent and the molybdenum grade of about 0.16 percent to produce WO3The recovery rate of about 65 percent of tungsten-molybdenum concentrate with 25 to 30 percent of content and about 30 percent of molybdenum content with 2 percent of recovery rate,the process mainly recovers the scheelite resource and the molybdenum oxide resource in the tungsten-molybdenum bulk concentrate, and does not recover in a targeted manner, so that the recovery rate of molybdenum is very low. Zhengzhou mineral comprehensive utilization research institute of Chinese geological academy of sciences and Changsha mining and metallurgy research institute of finite liability company disclose a molybdenum-tungsten oxide ore dressing process (CN101224441) and a dressing method (CN102489407A) for recovering scheelite/molybdenum oxide ore from molybdenum sulfide flotation tailings, respectively, and the same points are that: alkali size mixing, water glass as an inhibitor and fatty acid soap (emulsification or modification) as a collector of scheelite and molybdenum oxide, wherein the difference is in a normal-temperature flotation method adopted by CN102489407A and a heating flotation method adopted by CN 101224441. However, in the two processes, only calcium tungstate ore (i.e. scheelite) and calcium molybdenum (tungsten) ore in molybdenum oxide can be recovered by using fatty acid soap as a collector, the recovery effect on molybdenum bloom and tungsten bloom is very poor, so that the molybdenum oxide and tungsten oxide resources are lost, and meanwhile, WO in tungsten-molybdenum mixed concentrate obtained by the two processes3And the molybdenum content is relatively low, and if the molybdenum is directly treated in the process (APT) for producing ammonium paratungstate from low-grade scheelite middling, the production cost is high, and the molybdenum can be used only by further treatment.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a method for improving the enrichment effect of molybdenum oxide in scheelite flotation concentrate, and solve the technical problems of difficult recovery and serious loss of molybdenum oxide at present.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method for improving the enrichment effect of molybdenum oxide in tungsten flotation concentrate is provided, the method takes molybdenum sulfide flotation tailing slurry as a raw material to float scheelite, and the scheelite is obtained by flotation, thus obtaining the scheelite flotation concentrate enriched with molybdenum oxide;
the method comprises the following steps:
step one, adding a molybdenum oxide modifier, a regulator, a selective inhibitor, a collector and a collector powerful agent into molybdenum sulfide flotation tailing pulp in sequence, and carrying out normal-temperature flotation to obtain tungsten-molybdenum mixed rough concentrate pulp;
step two, concentrating the product of the step one;
adding a pH regulator, a desiccants, a selective inhibitor, an oleic acid soap and a collector powerful agent into the product obtained in the step two;
step four, diluting the product obtained in the step three, and then performing flotation to obtain scheelite flotation concentrate enriched with molybdenum oxide;
the molybdenum oxide modifier comprises Pb2+、Fe3+、Fe2+、Al3+、Ca2+、Mg2+And Ba2+One or more elements of (a);
the selective inhibitor comprises one or more of modified water glass, phosphate, modified starch, dextrin, tannin, cellulose, tartaric acid, citric acid, oxalic acid and aminophosphoric acid.
The molybdenum oxide and the tungsten contained in the raw materials mainly exist in the forms of calcium molybdate, molybdenum dioxide, molybdenum trioxide and calcium tungstate, and the raw materials contain one or more of quartz, calcite, fluorite and barite.
The collector powerful agent comprises one or more of oxidized kerosene, oxidized diesel oil, alkyl sulfate soap and ester thereof, alkyl sulfonic acid soap and ester thereof, hydroximic acid, naphthalene and derivative thereof and alkyl ammonium bromide.
The collector comprises oleic acid and derivatives thereof.
And (4) concentrating the product obtained in the first step to more than 60%.
And in the fourth step, the dilution is below 20 percent.
In the first step, the adding amount of the molybdenum oxide modifier, the regulator, the selective inhibitor, the collector and the collector powerful agent in each ton of molybdenum sulfide flotation tailing pulp is respectively 100 g-1000 g, 500 g-2000 g, 200 g-2000 g, 100 g-500 g and 50 g-300 g.
The adding amounts of the pH regulator, the desiccants, the selective inhibitor, the collector and the collector powerful agent in the third step are respectively 100-500 g/t, 200-800 g/t, 3000-8000 g/t, 0-100 g/t and 0-50 g/t in the ratio of the product in the second step.
Compared with the prior art, the invention has the following technical effects:
(1) the invention adds molybdenum oxide modifier in tailing slurry to modify the surface property of molybdenum oxide, especially the resources of molybdenum dioxide, molybdenum trioxide and calcium molybdate, the collecting agent of the invention adopts the combined action of the collecting agent powerful agent and oleic acid soap to selectively adsorb the surface of the modified molybdenum oxide to strengthen the recovery of molybdenum oxide in the rough separation section, and combines reasonable flotation agent and flotation process, under the premise of not influencing the grade of scheelite concentrate, the total recovery rate of molybdenum can reach more than 75%, the content of molybdenum oxide in the recycled scheelite is greatly improved, and the problems of difficult recovery and serious loss of molybdenum oxide at present are solved.
(2) According to the invention, the selective inhibitor is added to reduce the adverse effect of the calcium-containing gangue minerals with good floatability on the selection, the floatation medicament plays a certain inhibiting role on the gangue minerals such as fluorite, calcite and the like in the heating and drug removal process, and meanwhile, the collecting agent is added to prevent part of scheelite and molybdenum oxide from losing along with tailings due to drug removal in the heating and drug removal process.
The present invention will be explained in further detail with reference to examples.
Detailed Description
The method takes molybdenum sulfide flotation tailing slurry after molybdenum sulfide flotation as a raw material, and performs scheelite flotation to obtain scheelite flotation concentrate enriched with molybdenum oxide. Sequentially adding a molybdenum oxide modifier, a regulator, a selective inhibitor, a collector and a collector powerful agent into molybdenum sulfide flotation tailing pulp, and performing normal-temperature flotation to obtain tungsten-molybdenum mixed rough concentrate pulp; the molybdenum oxide modifier and the molybdenum oxide mineral surface are subjected to chemical reaction to generate substances which are easy to react with the collecting agent. The regulator in the step is selected conventionally, and can refer to the mineral dressing preparation in the field, and the sodium carbonate regulator is selected in the invention. And step two, concentrating the product obtained in the step one to more than 60%, mainly aiming at reducing production energy consumption and saving the dosage of production medicaments. Adding a pH regulator, a desiccants, a selective inhibitor, a collector and a collector powerful agent into the product obtained in the step two; the pH regulator can adjust the optimal action environment of the medicament, is a conventional choice in the field, the sodium hydroxide is selected, the gangue mineral surface collecting agent can be removed by the medicament removing agent, and the calcium and magnesium ions are selected and the selective inhibitor can selectively strengthen the inhibiting effect on the gangue mineral. And step four, diluting the product obtained in the step three, and performing flotation to obtain a scheelite flotation concentrate enriched in molybdenum oxide, wherein the flotation concentration is to separate target minerals and gangue minerals, and the lower the concentration of the ore pulp is, the better the separation effect is.
In the first step of the invention, the adding amounts of the molybdenum oxide modifier, the regulator, the selective inhibitor, the collector and the collector powerful agent in each ton of molybdenum sulfide flotation tailing slurry are respectively 100 g-1000 g, 500 g-2000 g, 200 g-2000 g, 100 g-500 g and 50 g-300 g; in the third step, the addition amounts of the pH adjusting agent, the desoxidant agent, the selective inhibitor, the collector and the collector synergist in the second step are respectively 100 g/t-500 g/t, 200 g/t-800 g/t, 3000 g/t-8000 g/t, 0-100 g/t and 0-50 g/t, and specific examples of the present invention are given below by taking only a certain value in the value range of each raw material as an example.
Example 1:
the embodiment provides a method for improving the enrichment effect of molybdenum oxide in scheelite flotation concentrate, wherein molybdenite flotation tailings of a certain tungsten-molybdenum ore deposit in Henan are selected, the main tungsten minerals in the tailings are scheelite, the molybdenum minerals are mainly molybdenum oxide, the content of tungsten trioxide is 0.1%, the content of molybdenum in the molybdenum oxide is 0.02%, the grinding fineness is-200%, and the content is 65%. The method specifically comprises the following steps:
step one, sequentially adding 200g/t of lead ion molybdenum oxide modifier, 1500g/t of sodium carbonate regulator, 1000g/t of modified water glass, 20g/t of citric acid and 500g/t of modified starch as gangue inhibitor, 300g/t of oleic soap as collector, 150g/t of oxidized kerosene and 100g/t of alkyl sulfate soap as collector powerful agent into 35% molybdenite flotation tailing slurry, and performing primary roughing and three-time rough scavenging to obtain tungsten-molybdenum mixed rough concentrate;
step two, concentrating the product obtained in the step one to 65%;
and step three, heating and removing the chemicals from the product obtained in the step two, respectively adding 400g/t of sodium hydroxide as a pH regulator, 500g/t of calcium and magnesium ions as a removing agent, 5000g/t of modified water glass, 200g/t of citric acid, 1500g/t of modified starch, 20g/t of a small amount of oleic soap and 20g/t of a collecting agent powerful agent, diluting the heat-preservation ore pulp to 18% of concentration, and carrying out concentration for three times to obtain the final tungsten-molybdenum mixed concentrate, wherein the detection result is as follows, wherein the tungsten trioxide content is 30%, the total recovery rate is 81%, the molybdenum content is 5.62%, and the total recovery rate is 75.87%.
Figure BDA0001290919230000071
Comparative example 1:
the comparison example shows a method for floating scheelite by using molybdenum sulfide flotation tailing slurry as a raw material, which is different from the method in example 1, a molybdenum oxide modifier, a selective inhibitor and a collector powerful agent are not added in the step one of the comparison example, and scheelite flotation concentrate is obtained by direct flotation after the step one, and the detection results are as follows, and the results show that the content of tungsten trioxide is 26.67%, the total recovery rate is 67.74%, the content of molybdenum is 2.15% and the total recovery rate is 27.30%.
Figure BDA0001290919230000072

Claims (2)

1. A method for improving the enrichment effect of molybdenum oxide in scheelite flotation concentrate is characterized by comprising the following steps:
step one, adding a molybdenum oxide modifier, a regulator, a selective inhibitor, a collector and a collector powerful agent into molybdenum sulfide flotation tailing pulp in sequence, and carrying out normal-temperature flotation to obtain tungsten-molybdenum mixed rough concentrate pulp;
step two, concentrating the product of the step one;
adding a pH regulator, a desiccants, a selective inhibitor, a collector and a collector powerful agent into the product obtained in the step two;
step four, diluting the product obtained in the step three, and then concentrating to obtain scheelite flotation concentrate enriched with molybdenum oxide;
the molybdenum oxide modifier comprises Pb2+、Fe3+、Fe2+、Al3+、Ca2+、Mg2+And Ba2+One or more elements of (a);
the selective inhibitor comprises one or more of modified water glass, phosphate, modified starch, dextrin, tannin, cellulose, tartaric acid, citric acid, oxalic acid and aminophosphoric acid;
molybdenum oxide and tungsten contained in the molybdenum sulfide flotation tailing slurry mainly exist in the forms of calcium molybdate, molybdenum dioxide, molybdenum trioxide, calcium tungstate and tungsten bloom, and the molybdenum sulfide flotation tailing slurry contains one or more of quartz, calcite, fluorite and barite;
the tungsten mineral in the molybdenum sulfide flotation tailing slurry is scheelite, the molybdenum mineral is mainly molybdenum oxide, the content of tungsten trioxide is 0.1%, the content of molybdenum in the molybdenum oxide is 0.02%, the grinding fineness is-200%, and the content is 65%;
the collector powerful agent comprises one or more of oxidized kerosene, oxidized diesel oil, alkyl sulfate soap and ester thereof, alkyl sulfonic acid soap and ester thereof, hydroximic acid, naphthalene and derivative thereof and alkyl ammonium bromide;
the collector comprises oleic acid and derivatives thereof;
concentrating the product obtained in the first step to more than 60%;
diluting to below 20% in the fourth step;
the adding amount of the molybdenum oxide modifier, the regulator, the selective inhibitor, the collector and the collector powerful agent in each ton of molybdenum sulfide flotation tailing pulp in the step one is respectively 100 g-1000 g, 500 g-2000 g, 200 g-2000 g, 300 g-500 g and 50 g-300 g.
2. The method according to claim 1, wherein the addition amounts of the pH regulator, the desolventizing agent, the selective inhibitor, the collector and the collector synergist in the third step are respectively 100g/t to 500g/t, 200g/t to 800g/t, 3000g/t to 8000g/t, 0g/t to 100g/t and 0g/t to 50g/t in the second step.
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