CN110876987B - Synchronous enhancer for efficient flotation and separation of refractory zinc oxide ore and preparation and application thereof - Google Patents

Synchronous enhancer for efficient flotation and separation of refractory zinc oxide ore and preparation and application thereof Download PDF

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CN110876987B
CN110876987B CN201911233185.XA CN201911233185A CN110876987B CN 110876987 B CN110876987 B CN 110876987B CN 201911233185 A CN201911233185 A CN 201911233185A CN 110876987 B CN110876987 B CN 110876987B
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enhancer
synchronous
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zinc oxide
preparation
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CN110876987A (en
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王振
徐龙华
肖军辉
王进明
傅开彬
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Xihe Qingyang Mining Co ltd
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Southwest University of Science 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
    • B03D1/018Mixtures of inorganic and organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • B03D2201/00Specified effects produced by the flotation agents
    • B03D2201/02Collectors
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B03SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
    • B03DFLOTATION; DIFFERENTIAL SEDIMENTATION
    • 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
    • B03D2203/04Non-sulfide ores

Abstract

The invention provides a synchronous enhancer for high-efficiency flotation separation of refractory zinc oxide ores, a preparation method and application thereof, belonging to the technical field of flotation separation of non-ferrous metal oxide ores. The synchronous enhancer comprises the following raw materials in parts by weight: 100 parts of 27% v/v ammonia water, 2-14 parts of phytic acid, 5-36 parts of kerosene, 15-53 parts of mercaptan and 24-35 parts of polyoxyethylene sorbitan fatty acid ester. The invention also provides a preparation method and an application method of the synchronous enhancer. The synchronous enhancer is used for flotation separation of conventional reagents of zinc oxide ores, and is combined with a proper flotation process, so that valuable zinc mineral collection and gangue mineral inhibition enhancement in a conventional flotation process can be synchronously realized, and the separation efficiency is improved.

Description

Synchronous enhancer for efficient flotation and separation of refractory zinc oxide ore and preparation and application thereof
Technical Field
The invention belongs to the technical field of flotation separation of non-ferrous metal oxidized ores; in particular to a reinforcing agent for realizing the synchronous enhancement of valuable mineral flotation and collection and gangue mineral inhibition in zinc oxide ores, and a preparation method and application of the synchronous reinforcing agent.
Background
Zinc is the fourth "common" metal, second only to iron, aluminum and copper, appearing silvery white in appearance, and is a fairly important metal in modern industry that is not millable for battery manufacture. Zinc can be alloyed with various nonferrous metals, the most important of which is brass composed of zinc and copper, tin, lead, etc., and can also be die-cast with aluminum, magnesium, copper, etc. Zinc is mainly used in the fields of steel, metallurgy, machinery, electricity, chemical industry, light industry, military, medicine and the like. Zinc mainly comes from zinc sulfide ore, but with continuous exploitation of resources, the demand for developing and utilizing zinc oxide resources is more and more urgent.
At present, the zinc oxide ore is mainly recovered by a sulfide-amine flotation method, but amine is sensitive to slime, mica and the like, particularly, the slime has negative electricity on the surface and can generate electrostatic adsorption with amine ions with positive electricity to consume a large amount of amine, and the property of the ore surface can be changed by the slime adsorbed on the ore surface, so that the selectivity is lost when a collecting agent acts on the ore surface, and the quality of concentrate is seriously influenced. A common solution to this problem is direct leaching or desliming flotation. However, the direct leaching method consumes a large amount of leaching reagents, and increases the production cost; the desliming flotation refers to the continuous adoption of a vulcanization-amine method for flotation after fine mud is removed, and still has the problems of high production cost and incapability of completely removing and recycling the fine mud.
Therefore, it is urgently needed to provide a method for realizing efficient flotation separation of the refractory zinc oxide ores.
Disclosure of Invention
The invention aims to solve the technical problems, and provides a synchronous enhancer for high-efficiency flotation separation of refractory zinc oxide ores, a preparation method and application thereof, so as to solve the problems of the zinc oxide ores in the flotation separation. The flotation separation synchronous enhancer provided by the invention can synchronously realize the enhancement of valuable zinc mineral collection and gangue mineral inhibition in the conventional flotation process of zinc oxide ores, and greatly improves the separation efficiency.
The invention aims to provide a high-efficiency flotation separation synchronous enhancer for refractory zinc oxide ores, which comprises the following raw materials in parts by weight: 90-120 parts of 27% ammonia water (v/v), 2-14 parts of phytic acid, 5-36 parts of kerosene, 15-53 parts of mercaptan and 24-35 parts of polyoxyethylene sorbitan fatty acid ester.
Further, the synchronous enhancer comprises the following raw materials: 100 parts of 27% ammonia water (v/v), 5 parts of phytic acid, 14 parts of kerosene, 35 parts of mercaptan and 32 parts of polyoxyethylene sorbitan fatty acid ester.
The invention also aims to provide a preparation method of the high-efficiency flotation separation synchronous enhancer for the refractory zinc oxide ore, which comprises the following preparation steps:
1) weighing 27% ammonia water and phytic acid according to corresponding mass ratio, and mixing to obtain base liquid of the synchronous enhancer;
2) fully mixing kerosene and mercaptan according to a mass ratio, and slowly adding the mixture into the base liquid of the synchronous enhancer obtained in the step 1) to obtain a mother liquid of the synchronous enhancer;
3) weighing corresponding parts by weight of polyoxyethylene sorbitan fatty acid ester, quickly adding the polyoxyethylene sorbitan fatty acid ester into the synchronous enhancer mother liquor obtained in the step 2), and intensively stirring to obtain a synchronous enhancer concentrated phase;
4) mixing the concentrated synchronous enhancer obtained in the step 3) with a proper amount of water to obtain the high-efficiency flotation separation synchronous enhancer for the difficult-to-separate zinc oxide ore.
Further, the mass ratio of the synchronous enhancer concentrated phase to the water in the step 4) is 1: 7-15.
Further, the pH of the base solution of the enhancer for synchronization obtained in step 1) is 7 ± 0.5.
Further, the kerosene and the mercaptan are stirred and mixed at 1500-2800 r/min in the step 2), and the fully mixed kerosene/mercaptan mixture is added into the base liquid of the synchronous enhancer at the flow rate of 250-880 mL/h.
Further, the adding speed of the oxyethylene sorbitan fatty acid ester in the step 3) is 2.5-8.8L/h, and the strong stirring speed is 4000-6000 r/min.
Further, mixing the synchronous enhancer concentrated phase in the step 4) with water, adding the synchronous enhancer concentrated phase into the water at a flow rate of 130-240 mL/h, and assisting with water bath at 40-65 ℃ and ultrasonic oscillation at 65-110W for 15-45 min.
The invention also aims to provide an application of the synchronous enhancer for the high-efficiency flotation separation of the difficult-to-separate zinc oxide ore, wherein the synchronous enhancer is applied to the conventional reagent flotation separation of the zinc oxide ore and is combined with a proper flotation process.
According to the application, the use temperature of the synchronous enhancer is-10-50 ℃ and the dosage of the enhancer is 50-80 g/t.
Compared with the prior art, the invention has the following beneficial effects:
(1) the raw materials adopted by the synchronous enhancer provided by the invention are common substances, and the synchronous enhancer is low in cost and easy to obtain;
(2) the synchronous enhancer provided by the invention has the characteristics of good pulp adaptability, stable property, low consumption, wide applicable pH range and the like;
(3) the synchronous enhancer provided by the invention is used for floating the zinc oxide ore, can synchronously realize the enhancement of valuable zinc mineral collection and gangue mineral inhibition in the conventional flotation process, and improves the separation efficiency.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is described in detail below with reference to the following embodiments, and it should be noted that the following embodiments are only for explaining and illustrating the present invention and are not intended to limit the present invention. The invention is not limited to the embodiments described above, but rather, may be modified within the scope of the invention.
Example 1
The synchronous enhancer of the invention is prepared according to the following method:
(1) mixing 100 parts of 27% (v/v) ammonia water and 5 parts of phytic acid to obtain a base liquid of the synchronous enhancer;
(2) fully mixing 14 parts of kerosene and 35 parts of mercaptan at a stirring speed of 1700r/min, and adding the fully mixed kerosene/mercaptan mixture into base liquid of the synchronous enhancer at a flow rate of 570mL/h to obtain mother liquid of the synchronous enhancer;
(3) taking 32 parts of polyoxyethylene sorbitan fatty acid ester, quickly adding the polyoxyethylene sorbitan fatty acid ester into the synchronous enhancer mother liquor at the adding speed of 8.8L/h, and strongly stirring the polyoxyethylene sorbitan fatty acid ester and the synchronous enhancer mother liquor at the speed of 5500r/min while adding to obtain a synchronous enhancer concentrated phase;
(4) the obtained concentrated phase of the synchronous enhancer is added into 10 times (by mass) of water at the flow rate of 175mL/h, and is assisted with a water bath at 45 ℃ and ultrasonic oscillation at 80W for 25min to obtain the synchronous enhancer used in the embodiment.
The synchronous enhancer is used for carrying out direct flotation test on certain zinc oxide ore in Sichuan Ganluo area. The raw ore contains 9.76% of zinc, a closed flotation test of 'first coarse, second scavenging, second refining and sequential return of middlings' is adopted, sodium sulfide is used as a vulcanizing agent, CMC and water glass are used as inhibitors, dodecylamine is used as a collecting agent, and 2#Oil is a foaming agent; after the collector was added, 55g/t of the same collector of the present invention was addedStep enhancer, used in pulp at pH 9 and temperature 25 ℃, flotation test results are shown in table 1, where the yield and recovery calculations are according to conventional methods in the art.
TABLE 1
Figure BDA0002304134450000051
Comparative example 1
The flotation test of zinc oxide ores was carried out without adding the reinforcing agent of the present invention under the same conditions as in example 1, and the results are shown in Table 2.
TABLE 2
Figure BDA0002304134450000052
As can be seen from tables 2 and 2, the enhancer of the present invention provides excellent flotation separation.
Example 2
The synchronous enhancer of the invention is prepared according to the following method:
(1) mixing 90 parts of 27% (v/v) ammonia water and 2 parts of phytic acid to obtain a base liquid of the synchronous enhancer;
(2) fully mixing 5 parts of kerosene and 15 parts of mercaptan at a stirring speed of 1500r/min, and adding the fully mixed kerosene/mercaptan mixture into base liquid of the synchronous enhancer at a flow rate of 250mL/h to obtain mother liquid of the synchronous enhancer;
(3) taking 24 parts of polyoxyethylene sorbitan fatty acid ester, quickly adding the polyoxyethylene sorbitan fatty acid ester into the synchronous enhancer mother liquor at the adding speed of 5.5L/h, and strongly stirring at the speed of 4000r/min while adding to obtain a synchronous enhancer concentrated phase;
(4) the obtained concentrated phase of the synchronous enhancer is added into water in an amount which is 7 times (by mass) the amount of the concentrated phase at the flow rate of 130mL/h, and water bath at 40 ℃ and ultrasonic oscillation at 65W are assisted for 15min, so that the synchronous enhancer used in the embodiment is obtained.
The synchronous enhancer is used for carrying out direct flotation test on certain zinc oxide ore in the Alba Sichuan area. The zinc content of the raw ore is 10.51 percent,adopts a closed flotation test of 'first rough, second sweep, second fine and returning middlings in sequence', sodium sulfide is used as a vulcanizing agent, CMC and water glass are used as inhibitors, dodecylamine is used as a collecting agent, 2#Oil is a foaming agent; after the collector was added, 50g/t of the above-mentioned simultaneous enhancer was added and used in a slurry at pH 9 and a temperature of 0 ℃, and the results of the flotation test are shown in table 3.
TABLE 3
Figure BDA0002304134450000061
Comparative example 2
The enhancer was prepared in the same manner as in example 2 except that 2 parts of phytic acid was omitted from the formulation, and the obtained enhancer was used in the flotation test of the above zinc oxide ore under the same conditions as in example 2, and the results are shown in Table 4.
TABLE 4
Figure BDA0002304134450000071
As can be seen from tables 3 and 4, when 2 parts of phytic acid was contained in the enhancer formulation of the present invention, a better flotation separation effect was obtained.
Example 3
The synchronous enhancer of the invention is prepared according to the following method:
(1) mixing 120 parts of 27% (v/v) ammonia water and 14 parts of phytic acid to obtain a base liquid of the synchronous enhancer;
(2) fully mixing 36 parts of kerosene and 53 parts of mercaptan at a stirring speed of 2800r/min, and adding the fully mixed kerosene/mercaptan mixture into base liquid of the synchronous enhancer at a flow rate of 880mL/h to obtain mother liquid of the synchronous enhancer;
(3) taking 15 parts of polyoxyethylene sorbitan fatty acid ester, quickly adding the polyoxyethylene sorbitan fatty acid ester into the synchronous enhancer mother liquor at the adding speed of 2.5L/h, and intensively stirring at the speed of 6000r/min while adding to obtain a synchronous enhancer concentrated phase;
(4) the obtained concentrated phase of the synchronous enhancer is added into 15 times (by mass) of water at the flow rate of 240mL/h, and water bath at 65 ℃ and ultrasonic oscillation at 110W are assisted for 45min to obtain the synchronous enhancer used in the embodiment.
The synchronous enhancer is used for carrying out direct flotation test on certain zinc oxide ore in Liangshan, Sichuan. The raw ore contains 8.69% of zinc, and adopts a closed flotation test of 'first coarse, second scavenging, second fine and returning middlings in sequence', sodium sulfide is used as a vulcanizing agent, CMC and water glass are used as inhibitors, dodecylamine is used as a collecting agent, and 2#Oil is a foaming agent; after the collector was added, 80g/t of the fortifier obtained in example 3 of the present invention was added and used in a slurry at a pH of 9 and a temperature of 50 ℃, and the results of the flotation test are shown in table 5.
TABLE 5
Figure BDA0002304134450000081
Comparative example 3
The reinforcing agent was prepared by the method of example 3, but 15 parts of polyoxyethylene sorbitan fatty acid ester was omitted from the formulation, and the reinforcing agent was obtained by directly mixing the mother liquor with water, and the obtained reinforcing agent was used in the above-mentioned flotation test of zinc oxide ore under the same conditions as in example 3, and the results obtained are shown in table 6.
TABLE 6
Figure BDA0002304134450000082
As can be seen from tables 5 and 6, the synchronous fortifier prepared by the method of the invention has better flotation separation effect.

Claims (10)

1. The high-efficiency flotation separation synchronous enhancer for the refractory zinc oxide ore is characterized by comprising the following raw materials in parts by weight: 90-120 parts of 27% v/v ammonia water, 2-14 parts of phytic acid, 5-36 parts of kerosene, 15-53 parts of mercaptan and 24-35 parts of polyoxyethylene sorbitan fatty acid ester.
2. The synchronous enhancer for high-efficiency flotation separation of the refractory zinc oxide ores according to claim 1, which comprises the following raw materials: 100 parts of 27% v/v ammonia water, 5 parts of phytic acid, 14 parts of kerosene, 35 parts of mercaptan and 32 parts of polyoxyethylene sorbitan fatty acid ester.
3. The preparation method of the high-efficiency flotation separation synchronous enhancer for the refractory zinc oxide ores according to claim 1 or 2, which is characterized by comprising the following preparation steps: 1) Weighing 27% v/v ammonia water and phytic acid according to corresponding mass ratio, and mixing the ammonia water and the phytic acid to obtain base liquid of the synchronous enhancer; 2) Fully mixing kerosene and mercaptan in parts by weight, and slowly adding the mixture into the base liquid of the synchronous enhancer obtained in the step 1) to obtain a mother liquid of the synchronous enhancer; 3) Weighing corresponding parts by weight of polyoxyethylene sorbitan fatty acid ester, quickly adding the polyoxyethylene sorbitan fatty acid ester into the synchronous enhancer mother liquor obtained in the step 2), and intensively stirring to obtain a synchronous enhancer concentrated phase; 4) Mixing the concentrated synchronous enhancer obtained in the step 3) with a proper amount of water to obtain the high-efficiency flotation separation synchronous enhancer for the difficult-to-separate zinc oxide ore.
4. The preparation method according to claim 3, wherein the mass ratio of the enhancer-synchronized concentrated phase to water in step 4) is 1: 7-15.
5. The method according to claim 3, wherein the pH of the fortifier base fluid obtained in step 1) is 7 ± 0.5.
6. The preparation method according to claim 3, wherein the kerosene and the mercaptan in the step 2) are stirred and mixed at 1500-2800 r/min, and the fully mixed kerosene/mercaptan mixture is added into the synchronous enhancer base fluid at a flow rate of 250-880 mL/h.
7. The preparation method according to claim 3, wherein the polyoxyethylene sorbitan fatty acid ester in the step 3) is added at a rate of 2.5 to 8.8L/h and the intensive stirring is carried out at a rate of 4000 to 6000 r/min.
8. The preparation method according to claim 3, wherein the step 4) of mixing the concentrated synchronous enhancer phase with water comprises adding the concentrated synchronous enhancer phase into water at a flow rate of 130-240 mL/h, and adding water bath at 40-65 ℃ and ultrasonic oscillation at 65-110W for 15-45 min.
9. The application of the synchronous enhancer for the high-efficiency flotation separation of the refractory zinc oxide ores according to claim 1 or 2 is characterized in that the synchronous enhancer is applied to the conventional chemical flotation separation of the zinc oxide ores and is carried out in combination with a flotation process.
10. The use according to claim 9, wherein the application temperature of the synchronous fortifier is-10 ℃ to 50 ℃, and the dosage of the fortifier is 50g/t to 80g/t based on the weight of ore pulp.
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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5560018A (en) * 1978-10-27 1980-05-06 Mitsui Mining & Smelting Co Ltd Zinc silicate mineral recovering method
CN1820853A (en) * 2006-02-09 2006-08-23 陈铁 Beneficiation method for zinc oxide mine
CN102964504A (en) * 2012-11-26 2013-03-13 张家港顺昌化工有限公司 Thickening agent and preparation method thereof
CN105642447A (en) * 2016-02-15 2016-06-08 深圳市瑞世兴科技有限公司 Zinc oxide ore floatation agent and preparation method thereof
CN106423581A (en) * 2016-11-15 2017-02-22 中南大学 Lead-antimony-zinc sulfide ore bulk flotation collecting agent and preparation and application thereof
CN106540815A (en) * 2016-11-09 2017-03-29 长春黄金研究院 A kind of microfine zinc oxide ore beneficiation method

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS5560018A (en) * 1978-10-27 1980-05-06 Mitsui Mining & Smelting Co Ltd Zinc silicate mineral recovering method
CN1820853A (en) * 2006-02-09 2006-08-23 陈铁 Beneficiation method for zinc oxide mine
CN102964504A (en) * 2012-11-26 2013-03-13 张家港顺昌化工有限公司 Thickening agent and preparation method thereof
CN105642447A (en) * 2016-02-15 2016-06-08 深圳市瑞世兴科技有限公司 Zinc oxide ore floatation agent and preparation method thereof
CN106540815A (en) * 2016-11-09 2017-03-29 长春黄金研究院 A kind of microfine zinc oxide ore beneficiation method
CN106423581A (en) * 2016-11-15 2017-02-22 中南大学 Lead-antimony-zinc sulfide ore bulk flotation collecting agent and preparation and application thereof

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