CN115722347B - Method for separating lead and antimony from paragenetic ore - Google Patents
Method for separating lead and antimony from paragenetic ore Download PDFInfo
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- CN115722347B CN115722347B CN202211306696.1A CN202211306696A CN115722347B CN 115722347 B CN115722347 B CN 115722347B CN 202211306696 A CN202211306696 A CN 202211306696A CN 115722347 B CN115722347 B CN 115722347B
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- antimony
- ore
- lead
- sulfide
- flotation
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- 229910052787 antimony Inorganic materials 0.000 title claims abstract description 30
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 27
- 238000005188 flotation Methods 0.000 claims abstract description 42
- 238000007158 vacuum pyrolysis Methods 0.000 claims abstract description 32
- 229910052981 lead sulfide Inorganic materials 0.000 claims abstract description 30
- 229940056932 lead sulfide Drugs 0.000 claims abstract description 30
- 239000012141 concentrate Substances 0.000 claims abstract description 24
- YPMOSINXXHVZIL-UHFFFAOYSA-N sulfanylideneantimony Chemical compound [Sb]=S YPMOSINXXHVZIL-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000005215 recombination Methods 0.000 claims abstract description 13
- 230000006798 recombination Effects 0.000 claims abstract description 13
- 229910052500 inorganic mineral Inorganic materials 0.000 claims abstract description 6
- 239000011707 mineral Substances 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- RLJMLMKIBZAXJO-UHFFFAOYSA-N lead nitrate Chemical compound [O-][N+](=O)O[Pb]O[N+]([O-])=O RLJMLMKIBZAXJO-UHFFFAOYSA-N 0.000 claims description 10
- 239000004571 lime Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 9
- 239000004088 foaming agent Substances 0.000 claims description 7
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- AEOCXXJPGCBFJA-UHFFFAOYSA-N ethionamide Chemical compound CCC1=CC(C(N)=S)=CC=N1 AEOCXXJPGCBFJA-UHFFFAOYSA-N 0.000 claims description 4
- 229960002001 ethionamide Drugs 0.000 claims description 4
- TUZCOAQWCRRVIP-UHFFFAOYSA-N butoxymethanedithioic acid Chemical compound CCCCOC(S)=S TUZCOAQWCRRVIP-UHFFFAOYSA-N 0.000 claims description 3
- 235000012204 lemonade/lime carbonate Nutrition 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000003795 chemical substances by application Substances 0.000 claims 4
- 230000003213 activating effect Effects 0.000 claims 2
- 239000012190 activator Substances 0.000 claims 1
- 238000002360 preparation method Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 10
- 239000000203 mixture Substances 0.000 abstract description 5
- 238000004321 preservation Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 10
- 238000003756 stirring Methods 0.000 description 8
- 235000008733 Citrus aurantifolia Nutrition 0.000 description 7
- 235000011941 Tilia x europaea Nutrition 0.000 description 7
- 238000005979 thermal decomposition reaction Methods 0.000 description 7
- GGLZPLKKBSSKCX-YFKPBYRVSA-N L-ethionine Chemical compound CCSCC[C@H](N)C(O)=O GGLZPLKKBSSKCX-YFKPBYRVSA-N 0.000 description 6
- 238000003723 Smelting Methods 0.000 description 6
- 238000001816 cooling Methods 0.000 description 6
- 239000008396 flotation agent Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 238000000197 pyrolysis Methods 0.000 description 4
- 238000005273 aeration Methods 0.000 description 3
- 238000000354 decomposition reaction Methods 0.000 description 3
- 239000003002 pH adjusting agent Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 229910052717 sulfur Inorganic materials 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- DSCFFEYYQKSRSV-UHFFFAOYSA-N 1L-O1-methyl-muco-inositol Natural products COC1C(O)C(O)C(O)C(O)C1O DSCFFEYYQKSRSV-UHFFFAOYSA-N 0.000 description 2
- VJXUJFAZXQOXMJ-UHFFFAOYSA-N D-1-O-Methyl-muco-inositol Natural products CC12C(OC)(C)OC(C)(C)C2CC(=O)C(C23OC2C(=O)O2)(C)C1CCC3(C)C2C=1C=COC=1 VJXUJFAZXQOXMJ-UHFFFAOYSA-N 0.000 description 2
- DSCFFEYYQKSRSV-KLJZZCKASA-N D-pinitol Chemical compound CO[C@@H]1[C@@H](O)[C@@H](O)[C@H](O)[C@H](O)[C@H]1O DSCFFEYYQKSRSV-KLJZZCKASA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 229910001245 Sb alloy Inorganic materials 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- 239000000956 alloy Substances 0.000 description 2
- 229910045601 alloy Inorganic materials 0.000 description 2
- 239000002140 antimony alloy Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000004484 Briquette Substances 0.000 description 1
- MBMLMWLHJBBADN-UHFFFAOYSA-N Ferrous sulfide Chemical compound [Fe]=S MBMLMWLHJBBADN-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000008395 clarifying agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002189 fluorescence spectrum Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- KAEAMHPPLLJBKF-UHFFFAOYSA-N iron(3+) sulfide Chemical compound [S-2].[S-2].[S-2].[Fe+3].[Fe+3] KAEAMHPPLLJBKF-UHFFFAOYSA-N 0.000 description 1
- 229910052973 jamesonite Inorganic materials 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 polyethylene terephthalate Polymers 0.000 description 1
- 229920000139 polyethylene terephthalate Polymers 0.000 description 1
- 239000005020 polyethylene terephthalate Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 229910052683 pyrite Inorganic materials 0.000 description 1
- NIFIFKQPDTWWGU-UHFFFAOYSA-N pyrite Chemical compound [Fe+2].[S-][S-] NIFIFKQPDTWWGU-UHFFFAOYSA-N 0.000 description 1
- 239000011028 pyrite Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
Classifications
-
- 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
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- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention belongs to the technical field of mineral separation, and particularly relates to a method for separating lead and antimony from symbiotic ores. The invention provides a method for separating lead and antimony from paragenetic ore, which comprises the following steps: carrying out vacuum pyrolysis on the symbiotic ore to realize ore phase recombination and obtain a recombined product; the temperature of the vacuum pyrolysis is 500-600 ℃, and the heat preservation time of the vacuum pyrolysis is 20-50 min; and (3) carrying out flotation on the recombined product to obtain lead sulfide concentrate and antimony sulfide tailings. The invention carries out vacuum pyrolysis on the symbiotic ore at a specific temperature to break up the original molecular composition of the symbiotic ore, and carries out recombination on the ore phase of the symbiotic ore to obtain lead sulfide and antimony sulfide; lead sulfide is separated by floatation, so that enrichment of lead sulfide and antimony sulfide is realized. The separation method provided by the invention is simple and easy to operate, and the treatment efficiency of the paragenetic ore is greatly improved.
Description
Technical Field
The invention belongs to the technical field of mineral separation, and particularly relates to a method for separating lead and antimony from symbiotic ores.
Background
Antimony is a gray metal with silver luster, and can form an alloy with wide application range with lead, and the hardness of the alloy is improved compared with mechanical strength. Antimony is a stabilizer and catalyst for the production of polyethylene terephthalate. Is also a clarifying agent for removing bubbles visible under a microscope in glass, and is mainly used for manufacturing television screens.
With the rapid consumption of antimony resources, the production raw materials of antimony are gradually changed from single sulphide ore (stibium ore) to antimonous polymetallic symbiotic ores such as jamesonite, antimonite and the like. However, the structure composition of the multi-metal paragenetic ore containing antimony is complex, and most of lead, antimony and iron in the paragenetic ore exist in the same ore phase, so that the lead and the antimony are difficult to be separated efficiently in a mineral separation mode. At present, the symbiotic ore is mainly treated in a pyrometallurgical mode, and the existing method for treating the symbiotic ore is complex and takes longer time, so that the large-scale treatment and comprehensive utilization of the antimonial polymetallic symbiotic ore are seriously restricted.
Disclosure of Invention
In view of the above, the invention provides a method for separating lead and antimony from the paragenetic ore, and the separation method provided by the invention can reconstruct ore phases in the paragenetic ore, and can separate lead sulfide and antimony sulfide through flotation, thereby greatly improving the beneficiation efficiency of the paragenetic ore.
In order to solve the technical problems, the invention provides a method for separating lead and antimony from paragenetic ore, which comprises the following steps:
Carrying out vacuum pyrolysis on the symbiotic ore to realize ore phase recombination and obtaining a recombination product, wherein the recombination product comprises lead sulfide and antimony sulfide; the temperature of the vacuum pyrolysis is 500-600 ℃;
and (3) carrying out flotation on the recombined product to obtain lead sulfide concentrate and antimony sulfide tailings.
Preferably, the vacuum degree of the vacuum pyrolysis is 1-10 Pa.
Preferably, the heating rate for heating to the vacuum pyrolysis temperature is 8-12K/min.
Preferably, the intergrowth ore medium phase comprises FeSb 4Pb6S14.
Preferably, the vacuum pyrolysis further comprises: grinding the paragenetic ore and briquetting.
Preferably, the vacuum pyrolysis has a heat preservation time of 20-50 min.
Preferably, the pre-flotation further comprises mixing the recombined product with a flotation solution comprising a flotation agent, a collector, a frother and an alkaline pH adjuster.
Preferably, the flotation agent comprises lead nitrate or pinitol oil; the collector comprises ethionamide or butyl xanthate; the foaming agent comprises No. two oil; the alkaline pH regulator comprises lime or sodium carbonate.
Preferably, the pH value of the flotation solution is 7-10.
Preferably, the grade of the lead sulfide concentrate is 57-66%; the grade of the antimony sulfide tailings is 36-44%.
The invention provides a method for separating lead and antimony from paragenetic ore, which comprises the following steps: carrying out vacuum pyrolysis on the symbiotic ore to realize ore phase recombination and obtain a recombined product, wherein the ore phase in the recombined product comprises PbS and Sb 2S3; the temperature of the vacuum pyrolysis is 500-600 ℃; and (3) carrying out flotation on the recombined product to obtain lead sulfide concentrate and antimony sulfide tailings. The invention carries out vacuum pyrolysis on the symbiotic ore at a specific temperature to break up the original molecular composition of the symbiotic ore, and carries out recombination on the ore phase of the symbiotic ore to obtain lead sulfide and antimony sulfide; lead sulfide is separated by floatation, so that enrichment of lead sulfide and antimony sulfide is realized. The separation method provided by the invention is simple and easy to operate, and the treatment efficiency of the paragenetic ore is greatly improved.
Drawings
FIG. 1 is a schematic flow chart of the method for treating paragenetic ore according to the embodiment of the invention.
Detailed Description
The invention provides a method for separating lead and antimony from paragenetic ore, which comprises the following steps:
Carrying out vacuum pyrolysis on the symbiotic ore to realize ore phase recombination and obtain a recombined product, wherein the ore phase in the recombined product comprises PbS and Sb 2S3; the temperature of the vacuum pyrolysis is 500-600 ℃;
and (3) carrying out flotation on the recombined product to obtain lead sulfide concentrate and antimony sulfide tailings.
The invention carries out vacuum pyrolysis on the symbiotic ore to realize ore phase recombination and obtain a recombination product. In the present invention, the intergrown ore middling phase preferably includes FeSb 4Pb6S14, and the intergrown ore middling phase also preferably includes FeS and ZnS. In the present invention, the vacuum pyrolysis is preferably further comprised of: grinding the paragenetic ore and briquetting. In the present invention, the mass percentage of 200 mesh undersize in the ground material is preferably more than 60%, more preferably 65 to 80%. The grinding mode is not particularly required, so long as the required particle size can be achieved. In the invention, the shape of the pressed product is preferably a cylinder, and the diameter of the cross section of the cylinder is preferably 25-35 mm, more preferably 30mm; the height of the cylinder is preferably 7 to 12mm, more preferably 8 to 10mm. In the present invention, the pressure of the briquette is preferably 10 to 20MPa, more preferably 13 to 15MPa. In the present invention, the briquetting is preferably carried out in a mould, the shape and size of which is preferably set according to the briquettes after briquetting. In the invention, the pressing block can prevent the material from escaping and diffusing under the vacuum condition.
In the invention, the temperature of the vacuum pyrolysis is 500-600 ℃, preferably 550-580 ℃; the heat preservation time of the vacuum pyrolysis is preferably 20-50 min, preferably 35-45 min; the heating rate to the vacuum pyrolysis temperature is preferably 8 to 12K/min, more preferably 10K/min. In the present invention, the vacuum degree of the vacuum pyrolysis is preferably 1 to 10Pa, more preferably 5 to 8Pa. In the present invention, the temperature increase is preferably performed under vacuum.
In the invention, too high vacuum pyrolysis temperature can cause volatilization of Sb 2S3 after mineral decomposition along with the increase of temperature and time; the temperature and time of vacuum pyrolysis are controlled within the above ranges, so that the symbiotic ore can be ensured to carry out pyrolysis reaction to obtain lead sulfide and antimony sulfide, and the loss of pyrolysis products caused by volatilization is avoided. For example, when the temperature is greater than 600 ℃ and less than or equal to 750 ℃, sb 2S3 volatilizes into the gas phase, while lead sulfide partially enters the gas phase in sublimated form; when the temperature is higher than 750 ℃, the antimony sulfide and the lead sulfide are decomposed, wherein the decomposition products of the antimony sulfide are Sb and S 2, and the decomposition products of the lead sulfide are Pb and S 2.
In the present invention, the vacuum pyrolysis further preferably includes: the product after vacuum pyrolysis is cooled. In the present invention, the system temperature after cooling is preferably 20 to 30 ℃, more preferably 25 to 28 ℃. In the present invention, the cooling is preferably furnace-following cooling.
In the present invention, the mineral phase of the recombinant product comprises PbS and Sb 2S3, and preferably FeS.
The invention carries out vacuum pyrolysis on the symbiotic ore to convert the ore phase of the symbiotic ore into metal sulfide, and fixes sulfur element in the sulfide ore, thereby reducing the generation of sulfur dioxide and avoiding environmental pollution. Compared with the traditional smelting method, the method provided by the invention better utilizes the characteristics of the substances, reduces the problems of energy consumption, pollution and the like in the traditional smelting, and accords with the concept of energy conservation and environmental protection.
After the recombinant product is obtained, the recombinant product is subjected to floatation to obtain lead sulfide concentrate and antimony sulfide tailings. In the present invention, the pre-flotation preferably further comprises: grinding the recombinant product; the mass percentage of 200 mesh undersize in the milled product is preferably 95% or more, more preferably 96 to 98%. The invention has no special requirement on the grinding as long as the required granularity can be obtained.
In the present invention, the pre-flotation preferably further comprises mixing the recombined product with a flotation solution, which preferably comprises a flotation agent, a collector, a frother and an alkaline pH adjuster. In the present invention, the flotation agent preferably comprises lead nitrate or pinitol oil, more preferably lead nitrate. In the present invention, the collector preferably includes ethionamide or butyl xanthate, more preferably ethionamide. In the invention, the collector is a collector of lead sulfide, so that the grade of lead sulfide concentrate is improved. In the present invention, the foaming agent preferably includes No. two oil. In the present invention, the alkaline pH adjuster preferably includes lime or sodium carbonate, more preferably lime.
In the present invention, the mass ratio of the flotation agent to the recombinant product is preferably 30 to 100 g/1 t, more preferably 50 to 80 g/1 t. In the present invention, the mass ratio of the collector to the recombinant product is preferably 20 to 100 g/1 t, more preferably 40 to 80 g/1 t. In the present invention, the mass ratio of the foaming agent to the recombinant product is preferably 10 to 50g:1t, more preferably 30 to 45g:1t. In the present invention, the mass ratio of the alkaline pH adjustor and the recombinant product is preferably 600 to 1000 g/1 t, more preferably 700 to 800 g/1 t.
In the present invention, the pH of the flotation solution is preferably 7 to 10, more preferably 8 to 9. The invention limits the pH value of the flotation solution to the above range to inhibit pyrite flotation and to increase the purity of the lead concentrate.
In the present invention, the method for preparing a flotation solution preferably comprises the steps of: and mixing a flotation agent, a collector, a foaming agent and an alkaline pH value regulator to obtain the flotation solution. In the present invention, the mixing is preferably performed under stirring, and the present invention has no special requirement for the stirring, as long as it can be uniformly mixed.
In the present invention, the flotation is preferably performed in a flotation machine. In the present invention, the rotation speed of the flotation machine is preferably 670 to 1200r/min, more preferably 800 to 1000r/min. In the present invention, flotation is complete when no froth is produced in the flotation machine.
In the present invention, the post-flotation preferably further comprises: and respectively drying the concentrate and the tailings obtained by flotation. The invention has no special requirements on the temperature and time of the drying, as long as the moisture on the surfaces of the concentrate and the tailings can be removed.
The invention separates lead sulfide from the recombined product through floatation to obtain lead sulfide concentrate, tailings after floatation comprise antimony sulfide and iron sulfide, and the lead sulfide concentrate and the tailings obtained through floatation can be directly used for smelting. In the invention, the grade of the lead sulfide concentrate is preferably 57-66%, more preferably 57.38-63.86%; the grade of the antimony sulfide tailings is preferably 36-44%, more preferably 38-43%. In the invention, the mass percentage of the ferric sulfide in the antimony sulfide tailings is preferably 11-14%, and more preferably 12-13%.
According to the separation method provided by the invention, under the vacuum condition, the original molecular composition of the symbiotic ore is broken through by controlling the pyrolysis temperature and the pyrolysis time, so that the aim of ore phase reconstruction is fulfilled, and the reconstructed product is subjected to floatation to realize efficient enrichment and separation of lead and antimony. The lead sulfide concentrate and the antimony sulfide tailings obtained by separation can be directly used for smelting lead and antimony respectively.
The separation method provided by the invention has the advantages of short process flow and high treatment efficiency, wherein the enriched product can be directly used in lead-antimony smelting without secondary treatment, compared with the traditional process, the production of lead-antimony alloy is avoided, and the problems of lead-antimony alloy production in the traditional smelting of paragenetic ore are solved from the source.
According to the embodiment of the invention, the symbiotic ore is treated according to the flow diagram shown in fig. 1; specifically, the symbiotic ore with the component FeSb 4Pb6S14 is subjected to vacuum thermal decomposition to obtain PbS, sb 2S3 and FeS, and then the mixture of Sb 2S3 and FeS and the PbS are obtained through floatation.
The technical solutions provided by the present invention are described in detail below in conjunction with examples for further illustrating the present invention, but they should not be construed as limiting the scope of the present invention.
Example 1
Grinding symbiotic ores with the components of FeSb 4Pb6S14, wherein the mass percentage of 200 mesh undersize products in the ground products is 70%; briquetting the grinded product in a cylindrical die with the height of 10mm and the diameter of 25mm, wherein the briquetting pressure is 10Mpa;
placing the pressed product in a vacuum furnace to carry out vacuum thermal decomposition for 45min under the conditions that the temperature is 520 ℃ and the vacuum degree is 1pa, and heating to 520 ℃ according to the heating rate of 10K/min; vacuum thermal decomposition and furnace cooling to 30 ℃ to obtain a recombinant product with main components of Sb 2S3, pbS and FeS;
Mixing lead nitrate, ethionine, no. two oil, lime and water under stirring to obtain a flotation solution with a pH value of 8; the flotation solution comprises 30g/L lead nitrate, 20g/L ethionine, 10g/L No. two oil and 1000g/L lime;
Grinding the recombined product, wherein the mass percentage of 200 mesh undersize products in the ground product is 97%; and (3) placing the ground recombinant product and the flotation solution in a flotation machine, starting aeration, stirring at a rotation speed of 1200r/min, collecting concentrate and tailings, and drying to obtain PbS concentrate and tailings Sb 2S3 and FeS.
Example 2
Grinding symbiotic ores with the components of FeSb 4Pb6S14, wherein the mass percentage of 200 mesh undersize products in the ground products is 75%; briquetting the grinded product in a die of a cylinder with the height of 7mm and the diameter of 25mm, wherein the briquetting pressure is 15Mpa;
Placing the pressed product in a vacuum furnace to carry out vacuum thermal decomposition for 50min under the conditions that the temperature is 500 ℃ and the vacuum degree is 5pa, and heating to 500 ℃ according to the heating rate of 10K/min; vacuum thermal decomposition and furnace cooling to 30 ℃ to obtain a recombinant product with main components of Sb 2S3, pbS and FeS;
Mixing lead nitrate, ethionine, no. two oil, lime and water under stirring to obtain a flotation solution with a pH value of 8; the flotation solution comprises 50g/L lead nitrate, 40g/L ethionine, 30g/L No. two oil and 1000g/L lime;
Grinding the recombined product, wherein the mass percentage of 200 mesh undersize products in the ground product is 97%; and (3) placing the ground recombinant product and the flotation solution in a flotation machine, starting aeration, stirring at a rotating speed of 1000r/min, collecting concentrate and tailings, and drying to obtain PbS concentrate and tailings Sb 2S3 and FeS.
Example 3
Grinding symbiotic ores with the components of FeSb 4Pb6S14, wherein the mass percentage of 200 mesh undersize products in the ground products is 80%; briquetting the grinded product in a die of a cylinder with the height of 5mm and the diameter of 30mm, wherein the briquetting pressure is 10Mpa;
Placing the pressed product in a vacuum furnace to carry out vacuum thermal decomposition for 20min under the conditions that the temperature is 550 ℃ and the vacuum degree is 10pa, and heating to 550 ℃ according to the heating rate of 10K/min; vacuum thermal decomposition and furnace cooling to 30 ℃ to obtain a recombinant product with main components of Sb 2S3, pbS and FeS;
Mixing lead nitrate, ethionine, no. two oil, lime and water under stirring to obtain a flotation solution with a pH value of 8; the flotation solution comprises 80g/L lead nitrate, 100g/L ethionine, 50g/L No. two oil and 700g/L lime;
Grinding the recombined product, wherein the mass percentage of 200 mesh undersize products in the ground product is 98%; and (3) placing the ground recombinant product and the flotation solution in a flotation machine, starting aeration, stirring at a speed of 670r/min, collecting concentrate and tailings, and drying to obtain PbS concentrate and tailings Sb 2S3 and FeS.
The grade and recovery rate of the lead sulfide concentrate and antimony sulfide tailings obtained in examples 1 to 3 were examined by fluorescence spectrum analysis, and the results are shown in Table 1.
Table 1 grade and recovery of concentrates and tailings obtained in examples 1 to 3
As can be seen from Table 1, the method provided by the invention can obtain high-grade lead sulfide and antimony sulfide, and the recovery rate of lead and antimony is higher.
Although the foregoing embodiments have been described in some, but not all, embodiments of the invention, it should be understood that other embodiments may be devised in accordance with the present embodiments without departing from the spirit and scope of the invention.
Claims (9)
1. A method for separating lead and antimony from intergrown ores, comprising the steps of:
Carrying out vacuum pyrolysis on the symbiotic ore to realize ore phase recombination and obtaining a recombination product, wherein the recombination product comprises lead sulfide and antimony sulfide; the temperature of the vacuum pyrolysis is 500-600 ℃;
carrying out flotation on the recombined product to obtain lead sulfide concentrate and antimony sulfide tailings;
The method comprises the steps of mixing a recombined product with a flotation solution before flotation, wherein the flotation solution comprises an activating agent, a collecting agent, a foaming agent and an alkaline pH value regulator; the collector comprises ethionamide or butyl xanthate; the preparation method of the flotation solution comprises the following steps: mixing an activating agent, a collecting agent, a foaming agent and an alkaline pH value regulator to obtain the flotation solution.
2. The method for separating lead and antimony from paragenetic ore of claim 1, wherein the vacuum degree of vacuum pyrolysis is 1-10 pa.
3. The method for separating lead and antimony from paragenetic ore according to claim 1, wherein the heating rate for heating to the vacuum pyrolysis temperature is 8-12 k/min.
4. The method of separating lead and antimony from intergrown ore according to claim 1, wherein the intergrown ore mineral phase comprises FeSb 4Pb6S14.
5. The method for separating lead and antimony from paragenetic ore according to any one of claims 1-4, wherein the vacuum pyrolysis is preceded by: grinding the paragenetic ore and briquetting.
6. The method for separating lead and antimony from paragenetic ore of claim 1, wherein the vacuum pyrolysis is carried out for 20-50 min.
7. The method of separating lead and antimony from intergrown ore according to claim 1, wherein the activator comprises lead nitrate; the foaming agent comprises No. two oil; the alkaline pH regulator comprises lime or sodium carbonate.
8. The method for separating lead and antimony from intergrowth ore according to claim 7, wherein the pH of the flotation solution is 7-10.
9. The method for separating lead and antimony from paragenetic ore according to claim 1, wherein the grade of the lead sulfide concentrate is 57-66%; the grade of the antimony sulfide tailings is 36-44%.
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| CN202211306696.1A CN115722347B (en) | 2022-10-25 | 2022-10-25 | Method for separating lead and antimony from paragenetic ore |
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| CN202211306696.1A CN115722347B (en) | 2022-10-25 | 2022-10-25 | Method for separating lead and antimony from paragenetic ore |
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| CN115722347A CN115722347A (en) | 2023-03-03 |
| CN115722347B true CN115722347B (en) | 2024-07-05 |
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| GB1349041A (en) * | 1971-12-30 | 1974-03-27 | Occidental Petroleum Corp | Hydro metallurgical preparation of the oxides of antimony and antimonic acid |
| US4081364A (en) * | 1976-07-08 | 1978-03-28 | Engelhard Minerals & Chemicals Corporation | Froth flotation method for stibnite |
| US5074994A (en) * | 1990-10-18 | 1991-12-24 | The Doe Run Company | Sequential and selective flotation of sulfide ores |
| CN1388255A (en) * | 2001-05-25 | 2003-01-01 | 柳州市环东金属材料厂 | Method of processing antimong-containing material |
| CN100558468C (en) * | 2007-05-23 | 2009-11-11 | 华锡集团车河选矿厂 | Novel technics of cassiterite clay flotation |
| CN101204681B (en) * | 2007-09-03 | 2010-12-08 | 沈阳鑫博工业技术发展有限公司 | Method of refining iron ore from alkaline red mud and making gangue neutral |
| CN101696475B (en) * | 2009-10-29 | 2012-08-01 | 昆明理工大学 | Method for separating ternary alloy of lead, tin and stibium |
| CN104451188B (en) * | 2014-11-18 | 2018-03-06 | 昆明理工大学 | A kind of method of application of vacuum jamesonite separation lead antimony |
| CN104694736B (en) * | 2015-03-23 | 2017-01-11 | 东北大学 | Calcium roasting floatation separation method for bastnaesite |
| CN106222397A (en) * | 2016-08-04 | 2016-12-14 | 中南大学 | A kind of utilize pyrite sulfidation roasting smithsonite and the method for Zn accumulation galvanized iron |
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| "脆硫铅锑矿的分解行为研究";王威等;《真空科学与技术学报》;20150731;第35卷(第7期);第862-866页 * |
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