A method of carbon-lead bulk concentrate flotation separation

By combining ultrafine grinding and surface passivation treatment with multiple flotation processes, the problems of high reagent consumption and environmental pollution in the separation of carbon-lead mixed concentrates have been solved, achieving efficient and environmentally friendly carbon-lead separation.

CN119114287BActive Publication Date: 2025-12-09安徽铜冠产业技术研究院有限责任公司
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Patent Information

Application Number
CN202411430393.X
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-10-14
Publication Date
2025-12-09
Estimated Expiration
2044-10-14

AI Technical Summary

Technical Problem

In carbonaceous sulfide lead-zinc ores, the natural floatability of carbonaceous materials is good, and they are closely associated with lead-zinc minerals. This results in high reagent consumption and low product grade during lead-zinc flotation, and the use of potassium dichromate depressant poses a significant environmental hazard.

Method used

After ultrafine grinding, surface passivation treatment is performed using sulfuric acid, ferric chloride, and alum. Combined with multiple flotation processes using frothers and activators, the mixed carbon-lead concentrate is separated, avoiding the use of potassium dichromate.

Benefits of technology

It achieves the recovery of high-grade lead concentrate (>65%) and high recovery rate (>98%), without the need for additional inhibitors, is environmentally friendly and simplifies the reagent system, and improves carbon-lead separation efficiency.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present application relates to a kind of methods for separating carbon-lead mixed concentrate by flotation, belonging to the technical field of mineral processing, carbon-lead mixed concentrate is ground after superfine, add water to the pulp concentration of 10-15%; Add sulfuric acid, iron chloride and alum in turn and aerate stirring, passivate the surface of galena in carbon-lead mixed concentrate;Add foaming agent (2# oil) to carry out carbon roughing to obtain carbon rough concentrate and roughing tailings, separate carbon rough concentrate and roughing tailings storage;Add foaming agent (2# oil) to roughing tailings to carry out two carbon roughing, and the tailings of scavenging are lead concentrate.The present application obtains lead concentrate, and the lead grade is greater than 65%, and the lead recovery rate is greater than 98%;Galena is passivated and flocculated agglomeration by using iron chloride and alum, and the separation of carbon-lead mixed concentrate does not need to add depressor to depress galena, which simplifies the reagent system of carbon-lead separation, and ideal separation effect is obtained.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of ore dressing, and particularly relates to a method for flotation separation of carbon-lead mixed concentrate. BACKGROUND

[0002] In carbon-containing lead-zinc sulfide ore, due to the better natural floatability of carbon and the close intergrowth between carbon and lead-zinc minerals, in the lead-zinc flotation process, not only the reagent consumption is large, but also carbon is easy to enter the lead-zinc concentrate product, resulting in low grade of the lead-zinc concentrate product and difficulty in obtaining qualified products.

[0003] Generally, for carbon-containing lead-zinc ore, the current process technology generally eliminates the influence of carbon on lead-zinc flotation through three ways, i.e., pre-decarbonization, carbon suppression direct flotation of lead and zinc, and carbon-lead mixed flotation and then separation, and the research on lead suppression carbon flotation is relatively less, and generally, potassium dichromate is used for lead suppression carbon flotation, and the effect is relatively ideal, but potassium dichromate is a toxic substance and is harmful to the environment. SUMMARY

[0004] The purpose of the present application is to provide a method for flotation separation of carbon-lead mixed concentrate to solve the above problems.

[0005] The present application achieves the above-mentioned purpose through the following technical solutions:

[0006] The present application provides a method for flotation separation of carbon-lead mixed concentrate, comprising the following steps:

[0007] Step S1, after the carbon-lead mixed concentrate is finely ground, water is added to a pulp concentration of 10-15%;

[0008] Step S2, sulfuric acid, ferric chloride and alum are sequentially added and aerated and stirred to passivate the surface of galena in the carbon-lead mixed concentrate;

[0009] Step S3, a frother (2# oil) is added to perform carbon roughing to obtain carbon rough concentrate and roughing tailings, and the carbon rough concentrate and the roughing tailings are stored separately;

[0010] Step S4, the frother (2# oil) is added to the roughing tailings to perform two times of carbon roughing, and the scavenging tailings are lead concentrate;

[0011] Step S5, an activator is added to the carbon rough concentrate for immersion concentration, the concentration solution is added three times, respectively at 12h, 24h and 36h of immersion, and is taken out at 48h of immersion, and river water is used to flush to the surface without activator residue to obtain carbon concentrate.

[0012] As a further optimization scheme of the present application, the carbon-lead mixed concentrate has a lead grade of 45.67%-52.64% and a carbon grade of 3.81%-6.88%, the lead concentrate is galena, the carbon concentrate is elemental organic carbon and carbonaceous shale, the fineness is 55%-0.074 mm, and the monomer dissociation degree of lead minerals is 95%; the grinding fineness of the carbon-lead mixed concentrate is (90%-95%) -0.015 mm, and the pulp concentration is 10-15%.

[0013] As a further optimization scheme of the present application, the sulfuric acid is used in an amount of 500-800 g / t, the pH value of the ore slurry is adjusted to 4-5, then 1000-1500 g / t of ferric chloride and 500-1000 g / t of alum are added, and the aeration stirring is performed for 22-26 h.

[0014] As a further optimization scheme of the present application, the carbon roughing frother (No. 2 oil) is used in an amount of 30-50 g / t, the No. 2 oil is used in an amount of 10-20 g / t in the first carbon roughing, and the No. 2 oil is used in an amount of 10-15 g / t in the second carbon roughing.

[0015] As a further optimization scheme of the present application, the frother (No. 2 oil) is one of butyl xanthate or pine oil.

[0016] As a further optimization scheme of the present application, the preparation process of the activator is that sodium hydroxide, quicklime, ore powder, cellulose, fermented wheat straw fragments and pure water are mixed, injected into a fermentation tank, and fermented for 1-2 days to obtain the activator.

[0017] As a further optimization scheme of the present application, according to weight parts, the preparation raw materials of the activator include 20-35 parts of sodium hydroxide, 45-50 parts of quicklime, 15-35 parts of ore powder, 5-10 parts of cellulose, 8-16 parts of fermented wheat straw fragments and 70-85 parts of pure water.

[0018] As a further optimization scheme of the present application, the preparation process of the ore powder is that arsenopyrite, tungsten ore and volcanic rock are ground, sieved, and the particles with a particle size of 1-3 cm are taken as the ore powder.

[0019] As a further optimization scheme of the present application, according to weight parts, the preparation raw materials of the ore powder include 30-35 parts of arsenopyrite, 20-30 parts of tungsten ore and 15-28 parts of volcanic rock.

[0020] The present application has the following beneficial effects:

[0021] (1) The present application obtains a lead concentrate with a lead grade greater than 65% and a lead recovery rate greater than 98%;

[0022] (2) using ferric chloride and alum for surface passivation and flocculation agglomeration of galena, the separation of carbon lead mixed concentrate does not need to add inhibitor to inhibit galena, which simplifies the reagent system of carbon lead separation and achieves ideal separation effect;

[0023] (3) the carbon lead mixed rough concentrate is superfine ground, and the fineness reaches 90%-95% 0.015mm, which not only increases the specific surface area of galena and is beneficial to surface passivation, but also plays a surface scrubbing and drug removal role, so that the carbon lead is easy to separate;

[0024] (4) ferric chloride and alum are natural inorganic salts, non-toxic and environmentally friendly, which eliminates the potential harm to human body and environment caused by using a large amount of potassium dichromate as a galena inhibitor;

[0025] (5) the cleaning solution is added in three times, respectively at 12h, 24h and 36h, and is taken out at 48h, and the carbon concentrate is obtained by washing with river water until there is no active agent residue on the surface, and the cleaning solution is added in three stages, which can increase the yield of carbon concentrate. BRIEF DESCRIPTION OF DRAWINGS

[0026] Figure 1 It is the flow chart of the carbon lead mixed concentrate separation method of the application. DETAILED DESCRIPTION

[0027] It is necessary to point out here that the following detailed description is only used to further illustrate the application, and cannot be understood as limiting the protection scope of the application, and the skilled in the art can make some non-essential improvements and adjustments to the application according to the above application content.

[0028] The method used in the application is a conventional method known by the skilled in the art, and the reagents and materials used are commercially available products, unless otherwise specified.

[0029] The preparation process of the fermented wheat straw pieces in the application is as follows: take the wheat straw of the season, crush it to a length of 2-3cm; put the wheat straw pieces in an open container, add water to cover the wheat straw pieces, ferment for 15d, filter out the water, and obtain the fermented wheat straw pieces.

[0030] Example 1

[0031] The lead grade of the carbon lead mixed concentrate is 45.67%, the carbon grade is 6.88%, the lead concentrate is galena, the carbon concentrate is elemental organic carbon and carbonaceous shale, the fineness is 55%-0.074mm, and the single liberation degree of lead minerals is 95%;

[0032] The galena is surface passivated by grinding the carbon-lead mixed concentrate to 95%-0.015mm, adding water to the slurry to a slurry concentration of 15%, and then sequentially adding 600g / t sulfuric acid, 1100g / t ferric chloride and 500g / t alum to the slurry, and aerating and stirring for 24h;

[0033] After the galena is surface passivated, 40g / t of No.2 oil is sequentially added to the slurry to perform carbon roughing, and a carbon rough concentrate and a roughing tailing are obtained. The roughing tailing is added with No.2 oil to perform two carbon scavenging roughing, the first time with 20g / t of No.2 oil and the second time with 10g / t of No.2 oil, and a lead concentrate is obtained from the scavenging tailing. The carbon rough concentrate is subjected to three times of cleaning to obtain a lead concentrate, and the cleaning process is as follows: the carbon rough concentrate is added with an activator to soak, the cleaning solution is added in three times, at 12h, 24h and 36h of soaking respectively, and the soaking is taken out at 48h of soaking, and the surface is washed with river water until no activator is left, and a carbon concentrate is obtained.

[0034] The preparation process of the activator is as follows: 20 parts of sodium hydroxide, 45 parts of quicklime, 15 parts of ore powder, 5 parts of cellulose, 8 parts of fermented wheat straw and 70 parts of pure water are mixed, and then poured into a fermentation tank, and fermented for 1d, and then taken out to obtain the activator.

[0035] The preparation process of the ore powder is as follows: 30 parts of arsenopyrite, 20 parts of tungsten ore and 15 parts of volcanic rock are ground, sieved, and particles with a particle size of 1-3cm are taken as the ore powder.

[0036] Comparative Example 1

[0037] The galena inhibitor is tested when potassium dichromate is used to separate the carbon-lead mixed concentrate. The carbon-lead mixed concentrate is ground to 95%-0.045mm, and the slurry is adjusted to a slurry concentration of 15%, and then 8000g / t of potassium dichromate, 40g / t of kerosene and 30g / t of No.2 oil are sequentially added to perform carbon roughing, and a carbon rough concentrate and a roughing tailing are obtained. The roughing tailing is added with kerosene to perform scavenging, the first time with 15g / t of kerosene and the second time with 10g / t of kerosene, and a lead concentrate is obtained from the scavenging tailing. The carbon rough concentrate is added with potassium dichromate to perform three times of cleaning, and a carbon concentrate is obtained, and the lime dosages of the first cleaning, the second cleaning and the third cleaning are 5000g / t, 2000g / t and 1000g / t respectively.

[0038] The test results of Example 1 and Comparative Example 1 are shown in Table 1.

[0039] Table 1 Test results of Example 1 and Comparative Example 1 (%)

[0040]

[0041] Example 2

[0042] The carbon-lead mixed concentrate has a lead grade of 52.64% and a carbon grade of 3.81%. The lead concentrate is galena, and the carbon concentrate is elemental organic carbon and carbonaceous shale. The fineness is 60%-0.074 mm, and the single liberation degree of lead minerals is 95%.

[0043] The carbon-lead mixed concentrate is ground to 95%-0.015 mm, and water is added to the slurry to a concentration of 15%. Then, 800 g / t of sulfuric acid, 1500 g / t of ferric chloride and 600 g / t of alum are sequentially added to the slurry, and the galena is surface passivated by stirring for 24 h.

[0044] After the surface of the galena is passivated, 45 g / t of No. 2 oil is sequentially added to the slurry to perform carbon roughing, and a carbon rough concentrate and a roughing tailing are obtained. The roughing tailing is added with No. 2 oil twice to perform carbon roughing. The first time, 25 g / t of No. 2 oil is added, and the second time, 15 g / t of No. 2 oil is added. The sweeping tailing is obtained as a lead concentrate. The carbon rough concentrate is subjected to three times of cleaning to obtain a lead concentrate. The cleaning process is as follows: the carbon rough concentrate is soaked with an activator, and the cleaning solution is added three times at 12 h, 24 h and 36 h, respectively. The soaking is stopped at 48 h, and the carbon concentrate is obtained by washing the surface with river water until no activator is left.

[0045] The preparation process of the activator is as follows: 35 parts of sodium hydroxide, 50 parts of quicklime, 35 parts of ore powder, 10 parts of cellulose, 16 parts of fermented wheat straw and 85 parts of pure water are mixed, and then poured into a fermentation tank. After 2 days of fermentation, the activator is obtained.

[0046] The preparation process of the ore powder is as follows: 35 parts of arsenic pyrite, 30 parts of tungsten ore and 28 parts of volcanic rock are ground and sieved, and particles with a particle size of 1-3 cm are taken as the ore powder.

[0047] Comparative Example 2

[0048] Potassium dichromate is used as a galena depressant for the separation of carbon-lead mixed concentrate. The carbon-lead mixed concentrate is ground to 95%-0.045 mm, and the slurry is adjusted to a concentration of 15%. Then, 6000 g / t of potassium dichromate, 30 g / t of kerosene and 25 g / t of No. 2 oil are sequentially added to the slurry to perform carbon roughing, and a carbon rough concentrate and a roughing tailing are obtained. The roughing tailing is added with kerosene to perform sweeping, and the sweeping tailing is obtained as a lead concentrate. The sweeping is performed twice, and 18 g / t of kerosene is added in the first sweeping, and 15 g / t of kerosene is added in the second sweeping. The carbon rough concentrate is added with potassium dichromate to perform three times of cleaning to obtain a carbon concentrate. The lime dosages for the first cleaning, the second cleaning and the third cleaning are 4000 g / t, 2000 g / t and 2000 g / t, respectively.

[0049] The test results of Example 2 and Comparative Example 2 are shown in Table 2.

[0050] Table 2 Test results of Example 2 and Comparative Example 2 (%)

[0051]

[0052] Under weakly acidic and aerobic conditions, Fe3+ in FeCl3 will have a strong redox reaction with galena, producing active Fe2+ in the surface lattice of galena, which will be rapidly oxidized to Fe3+ and react with K- and Al3+ in the alum to generate a dense jarosite (KFe3(SO4)2(OH)6) passivation film on the surface of galena, making the galena hydrophilic and the floatability inhibited. The main chemical reaction process is as follows:

[0053] PbS + 2Fe 3+ → 0.125S8 + 2Fe 2+ + Pb 2+

[0054] 2Fe 2+ + 0.5O2 + 2H + → 2Fe 3+ + H2O

[0055]

[0056] Jarosite (KFe3(SO4)2(OH)6) has great hydrophilicity, and after the formation of the jarosite (KFe3(SO4)2(OH)6) passivation film on the surface of galena, the hydrophilicity of the galena is greatly improved, and at the same time, Al3+ in the alum has a flocculation and aggregation effect on the fine-grained galena after surface passivation, further increasing the hydrophilicity, so that it is difficult for the collector to adsorb on the surface, and thus no additional lead depressant is needed for the separation of carbon-lead mixed concentrate

[0057] The above-described embodiments only express several embodiments of the present application, and the description is more specific and detailed, but it should not be understood as a limitation on the scope of the patent of the present application. It should be noted that for ordinary skilled in the art, without departing from the concept of the present application, a number of modifications and improvements can be made, which are within the scope of protection of the present application.

Claims

1. A method of carbon-lead bulk concentrate flotation separation, characterised by, The method comprises the following steps: Step S1, after superfine grinding of the carbon-lead mixed concentrate, water is added to a pulp concentration of 10-15%; Step S2, sulfuric acid, ferric chloride and alum are sequentially added and aerated and stirred to passivate the surface of the galena in the carbon-lead mixed concentrate; Step S3, a foaming agent is added to perform carbon roughing to obtain carbon rough concentrate and roughing tailings, and the carbon rough concentrate and the roughing tailings are stored separately; Step S4, the foaming agent is added to the roughing tailings to perform two times of carbon roughing, and the tailings of the carbon roughing are lead concentrate; Step S5, an activator is added to the carbon rough concentrate to perform leaching concentration, the leaching solution is added three times, respectively at 12h, 24h and 36h of leaching, and is taken out at 48h of leaching, and is washed to the surface with river water until no activator is left to obtain carbon concentrate; The preparation process of the activator is that sodium hydroxide, quicklime, ore powder, cellulose, fermented wheat straw and pure water are mixed, injected into a fermentation tank, and fermented for 1-2 days to obtain the activator; the preparation process of the ore powder is that arsenic pyrite, tungsten ore and volcanic rock are ground, sieved, and particles with a particle size of 1-3 cm are taken as the ore powder.

2. A method of carbon-lead bulk concentrate flotation separation according to claim 1, characterised in that, The carbon-lead mixed concentrate has a lead grade of 45.67%-52.64% and a carbon grade of 3.81%-6.88%, the lead concentrate is galena, the carbon concentrate is elemental organic carbon and carbonaceous shale, and the monomer liberation degree of the lead mineral is 95%; the grinding fineness of the carbon-lead mixed concentrate is 90%-95% of particles with a size of-0.015 mm, and the pulp concentration is 10-15%.

3. A method of carbon-lead bulk concentrate flotation separation according to claim 1, characterised in that, The sulfuric acid is used in an amount of 500-800g / t, the pH value of the ore pulp is adjusted to 4-5, 1000-1500g / t of ferric chloride and 500-1000g / t of alum are further added, and the aerated and stirred for 22-26h.

4. A method of carbon-lead bulk concentrate flotation separation according to claim 1, characterised in that, The foaming agent is used in an amount of 30-50g / t for the carbon roughing; in step S4, the foaming agent is used in an amount of 10-20g / t for the first time of carbon roughing and in an amount of 10-15g / t for the second time of carbon roughing.

5. A method of carbon-lead bulk concentrate flotation separation according to claim 1, characterised in that, The foaming agent is one of butyl xanthate or pine oil.

6. A method of carbon-lead bulk concentrate flotation separation according to claim 1, characterised in that, The preparation raw materials of the activator include, by weight parts, 20-35 parts of sodium hydroxide, 45-50 parts of quicklime, 15-35 parts of ore powder, 5-10 parts of cellulose, 8-16 parts of fermented wheat straw and 70-85 parts of pure water.

7. A method of carbon-lead bulk concentrate flotation separation according to claim 1, characterised in that, The preparation raw materials of the ore powder include, by weight parts, 30-35 parts of arsenic pyrite, 20-30 parts of tungsten ore and 15-28 parts of volcanic rock.

Citation Information

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