CN112718255B - Method for degrading mineral surface flotation reagent through electrochemical oxidation - Google Patents
Method for degrading mineral surface flotation reagent through electrochemical oxidation Download PDFInfo
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- CN112718255B CN112718255B CN202011424178.0A CN202011424178A CN112718255B CN 112718255 B CN112718255 B CN 112718255B CN 202011424178 A CN202011424178 A CN 202011424178A CN 112718255 B CN112718255 B CN 112718255B
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- B03—SEPARATION OF SOLID MATERIALS USING LIQUIDS OR USING PNEUMATIC TABLES OR JIGS; MAGNETIC OR ELECTROSTATIC SEPARATION OF SOLID MATERIALS FROM SOLID MATERIALS OR FLUIDS; SEPARATION BY HIGH-VOLTAGE ELECTRIC FIELDS
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Abstract
The invention discloses a method for electrochemically oxidizing and degrading a mineral surface flotation reagent. The method directly electrolyzes the flotation ore pulp by using impressed currents with different strengths and electrolytes with different concentrations and types according to the difference of electrochemical behaviors of different flotation reagents and the balance principle of flotation solution chemistry, so as to realize directional oxidation desorption and degradation of the organic reagents adsorbed on the surfaces of the minerals.
Description
Technical Field
The invention relates to a method for removing a mineral surface flotation reagent, in particular to a method for degrading the mineral surface flotation reagent through electrochemical oxidation, and belongs to the technical field of mineral separation.
Background
Along with the continuous development of the mineral engineering industry, mineral dressing medicaments are continuously updated, and organic medicaments gradually become the mainstream of the mineral dressing medicaments due to strong selectivity and collecting capacity of the organic medicaments, such as most of collecting agents of xanthate, sulfur nitrogen and thiamine of sulfide ores, sulfide ore inhibitor starch and modified products thereof, dextrin, humic acid, oxidized ore collecting agents of fatty acid, amine, hydroximic acid and the like. In flotation pulp, especially concentrate pulp, a large amount of organic agents are adsorbed on the surface of minerals. Most of the organic medicaments have complex structures, long hydrocarbon chains and many functional groups, and the organic medicaments not only rely on simple physical adsorption but also rely on strong chemical adsorption to act on the surface of minerals, so that the degradation of the organic medicaments is difficult. Excessive adsorption of the mineral surface agent influences adsorption of other agents in a subsequent beneficiation process on the one hand, and harmful gas is released in subsequent filtering and drying processes on the other hand, so that a serious environmental protection problem is caused. In addition, in the combined process of concentration and metallurgy, if a large amount of flotation reagents are adsorbed on the surface of flotation concentrate, the reagents can change the foam state when entering the pretreatment stage of the metallurgical acid method, so that the foam layer can grow rapidly, and the phenomena of overflow of a trough and the like can occur.
To date, methods for treating mineral surfaces in mineral slurries by adsorption of chemicals have been rare. Conventional treatment methods, such as the oxidizing method with a strong oxidizing agent such as potassium permanganate, have poor selectivity and low treatment efficiency, and although it is described in the literature that this method has a significant effect on the treatment of organic substances present in a solution, it is difficult to treat organic substances adsorbed on the surface of minerals. The electrolysis belongs to an advanced oxidation method and is widely applied to the industries of chemical industry, materials, mineral separation, metallurgy and the like. The electrochemical properties of different organic substances are obviously different, and different behaviors can be shown under the condition of an external power supply. The electrolytic method has higher treatment efficiency when treating single organic matters or organic matters in solution, but is rarely used for treating organic agents adsorbed on the surface of minerals in ore pulp. If the organic matter on the surface of the mineral is treated by an electrolytic method, the key of the technology is how to selectively degrade the organic matter and how to improve the degradation efficiency.
Disclosure of Invention
Aiming at the technical problem that the flotation reagent on the surface of the mineral is difficult to oxidize and degrade in the prior art, the invention aims to provide the method for directly treating the organic reagent adsorbed on the surface of the mineral in the flotation pulp by utilizing the electrochemical degradation method, which can realize the efficient degradation of residual or excessive reagent in the beneficiation process, can pertinently and selectively degrade the specific organic reagent adsorbed on the surface of the mineral, prevent the metal ions in the mineral from dissolving out and the reagent which does not influence the surface adsorption of other minerals, reduce the electric energy loss, solve the phenomenon that the reagent on the surface of the mineral overflows from a metallurgical pretreatment section in the beneficiation process, and achieve the purpose of effectively linking the flotation, beneficiation and metallurgy of different minerals.
In order to achieve the technical purpose, the invention provides a method for electrochemically oxidizing and degrading a mineral surface flotation reagent.
As a preferred scheme, the concentrate is metal sulfide ore or metal oxide ore; the metal sulfide ore is at least one of chalcopyrite, pyrite and sphalerite; the oxidized ore is at least one of scheelite, wolframite, calcite, fluorite, cassiterite and quartz.
As a preferred embodiment, the surface of the concentrate contains at least one of xanthate flotation agents, sulfur and nitrogen flotation agents, thiamine flotation agents, hydroxamic acid flotation agents, fatty acid flotation agents, and amine flotation agents.
In a more preferred embodiment, when the concentrate is a metal sulfide ore, the surface of the metal sulfide ore contains at least one of xanthate flotation agents, sulfur and nitrogen flotation agents and thiamine flotation agents.
In a more preferred embodiment, when the concentrate is a metal oxide ore, the surface of the metal oxide ore contains at least one of a hydroxamic acid flotation agent, a fatty acid flotation agent and an amine flotation agent.
As a preferable scheme, the electrolyte is at least one of halogen potassium salt, halogen sodium salt, sodium sulfate and potassium sulfate; the adding concentration of the electrolyte in the ore pulp is 10 g/L-500 g/L.
As a preferable scheme, when the concentrate is metal oxide ore, the corresponding electrolyte is selected to be halogen potassium salt and/or halogen sodium salt, and the adding concentration of the electrolyte in the concentrate ore pulp is 10-200 g/L.
As a preferable scheme, when the concentrate is metal sulfide ore, the corresponding electrolyte is selected from sodium sulfate and/or potassium sulfate, and the adding concentration of the electrolyte in the concentrate ore pulp is 200-500 g/L. The preferred sulfate salts may inhibit the dissolution of metal ions from the metal minerals during electrolysis.
As a preferable proposal, the concentration of the hydrogen ions in the ore pulp is adjusted to be 1 x 10-5mol/L～1×10-1mol/L. MineThe acidity of the slurry is adjusted by common inorganic acid such as hydrochloric acid.
As a preferable proposal, when the concentrate is metal oxide ore, the concentration of hydrogen ions in the ore pulp is adjusted to be 1 x 10-5mol/L～1×10-3mol/L. Metal oxide ores are easily dissolved by acid, and therefore a lower acid concentration is required.
As a preferable proposal, when the concentrate is metal sulfide ore, the concentration of hydrogen ions in the ore pulp is adjusted to be 1 x 10-3mol/L～1×10-1mol/L。
Preferably, the intensity of the current is 100 mA-5000 mA.
As a preferable scheme, when the concentrate is metal oxide ore, the corresponding current intensity is 500-5000 mA. The metal oxide ore has stronger adsorption capacity to the flotation collector, and the flotation collector can be deeply oxidized and degraded only by higher current density.
As a preferable scheme, when the concentrate is metal sulfide ore, the corresponding current intensity is 100-500 mA. The metal sulfide ore has strong reducibility, and the lower current density can prevent the metal ions in the ore from dissolving out
As a preferred scheme, the inert cathode and anode electrodes are graphite electrodes.
As a preferred embodiment: the invention provides a method for electrochemically oxidizing and degrading a mineral surface flotation reagent, which is characterized in that when concentrate is metal sulfide ore, 200-500 g/L sodium sulfate is added into ore pulp as electrolyte, and hydrochloric acid is adopted to adjust the concentration of hydrogen ions in the ore pulp to be 1 x 10-3mol/L～1×10-1And (3) placing inert negative and positive electrodes in the ore pulp, and introducing 100-500 mA current to carry out electrochemical oxidation degradation on the flotation agent on the surface of the concentrate in the ore pulp.
As a preferred embodiment: the invention provides a method for electrochemically oxidizing and degrading a mineral surface flotation reagent, which is characterized in that when concentrate is metal oxide ore, 10-200 g/L sodium chloride is added into ore pulp as electrolyte, and hydrochloric acid is adopted to adjust the concentration of hydrogen ions in the ore pulp to be 1 x 10-5mol/L～1×10-5mol/And L, placing inert positive and negative electrodes in the ore pulp, and introducing 500-5000 mA current to carry out electrochemical oxidation degradation on the flotation agent on the surface of the concentrate in the ore pulp.
The key point of the technical scheme of the invention is that selective removal of the flotation reagent on the surface of the metal mineral is realized by controlling electrolyte type selection, electrolysis condition, acidity condition and the like according to different metal minerals and different flotation reagents adsorbed on the surfaces of different minerals. Numerous studies have shown that the electrochemical properties of the flotation reagent adsorbed on the surface of the metal sulfide ore and the metal oxide ore are not only dependent on the type of the organic reagent but also related to the electrochemical properties of the surface of the mineral, so that an appropriate method is required for the electrolytic oxidative degradation of the flotation reagent on the surface of the mineral. For metal sulfide ores, the main anion in the mineral composition is sulfide ion S2-It has active chemical property and is easily oxidized into sulfate radical ions SO4 2-If the electrolytic current intensity is too high, metal ions such as copper, lead, bismuth and the like on the surface of the mineral are dissolved out, so that the degradation efficiency of the organic chemical on the surface is reduced, therefore, when the organic chemical on the surface of the sulfide ore is degraded through electro-oxidation, the current is controlled to be stable in a range that the organic chemical is degraded but the ions on the surface of the sulfide ore are not influenced, and a sulfate electrolyte is added to inhibit the electrolytic reaction of mineral components. For metal oxide ores, the mineral components are oxides and have stable properties. The difficulty of the electrolytic oxidation degradation of the organic medicament lies in that the organic medicament and the mineral surface have strong chemical adsorption, so the electrolytic oxidation degradation is carried out by using larger current intensity, the loss of water in ore pulp is controlled, the acidity cannot be too high, metal ions are easy to dissolve out due to too high acidity, and the electrolyte adopts conventional chloride to reduce the cost.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1. the method directly treats the organic agents adsorbed on the surfaces of the minerals in the ore pulp by an electrolytic oxidation method, has the characteristics of high degradation efficiency and good selectivity, is simple, has wide application range, and can be used for removing most of the organic agents in the ore dressing process.
2. The invention does not need to add dangerous chemical agents such as strong oxidant and the like, and is safe and non-toxic; no harmful fume is generated in the treatment process, and the method is clean and pollution-free.
3. The method for degrading the mineral surface flotation reagent by electrochemical oxidation can be used for a sulfide ore and oxide ore linking section (firstly, sulfide ore is floated and then oxide ore is floated) in a beneficiation process or a beneficiation and metallurgy linking section in a beneficiation and metallurgy combined process, is particularly suitable for a linking link of a beneficiation and metallurgy combined process of tungsten ore resources, can solve the problem that the enrichment of other useful minerals is influenced by excessive reagents in the beneficiation process, and can also eliminate the problems of harmful gas release in the subsequent filtering and drying processes of flotation concentrate, foam overflow grooves of a pretreatment section and the like in the beneficiation and metallurgy combined process.
4. The invention aims at different metal minerals and different flotation reagents adsorbed on the surfaces of different minerals, realizes the high-selectivity removal of the flotation reagents on the surfaces of the metal minerals by controlling the selection of the types of electrolytes, the electrolysis conditions, the acidity conditions and the like, can prevent the metal ions in the minerals from dissolving out, does not influence the reagents adsorbed on the surfaces of other minerals, and reduces the electric energy loss.
Drawings
FIG. 1 is a graph showing the relationship between the electrolysis time and the oxidative degradation effect in the electrochemical oxidative degradation and chemical removal process of tungsten concentrate pulp in example 3;
FIG. 2 is a graph showing the relationship between current density and oxidative degradation effect in the electrochemical oxidative degradation and reagent removal process of the tungsten concentrate pulp in example 4;
FIG. 3 is a graph showing the relationship between the pH of the pulp and the effect of oxidative degradation in the electrochemical oxidative degradation and reagent removal process performed on the tungsten concentrate pulp in example 5.
Detailed Description
The following examples are intended to further illustrate the present invention and are not intended to limit the scope of the invention as claimed.
Example 1
The multi-metal dressing plant of yellow terrace is a process for firstly flotating sulphide ore and then flotating oxide ore, a large amount of xanthate is remained in the dressing tailings (namely the tungsten dressing raw ore) of sulphur, so that the tungsten dressing section has excessive foam and is combinedThe properties are poor. Adopting the chemical agent on the surface of the sulfur-selecting tailings by electrolytic oxidation degradation, wherein the electrode is a graphite electrode, the current is 300mA, and the electrolyte is Na with the concentration of 200g/L2SO40.05mol/L hydrochloric acid was used in combination, and the electrolysis time was 0.5 hour. The COD values before and after electrolysis were as follows. The removal rate of organic matters on the surface of the mineral can reach 89.14 percent, which shows that the selectivity and the efficiency of the method are high.
Example 2
Flotation tungsten concentrate from Dongbo sorting factory in persimmon bamboo garden in Chenzhou, Hunan, contains a large amount of organic chemicals, mainly contains benzohydroxamic acid, and influences the filtration and packaging processes of products. A graphite electrode is selected, an impressed current is 1000mA, the concentration of NaCl electrolyte is 50g/L, 0.001mol/L hydrochloric acid is used, the electrolysis time is 1 hour, the electrolysis test is carried out on the flotation concentrate, and the changes of total organic carbon and total nitrogen in the solution are shown as follows. In the electrolysis process, the ore concentrate is prepared into ore pulp in advance by using distilled water, and organic matters on the surface of the mineral are desorbed from the surface of the mineral and enter the solution, so that the removal of the medicament on the surface of the mineral can be effectively realized.
Example 3
In order to solve the problem of foam overflow caused by the fact that agents adsorbed on the surface of minerals in the persimmon bamboo garden dressing and smelting combined process carry out metallurgical acid method pretreatment, a graphite electrode is selected, external current is 720mA, the concentration of electrolyte NaCl is 50g/L, 0.01mol/L hydrochloric acid is used, and an electrooxidation reagent removal test is carried out on the tungsten concentrate ore pulp subjected to flotation in the dressing and smelting combined process, and the result is shown in figure 1. It can be seen that as the electrolysis time increases, the foam layer formed by the acid foam pretreatment becomes thinner, the foam distribution becomes looser and the viscosity is obviously reduced.
Example 4
The flotation tungsten concentrate is taken as a research object, the surface organic reagent of the flotation tungsten concentrate is mainly benzohydroxamic acid to determine that the concentration of NaCl of an electrolyte is 30g/L, the electrode is a graphite electrode, and the current intensity test is carried out on the flotation tungsten concentrate, and the result is shown in figure 2. When the current is lower than 360mA, the change of the foam layer is not large, and when the current reaches or even exceeds 720mA, the foam layer is obviously reduced, and the foam becomes brittle and easy to break.
Example 5
In order to explore the influence of different pH values on the organic matters on the surface of the mineral subjected to electrolytic oxidation degradation, flotation tungsten concentrate is selected as a research object, the concentration of NaCl in electrolyte is determined to be 40g/L, and the result is shown in figure 3. It can be seen that with the continuous decrease of pH, the height of the foam layer is smaller and smaller, the foam viscosity is lower and lower, and the treatment effect is better and better.
Claims (9)
1. A method for electrochemically oxidizing and degrading a mineral surface flotation reagent is characterized by comprising the following steps: adding electrolyte into the ore pulp, adjusting the ore pulp to be acidic, placing inert positive and negative electrodes into the ore pulp, and introducing current to carry out electrochemical oxidation degradation on the flotation reagent on the surface of the concentrate in the ore pulp; the surface of the concentrate contains at least one of xanthate flotation agents, sulfur and nitrogen flotation agents, thiamine flotation agents, hydroximic acid flotation agents, fatty acid flotation agents and amine flotation agents.
2. The method for electrochemically oxidizing and degrading the chemical agent for the surface flotation of minerals according to claim 1, wherein:
the concentrate is metal sulfide ore, metal oxide ore or quartz;
the metal sulfide ore is at least one of chalcopyrite, pyrite and sphalerite;
the metal oxide ore is at least one of scheelite, wolframite, calcite, fluorite and cassiterite.
3. The method for electrochemically oxidizing and degrading the chemical agent for the surface flotation of minerals according to claim 1, wherein: when the concentrate is a metal sulfide ore, the surface of the metal sulfide ore contains at least one of xanthate flotation agents, sulfur and nitrogen flotation agents and thiamine flotation agents; when the concentrate is a metal oxide ore, the surface of the metal oxide ore contains at least one of hydroximic acid flotation agents, fatty acid flotation agents and amine flotation agents.
4. The method for electrochemically oxidizing and degrading the chemical agent for the surface flotation of minerals according to claim 1, wherein: the electrolyte is at least one of halogen potassium salt, halogen sodium salt, sodium sulfate and potassium sulfate; the adding concentration of the electrolyte in the ore pulp is 10 g/L-500 g/L.
5. The method for electrochemically oxidizing and degrading a mineral surface flotation reagent according to claim 1 or 4, wherein:
when the concentrate is metal oxide ore, the corresponding electrolyte is selected to be halogen potassium salt and/or halogen sodium salt, and the adding concentration of the electrolyte in the concentrate ore pulp is 10-200 g/L;
when the concentrate is metal sulfide ore, the corresponding electrolyte is selected to be sodium sulfate and/or potassium sulfate, and the adding concentration of the electrolyte in the concentrate ore pulp is 200-500 g/L.
6. The method for electrochemically oxidizing and degrading the chemical agent for the surface flotation of minerals according to claim 1, wherein: adjusting the concentration of hydrogen ions in the ore pulp to 1 x 10-5mol/L~ 1×10-1mol/L。
7. The method for electrochemically oxidizing and degrading a mineral surface flotation reagent according to claim 1 or 6, wherein:
when the concentrate is metal oxide ore, the concentration of hydrogen ions in the ore pulp is adjusted to 1 x 10-5mol/L~ 1×10-3mol/L；
When the concentrate is metal sulfide ore, the concentration of hydrogen ions in the ore pulp is adjusted to 1 x 10-3mol/L~ 1×10-1mol/L。
8. The method for electrochemically oxidizing and degrading the chemical agent for the surface flotation of minerals according to claim 1, wherein: the intensity of the current is 100 mA-5000 mA.
9. The method for electrochemically oxidatively degrading a mineral surface flotation reagent according to claim 1 or 8, wherein:
when the concentrate is metal oxide ore, the corresponding current intensity is 500-5000 mA;
when the concentrate is metal sulfide ore, the corresponding current intensity is 100-500 mA.
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