CN112371348B - Lead-zinc sulfide ore flotation separation inhibitor and application method thereof - Google Patents
Lead-zinc sulfide ore flotation separation inhibitor and application method thereof Download PDFInfo
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- CN112371348B CN112371348B CN202011477960.9A CN202011477960A CN112371348B CN 112371348 B CN112371348 B CN 112371348B CN 202011477960 A CN202011477960 A CN 202011477960A CN 112371348 B CN112371348 B CN 112371348B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/001—Flotation agents
- B03D1/004—Organic compounds
- B03D1/014—Organic compounds containing phosphorus
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/06—Depressants
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- B—PERFORMING OPERATIONS; TRANSPORTING
- 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
- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
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Abstract
The invention relates to the technical field of sulfide ore flotation reagents, in particular to a lead-zinc sulfide ore flotation separation inhibitor and an application method thereof. The invention specifically discloses an application method of a lead-zinc sulfide ore flotation separation inhibitor, which comprises the following steps of S1: adding water into lead-zinc sulfide minerals to obtain ore pulp; s2: adding 2-hydroxyphosphonoacetic acid into the pulp; s3: adjusting the pH value of the ore pulp; s4: and (4) performing air flotation to obtain a foam product and tailings. The inhibitor provided by the invention is simple to prepare, is environment-friendly and cannot generate pollution; the inhibitor has good solubility, strong selectivity, good inhibition effect, wide applicable pH range, small dosage, low price and easy large-scale popularization. The inhibitor has excellent inhibiting effect on sphalerite. The flotation separation method can be applied to flotation separation of lead-zinc bulk concentrates, and can realize high-efficiency flotation separation of sphalerite and galena.
Description
Technical Field
The invention relates to the technical field of sulfide ore flotation reagents, in particular to a lead-zinc sulfide ore flotation separation inhibitor and an application method thereof.
Background
The zinc blende is an important non-ferrous metal resource, occupies a great position in national economic development, and is widely applied to the fields of steel, chemical industry, machinery, electricity, military industry and the like. The zinc blende in China is rich in resources, but generally has the characteristics of less rich ores, more low-grade ores, more associated elements, complex ore properties and the like. By 2015, the zinc resource reserves which have been proved in China are 4103 ten thousand tons, and the zinc resource reserves are second to Australia and second in the world. Along with the rapid development of Chinese economy, the demand of China for zinc resources is increasing day by day, and industrial products taking lead and zinc as raw materials are widely applied to various fields of national economy. The sphalerite is usually associated with galena, and most of lead-zinc ores in China have low lead and high zinc, and lead and zinc are difficult to separate due to the characteristic of low lead and high zinc. Under the condition that high-grade sphalerite which is easy to select and is easy to select is exhausted in China, the development and utilization of lead-zinc ore which is difficult to select has important significance for relieving the pressure of resource shortage. In recent years, with the continuous and deep research, the lead-zinc flotation separation technology has made great progress, but still has great development space.
The method currently most used in the field of lead-zinc flotation separation is the suppression of sphalerite flotation galena, and sphalerite suppressants include inorganic suppressants such as cyanides (sodium cyanide, potassium cyanide, etc.), sulfites and thiosulfates (sodium sulfide, sodium hydrosulfide, sodium thiosulfate, etc.), and other organic suppressants such as azo compounds and sodium thioglycolate, etc. Cyanide has the characteristic of strong inhibition capacity on sphalerite, but because of the defects of high toxicity, great environmental pollution and dissolution of noble metals associated with gold and silver in the lead-zinc ore, the cyanide is basically abandoned at present. Sulfuric acid and sulfite are used to inhibit sphalerite by adding sulfur dioxide, sulfurous acid, sodium sulfite, sodium bisulfite, sodium thiosulfate, etc., and are generally used in combination with zinc sulfate. Sulfites and thiosulfates, at pH 4.5 to 6, have a strong inhibitory effect on zincblende, but the pH range of application is too small and sulfites are prone to oxidative failure. Many azo compounds are carcinogenic, and some azo compounds are not carcinogenic, but have similar toxicity to nitro compounds and aromatic amines. Thioglycolic acid is highly corrosive and has a strong pungent odor. The above-mentioned agents have problems of poor selectivity, environmental pollution, etc. Therefore, the zinc blende inhibitor is used as the key for the high-efficiency separation of lead and zinc flotation, and the development of the novel zinc blende inhibitor which is high-efficiency, non-toxic, low in cost and environment-friendly has very important economic value for the separation of lead and zinc sulfide ores.
In the aspect of medicament synthesis, Chinese patent CN111715410A discloses 'a combined inhibitor of zinc sulfide ore and application thereof', and the method utilizes water-soluble micromolecule carboxylic acid PESA and conventional inhibitor Na2SO3And ZnSO4The sphalerite inhibitor is prepared according to a certain mass ratio. Chinese patent CN110216017A reports "a combined inhibitor for improving the production index of wurtzite and application thereof", and the method prepares a wurtzite combined inhibitor consisting of calcium chloride, polyamine, sodium metabisulfite and sodium humate. The synthesis process is complex, wherein the sodium metabisulfite has strong SO2Odor, SO evolution on contact with strong acids2Corresponding salts are formed, and SO is decomposed at a temperature higher than 150 DEG C2And the environment is polluted. Chinese patent CN104437881A discloses a method for preparing a zincite inhibitor, which comprises the steps of preparing a solution with the mass percentage concentration of 30-35% by adding water into bark and sodium carbonate, standing, heating, stewing, mixing with sodium humate, adding water to prepare a solution, stirring the solution for 2-3h, and evaporating at 65-75 ℃ to obtain the zincite inhibitor. The method has complex synthesis process, increases the cost of preparing the medicament, and is difficult to use on a large scale. Chinese patent CN103909020A discloses a flotation separation inhibitor and a separation method for galena, pyrite and blende, which takes raw ore of lead-zinc sulphide ore as raw material, and adds SDSN (dimethyl dithiocarbamate: 2-methyl thioethylamine = 1-3: 1) as an inhibitor for blende and pyrite. Wherein, the dimethyl dithiocarbamate has stimulating effect on eyes, respiratory tract and skin, which is not suitable for large-scale popularization and application.
Disclosure of Invention
In view of the above disadvantages, the present invention aims to provide an inhibitor having a good inhibitory effect on sphalerite in lead-zinc sulfide ore, which has the advantages of strong selectivity, good inhibitory effect, low toxicity and no pollution.
The invention provides a lead-zinc sulfide ore flotation separation inhibitor which is 2-hydroxyphosphonoacetic acid.
The inhibitor provided by the application is an aqueous solution of 2-hydroxyphosphonoacetic acid, is mainly used as a metal cathode corrosion inhibitor, is widely applied to corrosion and scale inhibition of circulating cooling water systems in the industries of electric power, steel, medicine, petrifaction and the like, and is suitable for corrosion inhibitors. The inhibitor has the advantages of simple preparation, good chemical stability, difficult hydrolysis, difficult damage by acid and alkali, safe and reliable use and low cost.
The application of the flotation separation inhibitor for the lead-zinc sulfide ore is characterized in that: the inhibitor is used as an inhibitor of sphalerite and is used for flotation separation of sphalerite and galena.
The application also provides an application method of the flotation separation inhibitor for the lead-zinc sulfide ore, which comprises the following steps:
s1: adding water into lead-zinc sulfide minerals to obtain ore pulp;
s2: adding 2-hydroxyphosphonoacetic acid into the pulp;
s3: adjusting the pH value of the ore pulp;
s4: and (4) performing air flotation to obtain a foam product and tailings.
Further, the pH adjustment range in S3 is 4-12.
Further, a collector is added in the step S3.
Further, the collecting agent is at least one of xanthate, black powder, diesel oil, kerosene and hydrocarbon oil.
Further, a foaming agent is added to the S3.
Further, the concentration of 2-hydroxyphosphonoacetic acid added to S2 is 1-1000 mg/L.
Further, the lead-zinc sulfide minerals are mixed ores of sphalerite and galena.
In the application, the zinc blende inhibitor belongs to a small molecular organic matter, and the molecular result of the zinc blende inhibitor has phosphono, hydroxyl and carboxyl. The phosphonyl in the inhibitor molecule is easy to complex with zinc ions on the surface of the zinc blende, and simultaneously, the hydrophilic groups of hydroxyl and carboxyl are exposed in an aqueous solution, so that the mineral surface is inhibited from being hydrophilic, and the zinc blende is inhibited.
The invention has the beneficial effects that:
1) the inhibitor provided by the invention is simple to prepare, is environment-friendly and cannot generate pollution.
2) The inhibitor provided by the invention has the advantages of good solubility, strong selectivity, good inhibition effect, wide applicable pH range, small dosage, low price and easiness in large-scale popularization.
3) The separation effect and the separation cost of the inhibitor provided by the invention are obviously superior to those of the traditional zinc blende inhibitors such as sodium sulfide, sodium thiosulfate, sodium hydrosulfide, cyanide, sodium thioglycollate and the like in the prior art.
4) The inhibitor provided by the invention is low in dosage, environment-friendly, safe to add and safe to use.
5) The inhibitor has excellent inhibiting effect on sphalerite. The flotation separation method can be applied to flotation separation of lead-zinc bulk concentrates, and can realize high-efficiency flotation separation of sphalerite and galena.
Drawings
FIG. 1 is a system and flow chart of flotation reagents;
FIG. 2 is a graph of inhibitor concentration versus rate of ascent for example 1 of the present invention;
figure 3 is a graph of the pH value of the ore pulp and the flotation rate of the embodiment 2 of the invention.
Detailed Description
The present invention will be described in further detail with reference to examples, which are not intended to limit the technical scope of the present invention. The invention can be used for other purposes by anyone skilled in the art within the technical scope of the invention disclosure, and the relevant changes of raw materials, process conditions and the like can be properly realized by taking the technical content into consideration, and the invention can not depart from the technical content, and all similar substitutes and modifications which are obvious to those skilled in the art are deemed to be included in the technical scope of the invention.
In order to better explain the invention, the following text further illustrates the main content of the invention in connection with specific laboratory examples, but the content of the invention is not limited to the following examples only.
Example 1
2g of galena and sphalerite single mineral with the granularity of +38-74 mu m are respectively subjected to flotation, 50mL of distilled water is added into a 70mL tank-hanging flotation machine, and stirring and pulp mixing are carried out at the rotating speed of 1300r/min, so that the ore pulp is fully dispersed.
Adjusting the pH value of the ore pulp to 9 after adding the inhibitor, adding the medicament according to the medicament system described in figure 1, and stirring for 5min, 2min and 1min after adding the medicament, wherein the concentration of the type inhibitor is 0, 30, 50, 100, 200, 300, 400, 700 and 1000mg/L respectively. And (4) aerating and floating after stirring to obtain a foam product and tailings.
And respectively filtering, drying and weighing the foam product and the tailings, and calculating the floating rate, wherein the result is shown in figure 2.
The examples show that the inhibitor has weak inhibiting effect on galena, strong inhibiting effect on sphalerite, good selectivity and very low dosage.
Example 2
2g of galena and sphalerite single mineral with the granularity of 38-74 mu m are respectively floated, 50mL of distilled water is added into a 70mL tank-hanging flotation machine, and stirring and size mixing are carried out at the rotating speed of 1300r/min, so that the ore pulp is fully dispersed.
After the inhibitor is added, the pH value of the ore pulp of galena and the pH value of the ore pulp of sphalerite are adjusted to be 4, 6, 8, 9, 10 and 12, the adding sequence of the medicament is shown in figure 1, the inhibitor (100 mg/L), the butyl xanthate (20 mg/L) and the MIBC (20 mg/L) are added, and the medicament is sequentially stirred for 5min, 2min and 1min after being added. And (4) aerating and floating after stirring to obtain a foam product and tailings.
The foam product and the tailings were filtered, dried, weighed, and the flotation rate was calculated, the results are shown in fig. 3.
The examples show that the inhibitor has extremely low inhibitory effect on galena in the pH range of 6-12, the upward floating rate of the galena is as high as 90 percent, and the upward floating rate of the sphalerite is only 15 percent, which shows that the inhibitor has almost no inhibitory effect on the galena, has good inhibitory effect on the sphalerite and has wide applicable pH range.
Example 3
Taking 1.0g of galena and sphalerite single minerals with the particle size of between 38 and 74 mu m according to the weight ratio of 1: 1 proportion, adding 50mL of distilled water into a 70mL tank-hanging flotation machine, stirring and mixing pulp at the rotating speed of 1300r/min, and fully dispersing the pulp.
The adding sequence of the agents is shown in figure 1, after the inhibitor is added, the pH value of the ore pulp is adjusted to be 6, the inhibitor (700 mg/L), the butyl xanthate (20 mg/L) and the MIBC (20 mg/L) are added, and the agents are sequentially stirred for 5min, 2min and 1 min. And (4) aerating and floating after stirring to obtain a foam product and tailings.
And respectively filtering, drying and weighing the foam product and the tailings, calculating the floating rate, testing the grades of ZnS and PbS in the concentrate and calculating the recovery rates of ZnS and PbS. The results are shown in Table 1.
According to the embodiment, the inhibitor can realize the effective flotation separation of galena and sphalerite under the condition of 700mg/L, the galena recovery rate is up to 78.43%, and the sphalerite recovery rate is only 11.82%.
Example 4
Taking 1.0g of galena and sphalerite single minerals with the particle size of between 38 and 74 mu m according to the weight ratio of 1: 1 proportion, adding 50mL of distilled water into a 70mL tank-hanging flotation machine, stirring and mixing pulp at the rotating speed of 1300r/min, and fully dispersing the pulp.
The adding sequence of the agents is shown in figure 1, after the inhibitor is added, the pH value of the ore pulp is adjusted to be 8, the inhibitor (500 mg/L), the butyl xanthate (20 mg/L) and the MIBC (20 mg/L) are added, and the agents are sequentially stirred for 5min, 2min and 1 min. And (4) aerating and floating after stirring to obtain a foam product and tailings.
And respectively filtering, drying and weighing the foam product and the tailings, calculating the floating rate, testing the grades of ZnS and PbS in the concentrate and calculating the recovery rates of ZnS and PbS. The results are shown in Table 1.
According to the embodiment, the inhibitor can realize effective flotation separation of galena and sphalerite under the condition of 500mg/L, the galena recovery rate is up to 80.07%, and the sphalerite recovery rate is only 12.80%.
Example 5
Taking 1.0g of galena and sphalerite single minerals with the particle size of between 38 and 74 mu m according to the weight ratio of 1: 1 proportion, adding 50mL of distilled water into a 70mL tank-hanging flotation machine, stirring and mixing pulp at the rotating speed of 1300r/min, and fully dispersing the pulp.
The adding sequence of the agents is shown in figure 1, after the inhibitor is added, the pH value of the ore pulp is adjusted to 10, the inhibitor (200 mg/L), the butyl xanthate (20 mg/L) and the MIBC (20 mg/L) are added, and the agents are sequentially stirred for 5min, 2min and 1 min. And (4) aerating and floating after stirring to obtain a foam product and tailings.
And respectively filtering, drying and weighing the foam product and the tailings, calculating the floating rate, testing the grades of ZnS and PbS in the concentrate and calculating the recovery rates of ZnS and PbS. The results are shown in Table 1.
According to the embodiment, the inhibitor can realize the effective flotation separation of galena and sphalerite under the condition of 200mg/L, the galena recovery rate is up to 82.81%, and the sphalerite recovery rate is only 15.47%.
Example 6
Taking 1.0g of galena and sphalerite single minerals with the particle size of between 38 and 74 mu m according to the weight ratio of 1: 1 proportion, adding 50mL of distilled water into a 70mL tank-hanging flotation machine, stirring and mixing pulp at the rotating speed of 1300r/min, and fully dispersing the pulp.
The adding sequence of the agents is shown in figure 1, after the inhibitor is added, the pH value of the ore pulp is adjusted to be 12, the inhibitor (25 mg/L), the butyl xanthate (20 mg/L) and the MIBC (20 mg/L) are added, and the agents are sequentially stirred for 5min, 2min and 1 min. And (4) aerating and floating after stirring to obtain a foam product and tailings.
And respectively filtering, drying and weighing the foam product and the tailings, calculating the floating rate, testing the grades of ZnS and PbS in the concentrate and calculating the recovery rates of ZnS and PbS. The results are shown in Table 1.
According to the embodiment, the inhibitor can realize effective flotation separation of galena and sphalerite under the condition of 25mg/L, the galena recovery rate is up to 88.51%, and the sphalerite recovery rate is only 21.55%.
The embodiments of the present invention have been described above by way of example, but the description is only a preferred embodiment of the present invention and should not be construed as limiting the scope of the invention. All equivalent changes and modifications within the scope of the application of the present invention shall fall within the scope of the patent of the present invention.
Claims (7)
1. The application of the flotation separation inhibitor for the lead-zinc sulfide ore is characterized in that: 2-hydroxyphosphonoacetic acid is used as an inhibitor of sphalerite and is used for flotation separation of sphalerite and galena.
2. An application method of a lead-zinc sulfide ore flotation separation inhibitor is characterized by comprising the following steps:
s1: adding water into lead-zinc sulfide minerals to obtain ore pulp;
s2: adding 2-hydroxyphosphonoacetic acid into the ore pulp to be used as an inhibitor of the zinc blende for flotation separation of the zinc blende and galena;
s3: adjusting the pH value of the ore pulp;
s4: and (4) performing air flotation to obtain a foam product and tailings.
3. The method for applying the inhibitor for the flotation separation of lead-zinc sulfide ore according to claim 2, wherein the method comprises the following steps: the pH adjustment range in S3 is 4-12.
4. The method for applying the inhibitor for the flotation separation of lead-zinc sulfide ore according to claim 2, wherein the method comprises the following steps: a collector is also added in S3.
5. The method for applying the inhibitor for the flotation separation of lead-zinc sulfide ore according to claim 4, wherein the method comprises the following steps: the collecting agent is at least one of xanthate, black powder, diesel oil, kerosene and hydrocarbon oil.
6. The method for applying the inhibitor for the flotation separation of lead-zinc sulfide ore according to claim 2, wherein the method comprises the following steps: foaming agent is also added in S3.
7. The method for applying the inhibitor for the flotation separation of lead-zinc sulfide ore according to claim 2, wherein the method comprises the following steps: the concentration of 2-hydroxyphosphonoacetic acid added to S2 is 1-1000 mg/L.
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