CN115025887B - Molybdenum-lead separation inhibitor and preparation method and application thereof - Google Patents
Molybdenum-lead separation inhibitor and preparation method and application thereof Download PDFInfo
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- CN115025887B CN115025887B CN202210728114.2A CN202210728114A CN115025887B CN 115025887 B CN115025887 B CN 115025887B CN 202210728114 A CN202210728114 A CN 202210728114A CN 115025887 B CN115025887 B CN 115025887B
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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
- B03D1/018—Mixtures of inorganic and organic compounds
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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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- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention relates to the technical field of flotation separation, in particular to a molybdenum-lead separation inhibitor and a preparation method and application thereof. The molybdenum-lead separation inhibitor of the present invention comprises at least one of the compounds having the structure shown below:wherein R is 1 、R 2 Each independently selected from any one of hydrogen, halogen, hydroxy, carboxyl, amino, and mercapto; x is any one of O, NH and S. The molybdenum-lead separation inhibitor has the advantages of strong selectivity, good inhibition effect, small dosage, low toxicity and the like; the method is used for molybdenum-lead flotation separation, and can improve the recovery rate and grade of molybdenum concentrate.
Description
Technical Field
The invention relates to the technical field of flotation separation, in particular to a molybdenum-lead separation inhibitor and a preparation method and application thereof.
Background
Molybdenum has the excellent characteristics of high melting point, high temperature resistance, good thermosetting property and the like, so that the molybdenum has wide application in various fields of steel, machinery, electronics, chemical industry, weapons, aerospace, nuclear industry and the like, is an important nonferrous metal resource, and has an extremely important effect on national economy of China. Molybdenum resources are generally obtained from molybdenite in nature by flotation. Molybdenum mines are more or less associated with galena, both molybdenite and galena have good floatability characteristics, so that lead is unavoidable in molybdenum concentrates. The industrial molybdenum oxide used for steelmaking contains less than 0.050 percent of lead, molybdenum oxide with high lead content is difficult to export, and galena in molybdenum concentrate is extremely easy to form insoluble lead molybdate in the roasting process of a rotary kiln, so that the phenomenon of high insoluble molybdenum in the roasted molybdenum oxide, serious kiln sticking, ring forming and the like is caused, the recovery rate of molybdenum is influenced, the service life of the rotary kiln is also influenced, and lead can be converted into toxic gases such as yellow lead, lead and the like at the high temperature of steelmaking, thereby not only polluting the ecological environment, but also affecting the health of human bodies. Therefore, the lead content of the molybdenum concentrate is not allowed to be too high, either from production requirements or environmental requirements.
At present, the separation of molybdenite and galena is difficult to realize by common lead inhibitors. The existing molybdenum-lead separation inhibitor dichromate and phosphonosus have better effect, but the two medicaments are extremely toxic products, so that the cost is high, the dosage is large, the reserve is large, a large amount of unpleasant hydrogen sulfide gas can be released in the use process, nausea, vomiting and dyspnea can be caused after inhalation, and the suffocation can be caused until death, thus having great influence on the health of workers.
In view of this, the present invention has been made.
Disclosure of Invention
The first object of the present invention is to provide a molybdenum-lead separation inhibitor, which solves the problem of poor molybdenum-lead separation effect in the prior art in whole or in part, and has the advantages of strong selectivity, good inhibition effect, low dosage, low toxicity and the like.
The second aim of the invention is to provide a preparation method of the molybdenum-lead separation inhibitor, which is simple and convenient to operate, wide in raw material source, stable in product quality and suitable for large-scale industrial production.
The third object of the invention is to provide a molybdenum-lead flotation separation method, which comprises the steps of using the molybdenum-lead separation inhibitor, so that the recovery rate and grade of molybdenum concentrate can be improved, the grade of lead in the molybdenum concentrate can be reduced, and the comprehensive utilization rate of ore resources can be improved.
In order to achieve the above object of the present invention, the following technical solutions are specifically adopted:
the invention provides a molybdenum-lead separation inhibitor, which comprises at least one of compounds with the following structures:
wherein R is 1 、R 2 Each independently selected from any one of hydrogen, halogen, hydroxy, carboxyl, amino, and mercapto;
x is any one of O, NH and S.
The invention also provides a preparation method of the molybdenum-lead separation inhibitor, which comprises the following steps: the sulfhydryl compound and the glyoxylic acid react in an organic solvent to obtain a molybdenum-lead separation inhibitor;
the structural formula of the sulfhydryl compound is as follows:
the invention also provides a molybdenum-lead flotation separation method, which comprises the use of the molybdenum-lead separation inhibitor.
Compared with the prior art, the invention has the beneficial effects that:
the molybdenum-lead separation inhibitor provided by the invention can be selectively adsorbed on the surface of galena, so that the hydrophilicity of the surface of the galena is increased, and the difference of the hydrophilicity and hydrophobicity of the surface of molybdenite and the surface of the galena is increased, thereby realizing the effective separation of molybdenum and lead. The molybdenum-lead separation inhibitor has the advantages of strong selectivity and good inhibition effect, has the characteristics of good stability, wide application range, small dosage, environmental protection, low toxicity, safe use and the like, and can be widely applied to the field of mineral flotation. Particularly, the molybdenum-lead separation inhibitor is used for molybdenum-lead flotation, so that the grade and recovery rate of molybdenum concentrate can be remarkably improved, the grade of lead in the molybdenum concentrate is reduced, and the comprehensive utilization rate of resources in mineral products is improved.
Detailed Description
The technical solution of the present invention will be clearly and completely described in conjunction with the specific embodiments, but it will be understood by those skilled in the art that the examples described below are some, but not all, examples of the present invention, and are intended to be illustrative only and should not be construed as limiting the scope of the present invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The molybdenum-lead separation inhibitor, the preparation method and the application thereof are specifically described below.
In some embodiments of the invention there is provided a molybdenum lead separation inhibitor comprising at least one of the compounds having the structure shown below:
wherein R is 1 、R 2 Each independently selected from any one of hydrogen, halogen, hydroxy, carboxyl, amino, and mercapto;
x is any one of O, NH and S.
The front line track shape of the metal sites on the surface of the molybdenite is different from the front line track shape of the metal sites on the surface of the galena, and the front line track shape of the molybdenum-lead separation inhibitor with the structure can be matched with the front line track shape of the metal sites on the surface of the galena, so that the maximum overlapping can be achieved, and therefore, the current separation inhibitor with the structure can be selectively adsorbed on the surface of the galena; hydrophilic groups in the molybdenum-lead separation inhibitor can increase the hydrophilicity of the galena surface; thereby increasing the difference of the surface hydrophilicity and hydrophobicity of the molybdenite and galena and realizing the effective separation of molybdenum and lead. The molybdenum-lead separation inhibitor has the advantages of strong inhibition capability, good selectivity and the like. The method is used in the flotation process of molybdenum ore, and can improve the grade and recovery rate of molybdenum concentrate, reduce the grade of lead in molybdenum concentrate and improve the comprehensive utilization rate of resources in mineral products.
The molybdenum-lead separation inhibitor with the structure provided by the invention also has the characteristics of good stability, low toxicity, safer use and the like, can be widely used in the flotation process of minerals, and does not cause harm to human bodies and the environment.
In some embodiments of the invention, the molybdenum lead separation inhibitor comprises at least one of the compounds having a structure as shown in formulas (I) through (IV);
in some embodiments of the present invention, the molybdenum-lead separation inhibitor may be any one of compounds having a structure as shown in formulas (I) to (IV) or a combination of two or more thereof.
In some embodiments of the present invention, there is also provided a method for preparing the above molybdenum-lead separation inhibitor, including: the sulfhydryl compound and the glyoxylic acid react in an organic solvent to obtain a molybdenum-lead separation inhibitor;
the structural formula of the sulfhydryl compound is as follows:
in some embodiments of the invention, the thiol compound is any one of 1, 2-ethanedithiol, beta-mercaptoethylamine, beta-mercaptoethanol, and cysteine.
In some embodiments of the invention, the molar ratio of thiol compound to glyoxylic acid is 1:1.1 to 2; typically, but not by way of limitation, the molar ratio of thiol compound to glyoxylic acid is 1:1.1, 1:1.2, 1:1.3, 1:1.4, 1:1.5, 1:1.6, 1:1.7, 1:1.8, 1:1.9 or 1:2, etc.
In some embodiments of the invention, the volume molar ratio of organic solvent to mercapto compound is from 2 to 50mL/mmol; typical but non-limiting, for example, the volume molar ratio of organic solvent to mercapto compound is 2mL/mmol, 10mL/mmol, 20mL/mmol, 30mL/mmol, 40mL/mmol, or 50mL/mmol, etc.
In some embodiments of the invention, the organic solvent comprises a mass ratio of 1: 5-5: 1 alcohol and pyridine; typically, but not by way of limitation, the mass ratio of alcohol to pyridine is 1: 5. 2: 5. 3: 5. 4: 5. 1:1. 2:1. 3: 1. 3: 2. 4: 1. 4: 3. 4:5 or 5:1, etc.
In some embodiments of the invention, the alcohol comprises any one or more of a C1-C10 saturated alcohol and/or a C1-C10 unsaturated alcohol.
In some embodiments of the invention, the alcohol comprises one or more of methanol, ethanol, propanol, isopropanol, n-butanol, sec-butanol, tert-butanol, n-pentanol, iso-pentanol, tert-pentanol, and hexanol.
In some embodiments of the invention, the organic solvent includes ethanol and pyridine.
In some embodiments of the invention, the temperature of the reaction is from 5 to 80 ℃; the reaction time is 1-72 h; typical, but not limiting, temperatures of the reaction are, for example, 5 ℃, 10 ℃, 15 ℃, 20 ℃, 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃, or 80 ℃, etc.; typical, but not limiting, times for the reaction are, for example, 5h, 10h, 15h, 20h, 25h, 30h, 35h, 40h, 45h, 50h, 55h, 60h, 65h or 70h, etc.
The preparation method of the molybdenum-lead separation inhibitor provided by the invention is simple to operate, wide in preparation raw material sources, mild in reaction conditions, stable in product quality, high in product yield and suitable for large-scale industrial production.
In some embodiments of the invention, a molybdenum-lead flotation separation process is also provided, including the use of the molybdenum-lead separation inhibitor described above.
The molybdenum-lead separation inhibitor provided by the invention has the advantages of good selectivity, strong inhibition capability and the like, can effectively replace conventional medicaments such as phosphonomus and the like in the molybdenum ore flotation process, and can realize the high-efficiency flotation separation of molybdenite and galena.
In some embodiments of the invention, the molybdenum-lead flotation separation process described above includes adding a molybdenum-lead separation inhibitor to the molybdenum raw concentrate.
In some embodiments of the invention, the molybdenum content in the molybdenum concentrate is 10wt% to 20wt% and the lead content is 0.24wt% to 1.00wt%.
In some embodiments of the invention, the molybdenum rough concentrate is a molybdenum rough concentrate pulp, and the mass percentage of the molybdenum rough concentrate in the pulp is 10% -40%.
In some embodiments of the invention, the pulp has a pH of 6 to 10.
In some embodiments of the invention, the mass ratio of the molybdenum-lead separation inhibitor to the pulp is 0.0008 to 0.0012, based on the mass of solids: 1.
the features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
The preparation method of the molybdenum-lead separation inhibitor provided by the embodiment comprises the following steps:
25mmol of 1, 2-ethanedithiol was dissolved in 100mL of a mass ratio of 3:2, 28mmol of glyoxylic acid is added thereto at 20 ℃ in a mixed solvent of ethanol and pyridine, stirred for 2 hours, and then an off-white precipitate is separated by filtration, washed with ethanol, and finally white powder YZJ-01 is obtained.
Example 2
The preparation method of the molybdenum-lead separation inhibitor provided by the embodiment comprises the following steps:
25mmol of beta-mercaptoethylamine was dissolved in 100mL of a mass ratio of 5:2, 28mmol of glyoxylic acid is added thereto at 20 ℃ in a mixed solvent of ethanol and pyridine, stirred for 12 hours, and then an off-white precipitate is separated by filtration, washed with ethanol, and finally white powder YZJ-02 is obtained.
Example 3
The preparation method of the molybdenum-lead separation inhibitor provided by the embodiment comprises the following steps:
25mmol of beta-mercaptoethanol was dissolved in 100mL of a mass ratio of 5:2, 28mmol of glyoxylic acid is added thereto at 20 ℃ in a mixed solvent of ethanol and pyridine, stirred for 12 hours, and then an off-white precipitate is separated by filtration, washed with ethanol, and finally white powder YZJ-03 is obtained.
Example 4
The preparation method of the molybdenum-lead separation inhibitor provided by the embodiment comprises the following steps:
50mmol of 1, 2-ethanedithiol was dissolved in 100mL of a mass ratio of 5:2, 62mmol of glyoxylic acid is added thereto at 20 ℃ in a mixed solvent of ethanol and pyridine, stirred for 18 hours, and then an off-white precipitate is separated by filtration, washed with ethanol, and finally white powder YZJ-04 is obtained.
Example 5
The preparation method of the molybdenum-lead separation inhibitor provided by the embodiment comprises the following steps:
5mmol of 1, 2-ethanedithiol was dissolved in 100mL of a mass ratio of 5:2, 6mmol of glyoxylic acid is added thereto at 20 ℃ in a mixed solvent of ethanol and pyridine, stirred for 70 hours, and then an off-white precipitate is separated by filtration, washed with ethanol, and finally white powder YZJ-05 is obtained.
Example 6
The preparation method of the molybdenum-lead separation inhibitor provided by the embodiment comprises the following steps:
25mmol of 1, 2-ethanedithiol was dissolved in 100mL of a mass ratio of 1:5, 28mmol of glyoxylic acid is added to the mixed solvent of ethanol and pyridine at 20 ℃ and stirred for 15 hours, and then an off-white precipitate is separated by filtration and washed with ethanol, finally obtaining white powder YZJ-06.
Example 7
The preparation method of the molybdenum-lead separation inhibitor provided by the embodiment comprises the following steps:
25mmol of 1, 2-ethanedithiol was dissolved in 100mL of a mass ratio of 5:2, 28mmol of glyoxylic acid is added thereto at 5 ℃ and stirred for 48 hours, and then the off-white precipitate is separated by filtration and washed with ethanol, finally obtaining white powder YZJ-07.
Example 8
The preparation method of the molybdenum-lead separation inhibitor provided by the embodiment comprises the following steps:
25mmol of 1, 2-ethanedithiol was dissolved in 100mL of a mass ratio of 5:2, 28mmol of glyoxylic acid is added thereto at 80 ℃ in a mixed solvent of ethanol and pyridine, stirred for 1h, and then an off-white precipitate is separated by filtration, washed with ethanol, and finally white powder YZJ-08 is obtained.
Example 9
The preparation method of the molybdenum-lead separation inhibitor provided by the embodiment comprises the following steps:
25mmol of cysteine was dissolved in 100mL of a mass ratio of 5:2, 28mmol of glyoxylic acid is added thereto at 80 ℃ in a mixed solvent of ethanol and pyridine, stirred for 1h, and then an off-white precipitate is separated by filtration, washed with ethanol, and finally white powder YZJ-09 is obtained.
Comparative example 1
The molybdenum-lead separation inhibitor provided in this comparative example is sodium thioglycolate, and is commercially available. The manufacturer is Allatin with the content of 95 percent.
Comparative example 2
The molybdenum-lead separation inhibitor provided in this comparative example is fosinox, and the fosinox configuration method is as follows:
8g of NaOH is dissolved in 92g of water to obtain 8% NaOH aqueous solution; take 5.7g P 2 S 5 Dissolving in the 8% NaOH aqueous solution to obtain 105.7g of P with the mass percentage of 5.39% 2 S 5 A solution; the mass percentage of the P is 5.39% of 105.7g 2 S 5 402g of water was added to the solution to obtain 1.07% by mass of P 2 S 5 An aqueous solution.
Test example 1
The molybdenum-lead separation inhibitors of examples 1-8 and comparative examples 1-2 were used to perform experiments of upgrading and reducing impurity molybdenum on molybdenum rough concentrate, wherein the molybdenum rough concentrate mainly contains 14.59wt% of molybdenum and the lead content is 0.56wt%. Under the condition that ore grains with the fineness of less than 0.074mm account for 60 percent and the content of molybdenum rough concentrate in ore pulp is 20wt%, 10 parts of 250g of molybdenum rough concentrate ore pulp is taken, molybdenum-lead separation inhibitors YZJ-01, YZJ-02, YZJ-03, YZJ-04, YZJ-05, YZJ-06, YZJ-07, YZJ-08, sodium thioglycolate and phosphoxk are respectively added into each part of ore pulp for flotation performance comparison, the dosage of each inhibitor relative to the molybdenum rough concentrate is 1000g/t, and the obtained flotation results are shown in table 1.
TABLE 1
| Inhibitor species | Molybdenum grade/% | Molybdenum recovery/% | Lead grade/% |
| YZJ-01 | 30.10 | 98.15 | 0.27 |
| YZJ-02 | 30.29 | 98.42 | 0.23 |
| YZJ-03 | 30.14 | 98.28 | 0.32 |
| YZJ-04 | 31.33 | 98.58 | 0.30 |
| YZJ-05 | 29.93 | 99.00 | 0.22 |
| YZJ-06 | 31.08 | 97.47 | 0.30 |
| YZJ-07 | 30.53 | 97.89 | 0.28 |
| YZJ-08 | 30.46 | 98.55 | 0.26 |
| Sodium thioglycolate | 26.72 | 98.49 | 0.48 |
| Phosphonox | 28.56 | 96.74 | 0.39 |
As can be seen from the results in table 1, the molybdenum-lead separation inhibitors of examples 1 to 8 of the present invention have good effects in the molybdenum-lead flotation separation process, compared to the use of the conventional molybdenum-lead separation inhibitors sodium thioglycolate and fenox. The content of lead is obviously reduced in the flotation process, the grade of lead in concentrate obtained by roughing can be as low as 0.22%, and the recovery rate of molybdenum is as high as 99.00%. Therefore, the lead inhibitor provided by the invention has the advantages of good selectivity and strong inhibition capability, can effectively replace conventional medicaments such as phosphoxwell and the like in the molybdenum ore flotation process, and is widely applied to the sulfide ore flotation separation process, so that the comprehensive utilization rate of ore resources is improved.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.
Claims (10)
1. A molybdenum lead separation inhibitor comprising at least one of the compounds having the structure shown below:
wherein R is 1 、R 2 Each independently selected from any one of hydrogen, halogen, hydroxy, carboxyl, amino, and mercapto;
x is any one of O, NH and S.
2. The molybdenum-lead separation inhibitor according to claim 1, characterized by comprising at least one of compounds having a structure represented by the formulas (I) to (IV);
3. the method for producing a molybdenum-lead separation inhibitor according to claim 1 or 2, comprising: the sulfhydryl compound and the glyoxylic acid react in an organic solvent to obtain a molybdenum-lead separation inhibitor;
the structural formula of the sulfhydryl compound is as follows:
4. the method for producing a molybdenum-lead separation inhibitor according to claim 3, wherein the mercapto compound is any one of 1, 2-ethanedithiol, β -mercaptoethylamine, β -mercaptoethanol, and cysteine.
5. The method for producing a molybdenum-lead separation inhibitor according to claim 4, wherein the molar ratio of the mercapto compound to the glyoxylic acid is 1:1.1 to 2.
6. The method for producing a molybdenum-lead separation inhibitor according to claim 4, wherein the volume molar ratio of the organic solvent to the mercapto compound is 2 to 50mL/mmol.
7. The method for producing a molybdenum-lead separation inhibitor according to claim 4, wherein the organic solvent comprises a mixture of components in a mass ratio of 1: 5-5: 1 alcohol and pyridine.
8. The method for producing a molybdenum-lead separation inhibitor according to claim 7, wherein the alcohol comprises any one or more of a C1 to C10 saturated alcohol and/or a C1 to C10 unsaturated alcohol.
9. The method for producing a molybdenum-lead separation inhibitor according to claim 4, wherein the temperature of the reaction is 5 to 80 ℃; the reaction time is 1-72 h.
10. A molybdenum-lead flotation separation method, characterized by comprising the molybdenum-lead separation inhibitor prepared by using the molybdenum-lead separation inhibitor according to any one of claims 1 to 3 or the preparation method according to any one of claims 4 to 9.
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