CN110653070A - Multi-metal sulfide ore flotation separation inhibitor and flotation separation method thereof - Google Patents
Multi-metal sulfide ore flotation separation inhibitor and flotation separation method thereof Download PDFInfo
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- CN110653070A CN110653070A CN201910928902.4A CN201910928902A CN110653070A CN 110653070 A CN110653070 A CN 110653070A CN 201910928902 A CN201910928902 A CN 201910928902A CN 110653070 A CN110653070 A CN 110653070A
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- flotation separation
- polymetallic
- molybdenum
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- polymetallic sulphide
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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
- B03D1/01—Organic compounds containing nitrogen
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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
Abstract
The invention discloses a polymetallic sulphide ore flotation separation inhibitor and a flotation separation method thereof. The polymetallic sulfide ore flotation separation inhibitor provided by the invention has the advantages of simple preparation process, mild reaction conditions, safe use, convenient addition, easily obtained raw materials and the like, has the technical advantages of low toxicity, environmental protection, small dosage and good inhibition effect, and can effectively replace the traditional inhibitor. The multi-metal sulfide ore flotation separation inhibitor can effectively inhibit impurity minerals such as galena, chalcopyrite, sphalerite, pyrite, bismuthate and the like, can be widely applied to a flotation separation process of multi-metal sulfide ores such as copper-lead, lead-zinc, molybdenum-lead, molybdenum-sulfur, molybdenum-bismuth, copper-molybdenum, copper-lead-molybdenum and the like, and is beneficial to improving the separation index.
Description
Technical Field
The invention relates to a polymetallic sulphide ore flotation separation inhibitor and a flotation separation method thereof, belonging to the technical field of polymetallic sulphide ore beneficiation.
Background
In the development of national economy, mineral resources play a vital role, and various nonferrous metals such as copper, lead, zinc, molybdenum and the like extracted from the mineral resources make great contribution to the development of national economy, and are widely applied to various fields such as aerospace, electronic science and technology, high-performance materials, national defense science and technology and the like. However, the efficient comprehensive utilization of the refractory multi-metal resources has not been solved, such as the refractory multi-metal resources of copper, lead and zinc, the refractory multi-metal resources of molybdenum, and the like.
Flotation is one of the most common methods used in the processing of mineral resources. In the processing process of copper-lead-zinc refractory multi-metal resources, copper-lead separation is concerned by people. Because of the close floatability of copper and lead, the mixed flotation and re-separation process technology is generally adopted in the industry, which directly causes the difficulty of copper and lead separation. In actual production, two processes of inhibiting copper and lead are adopted, namely the separation of chalcopyrite by cyanide inhibition and the separation of galena by dichromate inhibition are respectively adopted, and although the two substances have high selectivity and good separation effect, the two substances are both extremely toxic substances and seriously damage the ecological environment, so people start to turn to the research, development and application of green and environment-friendly organic inhibitors.
In the processing process of molybdenum refractory polymetallic resources, because molybdenum is usually associated with other sulfide ores and the grade is generally low, the process technology of mixed flotation and re-separation is also adopted in industry, such as copper-molybdenum mixed flotation, copper-molybdenum-lead mixed flotation, molybdenum-sulfur mixed flotation, molybdenum-lead mixed flotation, molybdenum-bismuth mixed flotation and the like. Although molybdenite is excellent in floatability, other impurity sulfide ores also have good floatability, which, if not effectively separated, also affects the quality of the molybdenum concentrate. In industry, inorganic depressants (such as sulfide, hydrosulfate, cyanide, potassium dichromate, phosphorus (arsenic) nocks, and the like) are generally used for flotation separation of molybdenum bulk concentrates, but the inorganic depressants also have the problems of high toxicity, serious environmental pollution and the like. At present, organic inhibitors such as thioglycolate, Orfom D8 and M8 are mostly adopted in industry, and although the organic inhibitors overcome the defects of inorganic inhibitors to some extent, the inhibition effect is relatively poor, the dosage is large, and the use cost is high. Therefore, the development of the green and environment-friendly organic inhibitor has important practical significance.
Disclosure of Invention
In view of the above, the invention aims at the problems of high toxicity, difficult post-treatment and high environmental protection pressure of the existing inorganic inhibitor in the process of flotation separation of polymetallic sulphide ores, simultaneously solves the technical defects of poor ore adaptability, poor inhibition effect, large dosage and the like of the existing organic inhibitor, provides a multi-metal sulfide ore flotation separation inhibitor and a flotation separation method thereof, the obtained multi-metal sulfide ore flotation separation inhibitor not only has the advantages of low toxicity, safe use, convenient addition, easy acquisition of raw materials and the like, but also has stronger inhibiting power to various sulphide ores such as chalcopyrite, galena, pyrite, bismuthate and the like, can well achieve the aim of flotation separation of the polymetallic sulphide ores, the method can be widely applied to the flotation separation process of polymetallic sulfide ores such as copper-lead separation, lead-zinc separation, molybdenum-lead, molybdenum-sulfur, molybdenum-bismuth, copper-molybdenum, copper-lead-molybdenum and the like so as to improve the separation index.
In order to achieve the effect, the invention adopts the following technical scheme:
a polymetallic sulfide ore flotation separation inhibitor is prepared by the following steps:
the method comprises the steps of reacting polymaleic anhydride with an organic compound containing multiple amino groups for 1-24 hours at 0-100 ℃ to obtain an intermediate M, preferably reacting for 2-8 hours at 25-80 ℃, reacting for 2-12 hours at 30-90 ℃ in an alkaline solution by using the intermediate M and carbon disulfide, preferably reacting for 3-8 hours at 30-70 ℃, and obtaining the polymaleic anhydride.
Wherein, the intermediate M is a compound with a structure of formula (I) and/or formula (II),
in the formula (I) and the formula (II), R is C0-C6 alkyl, C2-C8 alkenyl, C2-C8 alkynyl, C6-C10 aryl or C6-C10 substituted aryl, Me is H, Na or K, n is 0-20000, m is 0-20000, n is 0-200001＝0～1000，n2＝1～1000；
The prepared flotation separation inhibitor of the polymetallic sulphide ore is a compound with a structure shown in a formula (III) and/or a formula (IV),
in the formulas (III) and (IV), R is C0-C6 alkyl, C2-C8 alkenyl, C2-C8 alkynyl, C6-C10 aryl or C6-C10 substituted aryl, Me is H, Na or K, n is 0-20000, m is 0-20000, n is 0-200001＝0～1000，n21 to 1000, corresponding to formula (I) and/or formula (II).
According to the technical scheme provided by the invention, the polymetallic sulfide ore flotation separation inhibitor provided by the invention is a nitrogen yellow to reddish brown solution prepared by taking environment-friendly polymaleic anhydride as an initial raw material, grafting an organic compound containing a plurality of amino groups to prepare a corresponding intermediate M, and then reacting the intermediate with carbon disulfide in an alkaline solution; the multi-metal sulphide ore flotation separation inhibitor has a strong inhibiting effect on sulphide ores such as galena, chalcopyrite, sphalerite, pyrite, bismuthate and the like, and can realize the flotation separation of multi-metal sulphide ores under various flotation process conditions.
The multi-metal sulfide ore flotation separation inhibitor provided by the invention has the advantages of simple preparation process, readily available raw materials, safety in use, convenience in addition and the like, has the advantages of small dosage, low toxicity, environmental friendliness and the like compared with the traditional inhibitors such as sulfide, hydrosulfide, cyanide, dichromate, phosphorus (arsenic) nocks, sodium thioglycollate and the like, and can be widely applied to the flotation separation mineral processing process of multi-metal sulfide ores such as copper lead, lead zinc, molybdenum lead, molybdenum sulfur, molybdenum bismuth, copper molybdenum, copper lead molybdenum and the like so as to improve the separation index.
Further, the molar ratio of the carbon disulfide to amino groups in the intermediate M is 1-1.2: 1; the molar ratio of the carbon disulfide to the alkaline compound in the alkaline solution is 1: 1-2.
Further, the molecular weight of the polymaleic anhydride is 100 to 1000000, and preferably 100 to 10000.
The molecular weight of the polymaleic anhydride determines n in the above structural formulas (I), (II), (III) and (IV)1And n2The numerical value of (c).
Further, the organic compound containing a plurality of amino groups is any one or a mixture of more of ethylenediamine, propylenediamine, butylenediamine, hexamethylenediamine, hydrazine hydrate, p-phenylenediamine, diethylenetriamine, triethylenetetramine, tetraethylenepentamine, polyvinylamine and polyethyleneimine;
the alkaline solution is one or more of sodium carbonate, potassium carbonate, sodium hydroxide and potassium hydroxide.
The invention also provides a method for flotation separation of the polymetallic sulphide ore by using the polymetallic sulphide ore flotation separation inhibitor, which comprises the following steps:
the polymetallic sulphide ore flotation separation inhibitor is added in the grinding or flotation process of the polymetallic sulphide ore, and the separation of the polymetallic sulphide ore can be realized through froth flotation, wherein the adding amount of the polymetallic sulphide ore flotation separation inhibitor relative to raw ore is 10-2000 g/t, and the adding amount relative to rough concentrate is 100-15000 g/t, preferably, the adding amount of the polymetallic sulphide ore flotation separation inhibitor relative to raw ore is 200-3000 g/t, and the adding amount relative to rough concentrate is 50-5000 g/t.
The multi-metal sulphide ore flotation separation inhibitor provided by the invention can be used for the flotation separation process of multi-metal sulphide ores such as copper-lead separation, lead-zinc separation, molybdenum-lead, molybdenum-sulfur, molybdenum-bismuth, copper-molybdenum, copper-lead-molybdenum and the like, and preferably, the multi-metal sulphide ores are any one or more of galena, chalcopyrite, sphalerite, pyrite and bismutite.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
In the following examples, the term "one or more" when used in the presence of raw materials or reagents means at least two kinds, and if not specifically stated, any ratio is indicated when the raw materials or reagents are used in several kinds.
Example 1
The polymetallic sulphide ore flotation separation inhibitor is prepared by the following steps:
placing 12.0g of polymaleic anhydride (the content of the maleic anhydride is 0.1mol) into a 100ml three-necked bottle, then adding 40ml of water, fully stirring, adding 0.74g of propane diamine (0.01 mol) at one time, and fully reacting for 3 hours at 30 ℃; then adding 20.0g of sodium hydroxide solution (containing 0.2mol of sodium hydroxide) with the mass concentration of 40%, stirring to fully dissolve the sodium hydroxide solution, gradually heating to 40 ℃, then adding 0.90g of carbon disulfide (0.012mol of carbon disulfide), fully stirring for 2 hours, then heating to 60 ℃, continuing to react for 3 hours, and obtaining light yellow polymetallic sulphide ore flotation separation inhibitor solution with the mass concentration of about 25% after the reaction is finished.
Example 2
The polymetallic sulphide ore flotation separation inhibitor is prepared by the following steps:
placing 12.0g of polymaleic anhydride (the content of the maleic anhydride is 0.1mol) into a 100ml three-necked bottle, then adding 40ml of water, fully stirring, adding 1.03g of diethylenetriamine (0.01 mol) at one time, and fully reacting for 3 hours at 30 ℃; then adding 20.0g of sodium hydroxide solution (containing 0.2mol of sodium hydroxide) with the mass concentration of 40%, stirring to fully dissolve the sodium hydroxide solution, gradually heating to 40 ℃, then adding 0.90g of carbon disulfide (0.012mol of carbon disulfide), fully stirring for 2h, then heating to 60 ℃, continuing to react for 3h, and obtaining the orange to reddish brown polymetallic sulfide ore flotation separation inhibitor solution with the mass concentration of about 25% after the reaction is finished.
Example 3
The method comprises the following steps of taking 2.0g of artificially mixed chalcopyrite and galena pure minerals with the mass ratio of 2:3 as raw mineral materials, carrying out a flotation separation test in an XFG5-35 groove-hanging flotation machine, adding 40ml of water, adjusting the rotation speed of the flotation machine to 1754r/min, adjusting the pH value in a groove to 8-9 by using sodium hydroxide, adding the multi-metal sulfide flotation separation inhibitor prepared in the embodiment 1 of the invention, wherein the using amount of the multi-metal sulfide flotation separation inhibitor is 2mg/L, adopting O-isopropyl-N-ethyl thiocarbamate as a chalcopyrite collecting agent, adopting methyl isobutyl carbinol as a foaming agent, using 10mg/L of the collecting agent and the foaming agent, carrying out flotation for 4min, and carrying out rough separation to obtain the lead concentrate with the copper grade of 28.9%, the lead content of 12.1%, the recovery rate of 93.1%, the lead grade of 80.6%, the copper of 1.5% and the recovery.
Example 4
The mineral raw material is actual copper-molybdenum-lead bulk flotation rough concentrate ore, wherein the molybdenum content is 13.78%, the copper content is 1.92% and the lead content is 0.29%, and phase analysis results show that the molybdenum mineral mainly exists in the form of molybdenite, the copper mineral mainly is chalcopyrite and the lead mineral mainly is galena. The molybdenum rough concentrate is reground, the flotation concentration of the ore pulp is kept to be about 15%, the polymetallic sulfide flotation separation inhibitor (400 g/t of rough concentration, 200g/t of first fine concentration, 100g/t of second fine concentration and 50g/t of third fine concentration), the collector diesel oil (50 g/t of rough concentration) and the foaming agent (20 g/t of rough concentration) prepared in the embodiment 2 are sequentially added, the mixture is fully stirred, and the molybdenum concentrate containing 52.58% of molybdenum, 0.065% of copper and 0.042% of lead can be obtained through one-time rough concentration and seven-time fine concentration.
Therefore, the multi-metal sulfide ore flotation separation inhibitor prepared by the embodiment of the invention has the advantages of low toxicity, safe use, convenient addition, easily obtained raw materials and the like, can be directly used or diluted for use, can also be used alone or mixed with other inhibitors, has strong inhibition on galena, chalcopyrite, pyrite, bismuthate ore, sphalerite and the like, and can well achieve the aim of multi-metal sulfide ore flotation separation, so that the multi-metal sulfide ore flotation separation inhibitor can be widely applied to the multi-metal sulfide ore flotation separation process of copper lead, lead zinc, molybdenum lead, molybdenum sulfur, molybdenum bismuth, copper molybdenum, copper lead molybdenum and the like, and the separation index can be improved.
Claims (7)
1. The polymetallic sulphide ore flotation separation inhibitor is characterized by being prepared by the following steps:
reacting polymaleic anhydride with an organic compound containing a plurality of amino groups for 1-24 hours at 0-100 ℃ to obtain an intermediate M, and reacting the intermediate M with carbon disulfide in an alkaline solution at 30-90 ℃ for 2-12 hours to obtain the polymetallic sulfide ore flotation separation inhibitor;
the intermediate M is a compound with a structure shown in a formula (I) and/or a formula (II),
in the formula (I) and the formula (II), R is C0-C6 alkyl, C2-C8 alkenyl, C2-C8 alkynyl, C6-C10 aryl or C6-C10 substituted aryl, Me is H, Na or K, n is 0-20000, m is 0-20000, n is 0-200001＝0～1000，n2＝1～1000。
2. The polymetallic sulphide ore flotation separation inhibitor according to claim 1, wherein the molar ratio of the carbon disulphide to the amino groups in the intermediate M is 1-1.2: 1;
the molar ratio of the carbon disulfide to the alkaline compound in the alkaline solution is 1: 1-2.
3. The polymetallic sulphide ore flotation separation suppressor of claim 1 or 2 wherein the polymaleic anhydride has a molecular weight of 100 to 1000000.
4. The polymetallic sulphide ore flotation separation inhibitor according to claim 1 or 2, wherein the organic compound containing a plurality of amino groups is any one or a mixture of ethylene diamine, propylene diamine, butylene diamine, hexamethylene diamine, hydrazine hydrate, p-phenylene diamine, diethylene triamine, triethylene tetramine, tetraethylene pentamine, polyethylene amine and polyethylene imine.
5. The polymetallic sulphide ore flotation separation suppressor according to claim 1 or 2, wherein the alkaline solution is an aqueous solution of any one or more of sodium carbonate, potassium carbonate, sodium hydroxide or potassium hydroxide.
6. A method for flotation separation of polymetallic sulphide ore by a polymetallic sulphide ore flotation separation inhibitor is characterized by comprising the following steps:
adding the polymetallic sulphide ore flotation separation inhibitor of any one of claims 1-5 in the grinding or flotation process of the polymetallic sulphide ore, and separating the polymetallic sulphide ore by froth flotation;
the adding amount of the polymetallic sulfide ore flotation separation inhibitor relative to raw ore is 10-2000 g/t, and the adding amount relative to rough concentrate is 100-15000 g/t.
7. The method for flotation separation of the polymetallic sulphide ores according to claim 6, wherein the polymetallic sulphide ores are any one or more of galena, chalcopyrite, sphalerite, pyrite and bismuthate.
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| CN201910928902.4A CN110653070B (en) | 2019-09-28 | 2019-09-28 | Multi-metal sulfide ore flotation separation inhibitor and flotation separation method thereof |
| ZA2020/01411A ZA202001411B (en) | 2019-09-28 | 2020-03-05 | Flotation separation inhibitor of polymetallic sulfide ore and flotation separation method thereof |
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| CN201910928902.4A CN110653070B (en) | 2019-09-28 | 2019-09-28 | Multi-metal sulfide ore flotation separation inhibitor and flotation separation method thereof |
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Cited By (2)
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| CN114950742A (en) * | 2022-06-15 | 2022-08-30 | 矿冶科技集团有限公司 | Galena flotation inhibitor and flotation separation method |
| CN115025887A (en) * | 2022-06-24 | 2022-09-09 | 矿冶科技集团有限公司 | Molybdenum-lead separation inhibitor and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114950742A (en) * | 2022-06-15 | 2022-08-30 | 矿冶科技集团有限公司 | Galena flotation inhibitor and flotation separation method |
| CN114950742B (en) * | 2022-06-15 | 2023-08-04 | 矿冶科技集团有限公司 | Galena flotation inhibitor and flotation separation method |
| CN115025887A (en) * | 2022-06-24 | 2022-09-09 | 矿冶科技集团有限公司 | Molybdenum-lead separation inhibitor and preparation method and application thereof |
| CN115025887B (en) * | 2022-06-24 | 2023-08-04 | 矿冶科技集团有限公司 | Molybdenum-lead separation inhibitor and preparation method and application thereof |
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| Publication number | Publication date |
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| ZA202001411B (en) | 2020-06-24 |
| CN110653070B (en) | 2021-04-02 |
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