CN114226071A - Molybdenite emulsified collector and preparation method thereof - Google Patents
Molybdenite emulsified collector and preparation method thereof Download PDFInfo
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- CN114226071A CN114226071A CN202111456733.2A CN202111456733A CN114226071A CN 114226071 A CN114226071 A CN 114226071A CN 202111456733 A CN202111456733 A CN 202111456733A CN 114226071 A CN114226071 A CN 114226071A
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- 229910052961 molybdenite Inorganic materials 0.000 title claims abstract description 45
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 87
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 63
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000002283 diesel fuel Substances 0.000 claims abstract description 30
- 235000019864 coconut oil Nutrition 0.000 claims abstract description 29
- 239000003240 coconut oil Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 14
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 37
- 238000005406 washing Methods 0.000 claims description 24
- 239000003995 emulsifying agent Substances 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 12
- 238000001914 filtration Methods 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 12
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 12
- 239000002131 composite material Substances 0.000 claims 2
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 abstract description 16
- 229910052750 molybdenum Inorganic materials 0.000 abstract description 16
- 239000011733 molybdenum Substances 0.000 abstract description 16
- 238000011084 recovery Methods 0.000 abstract description 15
- 230000001804 emulsifying effect Effects 0.000 abstract description 13
- 239000003795 chemical substances by application Substances 0.000 abstract description 12
- 239000012141 concentrate Substances 0.000 abstract description 11
- 238000005188 flotation Methods 0.000 abstract description 11
- 239000006185 dispersion Substances 0.000 abstract description 7
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000003921 oil Substances 0.000 description 15
- 235000019198 oils Nutrition 0.000 description 15
- 239000002245 particle Substances 0.000 description 12
- 230000000694 effects Effects 0.000 description 8
- 239000004215 Carbon black (E152) Substances 0.000 description 7
- 229930195733 hydrocarbon Natural products 0.000 description 7
- 150000002430 hydrocarbons Chemical class 0.000 description 7
- 238000009826 distribution Methods 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000839 emulsion Substances 0.000 description 3
- 239000006260 foam Substances 0.000 description 3
- 239000003350 kerosene Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Images
Classifications
-
- 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
-
- 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
- B03D2201/02—Collectors
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Inorganic Chemistry (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
Abstract
The invention relates to a molybdenite emulsifying collector which comprises 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 450-600 parts of methanol, 60 parts of concentrated sulfuric acid and 90-180 parts of water in parts by weight; the molybdenum ore emulsified collector has stable property, does not change obviously after standing for more than 3 months, and can obviously improve the dispersion performance of diesel oil in water. Under the condition that the ore concentrate grades are equivalent, the emulsified collecting agent prepared by the method can obtain molybdenum ore concentrate with the grade of 4.5% and the recovery rate of 86.5% after once roughing, and the molybdenum recovery rate is obviously improved when the diesel oil collecting agent is used singly. After the emulsified collecting agent is applied to molybdenite flotation, the rough concentration recovery rate of the molybdenite is effectively improved, and efficient recycling of molybdenite resources is facilitated.
Description
Technical Field
The invention belongs to the technical field of mineral processing, and particularly relates to a molybdenite emulsifying collector and a preparation method thereof.
Background
Molybdenite has good natural floatability and is therefore usually treated by flotation in the beneficiation process. The floating is carried out by adding hydrocarbon oil collecting agents, such as kerosene, diesel oil and the like, which act on the surface of the molybdenite to form an oil film, so that the hydrophobicity of the surface of the molybdenite is enhanced, the molybdenite can be adhered to the surface of bubbles and carried to the surface of ore pulp by the bubbles to form mineralized foam, and the mineralized foam is further separated from other minerals.
Hydrocarbon oil is insoluble in water and during flotation it is "broken" into small oil droplets by mechanical agitation and enters the slurry, an unstable system. Therefore, when the use amount of the hydrocarbon oil reaches a certain degree, the increase of the use amount of the hydrocarbon oil has no obvious effect on the increase of the molybdenum recovery rate, but leads to the embrittlement of flotation foam and the reduction of the molybdenum flotation recovery rate.
With the continuous development and utilization of molybdenum ore resources, high-grade molybdenum ore resources are gradually reduced, and low-grade molybdenite is gradually increased. At the moment, the defect of insufficient collecting capability of the traditional kerosene collecting agent gradually appears, and the current production requirement cannot be met. Compared with kerosene, diesel oil has stronger collecting capability, but the diesel oil has higher solidifying point, poor dispersion performance in water, is not beneficial to the flotation of molybdenum ore at low temperature, and has poor selectivity, so that a large amount of copper elements enter molybdenum concentrate to influence the quality of the concentrate. Practice shows that the emulsifier can effectively improve the dispersion effect and stability of the hydrocarbon oil collecting agent in water. Therefore, the problem that needs to be solved at present is to develop a high-performance molybdenite emulsifying collector to further improve the molybdenite flotation recovery effect.
Disclosure of Invention
The invention aims to provide an emulsifier for improving the dispersion effect and stability of a hydrocarbon oil type collector in water and a preparation method thereof.
The molybdenite emulsifying collector comprises, by weight, 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 450-600 parts of methanol, 60 parts of concentrated sulfuric acid and 90-180 parts of water.
Further, the molybdenite emulsifying collector comprises 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 600 parts of methanol, 60 parts of concentrated sulfuric acid and 100 parts of water in parts by weight.
Further, the molybdenite emulsifying collector comprises 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 500 parts of methanol, 60 parts of concentrated sulfuric acid and 90 parts of water in parts by weight.
Further, the molybdenite emulsifying collector comprises 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 450 parts of methanol, 60 parts of concentrated sulfuric acid and 180 parts of water according to parts by weight.
Further, the preparation method of the emulsified collector comprises the following specific processes: mixing coconut oil and methanol, adding into a three-neck flask, slowly dropwise adding concentrated sulfuric acid, reacting at 85 ℃ for 2.0h, washing the obtained product by a sodium carbonate solution for 3 times, standing to remove a water layer, washing by deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering by filter paper to obtain a liquid, namely the emulsifier.
Further, the preparation method of the emulsified collector comprises the following specific processes: mixing coconut oil and methanol, adding into a three-neck flask, slowly dropwise adding concentrated sulfuric acid, reacting at 95 ℃ for 1.5h, washing the obtained product by a sodium carbonate solution for 3 times, standing to remove a water layer, washing by deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering by filter paper to obtain a liquid, namely the emulsifier.
Further, the preparation method of the emulsified collector comprises the following specific processes: mixing coconut oil and methanol, adding into a three-neck flask, slowly dropwise adding concentrated sulfuric acid, reacting at 75 ℃ for 1.8h, washing the obtained product by a sodium carbonate solution for 3 times, standing to remove a water layer, washing by deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering by filter paper to obtain a liquid, namely the emulsifier.
The invention has the beneficial effects that: the molybdenite emulsifying collector provided by the invention has stable properties, does not change obviously after standing for more than 3 months, and can obviously improve the dispersion performance of diesel oil in water. Under the condition that the ore concentrate grades are equivalent, the emulsified collecting agent prepared by the method can obtain molybdenum ore concentrate with the grade of 4.5% and the recovery rate of 86.5% after once roughing, and the molybdenum recovery rate is obviously improved when the diesel oil collecting agent is used singly. After the emulsified collecting agent is applied to molybdenite flotation, the rough concentration recovery rate of the molybdenite is effectively improved, and efficient recycling of molybdenite resources is facilitated.
The present invention will be described in further detail with reference to examples.
Drawings
Fig. 1 is a graph showing the distribution of oil droplet sizes in the molybdenite emulsified collector prepared in example 2, which was measured by a laser particle size analyzer.
Fig. 2 is a graph showing the distribution of the sizes of oil droplets in the molybdenite emulsified collector prepared in example 3, which was measured by a laser particle size analyzer.
Fig. 3 is a graph showing the distribution of the sizes of oil droplets in the molybdenite emulsified collector prepared in example 4, which was measured by a laser particle size analyzer.
Detailed Description
To further explain the technical means and effects of the present invention adopted to achieve the intended purpose, the following detailed description of the embodiments, structural features and effects of the present invention will be made with reference to the accompanying drawings and examples.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.
Example 1
To provide an emulsifier which improves the dispersion effect and stability of a hydrocarbon oil type collector in water and a preparation method thereof.
The molybdenite emulsifying collector comprises, by weight, 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 450-600 parts of methanol, 60 parts of concentrated sulfuric acid and 90-180 parts of water.
Further, the molybdenite emulsifying collector comprises 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 600 parts of methanol, 60 parts of concentrated sulfuric acid and 100 parts of water in parts by weight.
Further, the molybdenite emulsifying collector comprises 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 500 parts of methanol, 60 parts of concentrated sulfuric acid and 90 parts of water in parts by weight.
Further, the molybdenite emulsifying collector comprises 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 450 parts of methanol, 60 parts of concentrated sulfuric acid and 180 parts of water according to parts by weight.
Further, coconut oil and methanol are analytical pure reagents, and concentrated sulfuric acid is sulfuric acid with the concentration of 98%.
Further, the preparation method of the emulsified collector comprises the following specific processes: mixing coconut oil and methanol, adding into a three-neck flask, slowly dropwise adding concentrated sulfuric acid, reacting at 85 ℃ for 2.0h, washing the obtained product by a sodium carbonate solution for 3 times, standing to remove a water layer, washing by deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering by filter paper to obtain a liquid, namely the emulsifier.
Further, the preparation method of the emulsified collector comprises the following specific processes: mixing coconut oil and methanol, adding into a three-neck flask, slowly dropwise adding concentrated sulfuric acid, reacting at 95 ℃ for 1.5h, washing the obtained product by a sodium carbonate solution for 3 times, standing to remove a water layer, washing by deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering by filter paper to obtain a liquid, namely the emulsifier.
Further, the preparation method of the emulsified collector comprises the following specific processes: mixing coconut oil and methanol, adding into a three-neck flask, slowly dropwise adding concentrated sulfuric acid, reacting at 75 ℃ for 1.8h, washing the obtained product by a sodium carbonate solution for 3 times, standing to remove a water layer, washing by deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering by filter paper to obtain a liquid, namely the emulsifier.
The preparation method adopts a three-neck flask as a reaction device, a heat collection type magnetic stirrer as heating equipment, the stirring speed is 300r/min, and anhydrous sodium carbonate is an analytical reagent.
Example 2
Raw materials: no. 0 diesel oil 4.5g, coconut oil 15.0g, methanol 50.0g, concentrated sulfuric acid 6.0g, water 9.0g
The preparation method comprises the following steps: mixing coconut oil and methanol, adding the mixture into a three-neck flask, slowly dropwise adding 6.0g of concentrated sulfuric acid, reacting at 95 ℃ for 1.5h, washing the product obtained by the reaction with a sodium carbonate solution for 3 times, standing to remove a water layer, washing with deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering with filter paper to obtain a liquid, namely the emulsifier. 0.5g of the emulsifier is taken and added into diesel oil, and water is added for stirring. The average particle size of the prepared emulsion is 59.46nm, as shown in figure 1, and the average particle size is the distribution of the oil drops in the molybdenite emulsified collector determined by a laser particle size analyzer.
Example 3
Raw materials: no. 0 diesel oil 4.5g, coconut oil 15.0g, methanol 60.0g, concentrated sulfuric acid 6.0g, water 10.0g
The preparation method comprises the following steps: mixing coconut oil and methanol, adding the mixture into a three-neck flask, slowly dropwise adding 6.0g of concentrated sulfuric acid, reacting at 85 ℃ for 2.0h, washing the product obtained by the reaction with a sodium carbonate solution for 3 times, standing to remove a water layer, washing with deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering with filter paper to obtain a liquid, namely the emulsifier. 0.5g of the emulsifier was added to 4.5g of diesel oil, and water was added thereto and stirred on a magnetic stirrer. The average particle size of the prepared emulsion is 40.07nm, as shown in fig. 2, which is the condition of particle size distribution of oil drops in the prepared molybdenite emulsified collector determined by a laser particle size analyzer.
Example 4
Raw materials: no. 0 diesel oil 4.5g, coconut oil 15.0g, methanol 45.0g, concentrated sulfuric acid 6.0g, water 18.0g
The preparation method comprises the following steps: mixing coconut oil and methanol, adding the mixture into a three-neck flask, slowly dropwise adding 6.0g of concentrated sulfuric acid, reacting at 75 ℃ for 1.8h, washing the product obtained by the reaction with a sodium carbonate solution for 3 times, standing to remove a water layer, washing with deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering with filter paper to obtain a liquid, namely the emulsifier. 0.5g of the emulsifier is taken and added into diesel oil, and water is added to stir on a magnetic stirrer. The average particle size of the prepared emulsion is 111.31nm, as shown in fig. 3, which is the condition of particle size distribution of oil drops in the prepared molybdenite emulsified collector determined by a laser particle size analyzer.
In order to verify the advantages of the invention, the same batch of molybdenite samples were floated by selecting diesel oil No. 0 and the emulsified collectors of the three embodiments of the invention, and the results of the first roughing are shown in the following table.
As can be seen from the table, when No. 0 diesel oil is used for flotation, the recovery rate of molybdenite is 83.5%, and after the emulsified collector prepared by the invention is used, the flotation recovery rates in examples 2, 3.0% and 1.3% are respectively improved, and the molybdenum grade of the concentrate is not significantly reduced. Wherein, with the best effect of the embodiment 3, the recovery rate of the molybdenum in the concentrate is improved by 3 percent under the condition that the grade of the molybdenum in the concentrate is slightly improved.
In conclusion, the molybdenite emulsifying collector has stable property, does not change obviously after standing for more than 3 months, and can obviously improve the dispersion performance of diesel oil in water. Under the condition that the ore concentrate grades are equivalent, the emulsified collecting agent prepared by the method can obtain molybdenum ore concentrate with the grade of 4.5% and the recovery rate of 86.5% after once roughing, and the molybdenum recovery rate is obviously improved when the diesel oil collecting agent is used singly. After the emulsified collecting agent is applied to molybdenite flotation, the rough concentration recovery rate of the molybdenite is effectively improved, and efficient recycling of molybdenite resources is facilitated.
The foregoing is a more detailed description of the invention in connection with specific preferred embodiments and it is not intended that the invention be limited to these specific details. For those skilled in the art to which the invention pertains, several simple deductions or substitutions can be made without departing from the spirit of the invention, and all shall be considered as belonging to the protection scope of the invention.
Claims (7)
1. The molybdenite emulsified collector is characterized in that: the composite material comprises 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 450-600 parts of methanol, 60 parts of concentrated sulfuric acid and 90-180 parts of water in parts by weight.
2. The emulsified collector for molybdenite as set forth in claim 1, wherein: according to the weight portion, the composite material comprises 45 portions of No. 0 diesel oil, 150 portions of coconut oil, 600 portions of methanol, 60 portions of concentrated sulfuric acid and 100 portions of water.
3. The emulsified collector for molybdenite as set forth in claim 1, wherein: 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 500 parts of methanol, 60 parts of concentrated sulfuric acid and 90 parts of water.
4. The emulsified collector for molybdenite as set forth in claim 1, wherein: 45 parts of No. 0 diesel oil, 150 parts of coconut oil, 450 parts of methanol, 60 parts of concentrated sulfuric acid and 180 parts of water.
5. The method of preparing an emulsified collector for molybdenite according to claim 1, wherein: the preparation method of the emulsified collector comprises the following specific processes: mixing coconut oil and methanol, adding into a three-neck flask, slowly dropwise adding concentrated sulfuric acid, reacting at 85 ℃ for 2.0h, washing the obtained product by a sodium carbonate solution for 3 times, standing to remove a water layer, washing by deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering by filter paper to obtain a liquid, namely the emulsifier.
6. The molybdenite emulsified collector and the preparation method thereof according to claim 1, wherein: the preparation method of the emulsified collector comprises the following specific processes: mixing coconut oil and methanol, adding into a three-neck flask, slowly dropwise adding concentrated sulfuric acid, reacting at 95 ℃ for 1.5h, washing the obtained product by a sodium carbonate solution for 3 times, standing to remove a water layer, washing by deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering by filter paper to obtain a liquid, namely the emulsifier.
7. The molybdenite emulsified collector and the preparation method thereof according to claim 1, wherein: the preparation method of the emulsified collector comprises the following specific processes: mixing coconut oil and methanol, adding into a three-neck flask, slowly dropwise adding concentrated sulfuric acid, reacting at 75 ℃ for 1.8h, washing the obtained product by a sodium carbonate solution for 3 times, standing to remove a water layer, washing by deionized water for 3 times, standing to remove the water layer, adding anhydrous sodium carbonate, drying, and filtering by filter paper to obtain a liquid, namely the emulsifier.
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