CN113731640B - Combined collector for low-grade fluorite ore separation and preparation method and application thereof - Google Patents
Combined collector for low-grade fluorite ore separation and preparation method and application thereof Download PDFInfo
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- CN113731640B CN113731640B CN202010478184.8A CN202010478184A CN113731640B CN 113731640 B CN113731640 B CN 113731640B CN 202010478184 A CN202010478184 A CN 202010478184A CN 113731640 B CN113731640 B CN 113731640B
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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
- B03D1/012—Organic compounds containing sulfur
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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
- B03D2201/02—Collectors
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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 a combined collector for separating low-grade fluorite ore, which belongs to the technical field of mineral processing, and comprises the following main components in percentage by mass: 55-70% of acidized oil; 10-25% of C14-C18 alkyl petroleum sodium sulfonate; 5-10% of sorbitan fatty acid ester; 3-10% of sodium abietate. The invention also discloses a preparation method and application of the combined collector. The combined collector has better dispersibility and selectivity, stable medicament property, non-sticky foam, easy dissipation and low temperature resistance, and can realize normal-temperature flotation. The preparation method of the invention has simple preparation process, easy operation and low cost.
Description
Technical Field
The invention belongs to the technical field of mineral processing, and relates to a combined collector for low-grade fluorite ore separation; the invention also relates to the combined collector and use.
The background technology is as follows:
fluorite is a strategic mineral resource, is a main raw material for preparing fluorine-containing compounds, and is widely applied to industrial departments such as metallurgy, chemical industry, ceramics, building materials, machinery, motors, aviation, agriculture, medicine, precision instruments and the like, and is an important high-energy material for advanced science and emerging industries such as atomic energy, rocket, aerospace and the like. At present, along with the rapid development of global fluorocarbon compounds, fluorine-containing polymers and fluorine-containing fine chemicals, the fluorite fine powder in the international market is in serious shortage, and fluorite becomes an extremely important resource, so that how to utilize and protect the resource and ensure the stable production of fluoride works in China have very important practical significance.
The fluorite ore deposit in China mainly comprises quartz-fluorite ore, calcite-fluorite ore, sulphide ore-fluorite ore, fluorite-barite-calcite ore and the like, wherein the separation difficulty of the calcite-fluorite ore is great, the main raw ore is complex in composition, the mineral symbiotic relationship is close, the embedding granularity is finer, gangue minerals have quartz silicate minerals and carbonate minerals, and particularly, the floatability of calcite and fluorite is similar, and the separation difficulty is great.
At present, the main treatment process for the ores is a single forward flotation process, the forward flotation process adopts multistage concentration to finally select qualified concentrate, and the collector adopts oleic acid fatty acid agents, but the collector has the defects of poor water solubility, poor low temperature resistance, poor selectivity, hard water resistance, low concentrate grade, large consumption and large index fluctuation. Especially in the northern air temperature lower environment, the ore pulp to be floated must be heated to more than 20 ℃ to ensure better floatation effect, which inevitably increases the production cost. Along with the increasing complexity of the properties of the selected ores, the multi-metal co-associated ores and the difficult ore dressing are increased, and the flotation performance of the multi-metal co-associated ores and the difficult ore dressing is improved by screening out various synergists and solubilizers and adding the synergists and solubilizers into the fatty acid collector, so that the multi-metal co-associated ores and the difficult ore dressing have important significance in realizing effective flotation separation of minerals and improving economic benefits and social benefits.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides the combined collector for separating the low-grade fluorite ore, which has the advantages of good selectivity, good dispersibility, hard water resistance, stable property, environmental protection, safety and good adaptability.
The invention aims to provide a preparation method of the combined collector for separating low-grade fluorite ores.
A further technical problem to be solved by the present invention is to provide the use of the combined collector for low-grade fluorite ore sorting.
The technical problems to be solved by the invention are realized by the following technical proposal. The invention relates to a combined collector for separating low-grade fluorite ores, which is characterized in that: the main components of the combined collector consist of the following raw materials in percentage by mass:
55-70% of acidized oil
15-25% of C14-C18 alkyl petroleum sodium sulfonate;
5-10% of sorbitan fatty acid ester;
3-10% of sodium abietate.
The invention relates to a combined collector for separating low-grade fluorite ores, which has the further preferable technical scheme that: the main components of the combined collector consist of the following raw materials in percentage by mass:
55-70% of acidized oil
15-20% of C14-C18 alkyl petroleum sodium sulfonate;
5-10% of sorbitan fatty acid ester;
3-8% of sodium abietate.
The invention relates to a combined collector for separating low-grade fluorite ores, which has the further preferable technical scheme that: the main components of the combined collector consist of the following raw materials in percentage by mass:
65-69% of acidizing oil
16-20% of C14-C18 alkyl petroleum sodium sulfonate;
6-10% of sorbitan fatty acid ester;
5-8% of sodium abietate.
The technical scheme of the combined collector for separating low-grade fluorite ore is characterized by comprising the following steps of:
1. the acidified oil is selected from one of bean acidified oil, cotton acidified oil or rapeseed acidified oil.
2. The sorbitan fatty acid ester is one or more selected from S-20, S-40, S-60 and S-80.
The invention also discloses a combined collector for separating low-grade fluorite ore, which is characterized in that: and heating the acidified oil and the C14-C18 alkyl petroleum sodium sulfonate to 70-80 ℃ according to the weight percentage, adding the sorbitan fatty acid ester, and finally adding the sodium abietate, and uniformly mixing to obtain the modified oil.
The invention also discloses a method for carrying out low-grade fluorite ore floatation by using the combined collector in any one of the technical schemes, which is characterized in that: the combined collector is used in the forward flotation process of the fluorite ore in a mode of dripping the raw materials; the flotation temperature of the direct flotation process is preferably 15-30 ℃, and the pH value is preferably 8-10. The amount of the combined collector is preferably 0.5-2.0kg/t of raw ore.
The combined collector for separating low-grade fluorite ore can be used as a combined collector in fluorite ore separation. When the combined collector is used for floatation, the grade of the concentrate CaF2 after floatation is 92.00-97.00% when the grade of the raw ore CaF2 is 25.00-49.00%, and the recovery rate of the concentrate CaF2 can reach 35.00-65.00% after floatation operation.
The combined collector for fluorite ore separation of the present invention is preferably adapted to a reagent developed for fluorite ore separation in an alkaline environment having a pH of 8 to 10.
The principle of the invention is as follows: the positioning ions on the surfaces of fluorite and calcite minerals are Ca 2+ The floatability of the two fatty acid systems is similar, the separation difficulty is high, and the qualified fluorite concentrate can be obtained through repeated concentration. Therefore, the novel structure fatty acid collector is screened, the flotation performance of the fatty acid collector is improved, and the novel structure fatty acid collector has important significance for realizing effective flotation separation of minerals and improving economic benefit and social benefit. The flotation performance of the fatty acid collector can be remarkably improved by screening out various synergists and solubilizers and then adding the synergists and solubilizers into the fatty acid collector.
Compared with the prior art, the invention has the following beneficial effects:
the main medicine in the low-grade fluorite ore positive flotation collector provided by the invention is acidified oil, the carbon chain length of the main medicine is mainly C18, the hydrophobicity is good, the collection performance is good, the C14-C18 alkyl sodium petroleum sulfonate has excellent water solubility and collection capacity, the main medicine has good synergistic effect after being compounded with the acidified oil, the collection capacity of a combined medicine can be increased, the excellent emulsifying, dispersing and solubilizing performances of sorbitan fatty acid ester can be improved, the dispersibility, hard water resistance and stability of the combined medicine can be improved after being compounded with the acidified oil, and the sodium abietate is taken as an auxiliary synergist to mainly enhance the medicine selectivity.
The preparation method of the invention mixes the medicaments evenly according to the limited sequence, can enhance the water solubility and selectivity and better exert the drug effect. Compared with the conventional reagent, the reagent provided by the invention has the characteristics of good selectivity, strong collection performance, low temperature resistance, low beneficiation cost and the like, and can be suitable for flotation of low-grade fluorite ore.
The medicament formula obtained by the method of the invention presents oily liquid at normal temperature, and has simple preparation process, easy operation and low production cost.
Detailed Description
The invention is further illustrated by the following examples, which are not to be construed as limiting the scope of the invention.
Embodiment 1, a combined collector for low-grade fluorite ore separation, wherein the combined collector mainly comprises the following raw materials in mass fraction:
acidified oil 68%
20% of C14-C18 alkyl petroleum sodium sulfonate;
7% of sorbitan fatty acid ester;
5% of sodium abietate.
The acidified oil is selected from one of bean acidified oil, cotton acidified oil or rapeseed acidified oil.
The sorbitan fatty acid ester is one or more selected from S-20, S-40, S-60 and S-80.
The preparation method comprises the following steps: and (3) mixing and heating the acidified oil and the sodium petroleum sulfonate to 70 ℃ according to the weight percentage, adding the sorbitan fatty acid ester, finally adding the sodium abietate, and uniformly mixing to obtain the modified oil.
Embodiment 2, a combined collector for low-grade fluorite ore separation, wherein the combined collector mainly comprises the following raw materials in mass fraction:
acidified oil 68%
20% of C14-C18 alkyl petroleum sodium sulfonate;
7% of sorbitan fatty acid ester;
5% of sodium abietate.
The acidified oil is selected from one of bean acidified oil, cotton acidified oil or rapeseed acidified oil.
The sorbitan fatty acid ester is one or two selected from S-20, S-40, S-60 and S-80.
The preparation method comprises the following steps: and (3) mixing and heating the acidified oil and the sodium petroleum sulfonate to 70 ℃ according to the weight percentage, adding the sorbitan fatty acid ester, finally adding the sodium abietate, and uniformly mixing to obtain the modified oil.
The method for carrying out low-grade fluorite ore flotation by using the combined collector comprises the following steps: the combined collector is used in the forward flotation process of the fluorite ore in a mode of dripping the raw materials; the flotation temperature of the direct flotation process is 22 ℃, the pH value is 9.5, and the consumption of the combined collector is 0.5kg/t of raw ore.
Embodiment 3, a combined collector for low-grade fluorite ore separation, wherein the combined collector mainly comprises the following raw materials in mass fraction:
67% of acidized oil
20% of C14-C18 alkyl petroleum sodium sulfonate;
8% of sorbitan fatty acid ester;
5% of sodium abietate.
The acidified oil is selected from one of bean acidified oil, cotton acidified oil or rapeseed acidified oil.
The sorbitan fatty acid ester is selected from one or 1 of any two of S-20, S-40, S-60 and S-80: 1.
The preparation method comprises the following steps: and (3) mixing and heating the acidified oil and the sodium petroleum sulfonate to 75 ℃ according to the weight percentage, adding the sorbitan fatty acid ester, finally adding the sodium abietate, and uniformly mixing to obtain the modified oil.
The method for carrying out low-grade fluorite ore flotation by using the combined collector comprises the following steps: the combined collector is used in the forward flotation process of the fluorite ore in a mode of dripping the raw materials; the flotation temperature of the direct flotation process is 22 ℃, the pH value is 9.5, and the consumption of the combined collector is 2.0kg/t of raw ore.
Embodiment 4, a combined collector for low-grade fluorite ore separation, wherein the combined collector mainly comprises the following raw materials in mass fraction:
67% of acidized oil
20% of C14-C18 alkyl petroleum sodium sulfonate;
8% of sorbitan fatty acid ester;
5% of sodium abietate.
The acidified oil is selected from one of bean acidified oil, cotton acidified oil or rapeseed acidified oil.
The sorbitan fatty acid ester adopts 1 for S-20, S-40, S-60 and S-80: 1:1: 1.
The preparation method comprises the following steps: and (3) mixing and heating the acidified oil and the sodium petroleum sulfonate to 75 ℃ according to the weight percentage, adding the sorbitan fatty acid ester, finally adding the sodium abietate, and uniformly mixing to obtain the modified oil.
The method for carrying out low-grade fluorite ore flotation by using the combined collector comprises the following steps: the combined collector is used in the forward flotation process of the fluorite ore in a mode of dripping the raw materials; the flotation temperature of the direct flotation process is 15 ℃, the pH value is 9.5, and the consumption of the combined collector is 1.0kg/t of raw ore.
Embodiment 5, a combined collector for low-grade fluorite ore separation, wherein the combined collector mainly comprises the following raw materials in mass fraction:
67% of acidized oil
20% of C14-C18 alkyl petroleum sodium sulfonate;
8% of sorbitan fatty acid ester;
5% of sodium abietate.
The acidified oil is selected from one of bean acidified oil, cotton acidified oil or rapeseed acidified oil.
The sorbitan fatty acid ester is selected from one of S-20, S-40, S-60 and S-80.
The preparation method comprises the following steps: and (3) mixing and heating the acidified oil and the sodium petroleum sulfonate to 75 ℃ according to the weight percentage, adding the sorbitan fatty acid ester, finally adding the sodium abietate, and uniformly mixing to obtain the modified oil.
The method for carrying out low-grade fluorite ore flotation by using the combined collector comprises the following steps: the combined collector is used in the forward flotation process of the fluorite ore in a mode of dripping the raw materials; the flotation temperature of the direct flotation process is 20 ℃, the pH value is 10, and the consumption of the combined collector is 1.2kg/t of raw ore.
Example 6, a combined collector for low-grade fluorite ore sorting preparation and application experiment:
(1) The raw materials with the following mass percentages are prepared: 67% of acidified oil, 20% of sodium petroleum sulfonate, 8% of sorbitan fatty acid ester, 5% of sodium abietate and 100% of the total components.
The acidified oil is soybean acidified oil, and the sorbitan fatty acid ester is S-20.
(2) Mixing the acidified oil with sodium petroleum sulfonate, heating to 75deg.C, adding sorbitan fatty acid ester, adding sodium abietate, and mixing.
(3) The prepared low-grade fluorite ore combined collector is used in the forward flotation process of the fluorite ore in a raw liquid dripping mode; the flotation temperature of the direct flotation process is 20 ℃, the pH value is 10.0, and the consumption of the combined collector is 1.0kg/t of raw ore.
(4) The result is that the grade of raw ore CaF2 is 32.06%, the grade of concentrate CaF2 after flotation is 95.18%, and the recovery rate of concentrate CaF2 after flotation is 63.56%.
Example 7, a combined collector preparation and application experiment for low-grade fluorite ore sorting two:
(1) The raw materials with the following mass percentages are prepared: 67% of acidified oil, 20% of sodium petroleum sulfonate, 8% of sorbitan fatty acid ester, 5% of sodium abietate and 100% of the total components.
The acidified oil is cotton acidified oil, and the sorbitan fatty acid ester is S-40.
(2) Mixing the acidified oil with sodium petroleum sulfonate, heating to 75deg.C, adding sorbitan fatty acid ester, adding sodium abietate, and mixing.
(3) The prepared low-grade fluorite ore combined collector is used in the forward flotation process of the fluorite ore in a raw liquid dripping mode; the flotation temperature of the direct flotation process is 15 ℃, the pH value is 9.5, and the consumption of the combined collector is 0.8kg/t of raw ore.
(4) The result was that the grade of raw ore CaF2 was 31.51%, the grade of concentrate CaF2 after flotation was 94.21%, and the recovery rate of concentrate CaF2 after flotation was 58.42%.
Example 8, a combined collector preparation and application comparison experiment for low grade fluorite ore sorting, three:
the combined reagent prepared in example 3 was compared with the flotation effect of two collectors currently in common use:
comparative test 1:
(1) The collector adopts sodium oleate, is prepared into 5% solution, and is used in the forward flotation process of fluorite ore; the flotation temperature of the positive flotation process is 20 ℃, the pH value is 10.0, and the consumption of the collector is 1.5kg/t.
(2) As a result, the grade of raw ore CaF2 was 32.06%, the grade of concentrate CaF2 after flotation was 91.44%, and the recovery rate of concentrate CaF2 after flotation was 62.23%
Comparative test 2:
(1) The collector adopts oleic acid, adopts an original liquid dripping mode, and is used in a forward flotation process of fluorite ore; the flotation temperature of the positive flotation process is 20 ℃, the pH value is 10.0, and the consumption of the collector is 1.5kg/t.
(2) As a result, the grade of raw ore CaF2 was 32.06%, the grade of concentrate CaF2 after flotation was 92.64%, and the recovery rate of concentrate CaF2 after flotation was 59.87%
| Name of the name | Grade/% | Concentrate yield/% | Concentrate CaF2 grade/% | Concentrate CaF2 recovery/% |
| Example 6 | 32.06 | 21.41 | 95.18 | 63.56 |
| Comparative test 1 | 32.06 | 19.05 | 91.44 | 54.33 |
| Comparative test 2 | 32.06 | 20.50 | 92.64 | 59.23 |
The comparative test can be seen: the combined collector of the invention is adopted to replace two collectors commonly used at present, the CaF2 grade of concentrate can be greatly improved, the recovery rate of CaF2 can be improved by more than 4%, and the economic benefit is remarkable.
The combinations of the components of the collector according to the present invention are not limited to the combinations of the agents provided in the examples, and any single combination or multiple combinations of the components of the collector are within the scope of the patent.
Claims (10)
1. The utility model provides a combination collector for low-grade fluorite ore deposit is selected separately which characterized in that: the main components of the combined collector consist of the following raw materials in percentage by mass:
55-70% of acidized oil
10-25% of C14-C18 alkyl petroleum sodium sulfonate;
5-10% of sorbitan fatty acid ester;
3-10% of sodium abietate.
2. A combined collector for low grade fluorite ore sorting as claimed in claim 1, wherein: the main components of the combined collector consist of the following raw materials in percentage by mass:
55-70% of acidized oil
15-20% of C14-C18 alkyl petroleum sodium sulfonate;
5-10% of sorbitan fatty acid ester;
3-8% of sodium abietate.
3. A combined collector for low grade fluorite ore sorting as claimed in claim 2, wherein: the main components of the combined collector consist of the following raw materials in percentage by mass:
65-69% of acidizing oil
16-20% of C14-C18 alkyl petroleum sodium sulfonate;
6-10% of sorbitan fatty acid ester;
5-8% of sodium abietate.
4. A combined collector for low grade fluorite ore sorting according to claim 1 or 2 or 3, characterized in that: the acidified oil is selected from one of bean acidified oil, cotton acidified oil or rapeseed acidified oil.
5. A combined collector for low grade fluorite ore sorting as claimed in claim 1, wherein: the sorbitan fatty acid ester is one or more selected from S-20, S-40, S-60 and S-80.
6. A method for preparing a combined collector for low-grade fluorite ore classification according to any one of claims 1 to 5, characterized in that: and heating the acidified oil and the C14-C18 alkyl petroleum sodium sulfonate to 70-80 ℃ according to the weight percentage, adding the sorbitan fatty acid ester, and finally adding the sodium abietate, and uniformly mixing to obtain the modified oil.
7. A method of low grade fluorite flotation using the combined collector of any one of claims 1-5, characterized in that: the combined collector is used in the forward flotation process of the fluorite ore in a raw liquid dripping mode.
8. The method according to claim 7, wherein: the dosage of the combined collector is 0.5-2.0kg/t of raw ore.
9. The method according to claim 7, wherein: the flotation temperature of the direct flotation process is 15-30 ℃ and the pH value is 8-9.
10. Use of a combined collector for low-grade fluorite ore classification according to any one of claims 1-5 as a combined collector in fluorite ore classification.
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