CN111482277B - Collecting agent for magnesium-silicon phosphate rock mixed reverse flotation, preparation method and beneficiation method - Google Patents
Collecting agent for magnesium-silicon phosphate rock mixed reverse flotation, preparation method and beneficiation method Download PDFInfo
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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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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/02—Froth-flotation processes
- B03D1/021—Froth-flotation processes for treatment of phosphate ores
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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
- B03D1/08—Subsequent treatment of concentrated product
- B03D1/082—Subsequent treatment of concentrated product of the froth product, e.g. washing
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D1/00—Flotation
- B03D1/08—Subsequent treatment of concentrated product
- B03D1/087—Subsequent treatment of concentrated product of the sediment, e.g. regrinding
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2201/00—Specified effects produced by the flotation agents
- B03D2201/02—Collectors
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- B03D—FLOTATION; DIFFERENTIAL SEDIMENTATION
- B03D2203/00—Specified materials treated by the flotation agents; specified applications
- B03D2203/02—Ores
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- B03D2203/06—Phosphate ores
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Abstract
The invention provides a collecting agent for magnesium-silicon phosphorite mixed reverse flotation, a preparation method and a beneficiation method. The beneficiation method comprises the following steps: (1) grinding the magnesium-silicon phosphate ore until the granularity is-0.074 mm and the proportion is 85%, and adding water to prepare ore pulp; (2) adding 15kg/t of sulfuric acid into the ore pulp, adding 300g/t of a special collecting agent, performing rough concentration operation, and scraping bubbles; the special collecting agent comprises the following components in parts by weight: 10-20 parts of oxidized paraffin soap, 5-15 parts of ether amine and 20-30 parts of kerosene; (3) performing one-time mixed reverse flotation scavenging operation on the tank bottom product obtained by roughing, and performing two-time mixed reverse flotation refining operation to obtain a refined tank bottom product, namely a phosphate concentrate product; (4) and (4) performing mixed reverse flotation scavenging operation on the foam product obtained by rough concentration, and scraping foam to obtain a scavenging foam product, namely tailings. The indexes of the phosphate concentrate product obtained by the method are improved, the types and the using amount of the reagents are small, and the beneficiation cost is reduced.
Description
Technical Field
The invention belongs to the technical field of mineral separation, and particularly relates to a collecting agent for magnesium-silicon phosphorite mixed reverse flotation, a preparation method and a mineral separation method.
Background
The phosphate ore can be subjected to crushing, ore grinding, stirring and flotation processes to obtain qualified phosphate concentrate products, and can be used for preparing phosphate fertilizers and phosphorus compound raw materials. At present, the method for ore dressing and enriching the phosphate ore is mainly a flotation method, and the flotation method comprises direct flotation and reverse flotation. The process in which the phosphorus mineral, the target product, is scraped off in froth during flotation is called forward flotation, and the process in which gangue minerals are scraped off is called reverse flotation. The conditioning agent used in the direct flotation is sodium carbonate or sodium hydroxide size mixing, proper inhibitor is used for inhibiting silicate gangue minerals, and fatty acid medicament is used as collecting agent for carrying out phosphate mineral flotation. The reverse flotation is carried out in the process of 'little floating and much restraining', so that the higher selectivity of the flotation process can be ensured, the flotation process is easy to control and stabilize, and the mechanical impurities and the difficulty of flotation foam conveying in the flotation process are reduced.
The phosphorite resource of China is ancient in the age of the finished ore and contains P2O5The middle-low grade, magnesium-silicon refractory sedimentary phosphate ore is taken as a main body. For magnesium silicon phosphate ore, in order to improve the quality of the concentrate, reverse flotation of gangue minerals (carbonate minerals or silicate minerals) is the effective method at present. The single magnesium phosphate rock reverse flotation adopts sulfuric acid, phosphoric acid or mixed phosphoric and phosphoric acid as a phosphate mineral inhibitor, and uses fatty acid medicament as a collecting agent to reverse flotation of carbonate gangue mineral; reverse flotation of siliceous phosphate ore is carried out by directly floating silicate gangue minerals in an alkaline medium by adopting an amine collecting agent. The magnesium-silicon phosphate ore is generally subjected to step-by-step ore dressing and enrichment by adopting a forward-reverse flotation combined process or a double-reverse flotation combined process. And during the positive-negative flotation, mixed rough concentrate of phosphate minerals and carbonate minerals is firstly selected, and the carbonate minerals are selected from the mixed rough concentrate by adopting the negative flotation, so that the remained phosphate concentrate product is obtained. During double reverse flotation, carbonate minerals are firstly selected out, then silicate minerals are selected out, and the remaining part is phosphate minerals. The prior forward-reverse flotation and double-reverse flotation step-by-step enrichment process for magnesium-silicon phosphate ore has the defects of long flow, more reagents, high cost, inconvenient operation and the like. The existing double reverse flotation operation is difficult to be carried out simultaneously, and only carbonate minerals and silicate minerals can be distributed and floatedThe separation effect of the phosphorus concentrate is poor, and the phosphorus concentrate product with high quality is difficult to obtain.
Therefore, whether the process flow of the existing double reverse flotation can be simplified, the quality of the phosphate concentrate obtained by the double reverse flotation can be improved, and a phosphate concentrate product with high grade and high recovery rate is obtained becomes a technical problem to be solved urgently.
Disclosure of Invention
The invention aims to solve the technical problems and provides a collector for the mixed reverse flotation of magnesium-silicon phosphorite, a preparation method and a beneficiation method. The beneficiation method combines the selection of the collecting agent, adopts the mixed reverse flotation process, does not need to perform the distribution of the reverse flotation process, enables the carbonate mineral and the silicate mineral to be simultaneously mixed and floated in the one-step reverse flotation process, and obtains the high-quality phosphate concentrate product. The collecting agent and the beneficiation method achieve the purposes of simplifying the existing double-reverse flotation process and reducing the cost, and meanwhile, high-quality phosphate concentrate products can be obtained by adopting the collecting agent and the beneficiation method under extremely low raw ore grade.
One of the purposes of the invention is to provide a beneficiation method for magnesium-silicon phosphorite mixed reverse flotation, which comprises the following steps:
(1) grinding raw magnesium-silicon phosphate ore to the granularity required by flotation, and adding water to prepare ore pulp;
(2) adding sulfuric acid and a special collecting agent into the ore pulp obtained in the step (1) to perform a 'one-rough one-sweep two-fine' mixed reverse flotation process, wherein the special collecting agent comprises the following components in parts by weight: 10-20 parts of oxidized paraffin soap, 5-15 parts of ether amine and 20-30 parts of kerosene; the dosage of the sulfuric acid is 15kg/t, and the dosage of the special collecting agent is 300 g/t;
the mixed reverse flotation process comprises the steps of primary roughing, primary scavenging and secondary concentration, wherein a tank bottom product obtained after the secondary concentration is a phosphate concentrate product; and performing primary roughing and primary scavenging to obtain a foam product, namely the tailings.
The above-mentioned technological process of the present invention is based on the collecting agent of the present invention, and adopts "one rough sweepThe two-concentrate hybrid reverse flotation process has the following advantages compared with the existing double reverse flotation process: in the reverse flotation process, the carbonate mineral and the silicate mineral can be simultaneously mixed and floated by combining the collecting agent of the invention by adopting a one-step method. Researches show that the collector has a synergistic composite effect in the one-step mixed reverse flotation process, can simultaneously collect carbonate and silicate gangue minerals, can simplify the flotation process of magnesium-silicon phosphate ore, reduce the types and the dosage of medicaments, reduce the medicament cost, improve the P content in a phosphate concentrate product2O5Content, and content of MgO and SiO in the product2The content of (a).
The collector has good selectivity, and can have strong selective collecting performance on silicate and carbonate gangue minerals and weaker collecting capability on phosphate minerals when a mixed reverse flotation step is carried out in an acidic medium. Meanwhile, the collecting agent can be used for separating ores P2O5High-quality phosphate concentrate products can be obtained under the condition of very low grade, and the aim of high-efficiency utilization of resources is fulfilled.
Further, in the step (1), the raw ore is ground to a particle size of-0.074 mm which accounts for 85 percent.
Further, in the step (1), the magnesium siliceous phosphate ore is firstly crushed to-2 mm, and then the crushed ore and water are fed into a mill according to the mass ratio of 5:3 and then are ground.
Further, water is added in the step (1) to prepare ore pulp with the liquid-solid ratio of 2L:1 kg.
Further, after the primary roughing operation is carried out in the step (2), foam scraping is carried out for 5 minutes to obtain a roughing foam product and a roughing tank bottom product; 5kg/t of sulfuric acid is added into the roughing foam product, and one scavenging operation is carried out.
Further, after primary scavenging operation is carried out in the step (2), foam scraping is carried out for 4 minutes to obtain a scavenging foam product, namely tailings, and the scavenging foam product is returned to the roughing operation.
Further, adding 120g/t of special collecting agent into the roughing tank bottom product obtained in the step (2), carrying out mixed reverse flotation and refining I operation, then scraping and soaking for 4 minutes to obtain a foam product of the refining I and a tank bottom product of the refining I, and returning the foam product of the refining I to the roughing operation.
And (3) further, in the step (2), performing mixed reverse flotation and concentration II operation on the bottom product of the concentration I tank, scraping and soaking for 3 minutes to obtain a foam product of the concentration II tank and a bottom product of the concentration II tank, returning the foam product of the concentration II tank to the concentration I operation, and obtaining the bottom product of the concentration II tank, namely the phosphorus concentrate product.
Specifically, the beneficiation method for the mixed reverse flotation of magnesium-silicon phosphorite comprises the following steps:
(1) grinding the magnesium-silicon phosphate ore until the granularity is-0.074 mm and the proportion is 85%, adding water to prepare ore pulp, and performing the mixed reverse flotation operation of the steps (2) - (5);
(2) adding 15kg/t of sulfuric acid into the ore pulp obtained in the step (1), then adding 300g/t of a special collecting agent, performing rough separation operation, and then scraping bubbles to obtain a rough separation foam product and a rough separation tank bottom product; the special collecting agent comprises the following components in parts by weight: 10-20 parts of oxidized paraffin soap, 5-15 parts of ether amine and 20-30 parts of kerosene;
(3) adding 5kg/t of sulfuric acid into the roughing foam product obtained in the step (2), performing mixed reverse flotation scavenging operation, then scraping foam, wherein the scraped scavenging foam product is tailings, and returning the scavenging tank bottom product to the roughing operation;
(4) adding 120g/t of special collecting agent into the bottom product of the roughing cell obtained in the step (2), performing mixed reverse flotation and fine selection I, then scraping bubbles, returning the scraped bubbles to the roughing cell, and allowing the bottom product of the cell to enter fine selection II;
(5) and (4) performing mixed reverse flotation concentration II operation on the product at the bottom of the concentration tank I obtained in the step (4), then scraping bubbles, and returning the scraped foam product to the concentration tank I operation, wherein the product at the bottom of the tank is the phosphate concentrate product.
The invention also aims to provide a special collecting agent for the mixed reverse flotation of magnesium siliceous phosphate ore, which comprises the following components in parts by weight: 10-20 parts of oxidized paraffin soap, 5-15 parts of ether amine and 20-30 parts of kerosene, wherein the beneficiation method of the magnesium-silicon phosphorite mixed reverse flotation process is as described above in the invention.
The third purpose of the invention is to provide a preparation method of the special collector, which comprises the following steps:
(1) weighing 20-30 parts of kerosene, slowly adding 10-20 parts of oxidized paraffin soap into the kerosene under ultrasonic stirring, and stirring and emulsifying for 5-20 minutes;
(2) slowly adding 5-15 parts of ether amine into the product obtained in the step (1), and continuing to stir and emulsify for 10-20 minutes by ultrasonic waves; obtaining the special collecting agent for the gangue mixed reverse flotation of the magnesium siliceous phosphate ore;
(3) and (3) slowly adding 9-99 parts of water into the product obtained in the step (2), and continuing to stir and emulsify for 10-30 minutes by ultrasonic waves to obtain the stock solution of the magnesium-silicon phosphorite mixed reverse flotation collector.
Compared with the prior art, the invention has the following beneficial effects: the agent of the invention is used as the gangue mineral reaction flotation collector, and a simplified mixed reverse flotation process of 'one rough and one sweep of two fine' is adopted, so that the indexes of phosphate concentrate products are superior to the indexes of the traditional step reverse flotation process, and the types and the dosage of the agent are less than those of the traditional step reverse flotation process, thereby greatly reducing the agent cost.
Drawings
FIG. 1 is a hybrid reverse flotation process according to an embodiment of the present invention;
fig. 2 is a conventional step-wise double reverse flotation process.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is described in detail below with reference to the following embodiments, and it should be noted that the following embodiments are only for explaining and illustrating the present invention and are not intended to limit the present invention. The invention is not limited to the embodiments described above, but rather, may be modified within the scope of the invention.
Example 1
A mineral separation method for the mixed reverse flotation of Mg-Si phosphorus ore features that the Mg-Si phosphorus ore from Sichuan is used as raw material and P in raw ore2O5Content 19.56% SiO2The content of the components is 19.63 percent,the MgO content is 7.65%, and the collecting agent adopted in the ore dressing is prepared by the following method:
(1) weighing raw materials, 30g of oxidized paraffin soap and 60g of kerosene;
(2) continuously stirring the weighed kerosene under the action of ultrasonic waves, slowly adding oxidized paraffin soap, and stirring and emulsifying for 10 minutes to fully dissolve and emulsify the kerosene;
(3) slowly adding 15g of ether amine after the operation of the step (2), continuously stirring under the action of ultrasonic waves, and stirring and emulsifying for 15 minutes to fully dissolve and emulsify the ether amine;
(4) adding 2000g of water slowly after the operation of the step (3), continuously stirring under the action of ultrasonic waves, and stirring and emulsifying for 20 minutes to obtain the collecting agent stock solution of the magnesium siliceous phosphate ore mixed reverse flotation silicate and carbonate gangue minerals for later use;
the operation of carrying out the mixed reverse flotation on the ore by adopting the collecting agent stock solution is as follows:
(1) crushing the magnesium siliceous phosphate ore to-2 mm, feeding the crushed ore and water into a mill according to the mass ratio of 5:3, grinding the crushed ore and water to-0.074 mm accounting for 85 percent, adding water until the liquid-solid ratio of ore pulp is 2:1, and performing mixed reverse flotation;
(2) adding 15Kg/t of sulfuric acid, adding 300g/t of collecting agent, performing rough concentration operation, and scraping and soaking for 5 minutes;
(3) adding 5Kg/t of sulfuric acid into the roughing foam product, performing mixed reverse flotation scavenging operation, scraping foam for 4 minutes, wherein the scraped foam product is tailings, and returning the bottom product of the tank to the roughing operation;
(4) adding 120g/t of collecting agent into the bottom product of the roughing tank, performing mixed reverse flotation and fine separation 1, scraping foam for 4 minutes, returning the scraped foam to the roughing operation, and allowing the bottom product of the roughing tank to enter fine separation 2;
(5) performing mixed reverse flotation concentration 2 operation on the bottom product of the concentration 1 tank, scraping foam for 3 minutes, returning the scraped foam product to the concentration 1 operation, and obtaining the bottom product of the tank, namely a phosphate concentrate product;
according to the beneficiation method, P can be finally obtained2O5The recovery rate of the high-quality phosphate concentrate product with the content of 33.26 percent is 85.48 percent. Compared with the traditional step-by-step double reverse methodThe flotation process is compared, the traditional process flow is shown in figure 2, and the test data and the dosage of the medicament are shown in table 1. The results obtained by comparison are shown in Table 1.
As can be seen from the data in Table 1, the raw ore P of middle and low grade is used2O5The gangue mineral collecting agent is combined with the gangue mineral collecting agent, the mineral separation method adopts a simplified mixed reverse flotation process of 'one rough one sweep two fine', the product index of the phosphate concentrate is superior to the index of the traditional step reverse flotation process, the types and the dosage of the reagents are less than those of the traditional step reverse flotation process, the reagent cost is greatly reduced, and the purpose of efficiently utilizing resources is achieved.
TABLE 1
Example 2
A mineral separation method for the mixed reverse flotation of Mg-Si phosphorus ore features that the Mg-Si phosphorus ore from Sichuan is used as its raw material, where P is2O5Content of 15.64%, SiO2The content of 23.58 percent and the content of MgO is 9.37 percent, and the gangue mineral collector used in the mineral separation is prepared by the following method:
(1) weighing raw materials, 25g of oxidized paraffin soap and 50g of kerosene;
(2) continuously stirring the weighed kerosene under the action of ultrasonic waves, slowly adding oxidized paraffin soap, and stirring and emulsifying for 15 minutes to fully dissolve and emulsify the kerosene;
(3) slowly adding 20g of etheramine after the operation of the step (2), continuously stirring under the action of ultrasonic waves, and stirring and emulsifying for 15 minutes to fully dissolve and emulsify the etheramine;
(4) and (4) slowly adding 2000g of water after the operation of the step (3), continuously stirring under the action of ultrasonic waves, and stirring and emulsifying for 20 minutes to obtain the collecting agent stock solution for the magnesium siliceous phosphate ore mixed reverse flotation silicate and carbonate gangue minerals for later use.
The operation of carrying out the mixed reverse flotation on the ore by adopting the collecting agent stock solution is as follows:
(1) crushing ores to the size of minus 2mm, feeding the crushed ores and water into a mill according to the weight ratio of 5:3, grinding the crushed ores and water to the size of minus 0.074mm accounting for 90 percent, adding water until the liquid-solid ratio of ore pulp is 2:1, and performing mixed reverse flotation;
(2) adding 20Kg/t of sulfuric acid, adding 350g/t of collecting agent, performing rough concentration operation, and scraping and soaking for 6 minutes;
(3) adding 6Kg/t of sulfuric acid into the roughing foam product, performing mixed reverse flotation scavenging operation, scraping foam for 5 minutes, wherein the scraped foam product is tailings, and returning the bottom product of the tank to the roughing operation;
(4) adding 150g/t of collecting agent into the bottom product of the roughing cell, performing mixed reverse flotation and fine selection 1 operation, scraping foam for 5 minutes, returning the scraped foam to the roughing operation, and allowing the bottom product of the cell to enter fine selection 2 operation;
(5) and (3) performing mixed reverse flotation concentration 2 operation on the product at the bottom of the tank of the concentration 1, scraping foam for 4 minutes, returning the scraped foam product to the concentration 1 operation, and obtaining the product at the bottom of the tank, namely the phosphate concentrate product.
P can be finally obtained2O5The recovery rate of the high-quality phosphate concentrate product with the content of 31.28 percent is 80.56 percent. Compared with the traditional step-by-step double reverse flotation process, the traditional step-by-step double reverse flotation process flow is shown in the figure 2, and the test data and the medicament dosage are shown in the table 2.
As can be seen from the data in Table 2, in the raw ore P2O5The gangue mineral collecting agent is selected at extremely low grade, the mineral separation method of the invention adopts a simplified mixed reverse flotation process of 'one coarse and one sweep of two fine', the indexes of phosphate concentrate products are superior to the indexes of the traditional step reverse flotation process, and the types and the dosage of medicaments are less than those of the traditional step reverse flotation process, thereby greatly reducing the medicament cost and achieving the purpose of efficiently utilizing resources.
TABLE 2
Claims (6)
1. The beneficiation method for the mixed reverse flotation of the magnesium-silicon phosphorite is characterized by comprising the following steps: grinding raw magnesium-silicon phosphate ore to the granularity required by flotation, and adding water to prepare ore pulp; (2) adding sulfuric acid and a special collecting agent into the ore pulp obtained in the step (1) to perform a 'one-rough-one-sweep-two-fine' mixed reverse flotation process, wherein the special collecting agent comprises the following components in parts by weight: 10-20 parts of oxidized paraffin soap, 5-15 parts of ether amine and 20-30 parts of kerosene; the dosage of the sulfuric acid is 15kg/t, and the dosage of the special collecting agent is 300 g/t; wherein the mixed reverse flotation process comprises the following steps: carrying out primary roughing operation, and scraping and foaming for 5 minutes after the primary roughing operation to obtain a roughing foam product and a roughing tank bottom product; adding 5kg/t of sulfuric acid into the roughing foam product, carrying out primary scavenging operation, scraping foam for 4 minutes after the primary scavenging operation is carried out, obtaining a scavenging foam product which is tailings, and returning the scavenging foam product to the roughing operation; adding 120g/t of special collecting agent into the obtained roughing tank bottom product, performing mixed reverse flotation and refining I operation, then scraping and soaking for 4 minutes to obtain a foam product of the refining I and a tank bottom product of the refining I, and returning the foam product of the refining I to the roughing operation; and (3) performing mixed reverse flotation and concentration II operation on the tank bottom product of the concentration I, scraping and soaking for 3 minutes to obtain a foam product of the concentration II and a tank bottom product of the concentration II, returning the foam product of the concentration II to the operation of the concentration I, and obtaining a tank bottom product of the concentration II, namely a phosphate concentrate product.
2. The beneficiation method for the mixed reverse flotation of magnesium-silicon phosphate ore according to claim 1, wherein in the step (1), the raw ore is ground to a particle size of-0.074 mm up to 85%.
3. The beneficiation method for the mixed reverse flotation of the magnesium siliceous phosphate ore according to the claim 2, characterized in that in the step (1), the magnesium siliceous phosphate ore is firstly crushed to-2 mm, and then the crushed ore and water are fed into a mill according to the mass ratio of 5:3 and then ground.
4. The beneficiation method for the mixed reverse flotation of magnesium-silicon phosphate ore according to claim 1, wherein water is added in the step (1) to prepare ore pulp with a liquid-solid ratio of 2L:1 kg.
5. The special collecting agent for the mixed reverse flotation of magnesium siliceous phosphate ore is characterized by comprising the following components in parts by weight: 10-20 parts of oxidized paraffin soap, 5-15 parts of ether amine and 20-30 parts of kerosene, wherein the beneficiation method for the magnesium siliceous phosphate rock mixed reverse flotation is as defined in any one of claims 1-4.
6. A preparation method of the special collector according to claim 5, characterized by comprising the following steps: weighing 20-30 parts of kerosene, slowly adding 10-20 parts of oxidized paraffin soap into the kerosene under ultrasonic stirring, and stirring and emulsifying for 5-20 minutes; (2) slowly adding 5-15 parts of ether amine into the product obtained in the step (1), and continuing to stir and emulsify for 10-20 minutes by ultrasonic waves; obtaining the special collecting agent for the gangue mixed reverse flotation of the magnesium siliceous phosphate ore; and (3) slowly adding 9-99 parts of water into the product obtained in the step (2), and continuing to stir and emulsify for 10-30 minutes by ultrasonic waves to obtain the collecting agent stock solution for the mixed reverse flotation of the magnesium siliceous phosphorite.
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| CN115672568B (en) * | 2022-12-30 | 2023-03-14 | 矿冶科技集团有限公司 | Method for preparing low-silicon high-grade phosphogypsum by reverse flotation and desiliconization of phosphogypsum waste residues |
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