CN111215247B - Inhibitor for high-calcium fluorite direct flotation and flotation method - Google Patents
Inhibitor for high-calcium fluorite direct flotation and flotation method Download PDFInfo
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- CN111215247B CN111215247B CN202010013778.1A CN202010013778A CN111215247B CN 111215247 B CN111215247 B CN 111215247B CN 202010013778 A CN202010013778 A CN 202010013778A CN 111215247 B CN111215247 B CN 111215247B
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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
- B03D1/014—Organic compounds containing phosphorus
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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
- B03D2203/04—Non-sulfide ores
Abstract
The invention provides an inhibitor for high-calcium fluorite direct flotation, which is an aqueous solution of ethylenediamine tetramethylene phosphonic acid. The invention also provides a high-calcium fluorite direct flotation method, which comprises the steps of crushing fluorite raw ore into powder and preparing the powder into ore pulp, then adding a pH regulator into the ore pulp to enable the pH value of the ore pulp to be controlled within 6-8 all the time, simultaneously adding water glass and sodium oleate into the ore pulp, conducting roughing and scavenging on the fluorite raw ore to obtain fluorite rough concentrate, finally adding an inhibitor containing ethylene diamine tetramethylene phosphonic acid into the ore pulp containing the fluorite rough concentrate, conducting concentrating on the fluorite rough concentrate to obtain the fluorite concentrate, wherein the total consumption of the ethylene diamine tetramethylene phosphonic acid of each ton of the fluorite raw ore is 70-450 g. The inhibitor has the advantages of low cost, obvious selectivity, mild use environment and no secondary pollution, can efficiently separate fluorite and calcite in the high-calcium fluorite, and has higher grade and recovery rate of the fluorite.
Description
Technical Field
The invention belongs to the technical field of mineral flotation, and particularly relates to an inhibitor for high-calcium fluorite direct flotation and a high-calcium fluorite direct flotation method using the inhibitor.
Background
Fluorite, also called fluorite, has CaF as its main component2Is the main source of industrial fluorine at present. The application field of fluorine covers industries such as new energy, new materials, national defense, photoelectricity, metallurgy, chemical industry and the like, and plays a role inCan not replace the function, therefore, the fluorite is considered as the strategic protection of mineral resources at home and abroad. The fluorite resource reserves in China are abundant, but most of the fluorite resources are associated ores, and single ore deposits are few.
In nature, fluorite is often closely symbiotic with other calcium-containing minerals, such as calcite, dolomite, scheelite, apatite and the like, and the separation and recovery of the fluorite from the minerals are mainly realized by a flotation method in the industry at present. The main principle of the flotation method is that different minerals are sorted according to the difference of surface properties, and finally a target mineral and a gangue mineral are obtained respectively, and fluorite and the calcium-containing gangue mineral are semi-soluble salt minerals and have similar calcium ion active sites on the surfaces, so that the soluble components on the surfaces of the minerals can be converted mutually, the surface physical and chemical properties of the different minerals are highly similar, and finally the flotation separation effect of the fluorite is quite unsatisfactory.
At present, when the fluorite and the calcium-containing gangue minerals are subjected to flotation separation operation, the separation aim is achieved mainly by adding a fatty acid collecting agent represented by sodium oleate and an inhibitor represented by water glass and modified water glass under a strong alkaline condition. However, when the content of the calcium-containing gangue minerals in the raw ore reaches a certain value, a large amount of gangue depressants are required to be added, the existing gangue depressants for fluorite flotation mainly comprise water glass and modified products thereof, such as acidified water glass and salinized water glass, tannic acid, starch and the like, and although the gangue depressants have certain inhibiting effect on calcite, the gangue depressants have poor selectivity, are difficult to obtain ideal flotation indexes, are large in dosage and pollute the environment. In addition, the strong alkaline ore pulp also seriously influences the recycling of return water.
Therefore, in order to achieve green and efficient separation between fluorite and calcium-containing gangue minerals, it is urgently required to find a novel gangue mineral inhibitor which can exhibit high selectivity under mild conditions.
Disclosure of Invention
The invention aims to provide a fluorite flotation inhibitor which is low in dosage, obvious in selectivity and environment-friendly, so as to solve the problems in the background technology.
In order to achieve the above objects, the present invention provides an inhibitor for high calcium fluorite direct flotation, which comprises ethylenediaminetetramethylenephosphonic acid, by which separation of fluorite from calcium-containing gangue minerals in fluorite raw ore is achieved.
Ethylenediamine tetramethylene phosphonic acid (EDTMPA), also known as ethylenediamine tetramethylene phosphonic acid, is a nitrogenous organic polybasic phosphonic acid, is white crystalline powder at normal temperature, has stable chemical properties, good acid and alkali resistance and high temperature resistance, is non-toxic and pollution-free, can be mixed and dissolved with water, and has the following specific molecular formula:
the ethylenediamine tetramethylene phosphonic acid has stronger metal ion chelating capacity. Specifically, ethylenediamine tetramethylene phosphonic acid dissociates eight pairs of positive and negative ions in water, which can react with multiple metal ions (such as Ca)2+、Mg2+、Zn2+、Cu2+、Fe2+Etc.) are chelated to form a double five-membered ring chelate and are loosely dispersed in water to destroy the normal growth of corresponding salt crystals, so that the double five-membered ring chelate can play a role in scale inhibition and scale removal, and is widely used as a scale inhibitor for circulating cooling water, but the research on the application of ethylenediamine tetramethylene phosphonic acid as a flotation inhibitor in a mineral separation process is almost not available.
In the invention, through the strong adsorption effect of a large number of phosphonic acid groups contained in the molecular structure of the ethylenediamine tetramethylene phosphonic acid on the surface of calcium-containing minerals, the ethylenediamine tetramethylene phosphonic acid shows obvious selectivity on gangue minerals contained in ore pulp, and the adsorption effect enhances the hydrophilicity of the surface of the gangue minerals, thereby achieving the purpose of inhibiting the gangue minerals from entering flotation foams and further realizing the efficient flotation separation between fluorite and the calcium-containing gangue minerals.
The invention also makes full use of the acidity of the ethylenediamine tetramethylene phosphonic acid, so that the surfaces of calcium-containing minerals such as calcite and the like are corroded, further more action sites are generated, and the calcium-containing minerals are selectively inhibited by the ethylenediamine tetramethylene phosphonic acid.
Preferably, the inhibitor is an aqueous solution of ethylenediaminetetramethylenephosphonic acid.
The inhibitor can be used for positive flotation of high-calcium fluorite ores, so that the inhibition effect on calcium-containing gangue minerals can be realized, the high-calcium fluorite ores mean that the mass of the calcium-containing gangue minerals accounts for more than 10% of the total mass of fluorite raw ores, and particularly when the calcium-containing gangue minerals are calcite, the flotation effect is obvious.
The invention also provides a high-calcium fluorite direct flotation method which comprises the step of using the inhibitor in the concentration process. Preferably, the total quantity of ethylenediamine tetramethylene phosphonic acid used per ton of fluorite raw ore in said beneficiation process is 70-450 g.
Specifically, the dosage of the ethylenediamine tetramethylene phosphonic acid has a great relationship with the content of the calcium-containing gangue minerals in the fluorite raw ore, and the total dosage of the ethylenediamine tetramethylene phosphonic acid is continuously increased along with the increase of the content of the calcium-containing gangue minerals. In fact, when the total usage amount of the ethylenediamine tetramethylene phosphonic acid per ton of fluorite raw ore reaches 70g, the excellent inhibition effect on the gangue mineral can be shown, the separation of fluorite and the gangue mineral can be well realized, and the usage amount of the ethylenediamine tetramethylene phosphonic acid is properly increased on the basis, so that the grade of the fluorite concentrate can be further improved.
Preferably, in the concentration process, the number of concentration is 6 to 8. When the fine selection is repeated for 6 to 8 times, the flotation cost performance is optimal; if the number of the reaction is less than 6, the grade of fluorite does not reach the standard, and if the number of the reaction is more than 8, the recovery rate is insufficient.
Preferably, the method specifically comprises the following steps:
1) crushing fluorite raw ore into powder and meeting the requirement of flotation granularity;
2) preparing ore powder into ore pulp, adding a first gangue mineral inhibitor, a collecting agent and a pH regulator into the ore pulp, and performing rough concentration and scavenging on fluorite raw ore to obtain fluorite rough concentrate;
3) adding a second gangue mineral inhibitor containing ethylenediamine tetramethylene phosphonic acid into ore pulp containing fluorite rough concentrates, and carrying out concentration on the fluorite rough concentrates to obtain the required fluorite concentrates, namely target minerals.
Considering cost factors, the first gangue mineral inhibitor is firstly used for roughing, and the aim is to realize primary enrichment of fluorite; the inhibitor provided by the invention is used for concentration as a second gangue mineral inhibitor, and has a better effect of enriching concentrate with lower gangue mineral content due to stronger selectivity of ethylenediamine tetramethylene phosphonic acid.
Preferably, in the step 2), the first gangue mineral inhibitor is water glass, namely, a sodium silicate aqueous solution, the collector is sodium oleate, the pH adjuster comprises a pH alkaline adjuster and/or a pH acidic adjuster, the pH alkaline adjuster is sodium carbonate or sodium hydroxide, and the pH acidic adjuster is sulfuric acid or hydrochloric acid.
Preferably, in the fluorite direct flotation process, the pH value of the ore pulp is controlled between 6 and 8.
Preferably, in the step 1), the content of the fraction with the grinding fineness of-0.074 mm in the ore powder accounts for 75-85% of the raw ore mass.
Preferably, in the step 2), the addition agents are added into the ore pulp, and the stirring is carried out during the aeration flotation, wherein the stirring speed is 1500-.
The technical scheme provided by the invention at least has the following beneficial effects:
1. according to the technical scheme, the ethylenediaminetetramethylenephosphonic acid is used as the gangue mineral inhibitor for the first time in the flotation process of the high-calcium fluorite ore, the floatability difference between the fluorite and the calcite is increased by performing high-selectivity inhibition on the calcite, a good flotation effect is shown, the loss of the fluorite in the flotation process is reduced, and the problem that the high-calcium fluorite is difficult to treat and utilize at present is solved.
2. The inhibitor provided by the invention has the advantages of easily available raw materials, low cost and no secondary pollution, is low in dosage, good in water solubility, strong in selectivity and high in stability in practical application, and has great popularization potential and market application prospect.
3. The inhibitor provided by the invention can realize that the flotation of the high-calcium fluorite ore is carried out in a mild environment without adding a large amount of acid or alkali, so that the cost is effectively saved, the problem of environmental pollution is avoided, the problem of increase of the consumption of the collecting agent caused by more calcium ions generated by dissolving calcite by acid is reduced, and the grade and the recovery rate of fluorite in the obtained fluorite concentrate are higher.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the description of the embodiments will be briefly introduced below, it is obvious that the drawings described below are only some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without inventive efforts, wherein:
FIG. 1 is a schematic flow diagram of a high calcium fluorite direct flotation process of the present invention;
Detailed Description
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.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1
In this example, a high-calcium fluorite ore from Hunan province is used as a raw material, and the sample mainly contains 16.11% of CaF2，13.56％CaCO3. The main gangue minerals are calcite and the like, wherein the calcite content is high, and the separation is difficult.
Referring to fig. 1, a high-calcium fluorite direct flotation method specifically includes the following steps:
1) crushing fluorite raw ore, and grinding the raw ore by using a ball mill to the fineness that the grain size of-0.074 mm accounts for 75-85% of the mass of the raw ore;
2) preparing ore powder into ore pulp, adding 1000g of water glass into each ton of ore pulp to serve as a first gangue mineral inhibitor, stirring for 5min, then adding 300g of sodium oleate serving as a collecting agent, stirring for 3min, and then adjusting the pH value of the ore pulp to 6-8 by hydrochloric acid;
3) stirring and aerating for 5min for flotation with aeration amount of 0.2m3Performing primary roughing and primary scavenging to obtain fluorite rough concentrate;
4) adding an ethylene diamine tetramethylene phosphonic acid aqueous solution into ore pulp containing fluorite rough concentrate to serve as a second gangue mineral inhibitor, wherein the dosage of ethylene diamine tetramethylene phosphonic acid corresponding to each ton of ore pulp in each fine concentration from one fine concentration to four fine concentration is 15g, the dosage of ethylene diamine tetramethylene phosphonic acid corresponding to each ton of ore pulp in each fine concentration from five fine concentration to seven fine concentration is 10g, stirring and inflating, and obtaining fluorite concentrate products after 7 times of fine concentration.
Example 2
In this example, a high calcium fluorite ore from Henan is used as a raw material, and the sample mainly contains 14.66% CaF2，19.23％CaCO3. The main gangue minerals are calcite and the like, wherein the calcite content is high, and the separation is difficult.
The direct flotation method adopted in the embodiment is basically the same as that of the embodiment 1, and the difference is that the dosage of the ethylenediamine tetramethylene phosphonic acid corresponding to each ton of ore pulp in the concentration of one to four in the step 4) is 30g, and the dosage of the ethylenediamine tetramethylene phosphonic acid corresponding to each ton of ore pulp in the concentration of five to seven in the step 4) is 20 g.
Example 3
In this example, Fujian high calcium fluorite ore was used as a raw material, and the sample mainly contained 25.46% CaF2，11.71％CaCO3. The main gangue minerals are calcite and the like, wherein the calcite content is high, and the separation is difficult.
The direct flotation method adopted in the embodiment is basically the same as that of the embodiment 1, and the difference is that the dosage of the ethylenediamine tetramethylene phosphonic acid corresponding to each ton of ore pulp in the concentration of one to four in the step 4) is 15g, and the dosage of the ethylenediamine tetramethylene phosphonic acid corresponding to each ton of ore pulp in the concentration of five to seven in the step 4) is 8 g.
Example 4
The ore sample adopted in the embodiment is the same as that in the embodiment 1, the direct flotation method is basically the same as that in the embodiment 1, and the difference is that in the embodiment, the dosage of the ethylenediamine tetramethylene phosphonic acid corresponding to each ton of ore pulp in the concentration of one to three in the step 4) is 15g, the dosage of the ethylenediamine tetramethylene phosphonic acid corresponding to each ton of ore pulp in the concentration of four is 10g, and the dosage of the ethylenediamine tetramethylene phosphonic acid corresponding to each ton of ore pulp in the concentration of five, the concentration of six and the concentration of seven is 5 g.
Example 5
The sample used in this example is the same as example 1, and the direct flotation process is essentially the same as example 1, except that in this example 100g ethylenediaminetetramethylenephosphonic acid per ton of pulp is used in each of the first to third beneficiates in step 4), 50g ethylenediaminetetramethylenephosphonic acid per ton of pulp is used in each of the fourth and fifth beneficiates, and 25g ethylenediaminetetramethylenephosphonic acid per ton of pulp is used in each of the sixth and seventh beneficiates.
Comparative example 1
The sample used in this example is the same as example 1, and the direct flotation process is essentially the same as example 1, except that this example uses 10g of ethylenediaminetetramethylenephosphonic acid per ton of pulp in the first to third steps of concentration and 5g of ethylenediaminetetramethylenephosphonic acid per ton of pulp in the fourth to seventh steps of concentration in step 4).
Comparative example 2
The sample used in this example is the same as example 1, the direct flotation process is essentially the same as example 1, except that in step 4) 100g of ethylenediaminetetramethylenephosphonic acid per ton of pulp is used for each of the first to fourth concentrates, 50g of ethylenediaminetetramethylenephosphonic acid per ton of pulp is used for the fifth concentrate, and 25g of ethylenediaminetetramethylenephosphonic acid per ton of pulp is used for the sixth and seventh concentrates.
Comparative example 3
The ore sample adopted in the embodiment is the same as the ore sample adopted in the embodiment 1, the direct flotation method is basically the same as the ore sample adopted in the embodiment 1, and the difference is only that the second gangue mineral inhibitor used in the embodiment in the step 4) is the water glass added in the step 2), 150g of water glass is used for each ton of ore pulp in the first concentration and the second concentration, 100g of water glass is used for each ton of ore pulp in the third concentration to the fifth concentration, and 50g of water glass is used for each ton of ore pulp in the sixth concentration and the seventh concentration.
Comparative example 4
The ore sample adopted in the embodiment is the same as the ore sample adopted in the embodiment 1, the direct flotation method is basically the same as the ore sample adopted in the embodiment 1, and the difference is only that the inhibitor used in the step 4) is the ethylene diamine tetra methylene phosphonic acid pentasodium water solution, the dosage of the ethylene diamine tetra methylene phosphonic acid pentasodium corresponding to each ton of ore pulp in the concentration one to four times is 15g, and the dosage of the ethylene diamine tetra methylene phosphonic acid pentasodium corresponding to each ton of ore pulp in the concentration five to seven times is 10 g.
Specific results are shown in table 1.
TABLE 1 Positive flotation decalcifying results for high calcium fluorite ores
According to the embodiment adopting the technical scheme, the invention introduces the ethylenediamine tetramethylene phosphonic acid as the second gangue mineral inhibitor for concentration to selectively inhibit the calcium-containing minerals, effectively realize the separation between two minerals with similar floatability, namely fluorite and calcite, and obtain the CaF in the fluorite concentrate2The grade of the product is over 95 percent, the recovery rate is not lower than 80 percent, and the industrial production requirement is met.
When the total usage amount of the ethylenediamine tetramethylene phosphonic acid in each ton of ore pulp reaches 70g, the separation data of fluorite and calcite is very good, on the basis, the usage amount is continuously increased to further improve the grade of fluorite concentrate, but considering the cost and the cost performance problem brought by the cost, the actual usage amount of the ethylenediamine tetramethylene phosphonic acid in each ton of ore pulp is preferably controlled below 100 g. It can be seen from comparative example 2 that if the usage amount of ethylenediamine tetramethylene phosphonic acid is too large, the fluorite and calcite are inhibited at the same time, so that the grade and recovery rate of the fluorite in the fluorite concentrate are reduced, and the flotation purpose cannot be realized.
It can be seen from the comparison of examples 3 and 4 that the present invention selects ethylenediaminetetramethylenephosphonic acid as gangue mineral inhibitor, and shows excellent selectivity in the direct flotation of high calcium fluorite, in contrast, the same technical effect as the present invention can not be obtained by other forms of conventional water glass or ethylenediaminetetramethylenephosphonic acid.
The above description is only a preferred embodiment of the present invention and is not intended to limit the scope of the present invention, and various modifications and changes may be made by those skilled in the art. Any improvement or equivalent replacement directly or indirectly applied to other related technical fields within the spirit and principle of the invention and the contents of the specification and the drawings of the invention shall be included in the protection scope of the invention.
Claims (5)
1. A high-calcium fluorite direct flotation method is characterized by comprising the following steps:
1) crushing fluorite raw ore into powder and meeting the requirement of flotation granularity;
2) preparing ore powder into ore pulp, adding a first gangue mineral inhibitor, a collecting agent and a pH regulator into the ore pulp, and performing rough concentration and scavenging on fluorite raw ore to obtain fluorite rough concentrate;
3) adding a second gangue mineral inhibitor containing ethylene diamine tetramethylene phosphonic acid into ore pulp containing fluorite rough concentrates, and carrying out concentration on the fluorite rough concentrates to obtain required fluorite concentrates, namely target minerals;
in the concentration process, the total consumption of the ethylenediamine tetramethylene phosphonic acid per ton of fluorite raw ore is 70-450 g.
2. The method of the positive flotation of high calcium fluorite according to claim 1, characterized in that the number of beneficiations is 6-8 in the beneficiating process.
3. The high calcium fluorite direct flotation process according to claim 1 wherein in said step 2) said first gangue mineral depressant is water glass, said collector is sodium oleate, said pH modifier comprises a pH alkaline modifier which is sodium carbonate or sodium hydroxide and/or a pH acidic modifier which is sulfuric acid or hydrochloric acid.
4. The process of claim 1, wherein the slurry is controlled to have a pH of 6 to 8 during the fluorite direct flotation process.
5. The method for the direct flotation of high-calcium fluorite according to the claim 1, characterized in that, in the step 1), the content of the fraction with the grinding fineness of-0.074 mm in the ore powder accounts for 75-85% of the raw ore mass.
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| CN111701728B (en) * | 2020-06-30 | 2021-07-30 | 中南大学 | Selective flotation separation method for fluorite and calcium-containing gangue |
| CN112138873B (en) * | 2020-09-16 | 2021-05-18 | 东北大学 | Application of selective inhibitor EDTMPS in flotation and desilication of magnesite |
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| BR112013024257A2 (en) * | 2011-03-22 | 2016-12-27 | Cytec Tech Corp | method for reducing or preventing fouling in a wet process phosphoric acid production process |
| CN102294296B (en) * | 2011-06-30 | 2013-09-04 | 中蓝连海设计研究院 | Floatation and enrichment process for silicon-calcium mass type fluorite ores |
| US9440242B2 (en) * | 2013-10-01 | 2016-09-13 | Ecolab Usa Inc. | Frothers for mineral flotation |
| CA2931004A1 (en) * | 2013-12-20 | 2015-06-25 | Chemtreat, Inc. | Mineral ore flotation using a modifier to enhance the hydrophobicity of the target material |
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