Flotation collector and preparation method thereof, combined flotation agent and application thereof

Abstract

The present invention discloses a flotation collector, a preparation method thereof, a combined flotation agent, and its application. The flotation collector comprises a dithiophosphate and a dimethylphenyl dithiophosphate having a specific structure. The combined flotation agent is used for flotation of nickel sulfide ore containing magnesium gangue, and comprises 30 to 60 parts of the flotation collector, 20 to 30 parts of a frother, 5 to 10 parts of an inhibitor, and 10 to 20 parts of water. The flotation collector of the present invention can significantly improve the collector's ability to capture pentlandite, effectively improve the problem of entrainment of magnesium silicate gangue in pentlandite concentrate, and reduce the amount of frother used. The combined flotation agent of the present invention increases the bubble capture capacity and the dispersibility of the salt agent in the solution, while increasing the stability of the foam and the high selectivity for nickel ore, thereby achieving the separation and flotation of nickel ore and serpentine gangue minerals, reducing the amount of flotation agent used and achieving the goal of increasing the concentrate yield.

Description

Technical Field

[0001] The present invention relates to the technical field of mineral processing and flotation, and in particular to a flotation collector for nickel sulfide ore containing magnesia gangue, a preparation method thereof, and a combined flotation agent and application thereof. Background Art

[0002] Nickel, known as the "vitamin" of industry, is an important raw material for nonferrous metals. It plays a significant role in industrial production, including alloys, electroplating, catalysis, batteries, dyes, and ceramics. Currently, most nickel sulfide ores in my country are produced from peridotite-facies basic rock deposits. The ore contains a high content of magnesium silicate gangue minerals, and magnesium silicate gangue (serpentine being a typical example) significantly interferes with flotation enrichment. Gangue minerals such as serpentine are easily argillized and adhere to the surface of pentlandite, increasing the MgO content in nickel concentrate. This creates a series of problems for subsequent concentrate smelting and generates significant energy consumption. There is an urgent need to develop efficient flotation methods to address this common problem.

[0003] The collectors commonly used for pentlandite at present are black powder agents, among which No. 25 black powder sodium dimethylphenyl dithiophosphate is more widely used. However, this type of collector has low selectivity for nickel, and black powder collectors have strong foaming properties, which causes serpentine gangue to be mixed in the flotation foam, reducing the nickel grade of the concentrate. Summary of the Invention

[0004] The present invention provides a flotation collector and a preparation method thereof, as well as a combined flotation agent and application thereof, which are used to solve the technical problems of low collecting capacity and selectivity of existing collectors, and enable effective flotation separation of nickel sulfide ore containing magnesium silicate gangue.

[0005] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0006] A flotation collector, characterized in that the collector comprises dithiophosphate and dimethylphenyl dithiophosphate;

[0007] The dithiophosphate includes at least one compound having the chemical structure shown in formula (1):

[0008] In the formula, R is a C1-C4 alkyl group; M is H, Na or K.

[0009] The design idea of ​​the above technical solution is that, as mentioned in the background technology, since the single collector dimethylphenol dithiophosphate has a strong foaming ability, it makes it easy for gangue minerals such as serpentine to be mixed in the flotation concentrate. Therefore, although it has the ability to collect pentlandite, its collection ability and selectivity for nickel are not high. However, the present invention innovatively discovered that when dimethylphenol dithiophosphate is mixed with dithiophosphate having the chemical structure of formula (1) and used as a collector for flotation of nickel sulfide ore, the two have a synergistic effect, which can significantly improve the collector's collection ability for pentlandite, and can also effectively improve the problem of entrainment of magnesium silicate gangue in pentlandite concentrate. Dicresol-based dithiophosphates have strong foaming properties and collecting abilities, while dithiophosphates have better selectivity. On the one hand, the two collectors with strong collecting abilities and good selectivity co-adsorb in different areas of the mineral surface, achieving functional complementarity. On the other hand, since the structures of dicresol-based dithiophosphates and dithiophosphates are similar, the more similar their spatial conformations are, the stronger the self-synergistic effect. Furthermore, since both dithiophosphates and dicresol-based dithiophosphates are ionic sulfide ore collectors, and the dithiophosphates proposed in the present invention have certain foaming properties, the amount of foaming agent used is reduced.

[0010] In the flotation collector of the present invention, the oxygen atom in the dithiophosphate molecule is located between the benzene ring and the methyl group, forming a new -OCH3 group. The movement of the oxygen atom causes the benzene ring and the phosphorus-sulfur double bond to form a conjugate, and the lone electron pair on the oxygen atom can be transferred between the benzene ring and the phosphorus-sulfur double bond through the conjugation effect. It is well known that the oxygen in the chelating agent structure acts as an electron donor atom and therefore tends to form a stable metal chelate ring with most elements, thereby increasing the electron cloud density of the polar group of the collector. The electron donating effect of the -OCH3 group and the conjugated system formed by the -OCH3 group and the benzene ring are the keys to improving the selective flotation of pentlandite by the collector.

[0011] In the flotation collector of the present invention, the short-chain C1-C4 alkyl groups in the dithiophosphate molecule are key to reducing the collector's foam entrainment in magnesium-containing silicate gangue. The carbon atoms on the benzene ring possess sp2 hybrid orbitals, while the carbon atoms on the saturated alkyl group possess sp3 hybrid orbitals. The electron-donating effect of the sp3 hybrid orbitals on the saturated alkyl group also increases the electron cloud density at the collector's chelating site, resulting in stronger collection performance. Furthermore, replacing the toluene group with a saturated alkyl group alters the tightness of the agent's adsorption. The benzene ring forms an electron sink on the surface and tends to lie horizontally on the mineral surface, while the linear chain tends to lie perpendicularly on the mineral surface, resulting in better adsorption. Furthermore, compared to the benzene ring substituents, the short-chain alkyl group significantly reduces the molecule's foaming ability.

[0012] As a further preferred embodiment of the above technical solution, the mass ratio of the dithiophosphate to the dimethylphenyl dithiophosphate is (1-30):(60-80).

[0013] As a further preferred embodiment of the above technical solution, the mass ratio of the dithiophosphate to the dicresol dithiophosphate is (10-30):(60-80). Since dithiophosphate has better selectivity for pentlandite and almost no capture ability for serpentine, the inventors have found that within a certain ratio range disclosed in the present invention, as the proportion of dithiophosphate increases, a concentrate with a higher nickel grade can be obtained when flotation separation of the two can be carried out.

[0014] Based on the same technical concept, the present invention also provides a method for preparing the above-mentioned nickel sulfide ore collector, comprising the following operations: preparing the dithiophosphate, and mixing the dithiophosphate with dimethylphenyl dithiophosphate;

[0015] The preparation method of the dithiophosphate comprises the following steps:

[0016] (1) Analytical pure anisole and phosphorus pentasulfide were heated to 155° C. to 160° C. under a protective atmosphere and refluxed until the reaction was complete, and the resulting precipitate was dried in vacuum to obtain an intermediate product;

[0017] (2) Na is stirred in alcohol ROH until it is completely dissolved to obtain a solution, the intermediate product is added to the solution, and the solution is heated to 70-100° C. to reflux and react until the reaction is complete, and the solid is separated to obtain the dithiophosphate.

[0018] Based on the same technical concept, the present invention also provides a combined flotation reagent comprising the following components in parts by weight:

[0019] 30-60 parts of collector, 20-30 parts of foaming agent, 5-10 parts of inhibitor and 10-20 parts of water;

[0020] The collector is the above-mentioned flotation collector or the flotation collector prepared by the above-mentioned preparation method.

[0021] The design concept of the above technical solution is that the present invention uses dithiophosphates and dimethyldithiophosphates as collectors, and forms a combined flotation agent with a frother, an inhibitor, and water. In the combined flotation agent, the dithiophosphates can form metal chelates with nickel, which are highly selectively adsorbed on the surface of the metallic nickel. The mixing of the frother and collector increases the bubble capture capacity. The combined flotation agent not only improves the dispersibility of the salt reagent in the solution, but also increases the stability of the foam and the high selectivity for nickel ores. Within a suitable range, it plays a role in the separation and flotation of nickel ore and serpentine gangue minerals, reducing the amount of flotation agent used and achieving the goal of increasing the concentrate yield.

[0022] As a further preferred embodiment of the above technical solution, the foaming agent includes methyl isobutyl carbinol and polyethylene glycol dibenzyl ether, and the mass ratio of methyl isobutyl carbinol and polyethylene glycol dibenzyl ether is (1-60): (1-80), and more preferably (40-50): (50-60). Methyl isobutyl carbinol is a commonly used flotation foaming agent with low price, and polyethylene glycol dibenzyl ether is an ether foaming agent. The foam produced is moderate in size and has good foam stability. When used for sulfide ore flotation, the dosage is small and the effect is good. The methyl isobutyl carbinol foaming agent of the alcohol type has stable foaming performance, strong foaming ability, non-sticky foam, and fast defoaming, while the polyethylene glycol dibenzyl ether foaming agent of the ether type is applicable to a wide pH range. The mixed use of the two forms a tightly bound adsorption layer due to the synergistic adsorption of the long and short chains, which can enhance the adaptability of the foaming agent and stabilize the flotation foam layer.

[0023] As a further preferred embodiment of the above technical solution, the inhibitor includes citric acid. Citric acid is an organic inhibitor for serpentine, and compared with commonly used inorganic inhibitors, it has the advantages of being inexpensive, easily degradable, and environmentally friendly.

[0024] Based on the same technical concept, the present invention also provides an application of the above-mentioned combined flotation reagent, wherein the combined flotation reagent is used for flotation of nickel sulfide ore containing magnesium gangue.

[0025] As a further preferred embodiment of the above technical solution, when the combined flotation reagent is used to flotate nickel sulfide ore containing magnesium gangue, the pH of the slurry during the flotation stage is 5 to 10, and more preferably 6 to 7. The inventors have found through research and experiments that when the slurry is within the pH range of this preferred solution, the flotation effect of the combined flotation reagent of the present invention can be further improved, thereby enhancing the selective separation of pentlandite from magnesium silicate gangue.

[0026] As a further preferred embodiment of the above technical solution, when the combined flotation reagent is used to flotate nickel sulfide ore containing magnesium gangue, the dosage of the combined flotation reagent is 100-400 g / t. In the present invention, the dosage of the reagent can be adjusted according to specific needs based on the flotation effect and economic benefits.

[0027] As a further preferred embodiment of the above technical solution, when the combined flotation reagent is used to carry out flotation operation on nickel sulfide ore containing magnesium gangue, the rotation speed of the flotation machine in the flotation stage is 1600-2000 r / min, and more preferably 1800-1950 r / min. The rotation speed is selected based on the commonly used flotation speed. In the nickel sulfide ore flotation pulp system, the surface of pentlandite is negatively charged, while the surface of serpentine is positively charged. The positively charged serpentine mud covers the pentlandite through heterogeneous coagulation. The inventors have found through research and experiments that increasing the rotation speed within a certain rotation speed range disclosed in the present invention can enhance dispersion. At the same time, the increase in the rotation speed allows more particles to achieve the effect of suspension from the bottom, and the probability of collision and adhesion with bubbles is increased.

[0028] Compared with the prior art, the advantages of the present invention are:

[0029] (1) When the flotation collector of the present invention is used to float nickel sulfide ore, the collector can significantly improve the collection ability of pentlandite, effectively improve the entrainment problem of magnesium silicate gangue in the pentlandite concentrate, and reduce the amount of foaming agent used;

[0030] (2) The combined flotation reagent of the present invention increases the bubble capture capacity and the dispersibility of the salt reagent in the solution, while increasing the stability of the foam and the high selectivity for nickel ore, thereby playing a role in the separation and flotation of nickel ore and serpentine gangue minerals, reducing the amount of flotation reagent used and achieving the goal of increasing the concentrate yield. BRIEF DESCRIPTION OF THE DRAWINGS

[0031] Figure 1 1 is a flotation flow chart of each embodiment. DETAILED DESCRIPTION

[0032] The present invention is further described in detail below with reference to specific examples. The grades of the various components of the nickel sulfide ores used in the examples and comparative examples are shown in Table 1 below.

[0033] Table 1. Composition of nickel sulfide ores used in various examples and comparative examples

[0034]

[0035] Example 1:

[0036] The flotation collector of this embodiment is composed of 10 parts by mass of dithiophosphate and 80 parts by mass of dimethylphenyl dithiophosphate.

[0037] Among them, dithiophosphate is a compound having the chemical structure shown in formula (1):

[0038] In the formula, R is a C3 alkyl group; M is Na;

[0039] Dimethylphenyl dithiophosphate is a compound having the chemical structure shown in formula (2);

[0040] In the formula, R is a methyl group of C1; M is Na.

[0041] The combined flotation reagent of this embodiment includes the following components in parts by weight:

[0042] 10 parts of dithiophosphate, 80 parts of dimethylphenyl dithiophosphate, 10 parts of foaming agent methyl isobutyl carbinol, 10 parts of foaming agent polyethylene glycol dibenzyl ether, 20 parts of inhibitor citric acid, 10 parts of water.

[0043] The combined flotation reagent of this embodiment is prepared by the following steps:

[0044] Prepare dithiophosphate, add dimethylphenyl dithiophosphate in proportion, then add frother, inhibitor and water in proportion, stir and mix at room temperature for 0.5 hours to obtain the combined flotation reagent of this embodiment.

[0045] Wherein, the preparation method of dithiophosphate is:

[0046] Analytical pure anisole (270 g, 2.5 mol) and phosphorus pentasulfide (111 g, 0.25 mol) were heated to reflux under nitrogen for 6 hours. The heating temperature was controlled between 155°C and 160°C, and the reflux rate was maintained at 1 drop of liquid per 6 to 10 seconds. After the reaction, the resulting precipitate was dried in vacuo to obtain the intermediate product.

[0047] A small piece of sodium (0.43 g, 18.7 mmol) was dissolved in propanol C3H8O (30 cm -3 ) and stirred at 0°C until completely dissolved. The intermediate product (3.78 g, 9.35 mmol) was added to the solution and heated to reflux at 70-100°C, maintaining a reflux rate of one drop per 6-10 seconds. The reaction time was approximately 1 hour. After the reaction, the reaction mixture was cooled to room temperature and the resulting colorless solution was filtered through a small pad of celite. The solvent was removed under reduced pressure to obtain a white solid (4.98 g, 98.5%), which was the dithiophosphate of this example.

[0048] The combined flotation reagent of this embodiment can be used to perform flotation operations on nickel sulfide ore containing magnesium gangue, and the flotation machine speed is controlled at 1950 r / min.

[0049] Example 2:

[0050] The flotation collector of this embodiment is composed of 20 parts by mass of dithiophosphate and 70 parts by mass of dimethylphenyl dithiophosphate.

[0051] Among them, dithiophosphate is a compound having the chemical structure shown in formula (1):

[0052] In the formula, R is a C3 alkyl group; M is Na;

[0053] Dimethylphenyl dithiophosphate is a compound having the chemical structure shown in formula (2);

[0054] In the formula, R is a methyl group of C1; M is Na.

[0055] The combined flotation reagent of this embodiment includes the following components in parts by weight:

[0056] 20 parts of dithiophosphate, 70 parts of dimethylphenyl dithiophosphate, 10 parts of foaming agent methyl isobutyl carbinol, 10 parts of foaming agent polyethylene glycol dibenzyl ether, 20 parts of inhibitor citric acid, 10 parts of water.

[0057] The preparation method of the combined flotation reagent of this embodiment is the same as that of Example 1.

[0058] The combined flotation reagent of this embodiment can be used to perform flotation operations on nickel sulfide ore containing magnesium gangue, and the flotation machine speed is controlled at 1800 r / min.

[0059] Example 3:

[0060] The flotation collector of this embodiment is composed of 30 parts by mass of dithiophosphate and 60 parts by mass of dimethylphenyl dithiophosphate.

[0061] Among them, dithiophosphate is a compound having the chemical structure shown in formula (1):

[0062] In the formula, R is a C3 alkyl group; M is Na;

[0063] Dimethylphenyl dithiophosphate is a compound having the chemical structure shown in formula (2);

[0064] In the formula, R is a methyl group of C1; M is Na.

[0065] The combined flotation reagent of this embodiment includes the following components in parts by weight:

[0066] 30 parts of dithiophosphate, 60 parts of dimethylphenyl dithiophosphate, 10 parts of foaming agent methyl isobutyl carbinol, 10 parts of foaming agent polyethylene glycol dibenzyl ether, 20 parts of inhibitor citric acid, 10 parts of water.

[0067] The preparation method of the combined flotation reagent of this embodiment is the same as that of Example 1.

[0068] The combined flotation reagent of this embodiment can be used to perform flotation operations on nickel sulfide ore containing magnesium gangue, and the flotation machine speed is controlled at 1850 r / min.

[0069] Example 4:

[0070] The flotation collector of this embodiment is composed of 30 parts by mass of dithiophosphate and 60 parts by mass of dimethylphenyl dithiophosphate.

[0071] Among them, dithiophosphate is a compound having the chemical structure shown in formula (1):

[0072] In the formula, R is a C3 alkyl group; M is Na;

[0073] Dimethylphenyl dithiophosphate is a compound having the chemical structure shown in formula (2);

[0074] In the formula, R is a methyl group of C1; M is Na.

[0075] The combined flotation reagent of this embodiment includes the following components in parts by weight:

[0076] 30 parts of dithiophosphate, 60 parts of dimethylphenyl dithiophosphate, 15 parts of foaming agent methyl isobutyl carbinol, 5 parts of foaming agent polyethylene glycol dibenzyl ether, 20 parts of inhibitor citric acid, 10 parts of water.

[0077] The preparation method of the combined flotation reagent of this embodiment is the same as that of Example 1.

[0078] The combined flotation reagent of this embodiment can be used to perform flotation operations on nickel sulfide ore containing magnesium gangue, and the flotation machine speed is controlled at 1850 r / min.

[0079] Example 5:

[0080] The flotation collector of this embodiment is composed of 30 parts by mass of dithiophosphate and 60 parts by mass of dimethylphenyl dithiophosphate.

[0081] Among them, dithiophosphate is a compound having the chemical structure shown in formula (1):

[0082] In the formula, R is a C3 alkyl group; M is Na;

[0083] Dimethylphenyl dithiophosphate is a compound having the chemical structure shown in formula (2);

[0084] In the formula, R is a methyl group of C1; M is Na.

[0085] The combined flotation reagent of this embodiment includes the following components in parts by weight:

[0086] 30 parts of dithiophosphate, 60 parts of dimethylphenyl dithiophosphate, 15 parts of foaming agent methyl isobutyl carbinol, 15 parts of foaming agent polyethylene glycol dibenzyl ether, 20 parts of inhibitor citric acid, 10 parts of water.

[0087] The preparation method of the combined flotation reagent of this embodiment is the same as that of Example 1.

[0088] The combined flotation reagent of this embodiment can be used to perform flotation operations on nickel sulfide ore containing magnesium gangue, and the flotation machine speed is controlled at 1850 r / min.

[0089] Comparative Example 1:

[0090] The combined flotation reagent of this comparative example is different from that of Example 3 in that the dithiophosphate and dicresylated dithiophosphate in Example 3 are replaced by an equal amount of dicresylated dithiophosphate in this comparative example.

[0091] Comparative Example 2:

[0092] The combined flotation reagent of this comparative example is different from that of Example 4 in that the dithiophosphate and dicresylated dithiophosphate in Example 3 are replaced by an equal amount of dicresylated dithiophosphate in this comparative example.

[0093] Comparative Example 3:

[0094] The combined flotation reagent of this comparative example is compared with the combined flotation reagent of Example 3; the only difference is that the component ratio of dithiophosphate to dimethylphenyl dithiophosphate in this comparative example is 40:50.

[0095] Example 6:

[0096] Except for the flotation machine speed, which is different from that in Example 3, all other aspects are the same as those in Example 3. The closed-circuit flotation test results at different speeds are shown in Table 2 below.

[0097] Table 2. Flotation recovery at different rotation speeds

[0098] Flotation machine speed / r / min Total concentrate / % Tailings / % 1600 84.54 15.46 1750 88.11 11.89 2000 89.07 10.93

[0099] Comparing the results in Table 2 and Example 3, it can be seen that when the combined flotation reagent is used to flotate the nickel sulfide ore containing magnesium gangue, the speed of the flotation machine during the flotation stage is 1600-2000 r / min, and more preferably 1800-1950 r / min.

[0100] The combined flotation reagents of each embodiment and comparative example are used to carry out flotation of nickel sulfide ore containing magnesium gangue. The flotation process is as follows: Figure 1As shown, the specific steps include:

[0101] (1) Grinding: Each closed-circuit flotation process is performed until 70% of the mineral particles have a size of less than 0.074 mm.

[0102] (2) In the first stage flotation operation, different proportions of reagents in the embodiment were added, and the order of adding the reagents was inhibitor, collector, and frother, and then slurry was adjusted to control the pH of the slurry to 6-7. The slurry was stirred for 2-5 minutes, and the speed of the flotation machine was controlled within 1800-1950 r / min. After the stirring and slurry adjustment was completed, scavenging was carried out for 10 minutes, concentrating was carried out for 8 minutes, and concentrating was carried out for 4 minutes to obtain concentrate 1.

[0103] (3) In the second-stage flotation operation, the first-stage slurry is re-ground to reduce the particle size of 85% of the minerals to less than 0.074 mm. After the slurry is uniform, the slurry is mixed with chemicals for about 7 minutes. After the mixing is completed, scavenging is carried out for 10 minutes, and then three concentrations are carried out to obtain concentrate 2; after three scavengings, tailings are obtained. The closed-circuit flotation process produces three products: concentrate 1, concentrate 2, and tailings.

[0104] (4) Results and Analysis. Each closed-circuit flotation cycle reached equilibrium after two cycles. The results of the example are the average of the results obtained after three cycles. Two closed-circuit flotation experiments were conducted for each implementation case. The grade / recovery rate of concentrate 1 and concentrate 2, as well as the grade of the tailings, obtained from the two experiments are referenced.

[0105] The closed-circuit flotation test results of each embodiment and comparative example are shown in Table 3 below.

[0106] Table 3 Closed circuit flotation test results of various embodiments and comparative examples

[0107]

[0108]

[0109]

[0110] From the flotation results of the various examples, it can be seen that the order of flotation effects is Example 3 > Example 2 > Example 4 > Example 5 > Example 1 > Comparative Example 3 > Comparative Example 1 > Comparative Example 2.

[0111] In Example 1-3, the proportion of dithiophosphate in the collector was gradually increased, and the flotation results showed that increasing the proportion of dithiophosphate had a better effect on flotation.

[0112] Comparing Examples 1-3 with Comparative Example 3, Example 3 > Example 2 > Example 1 > Comparative Example 3. The mass ratio of dithiophosphate to dimethylphenyl dithiophosphate exceeds the range of (1-30): (60-80), failing to achieve the flotation effect within the preferred mass ratio range.

[0113] Comparing Examples 1-5 with Comparative Examples 1 and 2, the flotation results are as follows: Example 3 > Example 2 > Example 4 > Example 5 > Example 1 > Comparative Example 1 > Comparative Example 2. It can be seen that the combined use of dimethylol dithiophosphates on the basis of dimethylol dithiophosphates can achieve a synergistic effect, achieving better flotation results than a single dimethylol dithiophosphate, and can also reduce the magnesium content in the concentrate.

[0114] Comparing Examples 3 and 4 with Comparative Examples 1 and 2, it can be seen that even if the ratio of the flotation frother is changed, the combination of dicresol dithiophosphate and dithiophosphate can achieve better results than single dicresol dithiophosphate.

[0115] The above is only a preferred embodiment of the present invention, and the scope of protection of the present invention is not limited to the above embodiment. For those skilled in the art, improvements and modifications obtained without departing from the technical concept of the present invention should also be considered as the scope of protection of the present invention.

Claims

1. A flotation collector for nickel sulfide ore containing magnesia gangue, characterized in that: The collector includes dithiophosphate and dimethylphenyl dithiophosphate; The dithiophosphate includes at least one compound having the chemical structure shown in formula (1): ; wherein R is a C1~C4 alkyl group; M is H, Na or K; the mass ratio of the dithiophosphate to the dimethylphenyl dithiophosphate is (1~30): (60~80).

2. The flotation collector according to claim 1, characterized in that The mass ratio of the dithiophosphate to the dimethylphenyl dithiophosphate is (10-30): (60-80).

3. A method for preparing a flotation collector according to claim 1 or 2, characterized in that: The method comprises the following operations: preparing the dithiophosphate, and mixing the dithiophosphate with dimethylphenyl dithiophosphate; The preparation method of the dithiophosphate comprises the following steps: (1) Analytical pure anisole and phosphorus pentasulfide were heated to 155°C~160°C under a protective atmosphere and refluxed until the reaction was complete. The resulting precipitate was dried in a vacuum to obtain an intermediate product; (2) Na or K is stirred in alcohol ROH until completely dissolved to obtain a solution, the intermediate product is added to the solution, and the solution is heated to 70-100° C. to reflux until the reaction is complete, and the solid is separated to obtain the dithiophosphate.

4. A combined flotation reagent, characterized in that: The composition comprises the following components in parts by weight: 30-60 parts of collector, 20-30 parts of foaming agent, 5-10 parts of inhibitor and 10-20 parts of water; The collector is the flotation collector according to any one of claims 1 to 2 or the flotation collector prepared by the preparation method according to claim 3.

5. The combined flotation reagent according to claim 4, characterized in that: The foaming agent comprises methyl isobutyl carbinol and polyethylene glycol dibenzyl ether, and the mass ratio of the methyl isobutyl carbinol to the polyethylene glycol dibenzyl ether is (1-60): (1-80).

6. The combined flotation reagent according to claim 4, characterized in that: The inhibitor includes citric acid.

7. Use of the combined flotation reagent according to any one of claims 4 to 6, characterized in that: The combined flotation reagent is used for flotation of nickel sulfide ore containing magnesium gangue, and the pH value of the ore pulp during the flotation stage is 5-10.

8. The use of the combined flotation reagent according to claim 7, characterized in that: When the combined flotation reagent is used to perform flotation on nickel sulfide ore containing magnesium gangue, the rotation speed of the flotation machine during the flotation stage is 1600-2000 r / min.

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