Synthesis and application method of efficient mineral separation agent

Abstract

The invention discloses a synthesis and application method of an efficient mineral separation agent, and the synthesis method comprises the following steps: dissolving sodium isopropyl xanthate in water, and adding hydrochloric acid to adjust the pH value of the solution to 6-7; heating the solution to 60-90 DEG C, adding benzyl chloride to react, preserving heat for 3-4 hours, standing after the reaction is completed, taking an organic phase, adding a sodium chloride aqueous solution into the organic phase, stirring, standing again, and taking an organic phase; adding monoethylamine into the organic phase to react, then standing and separating to take the organic phase, neutralizing and washing the organic phase by using a sodium hydroxide solution, standing and separating to obtain an upper-layer ethionine ester crude product and a lower-layer sodium benzyl mercaptide, and washing the ethionine ester crude product to obtain an ethionine ester finished product; according to the application method, the obtained efficient mineral separation agent is applied to mineral separation of copper-molybdenum raw ores. According to the method, the types of added chemicals are reduced, the cost and the operation difficulty are reduced, and the recovery rate and the grade of copper and molybdenum are improved.

Description

Technical Field

[0001] The invention relates to the technical field of mineral processing, and in particular to a synthesis and application method of a high-efficiency mineral processing agent. Background Art

[0002] At present, my country's mineral resources have the characteristics of low ore grade, complex mineral distribution and difficult processing. The mined ore needs to be processed in the beneficiation plant before entering the smelter to separate different minerals and enrich them. The most widely used method is froth flotation. Flotation is a process of selecting mineral particles by using the differences in the physical and chemical properties of the mineral surface. This process is achieved by adding one or more beneficiation agents to cause the difference in wetting (floatability) of the surfaces of different mineral particles. Ethiocarbamate is a very important type of non-ferrous metal flotation agent with low dosage and little impact on environmental pollution. Its synthesis methods mainly include dimethyl sulfate method, dimethyl sulfate method, isothiocyanate alcoholysis method, chloroacetic acid esterification method, etc., but the dimethyl sulfate method will produce toxic gas, the dimethyl sulfate method has a low reactant yield and is not easy to separate, and the isothiocyanate alcoholysis method and chloroacetic acid esterification method produce more by-products, small market demand, and difficult to process. Summary of the invention

[0003] The purpose of the present invention is to provide a method for synthesizing and applying an efficient mineral processing agent to solve the problems existing in the background technology.

[0004] To achieve the above object, the present invention provides the following technical solutions:

[0005] A method for synthesizing an efficient mineral processing agent comprises the following steps:

[0006] 1) Dissolve sodium isopropyl xanthate in water at room temperature, and add hydrochloric acid to adjust the pH value of the solution to 6-7;

[0007] 2) The above solution was heated to 60-90°C, benzyl chloride was added for reaction and kept warm for 3-4 hours. After the reaction was completed, the temperature was lowered to room temperature, and the aqueous phase and the organic phase were separated by standing. The organic phase was taken, and the molar ratio of sodium isopropyl xanthate and benzyl chloride was 1: (1-1.3);

[0008] 3) adding a 3-5% sodium chloride aqueous solution to the organic phase and stirring, and then standing to separate into an aqueous phase and an organic phase, and taking the organic phase;

[0009] 4) adding monoethylamine to the organic phase of step 3) for reaction, wherein the molar ratio of the organic phase to the monoethylamine is 1:(1-1.05), the reaction temperature is 30-70° C., the reaction time is 3-6 h, and after completion, the reaction is allowed to stand and separate into an aqueous phase and an organic phase, and the organic phase is taken;

[0010] 5) using 10-12% sodium hydroxide solution to neutralize and wash the organic phase of step 4), and standing to separate to obtain the upper layer of crude ethylthiocarbamate and the lower layer of sodium benzyl mercaptan;

[0011] 6) The crude ethylthiocarbamate product of step 5) is subjected to material washing treatment to obtain the finished ethylthiocarbamate product, and the sodium benzyl mercaptan in the lower layer is subjected to desalting treatment using dilute hydrochloric acid, and then processed and purified to obtain the finished benzyl mercaptan product.

[0012] The application method of the high-efficiency mineral processing agent obtained by the above synthesis method comprises the following steps:

[0013] 1) grinding the copper-molybdenum ore and mixing with water to prepare a slurry with a solid content of 40-50%, then adding lime to adjust the pH value to 7-8, adding ethiocarbamate and a foaming agent to obtain a roughing concentrate and a roughing tailing;

[0014] 2) The rougher concentrate obtained above is subjected to secondary concentration to obtain copper-molybdenum concentrate, and the rougher tailings are subjected to a scavenging selection to obtain tailings, and ethiocarbamate and a foaming agent are added during the scavenging selection;

[0015] The amount of ethiocarbamate added is 0.02-0.03% of the copper-molybdenum ore, and the amount of the foaming agent added is 0.01-0.02% of the copper-molybdenum ore;

[0016] Preferably, the copper-molybdenum ore has a content of 78-85% below -400 mesh after grinding;

[0017] Preferably, the foaming agent is pine oil.

[0018] Preferably, the roughing temperature and the sweeping temperature are 10-26°C.

[0019] Compared with the prior art, the present invention has the following beneficial effects: the present invention adopts a combination of ethionamide and a foaming agent, reduces the types of added reagents, reduces the cost and operation difficulty, and improves the recovery rate and grade of copper and molybdenum. The copper recovery rate is more than 88.05%, the molybdenum recovery rate is more than 85.13%, the copper grade is more than 23%, and the molybdenum grade is more than 0.45%. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a schematic diagram of the synthesis process of the present invention.

[0021] Figure 2 It is a schematic diagram of the application process of the present invention. DETAILED DESCRIPTION

[0022] The technical solution will be described clearly and completely below in conjunction with the specific embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0023] Example 1

[0024] A method for synthesizing an efficient mineral processing agent comprises the following steps: 1) dissolving sodium isopropyl xanthate in water at room temperature, and adding hydrochloric acid to adjust the pH value of the solution to 7;

[0025] 2) The solution was heated to 90°C, benzyl chloride was added to react and kept warm for 4 hours. After the reaction was completed, the temperature was lowered to room temperature, and the aqueous phase and the organic phase were separated. The organic phase was taken, and the molar ratio of sodium isopropyl xanthate and benzyl chloride was 1:1.1;

[0026] 3)3) Adding 3% sodium chloride aqueous solution with the same volume concentration to the above organic phase and stirring, the mixture was allowed to stand again to separate into an aqueous phase and an organic phase, and the organic phase was taken;

[0027] 4) adding monoethylamine to the organic phase of step 3) to carry out reaction, the molar ratio of organic phase to monoethylamine is 1:1.05, the reaction temperature is 70°C, the reaction time is 3h, and after completion, the reaction is allowed to stand and separate into aqueous phase and organic phase, and the organic phase is taken;

[0028] 5) neutralizing and washing the organic phase of step 4) with a 12% sodium hydroxide solution, and standing to separate to obtain an upper layer of crude ethylthiocarbamate and a lower layer of sodium benzyl mercaptan;

[0029] 6) The crude ethylthiocarbamate product of step 5) is subjected to material washing treatment to obtain the finished ethylthiocarbamate product, and the sodium benzyl mercaptan in the lower layer is subjected to desalting treatment using dilute hydrochloric acid, and then processed and purified to obtain the finished benzyl mercaptan product.

[0030] The application method of the high-efficiency mineral processing agent obtained by the above synthesis method comprises the following steps:

[0031] 1) grinding the copper-molybdenum ore and mixing with water to prepare a slurry with a solid content of 50%, then adding lime to adjust the pH value to 8, adding ethiocarbamate and a foaming agent to obtain a roughing concentrate and a roughing tailing;

[0032] 2) The rougher concentrate obtained above is subjected to secondary concentration to obtain copper-molybdenum concentrate, and the rougher tailings are subjected to a scavenging selection to obtain tailings, and ethiocarbamate and a foaming agent are added during the scavenging selection;

[0033] The addition amount of the above-mentioned ethiocarbamate is 0.03% of the copper-molybdenum ore, the addition amount of the foaming agent is 0.02% of the copper-molybdenum ore, the content of the copper-molybdenum ore below -400 mesh after grinding is 85%, the roughing temperature and the scavenging temperature are 22°C, and the foaming agent is pine oil.

[0034] The copper recovery rate of this embodiment is 89.45%, the molybdenum recovery rate is above 86.05%, the copper grade is 24%, and the molybdenum grade is 0.52%.

[0035] Example 2

[0036] A method for synthesizing an efficient mineral processing agent comprises the following steps: 1) dissolving sodium isopropyl xanthate in water at room temperature, and adding hydrochloric acid to adjust the pH value of the solution to 6;

[0037] 2) The solution was heated to 60°C, benzyl chloride was added to react and kept warm for 3 hours. After the reaction was completed, the temperature was lowered to room temperature, and the aqueous phase and the organic phase were separated. The organic phase was taken, and the molar ratio of sodium isopropyl xanthate and benzyl chloride was 1:1;

[0038] 3) adding a 5% sodium chloride aqueous solution to the organic phase and stirring, and then standing to separate into an aqueous phase and an organic phase, and taking the organic phase;

[0039] 4) adding monoethylamine to the organic phase of step 3) to carry out reaction, the molar ratio of the organic phase to the monoethylamine is 1:1, the reaction temperature is 30° C., the reaction time is 6 h, and after completion, the reaction is allowed to stand and separate into an aqueous phase and an organic phase, and the organic phase is taken;

[0040] 5) neutralizing and washing the organic phase of step 4) with a 10% sodium hydroxide solution, and allowing to stand for separation to obtain an upper layer of crude ethylthiocarbamate and a lower layer of sodium benzyl mercaptan;

[0041] 6) The crude ethylthiocarbamate product of step 5) is subjected to material washing treatment to obtain the finished ethylthiocarbamate product, and the sodium benzyl mercaptan in the lower layer is subjected to desalting treatment using dilute hydrochloric acid, and then processed and purified to obtain the finished benzyl mercaptan product.

[0042] The application method of the high-efficiency mineral processing agent obtained by the above synthesis method comprises the following steps:

[0043] 1) grinding the copper-molybdenum ore and mixing with water to prepare a slurry with a solid content of 40%, then adding lime to adjust the pH value to 7, adding ethiocarbamate and a foaming agent to obtain a roughing concentrate and a roughing tailing;

[0044] 2) The rougher concentrate obtained above is subjected to secondary concentration to obtain copper-molybdenum concentrate, and the rougher tailings are subjected to a scavenging selection to obtain tailings, and ethiocarbamate and a foaming agent are added during the scavenging selection;

[0045] The addition amount of the above-mentioned ethiocarbamate is 0.02% of the copper-molybdenum ore, the addition amount of the foaming agent is 0.01% of the copper-molybdenum ore, the content of the copper-molybdenum ore below -400 mesh after grinding is 78%, the roughing temperature and the scavenging temperature are 26°C, and the foaming agent is pine oil.

[0046] In this embodiment, the copper recovery rate is 90.05%, the molybdenum recovery rate is 88.53%, the copper grade is 26%, and the molybdenum grade is 0.56%.

[0047] Example 3

[0048] A method for synthesizing an efficient mineral processing agent comprises the following steps:

[0049] 1) Dissolve sodium isopropyl xanthate in water at room temperature, and add hydrochloric acid to adjust the solution pH to 6.5; 2) Heat the solution to 80°C, add benzyl chloride to react and keep warm for 3.5 hours. After the reaction is completed, cool to room temperature, stand to separate the aqueous phase and the organic phase, and take the organic phase, the molar ratio of sodium isopropyl xanthate to benzyl chloride is 1:1.2;

[0050] 3) adding a 4% sodium chloride aqueous solution to the organic phase and stirring, and then standing to separate into an aqueous phase and an organic phase, and taking the organic phase;

[0051] 4) adding monoethylamine to the organic phase of step 3) to carry out reaction, the molar ratio of the organic phase to monoethylamine is 1:1.02, the reaction temperature is 50°C, the reaction time is 4h, and after completion, the reaction is allowed to stand and separate into an aqueous phase and an organic phase, and the organic phase is taken;

[0052] 5) neutralizing and washing the organic phase of step 4) with 11% sodium hydroxide solution, and standing to separate to obtain the crude ethylthiocarbamate product in the upper layer and sodium benzyl mercaptan in the lower layer;

[0053] 6) The crude ethylthiocarbamate product of step 5) is subjected to material washing treatment to obtain the finished ethylthiocarbamate product, and the sodium benzyl mercaptan in the lower layer is subjected to desalting treatment using dilute hydrochloric acid, and then processed and purified to obtain the finished benzyl mercaptan product.

[0054] The application method of the high-efficiency mineral processing agent obtained by the above synthesis method comprises the following steps:

[0055] 1) grinding the copper-molybdenum ore and mixing with water to prepare a slurry with a solid content of 45%, then adding lime to adjust the pH value to 7.5, adding ethiocarbamate and a foaming agent to obtain a roughing concentrate and a roughing tailing;

[0056] 2) The rougher concentrate obtained above is subjected to secondary concentration to obtain copper-molybdenum concentrate, and the rougher tailings are subjected to a scavenging selection to obtain tailings, and ethiocarbamate and a foaming agent are added during the scavenging selection;

[0057] The addition amount of the above-mentioned ethiocarbamate is 0.025% of the copper-molybdenum ore, the addition amount of the foaming agent is 0.016% of the copper-molybdenum ore, and the content of the copper-molybdenum ore below -400 mesh after grinding is 83%; the roughing temperature and the scavenging temperature are 20°C, and the foaming agent is pine oil.

[0058] The copper recovery rate of this embodiment is more than 89.87%, the molybdenum recovery rate is 85.16%, the copper grade is 23.6%, and the molybdenum grade is 0.48%.

[0059] Example 4

[0060] A method for synthesizing an efficient mineral processing agent comprises the following steps:

[0061] 1) Dissolve sodium isopropyl xanthate in water at room temperature, and add hydrochloric acid to adjust the solution pH to 8; 2) Heat the solution to 75°C, add benzyl chloride to react and keep warm for 3.8 hours. After the reaction is completed, cool to room temperature, stand to separate the aqueous phase and the organic phase, and take the organic phase, the molar ratio of sodium isopropyl xanthate to benzyl chloride is 1:1.15;

[0062] 3) adding a 3% sodium chloride aqueous solution to the organic phase and stirring, and then standing to separate into an aqueous phase and an organic phase, and taking the organic phase;

[0063] 4) adding monoethylamine to the organic phase of step 3) to carry out reaction, the molar ratio of the organic phase to monoethylamine is 1:1.01, the reaction temperature is 60°C, the reaction time is 5h, and after completion, the reaction is allowed to stand and separate into an aqueous phase and an organic phase, and the organic phase is taken;

[0064] 5) neutralizing and washing the organic phase of step 4) with a 10% sodium hydroxide solution, and allowing to stand for separation to obtain an upper layer of crude ethylthiocarbamate and a lower layer of sodium benzyl mercaptan;

[0065] 6) The crude ethylthiocarbamate product of step 5) is subjected to material washing treatment to obtain the finished ethylthiocarbamate product, and the sodium benzyl mercaptan in the lower layer is subjected to desalting treatment using dilute hydrochloric acid, and then processed and purified to obtain the finished benzyl mercaptan product.

[0066] The application method of the high-efficiency mineral processing agent obtained by the above synthesis method comprises the following steps:

[0067] 1) grinding the copper-molybdenum ore and mixing with water to prepare a slurry with a solid content of 40%, then adding lime to adjust the pH value to 7, adding ethiocarbamate and a foaming agent to obtain a roughing concentrate and a roughing tailing;

[0068] 2) The rougher concentrate obtained above is subjected to secondary concentration to obtain copper-molybdenum concentrate, and the rougher tailings are subjected to a scavenging selection to obtain tailings, and ethiocarbamate and a foaming agent are added during the scavenging selection;

[0069] The addition amount of the above-mentioned ethiocarbamate is 0.02% of the copper-molybdenum ore, the addition amount of the foaming agent is 0.016% of the copper-molybdenum ore, and the content of the copper-molybdenum ore below -400 mesh after grinding is 85%; the roughing temperature and the scavenging temperature are 10°C, and the foaming agent is pine oil.

[0070] In this embodiment, the copper recovery rate is 88.35%, the molybdenum recovery rate is above 86.23%, the copper grade is 26%, and the molybdenum grade is 0.64%.

Claims

1. A method for synthesizing an efficient mineral processing agent, characterized in that: The following steps are involved: 1) Dissolve sodium isopropyl xanthate in water at room temperature, and add hydrochloric acid to adjust the pH value of the solution to 6-7; 2) The above solution was heated to 60-90°C, benzyl chloride was added for reaction and kept warm for 3-4 hours. After the reaction was completed, the temperature was lowered to room temperature, and the aqueous phase and the organic phase were separated by standing. The organic phase was taken, and the molar ratio of sodium isopropyl xanthate and benzyl chloride was 1: (1-1.3); 3) adding a 3-5% sodium chloride aqueous solution to the organic phase and stirring, and then standing to separate into an aqueous phase and an organic phase, and taking the organic phase; 4) adding monoethylamine to the organic phase of step 3) for reaction, wherein the molar ratio of the organic phase to the monoethylamine is 1:(1-1.05), the reaction temperature is 30-70° C., the reaction time is 3-6 h, and after completion, the reaction is allowed to stand and separate into an aqueous phase and an organic phase, and the organic phase is taken; 5) using 10-12% sodium hydroxide solution to neutralize and wash the organic phase of step 4), and standing to separate to obtain the upper layer of crude ethylthiocarbamate and the lower layer of sodium benzyl mercaptan; 6) The crude ethylthiocarbamate product of step 5) is subjected to material washing treatment to obtain the finished ethylthiocarbamate product, and the sodium benzyl mercaptan in the lower layer is subjected to desalting treatment using dilute hydrochloric acid, and then processed and purified to obtain the finished benzyl mercaptan product.

2. The application method of the high-efficiency mineral processing agent obtained by the synthesis method according to claim 1, characterized in that: The following steps are involved: 1) grinding the copper-molybdenum ore and mixing with water to prepare a slurry with a solid content of 40-50%, then adding lime to adjust the pH value to 7-8, adding ethiocarbamate and a foaming agent to obtain a roughing concentrate and a roughing tailing; 2) The rougher concentrate obtained above is subjected to secondary concentration to obtain copper-molybdenum concentrate, and the rougher tailings are subjected to a scavenging selection to obtain tailings, and ethiocarbamate and a foaming agent are added during the scavenging selection; The addition amount of the above-mentioned ethionamide is 0.02-0.03% of the copper-molybdenum ore, and the addition amount of the foaming agent is 0.01-0.02% of the copper-molybdenum ore.

3. The application method according to claim 2, characterized in that: The content of copper-molybdenum ore below -400 mesh after grinding is 78-85%.

4. The application method according to claim 2, characterized in that: The foaming agent is pine oil.

5. The application method according to claim 2, characterized in that: The roughing temperature and the sweeping temperature are 10-26°C.

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