Efficient collecting agent applied to iron ore reverse flotation desulfurization and preparation method and application of efficient collecting agent

By preparing dimercapto ethers or thioethers as collectors, the problems of insufficient collection capacity and irritating odor of traditional collectors for magnetic pyrite have been solved, achieving efficient and environmentally friendly desulfurization of iron ore.

CN120961310APending Publication Date: 2025-11-18NANJING MEISHAN METALLURGY DEV
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202511252100.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-09-03
Publication Date
2025-11-18

AI Technical Summary

Technical Problem

In existing iron ore reverse flotation desulfurization technologies, traditional collectors are insufficient for collecting magnetic pyrite and have a strong pungent odor, which affects the environment and workers' health.

Method used

Dithiol compounds were used as collectors to prepare dithiol ethers or thioethers through nucleophilic substitution reactions and alkaline hydrolysis, thereby enhancing the collection ability of pyrite. The high-purity collectors were then purified by silica gel column chromatography.

Benefits of technology

It significantly improves the harvesting efficiency of pyrite, reduces the sulfur content in iron concentrate, reduces VOC emissions, improves the working environment, and meets environmental protection requirements.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure SMS_1
    Figure SMS_1
  • Figure SMS_2
    Figure SMS_2
  • Figure SMS_3
    Figure SMS_3
Patent Text Reader

Abstract

The invention discloses an efficient collecting agent applied to iron ore reverse flotation desulfurization and a preparation method and application of the efficient collecting agent, and particularly relates to the technical field of beneficiation reagents. The efficient collecting agent is a dimercapto compound, sulfur atoms in molecules of the dimercapto compound show high electron donating capacity, and when the sulfur atoms react with metal ions, the sulfur atoms in the molecules of the dimercapto compound show high electron donating capacity; sulfur atoms form coordinate bonds with metal ions by means of lone pair electrons, and the dissociation tendency of the metal ions is remarkably reduced in the process, so that the overall stability of the formed complex is improved. The disulfhydryl compound can generate insoluble black complex precipitates with Fe < 2 + > ions in ore pulp, but cannot generate precipitates with Fe < 3 + > ions, so that the disulfhydryl agent has very strong collecting capacity on pyrite and cannot react with hematite, ether bonds are introduced into the disulfhydryl compound, the solubility, surface tension and molecular activity of the disulfhydryl compound can be increased, and the disulfhydryl compound can be used for collecting the hematite. The collecting capacity is enhanced, and effective separation of pyrite and hematite can be achieved by using dimercapto ether as the collecting agent.
Need to check novelty before this filing date? Find Prior Art

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of beneficiation reagents, and specifically relates to a high-efficiency collecting agent for iron ore reverse flotation desulfurization and a preparation method and application thereof. BACKGROUND

[0002] Iron ore is an important metal mineral resource in industrial production and is widely used in the fields of metallurgy, construction, machinery and the like. However, the iron ore often contains different amounts of sulfur elements, especially sulfides in the form of pyrite, which brings certain challenges to the purification and subsequent processing of the iron ore. The iron ore with a too high sulfur content will produce serious air pollution in the smelting process, which not only affects the quality of steel products but also causes environmental pollution and energy waste. Therefore, how to efficiently and economically remove the sulfur elements in the ore in the iron ore processing process has become an important issue to be solved in the current mineral smelting industry.

[0003] The reverse flotation desulfurization technology is a common iron ore desulfurization process, which separates pyrite from iron ore by adjusting the interaction between the ore and the flotation reagent to achieve the purpose of removing sulfur elements. The combined reagent for desulfurization of iron concentrate powder under alkaline conditions and the method for desulfurization of pyrrhotite by using the same

CN112871458A

CN103495506A

[0004] In recent years, with the mineral resources becoming increasingly poor, thin and miscellaneous, people's requirements for the comprehensive recovery rate of resources and the separation effect of flotation are increasing. The flotation separation of complex sulfide ore is becoming increasingly important, and the research on finding new and more effective collectors has become an important direction of sulfide ore flotation separation. SUMMARY

[0005] The present application is just for the problems existing in the prior art, and provides a high-efficiency collector for pyrite applied to desulfurization of iron ore reverse flotation and a preparation method thereof, which can overcome the problem of weak collecting ability of conventional collectors for magnetic pyrite, provides a new technology for efficient development of high-sulfur pyrite resources, and provides a brand-new direction for development of high-efficiency pyrite collectors.

[0006] To achieve the above-mentioned purpose, the present application provides the following technical scheme:

[0007] A high-efficiency collector for pyrite applied to desulfurization of iron ore reverse flotation has the structure of formula 1:

[0008]

[0009] Formula 1

[0010] In formula 1, R is an O or S atom, R1 and R2 are any one of C1-C6 short-chain alkyl or phenyl groups.

[0011] As a preferred technical scheme of the present application, R1 and R2 are any one of propylene, butylene or phenyl groups.

[0012] A preparation method of a high-efficiency collector for pyrite applied to desulfurization of iron ore reverse flotation, the preparation method comprising the following steps:

[0013] When R in formula 1 is an O atom, the steps are as follows:

[0014] Step 1a, dichloroalkyl ether or dibromodiphenyl ether is mixed with sodium hydrosulfide in dimethylformamide (DMF) and then the mixed solution is heated to reflux, nitrogen is introduced for protection during the heating and reflux process, a nucleophilic substitution reaction is carried out, and a mixed solution containing dimercapto ether is obtained;

[0015] Step 2a, after the mixed solution containing dimercapto ether is cooled, the pH is adjusted to 7-8 with dilute hydrochloric acid, then the mixed solution of dimercapto ether is extracted with ethyl acetate and dried with anhydrous sodium sulfate, then dimethylformamide (DMF) is removed by reduced pressure distillation, and finally the remaining product after reduced pressure distillation is purified by silica gel column chromatography to obtain the collector;

[0016] When R in formula 1 is an S atom, the steps are as follows:

[0017] Step 1b, 3-chloroalkylthioacetic acid ester or 4-chloroalkylthioacetic acid ester is mixed with sodium sulfide in dimethylformamide (DMF), and then the mixed solution is heated to reflux under water bath conditions, and nitrogen is introduced during the heating reflux process to obtain a mixed solution containing a thioether bond intermediate product;

[0018] Step 2b, an excess of sodium hydroxide is added to the mixed solution containing the thioether bond intermediate product to perform an alkaline hydrolysis reaction, and the reaction is performed under a water bath environment to obtain a mixed solution containing a dimercapto sulfide;

[0019] Step 3b, after the mixed solution containing the dimercapto sulfide is raised to room temperature, the pH of the solution is adjusted to 2-3 with dilute hydrochloric acid, then the dimercapto sulfide mixed solution is extracted with ethyl acetate and dried with anhydrous sodium sulfate, then dimethylformamide (DMF) is removed by reduced pressure distillation, and finally the remaining product after reduced pressure distillation is purified by silica gel column chromatography to obtain a collector.

[0020] As a preferred technical solution of the present application, the mobile phase of the silica gel column is petroleum ether / ethyl acetate at a volume ratio of 3:1.

[0021] As a preferred technical solution of the present application, the reaction temperature of the solution in step 1a is 60-120°C, and the reaction time of the solution is 6-12 hours.

[0022] As a preferred technical solution of the present application, the reaction temperature of the solution in step 1b is 0-5°C, and the reaction time of the solution is 2-6 hours.

[0023] As a preferred technical solution of the present application, the molar ratio of the thioether bond intermediate product to sodium hydroxide in step 2b is 1 / 2.5.

[0024] As a preferred technical solution of the present application, the reaction temperature of the solution in step 2b is 0-5°C, and the reaction time of the solution is 30 minutes.

[0025] An application of a high-efficiency collector for iron ore reverse flotation desulfurization, characterized in that it comprises the following steps:

[0026] (1) The raw ore is ground to a particle size of 75% of -74 μm, and a slurry with a concentration of 30% is prepared;

[0027] (2) The collector is added to the slurry at a dosage of 100 g / t, and the slurry is adjusted for 3 minutes;

[0028] (3) A foaming agent 2 # oil is added to the slurry at a dosage of 40 g / t, and the slurry is adjusted for 1 minute;

[0029] (4) The roughing time of the ore pulp is 4 minutes, and the obtained flotation froth is a sulfur concentrate, and the remaining ore pulp is an iron concentrate.

[0030] As a preferred technical solution of the present application, the raw ore is any one or more of hematite, magnetite, pyrite and pyrrhotite.

[0031] The present application has the following advantages:

[0032] The sulfur atom in the dimercapto compound has strong electron supply ability. When these compounds react with metal ions, the sulfur atom can coordinate with metal ions through its lone pair of electrons to form stable metal-sulfur bonds, reducing the mobility of metal ions and thus enhancing the stability of the complex. It can generate a black precipitate of insoluble complex with Fe 2+ ions in the ore pulp, but cannot generate a precipitate with Fe 3+ ions. Therefore, in the ore pulp, dimercapto reagents have strong collecting ability for pyrite and cannot react with hematite. The introduction of an ether bond in the dimercapto compound can increase its solubility, surface tension and molecular activity, and enhance its collecting ability. Therefore, using dimercapto ether as a collector can achieve effective separation of pyrite and hematite.

[0033] When using the traditional collector butyl xanthate 200 g / t + foaming agent 40 g / t, the sulfur grade in the iron concentrate obtained is 0.84%, while using dimercapto ether as a collector, the sulfur grade in the iron concentrate obtained is less than 0.55% at a reagent dosage of 100 g / t. Especially for pyrrhotite-containing pyrite, better desulfurization effect can be obtained, the VOCs emission is greatly reduced, the working environment of workers is greatly improved, the risk of harm to workers' health is reduced, and the increasingly stringent environmental protection requirements are met. DETAILED DESCRIPTION

[0034] The present application will be further illustrated in conjunction with the specific embodiments, and it should be understood that the following specific embodiments are only used to illustrate the present application and not to limit the scope of the present application.

[0035] Experimental reagents used in the examples:

[0036] Di(3-chloropropyl)ether purity 97% Mcclin

[0037] Sodium hydrosulfide purity 99.7%

[0038] DMF purity 99.8%

[0039] Dilute hydrochloric acid mass fraction 10%

[0040] Ethyl acetate purity 99.5%

[0041] Anhydrous sodium sulfate, 99.5% purity

[0042] 3-chloropropylthioacetate, 90% purity, Aldrich

[0043] Sodium sulfide, 99.5% purity

[0044] Sodium hydroxide, 99.5% purity

[0045] Bis(4-chlorobutyl)ether, 98% purity, MacLlvre

[0046] 4-chlorobutylthioacetate, 97% purity, MacLlvre

[0047] 4,4-dibromobiphenyl ether, 99% purity, Aldrich

[0048] Foaming agent 2 # Oil, 90% purity, Sino-Flair

[0049] Butyl xanthate, 90% purity, Sino-Flair

[0050] Experimental instruments used in the examples:

[0051] Silica gel column (Merck Silica gel 601 kg) with 6 nm pore size / 200 mesh, mobile phase is petroleum ether / ethyl acetate with a volume ratio of 3:1

[0052] Example 1

[0053] This example is an example of the preparation method of the novel high-efficiency pyrite collector di(3-mercaptopropyl) ether (molecular formula C6H 14 OS2) described in the application, which comprises the following steps:

[0054] (1) According to the mass fraction, 11 parts of di(3-chloropropyl) ether, 9 parts of sodium hydrosulfide, and 80 parts of dimethylformamide (DMF) are selected, then di(3-chloropropyl) ether and sodium hydrosulfide are dissolved in dimethylformamide (DMF) by stirring, the reaction temperature is adjusted to 60~80℃, the mixed solution is heated to reflux, nitrogen is introduced for protection during the heating and reflux process, the reaction time is 6 hours, a nucleophilic substitution reaction is carried out, and a mixed solution containing di(3-mercaptopropyl) ether is obtained, and the molecular structure of the reactant is as follows:

[0055]

[0056] (2) The mixed solution containing bis(3-mercaptopropyl) ether is cooled, and then its pH is adjusted to 7-8 with dilute hydrochloric acid, extracted with ethyl acetate and dried with anhydrous sodium sulfate. Dimethylformamide (DMF) is removed by vacuum distillation at 0.008 MPa and 80°C, and the remaining product is purified by silica gel column chromatography (petroleum ether / ethyl acetate = 3:1) to obtain the float sulfur collector bis(3-mercaptopropyl) ether. Its structural formula is HS-(CH2)3-O-(CH2)3-SH, and its molecular structure is as follows:

[0057]

[0058] Example 2

[0059] This example is an example of a preparation method of the novel and efficient pyrite collector bis(3-mercaptopropyl) sulfide (molecular formula C6H 14 S3) according to the present application, which comprises the following steps:

[0060] (1) According to the mass fraction, 31 parts of 3-chloropropyl thioacetate, 15 parts of sodium sulfide, and 54 parts of dimethylformamide (DMF) are selected, and then 3-chloropropyl thioacetate and sodium sulfide are dissolved in dimethylformamide (DMF) under stirring. The reaction is carried out in a water bath environment, the reaction temperature is adjusted to 0-5°C, nitrogen is introduced during the heating and reflux process, the reaction time is 2 hours, and a mixed solution containing a thioether bond intermediate product is obtained. The molecular structure of the reactant is as follows:

[0061]

[0062] (2) 21 parts of sodium hydroxide (mass fraction) are added to the mixed solution containing the thioether bond intermediate product to carry out alkaline hydrolysis reaction (the molar ratio of thioether bond intermediate product to sodium hydroxide is 1 / 2.5, at this time sodium hydroxide is excessive, and the solution is alkaline), and the reaction is carried out in a water bath environment. The reaction temperature is adjusted to 0-5°C, the reaction time is 30 minutes, and a mixed solution containing bis(3-mercaptopropyl) sulfide is obtained. The molecular structure of the intermediate product is as follows:

[0063]

[0064] (3) The mixed solution containing bis(3-mercaptopropyl) sulfide is brought to room temperature (15-30°C), and then its pH is adjusted to 2-3 with dilute hydrochloric acid, extracted with ethyl acetate and dried with anhydrous sodium sulfate. Dimethylformamide (DMF) is removed by vacuum distillation at 0.008 MPa and 80°C, and the remaining product is purified by silica gel column chromatography (petroleum ether / ethyl acetate = 3:1) to obtain the floating sulfur collector bis(3-mercaptopropyl) sulfide. Its structural formula is HS-(CH2)3-S-(CH2)3-SH, and the molecular structure is as follows:

[0065]

[0066] Example 3

[0067] This example is an example of a preparation method of the novel high-efficiency pyrite collector bis(4-mercaptobutyl) ether (molecular formula C8H 18 OS2) according to the present application, which comprises the following steps:

[0068] (1) According to the mass percentage: bis(4-chlorobutyl) ether 14 parts, sodium hydrosulfide 10 parts, dimethylformamide (DMF) 76 parts, then stirring and dissolving bis(4-chlorobutyl) ether and sodium hydrosulfide in dimethylformamide (DMF), adjusting the reaction temperature to 80-120°C, heating the mixed solution to reflux, and passing nitrogen gas during the heating reflux process, the reaction time is 8 hours, and the nucleophilic substitution reaction is carried out to obtain a mixed solution containing bis(4-mercaptobutyl) ether, and the molecular structure of the reactant is as follows:

[0069]

[0070] (2) The mixed solution containing bis(4-mercaptobutyl) ether is cooled, and then its pH is adjusted to 7-8 with dilute hydrochloric acid, extracted with ethyl acetate and dried with anhydrous sodium sulfate. Dimethylformamide (DMF) is removed by vacuum distillation at 0.008 MPa and 80°C, and the remaining product is purified by silica gel column chromatography (petroleum ether / ethyl acetate = 3:1) to obtain the floating sulfur collector bis(4-mercaptobutyl) ether. Its structural formula is HS-(CH2)4 -O-(CH2)4-SH, and the molecular structure is as follows:

[0071]

[0072] Example 4

[0073] This example is an example of a preparation method of the novel high-efficiency pyrite collector bis(4-mercaptobutyl) sulfide (molecular formula C8H 18 S3) according to the present application, which comprises the following steps:

[0074] (1) According to the mass fraction, 38 parts of 4-chlorobutylthioacetate, 14 parts of sodium sulfide, and 58 parts of dimethylformamide (DMF) are selected, then 4-chlorobutylthioacetate and sodium sulfide are stirred and dissolved in dimethylformamide (DMF), the whole reaction is carried out in a water bath environment, the reaction temperature is adjusted to 0-5℃, nitrogen is introduced during the heating reflux process, the reaction time is 6 hours, a mixed solution containing a thioether bond intermediate product is obtained, and the molecular structure of the reactant is as follows:

[0075]

[0076] (2) 25 parts of sodium hydroxide (mass fraction) are added to the mixed solution containing the thioether bond intermediate product to carry out alkaline hydrolysis reaction (the molar ratio of the thioether bond intermediate product to sodium hydroxide is 1 / 2.5, at this time, sodium hydroxide is excessive, and the solution is alkaline), and the reaction is carried out in a water bath environment, the reaction temperature is adjusted to 0-5℃, and the reaction time is 30 minutes, a mixed solution containing di(4-mercaptobutyl) sulfide is obtained, and the molecular structure of the intermediate product is as follows:

[0077]

[0078] (3) The mixed solution containing di(4-mercaptobutyl) sulfide is raised to room temperature (15-30℃), and the pH is adjusted to 2-3 with dilute hydrochloric acid, then extracted with ethyl acetate and dried with anhydrous sodium sulfate. Dimethylformamide (DMF) is removed by vacuum distillation at 0.008Mpa and 80℃, and the remaining product is purified by silica gel column (petroleum ether / ethyl acetate=3:1) chromatography to obtain the sulfur collector di(4-mercaptobutyl) sulfide. Its structural formula is HS-(CH2)4-S-(CH2)4-SH, and the molecular structure is as follows:

[0079]

[0080] Example 5

[0081] This example is one example of the preparation method of the novel high-efficiency pyrite collector di(4-mercaptophenyl) ether (molecular formula C 12 H 10 OS2) described in the application, which comprises the following steps:

[0082] (1) According to the mass fraction, 4,4-dibromobiphenyl ether 15 parts, sodium hydrosulfide 12 parts, dimethylformamide (DMF) 73 parts, then 4,4-dibromobiphenyl ether and sodium hydrosulfide are dissolved in dimethylformamide (DMF) by stirring, the reaction temperature is adjusted to 80-120℃, the mixed solution is heated to reflux, nitrogen is introduced during the heating and reflux process, the reaction time is 12 hours, the nucleophilic substitution reaction is carried out, and a mixed solution containing bis(4-mercaptophenyl) ether is obtained, and the molecular structure of the reactant is as follows:

[0083]

[0084] (2) After the mixed solution containing bis(4-mercaptophenyl) ether is cooled, its pH is adjusted to 7-8 with dilute hydrochloric acid, extracted with ethyl acetate and dried with anhydrous sodium sulfate. Dimethylformamide (DMF) is removed by vacuum distillation under the conditions of 0.008Mpa and 80℃, and the remaining product is purified by silica gel column (petroleum ether / ethyl acetate=3:1) chromatography to obtain the float sulfur collector bis(4-mercaptophenyl) ether. Its structural formula is HS-C6H4 -O-C6H4-SH, and the molecular structure is as follows:

[0085]

[0086] Example 6

[0087] This example is an application example of the high-efficiency pyrite collector prepared by examples 1-5 in the desulfurization of iron ore reverse flotation.

[0088] (1) Mineral raw material: the mineral raw material is a high-sulfur iron ore in Peru, which contains 60.14% of iron and 3.08% of sulfur. The phase analysis shows that the iron minerals mainly exist in the form of hematite and magnetite; the sulfur minerals mainly exist in the form of pyrite and pyrrhotite.

[0089] (2) The reagent system and operating conditions are as follows: 300g of the iron ore is ground to about 75% of-74 μm, mixed with 700ml of water, and added into a 1L hanging tank flotation machine for flotation test. 100g / t of the pyrite collector is added, stirred for 3 minutes, then 40g / t of the frother 2# oil is added, stirred for 1 minute, and after 4 minutes of flotation, the obtained flotation froth is a sulfur concentrate, and the remaining slurry is an iron concentrate. The sulfur concentrate and iron concentrate products are collected, filtered, dried, and weighed. Under the same conditions, 200g / t of butyl xanthate collector is added as a comparison, and the sulfur grade (coulometric titration) and sulfur recovery rate of the obtained products are shown in Table 1. #

[0090] Table 1 Desulfurization test results of iron ore reverse flotation (iron concentrate)

[0091]

[0092] All five new collectors (100 g / t) can reduce the sulfur grade of iron concentrate to a lower level of 0.46% ~ 0.62%. The butyl xanthate used in the comparative example still has a sulfur grade of 0.84% after desulfurization at double the dosage (200 g / t). This data clearly shows that the collector of the present application only needs half the dosage of butyl xanthate to achieve a desulfurization effect far superior to butyl xanthate, and can produce an iron concentrate product with lower sulfur content and higher quality.

[0093] Example 7

[0094] This example aims to provide a specific application example of the high-efficiency environmentally friendly pyrite collector to demonstrate its feasibility and superiority in replacing traditional collectors with strong irritating odor (such as xanthate) in large-scale industrial iron ore concentrators. It focuses on demonstrating that it can significantly reduce the irritating odor of the working environment, improve environmental indicators, and at the same time maintain stable or even better beneficiation technical indicators.

[0095] The original sulfide ore collector (Gansu Baiyin Chemical Plant, ethyl xanthate accounts for 90% by mass) is used in the flotation system of the iron ore concentrator, which produces a large amount of sulfur-containing irritating and odor gas during preparation and use, affecting the health of the operators, and the odor problem around the plant is serious, with high environmental pressure.

[0096] The industrial test described in this example was conducted from November 22 to November 30, 2023, for a total of 9 days, and a comparative test was conducted on 3 series and 5 series of the concentrator. The 3 series used the pyrite collector (7042H) described in the present application (the effective component is the pyrite collector described in Example 1, and the effective component accounts for 50% by mass, provided by Shenyang Feiwei Company), and the 5 series used the original sulfide ore collector of the concentrator.

[0097] The following table compares the main results of the iron ore industrial test using the collector 7042H of the present application and the traditional collector:

[0098]

[0099] The irritating odor problem that has existed for a long time on site has been completely solved, the VOCs emission has been greatly reduced, the working environment of the workers has been greatly improved, the risk of harm to the health of the workers has been reduced, and the increasingly stringent environmental protection requirements have been met. After replacing the traditional collector, not only the desulfurization target is completely achieved, but also the sulfur content of the iron concentrate is slightly optimized, and the dosage of the collector is also reduced, proving the high efficiency and selectivity of the collector. This example provides a mature and reliable technical solution and practical basis for the green and efficient separation of similar high-sulfur iron ore.

[0100] It should be noted that the above content only illustrates the technical idea of the present application, and cannot limit the protection scope of the present application. For ordinary skilled in the art, without departing from the principle of the present application, a number of improvements and refinements can be made, which fall within the protection scope of the claims of the present application.

Claims

1. A high-efficiency collector for desulfurization in iron ore reverse flotation, characterized in that, It has the structure of Formula 1: Formula 1 Wherein, R is an O or S atom, and R1 and R2 are any one of the short-chain alkyl or phenyl groups from C1 to C6.

2. The high-efficiency collector for desulfurization in iron ore reverse flotation according to claim 1, characterized in that, R1 and R2 are any one of propylene, butylene, and phenyl groups.

3. The method for preparing the high-efficiency collector for iron ore reverse flotation desulfurization as described in any one of claims 1-2, characterized in that, The preparation method includes the following steps: When R in Equation 1 is an O atom, the steps are as follows: Step 1a: Dissolve dichloroalkyl ether or dibromodiphenyl ether in sodium hydrosulfide in dimethylformamide (DMF), then heat the mixed solution to reflux, and purge with nitrogen gas during the reflux process to carry out a nucleophilic substitution reaction, thereby obtaining a mixed solution containing dithiol ether. Step 2a: After cooling, the mixed solution containing dimercaptoethers is adjusted to pH 7-8 with dilute hydrochloric acid. Then, the mixed solution of dimercaptoethers is extracted with ethyl acetate and dried with anhydrous sodium sulfate. Dimethylformamide (DMF) is then removed by vacuum distillation. Finally, the remaining product from vacuum distillation is purified by silica gel column chromatography to obtain the collector. When R in Equation 1 is an S atom, the steps are as follows: Step 1b: Dissolve 3-chloroalkylthioacetate or 4-chloroalkylthioacetate in sodium sulfide in dimethylformamide (DMF), then heat the mixture to reflux in a water bath while purging with nitrogen gas to obtain a mixed solution containing a thioether bond intermediate. Step 2b: Add excess sodium hydroxide to the mixed solution containing the intermediate product of thioether bond to carry out alkaline hydrolysis reaction in a water bath environment to obtain a mixed solution containing dimercaptothioether. Step 3b: After the mixed solution containing dimercaptosulfide is brought to room temperature, its pH is adjusted to 2-3 with dilute hydrochloric acid. Then, the mixed solution of dimercaptosulfide is extracted with ethyl acetate and dried with anhydrous sodium sulfate. Dimethylformamide (DMF) is then removed by vacuum distillation. Finally, the product remaining after vacuum distillation is purified by silica gel column chromatography to obtain the collector.

4. The method for preparing a high-efficiency collector for iron ore reverse flotation desulfurization according to claim 3, characterized in that, The mobile phase of the silica gel column is petroleum ether / ethyl acetate in a volume ratio of 3:

1.

5. The method for preparing a high-efficiency collector for desulfurization in iron ore reverse flotation according to claim 3, characterized in that, In step 1a, the reaction temperature of the solution is 60~120℃, and the reaction time is 6~12 hours.

6. The method for preparing a high-efficiency collector for desulfurization in iron ore reverse flotation according to claim 3, characterized in that, In step 1b, the reaction temperature of the solution is 0~5℃, and the reaction time is 2~6 hours.

7. The method for preparing a high-efficiency collector for desulfurization in iron ore reverse flotation according to claim 3, characterized in that, In step 2b, the molar ratio of the thioether bond intermediate to sodium hydroxide is 1 / 2.

5.

8. The method for preparing a high-efficiency collector for desulfurization in iron ore reverse flotation according to claim 3, characterized in that, In step 2b, the reaction temperature of the solution is 0~5℃, and the reaction time is 30 minutes.

9. The application of the high-efficiency collector for iron ore reverse flotation desulfurization as described in any one of claims 1-2, characterized in that, Includes the following steps: (1) Grind the raw ore to a particle size of -74μm, accounting for 75%, and make a slurry with a concentration of 30%; (2) Add the collector to the slurry at a dosage of 100g / t and adjust the slurry for 3 minutes; (3) Add 2g of foaming agent to the slurry at a dosage of 40g / t. # Add oil and mix for 1 minute; (4) The roughing time of the slurry is 4 minutes. The flotation foam obtained is sulfur concentrate, and the remaining slurry is iron concentrate.

10. The application of the high-efficiency collector for iron ore reverse flotation desulfurization according to claim 9, characterized in that, The raw ore is any one or more of hematite, magnetite, pyrite, and pyrrhotite.

Citation Information

Patent Citations

  • Agent for reverse flotation of iron ore and combination use method

    CN103495506A

  • Combined reagent for desulfurizing fine iron powder under alkaline condition and method for desulfurizing pyrrhotite by adopting combined reagent

    CN112871458A