CN112403684A - Synthesis method and application of xanthic acid-quaternary ammonium salt ionic liquid - Google Patents
Synthesis method and application of xanthic acid-quaternary ammonium salt ionic liquid Download PDFInfo
- Publication number
- CN112403684A CN112403684A CN202011336606.4A CN202011336606A CN112403684A CN 112403684 A CN112403684 A CN 112403684A CN 202011336606 A CN202011336606 A CN 202011336606A CN 112403684 A CN112403684 A CN 112403684A
- Authority
- CN
- China
- Prior art keywords
- xanthate
- quaternary ammonium
- ammonium salt
- ionic liquid
- salt ionic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Classifications
-
- 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
- B03D1/012—Organic compounds containing sulfur
-
- 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
- B03D2201/02—Collectors
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a synthesis method and application of xanthate-quaternary ammonium salt ionic liquid, wherein the synthesis method comprises the following steps: s1, mixing xanthate and quaternary ammonium salt according to a certain mixing molar ratio, putting the mixture into a single-neck flask with methanol stored therein, and stirring the mixture at room temperature until the mixture is completely dissolved; s2, magnetically stirring the mixed solution in the single-neck flask at the temperature of 25-55 ℃, and stopping reaction after stirring for 8-14 hours; s3, filtering the reaction liquid obtained in the step S2 for the first time, performing rotary evaporation on the filtered primary filtrate to remove a methanol solvent, and then washing for 20-35 min by using acetone or benzene in a shaking way; s4, carrying out secondary filtration on the solution washed in the step S3, removing redundant solids, and then carrying out rotary evaporation on the filtered secondary filtrate to remove an acetone or benzene solvent to obtain the required xanthate-quaternary ammonium salt ionic liquid; wherein: the xanthic acid is n-butyl xanthate or isobutyl xanthate; the quaternary ammonium salt is cetyl quaternary ammonium salt or tetradecyl quaternary ammonium salt.
Description
Technical Field
The invention belongs to the technical field of preparation and application of ionic liquid, and particularly relates to a synthesis method and application of xanthate-quaternary ammonium salt ionic liquid.
Background
The ionic liquid is a salt composed of cation and anion, is liquid at room temperature, and has stable property, low volatility, and resistance to certain gas (such as H)2S、CO2、SO2Etc.) has stronger dissolving capacity; meanwhile, the ionic liquid has excellent designability and can meet various requirements through the design of anions and cations.
At present, the bauxite in China is mainly diasporic bauxite, and the bauxite has the characteristics of high aluminum, high sulfur and low aluminum-silicon ratio. It is generally considered that bauxite with a sulfur content of more than 0.7% is high-sulfur bauxite, and the high-sulfur bauxite directly produces alumina, and a series of problems such as corrosion of equipment, excessive iron in sodium aluminate solution caused by dissolution of pyrite and the like are generated, so that the high-sulfur bauxite must be desulfurized firstly for economic utilization. At present, the reserves of high-sulfur diasporic bauxite are about 5.6 hundred million tons in China, wherein the high-grade ore with the aluminum-silicon ratio of more than 7 accounts for about 57.2 percent, the alumina can be produced by directly utilizing a Bayer process after desulfurization, and the middle-low-grade high-sulfur bauxite accounts for about 42.8 percent. This portion of ore must be simultaneously desulfurized and desilicated before it can be economically utilized.
The research at home and abroad aiming at the distributed flotation, desulfurization and desilication of the medium-low-grade high-sulfur bauxite relates to the research, and generally the desulphurization and desilication are carried out step by step, and some tests are also expanded. But few reports are currently reported aiming at the research and industrial application of the synchronous desulfurization and desilication of the reverse flotation of the medium-low-grade high-sulfur bauxite.
In the prior art, the main processes for desulfurization and desilication in high sulfur bauxite are flotation processes, wherein for desilication it is necessary to carry out a direct flotation of diaspore using fatty acid collectors; for flotation desulfurization, it is necessary to use an ionic collector or a nonionic collector, and among the ionic collectors, a sulfide ore collector is mainly used, for example: xanthates, thiocarbamates, thiols, thioureas and their corresponding esters.
In recent years, magdalen maciewska et al react 2-mercaptobenzothiazole (accelerator M) with 1-alkyl-3-methylimidazolium tetrafluoroborate to obtain 1-alkyl-3-methylimidazolium salt ionic liquid, which is used for vulcanization of nitrile rubber (NBR), and authors research on various properties of vulcanized products shows that the synthesized ionic liquid has a significant vulcanization acceleration effect. However, the xanthate reacts with the quaternary ammonium salt to synthesize the corresponding ionic liquid, and the ionic liquid is applied to the desulfurization and desilication of the high-sulfur bauxite by reverse flotation.
Disclosure of Invention
In view of this, the present invention aims to provide a synthesis method and an application of a xanthate-quaternary ammonium salt ionic liquid.
In order to achieve the purpose, the invention provides the following technical scheme:
a synthetic method of xanthate-quaternary ammonium salt ionic liquid comprises the following steps:
s1, mixing xanthate and quaternary ammonium salt according to a certain mixing molar ratio, putting the mixture into a single-neck flask with methanol stored therein, and stirring the mixture at room temperature until the mixture is completely dissolved;
s2, magnetically stirring the mixed solution in the single-neck flask at the temperature of 25-55 ℃, and stopping reaction after stirring for 8-14 hours;
s3, filtering the reaction liquid obtained in the step S2 for the first time, performing rotary evaporation on the filtered primary filtrate to remove a methanol solvent, and then washing for 20-35 min by using acetone or benzene in a shaking way;
s4, carrying out secondary filtration on the solution washed in the step S3, removing redundant solids, and then carrying out rotary evaporation on the filtered secondary filtrate to remove an acetone or benzene solvent to obtain the required xanthate-quaternary ammonium salt ionic liquid;
s5, drying the xanthate-quaternary ammonium salt ionic liquid obtained in the step S4 in vacuum for 24 hours to obtain a pure product, wherein the purity of the pure product is measured to be 76-88% by an ionometry.
Wherein:
the xanthate is n-butyl xanthate or isobutyl xanthate with the purity of more than 90 percent;
the quaternary ammonium salt adopts hexadecyl quaternary ammonium salt or tetradecyl quaternary ammonium salt with the purity of more than 95 percent.
Preferably, in the step S1, the mixing molar ratio of the xanthate to the quaternary ammonium salt is 0.5 to 2: 2 to 0.5.
Preferably, the n-butyl xanthate is sodium n-butyl xanthate or potassium n-butyl xanthate; the isobutyl xanthate is sodium isobutyl xanthate or potassium isobutyl xanthate.
Preferably, in step S1, the mixed solution after complete dissolution contains 60% to 95% methanol.
Preferably, in step S3, the solid-liquid mixture washed with acetone or benzene by shaking contains 70% to 95% of acetone or benzene.
Preferably, in the step S3, when washing with acetone shaking: the molar ratio of the xanthate to the quaternary ammonium salt is 1: 1-2; when benzene is used for washing in a shaking mode, the molar ratio of xanthate to quaternary ammonium salt is 0.5-2: 2 to 0.5.
In order to achieve the above purpose, the invention also provides the following technical scheme:
use of a xanthate-quat ionic liquid, wherein: the xanthic acid-quaternary ammonium salt ionic liquid is synthesized according to the synthesis method disclosed above, and the xanthic acid-quaternary ammonium salt ionic liquid is used as a flotation collector and applied to the removal of pyrite and silicate minerals in the reverse flotation synchronous desulfurization and desilication of medium-low grade high-sulfur bauxite.
Compared with the prior art, the invention has the following beneficial effects:
in conclusion, the synthesis method and the application of the xanthate-quaternary ammonium salt ionic liquid provided by the invention have the advantages of reasonable proportion and simple process, and effectively fill the application blank of the xanthate-quaternary ammonium salt ionic liquid in the synchronous desulfurization and desilication of the reverse flotation of the high-sulfur bauxite.
Specifically, the xanthate-quaternary ammonium salt ionic liquid prepared by the invention is used as a flotation collector and applied to the reverse flotation synchronous desulfurization and desilication of high-sulfur bauxite, so that pyrite and silicate minerals can be removed simultaneously, the purpose of improving the content of aluminum oxide and the ratio of aluminum to silicon in the aluminum concentrate is achieved, the content of total sulfur in the aluminum concentrate can be reduced to be below 0.2%, and the production efficiency and quality of aluminum oxide in low-grade high-sulfur bauxite are effectively improved.
Drawings
FIG. 1 is a process flow chart of reverse flotation synchronous desulfurization and desilication of Chongqing high-sulfur bauxite in example 1 of the present invention;
FIG. 2 is a process flow chart of reverse flotation synchronous desulfurization and desilication of Chongqing high-sulfur bauxite in example 2 of the present invention;
FIG. 3 is a flow chart of a process for reverse flotation and simultaneous desulfurization and desilication of a certain high-sulfur bauxite in Henan in accordance with example 3 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.
Example 1
A synthetic method of xanthate-quaternary ammonium salt ionic liquid comprises the following steps:
s1, adding 3.44g (0.02mol) of sodium n-butyl xanthate and 7.29g (0.02mol) of hexadecyl trimethyl ammonium bromide into a single-neck flask, then adding 100ml of methanol into the single-neck flask, and stirring at room temperature until the sodium n-butyl xanthate and the hexadecyl trimethyl ammonium bromide are completely dissolved;
s2, magnetically stirring the mixed solution in the single-neck flask at 35 ℃, and stopping reaction after stirring for 12 hours;
s3, filtering the reaction liquid obtained in the step S2 for the first time, performing rotary evaporation on the filtered primary filtrate to remove the methanol solvent, and then washing for 30min by shaking with 90ml of acetone;
s4, carrying out secondary filtration on the solution washed in the step S3, removing redundant solids, and then carrying out rotary evaporation on the filtered secondary filtrate to remove an acetone solvent to obtain the required xanthic acid-quaternary ammonium salt ionic liquid;
s5, carrying out vacuum drying on the xanthate-quaternary ammonium salt ionic liquid obtained in the step S4 for 24 hours to obtain a pure product, wherein the purity of the pure product is 82.35% through the measurement of an ionometry.
The application of the xanthic acid-quaternary ammonium salt ionic liquid is characterized in that the xanthic acid-quaternary ammonium salt ionic liquid is synthesized by the synthesis method disclosed in the embodiment, and the prepared xanthic acid-quaternary ammonium salt ionic liquid is used as a collecting agent and applied to the removal of pyrite and silicate minerals in the reverse flotation synchronous desulfurization and desilication of low-grade high-sulfur bauxite.
In this example, the following test is provided:
the chemical composition of a low grade high sulfur bauxite ore in Chongqing is shown in Table 1 below.
TABLE 1 analysis results of chemical composition of test ore samples
| Composition (I) | Al2O3 | SiO2 | Fe2O3 | TiO2 | K2O | Na2O |
| Content/% | 59.81 | 13.07 | 9.38 | 2.51 | 0.51 | 0.046 |
| Composition (I) | CaO | MgO | S | L.O.I | A/S | |
| Content/% | 0.87 | 0.46 | 1.83 | 11.51 | 4.58 |
The results of semi-quantitative analysis of phase composition based on X-ray spectra and elemental analysis are shown in Table 2.
TABLE 2 analysis results of mineral composition of test sample
| Name of physical phase | Diaspore | Boehmite (DAG) | Kaolinite | Illite stone |
| Content/% | 49 | 5.5 | 12 | 5 |
| Name of physical phase | Chlorite (chlorite) | Quartz | Calcite | Dolomite |
| Content/% | 14.5 | 2.1 | 1.7 | 0.9 |
| Name of physical phase | Anatase ore | Rutile type | Siderite ore | Pyrite |
| Content/% | 2.1 | 0.45 | 1.9 | 4.1 |
Under the conditions that the grinding fineness is 77.32% of 0.075mm, the flotation pH value of sodium carbonate slurry mixing is 8.5, the total using amount of activator anhydrous copper sulfate is 50g/t, the total using amount of inorganic high-molecular polymeric silicate inhibitor is 1000g/t, and the total using amount of newly-blended ionic liquid collector and foaming agent 2# oil is 400g/t +100g/t, a laboratory adopts a reverse flotation process flow of 'one coarse and one fine two sweeps' to perform a laboratory closed-loop experiment, and tests are performed in a 1.5L hanging-groove type flotation machine, so that the excellent indexes that the A/S is 6.63, the alumina content is 65.35%, the sulfur content is 0.19%, the recovery rate of the alumina is up to 83.47%, the alumina content of tailings is reduced to 41.83%, the A/S is reduced to 1.82, the A/S of the concentrates is improved by 2.05, and the sulfur content of the aluminum concentrates is also reduced to 0.19% are obtained. The experimental flow is shown in the attached figure 1, and the experimental results are shown in the table 3.
TABLE 3 laboratory closed-circuit reverse flotation synchronous desulfurization and desilication test results
| Product name | Yield/%) | Al2O3/％ | SiO2/％ | A/S | Al2O3Percent recovery% | S/％ |
| Aluminium concentrate | 76.37 | 65.35 | 9.85 | 6.63 | 83.47 | 0.19 |
| Sulfur silicon tailings | 23.63 | 41.83 | 23.00 | 1.82 | 16.53 | 7.07 |
| Raw ore | 100.00 | 59.79 | 13.06 | 4.58 | 100.00 | 1.82 |
Example 2
A synthetic method of xanthate-quaternary ammonium salt ionic liquid comprises the following steps:
s1, adding 3.44g (0.02mol) of sodium isobutyl xanthate and 11.04g (0.03mol) of tetradecyl dimethyl benzyl ammonium chloride into a single-neck flask, adding 120ml of methanol into the single-neck flask, and stirring at room temperature until the sodium isobutyl xanthate and the tetradecyl dimethyl benzyl ammonium chloride are completely dissolved;
s2, magnetically stirring the mixed solution in the single-neck flask at the temperature of 30 ℃, and stopping reaction after stirring for 14 hours;
s3, filtering the reaction solution obtained in the step S2 for the first time, performing rotary evaporation on the filtered primary filtrate to remove the methanol solvent, and then washing for 25min with 110ml of benzene in a shaking way;
s4, carrying out secondary filtration on the solution washed in the step S3, removing redundant solids, and then carrying out rotary evaporation on the filtered secondary filtrate to remove a benzene solvent to obtain the required xanthic acid-quaternary ammonium salt ionic liquid;
s5, carrying out vacuum drying on the xanthate-quaternary ammonium salt ionic liquid obtained in the step S4 for 24 hours to obtain a pure product, wherein the purity of the pure product is 79.47% as determined by an ionometry.
The application of the xanthic acid-quaternary ammonium salt ionic liquid is characterized in that the xanthic acid-quaternary ammonium salt ionic liquid is synthesized by the synthesis method disclosed in the embodiment, and the prepared xanthic acid-quaternary ammonium salt ionic liquid is used as a collecting agent and applied to the removal of pyrite and silicate minerals in the reverse flotation synchronous desulfurization and desilication of low-grade high-sulfur bauxite.
In this example, the following test is provided:
the chemical composition of a low grade high sulfur bauxite in Chongqing is shown in Table 5 below.
TABLE 4 analysis of chemical composition of test sample
| Composition (I) | Al2O3 | SiO2 | Fe2O3 | TiO2 | K2O | Na2O |
| Content/% | 58.58 | 13.03 | 10.65 | 2.53 | 0.52 | 0.050 |
| Composition (I) | CaO | MgO | S | L.O.I | A/S | |
| Content/% | 1.38 | 0.81 | 0.96 | 11.29 | 4.49 |
The results of semi-quantitative analysis of phase composition based on X-ray spectra and elemental analysis are shown in Table 5.
TABLE 5 analysis results of mineral composition of test sample
| Name of physical phase | Diaspore | Boehmite (DAG) | Kaolinite | Illite stone |
| Content/% | 48.3 | 5.4 | 13.2 | 6.2 |
| Name of physical phase | Chlorite (chlorite) | Quartz | Calcite | Dolomite |
| Content/% | 14.7 | 3.1 | 1.4 | 0.9 |
| Name of physical phase | Anatase ore | Rutile type | Siderite ore | Pyrite |
| Content/% | 2.2 | 0.6 | 2.3 | 2.1 |
Under the conditions that the grinding fineness is 77.46% of 0.075mm, the flotation pH value of sodium carbonate slurry mixing is 8.5, the total using amount of activator blue vitriod is 100g/t, the total using amount of water glass inhibitor is 800g/t, and the total using amount of newly-blended ionic liquid collector and foaming agent 2# oil is 300g/t +100g/t, a laboratory adopts a reverse flotation process flow of 'one coarse sweeping and two sweeps' to carry out a laboratory closed-loop experiment, and the experiment is carried out in a 1.5L hanging groove type flotation machine, so that the aluminum concentrate with the A/S of 5.36, the alumina content of 62.18%, the sulfur content of 0.11% and the alumina recovery rate of 85.10% is obtained, the alumina content of tailings is reduced to 42.65%, the A/S is reduced to 2.21, the A/S of the concentrate is improved by 0.94, and the sulfur content of the aluminum concentrate is also reduced to a good index of 0.11%. The experimental flow is shown in figure 2, and the experimental results are shown in table 6.
TABLE 6 laboratory closed-circuit reverse flotation synchronous desulfurization and desilication test results
| Product name | Yield/%) | Al2O3/％ | SiO2/％ | A/S | Al2O3Percent recovery% | S/％ |
| Aluminium concentrate | 79.67 | 62.18 | 11.61 | 5.36 | 85.10 | 0.11 |
| Sulfur silicon tailings | 20.33 | 42.65 | 19.32 | 2.21 | 14.90 | 4.06 |
| Raw ore | 100.00 | 58.21 | 13.18 | 4.42 | 100 | 0.94 |
Example 3
A synthetic method of xanthate-quaternary ammonium salt ionic liquid comprises the following steps:
s1, adding 5.64g (0.03mol) of potassium n-butyl xanthate and 8.24g (0.02mol) of tetradecyl dimethyl benzyl ammonium bromide into a single-neck flask, then adding 135ml of methanol into the single-neck flask, and stirring at room temperature until the potassium n-butyl xanthate and the tetradecyl dimethyl benzyl ammonium bromide are completely dissolved;
s2, magnetically stirring the mixed solution in the single-neck flask at 41 ℃, and stopping reaction after stirring for 9 hours;
s3, filtering the reaction solution obtained in the step S2 for the first time, performing rotary evaporation on the filtered primary filtrate to remove the methanol solvent, and then washing for 20min by using 140ml of benzene in a shaking way;
s4, carrying out secondary filtration on the solution washed in the step S3, removing redundant solids, and then carrying out rotary evaporation on the filtered secondary filtrate to remove a benzene solvent to obtain the required xanthic acid-quaternary ammonium salt ionic liquid;
s5, carrying out vacuum drying on the xanthate-quaternary ammonium salt ionic liquid obtained in the step S4 for 24 hours to obtain a pure product, wherein the purity of the pure product is 86.72% through the measurement of an ionometry.
The application of the xanthic acid-quaternary ammonium salt ionic liquid is characterized in that the xanthic acid-quaternary ammonium salt ionic liquid is synthesized by the synthesis method disclosed in the embodiment, and the prepared xanthic acid-quaternary ammonium salt ionic liquid is used as a collecting agent and applied to the removal of pyrite and silicate minerals in the reverse flotation synchronous desulfurization and desilication of low-grade high-sulfur bauxite.
In this example, the following test is provided:
the chemical composition of a certain low-grade high-sulfur bauxite in Henan is shown in Table 7 below.
TABLE 7 analysis results of chemical composition of test ore samples
The results of semi-quantitative analysis of phase composition based on X-ray spectra and elemental analysis are shown in Table 8.
TABLE 8 analysis results of mineral composition of test sample
| Name of physical phase | Diaspore | Kaolinite | Illite stone | Chlorite (chlorite) | Quartz |
| Content/% | 51.5 | 18.7 | 5.1 | 3.9 | 7.5 |
| Name of physical phase | Calcite | Dolomite | Anatase ore | Siderite ore | Pyrite |
| Content/% | 3.3 | 0.8 | 4.1 | 1.4 | 3.8 |
Under the conditions that the grinding fineness is 69.77% in a grinding process, the natural flotation pH value is 7.0-7.5, the total usage amount of an activator copper sulfate pentahydrate is 60g/t, the total usage amount of an acidified water glass inhibitor is 1200g/t, and the total usage amount of a newly-blended ionic liquid collector and a foaming agent 2# oil is 500g/t +150g/t, a laboratory adopts a reverse flotation process flow of 'one-coarse-two-fine-sweep' to perform a laboratory closed-loop experiment, and tests are performed in a 1.0L hanging groove type flotation machine, so that the excellent indexes that the A/S is 6.38, the alumina content is 64.77%, the sulfur content is 0.14%, the alumina recovery rate is 73.36%, the alumina content of tailings is reduced to 39.56%, the A/S is reduced to 1.89, the A/S of the concentrates is improved by 2.48, and the sulfur content of the aluminum concentrates is also reduced to 0.14% are obtained. The experimental flow is shown in figure 3, and the experimental results are shown in table 9.
TABLE 9 laboratory closed-circuit reverse flotation synchronous desulfurization and desilication test results
| Product name | Yield/%) | Al2O3/％ | SiO2/％ | A/S | Al2O3Percent recovery% | S/％ |
| Aluminium concentrate | 62.71 | 64.77 | 10.15 | 6.38 | 73.36 | 0.14 |
| Silicon sulfide tailMine | 37.29 | 39.56 | 20.98 | 1.89 | 14.90 | 3.98 |
| Raw ore | 100.00 | 55.37 | 14.19 | 3.90 | 100.00 | 1.57 |
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A synthetic method of xanthate-quaternary ammonium salt ionic liquid is characterized by comprising the following steps:
s1, mixing xanthate and quaternary ammonium salt according to a certain mixing molar ratio, putting the mixture into a single-neck flask with methanol stored therein, and stirring the mixture at room temperature until the mixture is completely dissolved;
s2, magnetically stirring the mixed solution in the single-neck flask at the temperature of 25-55 ℃, and stopping reaction after stirring for 8-14 hours;
s3, filtering the reaction liquid obtained in the step S2 for the first time, performing rotary evaporation on the filtered primary filtrate to remove a methanol solvent, and then washing for 20-35 min by using acetone or benzene in a shaking way;
s4, carrying out secondary filtration on the solution washed in the step S3, removing redundant solids, and then carrying out rotary evaporation on the filtered secondary filtrate to remove an acetone or benzene solvent to obtain the required xanthate-quaternary ammonium salt ionic liquid;
wherein:
the xanthate is n-butyl xanthate or isobutyl xanthate with the purity of more than 90 percent;
the quaternary ammonium salt adopts hexadecyl quaternary ammonium salt or tetradecyl quaternary ammonium salt with the purity of more than 95 percent.
2. The method for synthesizing the xanthate-quaternary ammonium salt ionic liquid according to claim 1, wherein in the step S1, the mixing molar ratio of the xanthate to the quaternary ammonium salt is 0.5-2: 2 to 0.5.
3. The method for synthesizing xanthate-quaternary ammonium salt ionic liquid as claimed in claim 2, wherein the n-butyl xanthate is sodium n-butyl xanthate or potassium n-butyl xanthate; the isobutyl xanthate is sodium isobutyl xanthate or potassium isobutyl xanthate.
4. The method for synthesizing the xanthate-quaternary ammonium salt ionic liquid according to claim 1 or 2, wherein in the step S1, the mixed solution after complete dissolution contains 60% to 95% of methanol.
5. The method for synthesizing the xanthate-quaternary ammonium salt ionic liquid as claimed in claim 1 or 2, wherein in the step S3, the solid-liquid mixed solution washed with acetone or benzene by shaking contains 70% to 95% of acetone or benzene.
6. The method for synthesizing the xanthate-quaternary ammonium salt ionic liquid according to claim 1, wherein the method comprises the following steps: in step S3, when washing with acetone shaking: the molar ratio of the xanthate to the quaternary ammonium salt is 1: 1-2; when benzene is used for washing in a shaking mode, the molar ratio of xanthate to quaternary ammonium salt is 0.5-2: 2 to 0.5.
7. The method for synthesizing the xanthate-quaternary ammonium salt ionic liquid according to claim 1, wherein after the step S4, the method further comprises:
s5, drying the xanthate-quaternary ammonium salt ionic liquid obtained in the step S4 in vacuum for 24 hours to obtain a pure product, wherein the purity of the pure product is measured to be 76-88% by an ionometry.
8. The application of the xanthate-quaternary ammonium salt ionic liquid is characterized in that: the xanthate-quaternary ammonium salt ionic liquid is synthesized by the synthesis method according to any one of claims 1 to 7, and is used as a flotation collector for removing pyrite and silicate minerals in the reverse flotation synchronous desulfurization and desilication of medium-low-grade high-sulfur bauxite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011336606.4A CN112403684A (en) | 2020-11-25 | 2020-11-25 | Synthesis method and application of xanthic acid-quaternary ammonium salt ionic liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011336606.4A CN112403684A (en) | 2020-11-25 | 2020-11-25 | Synthesis method and application of xanthic acid-quaternary ammonium salt ionic liquid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN112403684A true CN112403684A (en) | 2021-02-26 |
Family
ID=74842810
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011336606.4A Pending CN112403684A (en) | 2020-11-25 | 2020-11-25 | Synthesis method and application of xanthic acid-quaternary ammonium salt ionic liquid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112403684A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023193122A1 (en) * | 2022-04-04 | 2023-10-12 | Oxiquim S.A. | Stable ionic xanthate compositions in aqueous solution |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1507954A (en) * | 2002-12-16 | 2004-06-30 | 中南大学 | Collecting agent for antiflotation desilicification and preparing method thereof |
| CN101428206A (en) * | 2007-08-13 | 2009-05-13 | 中国科学院成都有机化学有限公司 | Double-tail quaternary ammonium salt cation surface active agent and preparation method thereof |
| CN101480633A (en) * | 2008-12-09 | 2009-07-15 | 紫金矿业集团股份有限公司 | Stepped-flotation separation desulfuration method of high-sulphur bauxite |
| CN102151614A (en) * | 2010-12-15 | 2011-08-17 | 中国铝业股份有限公司 | Method for dressing, desilicication and desulfuration of sulfur-containing bauxite |
| CN105562212A (en) * | 2015-03-18 | 2016-05-11 | 遵义能矿投资股份有限公司 | Method for desilication and desulfuration of sulfur-containing bauxite by floating |
| CN106046042A (en) * | 2016-05-31 | 2016-10-26 | 山东师范大学 | Preparing method for diphenyltin sulfide tripolymer |
| CN107442287A (en) * | 2017-08-14 | 2017-12-08 | 江西理工大学 | A kind of Gemini surfactant for mineral floating |
-
2020
- 2020-11-25 CN CN202011336606.4A patent/CN112403684A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1507954A (en) * | 2002-12-16 | 2004-06-30 | 中南大学 | Collecting agent for antiflotation desilicification and preparing method thereof |
| CN101428206A (en) * | 2007-08-13 | 2009-05-13 | 中国科学院成都有机化学有限公司 | Double-tail quaternary ammonium salt cation surface active agent and preparation method thereof |
| CN101480633A (en) * | 2008-12-09 | 2009-07-15 | 紫金矿业集团股份有限公司 | Stepped-flotation separation desulfuration method of high-sulphur bauxite |
| CN102151614A (en) * | 2010-12-15 | 2011-08-17 | 中国铝业股份有限公司 | Method for dressing, desilicication and desulfuration of sulfur-containing bauxite |
| CN105562212A (en) * | 2015-03-18 | 2016-05-11 | 遵义能矿投资股份有限公司 | Method for desilication and desulfuration of sulfur-containing bauxite by floating |
| CN106046042A (en) * | 2016-05-31 | 2016-10-26 | 山东师范大学 | Preparing method for diphenyltin sulfide tripolymer |
| CN107442287A (en) * | 2017-08-14 | 2017-12-08 | 江西理工大学 | A kind of Gemini surfactant for mineral floating |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2023193122A1 (en) * | 2022-04-04 | 2023-10-12 | Oxiquim S.A. | Stable ionic xanthate compositions in aqueous solution |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102489406B (en) | Method for treating sulfur bauxite | |
| CN102151614B (en) | Method for dressing, desilicication and desulfuration of sulfur-containing bauxite | |
| CN103272702B (en) | Flotation collector and method for obtaining high-grade magnesite concentrate from low-grade magnesite | |
| CN105540628A (en) | Method for producing aluminum oxide through sintering sulfur-containing monohydrallite and lime | |
| CN109290060A (en) | A kind of process for subsequent treatment and phosphate ore floatation method of phosphate ore flotation tailings | |
| CN102409177B (en) | Method for comprehensively recovering aluminum, silicon and titanium from pyrite tailings | |
| CN109019646A (en) | A method of Aluminum sol is prepared using gangue | |
| CN103421960B (en) | Method for efficiently recycling ferro-aluminium from bauxite tailings and synchronously preparing high siliceous residues | |
| CN111672636A (en) | Spodumene ore flotation collector and preparation method and application method thereof | |
| CN112403684A (en) | Synthesis method and application of xanthic acid-quaternary ammonium salt ionic liquid | |
| CN110408794A (en) | Asbestos deposit process for cleanly preparing | |
| CN102849764B (en) | Method for preparing pseudo-boehmite by pulverized fuel ash | |
| CN1244408C (en) | Floatation method of desulfurizing and desiliconizing diaspore type bauxite | |
| CN104828849B (en) | A kind of by the method for duralumin standby high-whiteness polyaluminium chloride made of stones | |
| CN101913633B (en) | Extraction technology of alumina and potassium sulfate from alunite by using hot-pressing leaching process | |
| CN101559965A (en) | Method for using medium and low-grade celestite ore to produce strontium carbonate under plateau conditions | |
| CN102838141A (en) | Process for producing magnesium hydrate by removing silicon and aluminum from magnesite | |
| CN103101952B (en) | Preparation method of high-purity high-molecular-ratio cryolite | |
| CN113617535B (en) | Flotation compound agent for synchronously desulfurizing, removing potassium, sodium, calcium and magnesium and application thereof | |
| CN110066128A (en) | A kind of magnesia swelling agent and preparation method thereof using the preparation of high calcium magnesite tailing | |
| CN107285350A (en) | A kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon | |
| CN109110783A (en) | Sodium sulphate and ammonium sulfate salt-mixture separation method and precipitation method for treatment of waste material | |
| CN1074390C (en) | Method of sorting the concentrate ore of bauxite from the ore of bauxite containing silicon mineral | |
| US3485579A (en) | Beneficiation of cryolite material | |
| CN109835930A (en) | A kind of production method of aluminium oxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210226 |