CN110642335A - Method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater - Google Patents
Method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/36—Obtaining tungsten
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- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
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- C—CHEMISTRY; METALLURGY
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- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/10—Nature of the water, waste water, sewage or sludge to be treated from quarries or from mining activities
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Abstract
A method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater relates to a method for recovering tungstate radicals in beneficiation wastewater. The invention aims to solve the technical problems of low recovery rate and low recovery rate of tungstate radicals in the existing scheelite beneficiation wastewater. The invention comprises the following steps: a polyaniline/carbon cloth composite electrode material, an Ag/AgCl electrode and a platinum electrode form a three-electrode system and are connected to an electrochemical workstation, the polyaniline/carbon cloth composite electrode material serves as a working electrode, the Ag/AgCl electrode serves as a reference electrode, the platinum electrode serves as a counter electrode, scheelite beneficiation wastewater to be treated serves as electrolyte, and electroadsorption is carried out under the condition of electric field force. The method has simple and rapid process, and the recovery rate of absorbing tungstate ions for 2h can reach 75%.
Description
Technical Field
The invention relates to a method for recovering tungstate radicals in beneficiation wastewater.
Background
At present, the recovery rate of scheelite beneficiation wastewater is not high, and particularly, beneficiation wastewater of sulfide ore and oxide ore symbiotic ore is mostly discharged up to the standard or only a small part of the beneficiation wastewater can be recovered. The concentration of heavy metal, suspended solid, chemical oxygen demand and the like in the mineral processing wastewater greatly exceed the national standard, and the influence on the periphery of a mineral processing plant is easily caused. Therefore, if the ore dressing wastewater can be harmlessly recycled, the environmental pollution can be controlled, the water resource can be saved, and huge social and economic benefits can be generated.
The recovery process of metal ions mainly comprises the following steps: chemical precipitation, redox, biological treatment, adsorption, and the like. The adsorption method is not only low in cost, but also not easy to cause secondary pollution, and is an effective method. The adsorption method can be divided into physical adsorption and chemical adsorption, wherein the chemical adsorption means that an adsorbent and an adsorbate undergo a chemical reaction to form a firm adsorption chemical bond or a surface complex, molecules of the adsorbate cannot move on the surface, and the adsorption capacity of the adsorption method is generally much stronger than that of physical adsorption.
Polyaniline is a conductive polymer and has three different forms of emeraldine salt form, fully reduced form and fully oxidized form. The polyaniline in emeraldine salt form has a large number of positive charges on the surface, and can adsorb most of anion ions.
Disclosure of Invention
The invention provides a method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater, aiming at solving the technical problems of low recovery rate and low recovery rate of tungstate radicals in scheelite beneficiation wastewater in the prior art.
The method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater comprises the following steps:
connecting a polyaniline/carbon cloth composite electrode material, an Ag/AgCl electrode and a platinum electrode to an electrochemical workstation to form a three-electrode system, wherein the polyaniline/carbon cloth composite electrode material is used as a working electrode, the Ag/AgCl electrode is used as a reference electrode, the platinum electrode is used as a counter electrode, scheelite beneficiation wastewater to be treated is used as electrolyte, and the electroadsorption is carried out for 2 to 6 hours under the condition that the voltage is 0.5 to 1.2V;
the preparation method of the polyaniline/carbon cloth composite electrode material comprises the following steps:
firstly, adding carbon cloth and aniline into HCl aqueous solution, completely immersing the carbon cloth into the mixed solution, and then carrying out ultrasonic treatment for 30-40 min to disperse the aniline on the surface of the carbon cloth;
the concentration of the HCl aqueous solution is 0.1-0.12 mol/L;
the volume ratio of the aniline to the HCl aqueous solution is 1 (30-35);
secondly, adding ammonium persulfate into HCl aqueous solution, and dissolving by ultrasonic wave;
the concentration of the HCl aqueous solution is 0.1-0.12 mol/L;
the volume ratio of the mass of the ammonium persulfate to the HCl aqueous solution is (0.5 g-0.6 g) 15 mL;
thirdly, dropwise adding the solution subjected to the ultrasonic treatment in the second step into the solution subjected to the ultrasonic treatment in the first step, and then putting the solution into a constant-temperature oscillator to perform constant-temperature oscillation for 12-15 h at the temperature of 8-10 ℃; taking out the carbon cloth, washing the carbon cloth by deionized water, and drying the carbon cloth at the temperature of 50-60 ℃ to obtain the polyaniline/carbon cloth composite electrode material; the volume ratio of the solution subjected to the ultrasonic treatment in the second step to the solution subjected to the ultrasonic treatment in the first step is 1 (1-1.1).
The invention discloses a polyaniline/carbon cloth composite electrode material, which provides an adsorption site for tungstate radicals through in-situ polymerization of aniline on the surface of carbon cloth. The material shows good effect to tungstate radical's absorption to because this material is electrode material, can strengthen the adsorption efficiency of material to tungstate radical after through exerting certain electric field force, and easily with the water separation, be difficult for causing secondary pollution, convenient the recovery.
The method has simple and rapid process, and the recovery rate of absorbing tungstate ions for 2h can reach 75%.
The polyaniline/carbon cloth composite electrode material can be used as an adsorbent to effectively adsorb tungstate radicals in a water body, the recovery rate of tungstate radical ions can reach 75%, and the recovery of tungsten in mineral processing wastewater is realized.
Drawings
FIG. 1 is an SEM image of the carbon cloth in step one of experiment one;
fig. 2 is an SEM image of a polyaniline/carbon cloth composite electrode material prepared in experiment one;
FIG. 3 is a plot of cyclic voltammograms for run two;
FIG. 4 is a data diagram of the adsorption capacity of the polyaniline/carbon cloth composite electrode material to tungstate ions in test III;
FIG. 5 is a cyclic voltammogram from run four;
FIG. 6 is a graph of tungstate adsorbed at different voltages versus time for test five.
Detailed Description
The first embodiment is as follows: the embodiment is a method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater, which comprises the following specific steps:
a polyaniline/carbon cloth composite electrode material, an Ag/AgCl electrode and a platinum electrode form a three-electrode system and are connected to an electrochemical workstation, the polyaniline/carbon cloth composite electrode material is used as a working electrode, the Ag/AgCl electrode is used as a reference electrode, the platinum electrode is used as a counter electrode, scheelite beneficiation wastewater to be treated is used as electrolyte, and electro-adsorption is carried out for 2-6 hours under the condition that the voltage is 0.5-1.2V.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the preparation method of the polyaniline/carbon cloth composite electrode material comprises the following steps:
firstly, adding carbon cloth and aniline into HCl aqueous solution, completely immersing the carbon cloth into the mixed solution, and then carrying out ultrasonic treatment for 30-40 min to disperse the aniline on the surface of the carbon cloth;
the concentration of the HCl aqueous solution is 0.1-0.12 mol/L;
the volume ratio of the aniline to the HCl aqueous solution is 1 (30-35);
secondly, adding ammonium persulfate into HCl aqueous solution, and dissolving by ultrasonic wave;
the concentration of the HCl aqueous solution is 0.1-0.12 mol/L;
the volume ratio of the mass of the ammonium persulfate to the HCl aqueous solution is (0.5 g-0.6 g) 15 mL;
thirdly, dropwise adding the solution subjected to the ultrasonic treatment in the second step into the solution subjected to the ultrasonic treatment in the first step, and then putting the solution into a constant-temperature oscillator to perform constant-temperature oscillation for 12-15 h at the temperature of 8-10 ℃; taking out the carbon cloth, washing the carbon cloth by deionized water, and drying the carbon cloth at the temperature of 50-60 ℃ to obtain the polyaniline/carbon cloth composite electrode material; the volume ratio of the solution subjected to the ultrasonic treatment in the second step to the solution subjected to the ultrasonic treatment in the first step is 1 (1-1.1). The rest is the same as the first embodiment.
The third concrete implementation mode: the first difference between the present embodiment and the specific embodiment is: electro-adsorbing for 2-3 h under the condition of 1V voltage. The rest is the same as the first embodiment.
The fourth concrete implementation mode: the second embodiment is different from the first embodiment in that: the carbon cloth described in the first step was the HCP 331N. The rest is the same as the second embodiment.
The fifth concrete implementation mode: the second embodiment is different from the first embodiment in that: the concentration of the HCl aqueous solution in the first step is 0.1 mol/L. The rest is the same as the second embodiment.
The sixth specific implementation mode: the second embodiment is different from the first embodiment in that: the volume ratio of the aniline to the HCl aqueous solution in the step one is 1: 33.3. The rest is the same as the second embodiment.
The seventh embodiment: the second embodiment is different from the first embodiment in that: and the concentration of the HCl aqueous solution in the second step is 0.1 mol/L. The rest is the same as the second embodiment.
The specific implementation mode is eight: the second embodiment is different from the first embodiment in that: and the volume ratio of the mass of the ammonium persulfate to the volume of the HCl aqueous solution in the second step is 0.548g to 15 mL. The rest is the same as the second embodiment.
The specific implementation method nine: the second embodiment is different from the first embodiment in that: in the third step, the solution obtained after the ultrasonic treatment in the second step is dripped into the solution obtained after the ultrasonic treatment in the first step, and then the solution is placed in a constant temperature oscillator to be subjected to constant temperature oscillation for 12 hours at the temperature of 8 ℃; and taking out the carbon cloth, washing the carbon cloth by using deionized water, and drying the carbon cloth at the temperature of 50 ℃ to obtain the polyaniline/carbon cloth composite electrode material. The rest is the same as the second embodiment.
The invention was verified with the following tests:
test one: the test is a preparation method of a polyaniline/carbon cloth composite electrode material, and the preparation method comprises the following specific steps:
firstly, adding carbon cloth and aniline into HCl aqueous solution, completely immersing the carbon cloth into the mixed solution, and then carrying out ultrasonic treatment for 30-40 min to disperse the aniline on the surface of the carbon cloth;
the concentration of the HCl aqueous solution is 0.1-0.12 mol/L;
the volume ratio of the aniline to the HCl aqueous solution is 1 (30-35);
the model of the carbon cloth in the first step is HCP 331N;
secondly, adding ammonium persulfate into HCl aqueous solution, and dissolving by ultrasonic wave;
the concentration of the HCl aqueous solution is 0.1-0.12 mol/L;
the volume ratio of the mass of the ammonium persulfate to the HCl aqueous solution is (0.5 g-0.6 g) 15 mL;
thirdly, dropwise adding the solution subjected to the ultrasonic treatment in the second step into the solution subjected to the ultrasonic treatment in the first step, and then putting the solution into a constant-temperature oscillator to perform constant-temperature oscillation for 12-15 h at the temperature of 8-10 ℃; and taking out the carbon cloth, washing the carbon cloth by using deionized water, and drying the carbon cloth at the temperature of between 50 and 60 ℃ to obtain the polyaniline/carbon cloth composite electrode material.
Fig. 1 is an SEM image of the carbon cloth in the first step of the first test, and it can be seen from fig. 1 that the carbon cloth is formed by interweaving a plurality of carbon fibers, and has tight connection and smooth surface, and the structure of the carbon cloth is favorable for the growth and fixation of polyaniline.
Fig. 2 is an SEM image of the polyaniline/carbon cloth composite electrode material prepared in the first experiment, and it can be seen from the SEM image that polyaniline uniformly grows on the surface of the carbon cloth, not only increasing the specific surface area of the carbon cloth, but also providing effective adsorption sites for the adsorption of tungstate radicals.
And (2) test II: and (3) connecting a three-electrode system consisting of the polyaniline/carbon cloth composite electrode material prepared in the first test, an Ag/AgCl electrode and a platinum electrode to an electrochemical workstation (Shanghai Chenghua electrochemical workstation CHI760E), and performing CV cyclic voltammetry scanning in 1mol/L sodium sulfate aqueous solution, wherein the scanning range is 0.2V-0.6V, and the scanning speed is 50 mV/s.
Fig. 3 is a cyclic voltammetry graph of a second test, in which a curve 1 is the polyaniline/carbon cloth composite electrode material prepared in the first test, and a curve 2 is the carbon cloth in the first test, and it can be seen from the graph that the polyaniline/carbon cloth composite electrode material has a larger electrochemical specific surface area and better electrochemical performance.
And (3) test III: the test is an influence test of pH on the adsorption of tungstate radicals by the polyaniline/carbon cloth composite electrode material, and comprises the following specific steps:
firstly, preparing 8 parts of 100mL of 10mg/L tungstate aqueous ion solution, and then respectively adjusting the pH values of the 8 parts of solution to be 2, 3, 4, 5, 6, 7, 8 and 9 by using 0.1mol/L hydrochloric acid aqueous solution and 0.1mol/L sodium hydroxide aqueous solution;
secondly, respectively adding a piece of polyaniline/carbon cloth composite electrode material prepared in the first test into 8 parts of solution, and then placing the mixture into a constant-temperature oscillator to oscillate for 4 hours at a constant temperature of 25 ℃;
and thirdly, respectively measuring the change of the concentration of tungstate ions before and after adsorption by using an ultraviolet spectrophotometer, and calculating the adsorption quantity.
The formula for calculating the adsorption amount is as follows:
q: the adsorption capacity (mg/g) of the material after 4h of adsorption,
C0: initial concentration of tungstate ions (mg/L),
Ce: the concentration (mg/L) of tungstate ions after 4 hours of adsorption,
v: the volume of the initial solution (L),
m: and (g) the mass of the adsorbent is the mass difference between the polyaniline/carbon cloth composite electrode material prepared in the first test and the carbon cloth prepared in the first test.
Fig. 4 is a data diagram of the adsorption capacity of the polyaniline/carbon cloth composite electrode material to tungstate ions in the third test, and it can be seen from the data diagram that the polyaniline/carbon cloth composite electrode material has the best adsorption performance to tungstate ions under the condition that the pH is 7, mainly because tungstate ions mainly exist in the form of poly tungstate ions under the acidic condition, and have a larger molecular weight and are not easy to adsorb. When the pH is alkaline, polyaniline on the carbon cloth easily falls off, resulting in deterioration of the adsorption performance.
And (4) testing: the test researches the oxidation-reduction potential of the polyaniline/carbon cloth material, and comprises the following specific test steps:
and (3) connecting a three-electrode system consisting of the polyaniline/carbon cloth composite electrode material prepared in the first test, an Ag/AgCl electrode and a platinum electrode to an electrochemical workstation (Shanghai Chenghua electrochemical workstation CHI760E), performing CV cyclic voltammetry scanning in 1mol/L sodium sulfate aqueous solution at a scanning range of-0.5V-1.5V and a scanning speed of 50mV/s to obtain a cyclic voltammetry curve, and observing the position of an oxidation reduction peak of the cyclic voltammetry curve.
FIG. 5 is a cyclic voltammogram of experiment IV, and it can be seen that the material shows an oxidation peak at about 1.2V and a reduction peak at about 0.8V. It can be demonstrated that polyaniline grows on the surface of the carbon cloth. The polyaniline can be reduced from an emeraldine salt form to a fully reduced form by applying a voltage of 0.8V or less, and can be oxidized from an emeraldine salt form to a fully oxidized form by applying a voltage of 1.2V or more. And the two structures have no good adsorption performance on tungstate radicals.
And (5) testing: the test is used for testing the influence of the electrifying condition on the adsorption performance of the polyaniline/carbon cloth composite electrode material, and comprises the following specific test steps:
the polyaniline/carbon cloth composite electrode material prepared in the first test, an Ag/AgCl electrode and a platinum electrode were connected to an electrochemical workstation (shanghai chenhua electrochemical workstation CHI760E), 100mL of 50mg/L tungstate aqueous solution was used as an electrolyte solution, and electro-adsorption was performed by a current-time method, and the polyaniline/carbon cloth composite electrode material was divided into 4 groups, which were no voltage applied, 0.5V applied, 1V applied, and 1.5V applied, and sampling was performed at each time interval. And then, respectively measuring the change of the concentration of tungstate ions in each group of samples by using an ultraviolet spectrophotometer.
FIG. 6 is a curve of the relation between tungstate radicals adsorbed at different voltages and time in the fifth test, wherein a is 1V, ● is 0.5V, ■ is no voltage, and a t is 1.5V, and it can be seen from the figure that the adsorption performance of the material is improved to a certain extent when the voltage is applied to 1V and 0.5V; the adsorption performance of the material is rather deteriorated when the applied voltage is 1.5V, because polyaniline is oxidized from the emeraldine salt form to the completely oxidized state at 1.5V to cause deterioration of the adsorption performance thereof; when 1V voltage is applied, tungstate ions in the solution are gathered on the surface of the electrode under the driving of the voltage, so that the material is more favorably adsorbed, and the recovery rate of the tungstate ions reaches 75%.
Claims (9)
1. A method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater is characterized in that the method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater comprises the following steps:
a polyaniline/carbon cloth composite electrode material, an Ag/AgCl electrode and a platinum electrode form a three-electrode system and are connected to an electrochemical workstation, the polyaniline/carbon cloth composite electrode material is used as a working electrode, the Ag/AgCl electrode is used as a reference electrode, the platinum electrode is used as a counter electrode, scheelite beneficiation wastewater to be treated is used as electrolyte, and electro-adsorption is carried out for 2-6 hours under the condition that the voltage is 0.5-1.2V.
2. The method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater according to claim 1, wherein the preparation method of the polyaniline/carbon cloth composite electrode material is as follows:
firstly, adding carbon cloth and aniline into HCl aqueous solution, completely immersing the carbon cloth into the mixed solution, and then carrying out ultrasonic treatment for 30-40 min;
the concentration of the HCl aqueous solution is 0.1-0.12 mol/L;
the volume ratio of the aniline to the HCl aqueous solution is 1 (30-35);
secondly, adding ammonium persulfate into HCl aqueous solution, and dissolving by ultrasonic wave;
the concentration of the HCl aqueous solution is 0.1-0.12 mol/L;
the volume ratio of the mass of the ammonium persulfate to the HCl aqueous solution is (0.5 g-0.6 g) 15 mL;
thirdly, dropwise adding the solution subjected to the ultrasonic treatment in the second step into the solution subjected to the ultrasonic treatment in the first step, and then putting the solution into a constant-temperature oscillator to perform constant-temperature oscillation for 12-15 h at the temperature of 8-10 ℃; taking out the carbon cloth, washing the carbon cloth by deionized water, and drying the carbon cloth at the temperature of 50-60 ℃ to obtain the polyaniline/carbon cloth composite electrode material; the volume ratio of the solution subjected to the ultrasonic treatment in the second step to the solution subjected to the ultrasonic treatment in the first step is 1 (1-1.1).
3. The method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater according to claim 1, wherein the method is characterized in that electro-adsorption is carried out for 2-3 hours under the condition that the voltage is 1V.
4. The method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater according to claim 2, wherein the type of the carbon cloth in the first step is HCP 331N.
5. The method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater according to claim 2, wherein the concentration of the HCl aqueous solution in the first step is 0.1 mol/L.
6. The method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater according to claim 2, wherein the volume ratio of aniline to HCl aqueous solution in the first step is 1: 33.3.
7. The method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater according to claim 2, wherein the concentration of the HCl aqueous solution in the second step is 0.1 mol/L.
8. The method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater according to claim 2, wherein the volume ratio of the mass of ammonium persulfate to the volume of the HCl aqueous solution in the second step is 0.548g:15 mL.
9. The method for recovering and adsorbing tungstate radicals in scheelite beneficiation wastewater according to claim 2, wherein in the third step, the solution subjected to ultrasonic treatment in the second step is dropwise added into the solution subjected to ultrasonic treatment in the first step, and then the solution is placed in a constant temperature oscillator and subjected to constant temperature oscillation at the temperature of 8 ℃ for 12 hours; and taking out the carbon cloth, washing the carbon cloth by using deionized water, and drying the carbon cloth at the temperature of 50 ℃ to obtain the polyaniline/carbon cloth composite electrode material.
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| ZHAO, XS等: "In situ preparation of highly stable polyaniline/W18O49 hybrid nanocomposite as efficient visible light photocatalyst for aqueous Cr(VI) reduction", 《JOURNAL OF HAZARDOUS MATERIALS》 * |
| 张蚰: "基于聚苯胺的电吸附法处理含铅离子废水的研究", 《常州大学学报（自然科学版）》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111392825A (en) * | 2020-03-11 | 2020-07-10 | 南昌航空大学 | Method for selectively adsorbing lead ions in heavy metal wastewater by electric field enhancement |
| CN111392825B (en) * | 2020-03-11 | 2021-12-07 | 南昌航空大学 | Method for selectively adsorbing lead ions in heavy metal wastewater by electric field enhancement |
| CN113684380A (en) * | 2021-08-30 | 2021-11-23 | 中南大学 | Tungsten extraction process and application thereof |
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|---|---|
| CN110642335B (en) | 2021-12-07 |
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