CN109364871B - Oxygen-deficient tungsten trioxide nanosheet adsorbent and preparation method thereof - Google Patents
Oxygen-deficient tungsten trioxide nanosheet adsorbent and preparation method thereof Download PDFInfo
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Abstract
The invention relates to an oxygen-deficient tungsten trioxide nanosheet adsorbent and a preparation method thereof. The oxygen-deficient tungsten trioxide nanosheet adsorbent is prepared from WO3The quantum dots are calcined in a reducing atmosphere-a mixed gas of argon and hydrogen. Because of the presence of the reducing gas H2From WO3Deprives lattice oxygen in the crystal lattice of (1), forming an oxygen-rich defect of WO3Nanosheets. The adsorption performance experiment shows that the tungsten trioxide has higher adsorption performance compared with the traditional tungsten trioxide, has good application prospect and economic benefit in the aspect of sewage treatment, and can be applied to the field of environmental management as an environmental functional material.
Description
Technical Field
The invention relates to the field of environment functional materials, in particular to an oxygen-deficient tungsten trioxide nanosheet adsorbent and a preparation method thereof.
Background
With the development of industry, the environmental pollution problem, especially the organic dye pollution problem in water body, is more serious, and the high toxicity and carcinogenicity thereof threaten the health of human body and organism. Effective removal of water pollutants is therefore critical for environmental remediation, and adsorption is currently one of the most widely used methods because it is easy to design and operate and exhibits great flexibility. Common organic dye adsorbents include clay minerals, zeolites, polymeric materials, and activated carbon, with activated carbon being the most widely used. However, the activated carbon regeneration temperature is high, so that the commercialization of the activated carbon adsorption system is difficult, and the development of practical application thereof is limited.
Metal oxides (including tin oxide, zinc oxide, iron oxide, manganese oxide, and the like) are considered as a novel adsorbent because the regeneration temperature is lower than that of activated carbon and the preparation process is simple; however, the adsorption capacity of the metal oxide is low. Tungsten trioxide (WO)3) As a metal semiconductor material of n-type Lewis acid, the metal semiconductor material has high stability and is widely applied to the field of environmental pollution treatment, but the metal semiconductor material has low adsorption capacity and slow adsorption kinetics, and in order to improve WO3Adsorption capacity and adsorption kinetics, development of WO with high adsorption capacity3Adsorbents are at hand.
Disclosure of Invention
The invention aims to overcome the technical defects in the prior art, solve the problems of low adsorption capacity and slow adsorption kinetics of tungsten trioxide, and provide an oxygen-deficient tungsten trioxide nanosheet adsorbent with high-efficiency adsorption capacity of organic micromolecular dyes and a preparation method thereof, so that the treatment efficiency of water pollutants is effectively improved and enhanced.
The technical purpose is realized by the following technical scheme:
in one aspect, the invention provides an oxygen-deficient tungsten trioxide nanosheet adsorbent prepared from WO3Quantum dots in Ar/H2Obtained after calcination in a mixed reducing atmosphere, WO3Quantum dot assembly to form WO3Nanosheets, WO3A large number of oxygen defects exist on the surface of the nanosheet, and the specific surface area and active sites of adsorption are increased.
On the other hand, the invention also provides a preparation method of the oxygen-deficient tungsten trioxide nanosheet adsorbent, which comprises the following preparation steps:
adding tungsten hexachloride into oleic acid and oleylamine to form a mixed solution A, performing ultrasonic dispersion on the mixed solution, adding ethanol when the mixed solution is transparent, and continuing performing ultrasonic dispersionObtaining a mixed solution B, putting the mixed solution B into a high-pressure kettle for reaction, centrifugally separating to prepare tungsten oxide quantum dots, and drying the prepared tungsten oxide quantum dots in vacuum; putting the dried tungsten oxide quantum dots in Ar/H2Calcining the mixture in a mixed reducing atmosphere to prepare the oxygen-deficient tungsten trioxide nanosheet adsorbent.
Preferably, the proportion of the tungsten hexachloride, the oleic acid, the oleylamine and the ethanol is 1-1.7 mmol: 10-20 mL: 0-2.5 mL: 0-10 mL.
The reaction temperature in the autoclave is 180-220 ℃, and the reaction time is 3-24 h;
the volume ratio of the argon to the hydrogen is 5: 95, wherein the gas flow is 50 mL/min;
the calcination temperature is 550 ℃, and the calcination time is 4-8 h.
In a further aspect, the invention further provides application of the prepared oxygen-deficient tungsten trioxide nanosheet adsorbent in adsorption of organic small molecule dye, and according to an embodiment of the invention, the oxygen-deficient WO provided by the invention3Methyl Orange (MO) in water can be completely removed after the nano-sheets are adsorbed for 10min in a dark state, and the adsorption capacity can reach 63.75 microgram-1. Has good adsorption effect on methylene blue and rhodamine B.
Compared with the prior art, the invention has the beneficial effects that:
the invention prepares WO3After quantum dots are subjected to calcination under the mixed gas of argon and hydrogen by regulating the calcination atmosphere, the oxygen-deficient WO containing a large number of oxygen defects is prepared3Nanosheets; because of the presence of the reducing gas H2From WO3Deprives lattice oxygen in the crystal lattice of (1), forming an oxygen-rich defect of WO3Nanosheets. Due to the presence of oxygen deficiency, oxygen deficient WO3The specific surface area of the nano-sheet is increased, the surface active sites are increased, and the traditional WO is avoided3WO of nanosheets3The agglomeration of the nano particles is solved, more active sites are provided for the adsorption of the target pollutants, and the adsorption capacity and the adsorption rate of the target pollutants can be improved. Compared with the conventional method at N2And WO prepared in air3The adsorption capacity and efficiency of the nano-sheets are greatly improved.
Meanwhile, the preparation method is simple to operate, the reagents are cheap, and the preparation method can be used for large-scale low-cost preparation3The nanosheet has a good adsorption effect on anionic dyes such as Methyl Orange (MO), methylene blue and rhodamine B, and has a good application prospect and economic benefits in the aspects of sewage treatment and the like.
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FIG. 1 shows WO prepared in three different calcination atmospheres in examples 2-43Transmission electron microscopy of the adsorbent: wherein, FIG. 1 (A) is WO3（Ar/H2) FIG. 1 (B) is WO3（N2) FIG. 1 (C) is WO3（Air）；
FIG. 2 shows the preparation of WO under different calcination atmospheres in examples 2-43The adsorption performance of the adsorbent to the dye MO is shown;
FIG. 3 shows different amounts of WO3（Ar/H2) And (3) a graph of the adsorption performance of the adsorbent to the dye MO.
Detailed Description
The invention is further illustrated by the following examples. Materials, reagents and the like used in examples are commercially available unless otherwise specified. The present invention will be described in further detail with reference to examples.
Example 1: WO3Preparation of quantum dots
1.7mmol (0.674 g) WCl6Placing the mixture into a beaker, adding 20mL of oleic acid and 2.5mL of oleylamine into the beaker, placing the mixture into an ultrasonic cleaning machine for ultrasonic dispersion, adding 10mL of ethanol for continuous ultrasonic treatment when the solution is transparent, pouring the dispersed mixture into a 50mL reaction kettle, placing the mixture into an oven, heating the mixture to 180 ℃, keeping the reaction for 3 hours, quickly cooling the mixture to room temperature after the reaction is finished, respectively washing the mixture with water and ethanol, and placing the mixture into a vacuum oven for drying to obtain WO3And (4) quantum dots.
Example 2: oxygen-deficient tungsten trioxide nanosheetPreparation: WO3（Ar/H2）
Take 0.3gWO3Putting quantum dots into a crucible, putting into a tubular furnace with programmed temperature, and performing Ar/H reaction2(v/v, 5%/95%) gas flow rate is 50mL/min, and the temperature is raised from room temperature to 550 ℃ at 5 ℃/min, and the temperature is kept for 4h, and the oxygen-deficient WO is obtained after cooling and grinding3Nanosheet WO3（Ar/H2）。
Example 3: n is a radical of2Preparation of WO by atmospheric calcination3Nanosheet: WO3（N2）
0.3gWO3Putting quantum dots into a crucible, putting the crucible into a tube furnace, and reacting in N2Under the atmosphere, the gas flow rate is 50mL/min, the temperature is raised from room temperature to 550 ℃ at the speed of 5 ℃/min, the temperature is kept for 4h, and the WO is obtained after cooling and grinding3（N2）。
Example 4: preparation of WO by calcination in air atmosphere3Nanosheet: WO3（Air）
0.3gWO3Putting the quantum dots into a crucible, putting the crucible into a tube furnace, heating the quantum dots to 550 ℃ at the speed of 50mL/min in the Air (Air) atmosphere at the speed of 5 ℃/min, keeping the temperature for 4h, cooling and grinding to obtain WO3（Air）。
FIG. 1 shows WO prepared in three different calcination atmospheres in examples 2-43Transmission electron micrograph of nanoplatelets (50 nm): wherein FIG. 1 (A) is Ar/H2WO prepared under calcination atmosphere3（Ar/H2) Nanosheets; FIG. 1 (B) is N2WO prepared under calcination atmosphere3（N2) Nanosheets; FIG. 1 (C) shows WO prepared in an atmosphere of air calcination3(Air) nanoplatelets. WO in FIG. 1 (A) as shown in FIG. 13（Ar/H2) The size of the nano sheet is 10-15nm, and the surface of the nano sheet is assembled by a plurality of nano particles, so that the nano sheet has more adsorption sites; WO in FIG. 1 (B)3（N2) Nanosheet at N2After atmosphere calcination of WO3The aggregation degree of the particles is increased, the aggregation is obvious, and the adsorption sites are reduced; FIG. 1 (C) WO3The flake size of the (Air) nanosheet after calcination in Air becomes large, about20 to 50nm, and WO3（Ar/H2) Adsorption sites are reduced compared to a reduction in surface small particles. At the same time, WO is calcined in different atmospheres by Table 13And analyzing the element composition of the nano material so as to determine the relative content of the material to the adsorption sites of the organic small molecule dye.
TABLE 1 WO calcination under blind atmosphere conditions3Element composition table of nano material
| Catalyst and process for preparing same | O/W ratio column | C/W ratio column | N/W ratio column | N/C ratio column |
| WO3(Ar/H2) | 1.505 | 0.7295 | 0.1563 | 0.2143 |
| WO3(N2) | 2.357 | 0.9821 | 0.3367 | 0.3429 |
| WO3(Air) | 2.991 | 1.049 | 0.3598 | 0.3429 |
As can be seen from Table 1: WO3（Ar/H2）、WO3（N2) And WO3(Air) the molar ratios of the O/W elements of the three are 1.505, 2.357 and 2.991, respectively, as indicated in Ar/H2WO calcined in mixed atmosphere3There are more oxygen defects, which provide more adsorption sites for efficient adsorption of the target contaminants.
Example 5: WO prepared in examples 2 to 43（Ar/H2）、WO3（N2) And WO3(Air) MO adsorption test
(1) 25mg of WO prepared in examples 2 to 4 were weighed out separately3（Ar/H2）、WO3（N2) And WO3(Air) was placed in a 100mL light reaction flask and 50mL of methyl orange aqueous solution (10 mg.L) was added-1) Placing the light reaction bottle in a light reaction instrument;
(2) magnetically stirring without visible light irradiation, and extracting 5mL of sample every 10min and centrifuging;
(3) the supernatant of (2) was taken out in a cuvette and measured at a wavelength of 463nm using a liquid ultraviolet-visible spectrophotometer (UV-2450), and the change in absorbance of the solution was recorded. FIG. 2 is WO3（Ar/H2）、WO3（N2) And WO3(Air) adsorption performance diagram of the nanoplatelets towards the dye MO; as shown in FIG. 2, WO3（Ar/H2) The adsorption performance to methyl orange is best and the adsorption rate is fastest. Therefore, the existence of oxygen defects can increase the adsorption capacity and adsorption rate of MO, and the removal efficiency of environmental pollutants is improved.
Example 6: WO3（Ar/H2) Effect of adsorbent dosage on MO adsorption
(1) 5mg, 10mg, 15mg and 25mg of WO prepared in example 2 were weighed out separately3（Ar/H2) Putting the mixture into a 100mL light reaction bottle, and respectively adding 50mL of the mixture with different concentrations (10-40 mg.L)-1) Placing the light reaction bottle in a light reaction instrument;
(2) magnetically stirring without visible light irradiation, extracting 5mL of sample after 120min, and centrifuging;
(3) taking the supernatant in (2) and measuring in a cuvette at a wavelength of 463nm by using a liquid ultraviolet-visible spectrophotometer (UV-2450), recording the change of absorbance of the solution, and FIG. 3 shows different amounts of the adsorbent WO3（Ar/H2) A graph of adsorption performance to dye MO; as can be seen from FIG. 3, the experimental result shows that when the dosage of the adsorbent is 5mg, the adsorption capacity of the adsorbent per unit mass to MO is the best, and the adsorption capacity can reach 63.75 mug-1. After the dosage of the adsorbent is increased, the adsorbent interacts with each other, and the adsorption effect is influenced.
Example 7: WO3（Ar/H2) Adsorption of adsorbent to other organic small molecular dye
(1) 25mg of WO prepared in example 2 above were weighed out separately3（Ar/H2) Put into a 100mL light reaction bottle, and 50mL rhodamine B and methylene blue aqueous solution (10 mg.L) are respectively added-1) Placing the light reaction bottle in a light reaction instrument;
(2) magnetically stirring without visible light irradiation, extracting 5mL of sample after 120min, and centrifuging;
(3) taking the supernatant in the step (2), measuring the supernatant in a cuvette by using a liquid ultraviolet visible spectrophotometer (UV-2450) at a wavelength of 463nm, and recording the change of the absorbance of the solution;
TABLE 2 Absorbance Change of example 7 solution
From the analysis of Table 2, WO3（Ar/H2) The adsorption rate of rhodamine B and methylene blue can reach more than 99 percent within 120 min. Thus, it is found that in Ar/H2Oxygen defects produced in an atmosphereForm WO3Has universal adsorbability to organic small molecule dyes.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (7)
1. Oxygen-deficient WO3The preparation method of the nanosheet adsorbent is characterized by comprising the following steps:
adding tungsten hexachloride into oleic acid and oleylamine to form a mixed solution A, performing ultrasonic dispersion on the mixed solution, adding ethanol when the mixed solution is transparent, continuing the ultrasonic dispersion to obtain a mixed solution B, putting the mixed solution B into a high-pressure kettle for reaction, and performing centrifugal separation to prepare WO3Quantum dot, WO to be prepared3Drying the quantum dots in vacuum; WO to be dried3The quantum dots are placed in the mixed gas atmosphere of argon and hydrogen to be calcined to prepare the oxygen-deficient WO3A nanosheet adsorbent; the proportion of the tungsten hexachloride, the oleic acid, the oleylamine and the ethanol is 1.7 mmol: 20mL of: 2.5 mL: 10 mL.
2. An oxygen-deficient WO according to claim 13The preparation method of the nanosheet adsorbent is characterized in that the reaction temperature in the autoclave is 180-220 ℃, and the reaction time is 3-24 hours.
3. An oxygen-deficient WO according to claim 13The preparation method of the nanosheet adsorbent is characterized in that the volume ratio of the argon to the hydrogen is 5: 95.
4. An oxygen-deficient WO according to claim 13The preparation method of the nanosheet adsorbent is characterized in that the gas flow is 50 mL/min.
5. According to claimAn oxygen-deficient WO according to claim 13The preparation method of the nanosheet adsorbent is characterized in that the calcining temperature is 550 ℃, and the calcining time is 4-8 h.
6. An oxygen-deficient WO according to claim 13The adsorbent prepared by the preparation method of the nanosheet adsorbent is applied to the adsorption of organic micromolecular dyes.
7. The use according to claim 6, wherein the organic small molecule dye is methyl orange, rhodamine B or methylene blue.
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| CN110314678A (en) * | 2019-07-12 | 2019-10-11 | 河北德龙环境工程股份有限公司 | A kind of ozone catalyst and preparation method thereof and the method for handling industrial wastewater |
| CN110538654A (en) * | 2019-08-23 | 2019-12-06 | 江苏大学 | Visible light response type Ag/WO3 binary composite photocatalyst and preparation method thereof |
| CN112844371A (en) * | 2021-02-03 | 2021-05-28 | 黑河学院 | Catalyst for photolysis of water to produce oxygen and preparation method thereof |
| CN114950435B (en) * | 2022-06-21 | 2023-02-03 | 阜阳师范大学 | Preparation method of cobalt oxide catalyst, product and application thereof |
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