CN109364871A - A kind of oxygen defect type tungstic trioxide nano-slice adsorbent and preparation method thereof - Google Patents
A kind of oxygen defect type tungstic trioxide nano-slice adsorbent and preparation method thereof Download PDFInfo
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- CN109364871A CN109364871A CN201811305929.XA CN201811305929A CN109364871A CN 109364871 A CN109364871 A CN 109364871A CN 201811305929 A CN201811305929 A CN 201811305929A CN 109364871 A CN109364871 A CN 109364871A
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/00—Treatment of water, waste water, or sewage
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Abstract
The present invention relates to a kind of oxygen defect type tungstic trioxide nano-slice adsorbents and preparation method thereof.The oxygen defect type tungstic trioxide nano-slice adsorbent is by WO3Quantum dot is calcined under the gaseous mixture of reducing atmosphere-argon gas and hydrogen.Because there is reducibility gas H2Presence, from WO3Lattice in capture Lattice Oxygen, form the WO rich in oxygen defect3Nanometer sheet.Absorption property experiment shows relative to traditional tungstic acid absorption property with higher, has a good application prospect in terms of sewage treatment and economic benefit, can be used as a kind of environment functional material and is applied to field of environmental improvement.
Description
Technical field
The present invention relates to environment functional material fields, and in particular to be a kind of absorption of oxygen defect type tungstic trioxide nano-slice
Agent and preparation method thereof.
Background technique
With the development of industry, the organic dyestuff pollution problem in problem of environmental pollution especially water body is more serious,
High toxicity and carcinogenicity have threatened the health of human body and biology.Therefore the pass that water pollutant is environmental improvement is effectively removed
Key, absorption method is one of most widely used method at present, because its easily designed and operation, and show very big flexible
Property.The machine dye sorbent of common are includes clay mineral, zeolite, high molecular material and active carbon, and wherein active carbon is answered
With the most extensively.However, the regeneration temperature due to active carbon is high, so that the commercialization difficulty of activated carbon adsorption system is larger, limit
The development of its practical application is made.
Metal oxide (including tin oxide, zinc oxide, iron oxide and manganese oxide etc.) is since its regeneration temperature is lower than work
Property charcoal, and preparation process is simple and be considered as a kind of new adsorbent；However, the adsorption capacity of metal oxide is low.Three oxygen
Change tungsten (WO3) it is used as a kind of lewis acidic metal semiconductor material of N-shaped, have higher stability and is widely used
In environmental pollution treatment field, but its attached capacity is low and adsorption dynamics adsorption kinetics is slow, in order to improve WO3Adsorption capacity and absorption power
It learns, develops the WO with high-adsorption-capacity3Adsorbent is extremely urgent.
Summary of the invention
It is an object of the invention to overcome technological deficiency existing in the prior art, solve tungstic acid adsorption capacity it is low with
And the problem that adsorption dynamics adsorption kinetics is slow, a kind of oxygen defect type tungstic acid with efficient absorption small organic molecule dyestuff ability is provided
Nanometer sheet adsorbent and preparation method thereof, to be effectively improved and be promoted the treatment effeciency of water pollutant.
Above-mentioned technical purpose that the invention is realized by the following technical scheme:
On the one hand, the present invention provides a kind of oxygen defect type tungstic trioxide nano-slice adsorbent, the adsorbent is by WO3Quantum dot
In Ar/H2It is obtained after being calcined under mixed reducing atmosphere, WO3Quantum dot assembles to form WO3Nanometer sheet, WO3It deposits on nanometer sheet surface
In a large amount of oxygen defect, the specific surface area and active site of absorption are increased.
On the other hand, the present invention also provides a kind of preparation method of oxygen defect type tungstic trioxide nano-slice adsorbent, packets
Include following preparation step:
Tungsten hexachloride is added in oleic acid and oleyl amine and forms mixed solution A, and mixed solution is carried out ultrasonic disperse, solution to be mixed
After ethyl alcohol is added when being transparent and continues ultrasonic disperse, mixed solution B is obtained, mixed solution B is put into autoclave and is reacted,
Tungsten oxide quantum dot is prepared in centrifuge separation, by the tungsten oxide quantum dot vacuum drying of preparation；By the tungsten oxide quantum dot of drying
It is placed in Ar/H2Oxygen defect type tungstic trioxide nano-slice adsorbent is prepared in calcining under mixed reducing atmosphere.
Preferably, the usage ratio relationship of the tungsten hexachloride, oleic acid, oleyl amine and ethyl alcohol be 1 ~ 1.7mmol:10 ~
20mL:0 ~ 2.5mL:0 ~ 10mL.
The temperature reacted in the autoclave be 180 ~ 220 DEG C, the reaction time be 3 ~ for 24 hours；
The volume ratio of the argon gas and hydrogen is 5:95, and the gas flow is 50mL/min；
The calcination temperature is 550 DEG C, and calcination time is 4 ~ 8h.
In another aspect, the present invention also provides the oxygen defect type tungstic trioxide nano-slice adsorbent of preparation adsorb it is organic small
Application in terms of molecular dye, according to an embodiment of the invention, oxygen defect type WO provided by the present invention3Nanometer sheet is in the dark state
The methyl orange (MO) in water can be completely removed after absorption 10min, adsorption capacity is up to 63.75 μ g.mg-1.To methylene blue and
Rhodamine B equally has good adsorption effect.
Compared with prior art, the medicine have the advantages that
The present invention is preparing WO3After quantum dot, by modulation calcination atmosphere, in the mixing of reducing atmosphere-argon gas and hydrogen
The oxygen defect type WO containing a large amount of oxygen defects has been prepared in calcining under gas3Nanometer sheet；Because there is reducibility gas H2Presence,
From WO3Lattice in capture Lattice Oxygen, form the WO rich in oxygen defect3Nanometer sheet.Due to the presence of oxygen defect, oxygen defect type
WO3The specific surface area of nanometer sheet increases and surface-active site is increased, and avoids traditional WO3The WO of nanometer sheet3The group of nano particle
Poly- problem, while more active sites are provided for the absorption of target contaminant, the absorption to target contaminant can be improved and hold
Amount and the rate of adsorption.Relative to traditional in N2With the WO being prepared in air3Nanometer sheet, adsorption capacity and efficiency obtain
Significantly promoted.
Meanwhile of the invention preparation method is easy to operate, reagent is cheap, can be used for large-scale low-cost preparation, according to this
The embodiment of invention, oxygen defect type WO provided by the present invention3Nanometer sheet is to methyl orange (MO), methylene blue and rhodamine B
Equal anionic dyes all have good adsorption effect, in terms of have a good application prospect and economic effect
Benefit.
Detailed description of the invention
Fig. 1 is the WO prepared under three kinds of different calcining atmosphere in embodiment 2-43The transmission electron microscope picture of adsorbent: where figure
It 1(A) is WO3(Ar/H2), Fig. 1 (B) be WO3(N2), Fig. 1 (C) be WO3(Air)；
Fig. 2 is the WO prepared under different calcining atmosphere in embodiment 2-43Absorption property figure of the adsorbent to dyestuff MO；
Fig. 3 is the WO of different amounts3(Ar/H2) adsorbent is to the absorption property figure of dyestuff MO.
Specific embodiment
Below with reference to specific implementation example, the present invention will be further described.Material therefor, reagent etc. are such as nothing in embodiment
Specified otherwise is commercially available.The present invention is described in further details below with reference to embodiment.
Embodiment 1:WO3The preparation of quantum dot
By 1.7mmol(0.674g) WCl6It is placed in a beaker, then 20mL oleic acid and 2.5mL oleyl amine is added into beaker, be put into
Ultrasonic disperse in supersonic cleaning machine is added 10mL ethyl alcohol when solution is transparent and continues ultrasound, pours into mixed liquor after dispersion
It in 50mL reaction kettle, is put into baking oven, is warming up to 180 DEG C, keep reaction time 3h, be rapidly cooled to room temperature after reaction,
After being washed respectively with water and ethyl alcohol, it is put into drying in vacuum drying oven and obtains WO3Quantum dot.
Embodiment 2: the preparation of oxygen defect type tungstic trioxide nano-slice: WO3(Ar/H2)
Take 0.3gWO3Quantum dot is placed in crucible, is put into the tube furnace of temperature programming, in Ar/H2(v/v, 5%/95%) atmosphere
Under, gas flow rate 50mL/min, and with 5 DEG C/min from room temperature to 550 DEG C, 4h is kept, oxygen is obtained after cooling grinding and lacks
Swaged WO3Nanometer sheet WO3(Ar/H2).
Embodiment 3:N2Calcining preparation WO in atmosphere3Nanometer sheet: WO3(N2)
By 0.3gWO3Quantum dot is placed in crucible, is put into tube furnace, in N2Under atmosphere, gas flow rate 50mL/min, and with
5 DEG C/min keeps 4h, obtains WO after cooling grinding from room temperature to 550 DEG C3(N2).
Embodiment 4: calcining preparation WO in air atmosphere3Nanometer sheet: WO3(Air)
By 0.3gWO3Quantum dot is placed in crucible, is put into tube furnace, under air (Air) atmosphere, gas flow rate 50mL/
Min, and with 5 DEG C/min from room temperature to 550 DEG C, 4h is kept, obtains WO after cooling grinding3(Air).
Fig. 1 is the WO prepared under three kinds of different calcining atmosphere in embodiment 2-43The transmission electron microscope picture (50nm) of nanometer sheet:
Wherein, Fig. 1 (A) is Ar/H2The WO prepared under calcining atmosphere3(Ar/H2) nanometer sheet；Fig. 1 (B) is N2It is prepared under calcining atmosphere
WO3(N2) nanometer sheet；Fig. 1 (C) is the WO prepared under air calcination atmosphere3(Air) nanometer sheet.As shown in Figure 1, WO in Fig. 1 (A)3
(Ar/H2) nanometer sheet size in 10-15nm, surface has many nano particles to assemble, have more adsorption sites；
WO in Fig. 1 (B)3(N2) nanometer sheet is in N2WO after being calcined in atmosphere3Particle aggregation degree increases, obvious, adsorption site of reuniting
Reduce；Fig. 1 (C) WO3(Air) calcined sheet becomes large-sized nanometer sheet in air, about 20 ~ 50nm, with WO3(Ar/H2)
It is reduced compared to surface little particle, adsorption site reduces.Meanwhile lower WO is calcined to different atmosphere by table 13The element of nano material
The analysis of composition determines the material to the relative amount in small organic molecule Dye Adsorption site with this.
The obstructed atmospheric condition of table 1. calcines lower WO3The element of nano material forms table
| Catalyst | 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 shown in Table 1: WO3(Ar/H2), WO3(N2) and WO3(Air) the O/W elemental mole ratios of three are respectively 1.505,
2.357 and 2.991, illustrate in Ar/H2The WO calcined under mixed atmosphere3Have more oxygen defects, this has for target contaminant
Effect absorption provides more adsorption sites.
Embodiment 5: the WO prepared in embodiment 2-43(Ar/H2), WO3(N2) and WO3(Air) MO adsorptivity test
(1) WO prepared in 25mg embodiment 2-4 is weighed respectively3(Ar/H2), WO3(N2) and WO3(Air) it is placed in 100mL light
In reaction flask, and 50mL methyl orange aqueous solution (10mg.L is added-1), light reaction bottle is placed in light reaction instrument；
(2) magnetic agitation under no radiation of visible light extracts 5mL sample every 10min and is centrifuged；
(3) supernatant in (2) is taken to use liquid ultraviolet-uisible spectrophotometer (UV-2450) in wavelength 463nm in cuvette
Lower measurement, the variation of recording solution absorbance.Fig. 2 is WO3(Ar/H2), WO3(N2) and WO3(Air) nanometer sheet is to dyestuff MO's
Absorption property figure；As shown in Fig. 2, WO3(Ar/H2) best to the absorption property of methyl orange and the rate of adsorption is most fast.It can be seen that
The presence of oxygen defect can increase the adsorption capacity and the rate of adsorption to MO, promote removal efficiency to environmental pollutants.
Embodiment 6:WO3(Ar/H2) influence of the adsorbent amount to MO adsorbance
(1) WO prepared in 5mg, 10mg, 15mg, 25mg above-described embodiment 2 is weighed respectively3(Ar/H2) it is placed in 100mL light reaction
In bottle, it is separately added into 50mL various concentration (10 ~ 40mg.L-1) methyl orange aqueous solution, light reaction bottle is placed in light reaction instrument；
(2) magnetic agitation under no radiation of visible light extracts 5mL sample and is centrifuged after 120min；
(3) supernatant in (2) is taken to use liquid ultraviolet-uisible spectrophotometer (UV-2450) in wavelength 463nm in cuvette
Lower measurement, the variation of recording solution absorbance, Fig. 3 are the adsorbent WO of different amounts3(Ar/H2) to the absorption property of dyestuff MO
Figure；From the figure 3, it may be seen that the experimental results showed that when the dosage of adsorbent is 5mg, unit mass adsorbent to the adsorbance of MO most
Good, adsorption capacity is up to 63.75 μ g.mg-1.It after the dosage of adsorbent increases, interacts between adsorbent, affects absorption effect
Fruit.
Embodiment 7:WO3(Ar/H2) suction-operated of the adsorbent to other small organic molecule dyestuffs
(1) WO prepared in 25mg above-described embodiment 2 is weighed respectively3(Ar/H2) be placed in 100mL light reaction bottle, and add respectively
Enter 50mL rhodamine B and aqueous solution of methylene blue (10mg.L-1), light reaction bottle is placed in light reaction instrument；
(2) magnetic agitation under no radiation of visible light extracts 5mL sample and is centrifuged after 120min；
(3) supernatant in (2) is taken to use liquid ultraviolet-uisible spectrophotometer (UV-2450) in wavelength 463nm in cuvette
Lower measurement, the variation of recording solution absorbance；
The solution absorbance of 2. embodiment 7 of table changes
It is analyzed by table 2. it is found that WO3(Ar/H2) in 120min to the adsorption rate of rhodamine B and methylene blue can reach 99% with
On.It follows that in Ar/H2The oxygen defect type WO prepared in atmosphere3There is universal adsorptivity to small organic molecule dyestuff.
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (9)
1. a kind of oxygen defect type WO3Nanometer sheet adsorbent, which is characterized in that the adsorbent is by WO3Quantum dot is in Ar/H2It is mixed
It is obtained after being calcined under the reducing atmosphere of conjunction, WO3Quantum dot assembles to form WO3Nanometer sheet, WO3There are oxygen defects on nanometer sheet surface.
2. a kind of oxygen defect type WO according to claim 13The preparation method of nanometer sheet adsorbent, which is characterized in that including
Following steps:
Tungsten hexachloride is added in oleic acid and oleyl amine and forms mixed solution A, and mixed solution is carried out ultrasonic disperse, solution to be mixed
After ethyl alcohol is added when being transparent and continues ultrasonic disperse, mixed solution B is obtained, mixed solution B is put into autoclave and is reacted,
Tungsten oxide quantum dot is prepared in centrifuge separation, by the tungsten oxide quantum dot vacuum drying of preparation；By the tungsten oxide quantum dot of drying
It is placed in calcining under the mixed gas atmosphere of argon gas and hydrogen and oxygen defect type WO is prepared3Nanometer sheet adsorbent.
3. a kind of oxygen defect type WO according to claim 23The preparation method of nanometer sheet adsorbent, which is characterized in that described
Tungsten hexachloride, oleic acid, oleyl amine and ethyl alcohol usage ratio relationship be 1 ~ 1.7mmol:10 ~ 20mL:0 ~ 2.5mL:0 ~ 10mL.
4. a kind of oxygen defect type WO according to claim 23The preparation method of nanometer sheet adsorbent, which is characterized in that described
Autoclave in the temperature reacted be 180 ~ 220 DEG C, the reaction time is 3 ~ for 24 hours.
5. a kind of oxygen defect type WO according to claim 23The preparation method of nanometer sheet adsorbent, which is characterized in that described
Argon gas and hydrogen volume ratio be 5:95.
6. a kind of oxygen defect type WO according to claim 23The preparation method of nanometer sheet adsorbent, which is characterized in that described
Gas flow be 50mL/min.
7. a kind of oxygen defect type WO according to claim 23The preparation method of nanometer sheet adsorbent, which is characterized in that described
Calcination temperature be 550 DEG C, calcination time be 4 ~ 8h.
8. a kind of oxygen defect type WO according to claim 13Nanometer sheet adsorbent is in terms of adsorbing organic small molecule dyes
Using.
9. application according to claim 8, which is characterized in that the small organic molecule dyestuff be methyl orange, rhodamine B or
Methylene blue.
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| CN109908891A (en) * | 2019-04-16 | 2019-06-21 | 齐鲁工业大学 | A kind of efficient oxygen vacancy tungsten trioxide nano fiber catalysis material and preparation method thereof |
| 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 |
| CN114950435A (en) * | 2022-06-21 | 2022-08-30 | 阜阳师范大学 | Preparation method of cobalt-oxygen catalyst, product and application thereof |
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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 |
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| CN112844371A (en) * | 2021-02-03 | 2021-05-28 | 黑河学院 | Catalyst for photolysis of water to produce oxygen and preparation method thereof |
| CN114950435A (en) * | 2022-06-21 | 2022-08-30 | 阜阳师范大学 | Preparation method of cobalt-oxygen catalyst, product and application thereof |
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