CN109225201A - A kind of preparation method and application of micro-nano tungsten oxide - Google Patents

A kind of preparation method and application of micro-nano tungsten oxide Download PDF

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CN109225201A
CN109225201A CN201810954025.3A CN201810954025A CN109225201A CN 109225201 A CN109225201 A CN 109225201A CN 201810954025 A CN201810954025 A CN 201810954025A CN 109225201 A CN109225201 A CN 109225201A
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tungsten oxide
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filter paper
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CN109225201B (en
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席晓丽
赵林艳
马立文
樊佑书
聂祚仁
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Beijing University of Technology
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/24Chromium, molybdenum or tungsten
    • B01J23/30Tungsten
    • AHUMAN NECESSITIES
    • A62LIFE-SAVING; FIRE-FIGHTING
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    • A62D3/00Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
    • A62D3/10Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation
    • A62D3/17Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by subjecting to electric or wave energy or particle or ionizing radiation to electromagnetic radiation, e.g. emitted by a laser
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39Photocatalytic properties
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    • C01G41/00Compounds of tungsten
    • C01G41/02Oxides; Hydroxides

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Abstract

The present invention provides a kind of preparation method of micro-nano tungsten oxide, by dispersing filter paper into sodium tungstate solution, makes that the gel presoma formed after pH is adjusted to be sufficiently adhering on filter paper, later by filtering and roasting, obtains tungsten oxide product.The present invention also proposes the product and its application that the preparation method obtains.Preparation method provided by the present invention has merged the advantages of liquid phase method raw material is uniformly mixed with solid phase method simple process, its core is using a kind of substance being easily removed as carrier, it can be directly transferred to progress calcination process in Muffle furnace after its load tungsten presoma and obtain oxidation tungsten product, without being further processed;And method therefor high-efficient simple, environmentally protective, process is short, product is controllable;Raw materials required for the reaction is all the raw material being conveniently easy to get in the market;Preparing resulting tungsten oxide has the characteristics that better crystallinity degree, of uniform size, soilless sticking, photocatalysis performance are good, can be widely applied to dyestuff degradation and other field of semiconductor photocatalyst.

Description

A kind of preparation method and application of micro-nano tungsten oxide
Technical field
The invention belongs to micro-nano material fields, and in particular to a kind of preparation of micro/nano level tungsten oxide material and its answer With.
Background technique
Tungsten oxide is a kind of widely used n-type semiconductor metal oxide, as a kind of cheap and stable transition gold Belong to oxide, tungsten oxide has photocatalysis, gas because the height of its structure is adjustable and unique physical and chemical performance is concerned The excellent performances such as quick, photochromic, electrochromism, be widely used in photocatalytic degradation, gas sensor, Flied emission equipment, In the equipment such as electrochromic device.Relative to same type of material TiO2, ZnO, NiO etc., tungsten oxide has narrower forbidden bandwidth, because This absorbable light using visible light wave range in sunlight, and it is not only limited to ultraviolet light.
Preparation method has significant impact to the physicochemical properties of material, because it directly affects synthesized material Crystal structure, particle size, service performance and practical application etc..There are many methods for preparing tungsten oxide at present, according to raw material Property and reaction process difference can be broadly divided into: vapor phase method, liquid phase method and solid phase method.Vapor- phase synthesis be it is a kind of using heating, etc. The various energy such as ionic drive or light radiation make the chemical substance of gaseous state or steam-like in gas phase or gas-solid interface in reactor On through chemically reacting form the technology of solid deposited object, physical vapour deposition (PVD) (PVD) and chemical gas-phase method (CVD) are more commonly used Vapor- phase synthesis technology.But vapor phase method general device higher cost, people usually consider to use liquid phase method at this time, compared to gas phase side Method, liquid phase synthesizing method (LPS) can preferably control the pattern of material, and can realize that liquid phase is closed at quite low temperatures At therefore, requirement of this method to energy and equipment is lower, greatly reduces cost.Liquid phase method mainly includes sol-gel Method, hydro-thermal method, template and electrochemical process etc., but there is also some problems, as sol-gel transition is more difficult, after template Phase treatment process is relatively complicated, hydro-thermal method needs further calcination processing, synthesis cycle longer etc..Solid phase method is by solid phase Variation generallys use to manufacture powder and wolframic acid or ammonium tungstate etc. are directly heated decomposition containing tungsten oxide prepares tungstic acid, It is characterized in that without phase transformation as the adjoint gas phase-solid phase of vapor phase method and liquid phase method, liquid-solid.For gas phase or liquid phase, Molecule is very sensitive to the reaction of external condition, and for solid phase, the diffusion of molecule (atom) is very slow, Set Status be it is various, The resulting solid phase powder of solid phase method and initial Solid raw materials can be same substance, may not be same substance.
Above-mentioned a variety of preparation methods still have some shortcomings.The available particle size of vapor phase method is small, with high purity Tungsten oxide material, but this method is higher to equipment and technical requirements, and synthesis is difficult, at high cost, product controllability is poor, at present Only rest on the laboratory research stage;Liquid phase method has the advantages that cost is relatively low, stable reaction, product are controllable, but its subsequent place Reason process is cumbersome, synthesis cycle is longer;Although solid phase method simple process, obtained product is easy to reunite, needs separating twice, and Quality is lower.
Summary of the invention
For short slab present in existing technology of preparing and deficiency, the primary purpose of the present invention is that providing a kind of micro-nano The novel processing step of tungsten oxide;This method has merged the advantages of liquid phase method raw material is uniformly mixed with solid phase method simple process, tool Have the advantages that process is short, simple and feasible, environmentally protective, product is controllable.
Another object of the present invention is to provide the micro-nanos with different-shape structure that a kind of above method is prepared Rice tungsten oxide product.
A further object of the present invention is to provide the applications of the micro-nano tungsten oxide.
Realize above-mentioned purpose technical solution of the present invention are as follows:
A kind of preparation method of micro-nano tungsten oxide makes to adjust and is formed after pH by dispersing filter paper into sodium tungstate solution Gel presoma is sufficiently adhering on filter paper, later by filtering and roasting, obtains tungsten oxide product.
Technical solution of the present invention is proposed in further detail below.
The preparation method of the micro-nano tungsten oxide, comprising steps of
(1) filter paper fragment is distributed in the water containing sodium tungstate, obtains dispersion;
(2) by dispersion obtained in step (1) when being stirred continuously with inorganic acid for adjusting pH, before obtaining glue Drive liquid solution;
(3) it after the precursor solution for obtaining step (2) is stood, is rinsed and filters, obtain being attached on filter paper Gluey tungsten presoma;
(4) filter paper that gluey tungsten presoma is attached in step (3) is subjected to high-temperature roasting processing, it is air-cooled after roasting To room temperature, obtained product is tungsten oxide.
Wherein, concentration of sodium tungstate is 10-80g/L in dispersion described in step (1).
Wherein, inorganic acid described in step (2) is hydrochloric acid, sulfuric acid or nitric acid, and concentration 1-8mol/L adjusts dispersion PH value is to pH=0.5-3.
Wherein, the time of standing described in step (3) is 0.5-12 hours.
Wherein, maturing temperature is 400-800 DEG C, calcining time 3-12 hours in step (4).Roasting crucible used can be with For corundum crucible, high-temperature roasting carries out in Muffle furnace.
The further preferred technical solution of the present invention is, by be not added or be added in the sodium tungstate solution adjusting control agent come Regulate and control product morphology, with the micro/nano level granular product or micron order hollow sphere product dispersed or one-dimensional product.It is one-dimensional Product is usually nano wire, nanometer rods, the one-dimensional structure such as nanobelt.
A preferred technical solution of the invention is also to contain adjusting control agent, the adjusting control agent in the sodium tungstate solution Mass ratio for one of zinc chloride, zinc sulfate, potassium sulfate, potassium chloride or a variety of, adjusting control agent and sodium tungstate is 0.5~1: 1。
The micro-nano tungsten oxide that the preparation method obtains.
Application of the micro-nano tungsten oxide in dyestuff degradation or semiconductor light electrotransformation.
The beneficial effects of the present invention are:
Preparation method provided by the present invention has merged the advantages of liquid phase method raw material is uniformly mixed with solid phase method simple process, Its core is can be directly transferred to be roasted in Muffle furnace after loading tungsten presoma using a kind of substance being easily removed as carrier Burning handles to obtain oxidation tungsten product, without being further processed;And method therefor high-efficient simple, environmentally protective, process is short, product can Control;Raw materials required for the reaction is all the raw material being conveniently easy to get in the market;It is equal with better crystallinity degree, size to prepare resulting tungsten oxide The features such as even, soilless sticking, photocatalysis performance are good can be widely applied to dyestuff degradation and other field of semiconductor photocatalyst.
Detailed description of the invention
Fig. 1 is the XRD diagram piece of 1 products therefrom of embodiment.
Fig. 2 is the SEM picture of 1 products therefrom of embodiment.
Fig. 3 is the SEM picture of 2 products therefrom of embodiment.
Fig. 4 is the XRD diagram piece of 2 products therefrom of embodiment.
Specific embodiment
Illustrate the present invention below by most preferred embodiment.Those skilled in the art institute it should be understood that, embodiment is only used to It illustrates rather than for limiting the scope of the invention.
In embodiment, unless otherwise instructed, means used are the means of this field routine.
Embodiment 1:
It is distributed to after commercial filter paper is shredded in the 50ml pure water of the sodium tungstate containing 1g, after being sufficiently mixed uniformly, is placed in magnetic force On blender, when being stirred continuously with 4mol/L hydrochloric acid conditioning solution pH value to pH=1, faint yellow gluey forerunner is obtained Liquid solution;After the presoma is stood 3 hours, several times with pure water and ethyl alcohol repeated flushing, and it is obtained by filtration and is attached on filter paper Gluey tungsten presoma, transfer them in corundum crucible later, in Muffle furnace in 600 DEG C high-temperature roasting 6 hours, Zhi Houkong It is cooled to room temperature to get final tungsten oxide product is arrived.
The above-mentioned tungsten oxide product of 0.01g is weighed, is dissolved in the methylene blue solution that 100ml concentration is 10mg/L, is protected from light Under the conditions of after uniform stirring 10min reaches adsorption equilibrium, above-mentioned mixed solution is placed in the xenon lamp equipped with filter plate (λ > 420nm) Under light source, the process of tungsten oxide photocatalytic degradation methylene blue under light can be guaranteed that continuous magnetic force stirs in reaction process by simulation It mixes and light source irradiates, and take supernatant to be detected in certain time.Prepared product has preferable photocatalytic degradation effect, In 180min, degradation efficiency is up to 94%.
Fig. 1 is the XRD diagram for the tungsten oxide product that embodiment 1 obtains, peak value and monoclinic phase WO3It is corresponding, as seen from the figure Prepared product crystallinity is good, and crystal phase is single, and no other impurities generate.Fig. 2 is the tungsten oxide product that embodiment 1 obtains SEM picture can clearly be seen that prepared Product size distribution is relatively uniform in figure, be micro/nano level nutty structure, Do not reunite.
Embodiment 2:
It is distributed to after commercial filter paper is shredded in the 50ml pure water of the sodium tungstate containing 1g, then to weigh 0.68g (5mM) zinc chloride molten It after wherein, being sufficiently mixed uniformly, is placed on magnetic stirring apparatus, when being stirred continuously with 4mol/L hydrochloric acid conditioning solution acid Basicity obtains faint yellow gluey precursor solution to pH=1;After the presoma is stood 3 hours, rushed repeatedly with pure water and ethyl alcohol It washes several times, and the gluey tungsten presoma being attached on filter paper is obtained by filtration, transfer them in corundum crucible later, in Muffle furnace It is interior in 600 DEG C high-temperature roasting 6 hours, be air-cooled to room temperature later to get to final tungsten oxide product.
Fig. 3 is the SEM picture for the tungsten oxide product that embodiment 2 obtains, and can clearly be seen that prepared product is in figure The micrometre hollow sphere structure that nano particle assembles, size are more uniform.Fig. 4 is the XRD for the tungsten oxide product that embodiment 2 obtains Figure, peak value correspond to monoclinic phase WO3(main) and hexagonal phase WO3, prepared product crystallinity is good as seen from the figure, removes main product Beyond the region of objective existence is generated without other impurities.
The visible light photocatalytic degradation process under xenon lamp simulation is carried out later, and method and step is the same as embodiment 1.Products therefrom also has There is preferable photocatalytic degradation effect, degradation efficiency is up to 99% in 180min.
Embodiment 3:
It is distributed to after commercial filter paper is shredded in the 50ml pure water of the sodium tungstate containing 1g, then to weigh 0.87g (5mM) potassium sulfate molten It after wherein, being sufficiently mixed uniformly, is placed on magnetic stirring apparatus, when being stirred continuously with 4mol/L hydrochloric acid conditioning solution acid Basicity obtains faint yellow gluey precursor solution to pH=1;After the presoma is stood 3 hours, rushed repeatedly with pure water and ethyl alcohol It washes several times, and the gluey tungsten presoma being attached on filter paper is obtained by filtration, transfer them in corundum crucible later, in Muffle furnace It is interior in 600 DEG C high-temperature roasting 6 hours, be air-cooled to room temperature later to get to final tungsten oxide product.
It is observed by SEM, it is seen that obtained tungsten oxide particles are one-dimensional rod-like pattern.XRD spectrum shows the peak value of product With WO3Corresponding, no other impurities generate.
Embodiment 4:
It is distributed to after commercial filter paper is shredded in the 50ml pure water of the sodium tungstate containing 1g, after being sufficiently mixed uniformly, is placed in magnetic force On blender, when being stirred continuously with 4mol/L hydrochloric acid conditioning solution pH value to pH=3, faint yellow gluey forerunner is obtained Liquid solution;After the presoma is stood 3 hours, several times with pure water and ethyl alcohol repeated flushing, and it is obtained by filtration and is attached on filter paper Gluey tungsten presoma, transfer them in corundum crucible later, in Muffle furnace in 600 DEG C high-temperature roasting 6 hours, Zhi Houkong It is cooled to room temperature to get final tungsten oxide product is arrived.
The pH value of the present embodiment dispersion is slightly higher, and the product that scanning electron microscopic observation obtains slightly is reunited.Therefore preferably compared with The dispersion of low ph value;But inorganic acid dosage has greater environmental impacts too much, therefore preferably in the pH value item of pH >=1 Part.
Embodiment 5:
It is distributed to after commercial filter paper is shredded in the 50ml pure water of the sodium tungstate containing 3g, after being sufficiently mixed uniformly, is placed in magnetic force On blender, when being stirred continuously with 4mol/L hydrochloric acid conditioning solution pH value to pH=1, faint yellow gluey forerunner is obtained Liquid solution;After the presoma is stood 3 hours, several times with pure water and ethyl alcohol repeated flushing, and it is obtained by filtration and is attached on filter paper Gluey tungsten presoma, transfer them in corundum crucible later, in Muffle furnace in 600 DEG C high-temperature roasting 6 hours, Zhi Houkong It is cooled to room temperature to get final tungsten oxide product is arrived.
Wolframic acid sodium content is higher in the present embodiment dispersion, and gained final product pattern is more irregular, is unfavorable for subsequent Using, therefore preferably in the concentration conditions of 15-25g/L.
Above embodiment be only preferred embodiments of the present invention will be described, not to the scope of the present invention into Row limits, and without departing from the spirit of the design of the present invention, this field ordinary engineering and technical personnel is to technical side of the invention The all variations and modifications that case is made, should fall within the scope of protection determined by the claims of the present invention.

Claims (10)

1. a kind of preparation method of micro-nano tungsten oxide, which is characterized in that by dispersing filter paper into sodium tungstate solution, make to adjust pH The gel presoma formed afterwards is sufficiently adhering on filter paper, later by filtering and roasting, obtains tungsten oxide product.
2. the preparation method of micro-nano tungsten oxide according to claim 1, which is characterized in that comprising steps of
(1) filter paper fragment is distributed in the water containing sodium tungstate, obtains dispersion;
(2) by dispersion obtained in step (1) when being stirred continuously with inorganic acid for adjusting pH, obtain gluey presoma Solution;
(3) it after the precursor solution for obtaining step (2) is stood, is rinsed and filters, obtain being attached to the glue on filter paper Tungsten presoma;
(4) filter paper for being attached with gluey tungsten presoma in step (3) is subjected to high-temperature roasting processing, is air-cooled to room after roasting Temperature, obtained product are tungsten oxide.
3. the preparation method of micro-nano tungsten oxide according to claim 2, which is characterized in that divide described in step (1) Concentration of sodium tungstate is 10-80g/L in granular media system.
4. the preparation method of micro-nano tungsten oxide according to claim 2, which is characterized in that inorganic described in step (2) Acid is hydrochloric acid, sulfuric acid or nitric acid, and concentration 1-8mol/L adjusts dispersion pH value to pH=0.5-3.
5. the preparation method of micro-nano tungsten oxide according to claim 2, which is characterized in that stood described in step (3) Time be 0.5-12 hours.
6. the preparation method of micro-nano tungsten oxide according to claim 2, which is characterized in that the roasting temperature in step (4) Degree is 400-800 DEG C, calcining time 3-12 hours.
7. the preparation method of micro-nano tungsten oxide according to claim 1-6, which is characterized in that by described Adjusting control agent is not added or is added in sodium tungstate solution to regulate and control product morphology, with the micro/nano level granular product dispersed or micro- Meter level hollow sphere product or one-dimensional product.
8. the preparation method of micro-nano tungsten oxide according to claim 7, which is characterized in that in the sodium tungstate solution also Containing adjusting control agent, the adjusting control agent is one of zinc chloride, zinc sulfate, potassium sulfate, potassium chloride or a variety of, adjusting control agent and wolframic acid The mass ratio of sodium is 0.5-1:1.
9. the micro-nano tungsten oxide that the described in any item preparation methods of claim 1-8 obtain.
10. application of the micro-nano tungsten oxide as claimed in claim 9 in dyestuff degradation or semiconductor light electrotransformation.
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CN112499667A (en) * 2020-12-31 2021-03-16 天津城建大学 Air-sensitive material with spiny cover flower-shaped hexagonal crystal phase zinc oxide/tungsten oxide heterogeneous multi-stage structure, synthesis method and application
CN113860372A (en) * 2021-10-14 2021-12-31 北京工业大学 Short-process preparation of W0.4Mo0.6O3And applications thereof

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Cited By (3)

* Cited by examiner, † Cited by third party
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CN112499667A (en) * 2020-12-31 2021-03-16 天津城建大学 Air-sensitive material with spiny cover flower-shaped hexagonal crystal phase zinc oxide/tungsten oxide heterogeneous multi-stage structure, synthesis method and application
CN113860372A (en) * 2021-10-14 2021-12-31 北京工业大学 Short-process preparation of W0.4Mo0.6O3And applications thereof
CN113860372B (en) * 2021-10-14 2023-09-26 北京工业大学 Short-process preparation W 0.4 Mo 0.6 O 3 Is provided and uses thereof

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