CN105236491A - Preparation method of filament-like W18O49 material - Google Patents

Preparation method of filament-like W18O49 material Download PDF

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CN105236491A
CN105236491A CN201510536148.1A CN201510536148A CN105236491A CN 105236491 A CN105236491 A CN 105236491A CN 201510536148 A CN201510536148 A CN 201510536148A CN 105236491 A CN105236491 A CN 105236491A
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solution
thread
preparation
autoclave
reaction
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CN105236491B (en
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黄剑锋
海国娟
介燕妮
曹丽云
李嘉胤
吴建鹏
孔新刚
卢靖
张博
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Shaanxi University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G41/00—Compounds of tungsten
    • C01G41/02—Oxides; Hydroxides
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer

Abstract

A preparation method of a filament-like W18O49 material includes the following steps: 1) adding WC16 into anhydrous ethanol to prepare a solution A being 0.03-0.08 mol/L in concentration; 2) adding octadecylamine to the solution A to obtain a solution B; 3) uniformly stirring the solution B under a sealed condition to obtain a solution C; and 4) adding the solution C into a high-pressure reaction kettle, performing a reaction in a homogeneous phase reactor at 140-180 DEG C and cooling a reaction product to obtain the filament-like W18O49 material. The preparation method is mild in reaction conditions and is low in required temperature and is simple in steps and high in repeatability. The filament-like W18O49 material has a strong adsorbility to methylene blue and an excellent photo-catalytic performance to methyl orange, and in particular, has certain adsorbility to the methyl orange in a dark reaction process. Before 40 min of a photo-reaction stage, the material reaches 80% in degradation of the methyl orange. It is predicted that the material has a high exploration value in performances.

Description

A kind of thread W 18o 49the preparation method of material
Technical field
The invention belongs to technical field of nanometer material preparation, be specifically related to a kind of thread W 18o 49the preparation method of material.
Background technology
WO 3be made up of perovskite structure unit, its crystalline structure is that the regular octahedron units shared zenithal alignment be made up of 1 tungsten atom and 6 Sauerstoffatoms forms.WO 3there is multiple crystal formation, as monocline (m-WO 3), three oblique (tr-WO 3), orthogonal (o-WO 3), four directions (te-WO 3), six side (h-WO 3) etc.Wherein monocline, three tiltedly, orthogonal, and hexagonal structure can stable existence at normal temperatures.The structure of crystal is to WO 3performance certain influence, the Tungsten oxide 99.999 crystalline structure as hexagonal structure has larger pore passage structure, can hold cation ic-converted for tungsten blue, be considered to good electrochromic material.WO 3be easy to the WO forming non-stoichiometric x.WO is there is in the crystalline structure of this type oxide 6structural unit shares the situation in rib and face.Wherein, W 18o 49having the oxygen defect of maximum, is known unique non-stoichiometric WO existed with pure form x.Since [ZHUYQ such as ZHU, HUWB, HSUWK, TERRONESM, GROBERTN, HAREJP.Tungstenoxidetree-likestructures [J] .ChemicalPhysicsLetters, 1999,309 (5/6): 327-334.] the broken micron dentrite of first passage obtains W 18o 49since nano wire, investigators utilize the multiple method such as thermal treatment, vapor phase growth to synthesize the W of different-shape 18o 49nanostructure, and detailed sign has been carried out to its stuctures and properties.This material, except having good air-sensitive, variable color and catalytic performance, shows good absorption-thermal transition performance to infrared light.
Within 2012, Japanese scholars leaf golden flower finds the W of 1-dimention nano filamentary texture further 18o 49material can catalytic reduction CO under visible light illumination 2gas [G.Xi, S.Ouyang, P.Li, J.Ye, Q.Ma, N.Su, H.Bai, C.Wang, UltrathinW 18o 49nanowireswithDiametersbelow1nm:Synthesis, Near-InfraredAbsorption, Photoluminescence, andPhotochemicalReductionofCarbonDioxide, AngewandteChemieInternationalEdition, 51 (2012) 2395-2399.], catalyzed reaction efficiency is high and do not need noble metal support, and this illustrates the W of nanostructure 18o 49material not only can make up WO 3the deficiency that material is active in light-catalyzed reaction, does not also need noble metal support, effectively can reduce the preparation cost of material, have good potential application foreground.Current W 18o 49material goes back Shortcomings in synthesis and the research in its photocatalysis performance field, needs to explore further.
The existing W preparing 1-dimention nano filamentary texture 18o 49the method of material is complicated, and obtained W 18o 49chemical purity low, pattern heterogeneity.
Summary of the invention
For overcoming the problems of the prior art, the object of the present invention is to provide that a kind of technological process is simple, reaction time is short, gained powder chemical constitution is homogeneous, crystal morphology size uniformity, the thread W of morphology controllable 18o 49the preparation method of material.
For achieving the above object, the technical solution used in the present invention is as follows:
1) by WCl 6join in dehydrated alcohol, be mixed with the solution A of 0.03 ~ 0.08mol/L;
2) in solution A, add stearylamine, obtain solution B; Wherein, WCl 6be 1:(0.8 ~ 2 with the ratio of the amount of substance of stearylamine);
3) solution B is stirred in confined conditions, obtain solution C;
4) solution C is joined in autoclave, after then reacting 12 ~ 28h at 140 ~ 180 DEG C in homogeneous reactor, cool to room temperature with the furnace, after centrifugal, washing, drying, obtain thread W 18o 49material.
Described stirring specifically first carries out magnetic agitation, then carries out supersound process.
The power of described supersound process is 60 ~ 80Hz, and the time of supersound process is 20 ~ 40min.
Described autoclave take tetrafluoroethylene as liner.
The filling ratio of described autoclave is 30 ~ 60%.
Described washing adopts dehydrated alcohol to carry out.
Described drying in vacuum drying oven or freeze drying box carry out.
The temperature of described drying is 40 ~ 60 DEG C, and the time is 3 ~ 12h.Compared with prior art, the beneficial effect that the present invention has: the present invention, by adding the stearylamine as tensio-active agent, can prepare and have obvious oriented growth and the relatively high pure phase W of crystallinity 18o 49material, overcomes W in prior art 18o 49the situation that material crystalline is lower; The present invention utilizes stearylamine for tensio-active agent, by controlling stearylamine (CH 3(CH 2) 16cH 2nH 2) consumption, thread length can well be regulated and controled, realize the controlledly synthesis of single filar length in nanometer and micrometer range.The present invention's preparation has the W of oxygen defect 18o 49during material, not blanketing with inert gas, prepares the finely dispersed W of pure phase at 140 ~ 180 DEG C 18o 49material, reaction conditions of the present invention is gentle, temperature required lower, and processing step is simple, and repeatability is high, and the thread W of the present invention's synthesis 18o 49material, have stronger absorption property to methylene blue, good photocatalysis performance is shown to tropeolin-D simultaneously, specifically there is certain absorption at cloudy, turbid phase product to tropeolin-D, before photoreaction stage, the degraded of 40min to tropeolin-D reaches 80%, and the prediction of its aspect of performance has larger exploration and is worth.
Accompanying drawing explanation
Fig. 1 is the W that the present invention is prepared under embodiment 1 condition 18o 49xRD figure spectrum.
Fig. 2 is the W that the present invention is prepared under embodiment 1 condition 18o 49sEM photo under 30k magnification.
Fig. 3 is the W that the present invention is prepared under embodiment 1 condition 18o 49sEM photo under 10k magnification.
Fig. 4 is W prepared by the embodiment of the present invention 1 18o 49to the degradation curve of tropeolin-D under 500W mercury lamp.
Embodiment
Be described in detail by specific embodiment below in conjunction with accompanying drawing.
Embodiment 1
1) by 0.7931gWCl 6join in 40mL dehydrated alcohol, be mixed with the solution A of 0.05mol/L;
2) in solution A, add 0.5390g analytical pure stearylamine (CH 3(CH 2) 16cH 2nH 2), obtain solution B;
3) solution B preservative film is sealed, avoid contacting with air, first adopt magnetic agitation 20min, more ultrasonic (60Hz) processes 30min, obtains solution C;
4) solution C being joined 100mL is in the autoclave of liner with tetrafluoroethylene, volume packing ratio is 40%, then after autoclave being sealed, room temperature is cooled to the furnace react 24h at 160 DEG C in homogeneous reactor after, centrifugal through dehydrated alcohol, washing 3 times, in vacuum drying oven in 60 DEG C of dry 3h, obtain thread W 18o 49material.
As seen from Figure 1: the W of product pure phase prepared by the present invention 18o 49material.As seen from Figure 2: the W that the present invention obtains 18o 49it is a kind of filamentary texture.As seen from Figure 3: the thread W that the present invention obtains 18o 49single length be about 0.8 ~ 1.5 μm.
As can be seen from Figure 4 have certain absorption at cloudy, turbid phase product to tropeolin-D, before photoreaction stage, the degraded of 40min to tropeolin-D reaches 80%.
Embodiment 2
1) by 0.9914gWCl 6join in 50mL dehydrated alcohol, be mixed with the solution A of 0.06mol/L;
2) in solution A, add 0.6468g analytical pure stearylamine (CH 3(CH 2) 16cH 2nH 2), obtain solution B;
3) solution B preservative film is sealed, avoid contacting with air, first adopt magnetic agitation 40min, more ultrasonic (60Hz) processes 20min, obtains solution C;
4) solution C being joined 100mL is in the autoclave of liner with tetrafluoroethylene, volume packing ratio is 40%, then after autoclave being sealed, room temperature is cooled to the furnace react 18h at 150 DEG C in homogeneous reactor after, centrifugal through dehydrated alcohol, washing 3 times, in vacuum drying oven in 60 DEG C of dry 3h, obtain thread W 18o 49material.
The thread W that this example obtains 18o 49single length be about 1 ~ 1.5 μm.
Embodiment 3
1) by 1.0259gWCl 6join in 60mL dehydrated alcohol, be mixed with the solution A of 0.08mol/L;
2) in solution A, add 2.5870g analytical pure stearylamine (CH 3(CH 2) 16cH 2nH 2), obtain solution B;
3) solution B preservative film is sealed, avoid contacting with air, first adopt magnetic agitation 20min, more ultrasonic (60Hz) processes 30min, obtains solution C;
4) solution C being joined 100mL is in the autoclave of liner with tetrafluoroethylene, volume packing ratio is 60%, then after autoclave being sealed, room temperature is cooled to the furnace react 18h at 170 DEG C in homogeneous reactor after, centrifugal through dehydrated alcohol, washing 3 times, in vacuum drying oven in 60 DEG C of dry 3h, obtain thread W 18o 49material.
The thread W that this example obtains 18o 49single length be about 1.3 ~ 1.8 μm.
Embodiment 4
1) by 0.4758gWCl 6join in 40mL dehydrated alcohol, be mixed with the solution A of 0.03mol/L;
2) in solution A, add 0.3881g analytical pure stearylamine (CH 3(CH 2) 16cH 2nH 2), obtain solution B;
3) solution B preservative film is sealed, avoid contacting with air, first adopt magnetic agitation 40min, more ultrasonic (60Hz) processes 10min, obtains solution C;
4) solution C being joined 100mL is in the autoclave of liner with tetrafluoroethylene, volume packing ratio is 60%, then after autoclave being sealed, room temperature is cooled to the furnace react 24h at 160 DEG C in homogeneous reactor after, centrifugal through dehydrated alcohol, washing 3 times, in vacuum drying oven in 60 DEG C of dry 3h, obtain thread W 18o 49material.
The thread W that this example obtains 18o 49single length be about 0.8 ~ 1.2 μm.
Embodiment 5
1) by WCl 6join in dehydrated alcohol, be mixed with the solution A of 0.04mol/L;
2) in solution A, add stearylamine, obtain solution B; Wherein, WCl 6be 1:0.8 with the ratio of the amount of substance of stearylamine;
3) solution B preservative film is sealed, avoid contacting with air, first adopt magnetic agitation 20min, stir under ultrasonic (80Hz) processes 20min air tight condition, obtain solution C;
4) solution C being joined 100mL is in the autoclave of liner with tetrafluoroethylene, volume packing ratio is 40%, then after autoclave being sealed, room temperature is cooled to the furnace react 28h at 140 DEG C in homogeneous reactor after, centrifugal through dehydrated alcohol, washing 4 times, in vacuum drying oven in 40 DEG C of dry 12h, obtain thread W 18o 49material.
Embodiment 6
1) by WCl 6join in dehydrated alcohol, be mixed with the solution A of 0.07mol/L;
2) in solution A, add stearylamine, obtain solution B; Wherein, WCl 6be 1:2 with the ratio of the amount of substance of stearylamine;
3) solution B preservative film is sealed, avoid contacting with air, first adopt magnetic agitation 20min, stir under ultrasonic (60Hz) processes 40min air tight condition, obtain solution C;
4) solution C being joined 100mL is in the autoclave of liner with tetrafluoroethylene, volume packing ratio is 50%, then after autoclave being sealed, room temperature is cooled to the furnace react 12h at 180 DEG C in homogeneous reactor after, centrifugal through dehydrated alcohol, washing 4 times, in vacuum drying oven in 50 DEG C of dry 8h,, obtain thread W 18o 49material.
Embodiment 7
1) by WCl 6join in dehydrated alcohol, be mixed with the solution A of 0.05mol/L;
2) in solution A, add stearylamine, obtain solution B; Wherein, WCl 6be 1:1.5 with the ratio of the amount of substance of stearylamine;
3) solution B preservative film is sealed, avoid contacting with air, first adopt magnetic agitation 20min, stir under ultrasonic (70Hz) processes 30min air tight condition, obtain solution C;
4) solution C being joined 100mL is in the autoclave of liner with tetrafluoroethylene, volume packing ratio is 55%, then after autoclave being sealed, room temperature is cooled to the furnace react 20h at 140 DEG C in homogeneous reactor after,, washing 4 time centrifugal through dehydrated alcohol, dry in freeze drying box, obtain thread W 18o 49material.

Claims (8)

1. a thread W 18o 49the preparation method of material, is characterized in that, comprises the following steps:
1) by WCl 6join in dehydrated alcohol, be mixed with the solution A of 0.03 ~ 0.08mol/L;
2) in solution A, add stearylamine, obtain solution B; Wherein, WCl 6be 1:(0.8 ~ 2 with the ratio of the amount of substance of stearylamine);
3) solution B is stirred in confined conditions, obtain solution C;
4) solution C is joined in autoclave, after then reacting 12 ~ 28h at 140 ~ 180 DEG C in homogeneous reactor, cool to room temperature with the furnace, after centrifugal, washing, drying, obtain thread W 18o 49material.
2. the thread W of one according to claim 1 18o 49the preparation method of material, is characterized in that, described in stir and specifically first carry out magnetic agitation, then carry out supersound process.
3. the thread W of one according to claim 2 18o 49the preparation method of material, is characterized in that, the power of described supersound process is 60 ~ 80Hz, and the time of supersound process is 20 ~ 40min.
4. the thread W of one according to claim 1 18o 49the preparation method of material, is characterized in that, described autoclave take tetrafluoroethylene as liner.
5. the thread W of the one according to claim 1 or 4 18o 49the preparation method of material, is characterized in that, the filling ratio of described autoclave is 30 ~ 60%.
6. the thread W of one according to claim 1 18o 49the preparation method of material, is characterized in that, described washing adopts dehydrated alcohol to carry out.
7. the thread W of one according to claim 1 18o 49the preparation method of material, is characterized in that, described drying in vacuum drying oven or freeze drying box carry out.
8. the thread W of the one according to claim 1 or 7 18o 49the preparation method of material, is characterized in that, the temperature of described drying is 40 ~ 60 DEG C, and the time is 3 ~ 12h.
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CN107159127A (en) * 2017-05-15 2017-09-15 济南大学 A kind of preparation method and application for heavy metal and the adsorbent of Dye Adsorption
CN107626300A (en) * 2017-09-30 2018-01-26 五邑大学 A kind of thermal drivers catalyst and its application
CN107999110A (en) * 2017-11-14 2018-05-08 肇庆市华师大光电产业研究院 A kind of Lacking oxygen tungsten oxide/nitridation carbon composite photocatalyst and its preparation method and application
CN109706476A (en) * 2019-02-28 2019-05-03 陕西科技大学 A kind of carbon cloth surfaces growth in situ W18O49The preparation method of self-supporting electrode material
CN109806902A (en) * 2019-02-28 2019-05-28 陕西科技大学 A kind of W18O49/NiWO4The preparation method of/NF self-supporting electrocatalysis material
CN111589460A (en) * 2020-06-03 2020-08-28 哈尔滨理工大学 W18O49BiOX composite photocatalytic material and preparation method thereof
CN114797852A (en) * 2022-03-17 2022-07-29 太原理工大学 Ru/W with oxygen-containing defects 18 O 49 Preparation method of photocatalyst and application of photocatalyst in hydrogen storage field

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Publication number Priority date Publication date Assignee Title
CN107159127A (en) * 2017-05-15 2017-09-15 济南大学 A kind of preparation method and application for heavy metal and the adsorbent of Dye Adsorption
CN107159127B (en) * 2017-05-15 2020-04-28 济南大学 Preparation method and application of adsorbent for heavy metal and dye adsorption
CN107626300A (en) * 2017-09-30 2018-01-26 五邑大学 A kind of thermal drivers catalyst and its application
CN107999110A (en) * 2017-11-14 2018-05-08 肇庆市华师大光电产业研究院 A kind of Lacking oxygen tungsten oxide/nitridation carbon composite photocatalyst and its preparation method and application
CN109706476A (en) * 2019-02-28 2019-05-03 陕西科技大学 A kind of carbon cloth surfaces growth in situ W18O49The preparation method of self-supporting electrode material
CN109806902A (en) * 2019-02-28 2019-05-28 陕西科技大学 A kind of W18O49/NiWO4The preparation method of/NF self-supporting electrocatalysis material
CN109706476B (en) * 2019-02-28 2021-02-09 陕西科技大学 Carbon cloth surface in-situ growth W18O49Preparation method of self-supporting electrode material
CN109806902B (en) * 2019-02-28 2021-07-06 陕西科技大学 W18O49/NiWO4Preparation method of/NF self-supporting electrocatalytic material
CN111589460A (en) * 2020-06-03 2020-08-28 哈尔滨理工大学 W18O49BiOX composite photocatalytic material and preparation method thereof
CN111589460B (en) * 2020-06-03 2022-09-23 哈尔滨理工大学 W 18 O 49 BiOX composite photocatalytic material and preparation method thereof
CN114797852A (en) * 2022-03-17 2022-07-29 太原理工大学 Ru/W with oxygen-containing defects 18 O 49 Preparation method of photocatalyst and application of photocatalyst in hydrogen storage field

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