CN103638923B - A kind of rare earth element nd doping Bi 2wO 6composite photo-catalyst and its preparation method and application - Google Patents

A kind of rare earth element nd doping Bi 2wO 6composite photo-catalyst and its preparation method and application Download PDF

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CN103638923B
CN103638923B CN201310415216.XA CN201310415216A CN103638923B CN 103638923 B CN103638923 B CN 103638923B CN 201310415216 A CN201310415216 A CN 201310415216A CN 103638923 B CN103638923 B CN 103638923B
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CN103638923A (en
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谈国强
黄靖
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Yancheng Heye Industrial Investment Co.,Ltd.
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Shaanxi University of Science and Technology
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Abstract

A kind of rare earth element nd doping Bi 2wO 6composite photo-catalyst and its preparation method and application, the mol ratio of respectively five water bismuth nitrates and tungstate dihydrate acid sodium being pressed Bi:W=2:1 is soluble in water, adds six water neodymium nitrates, the content R of Nd after stirring nd=2%-20%, R nd=n nd/ (n bi+ n nd) × 100%, obtains precursor liquid after continuing stirring, prepares Nd doping Bi by microwave-hydrothermal method with the power of 300W at 160-220 DEG C of insulation 30-120min 2wO 6composite photo-catalyst, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Nd 3+.Present invention incorporates the advantage of microwave and hydro-thermal method, technique is simple and easy to control, and manufacturing cycle is short, saves the energy, the rare earth element nd doping Bi of one-step synthesis 2wO 6composite photo-catalyst has good photocatalytic activity, can be used in degradation of organic substances.

Description

A kind of rare earth element nd doping Bi 2wO 6composite photo-catalyst and its preparation method and application
Technical field
The invention belongs to field of functional materials, relate to a kind of rare earth element nd doping Bi 2wO 6composite photo-catalyst and its preparation method and application.
Background technology
Along with modern civilization and scientific and technological develop rapidly, environmental pollution is more and more serious, Environmental Pollution and Control has become the important topic of global common concern, nearly twenty or thirty year, and the mankind's problem of curbing environmental pollution that develops into of Photocatalyst provides an effective approach.At present, desirability and urgency are showed to the searching of novel visible responsive photocatalyst.
Bismuth tungstate has following characteristics as a kind of novel photocatalyst: the Uv and visible light response that (1) is good; (2) thermally-stabilised; (3) photocatalysis is stablized; (4) advantage of lower cost; (5) environmental friendliness.Therefore, Bi 2wO 6the research and development of catalysis material, for improving solar energy utilization ratio, will have potential practical value in the depollution of environment and new energy development.But simultaneously also just because of its energy gap relative narrower, the recombination probability of photo-generate electron-hole is increased, reduces the efficiency of light quantum, thus have influence on Bi 2wO 6photocatalysis performance.
Rare earth because its special electron structure, has the spectral characteristic that general element is incomparable, and the 4f electronics with the compound that the rare earth atom of the 4f shell of underfill or ion are formed can generation transition between f-f configuration or between f-d configuration.Therefore, rare-earth metal doped ion is the focus begun one's study in recent years.Some rare earth oxide itself is also hopeful to use as photochemical catalyst, but generally speaking, carries out considerably less using simple rare earth oxide as the research of photochemical catalyst.And doping content also has a great impact reactivity, there is an optimum concentration value, usual low concentration is useful, high concentration is then unfavorable for the carrying out reacted, doping can cause the destruction of crystal structure too much, thus make catalyst lose catalytic performance, and doping is often difficult to play the effect regulating and change its band structure very little.
In recent years, hydrothermal method was adopted to prepare Bi 2wO 6nanocrystal becomes a focus of research.But, in traditional hydrothermal synthesis method, adopt common conduction often, this mode of heating have that the rate of heat addition is slow, the shortcoming such as reaction time length, heat skewness, thermograde are large, had a strong impact on the character of synthetic powder, particle scale etc.Microwave-hydrothermal method is using microwave as mode of heating, a kind of new method of nano-powder is prepared in conjunction with traditional hydro-thermal method, be suitable for being generalized in large-scale industrial production and go, in the field such as nano materials, ceramic material, show good development momentum and wide application prospect.
Summary of the invention
The object of the present invention is to provide a kind of rare earth element nd doping Bi 2wO 6composite photo-catalyst and its preparation method and application, this preparation method's reaction time is short, and technological process is simple, obtained Nd doping Bi 2wO 6composite photo-catalyst possesses good photocatalytic activity.
In order to achieve the above object, the present invention adopts following technical scheme:
A kind of rare earth element nd doping Bi 2wO 6the preparation method of composite photo-catalyst, comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o and Na 2wO 42H 2o puts into container according to the mol ratio of Bi:W=2:1, then in container, adds water be mixed with mixed solution, and is stirred by mixed solution;
Step 2: by Nd (NO 3) 36H 2o joins in mixed solution, obtains reactant liquor, wherein the addition R of Nd nd=2%-20%, R nd=n nd/ (n bi+ n nd) × 100%, n biand n ndbe respectively the mole of Bi and Nd, reactant liquor is at room temperature stirred, obtain precursor liquid;
Step 3: precursor liquid is moved in microwave hydrothermal reaction kettle, then microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, stops reaction after being incubated 30min-120min at 160 DEG C-220 DEG C;
Step 4: after question response temperature is down to room temperature, takes out microwave hydrothermal reaction kettle, isolates sediment wherein, then by sediment washing, ultrasonic disperse, freeze-day with constant temperature, obtains rare earth element nd doping Bi 2wO 6composite photo-catalyst.
Bi (NO in the mixed solution of described step 1 3) 35H 2the concentration of O is 0.1mol/L-0.6mol/L, Na 2wO 42H 2the concentration of O is 0.05mol/L-0.3mol/L.
The required time that stirs in described step 2 is 20-40min.
Set microwave reaction instrument in described step 3 from room temperature to 100 DEG C, often heat up 50 DEG C of insulation 8min from 100 DEG C, until temperature is raised to 160 DEG C-220 DEG C.
In described step 3, the packing ratio of microwave hydrothermal reaction kettle is 40%-70%, and the liner of microwave hydrothermal reaction kettle is polytetrafluoroethylene (PTFE) material.
Washing in described step 4 for deionized water and absolute ethyl alcohol respectively by sediment washing repeatedly to sediment in neutral, and carry out next time again through the natural sedimentation of a day after each washing and wash.
The time of the ultrasonic disperse in described step 4 is 30-60min.
The baking temperature of the freeze-day with constant temperature in described step 4 is 75-85 DEG C, and drying time is 12-24 hour.
Described rare earth element nd doping Bi 2wO 6the rare earth element nd doping Bi that the preparation method of composite photo-catalyst obtains 2wO 6composite photo-catalyst, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Nd 3+, wherein the content of Nd is R nd=2%-20%, and its pattern is for be self-assembled into flower type structure by nanometer sheet.
Described rare earth element nd doping Bi 2wO 6the rare earth element nd doping Bi that the preparation method of composite photo-catalyst obtains 2wO 6the application of composite photo-catalyst in degradation of organic substances.
Compared with prior art, the present invention has following beneficial effect:
Rare earth element nd doping Bi provided by the invention 2wO 6the preparation method of composite photo-catalyst, with five water bismuth nitrate (Bi (NO 3) 35H 2o) be Bi source, tungstate dihydrate acid sodium (Na 2wO 42H 2o) be W source, according to the mol ratio of Bi:W=2:1 by its preparation Bi soluble in water 2wO 6, then add six water neodymium nitrate (Nd (NO 3) 36H 2o), to Bi 2wO 6carry out Nd 3+doping, by microwave-hydrothermal method by Nd 3+introduce Bi 2wO 6in, prepare rare earth element nd doping Bi 2wO 6composite photo-catalyst, improves pure Bi 2wO 6the efficiency of photocatalysis to degrade organic matter under visible light.The microwave-hydrothermal method that the present invention adopts combines the heat characteristic of microwave uniqueness and the advantage of hydro-thermal method, do not need to add other additive, one-step synthesis product, reaction speed is fast, generated time is short, reaction condition is gentle, reaction efficiency is high, environmental friendliness, technique are simple and easy to control, manufacturing cycle is short, save the energy.
Rare earth element nd doping Bi provided by the invention 2wO 6composite photo-catalyst is orthorhombic phase structure, and regular appearance, purity are higher, has visible light-responded performance, and be a kind of visible light responsible photocatalytic material with high catalytic activity, its main component is Bi 2wO 6, and Bi 2wO 6in containing Nd 3+, its pattern is the structure being self-assembled into class flower pattern by nanometer sheet.Rare earth element nd doping Bi provided by the invention 2wO 6composite photo-catalyst has good visible light photocatalysis active, the Bi that do not adulterate that the photocatalytic activity under its visible ray is obtained under the same terms 2wO 6photocatalytic activity, improve pure phase Bi 2wO 6the problem that catalytic efficiency is low, can be used in degradation of organic substances, has a good application prospect.
Accompanying drawing explanation
Fig. 1 is rare earth element nd doping Bi prepared by the embodiment of the present invention 2 2wO 6the XRD figure of composite photo-catalyst;
Fig. 2 is rare earth element nd doping Bi prepared by the embodiment of the present invention 2 2wO 6the SEM figure of composite photo-catalyst, wherein the multiplication factor of a is 30k times, and the multiplication factor of b is 100k times;
Fig. 3 is rare earth element nd doping Bi prepared by the present invention 2wO 6the degradation rate curve map of composite photo-catalyst, wherein a is Bi when undoping 2wO 6degradation rate curve, b be embodiment 2 prepare rare earth element nd doping Bi 2wO 6the degradation rate curve of composite photo-catalyst.
Detailed description of the invention
Be described further the present invention below in conjunction with accompanying drawing and the preferred embodiment of the invention, it is pure that raw material is analysis.
Embodiment 1:
Rare earth element nd doping Bi 2wO 6the preparation method of composite photo-catalyst, comprises the following steps:
Step 1: take Bi (NO according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, then in beaker, adds deionized water be mixed with mixed solution, wherein Bi (NO 3) 35H 2the concentration of O is 0.2mol/L, Na 2wO 42H 2the concentration of O is 0.1mol/L, and magnetic agitation mixed solution 40min makes raw material wherein mix;
Step 2: take a certain amount of Nd (NO 3) 36H 2o joins in mixed solution, obtains reactant liquor, wherein the addition R of Nd nd=6%(R nd=n nd/ (n bi+ n nd) × 100%, n biand n ndbe respectively the mole of Bi and Nd), obtain precursor liquid by after reactant liquor at room temperature magnetic agitation 40min;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the packing ratio controlling microwave hydrothermal reaction kettle is 40%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, from room temperature to 100 DEG C, often heat up 50 DEG C of insulation 8min from 100 DEG C, until temperature is raised to 180 DEG C, stops reaction after being incubated 90min at 180 DEG C;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate sediment wherein, after respectively sediment washing being repeatedly neutrality to sediment with deionized water and absolute ethyl alcohol (carrying out next time again through the natural sedimentation of a day after each washing to wash), ultrasonic disperse 60min again, again 80 DEG C of freeze-day with constant temperature 12 hours, obtain rare earth element nd doping Bi 2wO 6composite photo-catalyst.
Obtained rare earth element nd doping Bi 2wO 6composite photo-catalyst, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Nd 3+, wherein the content of Nd is R nd=6%, and its pattern is the structure being self-assembled into class flower pattern by nanometer sheet.
Embodiment 2:
Rare earth element nd doping Bi 2wO 6the preparation method of composite photo-catalyst, comprises the following steps:
Step 1: take Bi (NO according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, then in beaker, adds 60ml deionized water be mixed with mixed solution, wherein Bi (NO 3) 35H 2the concentration of O is 0.1mol/L, Na 2wO 42H 2the concentration of O is 0.05mol/L, and magnetic agitation mixed solution 40min makes raw material wherein mix;
Step 2: take a certain amount of Nd (NO 3) 36H 2o joins in mixed solution, obtains reactant liquor, wherein the addition R of Nd nd=10%(R nd=n nd/ (n bi+ n nd) × 100%, n biand n ndbe respectively the mole of Bi and Nd), obtain precursor liquid by after reactant liquor at room temperature magnetic agitation 40min;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the packing ratio controlling microwave hydrothermal reaction kettle is 60%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, from room temperature to 100 DEG C, often heat up 50 DEG C of insulation 8min from 100 DEG C, until temperature is raised to 200 DEG C, stops reaction after being incubated 120min at 200 DEG C;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate sediment wherein, after respectively sediment washing being repeatedly neutrality to sediment with deionized water and absolute ethyl alcohol (carrying out next time again through the natural sedimentation of a day after each washing to wash), ultrasonic disperse 60min again, again 80 DEG C of freeze-day with constant temperature 12 hours, obtain rare earth element nd doping Bi 2wO 6composite photo-catalyst.
Obtained rare earth element nd doping Bi 2wO 6composite photo-catalyst, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Nd 3+, wherein the content of Nd is R nd=10%, and its pattern is the structure being self-assembled into class flower pattern by nanometer sheet.
Fig. 1 is rare earth element nd doping Bi prepared by the embodiment of the present invention 2 2wO 6the XRD figure of composite photo-catalyst, as can be seen from the figure, Nd adulterates Bi 2wO 6all diffraction maximums of composite photo-catalyst are consistent with PDF card (JCPDS NO.39-0256), are orthorhombic phase Bi 2wO 6structure, other impurity phases are not introduced in the doping of Nd.
Fig. 2 is rare earth element nd doping Bi prepared by the embodiment of the present invention 2 2wO 6the SEM figure of composite photo-catalyst, as can be seen from the figure, the Nd doping Bi of preparation 2wO 6composite photo-catalyst is made up of nanometer sheet, and these nanometer sheet are self-assembled into the structure of similar flower pattern.
Fig. 3 is rare earth element nd doping Bi prepared by the present invention 2wO 6the degradation rate curve of composite photo-catalyst, in figure, a, b curve is unadulterated Bi respectively 2wO 6with rare earth element nd doping Bi prepared by embodiment 2 2wO 6composite photo-catalyst to the degradation rate curve of organic degradation thing rhodamine B, ordinate A/A 0for the ratio of the concentration after certain rhodamine B degraded and its initial concentration in moment, wherein unadulterated Bi 2wO 6be according to method of the present invention, undope Nd (NO in step 2 3) 36H 2o obtains.As can be seen from the figure, the rare earth element nd doping Bi of embodiment 2 preparation 2wO 6composite photo-catalyst has very high photocatalysis performance, significantly improves the degradation rate of rhodamine B, and during 90min, its degradation rate is increased to 90% by by 60% when undoping, and rare earth element nd provided by the invention doping Bi is described 2wO 6composite photo-catalyst has good visible light photocatalysis active, can be used in degradation of organic substances.。
Embodiment 3
Rare earth element nd doping Bi 2wO 6the preparation method of composite photo-catalyst, comprises the following steps:
Step 1: take Bi (NO according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, then in beaker, adds deionized water be mixed with mixed solution, wherein Bi (NO 3) 35H 2the concentration of O is 0.6mol/L, Na 2wO 42H 2the concentration of O is 0.3mol/L, and magnetic agitation mixed solution 40min makes raw material wherein mix;
Step 2: take a certain amount of Nd (NO 3) 36H 2o joins in mixed solution, obtains reactant liquor, wherein the addition R of Nd nd=15%(R nd=n nd/ (n bi+ n nd) × 100%, n biand n ndbe respectively the mole of Bi and Nd), obtain precursor liquid by after reactant liquor at room temperature magnetic agitation 20min;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the packing ratio controlling microwave hydrothermal reaction kettle is 70%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, from room temperature to 100 DEG C, often heat up 50 DEG C of insulation 8min from 100 DEG C, until temperature is raised to 220 DEG C, stops reaction after being incubated 60min at 220 DEG C;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate sediment wherein, after respectively sediment washing being repeatedly neutrality to sediment with deionized water and absolute ethyl alcohol (carrying out next time again through the natural sedimentation of a day after each washing to wash), ultrasonic disperse 30min again, again 75 DEG C of freeze-day with constant temperature 24 hours, obtain rare earth element nd doping Bi 2wO 6composite photo-catalyst.
Obtained rare earth element nd doping Bi 2wO 6composite photo-catalyst, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Nd 3+, wherein the content of Nd is R nd=15%, and its pattern is the structure being self-assembled into class flower pattern by nanometer sheet.
Embodiment 4
Rare earth element nd doping Bi 2wO 6the preparation method of composite photo-catalyst, comprises the following steps:
Step 1: take Bi (NO according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, then in beaker, adds deionized water be mixed with mixed solution, wherein Bi (NO 3) 35H 2the concentration of O is 0.4mol/L, Na 2wO 42H 2the concentration of O is 0.2mol/L, and magnetic agitation mixed solution 40min makes raw material wherein mix;
Step 2: take a certain amount of Nd (NO 3) 36H 2o joins in mixed solution, obtains reactant liquor, wherein the addition R of Nd nd=18%(R nd=n nd/ (n bi+ n nd) × 100%, n biand n ndbe respectively the mole of Bi and Nd), obtain precursor liquid by after reactant liquor at room temperature magnetic agitation 40min;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the packing ratio controlling microwave hydrothermal reaction kettle is 50%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, from room temperature to 100 DEG C, often heat up 50 DEG C of insulation 8min from 100 DEG C, until temperature is raised to 160 DEG C, stops reaction after being incubated 30min at 160 DEG C;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate sediment wherein, after respectively sediment washing being repeatedly neutrality to sediment with deionized water and absolute ethyl alcohol (carrying out next time again through the natural sedimentation of a day after each washing to wash), ultrasonic disperse 40min again, again 85 DEG C of freeze-day with constant temperature 12 hours, obtain rare earth element nd doping Bi 2wO 6composite photo-catalyst.
Obtained rare earth element nd doping Bi 2wO 6composite photo-catalyst, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Nd 3+, wherein the content of Nd is R nd=18%, and its pattern is the structure being self-assembled into class flower pattern by nanometer sheet.
Embodiment 5
Rare earth element nd doping Bi 2wO 6the preparation method of composite photo-catalyst, comprises the following steps:
Step 1: take Bi (NO according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, then in beaker, adds deionized water be mixed with mixed solution, wherein Bi (NO 3) 35H 2the concentration of O is 0.3mol/L, Na 2wO 42H 2the concentration of O is 0.15mol/L, and magnetic agitation mixed solution 40min makes raw material wherein mix;
Step 2: take a certain amount of Nd (NO 3) 36H 2o joins in mixed solution, obtains reactant liquor, wherein the addition R of Nd nd=2%(R nd=n nd/ (n bi+ n nd) × 100%, n biand n ndbe respectively the mole of Bi and Nd), obtain precursor liquid by after reactant liquor at room temperature magnetic agitation 30min;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the packing ratio controlling microwave hydrothermal reaction kettle is 55%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, from room temperature to 100 DEG C, often heat up 50 DEG C of insulation 8min from 100 DEG C, until temperature is raised to 190 DEG C, stops reaction after being incubated 50min at 190 DEG C;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate sediment wherein, after respectively sediment washing being repeatedly neutrality to sediment with deionized water and absolute ethyl alcohol (carrying out next time again through the natural sedimentation of a day after each washing to wash), ultrasonic disperse 50min again, again 80 DEG C of freeze-day with constant temperature 16 hours, obtain rare earth element nd doping Bi 2wO 6composite photo-catalyst.
Obtained rare earth element nd doping Bi 2wO 6composite photo-catalyst, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Nd 3+, wherein the content of Nd is R nd=2%, and its pattern is the structure being self-assembled into class flower pattern by nanometer sheet.
Embodiment 6
Rare earth element nd doping Bi 2wO 6the preparation method of composite photo-catalyst, comprises the following steps:
Step 1: take Bi (NO according to the mol ratio of Bi:W=2:1 3) 35H 2o and Na 2wO 42H 2o puts into beaker, then in beaker, adds deionized water be mixed with mixed solution, wherein Bi (NO 3) 35H 2the concentration of O is 0.5mol/L, Na 2wO 42H 2the concentration of O is 0.25mol/L, and magnetic agitation mixed solution 40min makes raw material wherein mix;
Step 2: take a certain amount of Nd (NO 3) 36H 2o joins in mixed solution, obtains reactant liquor, wherein the addition R of Nd nd=20%(R nd=n nd/ (n bi+ n nd) × 100%, n biand n ndbe respectively the mole of Bi and Nd), obtain precursor liquid by after reactant liquor at room temperature magnetic agitation 40min;
Step 3: precursor liquid is moved in teflon-lined microwave hydrothermal reaction kettle, the packing ratio controlling microwave hydrothermal reaction kettle is 65%, again microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, from room temperature to 100 DEG C, often heat up 50 DEG C of insulation 8min from 100 DEG C, until temperature is raised to 170 DEG C, stops reaction after being incubated 100min at 170 DEG C;
Step 4: after question response temperature is down to room temperature, take out microwave hydrothermal reaction kettle, isolate sediment wherein, after respectively sediment washing being repeatedly neutrality to sediment with deionized water and absolute ethyl alcohol (carrying out next time again through the natural sedimentation of a day after each washing to wash), ultrasonic disperse 45min again, again 75 DEG C of freeze-day with constant temperature 20 hours, obtain rare earth element nd doping Bi 2wO 6composite photo-catalyst.
Obtained rare earth element nd doping Bi 2wO 6composite photo-catalyst, its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Nd 3+, wherein the content of Nd is R nd=20%, and its pattern is the structure being self-assembled into class flower pattern by nanometer sheet.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of those of ordinary skill in the art by reading description of the present invention to any equivalence that technical solution of the present invention is taked, is claim of the present invention and contains.

Claims (7)

1. a rare earth element nd doping Bi 2wO 6the preparation method of composite photo-catalyst, is characterized in that, comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o and Na 2wO 42H 2o puts into container according to the mol ratio of Bi:W=2:1, then in container, adds water be mixed with mixed solution, and is stirred by mixed solution; Wherein Bi (NO in mixed solution 3) 35H 2the concentration of O is 0.1mol/L ~ 0.6mol/L, Na 2wO 42H 2the concentration of O is 0.05mol/L ~ 0.3mol/L;
Step 2: by Nd (NO 3) 36H 2o joins in mixed solution, obtains reactant liquor, wherein the addition R of Nd nd=2%-20%, R nd=n nd/ (n bi+ n nd) × 100%, n biand n ndbe respectively the mole of Bi and Nd, reactant liquor is at room temperature stirred, obtain precursor liquid;
Step 3: precursor liquid is moved in microwave hydrothermal reaction kettle, then microwave hydrothermal reaction kettle is put into microwave hydrothermal reaction, setting power is 300W, stops reaction after being incubated 30min-120min at 160 DEG C-220 DEG C;
Step 4: after question response temperature is down to room temperature, takes out microwave hydrothermal reaction kettle, isolates sediment wherein, then by sediment washing, ultrasonic disperse 30-60min, freeze-day with constant temperature 12-24 hour at 75-85 DEG C, obtains rare earth element nd doping Bi 2wO 6composite photo-catalyst.
2. rare earth element nd doping Bi according to claim 1 2wO 6the preparation method of composite photo-catalyst, is characterized in that: the required time that stirs in described step 2 is 20-40min.
3. rare earth element nd doping Bi according to claim 1 2wO 6the preparation method of composite photo-catalyst, is characterized in that: set microwave reaction instrument in described step 3 from room temperature to 100 DEG C, and often heat up 50 DEG C of insulation 8min from 100 DEG C, until temperature is raised to 160 DEG C-220 DEG C.
4. rare earth element nd doping Bi according to claim 1 2wO 6the preparation method of composite photo-catalyst, is characterized in that: in described step 3, the packing ratio of microwave hydrothermal reaction kettle is 40%-70%, and the liner of microwave hydrothermal reaction kettle is polytetrafluoroethylene (PTFE) material.
5. rare earth element nd doping Bi according to claim 1 2wO 6the preparation method of composite photo-catalyst, is characterized in that: the washing in described step 4 for deionized water and absolute ethyl alcohol respectively by sediment washing repeatedly to sediment in neutral, and carry out next time again through the natural sedimentation of a day after each washing and wash.
6. according to the rare earth element nd doping Bi in claim 1-5 described in any one 2wO 6the rare earth element nd doping Bi that the preparation method of composite photo-catalyst obtains 2wO 6composite photo-catalyst, is characterized in that: its main component is the Bi of orthorhombic phase 2wO 6, and Bi 2wO 6in containing Nd 3+, wherein the content of Nd is R nd=2%-20%, and its pattern is for be self-assembled into flower type structure by nanometer sheet.
7. according to the rare earth element nd doping Bi in claim 1-5 described in any one 2wO 6the rare earth element nd doping Bi that the preparation method of composite photo-catalyst obtains 2wO 6the application of composite photo-catalyst in degradation of organic substances.
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CN107185521A (en) * 2017-05-19 2017-09-22 盐城工学院 A kind of catalysis material and preparation method thereof
CN108435227A (en) * 2018-03-14 2018-08-24 苏州甫众塑胶有限公司 A kind of preparation method of efficient stable catalysis material
CN108479759B (en) * 2018-04-24 2021-02-02 吉林建筑大学 Visible light response type lanthanum-doped bismuth tungstate catalyst and preparation method thereof
CN110694611B (en) * 2019-10-15 2022-08-09 大连工业大学 Rare earth modified nRe-M x WO 3 F y Particles and method for producing same
CN111841529A (en) * 2020-07-30 2020-10-30 陕西科技大学 Rare earth doped flaky Tb/Bi2WO6Nano material and preparation method and application thereof
CN114075074B (en) * 2020-08-17 2023-03-14 厦门稀土材料研究所 Rare earth doped tungstate-based high-entropy ceramic and preparation method thereof
CN116532084A (en) * 2023-04-28 2023-08-04 淮安兴淮消防设备有限公司 Nd-doped Bi 2 WO 6 Preparation and application of nanoflower-biomass porous carbon material

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102513096A (en) * 2011-11-17 2012-06-27 陕西科技大学 Co-doped visible light response bismuth tungstate photochemical catalyst and preparation method thereof
CN102553569A (en) * 2011-12-19 2012-07-11 陕西科技大学 Method for preparing nitrogen-doped bismuth tungstate powder photocatalyst through microwave hydrothermal method
CN102718263A (en) * 2012-06-25 2012-10-10 陕西科技大学 Method for preparing fluorine-mixed bismuth tungstate powder through microwave hydrothermal method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102513096A (en) * 2011-11-17 2012-06-27 陕西科技大学 Co-doped visible light response bismuth tungstate photochemical catalyst and preparation method thereof
CN102553569A (en) * 2011-12-19 2012-07-11 陕西科技大学 Method for preparing nitrogen-doped bismuth tungstate powder photocatalyst through microwave hydrothermal method
CN102718263A (en) * 2012-06-25 2012-10-10 陕西科技大学 Method for preparing fluorine-mixed bismuth tungstate powder through microwave hydrothermal method

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
钨酸铋纳米粉体的合成及光催化性能研究;宋丽花;《中国优秀硕士学位论文全文数据库 工程科技I辑》;20121015(第10期);B020-839正文第38-40页 *

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