CN105435778B - A kind of nanometer-material-modified layered titanium potassium niobate and its preparation method and application - Google Patents

A kind of nanometer-material-modified layered titanium potassium niobate and its preparation method and application Download PDF

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CN105435778B
CN105435778B CN201510439032.6A CN201510439032A CN105435778B CN 105435778 B CN105435778 B CN 105435778B CN 201510439032 A CN201510439032 A CN 201510439032A CN 105435778 B CN105435778 B CN 105435778B
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CN105435778A (en
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杨萍
刘赛
胡俊
何杰
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Anhui University of Science and Technology
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Abstract

The invention discloses a kind of nanometer-material-modified layered titanium potassium niobate, its raw material includes by weight:Ion exchange product 0.1 4, SDBS 0.01 0.5, KMnO40.1 1, deionized water 10 50;Wherein, the raw material of ion exchange product includes predecessor and 0.5 3mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:400‑800;The raw material of predecessor includes by weight:K2CO30.5 4, TiO20.1 4, Nb2O50.1‑5;The invention also discloses a kind of preparation method of nanometer-material-modified layered titanium potassium niobate;The invention also discloses a kind of application of nanometer-material-modified layered titanium potassium niobate;Inventive article has excellent absorption and ultraviolet catalytic effect, and photocatalysis efficiency is high, available for absorption and under ultraviolet light catalytic degradation organic dyestuff.

Description

A kind of nanometer-material-modified layered titanium potassium niobate and its preparation method and application
Technical field
The present invention relates to nanometer-material-modified layered titanium potassium niobate technical field, more particularly to a kind of nanometer-material-modified layer Shape titanium potassium niobate and its preparation method and application.
Background technology
In recent years, environmental protection turns into the important motivity of the environmentally friendly catalyst of people's R and D.People chase after The target asked is each molecule in raw material is changed into target product, and any waste and byproduct are not produced, is realized dirty The zero-emission of thing is contaminated, and does not use any poisonous and hazardous raw material, catalysts and solvents in production, environmentally friendly production is prepared Product.But environmental pollution is still the Tough questions faced needed for current human social.Therefore, urged using semiconductor light Change oxidation technology curb environmental pollution problem basis developed rapidly with application study, as both at home and abroad most active research field One of.Zhai etc. is by NiO and HTiNbO5The NiO/HTiNbO of composite modified preparation5, rhodamine B can be degraded to aliphatic organic The oxide of compound and simple carbon.The research about nanometer-material-modified layered titanium potassium niobate does not reach demand also at present, How to prepare it is a kind of there is high absorption and excellent ultraviolet catalytic effect to organic dyestuff (MB), and be remarkably improved to there is engine dyeing The nanometer-material-modified layered titanium potassium niobate of the catalytic efficiency of material turns into the current technical issues that need to address.
The content of the invention
The present invention proposes a kind of nanometer-material-modified layered titanium potassium niobate and its preparation method and application, and product has excellent Different absorption and ultraviolet catalytic effect, high catalytic efficiency, can be applied to catalytic degradation organic dyestuff.
A kind of nanometer-material-modified layered titanium potassium niobate proposed by the present invention, its raw material includes by weight:Ion exchange 0.1-4 parts of product, 0.01-0.5 parts of SDBS, KMnO40.1-1 parts, 10-50 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 0.5-3mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:400-800;
Wherein, the raw material of predecessor includes by weight:K2CO30.5-4 parts, TiO20.1-4 parts, Nb2O50.1-5 parts.
Preferably, its raw material includes by weight:0.5-2 parts of ion exchange product, 0.05-0.2 parts of SDBS, KMnO4 0.3-0.5 parts, 18-22 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 1-2mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:500-600;
Wherein, the raw material of predecessor includes by weight:K2CO31-1.5 part, TiO21.2-2 part, Nb2O52-3 parts.
Preferably, its raw material includes by weight:0.8-1.2 parts of ion exchange product, 0.08-0.12 parts of SDBS, KMnO40.35-0.46 parts, 19-21 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 1.6-1.8mol/L Mn (NO3)2Solution, predecessor with Mn(NO3)2The w/v g of solution:Ml is 1:550-560;
Wherein, the raw material of predecessor includes by weight:K2CO31.2-1.4 part, TiO21.5-1.6 part, Nb2O5 2.4- 2.7 part.
Invention additionally discloses a kind of nanometer-material-modified layered titanium potassium niobate preparation method, comprise the following steps:
S1, by K2CO3、TiO2And Nb2O5Grind uniform after mixing, in 60-100 DEG C of dry 10-15h, feeding Muffle furnace 20-40h is calcined in 900-1300 DEG C, it is uniform to take out grinding, washing, dry predecessor;
S2, predecessor is dispersed in Mn (NO3)2In solution, stirring is shaken at 15-40 DEG C, suction filtration, washing, 70-90 is taken out DEG C drying, grind, obtain ion exchange product;
S3, addition SDBS, KMnO into ion exchange product4And deionized water, it is then fed into polytetrafluoroethylliner liner 1-4h is stirred in autoclave, autoclave is put into baking oven, 140-180 DEG C of reaction 10-15h of setting constant temperature, cooling Taken out to normal temperature, nanometer-material-modified layered titanium potassium niobate is arrived in centrifugation, washing.
By KTiNbO5I.e. predecessor, ion exchange product is obtained by ion exchange, then obtains mesoporous through hydro-thermal reaction Material is nanometer-material-modified layered titanium potassium niobate, and it is as shown in Figure 5 that it synthesizes schematic diagram.
Preferably, in S1, by K2CO3、TiO2And Nb2O5Grind uniform after mixing, in 75-90 DEG C of dry 11-13h, send Enter in Muffle furnace and to be calcined 20-26h in 1000-1200 DEG C, it is uniform to take out grinding, washing, dry predecessor.
Preferably, in S2, by Mn (NO3)2Solution is divided into isometric 4-8 parts, and predecessor is dispersed in into a Mn (NO3)2 In solution, at 15-40 DEG C after concussion stirring 40-50h, static 10-15h, Mn (NO are changed3)2Solution, so repeatedly to being finished Mn (NO3)2Solution, washing, 70-90 DEG C of drying grinds, obtains ion exchange product.
Preferably, in S2, by Mn (NO3)2Solution is divided into isometric 5-6 parts, and predecessor is dispersed in into a Mn (NO3)2 In solution, at 20-30 DEG C after concussion stirring 45-50h, static 10-14h, Mn (NO are changed3)2Solution, so repeatedly to being finished Mn (NO3)2Solution, washing, 78-84 DEG C of drying grinds, obtains ion exchange product.
Preferably, in S3, SDBS, KMnO are added into ion exchange product4And deionized water, it is then fed into polytetrafluoro 1.5-2.5h is stirred in the autoclave of ethene inner bag, autoclave is put into baking oven, 155-165 DEG C of setting constant temperature is anti- 11-13h is answered, normal temperature taking-up is cooled to, nanometer-material-modified layered titanium potassium niobate is arrived in centrifugation, washing.
Invention additionally discloses a kind of nanometer-material-modified layered titanium potassium niobate application, available for absorption and in ultraviolet light Lower catalytic degradation organic dyestuff.
Preferably, the organic dyestuff is methylene blue.
In the present invention, Layered titanoniobate is that octahedra be connected with each other by common side or corner-sharing centered on Ti and Nb spreads Piece is transformed into form layer structure, stratiform KTiNbO5Have the advantages that ion is commutative, interlayer structure is homogeneous controllable, excessively There is golden oxide predecessor in unique catalytic and semiconductive, the present invention to be that layered titanium potassium niobate has certain photocatalysis Activity, uses it as matrix, exchanges its plate interlayer cation with high concentration Mn2+ solions, then by hydro-thermal method reaction, The material is modified into nano-grade size, the Subjective and Objective of so nanometer-material-modified layered titanium potassium niobate of product is that photocatalysis is lived Property semi-conducting material, due to the interaction of Subjective and Objective, this nanometer-material-modified layered titanium potassium niobate will have than single Material is more rich physically or chemically, and it can produce electronics coupled effect on interface, can effectively suppress photoproduction current-carrying Son it is compound, so as to improve the photocatalytic activity of whole composite, so can realize high absorption to organic dyestuff (MB) and Excellent ultraviolet catalytic effect, substantially increases catalytic efficiency of the organic dyestuff such as methylene blue in product surface.
Brief description of the drawings
Fig. 1 is a kind of preparation technology flow chart of nanometer-material-modified layered titanium potassium niobate proposed by the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph of nanometer-material-modified layered titanium potassium niobate proposed by the present invention.
Fig. 3 is the XRD of nanometer-material-modified layered titanium potassium niobate proposed by the present invention.
Fig. 4 is ultraviolet-visible spectrum point of the nanometer-material-modified layered titanium potassium niobate proposed by the present invention to methylene blue Analysis figure.
Fig. 5 is the synthesis schematic diagram of nanometer-material-modified layered titanium potassium niobate proposed by the present invention.
Embodiment
As shown in Figure 1,2,3, 4, Fig. 1 is a kind of preparation work of nanometer-material-modified layered titanium potassium niobate proposed by the present invention Skill flow chart;Fig. 2 is the scanning electron microscope (SEM) photograph of nanometer-material-modified layered titanium potassium niobate proposed by the present invention;Fig. 3 carries for the present invention The XRD of the nanometer-material-modified layered titanium potassium niobate gone out;Fig. 4 is nanometer-material-modified layered titanium potassium niobate proposed by the present invention To the ultraviolet-visible spectrum analysis chart of methylene blue.
Below, technical scheme is described in detail by specific embodiment.
Embodiment 1
A kind of nanometer-material-modified layered titanium potassium niobate, its raw material includes by weight:0.1 part of ion exchange product, 0.5 part of SDBS, KMnO40.1 part, 50 parts of deionized water;kk
Wherein, the raw material of ion exchange product includes predecessor and 0.5mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:400;
Wherein, the raw material of predecessor includes by weight:K2CO30.5 part, TiO24 parts, Nb2O50.1 part.
Embodiment 2
A kind of nanometer-material-modified layered titanium potassium niobate, its raw material includes by weight:4 parts of ion exchange product, SDBS 0.01 part, KMnO41 part, 10 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 3mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:800;
Wherein, the raw material of predecessor includes by weight:K2CO34 parts, TiO20.1 part, Nb2O55 parts.
Embodiment 3
A kind of nanometer-material-modified layered titanium potassium niobate, its raw material includes by weight:0.5 part of ion exchange product, 0.2 part of SDBS, KMnO40.3 part, 22 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 1mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:500;
Wherein, the raw material of predecessor includes by weight:K2CO31 part, TiO22 parts, Nb2O52 parts.
Reference picture 1, the preparation method of described nanometer-material-modified layered titanium potassium niobate, comprises the following steps:
S1, by K2CO3、TiO2And Nb2O5Grind uniform after mixing, in 910 DEG C in 60 DEG C of dry 15h, feeding Muffle furnace 39h is calcined, it is uniform to take out grinding, washing, dry predecessor.
S2, predecessor is dispersed in Mn (NO3)2In solution, stirring is shaken at 15 DEG C, suction filtration is taken out, washed, 88 DEG C of drying, Grind, obtain ion exchange product;
S3, addition SDBS, KMnO into ion exchange product4And deionized water, it is then fed into polytetrafluoroethylliner liner 1h is stirred in autoclave, autoclave is put into baking oven, 178 DEG C of reaction 10h of setting constant temperature are cooled to normal temperature and taken Go out, centrifuge, nanometer-material-modified layered titanium potassium niobate is arrived in washing.
Embodiment 4
A kind of nanometer-material-modified layered titanium potassium niobate, its raw material includes by weight:2 parts of ion exchange product, SDBS 0.05 part, KMnO40.5 part, 18 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 2mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:600;
Wherein, the raw material of predecessor includes by weight:K2CO31.5 parts, TiO21.2 parts, Nb2O53 parts.
The preparation method of described nanometer-material-modified layered titanium potassium niobate, comprises the following steps:
S1, by K2CO3、TiO2And Nb2O5Grind uniform after mixing, in 1300 DEG C in 99 DEG C of dry 10h, feeding Muffle furnace 21h is calcined, it is uniform to take out grinding, washing, dry predecessor.
S2, by Mn (NO3)2Solution is divided into isometric 4 parts, and predecessor is dispersed in into a Mn (NO3)2In solution, at 40 DEG C After concussion stirring 40h, static 15h, Mn (NO are changed3)2Solution, so repeatedly to being finished Mn (NO3)2Solution, washing, 70 DEG C of bakings It is dry, grind, obtain ion exchange product
S3, addition SDBS, KMnO into ion exchange product4And deionized water, it is then fed into polytetrafluoroethylliner liner 4h is stirred in autoclave, autoclave is put into baking oven, 142 DEG C of reaction 15h of setting constant temperature are cooled to normal temperature and taken Go out, centrifuge, nanometer-material-modified layered titanium potassium niobate is arrived in washing.
Embodiment 5
A kind of nanometer-material-modified layered titanium potassium niobate, its raw material includes by weight:0.8 part of ion exchange product, 0.12 part of SDBS, KMnO40.35 part, 21 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 1.6mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:550;
Wherein, the raw material of predecessor includes by weight:K2CO31.2 parts, TiO21.6 parts, Nb2O52.4 part.
The preparation method of described nanometer-material-modified layered titanium potassium niobate, comprises the following steps:
S1, by K2CO3、TiO2And Nb2O5Grind uniform after mixing, in 1000 DEG C in 76 DEG C of dry 13h, feeding Muffle furnace 25h is calcined, it is uniform to take out grinding, washing, dry predecessor.
S2, by Mn (NO3)2Solution is divided into isometric 8 parts, and predecessor is dispersed in into a Mn (NO3)2In solution, at 15 DEG C After concussion stirring 50h, static 10h, Mn (NO are changed3)2Solution, so repeatedly to being finished Mn (NO3)2Solution, washing, 90 DEG C of bakings It is dry, grind, obtain ion exchange product.
S3, addition SDBS, KMnO into ion exchange product4And deionized water, it is then fed into polytetrafluoroethylliner liner 1.6h is stirred in autoclave, autoclave is put into baking oven, 165 DEG C of reaction 11h of setting constant temperature are cooled to normal temperature and taken Go out, centrifuge, nanometer-material-modified layered titanium potassium niobate is arrived in washing.
Described nanometer-material-modified layered titanium potassium niobate can be used for absorption organic dyestuff.
Embodiment 6
A kind of nanometer-material-modified layered titanium potassium niobate, its raw material includes by weight:1.2 parts of ion exchange product, 0.08 part of SDBS, KMnO40.46 part, 19 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 1.8mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:560;
Wherein, the raw material of predecessor includes by weight:K2CO31.4 parts, TiO21.5 parts, Nb2O52.7 part.
The preparation method of described nanometer-material-modified layered titanium potassium niobate, comprises the following steps:
S1, by K2CO3、TiO2And Nb2O5Grind uniform after mixing, in 1950 DEG C in 90 DEG C of dry 11h, feeding Muffle furnace 21h is calcined, it is uniform to take out grinding, washing, dry predecessor.
S2, by Mn (NO3)2Solution is divided into isometric 5 parts, and predecessor is dispersed in into a Mn (NO3)2In solution, at 30 DEG C After concussion stirring 45h, static 14h, Mn (NO are changed3)2Solution, so repeatedly to being finished Mn (NO3)2Solution, washing, 78 DEG C of bakings It is dry, grind, obtain ion exchange product.
S3, addition SDBS, KMnO into ion exchange product4And deionized water, it is then fed into polytetrafluoroethylliner liner 2.5h is stirred in autoclave, autoclave is put into baking oven, 156 DEG C of reaction 13h of setting constant temperature are cooled to normal temperature and taken Go out, centrifuge, nanometer-material-modified layered titanium potassium niobate is arrived in washing.
Described nanometer-material-modified layered titanium potassium niobate can be used for absorption organic dyestuff.
Embodiment 7
A kind of nanometer-material-modified layered titanium potassium niobate, its raw material includes by weight:Ion exchange product 1g, SDBS 0.1g, KMnO40.458g, deionized water 20g;
Wherein, the raw material of ion exchange product includes predecessor and 1.5mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:Ml is 1:560;
Wherein, the raw material of predecessor includes by weight:K2CO31.3296g, TiO21.5373g, Nb2O5 2.5571g。
The preparation method of described nanometer-material-modified layered titanium potassium niobate, comprises the following steps:
S1, by K2CO3、TiO2And Nb2O5It is mixed in agate mortar and grinds uniform, in 80 DEG C of dry 12h, sends into Muffle furnace In be calcined 24h in 1100 DEG C, it is uniform to take out grinding, through distilling water washing, dry white solid powder predecessor.
S2, by Mn (NO3)2Solution is divided into isometric 5 parts, and predecessor is dispersed in into a Mn (NO3)2In solution, at 25 DEG C After concussion stirring 48h, static 12h, Mn (NO are changed3)2Solution, so repeatedly to being finished Mn (NO3)2Solution, washing, 80 DEG C of bakings It is dry, grind, obtain ion exchange product;
S3, addition SDBS, KMnO into ion exchange product4And deionized water, it is then fed into polytetrafluoroethylliner liner Magnetic agitation 2h in autoclave, autoclave is put into baking oven, 160 DEG C of reaction 12h of setting constant temperature, is cooled to normal temperature Take out, nanometer-material-modified layered titanium potassium niobate is arrived in centrifugation, washing, and reference picture 2, Fig. 3, what is respectively prepared is nanometer-material-modified The scanning electron microscope (SEM) photograph and XRD of layered titanium potassium niobate.As seen from Figure 2, after manganese ion exchange and hydro-thermal reaction, titanium niobium The interlayer structure of sour potassium is opened, and whole material shows mesoporous sandwich construction.By most of feature of 10 to 60 degree in Fig. 3 Peak can be attributed to the peak of titanium potassium niobate, it is possible thereby to judge the doping by manganese ion and further hydro-thermal reaction, although The pattern of titanium potassium niobate is changed, but the main body of material is still based on titanium potassium niobate.
After hydro-thermal reaction, additive Mn titanium potassium niobate pattern is changed into mesoporous layer structure, and such material can be used for adsorbing Methylene blue, nanometer-material-modified layered titanium potassium niobate adsorbs the specific adsorption process of methylene blue and is:
To nanometer-material-modified layered titanium potassium niobate add deionized water be configured to concentration be 16% mixed liquor, be placed in from It is standby in heart test tube;
1), 100mL is taken to be added in three conical flasks respectively the 0.02g/L methylene blue solutions newly prepared, magnetic force is stirred Mixing makes it suspend, and is separately added into 0.5mL, 0.7mL, 1.0mL finely dispersed mixed liquor, and lucifuge absorption takes every 5min The 1.0mL solution is simultaneously centrifuged, and is diluted to 6mL with liquid-transfering gun, then carries out ultraviolet-visible light adsorption analysis.
2), 100mL is taken to be added in glass cold-trap reactor respectively the 0.02g/L methylene blue solutions newly prepared, plus Enter 0.7mL mixed liquors, magnetic agitation makes it suspend, at once the photocatalysis under 500W xenon lamps, the 1.0mL solution is taken every 5min And centrifuge, and 6mL is diluted to liquid-transfering gun, then carry out ultraviolet-visible light adsorption analysis.
3), 100mL is taken to be added in glass cold-trap reactor respectively the 0.02g/L methylene blue solutions newly prepared, plus Enter 0.7mL mixed liquors, magnetic agitation makes it suspend, after lucifuge absorption 0.5h, the photocatalysis under 500W xenon lamps takes every 5min The 1.0mL solution is simultaneously centrifuged, and is diluted to 6mL with liquid-transfering gun, then carries out ultraviolet-visible light adsorption analysis.
4), 100mL is taken to be added in glass cold-trap reactor respectively the 0.02g/L methylene blue solutions newly prepared, plus Entering 0.7mL, lucifuge is adsorbed to the mixed liquor of saturation, and magnetic agitation makes it suspend, the photocatalysis under 500W xenon lamps, every 5min takes the 1.0mL solution and centrifuged, and is diluted to 6mL with liquid-transfering gun, then carries out ultraviolet-visible light adsorption analysis.
Wherein, to methylene blue absorption and catalytic hydrogenation is used to evaluate synthesized nanometer-material-modified layered titanium The absorption of potassium niobate and catalytic capability, ultraviolet-visible spectrum is to illustrate the catalytic oxidation process to methylene blue.
Reference picture 4, by ultraviolet-visible light analysis of spectrum, there is obvious absworption peak to methylene blue at 664nm, however, When nanometer-material-modified layered titanium potassium niobate is mixed with methylene blue solution, over time, peak at 664nm by Decrescence weak, this shows, under the absorption or catalytic action of nanometer-material-modified layered titanium potassium niobate methylene blue gradually by by Gradually adsorb or be degraded into other products of ultraviolet-visible light without absorption.Reaction rate can be shown at once.When When being tested under the conditions of lucifuge the rate of adsorption of nanometer-material-modified layered titanium potassium niobate, with nanometer-material-modified stratiform The increase of titanium niobic acid potassium application rate, adsorption effect is more obvious, so that can reach 98% in the blue adsorption rate of 35nim methylenes. The more moderate 0.7mL of nanometer-material-modified layered titanium potassium niobate amount ratio in adsorption experiment is taken, methylene blue solution is adopted respectively Cut-off connects photocatalytic after photocatalytic, absorption 0.5h and degraded, and treats nanometer-material-modified layered titanium potassium niobate to methylene blue Photocatalytic degradation again after adsorption saturation, reaches more than 95%, the nano material from the degradation rate of methylene blue after 255min Modification layered titanium potassium niobate has excellent Photocatalytic Degradation Property, in summary, the nanometer-material-modified stratiform that the present invention is synthesized Titanium potassium niobate not only has high absorption capacity to methylene blue but also with excellent Photocatalytic Degradation Property.
The foregoing is only a preferred embodiment of the present invention, but protection scope of the present invention be not limited thereto, Any one skilled in the art the invention discloses technical scope in, technique according to the invention scheme and its Inventive concept is subject to equivalent substitution or change, should all be included within the scope of the present invention.

Claims (9)

1. a kind of nanometer-material-modified layered titanium potassium niobate, it is characterised in that its raw material includes by weight:Ion exchange product 0.1-4 parts, 0.01-0.5 parts of SDBS, KMnO40.1-1 parts, 10-50 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 0.5-3mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:ML is 1:400-800;
Wherein, the raw material of predecessor includes by weight:K2CO30.5-4 parts, TiO20.1-4 parts, Nb2O50.1-5 parts;
The method for preparing the nanometer-material-modified layered titanium potassium niobate comprises the following steps:
S1, by K2CO3、TiO2And Nb2O5Grind uniform after mixing, in 60-100 DEG C of drys 10-15h, send into Muffle furnace in 900-1300 DEG C of roasting 20-40h, it is uniform to take out grinding, washing, dry predecessor;
S2, predecessor is dispersed in Mn (NO3)2In solution, stirring is shaken at 15-40 DEG C, suction filtration, washing, 70-90 DEG C of baking is taken out It is dry, grind, obtain ion exchange product;
S3, addition SDBS, KMnO into ion exchange product4And deionized water, the high pressure for being then fed into polytetrafluoroethylliner liner is anti- Answer and 1-4h is stirred in kettle, autoclave is put into baking oven, 140-180 DEG C of reaction 10-15h of setting constant temperature is cooled to normal temperature Take out, centrifugation, washing obtains nanometer-material-modified layered titanium potassium niobate.
2. nanometer-material-modified layered titanium potassium niobate according to claim 1, it is characterised in that its raw material is wrapped by weight Include:0.5-2 parts of ion exchange product, 0.05-0.2 parts of SDBS, KMnO40.3-0.5 parts, 18-22 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 1-2mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2 The w/v g of solution:ML is 1:500-600;
Wherein, the raw material of predecessor includes by weight:K2CO31-1.5 part, TiO21.2-2 part, Nb2O52-3 parts.
3. nanometer-material-modified layered titanium potassium niobate according to claim 1, it is characterised in that its raw material is wrapped by weight Include:0.8-1.2 parts of ion exchange product, 0.08-0.12 parts of SDBS, KMnO40.35-0.46 parts, 19-21 parts of deionized water;
Wherein, the raw material of ion exchange product includes predecessor and 1.6-1.8mol/L Mn (NO3)2Solution, predecessor and Mn (NO3)2The w/v g of solution:ML is 1:550-560;
Wherein, the raw material of predecessor includes by weight:K2CO31.2-1.4 part, TiO21.5-1.6 part, Nb2O5 2.4-2.7 Part.
4. nanometer-material-modified layered titanium potassium niobate according to claim 1, it is characterised in that in S1, by K2CO3、 TiO2And Nb2O5Grind uniform after mixing, 20- is calcined in 1000-1200 DEG C in 75-90 DEG C of dry 11-13h, feeding Muffle furnace 26h, it is uniform to take out grinding, washing, dry predecessor.
5. nanometer-material-modified layered titanium potassium niobate according to claim 1, it is characterised in that in S2, by Mn (NO3)2 Solution is divided into isometric 4-8 parts, and predecessor is dispersed in into a Mn (NO3)2In solution, concussion stirring 40-50h at 15-40 DEG C, After static 10-15h, Mn (NO are changed3)2Solution, so repeatedly to being finished Mn (NO3)2Solution, washing, 70-90 DEG C of drying is ground It is broken, obtain ion exchange product.
6. nanometer-material-modified layered titanium potassium niobate according to claim 1, it is characterised in that in S2, by Mn (NO3)2 Solution is divided into isometric 5-6 parts, and predecessor is dispersed in into a Mn (NO3)2In solution, concussion stirring 45-50h at 20-30 DEG C, After static 10-14h, Mn (NO are changed3)2Solution, so repeatedly to being finished Mn (NO3)2Solution, washing, 78-84 DEG C of drying is ground It is broken, obtain ion exchange product.
7. nanometer-material-modified layered titanium potassium niobate according to claim 1, it is characterised in that in S3, handed over to ion Change addition SDBS, KMnO in product4And deionized water, 1.5- is stirred in the autoclave for being then fed into polytetrafluoroethylliner liner 2.5h, autoclave is put into baking oven, 155-165 DEG C of reaction 11-13h of setting constant temperature, is cooled to normal temperature taking-up, is centrifuged, Wash nanometer-material-modified layered titanium potassium niobate.
8. a kind of application of nanometer-material-modified layered titanium potassium niobate according to claim any one of 1-3, its feature exists In available for absorption and catalytic degradation organic dyestuff under ultraviolet light.
9. the application of nanometer-material-modified layered titanium potassium niobate according to claim 8, it is characterised in that described to have engine dyeing Expect for methylene blue.
CN201510439032.6A 2015-07-22 2015-07-22 A kind of nanometer-material-modified layered titanium potassium niobate and its preparation method and application Active CN105435778B (en)

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