CN103301833A - Yb<3+>-Tm<3+>-Li<+> triple-doped Bi2WO6/CNTs (carbon nanotubes) upconversion photocatalytic material - Google Patents

Yb<3+>-Tm<3+>-Li<+> triple-doped Bi2WO6/CNTs (carbon nanotubes) upconversion photocatalytic material Download PDF

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CN103301833A
CN103301833A CN2013100441207A CN201310044120A CN103301833A CN 103301833 A CN103301833 A CN 103301833A CN 2013100441207 A CN2013100441207 A CN 2013100441207A CN 201310044120 A CN201310044120 A CN 201310044120A CN 103301833 A CN103301833 A CN 103301833A
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CN103301833B (en
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朱南文
黄寿强
楼紫阳
袁海平
单爱党
谷麟
苗琛
寿宗奇
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Shanghai Jiaotong University
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Abstract

The invention discloses a Yb<3+>-Tm<3+>-Li<+> triple-doped Bi2WO6/CNTs (carbon nanotubes) upconversion photocatalytic material which is prepared by the following steps of: performing acidic purification on CNTs, filtering and rinsing the CNTs, performing vacuum drying on the CNTs, and adding the CNTs into a Bi(NO3)3*5H2O aqueous solution to obtain a colloid solution I containing Bi<3+>; adding Na2WO4*2H2O into the colloid solution I, and then adding Yb(NO3)3*5H2O and Tm(NO3)3*5H2O and LiNO3 into the solution to obtain a colloid solution II; and continuously performing a hydrothermal reaction at 120-180 DEG C, and calcining products under inert gas with the temperature of 400-700 DEG C after being subjected to centrifugation and drying. An absorption belt edge of the photocatalytic material disclosed by the invention is 550 nm or so; compared with the photocatalytic activity of pure Bi2WO6, the photocatalytic activity of the Yb<3+>-Tm<3+>-Li<+> triple-doped Bi2WO6/CNTs upconversion photocatalytic material is greatly improved; and the Yb<3+>-Tm<3+>-Li<+> triple-doped Bi2WO6/CNTs upconversion photocatalytic material has a good effect of degrading organic dye wastewater.

Description

Yb 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs
Technical field
The invention belongs to field of photocatalytic material, be specifically related to a kind of Yb 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs.
Background technology
Last converting photocatalysis material is a kind of new material that can be used for difficult biochemical treatment of Organic Wastewater, and this material is composited by the rare earth ion with up-conversion luminescence function and catalysis material.Rare earth ion with up-conversion luminescence function mainly contains Er 3+, Tm 3+, Ho 3+, Yb 3+Deng, these ions have abundant energy level, low-energy photon can be converted to high-energy photons, namely have the function that long wavelength's light is converted to the light of shorter wavelength.Catalysis material is generally with TiO 2, ZnO, CdS etc. are material, these materials can utilize the short light of sunshine medium wavelength to drive photochemical reaction and then make that organic matter obtains degraded in the waste water.Therefore, with Er 3+, Tm 3+, Ho 3+, Yb 3+Introduce in the catalysis material Deng rare earth ion, with the converting photocatalysis material is had the near infrared light in the sunshine or visible light are converted to more short wavelength's visible light and the function of ultraviolet light, thereby can obtain more short-wavelength light exciting light catalytic reactions, effectively improve the utilization rate of sunshine.
Bi 2WO 6Be the TiO that a kind of ratio is used always at present 2Have the more novel photocatalysis material of low energy gap width, its energy gap is 2.7eV, has visible light (＜459nm) catalytic activity.If it is rare earth ion doped to Bi will to go up conversion 2WO 6In, may be than the rear-earth-doped TiO of present report 2Has higher sunshine utilization ratio.There is bibliographical information to claim, the alkali metal Li of ionic radius minimum +Can improve Er greatly 3+/ Yb 3+Last switching emission light intensity (pertinent literature: Chinese Journal of Inorganic Chemistry, 2011,27,776; Opt.Mater.2011,284,3311), but shut the rare earth ion doped Bi of conversion 2WO 6Near infrared light catalytic activity and Li +Doping Bi 2WO 6Research still do not have report.
In addition, from existing research, (carbon nanotubes CNTs) is the One-dimensional Quantum lead with excellent conductive performance, the migration of the light induced electron that is highly advantageous to CNT.Simultaneously, it can sensitized semiconductor, reduces semi-conductive energy gap, and can also have the good adsorption effect to dissolved organic matter in wastewater treatment, prolongs the time of contact on organic pollution and catalysis material surface, raising photocatalytic degradation efficient.Therefore, CNT and TiO 2, BiVO 4Deng compound its photocatalysis performance (pertinent literature: J.Phys.Chem.C, 2011,115,22025 of can greatly improving of catalysis material; J.Am.Chem.Soc.2007,129,9401; The patent No.: CN102744058A; Rare Metals, 2011,30,199), but CNT and Bi 2WO 6Combination still do not have report at present.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of Yb with near infrared light catalytic activity is provided 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs.
The objective of the invention is to be achieved through the following technical solutions:
The present invention relates to a kind of Yb 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs, described Yb 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs can be prepared by a method comprising the following steps and get:
A, will CNTs acid purify, filter the back with the deionized water rinse to neutral, disperse and vacuum drying;
B, at Bi (NO 3) 35H 2CNTs in the O aqueous solution behind the described vacuum drying of adding steps A obtains containing Bi 3+Colloidal solution I;
The described Bi that contains of C, step B 3+Colloidal solution I in add Na 2WO 42H 2O, Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3, get colloidal solution II;
D, with the described colloidal solution II of step C 120～180 ℃ of hydro-thermal reactions, products therefrom is calcined under 400～700 ℃ of inert gas shielding conditions after centrifugal and drying, namely gets described Yb 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs.
Preferably, in the steps A, described acid the purification is specially: CNTs is added in the chloroazotic acid, carry out acidity and purify under 80 ℃, add the CNTs1 gram in the described chloroazotic acid of every 10mL.
Preferably, in the steps A, described dispersion is specially: described deionized water rinse is added in the absolute ethyl alcohol to neutral CNTs, and ultrasonic dispersion adds the CNTs1 gram in the described absolute ethyl alcohol of every 10mL.
Preferably, among the step B, the described Bi (NO that states 3) 35H 2The concentration of the O aqueous solution is 0.1mol/L, the described Bi (NO of every 50mL 3) 3CNTs0.0349 in the 5HxO aqueous solution behind the described vacuum drying of adding steps A～0.6978 gram.
Preferably, among the step C, described Na 2WO 42H 2O, Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3Adding be specially: the Na that adds earlier 0.05mol/L 2WO 4The 2HxO aqueous solution after the ultrasonic dispersion, adds Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3Mixture, continue ultrasonic dispersion, get colloidal solution II; Described Bi 3+: WO 4 2-: Yb 3+: Tm 3+: Li +Mol ratio be 1: 0.5: 0.2: (0.001～0.05): 0.1.
Preferably, among the step D, the described hydro-thermal reaction time is 2～12h.
Preferably, among the step D, the time of described calcining is 1～4h.
Principle of the present invention is to utilize Yb 3+To the high absorption efficiency of near infrared light, the energy that absorbs is passed to Tm 3+, Tm 3+Can send green glow, blue light and ultraviolet light by two photons or multi-photon absorption and excite Bi 2WO 6And Li +Doping can destroy Tm 3+The crystalline field symmetry, make Tm 3+Transmitting green light, blue light and ultraviolet light intensity are significantly strengthened.CNT and Bi 2WO 6Compound, not only can increase the migration rate of light induced electron, and can reduce Bi 2WO 6Energy gap, make it absorb band edge and expand more long wavelength's visible-range to, thereby increase the absorption to green glow, blue light.
The present invention has following beneficial effect: the Yb of the present invention's preparation 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs can be converted to the near infrared light of 980nm the blue light of 510 green glow, 476nm and 452nm and the ultraviolet light of 362nm, 347nm and 291nm, can make that methylene blue waste water fades, the organic contamination substrate concentration descends.
The specific embodiment
The present invention is described in detail below in conjunction with specific embodiment.Following examples will help those skilled in the art further to understand the present invention, but not limit the present invention in any form.Should be pointed out that to those skilled in the art, without departing from the inventive concept of the premise, can also make some distortion and improvement.These all belong to protection scope of the present invention.
The invention provides a kind of Yb 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs, enumerate the present invention of embodiment below and be described in further detail:
Embodiment 1
(1) according to per 1 gram CNTs (CNT, carbon nanotubes) needs the ratio of 10mL chloroazotic acid (concentrated hydrochloric acid and red fuming nitric acid (RFNA) volume ratio are 3: 1), CNTs is added in the chloroazotic acid, carry out acidity and purify under 80 ℃ of conditions, the product that obtains is extremely neutral with the distilled water rinse after filtration;
(2) restrain the ratio that CNTs needs the 10mL absolute ethyl alcohol according to per 1, to the beaker that absolute ethyl alcohol is housed, adopt ultrasonic wave that it is disperseed and vacuum drying the transferred product after the acid purification of step (1);
(3) compound concentration is the Bi (NO of 0.1mol/L 3) 35H 2The O aqueous solution is according to the Bi (NO of every 50mL 3) 35H 2The O aqueous solution need add the ratio of 0.0349gCNTs, at Bi (NO 3) 35H 2The CNTs that adds step (2) gained in the O aqueous solution carries out ultrasonic wave and disperses, and obtains containing Bi 3+Colloidal solution;
(4) compound concentration is the Na of 0.05mol/L 2WO 42H 2The O aqueous solution is according to Bi 3+: WO 4 2-Mol ratio be 1: 0.5 mode, with Na 2WO 42H 2The O aqueous solution is added drop-wise to the Bi that contains of step (3) gained 3+Colloidal solution in, carry out ultrasonic wave and disperse;
(5) according to Bi 3+: Yb 3+: Tm 3+: Li +Mol ratio be 1: 0.2: 0.001: 0.1 mode takes by weighing Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3, and it is joined in the colloidal solution of step (4) gained, carry out ultrasonic wave and disperse;
(6) colloidal solution with gained in the step (5) is transferred in the polytetrafluoroethylene (PTFE) reactor, carries out 2 hours hydro-thermal reaction under 120 ℃ of conditions, and products therefrom is after centrifugal and drying, and calcining namely got Yb in 1 hour under 400 ℃ of nitrogen protection conditions 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs.
The Yb that the present invention is prepared 3+-Tm 3+-Li +Three doping Bi 2WO 6The absorption band edge of the last converting photocatalysis material of/CNTs is about 480nm, it excites down at the 980nm near infrared light, can send the blue light of 476nm and 452nm and the ultraviolet light of 362nm, 347nm and 291nm, making concentration is that the percent of decolourization of methylene blue waste water in 12 hours of 10mg/L reaches 75%, COD clearance and reach 63%.
Embodiment 2
(1) according to per 1 gram CNTs (CNT, carbon nanotubes) needs the ratio of 10mL chloroazotic acid (concentrated hydrochloric acid and red fuming nitric acid (RFNA) volume ratio are 3: 1), CNTs is added in the chloroazotic acid, carry out acidity and purify under 80 ℃ of conditions, the product that obtains is extremely neutral with the distilled water rinse after filtration;
(2) restrain the ratio that CNTs needs the 10mL absolute ethyl alcohol according to per 1, to the beaker that absolute ethyl alcohol is housed, adopt ultrasonic wave that it is disperseed and vacuum drying the transferred product after the acid purification of step (1);
(3) compound concentration is the Bi (NO of 0.1mol/L 3) 35H 2The O aqueous solution is according to the Bi (NO of every 50mL 3) 35H 2The O aqueous solution need add the ratio of 0.1745gCNTs, at Bi (NO 3) 35H 2The CNTs that adds step (2) gained in the O aqueous solution carries out ultrasonic wave and disperses, and obtains containing Bi 3+Colloidal solution;
(4) compound concentration is the Na of 0.05mol/L 2WO 42H 2The O aqueous solution is according to Bi 3+: WO 4 2-Mol ratio be 1: 0.5 mode, with Na 2WO 42H 2The O aqueous solution is added drop-wise in the colloidal solution that contains Bi3+ of step (3) gained, carries out ultrasonic wave and disperses;
(5) according to Bi 3+: Yb 3+: Tm 3+: Li +Mol ratio be 1: 0.2: 0.05: 0.1 mode takes by weighing Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3, and it is joined in the colloidal solution of step (4) gained, carry out ultrasonic wave and disperse;
(6) colloidal solution with gained in the step (5) is transferred in the polytetrafluoroethylene (PTFE) reactor, carries out 12 hours hydro-thermal reaction under 180 ℃ of conditions, and products therefrom is after centrifugal and drying, and calcining namely got Yb in 4 hours under 500 ℃ of nitrogen protection conditions 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs.
The Yb that the present invention is prepared 3+-Tm 3+-Li +Three doping Bi 2WO 6The absorption band edge of the last converting photocatalysis material of/CNTs is about 550nm, it excites down at the 980nm near infrared light, can send the blue light of 510 green glow, 476nm and 452nm and the ultraviolet light of 362nm, 347nm and 291nm, making concentration is that the percent of decolourization of methylene blue waste water in 12 hours of 10mg/L reaches 95%, COD clearance and reach 82%.
Embodiment 3
(1) according to per 1 gram CNTs (CNT, carbon nanotubes) needs the ratio of 10mL chloroazotic acid (concentrated hydrochloric acid and red fuming nitric acid (RFNA) volume ratio are 3: 1), CNTs is added in the chloroazotic acid, carry out acidity and purify under 80 ℃ of conditions, the product that obtains is extremely neutral with the distilled water rinse after filtration;
(2) restrain the ratio that CNTs needs the 10mL absolute ethyl alcohol according to per 1, to the beaker that absolute ethyl alcohol is housed, adopt ultrasonic wave that it is disperseed and vacuum drying the transferred product after the acid purification of step (1);
(3) compound concentration is the Bi (NO of 0.1mol/L 3) 35H 2The O aqueous solution is according to the Bi (NO of every 50mL 3) 35H 2The O aqueous solution need add the ratio of 0.6978gCNTs, at Bi (NO 3) 35H 2The CNTs that adds step (2) gained in the O aqueous solution carries out ultrasonic wave and disperses, and obtains containing Bi 3+Colloidal solution;
(4) compound concentration is the Na of 0.05mol/L 2WO 42H 2The O aqueous solution is according to Bi 3+: WO 4 2-Mol ratio be 1: 0.5 mode, with Na 2WO 42H 2The O aqueous solution is added drop-wise to the Bi that contains of step (3) gained 3+Colloidal solution in, carry out ultrasonic wave and disperse;
(5) according to Bi 3+: Yb 3+: Tm 3+: Li +Mol ratio be 1: 0.2: 0.01: 0.1 mode takes by weighing Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3, and it is joined in the colloidal solution of step (4) gained, carry out ultrasonic wave and disperse;
(6) colloidal solution with gained in the step (5) is transferred in the polytetrafluoroethylene (PTFE) reactor, carries out 6 hours hydro-thermal reaction under 140 ℃ of conditions, and products therefrom is after centrifugal and drying, and calcining namely got Yb in 2 hours under 600 ℃ of nitrogen protection conditions 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs.
The Yb that the present invention is prepared 3+-Tm 3+-Li +Three doping Bi 2WO 6The absorption band edge of the last converting photocatalysis material of/CNTs is about 550nm, it excites down at the 980nm near infrared light, can send the blue light of 510 green glow, 476nm and 452nm and the ultraviolet light of 362nm, 347nm and 291nm, making concentration is that the percent of decolourization of methylene blue waste water in 12 hours of 10mg/L reaches 83%, COD clearance and reach 70%.
Embodiment 4
(1) according to per 1 gram CNTs (CNT, carbon nanotubes) needs the ratio of 10mL chloroazotic acid (concentrated hydrochloric acid and red fuming nitric acid (RFNA) volume ratio are 3: 1), CNTs is added in the chloroazotic acid, carry out acidity and purify under 80 ℃ of conditions, the product that obtains is extremely neutral with the distilled water rinse after filtration;
(2) restrain the ratio that CNTs needs the 10mL absolute ethyl alcohol according to per 1, to the beaker that absolute ethyl alcohol is housed, adopt ultrasonic wave that it is disperseed and vacuum drying the transferred product after the acid purification of step (1);
(3) compound concentration is the Bi (NO of 0.1mol/L 3) 35H 2The O aqueous solution is according to the Bi (NO of every 50mL 3) 35H 2The O aqueous solution need add the ratio of 0.3489gCNTs, at Bi (NO 3) 35H 2The CNTs that adds step (2) gained in the O aqueous solution carries out ultrasonic wave and disperses, and obtains containing Bi 3+Colloidal solution;
(4) compound concentration is the Na of 0.05mol/L 2WO 42H 2The O aqueous solution is according to Bi 3+: WO 4 2-Mol ratio be 1: 0.5 mode, with Na 2WO 42H 2The O aqueous solution is added drop-wise to the Bi that contains of step (3) gained 3+Colloidal solution in, carry out ultrasonic wave and disperse;
(5) according to Bi 3+: Yb 3+: Tm 3+: Li +Mol ratio be 1: 0.2: 0.03: 0.1 mode takes by weighing Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3, and it is joined in the colloidal solution of step (4) gained, carry out ultrasonic wave and disperse;
(6) colloidal solution with gained in the step (5) is transferred in the polytetrafluoroethylene (PTFE) reactor, carries out 9 hours hydro-thermal reaction under 160 ℃ of conditions, and products therefrom is after centrifugal and drying, and calcining namely got Yb in 3 hours under 700 ℃ of nitrogen protection conditions 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs.
The Yb that the present invention is prepared 3+-Tm 3+-Li +Three doping Bi 2WO 6The absorption band edge of the last converting photocatalysis material of/CNTs is about 550nm, it excites down at the 980nm near infrared light, can send the blue light of 510 green glow, 476nm and 452nm and the ultraviolet light of 362nm, 347nm and 291nm, making concentration is that the percent of decolourization of methylene blue waste water in 12 hours of 10mg/L reaches 88%, COD clearance and reach 76%.
More than specific embodiments of the invention are described.It will be appreciated that the present invention is not limited to above-mentioned specific implementations, those skilled in the art can make various distortion or modification within the scope of the claims, and this does not influence flesh and blood of the present invention.

Claims (7)

1. Yb 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs is characterized in that described material can be prepared by a method comprising the following steps and get:
A, will CNTs acid purify, filter the back with the deionized water rinse to neutral, disperse and vacuum drying;
B, at Bi (NO 3) 35H 2CNTs in the O aqueous solution behind the described vacuum drying of adding steps A obtains containing Bi 3+Colloidal solution I;
C, at the described Bi that contains of step B 3+Colloidal solution I in add Na 2WO 42H 2O, Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3, get colloidal solution II;
D, with the described colloidal solution II of step C 120～180 ℃ of hydro-thermal reactions, products therefrom is calcined under 400～700 ℃ of inert gas shielding conditions after centrifugal and drying, namely gets described Yb 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs.
2. Yb according to claim 1 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs is characterized in that, in the steps A, described acid the purification is specially: CNTs is added in the chloroazotic acid, carry out acidity and purify under 80 ℃, add the CNTs1 gram in the described chloroazotic acid of every 10mL.
3. Yb according to claim 1 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs is characterized in that, in the steps A, described dispersion is specially: described deionized water rinse is added in the absolute ethyl alcohol to neutral CNTs, and ultrasonic dispersion adds the CNTs1 gram in the described absolute ethyl alcohol of every 10mL.
4. Yb according to claim 1 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs is characterized in that, among the step B, and described Bi (NO 3) 35H 2The concentration of the O aqueous solution is 0.1mol/L, the described Bi (NO of every 50mL 3) 35H 2CNTs0.0349 in the O aqueous solution behind the described vacuum drying of adding steps A～0.6978 gram.
5. Yb according to claim 1 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs is characterized in that, among the step C, and described Na 2WO 42H 2O, Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3Adding be specially: the Na that adds earlier 0.05mol/L 2WO 42H 2The O aqueous solution after the ultrasonic dispersion, adds Yb (NO 3) 35H 2O, Tm (NO 3) 35H 2O, LiNO 3Mixture, continue ultrasonic dispersion, get colloidal solution II; Described Bi 3+: WO 4 2-: Yb 3+: Tm 3+: Li +Mol ratio be 1: 0.5: 0.2: (0.001～0.05): 0.1.
6. Yb according to claim 1 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs is characterized in that, among the step D, the described hydro-thermal reaction time is 2～12h.
7. Yb according to claim 1 3+-Tm 3+-Li +Three doping Bi 2WO 6The last converting photocatalysis material of/CNTs is characterized in that, among the step D, the time of described calcining is 1～4h.
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CN108754391A (en) * 2018-07-26 2018-11-06 中原工学院 Bi2WO6The preparation method and application of the compound-modified dynamic interception stainless steel wire of crystallite
CN108975710A (en) * 2018-07-26 2018-12-11 中原工学院 The preparation method and applications of glazed tile for river phytal zone slope protection
CN108993609A (en) * 2018-08-16 2018-12-14 南京工业大学 A kind of preparation method and applications of high-dispersion metal catalyst
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