CN105251475A - Preparation method and application of novel chromium titanate photocatalytic material - Google Patents
Preparation method and application of novel chromium titanate photocatalytic material Download PDFInfo
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- CN105251475A CN105251475A CN201510626583.3A CN201510626583A CN105251475A CN 105251475 A CN105251475 A CN 105251475A CN 201510626583 A CN201510626583 A CN 201510626583A CN 105251475 A CN105251475 A CN 105251475A
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Abstract
Belonging to the field of inorganic photocatalytic materials, the invention discloses a preparation method and application of a novel chromium titanate photocatalytic material. The novel chromium titanate photocatalytic material can be prepared by high temperature solid state method and sol-gel method respectively, the preparation methods are simple, and the prepared photocatalytic material has uniformly distributed granularity and good chemical stability. The photocatalyst has good photocatalytic effect driven by visible light. Experiments confirm that the photocatalyst can effectively degrade organic pollutants under visible light radiation, and is an ideal photocatalytic material.
Description
Technical field
the present invention relates to a kind of preparation method and application thereof of novel inorganic photocatalyst material, particularly for the photochemical catalyst Cr of degradable organic pollutant
2
ti
5
o
13
and preparation method thereof, belong to inorganic field of photocatalytic material.
Background technology
century human kind sustainable development face two greatly challenge be exactly environmental problem and energy problem.And energy security, harmony and natural environment are the necessary conditions of social realization sustainable development.The sun one to shine tellurian energy equivalence second and to burn the energy discharged in 5,000,000 tons of standard coals, and it is more than 10,000 times that the mankind consume gross energy current year that the sun is irradiated to tellurian energy for 1 year.Therefore, efficient quick ground utilizes, changes and store solar energy is the target that people make great efforts.Photochemical catalyst just refers to that, under ultraviolet light, visible or infrared light irradiate, photochemical catalyst changes the speed of chemical reaction or initial reaction after absorbing luminous energy, and the chemical modification of the composition that induces reaction.The crisis that the exhausted and greenhouse effects of fossil energy bring effectively can be solved by the photocatalytic water technology converting solar energy into Hydrogen Energy; and photocatalytic degradation toxic organic pollutant and self-cleaning surface technology; for we provide a good living environment, therefore photocatalysis technology will become one of important means of coping with challenges.
self-discovery monocrystalline TiO
2
can photochemical catalyzing on electrode, conductor photocatalysis is subject to rapidly the common concern of various countries researcher.Conductor photocatalysis, based on band theory of solid, when semiconductor absorber energy is greater than the electronics of band gap width, due to the valence-band electrons generation band-to-band transition of semiconductor, namely transits to conduction band from valence band, the electronics (e in its valence band
-
) will be stimulated transits to conduction band, produces corresponding hole (h in valence band simultaneously
+
), define electron-hole pair.The electronics produced, hole are separated and move to particle surface under internal electric field effect.Photohole has very strong electronic capability, there is strong oxidizing property, the electronics in semiconductor grain surface adsorbed material or solvent can be captured, make the not light absorbing material of script oxidized, electron acceptor is then reduced by accepting the electronics on surface, completes light-catalyzed reaction process.Photochemical catalyst plays a key effect in light-catalyzed reaction, it can make reactive material generation chemical change after absorption light, the photochemical catalyst of excitation state can circulate and generate intermediate material with reactant effect in multiple times, and ensures after self before the reaction constant by this effect.
although photocatalysis research has carried out the several years, at present the photochemical catalyst of report still also exist that light conversion efficiency is low, poor stability and the problem such as spectral response range is narrow.Chinese patent CN201310406164 reports visible light-responded photochemical catalyst Sr
3
ce
2
ti
6
o
19
and preparation method thereof, Chinese patent CN201410501769 reports visible light-responded photochemical catalyst Bi simultaneously
2
sm
4
ti
5
o
19
and preparation method thereof.On these report bases about titanate photocatalyst, we have studied a kind of novel photochemical catalyst Cr
2
ti
5
o
13
, find that this compounds has excellent visible light responsible photocatalytic performance, and there is no report at present.
Summary of the invention
meaning of the present invention is to provide metatitanic acid chromium photochemical catalyst that a kind of preparation method is simple, photocatalytic activity good, have a extensive future and preparation method thereof.
for reaching above object, the technical solution used in the present invention is:
a novel metatitanic acid chromium catalysis material, its chemical formula is Cr
2
ti
5
o
13
.
preparation method one: adopt high temperature solid-state method, comprise the steps:
(1) to contain titanium ion Ti
4+
compound, containing chromium ion Cr
3+
compound be raw material, by general formula Cr
2
ti
5
o
13
the stoichiometric proportion of middle corresponding element takes each raw material, grinds and mixes;
(2) the mixture precalcining in air atmosphere step (1) obtained, precalcining temperature is 300 ~ 700 DEG C, and calcination time is 3 ~ 16 hours, and naturally after cooling, grinding makes it mix;
(3) calcined in air atmosphere by the mixture that step (2) obtains, calcining heat is 700 ~ 1050 DEG C, and calcination time is 4 ~ 16 hours, naturally cools, and namely obtains a kind of novel metatitanic acid chromium photocatalytic powder material after grinding evenly.
above-mentioned contains titanium ion Ti
4+
compound be titanium oxide TiO
2
; Described contains chromium ion Cr
3+
compound be chromium oxide Cr
2
o
3
, chromic nitrate Cr (NO
3
)
3
9H
2
o, chromium hydroxide Cr (OH)
3
with chromium chloride CrCl
3
6H
2
one in O.
calcining heat described in step (2) is 350 ~ 650 DEG C, and calcination time is 4 ~ 15 hours; Calcining heat described in step (3) is 750 ~ 1000 DEG C, and calcination time is 5 ~ 15 hours.
preparation method two: adopt sol-gel process, comprise the following steps:
(1) by chemical formula Cr
2
ti
5
o
13
in the stoichiometric proportion of each element, first take containing titanium ion Ti
4+
compound, add appropriate glacial acetic acid solution, add thermal agitation, until complete hydrolysis; Take containing Cr ion Cr
3+
compound, add appropriate deionized water and stirring, until dissolve completely, finally, by the mixing of two kinds of solution, stir at 70-100 DEG C and obtain uniform colloidal sol;
(2) placed in an oven by above-mentioned colloidal sol, temperature is 50 DEG C-100 DEG C, and the time is 12 hours, obtains xerogel;
(3) after naturally cooling, take out presoma, calcine in air atmosphere, calcining heat is 750 ~ 1000 DEG C, and calcination time is 3 ~ 18 hours, and naturally after cooling, namely grinding evenly obtains a kind of metatitanic acid chromium photocatalytic powder material.
above-mentioned contains titanium ion Ti
4+
compound be butyl titanate C
16
h
36
o
4
ti and tetraisopropyl titanate C
12
h
28
o
4
one in Ti; Described contains chromium ion Cri
3+
compound be chromic nitrate Cr (NO
3
)
3
9H
2
o and chromium chloride CrCl
3
6H
2
the one of O.
calcining heat described in step (3) is 800 ~ 950 DEG C, and calcination time is 4 ~ 16 hours.
compared with prior art, technical solution of the present invention advantage is:
(1) Cr prepared
2
ti
5
o
13
the photocatalytic activity of photochemical catalyst is very good, and the degradation rate of 240 minutes photocatalytic degradation methylene blues can reach 93%, can photocatalytic degradation methylene blue efficiently.
(2) Cr prepared
2
ti
5
o
13
sample thing is mutually pure, and even particle distribution.
(3) Cr is prepared
2
ti
5
o
13
the raw material sources of photochemical catalyst is very extensive and cheap, and preparation method is simple simultaneously, and energy consumption is little, and cost is low.
(4) the present invention discharges without waste gas and waste liquid, environmental friendliness, Cr
2
ti
5
o
13
photochemical catalyst is a kind of inorganic catalysis material of green safety.
Accompanying drawing explanation
the Cr of Fig. 1 obtained by the embodiment of the present invention 1
2
ti
5
o
13
the X-ray powder diffraction pattern of sample;
the Cr of Fig. 2 obtained by the embodiment of the present invention 1
2
ti
5
o
13
the diffuse reflection collection of illustrative plates of sample;
the Cr of Fig. 3 obtained by the embodiment of the present invention 1
2
ti
5
o
13
the SEM figure of sample;
the Cr of Fig. 4 obtained by the embodiment of the present invention 1
2
ti
5
o
13
sample when illumination to the degradation curve of organic dyestuff methylene blue;
the Cr of Fig. 5 obtained by the embodiment of the present invention 1
2
ti
5
o
13
the kinetic curve figure of sample degradation methylene blue;
the Cr of Fig. 6 obtained by the embodiment of the present invention 5
2
ti
5
o
13
the X-ray powder diffraction pattern of sample;
the Cr of Fig. 7 obtained by the embodiment of the present invention 5
2
ti
5
o
13
the diffuse reflection collection of illustrative plates of sample;
the Cr of Fig. 8 obtained by the embodiment of the present invention 5
2
ti
5
o
13
the SEM figure of sample;
the Cr of Fig. 9 obtained by the embodiment of the present invention 5
2
ti
5
o
13
sample when illumination to the degradation curve of organic dyestuff methylene blue;
the Cr of Figure 10 obtained by the embodiment of the present invention 5
2
ti
5
o
13
the kinetic curve figure of sample degradation methylene blue.
Detailed description of the invention
below in conjunction with drawings and Examples, technical solution of the present invention is further described.
, in order to obtain the composite oxides used in the present invention, first use solid-phase synthesis to prepare powder, namely raw material according to the metering of target constitutional chemistry than mixing, then to synthesize in air atmosphere at ambient pressure.
, in order to effectively utilize light, the size of the photochemical catalyst in the present invention is preferably in micron level, or even nano particle, and specific area is larger.With oxide powder prepared by solid-phase synthesis, its particle is comparatively large and surface area is less, but can prepare photochemical catalyst particle diameter is diminished by using chemical solution method instead.
, photocatalytic degradation methylene blue activity rating adopt self-control photocatalytic reaction device, illuminator is 500 watts of cylindrical xenon lamps, the cylindrical light catalytic reaction instrument that reactive tank uses pyrex to make, illuminator is inserted in reactive tank, and passing into condensed water cooling, during reaction, temperature is room temperature.Catalyst amount 100 milligrams, liquor capacity 250 milliliters, the concentration of methylene blue is 10 mg/litre.Catalyst is placed in reactant liquor, starts illumination after opening condensed water, gets a sample after illumination at set intervals, centrifugal, gets its supernatant, measures the absorbance of methylene blue solution with ultraviolet-visible spectrophotometer in wavelength 664-666 nanometers.According to Lambert-Beer's law, the absorbance of solution is directly proportional to concentration, therefore concentration can be replaced to calculate clearance, as the clearance of methylene blue solution by absorbance.Computing formula: degradation rate=(1-C/C
0
) × 100%=(1-A/A
0
) × 100%, wherein C
0
, C is respectively concentration before and after photocatalytic degradation, A
0
, A be respectively degraded before and after absorbance.
embodiment 1:
according to chemical formula Cr
2
ti
5
o
13
, take chromium oxide Cr respectively
2
o
3
: 1.52 grams, titanium dioxide TiO
2
: 3.994 grams, add in agate mortar appropriate acetone mixed grinding evenly after, in air atmosphere, carry out precalcining, calcine 4 hours at 350 DEG C, finally with after stove cooling, take out sample; By the raw material of precalcining that obtains again in mortar with the abundant mixed grinding of identical method evenly after, again calcine in air atmosphere, calcine 5 hours at 750 DEG C, after cooling, grinding obtains metatitanic acid chromium Cr
2
ti
5
o
13
catalyst.
see accompanying drawing 1, it is the X-ray powder diffraction pattern by sample prepared by the present embodiment technical scheme, and XRD test result shows, prepared metatitanic acid chromium Cr
2
ti
5
o
13
degree of crystallinity is better, occurs without dephasign;
see accompanying drawing 2, it is the diffuse reflection spectrum by sample prepared by the present embodiment technical scheme, and as can be seen from the figure, this sample has stronger absorption at visible wavelength range;
see accompanying drawing 3, it is the SEM(SEM by sample prepared by the present embodiment technical scheme) collection of illustrative plates, as can be seen from the figure, gained sample particle is uniformly dispersed;
see accompanying drawing 4, it is to the degradation curve of organic dyestuff methylene blue by sample prepared by the present embodiment technical scheme.As can be seen from the figure, the degradation rate of this sample photocatalytic degradation methylene blue reaches 82% in 300 minutes, and the metatitanic acid chromium Cr prepared is described
2
ti
5
o
13
material has good photocatalytic activity;
see accompanying drawing 5, it is the kinetic curve figure by sample degradation methylene blue prepared by the present embodiment technical scheme, and as can be seen from the figure, the apparent kinetics speed constant of this sample photocatalytic degradation methylene blue is 0.00676 minute
-1
.
embodiment 2:
according to chemical formula Cr
2
ti
5
o
13
, take chromic nitrate Cr (NO respectively
3
)
3
9H
2
o:1.6 gram, titanium dioxide TiO
2
: 0.799 gram, add in agate mortar appropriate acetone mixed grinding evenly after, in air atmosphere, carry out precalcining, calcine 8 hours at 450 DEG C, after stove cooling, take out sample; The raw material of precalcining is again even with the abundant mixed grinding of identical method, and again calcine in air atmosphere, calcine 8 hours at 850 DEG C, after cooling, grinding obtains metatitanic acid chromium Cr
2
ti
5
o
13
catalyst.
its main structure and morphology, diffuse reflection spectrum, SEM collection of illustrative plates, similar to embodiment 1 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
embodiment 3:
according to chemical formula Cr
2
ti
5
o
13
, take chromium hydroxide Cr (OH) respectively
3
: 1.03 grams, titanium dioxide TiO
2
: 1.997 grams, add in agate mortar appropriate acetone mixed grinding evenly after, precalcining is carried out in air atmosphere, 550 DEG C of calcinings 12 hours, after stove cooling, take out sample the raw material of precalcining is again even with the abundant mixed grinding of identical method, again calcine in air atmosphere, calcine 12 hours at 950 DEG C, cooling grinding obtains metatitanic acid chromium Cr
2
ti
5
o
13
catalyst.
its main structure and morphology, diffuse reflection spectrum, SEM collection of illustrative plates, similar to embodiment 1 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
embodiment 4:
according to chemical formula Cr
2
ti
5
o
13
, take chromium chloride CrCl respectively
3
6H
2
o:1.066 gram, titanium dioxide TiO
2
: 0.799 gram, add in agate mortar appropriate acetone mixed grinding evenly after, precalcining is carried out in air atmosphere, 650 DEG C of calcinings 15 hours, after stove cooling, take out sample the raw material of precalcining is again even with the abundant mixed grinding of identical method, again calcine in air atmosphere, calcine 15 hours at 1000 DEG C, cooling grinding obtains metatitanic acid chromium Cr
2
ti
5
o
13
catalyst.
its main structure and morphology, diffuse reflection spectrum, SEM collection of illustrative plates, similar to embodiment 1 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
embodiment 5:
according to chemical formula Cr
2
ti
5
o
13
, take chromic nitrate Cr (NO
3
)
3
9H
2
o:2.000 gram is dissolved in deionized water, takes butyl titanate C
16
h
36
o
4
ti:4.254 gram, and add appropriate glacial acetic acid, heating is stirred to complete hydrolysis, then two kinds of solution are mixed 80 DEG C of magnetic agitation a period of times until obtain colloidal sol.Obtain colloidal sol the most at last to place in baking oven, design temperature is 80 DEG C, dries and obtains xerogel after 12 hours, naturally cools, and take out presoma, calcine in air atmosphere, calcining heat is 800 DEG C, and calcination time is 4 hours, namely obtains metatitanic acid chromium Cr after cooling grinding
2
ti
5
o
13
catalyst.
see accompanying drawing 6, it is the X-ray powder diffraction pattern by sample prepared by the present embodiment technical scheme, and XRD test result shows, prepared metatitanic acid chromium Cr
2
ti
5
o
13
also be monophase materials, degree of crystallinity is very good;
see accompanying drawing 7, it is the diffuse reflection spectrum by sample prepared by the present embodiment technical scheme, and as can be seen from the figure, this sample has stronger absorption in visible wavelength range;
see accompanying drawing 8, it is the SEM(SEM by sample prepared by the present embodiment technical scheme) collection of illustrative plates, as can be seen from the figure, gained sample particle granularity is tiny and be uniformly dispersed;
see accompanying drawing 9, it is to the degradation curve of organic dyestuff methylene blue by sample prepared by the present embodiment technical scheme.As can be seen from the figure, the degradation rate of this sample photocatalytic degradation methylene blue can reach 93% in 240 minutes, and the metatitanic acid chromium Cr prepared is described
2
ti
5
o
13
material has extraordinary photocatalytic activity;
see accompanying drawing 10, it is the kinetic curve figure by sample degradation methylene blue prepared by the present embodiment technical scheme, and as can be seen from the figure, the apparent kinetics speed constant of this sample photocatalytic degradation methylene blue is 0.01165 minute
-1
.
embodiment 6:
according to chemical formula Cr
2
ti
5
o
13
, take chromium chloride CrCl
3
6H
2
o:1.332 gram is dissolved in deionized water, takes butyl titanate C
16
h
36
o
4
ti:4.254 gram, and add appropriate glacial acetic acid, heating is stirred to complete hydrolysis, then two kinds of solution are mixed 80 DEG C of magnetic agitation a period of times until obtain colloidal sol.The colloidal sol obtained the most at last is placed in baking oven, and design temperature is 80 DEG C, dries and obtains xerogel after 12 hours, naturally cools, and take out presoma, calcine in air atmosphere, calcining heat is 800 DEG C, and calcination time is 4 hours, namely obtains metatitanic acid chromium Cr after cooling grinding
2
ti
5
o
13
catalyst.
its main structure and morphology, diffuse reflection spectrum, SEM collection of illustrative plates, similar to embodiment 5 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
embodiment 7:
according to chemical formula Cr
2
ti
5
o
13
, take chromic nitrate Cr (NO
3
)
3
9H
2
o:2.00 gram is dissolved in deionized water, takes tetraisopropyl titanate C
12
h
28
o
4
ti:3.553 gram, and add appropriate glacial acetic acid, heating is stirred to complete hydrolysis, then two kinds of solution are mixed 80 DEG C of magnetic agitation a period of times until obtain colloidal sol.The colloidal sol obtained the most at last is placed in baking oven, and design temperature is 80 DEG C, dries and obtains xerogel after 12 hours, naturally cools, and take out presoma, calcine in air atmosphere, calcining heat is 800 DEG C, and calcination time is 4 hours, namely obtains metatitanic acid chromium Cr after cooling grinding
2
ti
5
o
13
catalyst.
its main structure and morphology, diffuse reflection spectrum, SEM collection of illustrative plates, similar to embodiment 5 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
embodiment 8:
according to chemical formula Cr
2
ti
5
o
13
, take chromium chloride CrCl
3
6H
2
o:1.332 gram is dissolved in deionized water, takes tetraisopropyl titanate C
12
h
28
o
4
ti:3.553 gram, and add appropriate glacial acetic acid, heating is stirred to complete hydrolysis, then two kinds of solution are mixed 80 DEG C of magnetic agitation a period of times until obtain colloidal sol.The colloidal sol obtained the most at last is placed in baking oven, and design temperature is 80 DEG C, dries and obtains xerogel after 12 hours, naturally cools, and take out presoma, calcine in air atmosphere, calcining heat is 800 DEG C, and calcination time is 4 hours, namely obtains metatitanic acid chromium Cr after cooling grinding
2
ti
5
o
13
catalyst.
its main structure and morphology, diffuse reflection spectrum, SEM collection of illustrative plates, similar to embodiment 5 with the kinetic curve of degradation of methylene blue to the degradation rate of methylene blue.
Claims (7)
1. the preparation method of novel metatitanic acid chromium catalysis material and an application, is characterized in that: its chemical formula is Cr
2ti
5o
13.
2. the preparation method of a kind of novel metatitanic acid chromium catalysis material according to claim 1, adopts high temperature solid-state method, it is characterized in that comprising the steps:
(1) to contain titanium ion Ti
4+compound, containing chromium ion Cr
3+compound be raw material, by general formula Cr
2ti
5o
13the stoichiometric proportion of middle corresponding element takes each raw material, grinds and mixes;
(2) the mixture precalcining in air atmosphere step (1) obtained, precalcining temperature is 300 ~ 700 DEG C, and calcination time is 3 ~ 16 hours, and naturally after cooling, grinding makes it mix;
(3) calcined in air atmosphere by the mixture that step (2) obtains, calcining heat is 700 ~ 1050 DEG C, and calcination time is 4 ~ 16 hours, naturally cools, and namely obtains a kind of novel metatitanic acid chromium photocatalytic powder material after grinding evenly.
3. the preparation method of a kind of novel metatitanic acid chromium catalysis material according to claim 2, is characterized in that: described contains titanium ion Ti
4+compound be titanium oxide TiO
2; Described contains chromium ion Cr
3+compound be chromium oxide Cr
2o
3, chromic nitrate Cr (NO
3)
39H
2o, chromium hydroxide Cr (OH)
3with chromium chloride CrCl
36H
2one in O.
4. the preparation method of a kind of novel metatitanic acid chromium catalysis material according to claim 2, it is characterized in that: the calcining heat described in step (2) is 350 ~ 650 DEG C, calcination time is 4 ~ 15 hours; Calcining heat described in step (3) is 750 ~ 1000 DEG C, and calcination time is 5 ~ 15 hours.
5. the preparation method of a kind of novel metatitanic acid chromium catalysis material according to claim 1, adopts sol-gel process, it is characterized in that comprising the following steps:
(1) by chemical formula Cr
2ti
5o
13in the stoichiometric proportion of each element, first take containing titanium ion Ti
4+compound, add appropriate glacial acetic acid solution, add thermal agitation, until complete hydrolysis; Take containing Cr ion Cr
3+compound, add appropriate deionized water and stirring, until dissolve completely, finally, by the mixing of two kinds of solution, stir at 70-100 DEG C and obtain uniform colloidal sol;
(2) placed in an oven by above-mentioned colloidal sol, temperature is 50 DEG C-100 DEG C, and the time is 12 hours, obtains xerogel;
(3) after naturally cooling, take out presoma, calcine in air atmosphere, calcining heat is 750 ~ 1000 DEG C, and calcination time is 3 ~ 18 hours, and naturally after cooling, namely grinding evenly obtains a kind of metatitanic acid chromium photocatalytic powder material.
6. the preparation method of a kind of novel metatitanic acid chromium catalysis material according to claim 5, is characterized in that: described contains titanium ion Ti
4+compound be butyl titanate C
16h
36o
4ti and tetraisopropyl titanate C
12h
28o
4one in Ti; Described contains chromium ion Cri
3+compound be chromic nitrate Cr (NO
3)
39H
2o and chromium chloride CrCl
36H
2the one of O.
7. the preparation method of a kind of novel metatitanic acid chromium catalysis material according to claim 5, it is characterized in that: the calcining heat described in step (3) is 800 ~ 950 DEG C, calcination time is 4 ~ 16 hours.
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|---|---|---|---|
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|---|---|---|---|
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ID=55091571
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Cited By (1)
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|---|---|---|---|---|
| CN105903463A (en) * | 2016-05-23 | 2016-08-31 | 渤海大学 | Preparation method of chromium titanate porous visible light catalytic material |
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Application publication date: 20160120 |