CN104841433A - Hematite photocatalyst with twin-crystal structure and preparation method thereof - Google Patents
Hematite photocatalyst with twin-crystal structure and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a hematite photocatalyst with a twin-crystal structure and a preparation method thereof, and belongs to the technical field of hematite photocatalysts. The method comprises the following steps: mixing polyacrylic acid and iron nitrate nonahydrate according to a mole ratio of 2:1-3:1, and then dissolving a mixture into ethyl alcohol, wherein the mass volume concentration of a solid material in a reaction system is 0.01-0.05mg/L; then stirring and reacting for 4-10h at room temperature and at the speed of 200-600rpm; then performing suction filtration on an obtained mixture solution, drying a suction filtration product at the temperature of 60-80 DEG C, sintering a dried product for 3-5h at the temperature of 400-600 DEG C in the air atmosphere, naturally cooling to the room temperature so as to obtain the final template-removed hematite photocatalyst. In the photocatalytic process, more active sites can be provided by a sample with the twin-crystal structure, and higher photocatalytic activity is obtained finally.
Description
Technical field
The invention belongs to bloodstone photocatalyst technology field, be specifically related to a kind of bloodstone photochemical catalyst with twin structure and preparation method thereof.
Background technology
Photocatalysis, due to its high efficiency, high-energy source utilization rate, has very important function and position in the fields such as the renewable sources of energy and degraded environmental contaminants.Therefore explore the photochemical catalyst of function admirable, and the degradation process realizing simulated environment pollutant has extensively and profound significance.
Many conductor oxidates, sulfide and nitride is had all to have photocatalytic activity.But the absorption edge of most of oxide, only at ultraviolet region, which has limited its use to most of solar spectrum.Although sulfide and nitride have lower band gap, the stability of these materials in aqueous medium is very poor.For overcoming these inferior positions, bloodstone becomes the semiconductor light-catalyst recently received much concern.Bloodstone (α-Fe
2o
3) be ferriferous oxide the most stable in most of aqueous environment (pH>3).The band gap narrow due to it is about 2.2eV, and the absorbent spectral region of bloodstone can reach 600nm, namely can utilize the solar spectrum energy up to 40%, and with low cost, is one of the most cheap semi-conducting material.Its photocatalytic activity may be used for H
2produce, can fuel cell be further used for.Therefore, bloodstone is widely studied as promising photochemical catalyst.But the photocatalysis performance of bloodstone is subject to the restriction of some factors, as the high and low diffusion length of recombination rate and the poorly conductive in electronics and hole, cause efficiency low.Researcher has carried out a lot of trial and has overcome these difficulties, and such as Nanostructure fabrication is to reduce the recombination rate of electronics and hole, and the suitable metal that adulterates is to strengthen electrical conductivity thus to improve charge transport capability etc.
Summary of the invention
The technical problem to be solved in the present invention is to provide bloodstone photochemical catalyst with twin structure that a kind of output is higher, catalytic efficiency is higher and preparation method thereof.
The present invention adopts polyacrylic acid template, through stirring at normal temperature and high-temperature process two steps, has prepared a kind of bloodstone photochemical catalyst with twin structure.The present invention by the regulable control to pulp furnish, and then adjusts pattern and the size of product, thus obtains the good bloodstone of photocatalysis performance; Again by adopting Ultraviolet visible absorption spectrum measuring technology to study the photocatalysis performance of bloodstone to the degraded of methyl orange.
A kind of preparation method with the bloodstone photochemical catalyst of twin structure of the present invention, it is characterized in that: be to be dissolved in ethanol after the ratio mixing of polyacrylic acid and nine water ferric nitrates 2:1 ~ 3:1 in molar ratio, in reaction system, the mass body volume concentrations of solid matter is 0.01 ~ 0.05 mg/litre; Then at room temperature, 200 ~ 600 revs/min of lower stirring reactions 4 ~ 10 hours; Afterwards by obtained mixture solution suction filtration, dry under suction filtration product 60 ~ 80 DEG C of conditions, dry product and under air atmosphere, 400 ~ 600 DEG C of conditions, sinter 3 ~ 5 hours again, after naturally cooling to room temperature, finally removed the bloodstone photochemical catalyst of template.
Prepared bloodstone photochemical catalyst is bloodstone phase, corresponding with the standard diagram of PDF card 33-0664, sees Fig. 1.And have loose structure, pattern is hole shape, as shown in Figure 2.
Photo-catalytic degradation of methyl-orange is tested:
The bloodstone photochemical catalyst 100 milligrams prepared is joined in the methyl orange solution of 150 milliliters, with the high voltage mercury lamp radiation of 500W, wherein the spectral region of high-pressure sodium lamp comprises visual field and two, ultra-violet (UV) band wave band, and the initial concentration of methyl orange solution is 10 mg/litre.Every the identical time period (20 minutes), take out the mixing material of 2 milliliters, the absorption spectrum of test methyl orange, draws the degradation rate of methyl orange eventually through the peak position Strength Changes situation calculating methyl orange characteristic peak (462nm) in absorption spectrum.Whole photocatalysis experimentation is 2 hours.
Any time, the computing formula of methyl orange degradation rate was: c=a/b*100%, and in formula, c is the methyl orange degradation rate in this moment, and a is the methyl orange characteristic peak intensity in this moment, and b is experiment initial time methyl orange characteristic peak intensity.
Wherein, sample classification is source of iron group and polyacrylic acid group.Identical point is be all prepare bloodstone by the mol ratio of change polyacrylic acid and source of iron.The excursion of the mol ratio of polyacrylic acid and nine water ferric nitrates is 3:1 ~ 2:1, and difference is that polyacrylic amount is fixed (540mg) by being prepared as of source of iron group, changes the amount of source of iron; The amount of source of iron is fixed (2018mg) by being prepared as of polyacrylic acid group, changes polyacrylic amount.
Accompanying drawing explanation
In order to the technical scheme that is illustrated more clearly in the present invention and the performance preparing material thereof, provide relevant indicators below.
Fig. 1 is the X-ray electronic diffraction collection of illustrative plates of polyacrylic acid 720;
Fig. 2 is the scanning electron microscope diagram spectrum of source of iron 2018;
Fig. 3 is in source of iron group, when polyacrylic amount is identical, to the final degradation rate figure of comparison methyl orange;
Fig. 4 is source of iron group and the contrast of polyacrylic acid group photocatalysis performance, i.e. the final degradation rate figure of source of iron 2018 and polyacrylic acid 720 pairs of methyl oranges;
Fig. 5 is source of iron 2018 (a) and polyacrylic acid 720 (b) SEAD figure.
As can be seen from the X-ray electronic diffraction collection of illustrative plates of Fig. 1, polyacrylic acid 720 is by bloodstone phase composition, and diffraction peak is corresponding with the characteristic peak of the standard diagram of PDF card 33-0664 respectively, illustrates that prepared sample crystallinity is good, is conducive to regulating and controlling other performance parameters.In photocatalytic process, can better control environment parameter, to reach best degradation effect.
Composed as can be seen from the scanning electron microscope diagram of Fig. 2, source of iron 2018 has porous pattern, pore space structure.In light-catalysed process, this structure can provide larger specific area, and then better absorbs and utilize light, is conducive to improving photocatalytic activity.
As seen from Figure 3, source of iron group is respectively source of iron 1009 (53%) for the final catalysis degradation modulus of methyl orange, source of iron 2018 (63%), source of iron 4036 (54%).Illustrate that source of iron group sample all has the ability of certain photo-catalytic degradation of methyl-orange, and the photocatalytic degradation capability of source of iron 2018 is best in source of iron group.
Can be observed by Fig. 4, polyacrylic acid 720 is 74% for the final catalysis degradation modulus of methyl orange.This numerical value is higher than source of iron 2018 (63%).Illustrate that polyacrylic acid group sample is compared with source of iron group sample, has the ability of more excellent photo-catalytic degradation of methyl-orange.
As can be seen from the SEAD collection of illustrative plates of Fig. 5, source of iron 2018 has polycrystalline electron diffraction speckle feature, and polyacrylic acid 720 has twin electronic diffraction speckle feature.The indices of crystallographic plane drawing two diffraction spots in figure corresponding are respectively (006) and (024).Two groups of angled staggered existence of Bragg's lattice, form twin structure.This twin structure may be caused by the architectural feature of hole pattern junction.And the photocatalytic degradation capability of polyacrylic acid 720 is better than source of iron 2018.Illustrate that twin structure is conducive to photo-catalytic degradation of methyl-orange, tracing sth. to its source is that the sample possessing twin structure has more binding site, and these binding sites are conducive to absorption and the utilization of light.In photocatalytic process, having twin structure sample can provide more active sites, the good photocatalytic activity of final acquisition.
Detailed description of the invention:
Below in conjunction with embodiment, the invention will be further described, but the present invention is not limited to these embodiments.Embodiment 1:
The monitoring technique of the preparation technology of bloodstone, the proportioning of mixed material and photocatalysis performance is described above, be not both by changing source of iron amount, here we select the consumption of nine water ferric nitrates to be 4036mg (photochemical catalyst prepared under representing this routine condition by source of iron 4036 afterwards).
To be dissolved in ethanol after the ratio mixing of polyacrylic acid and nine water ferric nitrates 4:3 in molar ratio, in reaction system, the mass body volume concentrations of solid matter be 0.02 mg/litre; Then at room temperature, 600 revs/min of lower stirring reactions 4 hours; Afterwards by obtained mixture solution suction filtration, suction filtration product is dried under 60 DEG C of conditions, dry product to sinter under air atmosphere, 400 DEG C of conditions, finally removed the bloodstone photochemical catalyst of template after naturally cooling to room temperature, the quality of products therefrom is about 300mg again.
The bloodstone photochemical catalyst obtained by the present embodiment 100 milligrams joins in the methyl orange solution of 150 milliliters, and with the high voltage mercury lamp radiation of 500W, the initial concentration of methyl orange solution is 10 mg/litre.Every the identical time period (20 minutes), take out the mixing material of about 2 milliliters, the absorption spectrum of test methyl orange, draws the degradation rate of methyl orange eventually through the peak position Strength Changes situation calculating methyl orange characteristic peak in absorption spectrum.Methyl orange degradation rate reaches more than 53%.
Embodiment 2
The monitoring technique of the preparation technology of bloodstone, the proportioning of mixed material and photocatalysis performance as described in Example 1, be not both by changing source of iron amount, here we select the consumption of nine water ferric nitrates to be 2018mg (photochemical catalyst prepared under representing this routine condition by source of iron 2018 afterwards).
To be dissolved in ethanol after the ratio mixing of polyacrylic acid and nine water ferric nitrates 8:3 in molar ratio, in reaction system, the mass body volume concentrations of solid matter be 0.02 mg/litre; Then at room temperature, 600 revs/min of lower stirring reactions 4 hours; Afterwards by obtained mixture solution suction filtration, suction filtration product is dried under 60 DEG C of conditions, dry product to sinter under air atmosphere, 400 DEG C of conditions, finally removed the bloodstone photochemical catalyst of template after naturally cooling to room temperature, the quality of products therefrom is about 350mg again.
The bloodstone photochemical catalyst obtained by the present embodiment 100 milligrams joins in the methyl orange solution of 150 milliliters, and with the high voltage mercury lamp radiation of 500W, the initial concentration of methyl orange solution is 10 mg/litre.Every the identical time period (20 minutes), take out the mixing material of about 2 milliliters, the absorption spectrum of test methyl orange, draws the degradation rate of methyl orange eventually through the peak position Strength Changes situation calculating methyl orange characteristic peak in absorption spectrum.Methyl orange degradation rate reaches more than 63%.
Embodiment 3
The monitoring technique of the preparation technology of iron ore, the proportioning of mixed material and photocatalysis performance as described in Example 1, be not both by changing source of iron amount, here we select the consumption of nine water ferric nitrates to be 1009mg (photochemical catalyst prepared under representing this routine condition by source of iron 1009 afterwards).
To be dissolved in ethanol after the ratio mixing of polyacrylic acid and nine water ferric nitrates 16:3 in molar ratio, in reaction system, the mass body volume concentrations of solid matter be 0.02 mg/litre; Then at room temperature, 600 revs/min of lower stirring reactions 4 hours; Afterwards by obtained mixture solution suction filtration, suction filtration product is dried under 60 DEG C of conditions, dry product to sinter under air atmosphere, 400 DEG C of conditions, finally removed the bloodstone photochemical catalyst of template after naturally cooling to room temperature, the quality of products therefrom is about 300mg again.
The bloodstone photochemical catalyst obtained by the present embodiment 100 milligrams joins in the methyl orange solution of 150 milliliters, and with the high voltage mercury lamp radiation of 500W, the initial concentration of methyl orange solution is 10 mg/litre.Every the identical time period (20 minutes), take out the mixing material of about 2 milliliters, the absorption spectrum of test methyl orange, draws the degradation rate of methyl orange eventually through the peak position Strength Changes situation calculating methyl orange characteristic peak in absorption spectrum.Methyl orange degradation rate reaches more than 54%.
Contrast (as Fig. 1) by embodiment 1,2,3, this illustrates that source of iron 4036, source of iron 1009 and polyacrylic consumption do not match, and limits the development on photocatalysis performance.And the source of iron 2018 groups that molar ratio is 8:3 is the most suitable.So in the following discussion, we all with source of iron 2018 for experimental subjects.
Embodiment 4
The monitoring technique of the preparation technology of iron ore, the proportioning of mixed material and photocatalysis performance as described in Example 1, be not both by changing polyacrylic amount, here we select polyacrylic consumption to be 1080mg (photochemical catalyst prepared under representing this routine condition with polyacrylic acid 1080 afterwards).
To be dissolved in ethanol after the ratio mixing of polyacrylic acid and nine water ferric nitrates 3:1 in molar ratio, in reaction system, the mass body volume concentrations of solid matter be 0.02 mg/litre; Then at room temperature, 600 revs/min of lower stirring reactions 4 hours; Afterwards by obtained mixture solution suction filtration, suction filtration product is dried under 60 DEG C of conditions, dry product and under air atmosphere, 400 DEG C of conditions, sinter 5 hours again, finally removed the bloodstone photochemical catalyst of template after naturally cooling to room temperature, the quality of products therefrom is about 320mg.
The bloodstone photochemical catalyst obtained by the present embodiment 100 milligrams joins in the methyl orange solution of 150 milliliters, and with the high voltage mercury lamp radiation of 500W, the initial concentration of methyl orange solution is 10 mg/litre.Every the identical time period (20 minutes), take out the mixing material of about 2 milliliters, the absorption spectrum of test methyl orange, draws the degradation rate of methyl orange eventually through the peak position Strength Changes situation calculating methyl orange characteristic peak in absorption spectrum.The final degradation rate of methyl orange can reach 70% first.
Embodiment 5
The monitoring technique of the preparation technology of iron ore, the proportioning of mixed material and photocatalysis performance as described in Example 1, be not both by changing polyacrylic amount, here we select polyacrylic consumption to be 720mg (photochemical catalyst prepared under representing this routine condition with polyacrylic acid 720 afterwards).
To be dissolved in ethanol after the ratio mixing of polyacrylic acid and nine water ferric nitrates 2:1 in molar ratio, in reaction system, the mass body volume concentrations of solid matter be 0.02 mg/litre; Then at room temperature, 200 revs/min of lower stirring reactions 10 hours; Afterwards by obtained mixture solution suction filtration, suction filtration product is dried under 80 DEG C of conditions, dry product and under air atmosphere, 600 DEG C of conditions, sinter 3 hours again, finally removed the bloodstone photochemical catalyst of template after naturally cooling to room temperature, the quality of products therefrom is about 360mg.
The bloodstone photochemical catalyst obtained by the present embodiment 100 milligrams joins in the methyl orange solution of 150 milliliters, and with the high voltage mercury lamp radiation of 500W, the initial concentration of methyl orange solution is 10 mg/litre.Every the identical time period (20 minutes), take out the mixing material of about 2 milliliters, the absorption spectrum of test methyl orange, draws the degradation rate of methyl orange eventually through the peak position Strength Changes situation calculating methyl orange characteristic peak in absorption spectrum.The final degradation rate of methyl orange can reach 74%, and as shown in Figure 2, the final degradation rate of polyacrylic acid 720 reaches the best under identical testing conditions.
Embodiment 6
As described in Example 1, difference is the monitoring technique of the preparation technology of bloodstone, the proportioning of mixed material and photocatalysis performance, utilizes SEAD to compose and tests sample.That tests the results are shown in Figure 3, the SEAD spectrum of source of iron 2018 is polycrystalline, and the SEAD spectrum of polyacrylic acid 720 forms twin, this means that polyacrylic acid 720 can provide more binding site in photocatalytic process, i.e. active site, advantageously in absorption and the utilization of light, there is facilitation to photocatalytic process.
Claims (5)
1. one kind has the preparation method of the bloodstone photochemical catalyst of twin structure, it is characterized in that: be to be dissolved in ethanol after the ratio mixing of polyacrylic acid and nine water ferric nitrates 2:1 ~ 3:1 in molar ratio, stirred at ambient temperature, then the mixture solution suction filtration will obtained, suction filtration product sinters 3 ~ 5 hours after drying again under air atmosphere, 400 ~ 600 DEG C of conditions, is finally removed the bloodstone photochemical catalyst of template after naturally cooling to room temperature.
2. a kind of preparation method with the bloodstone photochemical catalyst of twin structure as claimed in claim 1, is characterized in that: in reaction system, the mass body volume concentrations of solid matter is 0.01 ~ 0.05 mg/litre.
3. a kind of preparation method with the bloodstone photochemical catalyst of twin structure as claimed in claim 1, is characterized in that: be 200 ~ 600 revs/min of lower stirring reactions 4 ~ 10 hours.
4. a kind of preparation method with the bloodstone photochemical catalyst of twin structure as claimed in claim 1, is characterized in that: be dry under 60 ~ 80 DEG C of conditions.
5. there is a bloodstone photochemical catalyst for twin structure, it is characterized in that: be prepared by the method for Claims 1 to 4 described in any one.
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