CN102500354A - Beta-bismuth oxide/magnesium aluminum metal oxide photo-catalyst and preparation as well as application thereof - Google Patents
Beta-bismuth oxide/magnesium aluminum metal oxide photo-catalyst and preparation as well as application thereof Download PDFInfo
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Abstract
The invention relates to a beta-bismuth oxide/magnesium aluminum metal oxide photo-catalyst and preparation as well as application thereof. The composition of the photo-catalyst comprises tetragonal phase beta-bismuth oxide and magnesium aluminum metal oxide; the preparation method of the photo-catalyst comprises the following steps of: (1) dissolving soluble magnesium salt and soluble aluminum salt into water to obtain mixed salt solution; dissolving soluble carbonate and inorganic alkali in water to obtain mixed alkali solution; mixing the two solutions under heating; and reacting to obtain magnesium aluminum layered double hydroxide; (2) calcining the magnesium aluminum layered double hydroxide to obtain magnesium aluminum mixed metal oxide, and then placing in soluble carbonate solution to obtain reduced magnesium aluminum layered double hydroxide; and (3) mixing the reduced magnesium aluminum layered double hydroxide and bismuth nitrate pentahydrate, grinding, drying and calcining to obtain the photo-catalyst, wherein the photo-catalyst is applied to purification treatment of dye wastewater. The photo-catalyst provided by the invention has the advantages of high visible light catalytic activity, simple preparation process and production equipment, environmental friendliness and easiness in industrial production.
Description
Technical field
The invention belongs to visible light composite photo-catalyst and preparation thereof and application, particularly a kind of beta oxidation bismuth/magnalium metal oxide photocatalyst and preparation and application.
Background technology
Environmental problem is one of social key subjects that faced of mankind nowadays.Photocatalysis technology can be a chemical energy with conversion of solar energy effectively, makes pollutant generation oxidation-reduction reaction, generates innocuous substances such as carbon dioxide, water and salt, for the solution of this problem provides a desirable approach.Titanium dioxide is as the most frequently used catalyst, have nontoxic, catalytic activity is high, chemical stability good, advantage such as cheap.Yet, because the restriction of the band gap width of titanium dioxide own makes it can only absorb the ultraviolet light that only accounts for the sunshine fraction, and does not have response to accounting for the most visible light of sunshine.So in thereafter 20 years, research object mainly concentrates on the modification aspect to titanium dioxide,, realize the visible light-responded of titanium dioxide with this like transient metal doped, nonmetal doping and metal and nonmetal codope etc.Through to titania modified, although can improve its spectral response range, make it have certain visible light activity, quantum efficiency is lower, and there are many deficiencies in modification itself.Therefore, the development of new visible light catalyst becomes the focus direction of the research of photocatalysis in recent years.
Bismuth oxide is as a kind of important semi-conducting material, and energy gap is narrower, visible light absorbing, and the research to its photocatalysis performance in recent years deepens continuously.Bismuth oxide exists with four kinds of crystalline phases usually: monocline phase (α), cubic phase (β), face-centered cubic phase (γ) and body-centered cubic be (δ) mutually.The 2.85eV of band gap from the 2.58eV of cubic phase beta oxidation bismuth to monocline phase alpha-oxidation bismuth do not wait.Wherein, cubic phase beta oxidation bismuth has narrower band gap width, can effectively absorb visible light.Research in recent years shows that equally cubic phase beta oxidation bismuth possesses higher photocatalytic activity, has a extensive future.Yet pure cubic phase beta oxidation bismuth is a kind of metastable phase compound, at room temperature can not stable existence.Generally stablize cubic phase oxidation bismuth, like doped Ti, Mo, Ca, Sr, Ba, Eu and Sb etc. through mixing of metal ion.But the preparation method of the cubic phase beta oxidation bismuth of doping metals is comparatively complicated, and the efficient of photochemical catalyst is not high, thus to a great extent limit the application of bismuth oxide in photocatalysis field.
Layered double-hydroxide is called anionic clay again, is the very layered double hydroxide of similar water magnesite of a kind of structure.The basic structure formula is: [M
2+ 1-xM
3+ x(OH)
2]
X+A
M- X/mNH
2O, wherein: M
2+Be Mg
2+, Zn
2+And Fe
2+Deng divalent metal; M
3+Be Al
3+And Fe
3+Deng trivalent metal cation; A
M-Be CO
3 2-, Cl
-, NO
3 -And SO
4 2-Deng anion.Layered double-hydroxide is after roasting, and structural hydroxyl and interlayer anion are overflowed, thereby are converted into the mixing bimetallic oxide.Exist under certain humidity (or water) and the anionic condition, mixed oxide can recover the structure of stratiform, i.e. " memory " effect.Layered double-hydroxide and roasting derivative thereof all possess higher specific surface area, often are used as catalyst carrier.But up to now, about the document and the patent of bismuth oxide and layered double-hydroxide or its roasting derivative Combined Processing are not appeared in the newspapers as yet.
Summary of the invention
Technical problem to be solved by this invention provides a kind of beta oxidation bismuth/magnalium metal oxide photocatalyst and preparation and application; This photochemical catalyst has possessed higher visible light catalysis activity; Purified treatment field at waste water from dyestuff has a good application prospect; This preparation technology and production equipment are simple, and be environmentally friendly, is easy to suitability for industrialized production.
A kind of beta oxidation bismuth of the present invention/magnalium metal oxide photocatalyst; Its component comprises: cubic phase beta oxidation bismuth and magnalium mixed-metal oxides; Wherein the magnalium mixed-metal oxides is magnalium laminar double-hydroxide derived compounds after high-temperature calcination of reduction, and the mass ratio of cubic phase beta oxidation bismuth and magnalium mixed-metal oxides is 1: 3～5: 1.
The preparation method of a kind of beta oxidation bismuth of the present invention/magnalium metal oxide photocatalyst comprises:
(1) under the room temperature, 2: 1 in molar ratio～4: 1 soluble in water with solubility magnesium salts and aluminum soluble salt, gets mixing salt solution; By mole be 1: 1～1: 6 soluble carbon hydrochlorate and solubility inorganic base is soluble in water, mixed ammonium/alkali solutions; Under 70～100 ℃, said mixing salt solution is dropwise joined in the said mixed ammonium/alkali solutions, reaction 2～24h is through the dry magnalium laminar double-hydroxide that gets of washing;
(2) above-mentioned magnalium laminar double-hydroxide is obtained the magnalium mixed-metal oxides in 400～600 ℃ of calcining 2～4h; At room temperature, the magnalium mixed-metal oxides with gained places 0.1～1mol/L soluble carbon acid salt solution, magnetic agitation 12～48h, the dry magnalium laminar double-hydroxide that obtains reducing of warp washing;
(3) at room temperature with the magnalium laminar double-hydroxide and the mixing of five water bismuth nitrates of above-mentioned reduction, fully grind then, dry back promptly gets in 300～500 ℃ of calcining 2～6h.
Solubility magnesium salts in the said step (1) is magnesium nitrate or magnesium chloride, and aluminum soluble salt is aluminum nitrate or aluminium chloride.
Soluble carbon hydrochlorate in said step (1) and (2) is potash, sodium carbonate or ammonium carbonate, and the solubility inorganic base is potassium hydroxide or NaOH.
Washing in said step (1) and (2) is for using deionized water and absolute ethanol washing respectively.
The magnalium laminar double-hydroxide of reduction and the mass ratio of five water bismuth nitrates are 2: 1～1: 5 in the said step (3).
When calcining in the said step (3), heating rate is 8-30 ℃/min.
Through step (2), magnalium laminar double-hydroxide is after calcining, reduction, and layer structure is restored, and specific surface is higher, is suitable as catalyst carrier more.
Heating mode when calcining in the step (3) is for being rapidly heated, and heating rate is not less than 8 ℃/min, because there is multiple crystal formation in bismuth oxide, the too slow composite photo-catalyst of heating rate can produce dephasign, thereby influences photocatalysis performance; Heat treated temperature range is 300～500 ℃, and temperature retention time is 2～6h.
A kind of beta oxidation bismuth of the present invention/magnalium metal oxide photocatalyst is applied to the purified treatment of waste water from dyestuff.
Bismuth oxide/magnalium mixed-metal oxides visible light composite photo-catalyst is dispersed in the methylene blue solution; With the 500W xenon lamp is light source; Adopt the JZ-420 optical filter that the light below the 420nm is filtered; Behind radiation of visible light, solution is colourless by blue stain very soon, shows that composite photo-catalyst has stronger photocatalysis performance.The concentration of composite photo-catalyst in water is 0.4g/L～20g/L, but bubbling air or oxygen quicken photocatalytic process in the photocatalytic process.
Among the present invention, the effect of magnalium laminar double-hydroxide mainly contains:
(1) as the carrier of catalyst, make bismuth oxide be evenly dispersed in its surface, avoided the gathering of bismuth oxide effectively in sintering process.
(2) as the material of participating in reaction, in the process of grinding, the CO of its interlayer
3 2-And OH
-Generated certain intermediate product with the reaction of five water bismuth nitrates probably, after calcining, changed into cubic phase beta oxidation bismuth, magnalium laminar double-hydroxide is converted into the magnalium mixed-metal oxides simultaneously.
(3) ion of doping is provided, in the process of reaction, has a spot of Mg
2+And Al
3+Got in the lattice of cubic phase beta oxidation bismuth, thereby made photochemical catalyst be able to stable existence in room temperature.
Beneficial effect
(1) stable under the photochemical catalyst room temperature of the present invention, possessed higher visible light catalysis activity simultaneously, have a good application prospect in the purified treatment field of waste water from dyestuff;
(2) the present invention adopts solid phase method to prepare visible light composite catalyst, and preparation technology and production equipment are simple, and be environmentally friendly, is easy to suitability for industrialized production;
(3) utilize xenon lamp as the simulation visible light, the light source of reaction, the photochemical catalyst of preparation can be realized the efficient degradation to methylene blue in the water body, has a good application prospect in the purified treatment field of waste water from dyestuff.
Description of drawings
Fig. 1 is the sample 1# of embodiment 2 preparations and the X-ray diffractogram of control sample 0#;
Fig. 2 is the high-resolution-ration transmission electric-lens photo of the sample 1# of embodiment 2 preparations;
Fig. 3 is the ultraviolet-visible diffuse reflection spectrum of the sample 1# of embodiment 2 preparations;
Fig. 4 be the sample 2# for preparing of sample 1# and the embodiment 3 of embodiment 2 preparation and control sample 0# as photocatalyst for degrading methylene blue concentration over time.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
(1) under the room temperature, takes by weighing 38.12g magnesium chloride hexahydrate and 22.64g Aluminum Chloride Hexahydrate and add in the 131.5ml water, be stirred to dissolving fully, get mixing salt solution; Other takes by weighing 26.25g NaOH and 33.19g sodium carbonate adds in the 187.5ml water, is stirred to dissolving fully, gets mixed ammonium/alkali solutions; Mixed ammonium/alkali solutions is poured in the there-necked flask, placed oil bath pan, oil bath pan is heated to 90 ℃, mixing salt solution dropwise is added drop-wise in the mixed ammonium/alkali solutions.After dropwising, insulation 4h.Use deionized water and absolute ethanol washing 6 times and 2 times after insulation finishes respectively,, obtain magnalium laminar double-hydroxide through 90 ℃ of dry 24h.
(2) magnalium laminar double-hydroxide calcining under 500 ℃ was obtained the magnalium mixed-metal oxides in 4 hours.Take by weighing the 31.8g natrium carbonicum calcinatum and add the 300ml deionized water; Magnetic agitation is dissolved fully; The magnalium mixed-metal oxides 4.5g that gets again after the above-mentioned calcining adds in the beaker, and at room temperature magnetic agitation 24h washs product respectively 6 times and 2 times with deionized water and absolute ethyl alcohol; Through 90 ℃ of dry 24h, the magnalium laminar double-hydroxide that obtains reducing.
Under the room temperature, take by weighing the magnalium laminar double-hydroxide and the 2.08g five water bismuth nitrates of the reduction of 2.00g embodiment 1 preparation, place agate mortar, fully grind after the adding small amount of ethanol, through 70 ℃ of dry 24h.With powder 400 ℃ of calcining 4h in air, heating rate is 15 ℃/min.Resulting a kind of beta oxidation bismuth/magnalium mixed-metal oxides visible light composite photo-catalyst is designated as 1#.
Fig. 1 has provided the XRD figure spectrum of the sample 1# for preparing in the present embodiment.In order to compare, Fig. 1 gives the XRD figure spectrum of five water bismuth nitrates product (being designated as 0#) behind 400 ℃ of calcining 4h in air simultaneously.The reference standard collection of illustrative plates, the characteristic diffraction peak of the corresponding monocline alpha-oxidation of the diffraction maximum of sample 0# bismuth, and the characteristic diffraction peak of the corresponding tetragonal beta oxidation of the diffraction maximum of sample 1# bismuth.Explanation thus, the existence of magnalium laminar double-hydroxide has been played crucial effect to the formation of the cubic crystalline phase of bismuth oxide in the composite photo-catalyst.
Fig. 2 has provided the high-resolution-ration transmission electric-lens photo of the sample 1# for preparing in the present embodiment, can see bismuth oxide lattice fringe clearly among the figure, shows that bismuth oxide has good degree of crystallinity.
Fig. 3 has provided the ultraviolet-visible light diffuse reflection spectrum of the sample 1# of present embodiment preparation, can know that by figure composite catalyst has stronger absorption at visible region.
Embodiment 3
Under the room temperature, take by weighing the magnalium laminar double-hydroxide and the 3.12g five water bismuth nitrates of the reduction of 1.50g embodiment 1 preparation, place agate mortar, fully grind after the adding small amount of ethanol, through 70 ℃ of dry 24h.With powder 400 ℃ of calcining 3h in air, heating rate is 12 ℃/min.Resulting a kind of beta oxidation bismuth/magnalium mixed-metal oxides visible light composite photo-catalyst is designated as 2#.
Embodiment 4
The sample 1# of embodiment 2 preparations is used as the visible light catalyst degradation of methylene blue, is light source with the 500W xenon lamp, adopts the JZ-420 optical filter that the light below the 420nm is filtered.Take by weighing 0.2g sample 1# and add 100ml, concentration is in the methylene blue of 10mg/L, and the dark 30min that stirs makes methylene blue reach absorption/desorption balance at catalyst surface.Open light source then and carry out light-catalyzed reaction; Every separated 20min gets the 3ml reactant liquor; After centrifugation, get supernatant liquor; (model is Lambda 35, and PerkinElmer America) surveys the variation that absorbance is confirmed methylene blue concentration in the degradation process at wavelength 630nm place to utilize the ultraviolet-visible absorption spectroscopy appearance then.
The sample 2# of embodiment 3 preparations is used as the visible light catalyst degradation of methylene blue, is light source with the 500W xenon lamp, adopts the JZ-420 optical filter that the light below the 420nm is filtered.Take by weighing 0.2g sample 2# and add 100ml, concentration is in the methylene blue of 10mg/L, and the dark 30min that stirs makes methylene blue reach absorption/desorption balance at catalyst surface.Open light source then and carry out light-catalyzed reaction; Every separated 20min gets the 3ml reactant liquor; After centrifugation, get supernatant liquor; (model is Lambda 35, and PerkinElmer America) surveys the variation that absorbance is confirmed methylene blue concentration in the degradation process at wavelength 630nm place to utilize the ultraviolet-visible absorption spectroscopy appearance then.
Fig. 4 be in the present embodiment sample 1# and sample 2# as photocatalyst for degrading methylene blue concentration over time, the effect that gives control sample 0# catalytic degradation methylene blue solution simultaneously compares (experiment condition of 0# catalytic degradation methylene blue solution with present embodiment in consistent).As can be seen from the figure, composite photo-catalyst has all possessed higher visible light catalysis activity.Although the content of bismuth is higher than composite photo-catalyst far away among the control sample 0#, its catalytic activity is far away from composite photo-catalyst.
Claims (8)
1. beta oxidation bismuth/magnalium metal oxide photocatalyst; Its component comprises: cubic phase beta oxidation bismuth and magnalium mixed-metal oxides; Wherein the magnalium mixed-metal oxides is magnalium laminar double-hydroxide derived compounds after high-temperature calcination of reduction, and the mass ratio of cubic phase beta oxidation bismuth and magnalium mixed-metal oxides is 1: 3～5: 1.
2. the preparation method of beta oxidation bismuth/magnalium metal oxide photocatalyst comprises:
(1) under the room temperature, 2: 1 in molar ratio～4: 1 soluble in water with solubility magnesium salts and aluminum soluble salt, gets mixing salt solution; By mole be 1: 1～1: 6 soluble carbon hydrochlorate and solubility inorganic base is soluble in water, mixed ammonium/alkali solutions; Under 70～100 ℃, said mixing salt solution is dropwise joined in the said mixed ammonium/alkali solutions, reaction 2～24h is through the dry magnalium laminar double-hydroxide that gets of washing;
(2) above-mentioned magnalium laminar double-hydroxide is obtained the magnalium mixed-metal oxides in 400～600 ℃ of calcining 2～4h; At room temperature, the magnalium mixed-metal oxides with gained places 0.1～1mol/L soluble carbon acid salt solution, magnetic agitation 12～48h, the dry magnalium laminar double-hydroxide that obtains reducing of warp washing;
(3) at room temperature with the magnalium laminar double-hydroxide and the mixing of five water bismuth nitrates of above-mentioned reduction, fully grind then, dry back promptly gets in 300～500 ℃ of calcining 2～6h.
3. the preparation method of a kind of beta oxidation bismuth according to claim 1/magnalium metal oxide photocatalyst, it is characterized in that: the solubility magnesium salts in the said step (1) is magnesium nitrate or magnesium chloride, aluminum soluble salt is aluminum nitrate or aluminium chloride.
4. the preparation method of a kind of beta oxidation bismuth according to claim 1/magnalium metal oxide photocatalyst; It is characterized in that: the soluble carbon hydrochlorate in said step (1) and (2) is potash, sodium carbonate or ammonium carbonate, and the solubility inorganic base is potassium hydroxide or NaOH.
5. the preparation method of a kind of beta oxidation bismuth according to claim 1/magnalium metal oxide photocatalyst, it is characterized in that: the washing in said step (1) and (2) is for using deionized water and absolute ethanol washing respectively.
6. the preparation method of a kind of beta oxidation bismuth according to claim 1/magnalium metal oxide photocatalyst is characterized in that: the magnalium laminar double-hydroxide of reduction and the mass ratio of five water bismuth nitrates are 2: 1～1: 5 in the said step (3).
7. the preparation method of a kind of beta oxidation bismuth according to claim 1/magnalium metal oxide photocatalyst is characterized in that: when calcining in the said step (3), heating rate is 8-30 ℃/min.
8. beta oxidation bismuth/magnalium metal oxide photocatalyst is applied to the purified treatment of waste water from dyestuff.
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Cited By (2)
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| CN113145124A (en) * | 2021-04-15 | 2021-07-23 | 浙江工业大学 | 3D core-shell beta-bismuth oxide/cobalt aluminum hydrotalcite direct Z-type heterojunction catalyst and preparation method and application thereof |
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Cited By (4)
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| CN105664958A (en) * | 2016-01-20 | 2016-06-15 | 重庆大学 | Photocatalytic material and method for preparing same |
| CN105664958B (en) * | 2016-01-20 | 2018-04-13 | 重庆大学 | A kind of catalysis material and preparation method thereof |
| CN113145124A (en) * | 2021-04-15 | 2021-07-23 | 浙江工业大学 | 3D core-shell beta-bismuth oxide/cobalt aluminum hydrotalcite direct Z-type heterojunction catalyst and preparation method and application thereof |
| CN113145124B (en) * | 2021-04-15 | 2022-06-21 | 浙江工业大学 | 3D core-shell beta-bismuth oxide/cobalt aluminum hydrotalcite direct Z-type heterojunction catalyst and preparation method and application thereof |
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