CN102151577B - Ag3PO4/Mg-Al LDO (Layered Double Oxide) visible light composite photo catalyst, preparation and application thereof - Google Patents

Ag3PO4/Mg-Al LDO (Layered Double Oxide) visible light composite photo catalyst, preparation and application thereof Download PDF

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CN102151577B
CN102151577B CN 201110031651 CN201110031651A CN102151577B CN 102151577 B CN102151577 B CN 102151577B CN 201110031651 CN201110031651 CN 201110031651 CN 201110031651 A CN201110031651 A CN 201110031651A CN 102151577 B CN102151577 B CN 102151577B
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ldo
visible light
catalyst
composite photo
ldh
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CN102151577A (en
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张青红
崔显炉
王宏志
李耀刚
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Donghua University
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Abstract

The invention relates to an Ag3PO4/Mg-Al LDO (Layered Double Oxide) visible light composite photo catalyst, preparation and application thereof. The photo catalyst comprises Ag3PO4 nanometer particles and magnesium-aluminum double metal oxides Mg-Al LDO with a mass ratio of 1:10 to 5:1. A preparation method comprises the following steps of: dispersing magnesium-aluminum layered double hydroxides obtained by a co-precipitation method into the solution of soluble phosphate, adding a silver nitrate solution, stirring for 4-24 hours, washing and roasting to obtain the Ag3PO4/Mg-Al LDO visible light composite photo catalyst. The photo catalyst is applied to degrading and removing of anion pollutants in dye waste water. While maintaining the characteristic of strong adsorptive property of an adsorbent, the Ag3PO4/Mg-Al LDO visible light composite photo catalyst also has higher visible light catalytic activity so as to have good application prospect in the purification and treatment field of the dye waste water; and the preparation technology and production equipment are simple, environmentally friendly, and easy for industrial production.

Description

A kind of Ag 3PO 4/ Mg-Al LDO visible light composite photo-catalyst and preparation and application thereof
Technical field
The invention belongs to the field of visible light composite photo-catalyst, particularly a kind of Ag 3PO 4/ Mg-Al LDO visible light composite photo-catalyst and preparation and application thereof.
Background technology
1972, Fujishima and Honda found with TiO 2Under ultraviolet light, has catalyzing and decomposing H as the light anode 2O produces H 2And O 2Phenomenon, indicate that multiphase photocatalysis research has begun a New Times.Over more than 30 year, photocatalysis is a relatively more popular science of research field always.But because TiO 2The restriction of band gap width own makes it can only absorb the ultraviolet light that only accounts for the sunshine fraction, and to accounting for the most visible light of sunshine without response.So in thereafter 20 years, research object mainly concentrates on TiO 2The modification aspect, such as transient metal doped, nonmetal doping and metal and nonmetal codope etc., realize TiO with this 2Visible light-responded.By to TiO 2Modification although can improve its spectral response range, makes it have certain visible light activity, and 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 in recent years photocatalysis research.
With TiO 2Compare Ag 3PO 4Energy gap is narrower, is about 2.45eV, thereby can effectively absorb visible light.Ag 3PO 4As a kind of novel visible catalyst, with present photocatalytic activity visible light catalyst preferably, such as BiVO 4, WO 3, TiO 2-xN xDeng comparing, has higher visible light catalytic efficient.[Zhiguo Yi, Jinhua Ye, Naoki Kikugawa et al., An orthophosphate semiconductor with photooxidation properties under visible-light irradiation, Nature Mater., 2010,9:559-564] still, the Ag for preparing by general chemical method 3PO 4Crystallite dimension is large, distributes wide, and specific area is low, thereby affects to a great extent the further raising of its photocatalytic activity.
Layered double-hydroxide (layered double hydroxides is called for short LDH) is called again anionic clay, 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 mBe CO 3 2-, Cl -, NO 3 -And SO 4 2-Deng anion.LDH is after roasting, and structural hydroxyl and interlayer ion are overflowed, thereby are converted into bimetal composite oxide (LDO).LDH and roasting derivative thereof all possess higher specific area, are often used as catalyst carrier.The introducing of carrier makes its catalysis material that supports have higher catalytic activity and selective, helps on the one hand the raising of catalyst heat endurance, avoid gathering and the sintering of component, thereby it is less to obtain crystal grain, the catalyst that distribution of sizes is narrower; LDH and roasting derivative thereof can be adsorbed in organic dyestuff the surface of composite catalyst on the other hand, improve to a greater degree the activity of catalyst.
But up to now, about with Ag 3PO 4Nano particle there is not yet relevant report to document and the patent that Mg-Al LDO carries out modification.
Summary of the invention
Technical problem to be solved by this invention provides a kind of Ag 3PO 4/ Mg-Al LDO visible light composite photo-catalyst and preparation and application thereof, this catalyst has kept the strong characteristics of the absorption property of adsorbent own, possessed simultaneously higher visible light catalysis activity,, have a good application prospect in the purified treatment field of waste water from dyestuff; This preparation technology and production equipment are simple, and be environmentally friendly, is easy to suitability for industrialized production.
A kind of Ag of the present invention 3PO 4/ Mg-Al LDO visible light composite photo-catalyst, its component comprises: mass ratio is 1: 10～5: 1 Ag 3PO 4Nano particle and magnalium bimetallic oxide Mg-Al LDO.
This loaded Ag 3PO 4Mg-Al LDO in, described Ag 3PO 4Nanoparticle size is 15～250nm, and magnalium bimetallic oxide thickness is 4～15nm, the specific area 40～220m of composite photo-catalyst 2/ g.
A kind of Ag of the present invention 3PO 4The preparation method of/Mg-Al LDO visible light composite photo-catalyst comprises:
(1) under the room temperature, is that 2: 1～4: 1 magnesium salts and the aluminium salt of solubility is soluble in water with mol ratio, gets mixing salt solution; With mol ratio be again: carbonate and the inorganic base of 1: 1～1: 6 solubility are soluble in water, get mixed ammonium/alkali solutions; In 0～50 ℃ mixing salt solution is dropwise added in the mixed ammonium/alkali solutions, be warming up to 70～100 ℃ of reaction 2～24h, washing, drying gets Mg-Al-CO 3LDH;
(2) under the room temperature, with above-mentioned Mg-Al-CO 3LDH adds in the soluble phosphoric acid salting liquid, stirs and forms suspension, and add again liquor argenti nitratis ophthalmicus and under room temperature, stir 4～24h, washing, drying gets Ag 3PO 4/ Mg-Al-CO 3The compound of LDH, wherein, Mg-Al-CO 3The mass ratio of LDH and soluble phosphate is 1: 5～10: 1, and the mol ratio of soluble phosphate and silver nitrate is 1: 3～3: 1;
(3) with above-mentioned Ag 3PO 4/ Mg-Al-CO 3The compound of LDH obtains Ag in 400～600 ℃ of calcining 2～4h 3PO 4/ Mg-AlLDO visible light composite photo-catalyst.
Magnesium salts in the described step (1) is magnesium nitrate or magnesium chloride, and aluminium salt is aluminum nitrate or aluminium chloride.
Carbonate in the described step (1) is potash, sodium carbonate or ammonium carbonate, and inorganic base is potassium hydroxide or NaOH.
Soluble phosphate in the described step (2) is potassium phosphate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, sodium phosphate, sodium hydrogen phosphate or sodium dihydrogen phosphate.
Washing in described step (1) and (2) is for using respectively deionized water and absolute ethanol washing.
A kind of Ag of the present invention 3PO 4/ Mg-Al LDO visible light composite photo-catalyst is applied to degraded and the removal of anionic pollutant in the waste water from dyestuff.
The present invention drops in this process of mixed ammonium/alkali solutions at mixing salt solution, and crystal nucleation and growth occur simultaneously, and feed time is longer, and particle diameter distributes wider.Adopt multitube reinforced simultaneously, shortened the time of this process, be conducive to the even distribution of crystallite dimension.Reinforced process is carried out under a lower temperature (0～50 ℃), so that crystal nucleation speed is faster, growth rate is slower, thereby so that grain size distribution is more even.Through roasting, Ag 3PO 4/ Mg-Al-CO 3Mg-Al-CO in the compound of LDH 3The structural hydroxyl of LDH and interlayer CO 3 2-Ion is overflowed, former Mg-Al-CO 3The LDH structure is destroyed gradually, is converted into composite oxides, thereby obtains Ag 3PO 4/ Mg-Al LDO.Presoma Mg-Al-CO 3The crystallite dimension of LDH and distribution have determined crystallite dimension and the distribution of Mg-Al LDO, yet with respect to presoma Mg-Al-CO 3LDH, Mg-Al LDO specific area is larger, and adsorption capacity is stronger.Through roasting, with Ag 3PO 4/ Mg-Al-CO 3LDH is converted into Ag 3PO 4/ Mg-AlLDO makes composite catalyst possess higher specific area and stronger absorption property.
With Ag 3PO 4/ Mg-Al LDO visible light composite photo-catalyst is dispersed in the azogeramine solution, take the 500W xenon lamp as light source, adopt the JZ-420 optical filter that the light below the 420nm is filtered, behind radiation of visible light, solution is very fast to be become colorless by redness, and composite powder becomes redness by black first, shows that composite photo-catalyst has stronger absorption property, slowly become black by redness again, show that the dyestuff of absorption is degraded.The concentration of composite photo-catalyst in water is 0.4g/L～20g/L, can pass into air or oxygen in the photocatalytic process and accelerate photocatalytic process.
Beneficial effect
(1) the present invention has kept the strong characteristics of the absorption property of adsorbent own, has possessed simultaneously higher visible light catalysis activity, has a good application prospect in the purified treatment field of waste water from dyestuff;
(2) this preparation technology and production equipment are simple, and be environmentally friendly, is easy to suitability for industrialized production.
Description of drawings
Fig. 1 is the Ag of embodiment 2 preparations 3PO 4The X-ray diffractogram of/Mg-Al LDO;
Fig. 2 is the Ag of embodiment 2 preparations 3PO 4/ Mg-Al LDO (Ag 3PO 4Wt%=50%) and the Ag of embodiment 3 preparation 3PO 4/ Mg-Al LDO (Ag 3PO 4Wt%=25%) UV-Vis DRS spectrum;
Fig. 3 is the Ag of embodiment 2 preparations 3PO 4/ Mg-Al LDO as photocatalyst for degrading azogeramine concentration over time;
Fig. 4 is the Ag of embodiment 2 preparations 3PO 4Infrared spectrum behind/Mg-Al LDO and the photocatalysis azogeramine thereof as a comparison, has provided the infrared spectrum of azogeramine.
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 for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications 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 limited range equally.
Embodiment 1
Under the room temperature, take by weighing 76.24g magnesium chloride hexahydrate and 45.27g Aluminum Chloride Hexahydrate and add in the 262.5ml water, be stirred to fully dissolving, get mixing salt solution.Other takes by weighing 52.5g NaOH and 66.38g sodium carbonate adds in the 375ml water, is stirred to fully dissolving, 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 50 ℃, adopt three constant voltage droppers that mixing salt solution dropwise is added drop-wise in the mixed ammonium/alkali solutions.After dropwising, oil bath pan is heated to 90 ℃, insulation 4h.Use respectively deionized water and absolute ethanol washing 6 times and 2 times after insulation finishes, through 90 ℃ of dry 24h, obtain Mg-Al-CO 3LDH.
Embodiment 2
Under the room temperature, take by weighing the 4.8g disodium hydrogen phosphate and join in the 150ml water, be stirred to fully dissolving, take by weighing again the Mg-Al-CO of 3g embodiment 1 preparation 3LDH joins in the mentioned solution, stirred suspension 10min.Take by weighing the 2.3g silver nitrate and add in the 50ml water, lucifuge joins in the above-mentioned suspension after being stirred to fully dissolving, and at room temperature lucifuge stirs 24h.After reaction finishes, with distilled water washing 6 times, through 70 ℃ of oven dry 24h.With powder 400 ℃ of calcining 4h in air, obtain Ag 3PO 4/ Mg-Al LDO (Ag 3PO 4Wt%=50%).
Fig. 1 is the Ag of the present embodiment preparation 3PO 4The X-ray diffractogram of/Mg-Al LDO, the Ag shown in the figure 3PO 4Characteristic peak is fairly obvious, simultaneously, the characteristic peak of simple substance Ag also occurred, shows Ag 3PO 4The chemical environment of Ag is with Ag in the compound of/Mg-Al LDO 3PO 4Be main, contain part simple substance Ag.And Mg-Al LDO occurs with unbodied form.Fig. 2 is the Ag of embodiment 2 preparations 3PO 4/ Mg-Al LDO (Ag 3PO 4Wt%=50%) ultraviolet-visible light diffuse reflection spectrum is seen Fig. 2, and composite catalyst all has stronger absorption at visible region.Ag 3PO 4The absorption band edge be about 530nm, composite catalyst mainly is because after 400 ℃ of calcinings in the absorption greater than the 530nm place, the Ag of part in the sample 3PO 4Be converted into simple substance Ag.
Embodiment 3
Under the room temperature, take by weighing the 1.6g disodium hydrogen phosphate and join in the 150ml water, be stirred to fully dissolving, take by weighing again the Mg-Al-CO of 3g embodiment 1 preparation 3LDH joins in the mentioned solution, stirred suspension 10min.Take by weighing the 0.77g silver nitrate and add in the 50ml water, lucifuge joins in the above-mentioned suspension after being stirred to fully dissolving, and at room temperature lucifuge stirs 24h.After reaction finishes, with distilled water washing 6 times, through 70 ℃ of oven dry 24h.With powder 400 ℃ of calcining 4h in air, obtain Ag 3PO 4/ Mg-Al LDO (Ag 3PO 4Wt%=25%).
Fig. 2 has provided the Ag of the present embodiment preparation 3PO 4/ Mg-Al LDO (Ag 3PO 4Wt%=25%) ultraviolet-visible light diffuse reflection spectrum, composite catalyst all has stronger absorption at visible region.
Embodiment 4
Ag with embodiment 2 preparations 3PO 4/ Mg-Al LDO take the 500W xenon lamp as light source, adopts the JZ-420 optical filter that the light below the 420nm is filtered as visible light catalyst degraded azogeramine.Take by weighing 0.2gAg 3PO 4/ Mg-Al LDO adds 100ml, and concentration is in the azogeramine solution of 50mg/L, and the dark 30min that stirs makes azogeramine reach absorption/desorption balance at catalyst surface.Then open light source and carry out light-catalyzed reaction, get the 3ml reactant liquor every 10min, after centrifugation, get supernatant liquor, then (model is Lambda 35 to utilize the ultraviolet-visible absorption spectroscopy instrument, Perkin Elmer, America) survey the variation that absorbance is determined azogeramine concentration in the degradation process at wavelength 505nm place.
Fig. 3 is Ag in the present embodiment 3PO 4/ Mg-Al LDO is used as visible light catalyst degraded azogeramine, as can be seen from the figure, and Ag 3PO 4/ Mg-Al LDO visible light composite photo-catalyst has kept the strong characteristics of the adsorptivity ability of adsorbent own, has possessed simultaneously higher visible light catalysis activity.
Fig. 4 has provided Ag 3PO 4/ Mg-Al LDO, and the infrared spectrum of compound behind the catalysis azogeramine, the infrared spectrum that wherein gives azogeramine compares.From figure, can see this compound behind the photocatalytic degradation azogeramine, the peak type almost with catalysis before Ag 3PO 4/ Mg-Al LDO is consistent, the characteristic peak of azogeramine do not occur, thereby the proof azogeramine is decomposed.
Embodiment 5
Under the room temperature, take by weighing 40.35g two water magnesium nitrates and 20.56g nine water aluminum nitrates and add in the 262.5ml water, be stirred to fully dissolving, get mixing salt solution.Other takes by weighing 50.06g potassium hydroxide and 20.56g potash adds in the 375ml water, is stirred to fully dissolving, 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 50 ℃, adopt three constant voltage droppers that mixing salt solution dropwise is added drop-wise in the mixed ammonium/alkali solutions.After dropwising, oil bath pan is heated to 90 ℃, insulation 4h.Use respectively deionized water and absolute ethanol washing 6 times and 2 times after insulation finishes, through 90 ℃ of dry 24h, obtain Mg-Al-CO 3LDH.
Under the room temperature, take by weighing 0.5g three water potassium phosphates and join in the 150ml water, be stirred to fully dissolving, take by weighing again the Mg-Al-CO of the above-mentioned preparation of 5g 3LDH joins in the mentioned solution, stirred suspension 10min.Take by weighing the 1.5g silver nitrate and add in the 50ml water, lucifuge joins in the above-mentioned suspension after being stirred to fully dissolving, and at room temperature lucifuge stirs 4h.After reaction finishes, with distilled water washing 6 times, through 70 ℃ of oven dry 24h.With powder 600 ℃ of calcining 2h in air, obtain Ag 3PO 4/ Mg-AlLDO.

Claims (7)

1. Ag 3PO 4/ Mg-Al LDO visible light composite photo-catalyst, its component is: mass ratio is the Ag of 1:10～5:1 3PO 4Nano particle and magnalium bimetallic oxide Mg-Al LDO; Described Ag 3PO 4Nanoparticle size is 15～250nm, and magnalium bimetallic oxide Mg-Al LDO thickness is 4～15nm, the specific area 40～220m of composite photo-catalyst 2/ g;
Described Ag 3PO 4The preparation method of/Mg-Al LDO visible light composite photo-catalyst comprises:
(1) under the room temperature, is that magnesium salts and the aluminium salt of solubility of 2:1～4:1 is soluble in water with mol ratio, gets mixing salt solution; With mol ratio be again: carbonate and the inorganic base of the solubility of 1:1～1:6 are soluble in water, get mixed ammonium/alkali solutions; In 0～50 ℃ mixing salt solution is dropwise added in the mixed ammonium/alkali solutions, be warming up to 70～100 ℃ of reaction 2～24h, through washing the dry Mg-Al-CO of getting 3LDH;
(2) under the room temperature, with above-mentioned Mg-Al-CO 3LDH adds in the soluble phosphoric acid salting liquid, stirs and forms suspension, adds liquor argenti nitratis ophthalmicus again and stir 4～24h under room temperature, through washing the dry Ag of getting 3PO 4/ Mg-Al-CO 3The compound of LDH, wherein, Mg-Al-CO 3The mass ratio of LDH and soluble phosphate is 1:5～10:1, and the mol ratio of soluble phosphate and silver nitrate is 1:3～3:1;
(3) with above-mentioned Ag 3PO 4/ Mg-Al-CO 3The compound of LDH obtains Ag in 400～600 ℃ of calcining 2～4h 3PO 4/ Mg-Al LDO visible light composite photo-catalyst.
2. Ag as claimed in claim 1 3PO 4The preparation method of/Mg-Al LDO visible light composite photo-catalyst comprises:
(1) under the room temperature, is that magnesium salts and the aluminium salt of solubility of 2:1～4:1 is soluble in water with mol ratio, gets mixing salt solution; With mol ratio be again: carbonate and the inorganic base of the solubility of 1:1～1:6 are soluble in water, get mixed ammonium/alkali solutions; In 0～50 ℃ mixing salt solution is dropwise added in the mixed ammonium/alkali solutions, be warming up to 70～100 ℃ of reaction 2～24h, through washing the dry Mg-Al-CO of getting 3LDH;
(2) under the room temperature, with above-mentioned Mg-Al-CO 3LDH adds in the soluble phosphoric acid salting liquid, stirs and forms suspension, adds liquor argenti nitratis ophthalmicus again and stir 4～24h under room temperature, through washing the dry Ag of getting 3PO 4/ Mg-Al-CO 3The compound of LDH, wherein, Mg-Al-CO 3The mass ratio of LDH and soluble phosphate is 1:5～10:1, and the mol ratio of soluble phosphate and silver nitrate is 1:3～3:1;
(3) with above-mentioned Ag 3PO 4/ Mg-Al-CO 3The compound of LDH obtains Ag in 400～600 ℃ of calcining 2～4h 3PO 4/ Mg-Al LDO visible light composite photo-catalyst.
3. a kind of Ag according to claim 2 3PO 4The preparation method of/Mg-Al LDO visible light composite photo-catalyst is characterized in that: the magnesium salts in the described step (1) is magnesium nitrate or magnesium chloride, and aluminium salt is aluminum nitrate or aluminium chloride.
4. a kind of Ag according to claim 2 3PO 4The preparation method of/Mg-Al LDO visible light composite photo-catalyst is characterized in that: the carbonate in the described step (1) is potash, sodium carbonate or ammonium carbonate, and inorganic base is potassium hydroxide or NaOH.
5. a kind of Ag according to claim 2 3PO 4The preparation method of/Mg-Al LDO visible light composite photo-catalyst is characterized in that: the soluble phosphate in the described step (2) is potassium phosphate, dipotassium hydrogen phosphate, potassium dihydrogen phosphate, sodium phosphate, sodium hydrogen phosphate or sodium dihydrogen phosphate.
6. a kind of Ag according to claim 2 3PO 4The preparation method of/Mg-Al LDO visible light composite photo-catalyst is characterized in that: the washing in described step (1) and (2) is and uses respectively deionized water and absolute ethanol washing.
7. Ag as claimed in claim 1 3PO 4/ Mg-Al LDO visible light composite photo-catalyst is applied to degraded and the removal of anionic pollutant in the waste water from dyestuff.
CN 201110031651 2011-01-28 2011-01-28 Ag3PO4/Mg-Al LDO (Layered Double Oxide) visible light composite photo catalyst, preparation and application thereof Expired - Fee Related CN102151577B (en)

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