CN102671685B - Photocatalytic basic lanthanum carbonate and preparation method and application thereof - Google Patents
Photocatalytic basic lanthanum carbonate and preparation method and application thereof Download PDFInfo
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- CN102671685B CN102671685B CN2012101838182A CN201210183818A CN102671685B CN 102671685 B CN102671685 B CN 102671685B CN 2012101838182 A CN2012101838182 A CN 2012101838182A CN 201210183818 A CN201210183818 A CN 201210183818A CN 102671685 B CN102671685 B CN 102671685B
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Abstract
The invention discloses a photocatalytic basic lanthanum carbonate (LaCO3OH) and a preparation method and application thereof. The photocatalytic basic lanthanum carbonate (LaCO3OH) prepared by the hydrothermal method is applied in photocatalytic water splitting for oxygen production and the photocatalytic degradation of organic pollutants in the environment. The basic lanthanum carbonate (LaCO3OH) is applied in the field of photocatalysis for the first time. The preparation method is simple, complex and expensive equipment is not needed, synthesis conditions are mild, and thereby the invention is easy to popularize on a large scale.
Description
Technical field
The invention belongs to the technical field of new material preparation and photocatalysis environmental pollution improvement and photocatalytic hydrogen production by water decomposition, be specifically related to photochemical catalyst basic carbonate lanthanum (LaCO
3OH) and its preparation method and application.
Technical background
Day by day serious along with energy crisis and problem of environmental pollution, how the Faced In Sustainable Development huge challenge of human society, effectively utilize solar energy and administer and pollute and tap a new source of energy that oneself causes the extensive concern of countries in the world.In recent years, Photocatalitic Technique of Semiconductor is because of the important application prospect in hydrogen energy source exploitation and environmental pollution improvement, and is subject to various fields scientific worker's extensive concern, but due to traditional TiO
2Based photocatalyst exists quantum efficiency to hang down and the shortcomings such as solar energy utilization ratio is low, restricted the practical application of photocatalysis technology, thereby the design of the develop of new and effective photochemical catalyst is utilize solar energy to curb environmental pollution and develop one of key technology of hydrogen energy source.
Summary of the invention
The object of the present invention is to provide photochemical catalyst basic carbonate lanthanum (LaCO
3OH) and its preparation method and application, its preparation method is simple, does not need equipment, the synthesis condition gentleness of complex and expensive, is conducive to large-scale promotion.
For achieving the above object, the present invention adopts following technical scheme:
Photochemical catalyst of the present invention is basic carbonate lanthanum (LaCO
3OH), be applied to photocatalysis degradation organic contaminant and photocatalytic hydrogen production by water decomposition.
The preparation method of this photochemical catalyst is hydrothermal synthesis method, and concrete steps are as follows:
The preparation of basic carbonate lanthanum: will be as the urea (CO (NH of carbon source
2)
2) or the mixture (NaOH/Na of NaOH and sodium carbonate
2CO
3) be dissolved in one or both the mixed solvent in deionized water, ethylene glycol or ethanol and make the carbon source solution that concentration is 0.1 ~ 1 mol/L; Will be as the compound solid in lanthanum source: a kind of in lanthana, lanthanum nitrate or lanthanum acetate be dissolved in one or both the mixed solvent in deionized water, ethylene glycol or ethanol and makes the lanthanum source solution that concentration is 0.01 ~ 0.1 mol/L; In the solution of lanthanum source, drip while stirring carbon source solution, continue to stir 30 ~ 180 minutes, move in autoclave 90 ~ 180 ℃ of isothermal reactions 12 ~ 24 hours, naturally cool to room temperature, precipitation respectively water and the centrifugal several of ethanol washing (to ion concentration<10ppm), 40 ~ 120 ℃ of dryings were ground in 6 ~ 24 hours, obtained the basic carbonate lanthanum powder of white, and particle diameter is 20 ~ 90 nm; Described carbon source is 1: 1～10: 1 with the ratio of the amount of substance in lanthanum source; Described stirring is magnetic agitation, and mixing speed is 400 ~ 1000 rad/min.
Remarkable advantage of the present invention is:
(1) the present invention is applied to photocatalysis field by the basic carbonate lanthanum first, is a kind of novel photolysis water hydrogen and the photochemical catalyst of degradable organic pollutant, can effectively carry out light-catalyzed reaction.
(2) preparation method of the present invention is simple, is conducive to large-scale popularization.
The accompanying drawing explanation
Fig. 1 is LaCO of the present invention
3The X-ray diffraction of OH (XRD) figure.
Fig. 2 is LaCO of the present invention
3OH is as the situation of catalyst photolysis water hydrogen.
Fig. 3 is LaCO of the present invention
3OH is as the situation of methyl orange in catalyst photocatalytic degradation water.
The specific embodiment
Photochemical catalyst of the present invention is the basic carbonate lanthanum, is applied to photolysis water hydrogen and photocatalysis degradation organic contaminant.
The preparation method of this photochemical catalyst is hydro-thermal method:
Concrete steps are as follows: will be dissolved in as the mixture of the alkali solid urea of carbon source or NaOH and sodium carbonate in one or both the mixed solvent in deionized water, ethylene glycol or ethanol and make the carbon source solution that concentration is 0.1 ~ 1 mol/L; To be dissolved in one or both the mixed solvent in deionized water, ethylene glycol or ethanol and make the lanthanum source solution that concentration is 0.01 ~ 0.1 mol/L as a kind of in compound solid lanthana, lanthanum nitrate or the lanthanum acetate in lanthanum source; In the solution of lanthanum source, drip while stirring carbon source solution, continue to stir 30 ~ 180 minutes, move in autoclave 90 ~ 180 ℃ of isothermal reactions 12 ~ 24 hours, naturally cool to room temperature, precipitation respectively water and the centrifugal several of ethanol washing (to ion concentration<10ppm), 40 ~ 120 ℃ of dryings obtained the basic carbonate lanthanum powder of white in 6 ~ 24 hours, and particle diameter is 20 ~ 90 nm; Described carbon source is 1: 1～10: 1 with the ratio of the amount of substance in lanthanum source; Described stirring is magnetic agitation, and mixing speed is 400 ~ 1000 rad/min.
Take 0.006 mol CO (NH
2)
2Solid is dissolved in 40 mL water-ol mixed solvent (V
Water: V
Ethanol=make urea liquid in 35:5); Take 0.001 mol La (NO
3)
36H
2The O solid is dissolved in 35 mL deionized waters and makes lanthanum nitrate hexahydrate, in lanthanum nitrate hexahydrate, drip while stirring the urea liquid for preparing, continue to stir 30 minutes, mixed liquor is moved in autoclave, 90 ℃ of lower constant temperature 24 hours, naturally be cooled to room temperature, by gained precipitate centrifugal, washing, 40 ℃ of constant pressure and dries ground in 24 hours, obtained white LaCO
3The OH powder.
Take 0.006 mol CO (NH
2)
2Solid is dissolved in 55 mL water-ol mixed solvent (V
Water: V
Ethanol=make urea liquid in 35:20); Take 0.001 mol La (NO
3)
36H
2The O solid is dissolved in 35 mL deionized waters and makes lanthanum nitrate hexahydrate, in lanthanum nitrate hexahydrate, drip while stirring the urea liquid for preparing, continue to stir 180 minutes, mixed liquor is moved in autoclave, 180 ℃ of lower constant temperature 12 hours, naturally be cooled to room temperature, by gained precipitate centrifugal, washing, 120 ℃ of constant pressure and dries ground in 12 hours, obtained white LaCO
3The OH powder.
Take 0.006 mol CO (NH
2)
2Solid is dissolved in 45 mL water-ol mixed solvent (V
Water: V
Ethanol=make urea liquid in 35:10); Take 0.001 mol La (NO
3)
36H
2The O solid is dissolved in 35 mL deionized waters and makes lanthanum nitrate hexahydrate, in lanthanum nitrate hexahydrate, drip while stirring the urea liquid for preparing, continue to stir 60 minutes, mixed liquor is moved in autoclave, 120 ℃ of lower constant temperature 24 hours, naturally be cooled to room temperature, by gained precipitate centrifugal, washing, 60 ℃ of constant pressure and dries ground in 24 hours, obtained white LaCO
3The OH powder.Fig. 1 has showed novel photocatalyst LaCO of the present invention
3The X-ray diffraction of OH (XRD) figure, from finding the LaCO for preparing figure
3OH is pure phase, its correspondence be the LaCO of iris phase
3OH(JCPDS:49-0981), the sample grain size is about 59.3 nm.
The reaction of photolysis water hydrogen is to carry out in the circulating system of an atmospheric pressure sealed, reactor is that a volume is the cylindrical jacketed reactor of 250 ml, middle quartz socket tube, for placing ultraviolet source, is remained reaction temperature 20 by the outer condensed water of chuck during reaction
°The C left and right.The LaCO that embodiment 1 is made
3OH powder photocatalyst hydrogen production by water decomposition, take 100 mg samples in reactor, then adds 165 mL H
2O, and even by magnetic stirrer.Before reaction, whole system first vacuumizes with mechanical pump, then is filled with high-purity Ar, repeats this process 3 times, eliminates the air in system.Argon gas be filled with complete after, add the sacrifice agent methyl alcohol of 5ml, open agitator and gas circulator, after adsorption equilibrium 30 min, turn on light.Gas-phase product in course of reaction is squeezed into six-way valve by gas circulator, by on-line chromatograph, is detected and is analyzed.The situation of photodissociation aquatic products hydrogen as shown in Figure 2, from finding out on scheming, after turning on light, there is hydrogen to produce, and along with the output of the prolongation hydrogen of light application time increases, when illumination 10 hours, its hydrogen output is about 152 μ mol, and average hydrogen-producing speed is about 15.80 μ molh
-1, greater than Detitanium-ore-type TiO
2Photocatalysis efficiency under the same conditions, i.e. hydrogen output 45 μ mol, hydrogen-producing speed 4.79 μ molh
-1.
The photocatalytic degradation reaction of organic pollutants is to carry out in homemade intermittent reaction device, reactor is by cylindric crystal reaction tube and outer equally distributed four the ultraviolet lamp tube (Philips of pipe, 4W, 254 nm) form, by magnetic agitation, remain the suspended state of photochemical catalyst in solution.The LaCO that embodiment 1 is made
3The OH powder is used as the methyl orange (MO) in photocatalyst for degrading water: at catalyst concn, be 3.3 g/L, methyl orange concentration is 10 ppm, ultraviolet light is (under λ=254nm) irradiates, pipette at regular intervals 4.0 mL reactant liquors, after centrifugation, get supernatant liquor and carry out the uv-visible absorption spectra analysis, the light absorption value of characteristic absorption peak is determined its change in concentration in degradation process per sample.The situation of photo-catalytic degradation of methyl-orange as shown in Figure 3, as can be seen from the figure, LaCO under illumination
3The degraded highly significant of OH sample to MO, after illumination 180 min, the degradation rate of MO reaches 88%, and contrast and experiment shows, and when unglazed photograph and catalyst-free existed, the concentration of MO did not all have significant change.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (6)
1. the application of a photochemical catalyst basic carbonate lanthanum is characterized in that: the chemical formula of described photochemical catalyst basic carbonate lanthanum is LaCO
3OH; Described photochemical catalyst basic carbonate lanthanum is applied to photocatalytic hydrogen production by water decomposition and Degradation of Organo-pollutants in Water with Photo-catalysis.
2. the application of photochemical catalyst basic carbonate lanthanum according to claim 1 is characterized in that: the preparation method of described photochemical catalyst basic carbonate lanthanum is the hydro-thermal one-step synthesis.
3. the application of photochemical catalyst basic carbonate lanthanum according to claim 2, it is characterized in that: described preparation method's concrete steps are as follows: will as the alkali solid of carbon source, be dissolved in solvent and make carbon source solution; To as the compound solid in lanthanum source, be dissolved in solvent and make lanthanum source solution; In the solution of lanthanum source, drip while stirring carbon source solution, continue to stir 30 ~ 180 minutes, mixed liquor is moved in autoclave to 90 ~ 180 ℃ of constant temperature 12 ~ 24 hours, gained precipitation water and ethanol centrifuge washing, to ion concentration<10ppm, 40 ~ 120 ℃ of dryings were ground in 6 ~ 24 hours, obtained the basic carbonate lanthanum powder of white.
4. the application of photochemical catalyst basic carbonate lanthanum according to claim 3, it is characterized in that: described carbon source is urea, or the mixture of NaOH and sodium carbonate; Described solvent is one or both the mixture in deionized water, ethylene glycol, ethanol; Described lanthanum source is a kind of in lanthana, lanthanum nitrate, lanthanum acetate; Described carbon source solution concentration is 0.1 ~ 1 mol/L, and lanthanum source solution concentration is 0.01 ~ 0.1 mol/L.
5. the application of photochemical catalyst basic carbonate lanthanum according to claim 3 is characterized in that: described carbon source is 1: 1～10: 1 with the ratio of the amount of substance in lanthanum source.
6. the application of photochemical catalyst basic carbonate lanthanum according to claim 3, it is characterized in that: described stirring is magnetic agitation, mixing speed is 400 ~ 1000 rad/min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10322409B1 (en) | 2018-03-05 | 2019-06-18 | King Fahd University Of Petroleum And Minerals | Low temperature hydrothermal method for the preparation of LaCO3OH nanoparticles |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103933962B (en) * | 2014-04-10 | 2016-09-28 | 重庆工商大学 | The lanthanum compound application as photocatalyst and the preparation method of lanthanum compound |
| CN104592994B (en) * | 2015-01-14 | 2018-01-02 | 惠州学院 | A kind of preparation method of the dendritic europium doping lanthanum hydroxycarbonate red fluorescence powder of triangle |
| CN105016372B (en) * | 2015-07-27 | 2017-03-01 | 陕西科技大学 | A kind of self assembly wheat head shape SmCO3(OH) preparation method of nano material |
| CN109999871B (en) * | 2019-04-15 | 2021-08-24 | 常州大学 | La2O2CO3Preparation method and application of nano triangular plate loaded Pd catalyst |
| CN110075893B (en) * | 2019-04-24 | 2022-02-11 | 莆田学院 | Photocatalyst and preparation method and application thereof |
| CN113019305B (en) * | 2021-03-03 | 2021-10-15 | 重庆三峡学院 | Preparation and application of porous lanthanum carbonate hydroxide phosphate adsorbent |
| CN113336254A (en) * | 2021-05-12 | 2021-09-03 | 中国北方稀土（集团）高科技股份有限公司 | Method for preparing hexagonal system lanthanum hydroxycarbonate by hydrothermal synthesis |
| CN114314634B (en) * | 2022-01-05 | 2023-11-10 | 合肥学院 | Basic lanthanum carbonate microsphere with three-dimensional structure and preparation method thereof |
Citations (1)
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| CN101279757A (en) * | 2008-05-22 | 2008-10-08 | 同济大学 | Method for preparing lanthanum subcarbonate nana-/micro-crystal by double hydrolysis regulation |
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| CN101279757A (en) * | 2008-05-22 | 2008-10-08 | 同济大学 | Method for preparing lanthanum subcarbonate nana-/micro-crystal by double hydrolysis regulation |
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| Jing Wang et al.A facile and green synthesis route to C@LaCO3OH core-shell microspheres using colloidal carbonaceous spheres as template and its by-products as carbon source.《Solid State Sciences》.2010,第12卷 |
| Jing Wang et al.A facile and green synthesis route to CLaCO3OH core-shell microspheres using colloidal carbonaceous spheres as template and its by-products as carbon source.《Solid State Sciences》.2010,第12卷 * |
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| Youjin Zhang et al.Synthesis, Characterization, and Photoluminescence Property of LaCO3OH Microspheres.《Inorg. Chem.》.2007,第46卷(第11期), |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US10322409B1 (en) | 2018-03-05 | 2019-06-18 | King Fahd University Of Petroleum And Minerals | Low temperature hydrothermal method for the preparation of LaCO3OH nanoparticles |
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