CN103263943A - Preparation method of LaF3O3/SBA-15 and application - Google Patents
Preparation method of LaF3O3/SBA-15 and application Download PDFInfo
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- CN103263943A CN103263943A CN2013101773977A CN201310177397A CN103263943A CN 103263943 A CN103263943 A CN 103263943A CN 2013101773977 A CN2013101773977 A CN 2013101773977A CN 201310177397 A CN201310177397 A CN 201310177397A CN 103263943 A CN103263943 A CN 103263943A
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Abstract
The invention belongs to the technical field of preparation of a novel material, and in particular discloses a preparation method and an application of a meso-porous silicon SBA-15-loaded ABO3 perovskite LaFeO3 catalyst which has excellent catalytic oxidation and elimination performance to organic dyes in aqueous liquids. The preparation method comprises the following steps: first, dissolving corresponding metal nitrate and a certain amount of citric acid in a mixed liquid of ethanol and water; and then, adding a certain amount of meso-porous silicon SBA-15 and preparing the loaded perovskite catalyst by a sol-gel method. The catalyst has excellent adsorption and oxydative degradation capacities, and the degradation effect is simple in realizing condition: a hydrogen peroxide liquor is used as an oxidant at room temperature and can be recycled with substantially unchanged activity. The preparation method is simple in preparation process, low in cost, environmental-friendly and excellent in product performance, and has wide application prospect.
Description
Technical field
The present invention relates to the preparing technical field of new material, be specifically related to a kind of support type ABO
3Perovskite LaFeO
3/ SBA-15 Preparation of catalysts method and the application in catalytic oxidation elimination water body organic dyestuff thereof.
Background technology
Industrial dye waste water have toxicity big, have a very wide distribution, characteristics such as concentration height, colourity are dark, environment has been caused extremely serious pollution; Simultaneously also can directly or indirectly influence human beings'health by the enrichment of food chain.At present, the improvement of industrial wastewater has been caused environmentalist's extensive concern.
Catalysis method is a kind of effective ways of eliminating and administering industrial dye waste water.Such as: the catalytic wet hydrogen peroxide oxidation (CWHPO) that occur the eighties in 20th century, it is to add hydrogenperoxide steam generator (replacement oxygen) as oxidant in traditional catalytic wet oxidation (WCO) treatment process, improved the degradation efficiency to dyestuff greatly, and reaction temperature and pressure have been reduced, make it to react at normal temperatures and pressures, thereby reduced the cost that industrial dye waste water is handled.
According to the state of catalyst, it can be divided into homogeneous phase and heterogeneous catalysis wet oxidation.Among the former, catalyst and waste water mix fully, and the stripping phenomenon of catalyst is serious, and for the regeneration of resource, prevent secondary pollution problems, must carry out follow-up catalyst recovery and handle, make that technical difficulty strengthens, processing cost raises.Among the latter, catalyst is the solid phase, mainly contains noble metal, transition metal and rare earth metal.This class catalyst and waste water convenient separation, handling process is simple.But noble metal and rare-earth metal catalyst production process complexity are expensive, and there are problems such as active component stripping and inactivation in transition-metal catalyst under acid condition.But, this class catalyst, particularly metal oxide catalyst are because its excellent catalytic performance, advantage such as cheap, easily separated still have been subjected to paying attention to widely in actual applications.Be to seek a class catalytic activity height, the metal oxide catalyst of stable in properties and reusable edible in the topmost task in this field at present.
In recent years in the document, has ABO
3Type perovskite oxide LaFeO
3The degraded that is used for waste water from dyestuff has obtained numerous Conservation Scientist's very big concern (as: Advanced Materials Research465 (2012) 37-43), but reaction condition is generally photocatalytic degradation, and experiment condition is harsh relatively.Also having document (Journal of Nanoparticle Research12 (2010) 967-974) to report with SBA-16 is that the template preparation has LaFeO poroid, bigger serface
3Oxide is used for the photocatalytic degradation of dye rhodamine B.LaFeO in these reports
3Be to use as a kind of photochemical catalyst, required experimental facilities is had relatively high expectations, and also exists certain difficulty in actual applications.Document (Applied Catalysis B:Environmental125 (2012) 418-424) report LaCuO is also arranged recently
3As catalyst hydrogenperoxide steam generator oxidation rhodamine B, but prepared specific surface area of catalyst is little, has limited it to absorption and the oxidability of dyestuff.
Summary of the invention
At the deficiencies in the prior art, the object of the present invention is to provide the novel SBA-15 load LaFeO of a class
3(be LaFeO
3/ SBA-15) Catalysts and its preparation method and application.Transmission electron microscope (TEM) result shows the LaFeO in the catalyst
3Be highly dispersed on the SBA-15 surface, grain diameter is between 10 – 20nm, and SBA-15 can also keep original pore structure not to be destroyed.The catalyst of this support type not only can improve LaFeO
3Decentralization and utilization rate, simultaneously because the pore structure of SBA-15 has also improved the adsorption capacity to organic dyestuff.LaFeO
3And this mutual collaboration capabilities between the SBA-15 makes catalyst demonstrate the organic dyestuff of catalytic oxidation elimination efficiently performance.Further result of study shows that this catalyst can also be in wideer pH range applications, and can keep active constant through recycling at least 6 times.
The technical scheme that realization the object of the invention is taked is as follows:
A kind of LaFeO
3/ SBA-15 catalyst, the employing sol-gel process prepares and gets, and its concrete preparation process is as follows:
(1) in molar ratio for the ratio of 1:1:2.4 with lanthanum nitrate 0.01mol, ferric nitrate 0.01mol with citric acid 0.024mol joins distilled water and the absolute ethyl alcohol volume ratio is in the 30mL mixed liquor of 1:2, after treating stirring and dissolving, add 2g SBA-15, continue to stir and evenly mix, get reactant mixture.
This method does not have specific (special) requirements to SBA-15, and the used SBA-15 of the application makes by oneself according to conventional method for the inventor laboratory, and concrete preparation method sees the specific embodiment.
(2) above reactant mixture is placed 70 ° of C stirred in water bath and steaming to gel state, be placed in 100 ° of C baking ovens dry subsequently again.
(3) will dry sample takes out and to be placed on that calcined crystalline obtains target product in the Muffle furnace.The Muffle furnace temperature-rise period is as follows: the heating rate with 2 ° of C/min rises to 500 ° of C from room temperature, and behind the maintenance 4h, the heating rate with 2 ° of C/min rises to 700 ° of C again, keeps 4h again, is cooled to room temperature subsequently, takes out namely.
Compared with prior art, advantage of the present invention and beneficial effect are as follows:
The preparation method of product of the present invention is simple to operate, and load has LaFeO
3The SBA-15 of catalyst can keep original meso-hole structure, has also improved active component LaFeO simultaneously
3Degree of scatter and specific area.Catalyst LaFeO
3/ SBA-15 is oxidant with the hydrogenperoxide steam generator, as the heterogeneous Fenton reagent of a class, all have the performance that good catalytic oxidation is eliminated organic dyestuff under acid, alkali condition, and active component the stripping phenomenon can not take place.Even catalyst still can remain unchanged through six circulation back activity, has favorable actual application prospect.
Description of drawings
Fig. 1 is the LaFeO of embodiment 1 preparation
3/ SBA-15 and corresponding SBA-15 and LaFeO
3(A) little angle and (B) big angle X-ray powder diffraction pattern.
Fig. 2 is the LaFeO of embodiment 1 preparation
3(A) N of/SBA-15
2-adsorption; (B) pore size distribution curve; (C) Fe2p photoelectron spectroscopy figure; (D) transmission electron microscope picture.
Fig. 3 is the LaFeO of (A) embodiment 1 preparation
3/ SBA-15, SBA-15 and LaFeO
3Adsorption capacity to rhodamine B compares; (B) LaFeO of embodiment 1 preparation
3/ SBA-15 and corresponding LaFeO
3To low concentration rhodamine B (2 * 10
-5Mol/L) catalytic oxidation activity; (C) LaFeO of embodiment 1 preparation
3/ SBA-15 and corresponding LaFeO
3To high concentration rhodamine B (1 * 10
-3Mol/L) catalytic oxidation activity; (D) LaFeO of embodiment 1 preparation
3The low concentration rhodamine B (2 * 10 of/SBA-15
-5Mol/L) six circulation catalytic oxidation activities; (E) LaFeO of embodiment 1 preparation
3/ SBA-15 under condition of different pH in the 90min to low concentration rhodamine B (2 * 10
-5Mol/L) oxidative degradation activity; (F) LaFeO of embodiment 1 preparation
3Catalyzing oxidizing degrading activity in during the different dyes 2h of/SBA-15.
The specific embodiment
Following applicant will be described in detail preparation method of the present invention and application in conjunction with specific embodiments, understand so that those skilled in the art has further the present invention.But following examples should not be interpreted as the restriction of scope that the present invention is asked for protection by any way.
Embodiment 1: a kind of LaFeO
3The preparation method of/SBA-15, step is as follows:
(1) get 0.01mol lanthanum nitrate, 0.01mol ferric nitrate, 0.024mol citric acid, 10mL distilled water and 20mL absolute ethyl alcohol, with they be put in mix in the beaker after, add 2g SBA-15, and continue to stir.
The preparation method of the SBA-15 that relates in present embodiment and the subsequent embodiment is as follows:
Getting 5g P123 is dissolved in the mixed solvent that 75g distilled water and 150g HCl (2M) form.After vigorous stirring is dissolved fully to P123 under 35 ° of C, slowly drip the 10.5g ethyl orthosilicate after, under 35 ° of C, continue to stir 24h.100 ° of C crystallization 24h in the crystallization jar then, cooling, suction filtration get white powder, and with distilled water washing 5-6 time, cool off after 550 ° of C calcine 6h in the dry 24h of 100 ° of C, Muffle furnace again, namely.
(2) above reactant mixture is placed on the magnetic force heating stirrer, in 70 ° of C stirred in water bath and steam to gel state, be placed in 100 ° of C baking ovens dry subsequently again.
(3) dried sample is taken out and puts into the Muffle furnace calcined crystalline obtain target product.The Muffle furnace temperature-rise period is as follows: rise to 500 ° of C with 2 ° of C/min from room temperature, behind the maintenance 4h, be warming up to 700 ° of C with 2 ° of C/min, keep being down to room temperature behind the 4h again, obtain target product LaFeO
3/ SBA-15.
The instrument of product characterizes:
(1) the little angle of product and big angle X-ray powder diffraction are analyzed, and see accompanying drawing 1 (A) and (B).Small-angle diffraction test spectrogram (A) illustrates LaFeO
3/ SBA-15 catalyst has kept the meso-hole structure of carrier S BA-15; Big angle diffraction test spectrogram (B) illustrates LaFeO
3/ SBA-15 catalyst has LaFeO
3Type perovskite structure and do not have other metal oxide impurities.
(2) N
2-adsorption is seen accompanying drawing 2 (A), and the result shows that product has H1 type thermoisopleth.Calculate through BET formula, try to achieve the specific area of this mesoporous supported catalyst less than carrier S BA-15, simultaneously according to graph of pore diameter distribution accompanying drawing 2 (B), the aperture of this mesoporous supported catalyst is less than carrier S BA-15, illustrate that the active component perovskite enters into the mesopore orbit of SBA-15 or stopped up the part duct, has reduced surface area and aperture.
(3) x-ray photoelectron spectroscopy is seen accompanying drawing 2 (C), by consult the XPS databook as can be known in this supported catalyst the Fe element mainly exist with+3 valencys.
(4) transmission electron microscope picture is seen accompanying drawing 2 (D), can see clearly that from figure SBA-15 meso-hole structure and particle diameter are the LaFeO of 10-20nm
3Particle, this characterization result and XRD, N
2-adsorption is unanimity as a result, has confirmed perovskite LaFeO
3Be that high degree of dispersion is on the surface of mesoporous silicon SBA-15.
Below be the embodiment that uses, all in room temperature (20-25 ℃) operation down.
Embodiment 2:
The LaFeO that embodiment 1 makes
3The adsorption capacity of the rhodamine B of/SBA-15:
Experimentation is as follows: rhodamine B solution (2 * 10
-5Mol/L) 50mL, LaFeO
3/ SBA-15 the amount of being incorporated as 0.1g, the about 1h of magnetic agitation reaches adsorption equilibrium, after the filtration, measures the absorbance A of filtrate at the 550nm wavelength with 722E type visible spectrophotometer.If the rhodamine B solution absorbance A after the absorption reduces, the catalyst solid after the filtration will join in the new rhodamine B solution of equal-volume same concentrations again, carry out absorption again.This process repeats that the absorbance of rhodamine B no longer descends in solution, thinks that catalyst absorption is saturated.By the calibration curve of concentration-absorbance, draw absorption back rhodamine B concentration, and then obtain adsorbance.Adsorb the calculating of saturated back to the saturated extent of adsorption of rhodamine B, Fig. 3 (A).
Be check perovskite LaFeO
3To the influence of carrier S BA-15 absorption property, carry out check experiment.With LaFeO
3/ SBA-15 replaces with SBA-15 (0.1g), all the other operations and above-mentioned LaFeO
3/ SBA-15 adsorption experiment process unanimity is adsorbed saturated back and is calculated saturated extent of adsorption, with LaFeO
3The saturated extent of adsorption of/SBA-15 compares, Fig. 3 (A).LaFeO among the figure
3The adsorption capacity of/SBA-15 is slightly less than pure carrier, and this is because LaFeO
3Occupied due to the part duct among the SBA-15.The LaFeO of load not
3(it prepares except not adding the SBA-15 carrier, and all the other are with embodiment 1) do not adsorb (among Fig. 3 A as seen) substantially to RhB, can ignore.Therefore, although LaFeO
3The adsorption capacity of the RhB of/SBA-15 is littler than SBA-15, but much larger than the LaFeO of load not
3Thereby, can more efficiently the RhB oxidation be eliminated.
Embodiment 3:
In order to detect LaFeO
3The superiority of/SBA-15 has relatively contrasted not load LaFeO
3(it prepares except not adding the SBA-15 carrier, and all the other are with embodiment 1) is to the catalytic degradation situation of low concentration rhodamine B solution.LaFeO after absorption among the embodiment 2 is saturated
3/ SBA-15 catalyst joins the fresh rhodamine B solution (2 * 10 of 50mL
-5Mol/L) in, behind the magnetic agitation 30min, add 1mL hydrogenperoxide steam generator (mass fraction is 30%), take out 4mL solution every 30min, after the filtration, measure absorbance and be converted to rhodamine B concentration, draw degrading activity to time changing curve, Fig. 3 (B).The not load LaFeO of figure mean quality
3With support type LaFeO
3/ SBA-15 catalyst approaches the change curve of RhB conversion ratio with the reaction time.Yet it is pointed out that LaFeO in the support type perovskite
3Load capacity be 55%, and the RhB of carrier S BA-15 does not have the catalytic degradation ability; In addition, LaFeO
3Be adsorbed on the rhodamine B in its duct before the rhodamine B of institute's oxidation also comprises on/the SBA-15.Therefore, on the whole, support type LaFeO
3The LaFeO of 0.055g among the/SBA-15
3Has the not load LaFeO than 0.1g
3Higher to RhB catalytic degradation activity.This has not only saved active component LaFeO
3Consumption, also improved ability eliminated in the oxidation of rhodamine B.
Embodiment 4:
Although we can illustrate LaFeO from embodiment 3
3LaFeO among the/SBA-15
3High usage, but on scheming, intuitively seem not to be clearly.Thereby, for further specifying LaFeO
3The superiority of/SBA-15, we have compared not load LaFeO
3With support type LaFeO
3The catalytic degradation situation of the higher concentration rhodamine B of/SBA-15 solution.The rhodamine B solution concentration is increased to 10
-3Mol/L, the addition of catalyst (be among the embodiment 2 saturated to rhodamine B absorption after catalyst) is 0.3g, all the other operations are consistent with embodiment 3 methods.The corresponding absorbance of different time points is drawn degrading activity curve over time, Fig. 3 (C).This moment, the catalytic degradation ability of two class catalyst had tangible difference, support type LaFeO under the same terms as can be seen
3The catalytic performance of/SBA-15 is far above the LaFeO of load not
3(such as in reaction during 3h, it is about 90% that the former degrading activity can reach, and the latter is about 40%) clearly shown LaFeO
3/ SBA-15 has than load LaFeO not
3Better catalytic oxidation ability.
Embodiment 5:
For detecting LaFeO
3The service life of the rhodamine B solution degradation of/SBA-15, the catalyst behind the catalytic degradation reaction among the embodiment 3 is filtered, join again and fill 50mL rhodamine B solution (2 * 10
-5Mol/L) in the beaker, stir and carry out the catalytic degradation reaction second time, concrete operations are with embodiment 3.Carry out six circulations (containing first) reaction successively, test more different cycle-indexes catalytic degradation activity when the reaction time is 120min, Fig. 3 (D).The result shows that after six circulations, catalytic efficiency does not have obvious reduction, shows catalyst stable in properties in the degraded of water dyestuff, and long service life has the prospect of commercial Application.
Embodiment 6:
In order to detect LaFeO
3/ SBA-15 to the degraded situation of rhodamine B, carries out following control experiment under different pH environment.After adding hydrogen peroxide, regulate pH to 2.28 respectively with dilute sulfuric acid or sodium hydroxide solution, 7.3,9.29,10.46, remaining reaction condition and operation are consistent with embodiment 3 methods.Test is the catalytic degradation activity under the condition of different pH when the reaction time is 120min relatively, Fig. 3 (E).From figure as can be known, catalyst is in the activity that can both demonstrate the catalytic oxidation rhodamine B more than 90% between the pH=2-10.And the catalytic degradation reaction of traditional F enton reagent needs could realize in the solution of pH＜4, and LaFeO is described
3/ SBA-15 catalyst has enlarged the scope of application of pH when traditional F enton reagent is degraded to the water dyestuff.
Embodiment 7:
In order to check LaFeO
3The degraded situation of the variety classes dyestuff of/SBA-15 is carried out following control experiment.With reactive brilliant red x-3b (2 * 10
-5Mol/L), direct fast scarlet 4 BS (2 * 10
-5Mol/L) and methylene blue MB (2.675 * 10
-5Mol/L) substitute rhodamine B, remaining reaction condition and operation are consistent with embodiment 3 methods.Catalyst was to the degrading activity of various organic dyestuff, Fig. 3 (F) when relatively the reaction time was 120min.The result shows that catalyst all has catalytic degradation efficient preferably to above-mentioned four kinds of dyestuffs, and wherein the degradation effect to rhodamine B is best, reaches 100%, and LaFeO is described
3/ SBA-15 has the ability of good catalytic degradation organic dyestuff, and wide prospect in industrial application is arranged.
Claims (4)
1. LaFeO
3The preparation method of/SBA-15, its step is as follows:
(1) in molar ratio for the ratio of 1:1:2.4 with lanthanum nitrate 0.01mol, ferric nitrate 0.01mol with citric acid 0.024mol joins distilled water and the absolute ethyl alcohol volume ratio is in the 30mL mixed liquor of 1:2, after treating stirring and dissolving, add 2g SBA-15, continue to stir and evenly mix, get reactant mixture;
(2) above reactant mixture is placed under 70 C and to stir and steam to gel state, be placed in the 100 C baking ovens dry subsequently again;
(3) will dry sample takes out and to be placed on that calcined crystalline obtains target product in the Muffle furnace, the Muffle furnace temperature-rise period is as follows: the heating rate with 2 C/min rises to 500 C from room temperature, after keeping 4h, heating rate with 2 C/min rises to 700 C again, keep 4h again, be cooled to room temperature subsequently, take out namely.
Method according to claim 1 preparation and LaFeO
3/ SBA-15 is as catalyst application in the organic dyestuff in the catalyzing oxidizing degrading aqueous phase solution.
3. application according to claim 2 is characterized in that: described organic dyestuff is rhodamine B, reactive brilliant red, methylene blue or fast scarlet.
4. according to claim 2 or 3 described application, it is characterized in that: described organic dyestuff is rhodamine B.
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