A kind of large pore material of load cerium oxide nano-rod
Technical field
The invention belongs to field of nanometer material technology, be specifically related to load cerium oxide nano on three-dimensional ordered macroporous material.
Background technology
Nano material refers in three dimensions, to have one dimension at least in nanoscale scope or the material that is made up of as elementary cell them.Nano material has just been born just several years, is had the special performance in physics and chemistry aspect, and causes people's interest, and make this field become " star " in material science with it.
Rare earth nano material, due to its good performance, just receives much concern.According to lot of documents, rare earth nano material is just being widely used in traditional industry and high-tech area, at optical glass, polishing material, fluorescence and laser material, semiconductor, optical fiber, adulterant and sintering aid in function ceramics preparation, the fields such as petroleum catalytic cracking are all widely used.Preparation CeO
2method have the precipitation method, sol-gel process, hydro-thermal method, thermal decomposition method, microemulsion method, electrochemical process etc.But CeO at present does not also grow on cuttlebone
2the research of nano particle.At present synthetic CeO
2nano material is all generally not have carrier directly synthetic.For example, according to the literature, taking cerium chloride as cerium source, CTAB is dispersant, Ce
3+: the NaOH that CTAB mol ratio is 1/2,12mol/L is precipitating reagent, and water makees solvent, and 180 DEG C of hydro-thermal 24h, obtain CeO
2nano wire.This experiment condition with surfactant control pattern is relatively strict, poor repeatability.And preparation method's gentleness of the present invention is simple to operate, with low cost, adopt natural three-dimensional ordered macroporous material as carrier, can be to CeO
2nano material is carried out recycling, has good facilitation to realizing Green Chemistry.
Summary of the invention
For the above state of the art, the technical problem to be solved in the present invention is: for existing on cuttlebone material load C eO
2the blank of nanometer, provides a kind of mild condition, and preparation process is simple, the three-dimensional ordered macroporous material of load cerium oxide nano with low cost.The present invention for solving the problems of the technologies described above taked scheme is: the three-dimensional ordered macroporous material of synthetic a kind of novel load cerium oxide nano, and described preparation method is taking cerous salt as cerium source, by hydro-thermal legal system preparing cerium oxide nanometer, specifically comprises the following steps:
Take cerium salt and precipitating reagent (mol ratio is 1:0.5~4), add a certain amount of deionized water, making cerium ion concentration is 0.2~1mol/L, after rapid stirring 5min~30min, add the dispersant of 5~40wt% (based on cerium salt), stir 5min~20h;
Above-mentioned mixed liquor is transferred in the autoclave with tetrafluoroethene liner, added large pore material section, 90~200 DEG C of insulation reaction 2~24h;
After reaction finishes, naturally cool to room temperature, ethanol and deionized water rinsing several for reacted large pore material, dry, and obtains the three-dimensional ordered macroporous material of described load cerium oxide nano-rod.
Alternatively, described three-dimensional ordered macroporous material is selected from cuttlebone, porcine cancellous bone, one or more in balanite.
Alternatively, described cerium salt is selected from least one in cerous nitrate, cerium chloride, cerous sulfate and cerous acetate.
Alternatively, described dispersant is PEG-600 (polyvinyl alcohol-600), PVP (polyvinylpyrrolidone).
Optionally, described precipitating reagent is NaOH, ammoniacal liquor, NaHCO
3, Na
2cO
3, at least one in sodium tert-butoxide.
Compared with prior art, advantage of the present invention is as follows:
1, select natural large pore material as carrier, the not only orderly homogeneous in duct, and environmental protection, avoids the reagent contamination of chemical synthesis hole material;
2, reaction condition gentleness, operating procedure is simple;
3, the recovery of prepared material and reuse convenient.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph that the load of the embodiment of the present invention has the three-dimensional ordered macroporous material of cerium oxide nano-rod.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearer, below in conjunction with specific embodiment, and with reference to accompanying drawing, the present invention is described in more detail.
Embodiment 1
Take (2mmol, 0.868g) Ce (NO
3)
36H
2o, (1mmol, 0.040g) NaOH add in 10mL water, after rapid stirring 5min; Add again 0.087g PEG-600, stir 5min, mixed liquor is transferred to 25mL and has in teflon-lined autoclave, put into 3~4 cuttlebone sections, sealing, put into baking oven at 120 DEG C of insulation reaction 2h, after reaction finishes, naturally cool to room temperature, take out cuttlebone, wash 3 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens and dry, obtaining load has the three-dimensional ordered macroporous material of cerium oxide nano-rod.This is ESEM (SEM) observation for product, and referring to Fig. 1, product is bar-shaped nanostructured.
Embodiment 2
Take (2mmol, 0.493g) CeCl
3, (8mmol, 0.769g) sodium tert-butoxide adds in 10mL water, after rapid stirring 30min; Add again 0.1972g PVP, stir 20h, mixed liquor is transferred to 25mL and has in teflon-lined autoclave, put into 3~4 porcine cancellous bone sections, sealing, put into baking oven at 90 DEG C of insulation reaction 18h, after reaction finishes, naturally cool to room temperature, take out porcine cancellous bone, wash 2 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens and dry, obtaining load has the three-dimensional ordered macroporous material of cerium oxide nano-rod.
Embodiment 3
Take (5mmol, 2.022g) Ce
2(SO
4)
38H
2o, (10mmol, 1.060g) Na
2cO
3add in 10mL water, after rapid stirring 15min; Add again 0.1011g PVP, stir 2h, mixed liquor is transferred to 25mL and has in teflon-lined autoclave, put into 3~4 balanite sections, sealing, put into baking oven at 160 DEG C of insulation reaction 24h, after reaction finishes, naturally cool to room temperature, take out balanite, wash 3 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens and dry, obtaining load has the three-dimensional ordered macroporous material of cerium oxide nano-rod.
Embodiment 4
Take (10mmol, 3.172g) cerous acetate, (10mmol, 0.840g) NaHCO
3, add in 10mL water, after rapid stirring 15min; Add 0.317g PEG-600, stir 10h, mixed liquor is transferred to 25mL and has in teflon-lined autoclave, put into 3~4 cuttlebone sections, sealing, put into baking oven at 200 DEG C of insulation reaction 10h, after reaction finishes, naturally cool to room temperature, take out cuttlebone, wash 3 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens and dry, obtaining load has the three-dimensional ordered macroporous material of cerium oxide nano-rod.
Embodiment 5
Take (2mmol, 0.8682g) Ce (NO
3)
36H
2o, 2mL 25% ammonia spirit, add in 10mL water, after rapid stirring 10min; Add again 0.4342g PEG-600, stir 5h, mixed liquor is transferred to 25mL and has in teflon-lined autoclave, put into 3~4 cuttlebone sections, sealing, put into baking oven at 140 DEG C of insulation reaction 15h, after reaction finishes, naturally cool to room temperature, take out cuttlebone, wash 4 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens and dry, obtaining load has the three-dimensional ordered macroporous material of cerium oxide nano-rod.
Those of ordinary skill in the field are to be understood that: the foregoing is only specific embodiments of the invention; be not limited to the present invention; within the spirit and principles in the present invention all, any amendment of making, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.