CN104150437B - A kind of large pore material of Supporting cerium oxide nanometer rods - Google Patents
A kind of large pore material of Supporting cerium oxide nanometer rods Download PDFInfo
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- CN104150437B CN104150437B CN201410377043.1A CN201410377043A CN104150437B CN 104150437 B CN104150437 B CN 104150437B CN 201410377043 A CN201410377043 A CN 201410377043A CN 104150437 B CN104150437 B CN 104150437B
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- large pore
- pore material
- cerium oxide
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Abstract
The invention discloses a kind of large pore material of Supporting cerium oxide nanometer rods, be characterized in selecting natural large pore material to be carrier, in conjunction with conventional hydrothermal method, prepare the There-dimensional ordered macroporous materials that load has cerium oxide nano, operating procedure is simple, environmental protection.
Description
Technical field
The invention belongs to field of nanometer material technology, be specifically related to Supporting cerium oxide nanometer on There-dimensional ordered macroporous materials.
Background technology
Nano material refers to the material having at least one dimension to be in nanoscale scope or to be made up of as elementary cell them in three dimensions.Nano material has just been born just several years, with it there is the special performance in physics and chemistry aspect, and cause the interest of people, and make this field become " star " in material science.
Rare earth nano material, due to its excellent 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 in function ceramics preparation and sintering aid, 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 also on cuttlebone, do not grow CeO at present
2the research of nano particle.Current synthesis CeO
2nano material is all generally do not have carrier directly to synthesize.Such as, according to the literature, take cerium chloride as cerium source, CTAB is dispersant, Ce
3+: CTAB mol ratio is the NaOH of 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 of the present invention is gentle, simple to operate, with low cost, adopt native three dimensional Ordered Macroporous Materials as carrier, can to CeO
2nano material carries 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 There-dimensional ordered macroporous materials of Supporting cerium oxide nanometer with low cost.The present invention for solving the problems of the technologies described above taked scheme is: the There-dimensional ordered macroporous materials synthesizing a kind of novel Supporting cerium oxide nanometer, and described preparation method take cerous salt as cerium source, prepares cerium oxide nano, specifically comprise the following steps by hydro-thermal method:
Take cerium salt and precipitating reagent (mol ratio is 1:0.5 ~ 4), add a certain amount of deionized water, make cerium ion concentration be 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, adds large pore material section, 90 ~ 200 DEG C of insulation reaction 2 ~ 24h;
After reaction terminates, naturally cool to room temperature, reacted large pore material ethanol and deionized water rinsing for several times, are dried, are namely obtained the There-dimensional ordered macroporous materials of described Supporting cerium oxide nanometer rods.
Alternatively, described There-dimensional ordered macroporous materials 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, not only duct is homogeneous in order, and environmental protection, avoids the reagent contamination of chemical synthesis Porous materials;
2, reaction condition is gentle, and operating procedure is simple;
3, prepared material recovery and reuse convenient.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope (SEM) photograph that the load of the embodiment of the present invention has the There-dimensional ordered macroporous materials of cerium oxide nano-rod.
Detailed description of the invention
For making the object, technical solutions and advantages of the present invention clearly understand, 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 0.087g PEG-600 again, stir 5min, mixed liquor is transferred to 25mL to have in teflon-lined autoclave, puts into 3 ~ 4 cuttlebone sections, sealing, put into baking oven at 120 DEG C of insulation reaction 2h, naturally cool to room temperature after reaction terminates, take out cuttlebone, wash 3 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens to dry, namely obtain the There-dimensional ordered macroporous materials that load has cerium oxide nano-rod.This product ESEM (SEM) is observed, and see 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 0.1972g PVP again, stir 20h, mixed liquor is transferred to 25mL to have in teflon-lined autoclave, puts into 3 ~ 4 porcine cancellous bone sections, sealing, put into baking oven at 90 DEG C of insulation reaction 18h, naturally cool to room temperature after reaction terminates, take out porcine cancellous bone, wash 2 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens to dry, namely obtain the There-dimensional ordered macroporous materials that load has 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 0.1011g PVP again, stir 2h, mixed liquor is transferred to 25mL to have in teflon-lined autoclave, puts into 3 ~ 4 balanite sections, sealing, put into baking oven at 160 DEG C of insulation reaction 24h, naturally cool to room temperature after reaction terminates, take out balanite, wash 3 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens to dry, namely obtain the There-dimensional ordered macroporous materials that load has 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 to have in teflon-lined autoclave, puts into 3 ~ 4 cuttlebone sections, sealing, put into baking oven at 200 DEG C of insulation reaction 10h, naturally cool to room temperature after reaction terminates, take out cuttlebone, wash 3 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens to dry, namely obtain the There-dimensional ordered macroporous materials that load has cerium oxide nano-rod.
Embodiment 5
Take (2mmol, 0.8682g) Ce (NO
3)
36H
2o, 2mL 25% ammonia spirit, adds in 10mL water, after rapid stirring 10min; Add 0.4342g PEG-600 again, stir 5h, mixed liquor is transferred to 25mL to have in teflon-lined autoclave, puts into 3 ~ 4 cuttlebone sections, sealing, put into baking oven at 140 DEG C of insulation reaction 15h, naturally cool to room temperature after reaction terminates, take out cuttlebone, wash 4 times with distilled water and ethanol respectively, put into 60 DEG C of baking ovens to dry, namely obtain the There-dimensional ordered macroporous materials that load has 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 made, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (2)
1. a large pore material for Supporting cerium oxide nanometer rods, is characterized in that, the preparation method of described large pore material comprises:
Take cerium salt and precipitating reagent, mol ratio is 1:0.5 ~ 4, adds a certain amount of deionized water, makes cerium ion concentration be 0.2 ~ 3mol/L, after rapid stirring 5min ~ 30min, adds the dispersant based on cerium salt 5 ~ 40wt%, stirs 5min ~ 20h;
Above-mentioned mixed liquor is transferred in the autoclave with tetrafluoroethene liner, adds large pore material section, 90 ~ 200 insulation reaction 2 ~ 24h;
After reaction terminates, naturally cool to room temperature, reacted large pore material ethanol and deionized water rinsing for several times, are dried, are namely obtained the There-dimensional ordered macroporous materials of described Supporting cerium oxide nanometer rods;
Described three-dimensional large pore material is selected from cuttlebone, porcine cancellous bone, one or more in balanite;
Described dispersant is any one in PVP (polyvinylpyrrolidone) or PEG-600 (polyethylene glycol-600).
2. the preparation method of the large pore material of Supporting cerium oxide nanometer rods according to claim 1, is characterized in that, described cerium nanometer is club shaped structure, and is carried on There-dimensional ordered macroporous materials.
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|---|---|---|---|---|
| CN101239308A (en) * | 2008-03-18 | 2008-08-13 | 江苏工业学院 | Method for preparing attapulgite loading with nano cerium oxide |
| CN101407330A (en) * | 2008-10-30 | 2009-04-15 | 上海大学 | Method of preparing cerium oxide nano-rod |
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| JP2002523618A (en) * | 1998-08-19 | 2002-07-30 | ザ ダウ ケミカル カンパニー | Method for producing nano-sized metal oxide powder |
| US7943106B2 (en) * | 2005-03-18 | 2011-05-17 | Antaria Limited | Rare earth nanorods |
| CN102050479B (en) * | 2011-01-27 | 2012-05-23 | 山东交通学院 | Ceric oxide nanorod and preparation method thereof |
| CN102633534A (en) * | 2012-04-23 | 2012-08-15 | 清华大学 | Method for introducing rare-earth oxide nanorod into porous material |
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| CN101239308A (en) * | 2008-03-18 | 2008-08-13 | 江苏工业学院 | Method for preparing attapulgite loading with nano cerium oxide |
| CN101407330A (en) * | 2008-10-30 | 2009-04-15 | 上海大学 | Method of preparing cerium oxide nano-rod |
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