CN102115146A - Nano-structured cerium oxide with and application thereof - Google Patents
Nano-structured cerium oxide with and application thereof Download PDFInfo
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- CN102115146A CN102115146A CN 201110001703 CN201110001703A CN102115146A CN 102115146 A CN102115146 A CN 102115146A CN 201110001703 CN201110001703 CN 201110001703 CN 201110001703 A CN201110001703 A CN 201110001703A CN 102115146 A CN102115146 A CN 102115146A
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Abstract
The invention relates to nano-structured cerium oxide and applications thereof and belongs to the technical field of inorganic nano-materials and applications. The nano-structured cerium oxide is produced at room temperature by chemical coprecipitation process. The nano-structured cerium oxide is added to a waste liquid of Congo red dye to degrade the waste liquid of Congo red dye. The preparation of nano-structured cerium oxide doesn't need the harsh experimental conditions such as high temperature and high pressure, has a low cost and a simple process, and doesn't adopt other pollutants in the preparation process. The product of nano-structured cerium oxide has a low price and a high purity. The nano-structured cerium oxide material is used as a catalyst to degrade the waste liquid of Congo red dye at room temperature and normal pressure, so as to effectively solve the problems during the degradation of the waste liquid of Congo red dye, such as complex process of catalysts, harsh requirements for degradation conditions, poor treatment effect, high cost and secondary pollution.
Description
Technical field:
The present invention relates to a kind of nanostructure cerium oxide and application thereof, belong to inorganic nano material and applied technical field.
Background technology:
The 4f electronic configuration of rare earth element uniqueness makes it have special light, sound, electricity, magnetic property, is described as the treasure-house of novel material.CeO
2Be a kind of important cheapness and broad-spectrum rare earth oxide, after the cerium dioxide nanoization, on original basis, show more character, as small-size effect, high-ratio surface effect, quantum effect, extremely strong light, electricity, magnetic property, supraconductivity, and high chemically reactive, make its high-tech area that important use be arranged at optical material, luminescent material, magneticsubstance, battery material, electrochemistry and catalyzer.Cerium oxide (CeO
2) be a kind of important rare earth oxide, have unusual good physical and chemical performance behind its nanometer at aspects such as sound, light, magnetic, heat, catalysis and chemically reactives, and be widely used in purifying vehicle exhaust catalytic material, photocatalyst, corrosion protection coating, gas sensor, fuel cell, ion film, and polishing material aspect.In recent years, the cerium oxide of nanostructure is shown up prominently aspect dyeing water treatment.Yet, prepare CeO at present
2Also there are problems such as particle agglomeration is serious, size distribution is inhomogeneous, monodispersity is poor, unstable properties in the method (mainly containing the precipitator method, microemulsion method, thermal decomposition method, combustion synthesis method, sol-gel method, electrochemical process, hydrothermal method etc.) relatively more commonly used of nano particle, thereby has a strong impact on CeO
2The performance of material and application.Simultaneously, some preparation method also needs specific equipment, some raw materials cost height, complex process, some seriously polluted should not popularization.Therefore, find a kind of reaction conditions simple, reaction process is easy to control, reacts even, cheap and easily synthetic CeO
2The method of nanostructure is for effectively utilizing CeO
2Dye wastewater treatment using has important scientific meaning and using value.
Waste water from dyestuff COD concentration height, colourity is big and contain hazardous and noxious substances.Congo red a kind of as in the dyestuff, produce and use in the turnover rate height, waste water has tangible colourity, easily enters water body, and is as discharging without handling directly, very big to the damaging effect of environment.The effect that traditional treatment process obtains is very undesirable, therefore studies its effective treatment process and has important practical significance.At present, the method for treatment of dyeing and printing mainly contains two big classes: physico-chemical process and biological method.But these treatment processs exist complex process, degradation condition requirement harshness, treatment effect is not obvious, cost is higher, have secondary pollution problems, are difficult to realize industrialization.Exploring a kind of simple, simple to operate dyestuff catalyzer is more and more paid attention to.
Summary of the invention:
The present invention aims to provide a kind of nanostructure cerium oxide and application thereof, and catalyst process complexity, the degradation condition that solves the Congo red waste water from dyestuff of degraded requires harshness, treatment effect is not obvious, cost is higher, have secondary pollution problems.
Technical scheme of the present invention is at first to adopt chemical coprecipitation at room temperature to prepare the nanostructure cerium oxide, and is right
After the nanostructure cerium oxide is dropped in the Congo red dyeing waste water the Congo red dyeing waste water of degrading.
Concrete steps of the present invention are as follows:
1. prepare the tensio-active agent settled solution: get a certain amount of cetyl trimethylammonium bromide, promptly analytical pure CTAB is dissolved in it fully and obtains transparent settled solution CTAB solution in the 40ml deionized water; The CTAB strength of solution is 0.1-0.6mol/L;
2. prepare cerium solution: get a certain amount of analytical pure CeCl
3Or Ce (NO
3)
3Place the 100ml beaker, toward wherein adding 300 rev/mins of magnetic agitation of 50ml deionized water, be transparent settled solution until dissolving fully, the concentration of chloride soln is 0.1mol/L;
3. in cerium solution, drip CTAB solution 40ml and 300 rev/mins of magnetic agitation and obtain the CTAB and the cerium mixed salt solution of homogeneous transparent after 30 minutes; 300 rev/mins of magnetic agitation then, and the ammonia soln of the 25wt% that configures slowly is added drop-wise in the mixing solutions of CTAB and cerium salt; Beaker is sealed, continued in room temperature ageing 30min-10 days after 2 hours of 300 rev/mins of magnetic agitation;
4. after ageing finishes precipitation is filtered, removed CTAB 5 times with the distilled water centrifuge washing, at room temperature obtaining pattern more after drying is particle, rod, particle and excellent blended nanostructure cerium oxide.
The nanostructure cerium oxide that above-mentioned steps is obtained is as the application of the Congo red waste water of degrade azo dyestuff.
Used water is deionized water or distilled water among the present invention, preferred deionized water.
The invention has the advantages that:
1, preparation condition is simple, and reaction process is easy to control, and equipment requirements is low, and reaction evenly need not calcining, product cheapness and purity height.
2, degraded is carried out at normal temperatures and pressures, and operating procedure is simple, and degradation speed is fast, and condition is controlled easily, energy-efficient and low-cost.
Description of drawings:
Fig. 1 is the X-ray powder diffraction figure of the Congo red solution of degraded front and back cerium oxide nanoparticles in the example 1.
Fig. 2 is the high resolution transmission electron microscopy figure of the preceding cerium oxide nanoparticles of the Congo red solution of degraded in the example 1.
Fig. 3 is the uv-absorbing figure before and after cerium oxide nanoparticles is degraded to Congo red dye solution in the example 1.
Fig. 4 is the X-ray powder diffraction figure of the Congo red solution of degraded front and back cerium oxide nano-rod in the example 2.
Fig. 5 is the scanning electron microscope diagram of the preceding cerium oxide nano-rod of the Congo red solution of degraded in the example 2.
Fig. 6 is the uv-absorbing figure before and after cerium oxide nano-rod is degraded to Congo red dye solution in the example 2.
Fig. 7 is the Congo red solution of degraded front and back cerium oxide nano-rod+particulate X-ray powder diffraction figure in the example 3.
Fig. 8 is the preceding cerium oxide nano-rod of the Congo red solution of degraded+particulate transmission electron microscope figure in the example 3.
Fig. 9 is the uv-absorbing figure before and after cerium oxide nano-rod+particle is degraded to Congo red dye solution in the example 3.
Embodiment:
Below for adopting cerium oxide nanoparticles, nanometer rod, nano particle and nanometer rod mixture that the described preparation process of summary of the invention obtains and the example of the Congo red waste water of degrade azo dyestuff thereof, understand the present invention with further.
Embodiment 1:
The CeCl of preparation 0.1mol/L
36H
2Each 40ml of CTAB solution of O solution and 0.1mol/L after half an hour is stirred in mixing, adds 36ml NH
3H
2O stirred 2 hours, with still aging 20 minutes of the mixture that obtains.Outwell supernatant liquid, with the precipitation distilled water wash that obtains, centrifugation, dry under room temperature; Grind, obtain cerium oxide nanoparticles.
The Congo red solution of preparation 80mg/L is got 50ml and is put into reaction vessels, adds the cerium oxide nanoparticles for preparing, and stirs under natural light, and takes out 4ml solution under different time sections, the solution after centrifugation obtains degrading.
The cerium oxide nanoparticles powder of gained, the solid particulate of degraded back gained are carried out the X-ray diffraction analysis, as shown in Figure 1.The diffraction peak of cerium oxide nanoparticles is CeO
2Characteristic diffraction peak, can confirm that the product that obtains is cerium dioxide and inclusion-free.Contrast degraded rear oxidation cerium nano particle and Congo red XRD figure spectrum do not have Congo red characteristic peak in the degraded rear oxidation cerium nano particle, illustrate that water-soluble azoic dyestuff is degraded.
The TEM photo of product as shown in Figure 2, as seen from the figure, the CeO of present method preparation
2Nano Ce O for good dispersity, pattern rule
2Particle, particle diameter are the 5-10 nanometer.To before degrading and the Congo red dye solution behind the different degradation times carry out uv-absorbing and test, the result as shown in Figure 3, find out from figure, Congo red solution after the degraded significantly weakens in the increase along with degradation time of the absorption peak strength at 343nm and 496nm place, absorption peak strength is almost nil after 240 minutes, illustrates that water-soluble dyestuff is degraded.
Embodiment 2:
The CeCl of preparation 0.1mol/L
36H
2Each 40ml of CTAB solution of O solution and 0.3mol/L after half an hour is stirred in mixing, adds 36mlNH
3H
2O stirred 24 hours, with still aging 10 days of the mixture that obtains.Outwell supernatant liquid, with the precipitation distilled water wash that obtains, centrifugation, dry under room temperature; Grind, obtain cerium oxide nano-rod.
The Congo red solution of preparation 50mg/L is got 50ml and is put into reaction vessels, adds the cerium oxide nano-rod for preparing, and stirs under natural light, and takes out 4ml solution under different time sections, the solution after centrifugation obtains degrading.
The cerium oxide nano-rod powder of gained, the solid particulate of degraded back gained are carried out the X-ray diffraction analysis, as shown in Figure 4.The diffraction peak of cerium oxide nanoparticles is CeO
2Characteristic diffraction peak, can confirm that the product that obtains is cerium dioxide and inclusion-free.Contrast degraded rear oxidation cerium nano particle and Congo red XRD figure spectrum do not have Congo red characteristic peak in the degraded rear oxidation cerium nano particle, illustrate that water-soluble azoic dyestuff is degraded.
The SEM photo of product as seen from the figure, a process for preparing CeO as shown in Figure 5
2Nanometer rod, diameter are the 100-200 nanometer.
Congo red dye solution before and after the degraded is carried out the uv-absorbing test, the result as shown in Figure 6, as seen from the figure, Congo red solution after the degraded significantly weakens in the increase along with degradation time of the absorption peak strength at 343nm and 496nm place, absorption peak strength is almost nil after 180 minutes, illustrates that water-soluble dyestuff is degraded.
Embodiment 3:
The CeCl of preparation 0.1mol/L
36H
2Each 40ml of CTAB solution of O solution and 0.1mol/L after half an hour is stirred in mixing, adds 36ml NH
3H
2O stirred 24 hours, with still aging 10 days of the mixture that obtains.Outwell supernatant liquid, with the precipitation distilled water wash that obtains, centrifugation, dry under room temperature; Grind, obtain cerium oxide nanoparticles and nanometer rod mixture.
The Congo red solution of preparation 50mg/L, get 50ml and put into reaction vessels, add the cerium oxide prepare and receive nano particle and nanometer rod mix powder, under natural light, stir, and under different time sections, take out 4ml solution, the solution after centrifugation obtains degrading.
Cerium oxide nano-rod+the powder of nanometric particles of gained, the solid particulate of degraded back gained are carried out the X-ray diffraction analysis, as shown in Figure 7.The diffraction peak of cerium oxide nanoparticles is CeO
2Characteristic diffraction peak, can confirm that the product that obtains is cerium dioxide and inclusion-free.Contrast degraded rear oxidation cerium nano particle and Congo red XRD figure spectrum do not have Congo red characteristic peak in the degraded rear oxidation cerium nano particle, illustrate that water-soluble azoic dyestuff is degraded.
The TEM photo of product as shown in Figure 8, as seen from the figure, the CeO that a process for preparing
2Pattern is the mixture of nanometer rod and nano particle, good dispersity, and wherein nano particle diameter is about the 5-10 nanometer, and the nanometer rod diameter is about the 100-150 nanometer.
Congo red dye solution before and after the degraded is carried out the uv-absorbing test, the result as shown in Figure 9, as seen from the figure, Congo red solution after the degraded significantly weakens in the increase along with degradation time of the absorption peak strength at 343nm and 496nm place, absorption peak strength is almost nil after 180 minutes, illustrates that water-soluble dyestuff is degraded.
Claims (2)
1. nanostructure cerium oxide is characterized in that the nanostructure cerium oxide obtains through being prepared as follows step at ambient temperature:
1. prepare the tensio-active agent settled solution: get a certain amount of cetyl trimethylammonium bromide, promptly analytical pure CTAB is dissolved in it fully and obtains transparent settled solution CTAB solution in the 50ml deionized water; The CTAB strength of solution is 0.1-0.6mol/L;
2. prepare cerium solution: get a certain amount of analytical pure CeCl
3Or Ce (NO
3)
3Place the 100ml beaker, toward wherein adding 300 rev/mins of magnetic agitation of 50ml deionized water, be transparent settled solution until dissolving fully, the concentration of chloride soln is 0.1mol/L;
3. in cerium solution, drip CTAB solution 40ml and 300 rev/mins of magnetic agitation and obtain the CTAB and the cerium mixed salt solution of homogeneous transparent after 30 minutes; 300 rev/mins of magnetic agitation then, and the ammonia soln of the 25wt% that configures slowly is added drop-wise in the mixing solutions of CTAB and cerium salt; Beaker is sealed, continued in room temperature ageing 30min-10 days after 2 hours of 300 rev/mins of magnetic agitation;
4. after ageing finishes precipitation is filtered, removed CTAB 5 times with the distilled water centrifuge washing, obtaining pattern more after drying is particle, rod, particle and excellent blended nanostructure cerium oxide.
2. the described nanostructure cerium oxide of claim 1 is characterized in that the application of nanostructure cerium oxide as the Congo red waste water of degrade azo dyestuff.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515567A (en) * | 2011-12-14 | 2012-06-27 | 渤海大学 | Method for preparing nano CeO2 film having UV shielding property |
| CN103214015A (en) * | 2013-04-12 | 2013-07-24 | 内蒙古科技大学 | Method for regulating and controlling synthesized petaloid cerium oxide by utilizing cationic polyelectrolyte template |
| CN107335422A (en) * | 2017-06-06 | 2017-11-10 | 浙江师范大学 | A kind of preparation method of carbon functionalization cerium oxide |
| CN111302381A (en) * | 2020-03-04 | 2020-06-19 | 巢湖学院 | Magnetic cerium oxide and preparation method thereof |
| CN114149021A (en) * | 2021-12-09 | 2022-03-08 | 柯子星 | Method for preparing nano cerium from oriental beauty tea extract and application |
| CN115215499A (en) * | 2022-07-18 | 2022-10-21 | 北京师范大学 | Household multi-effect ceramic water purifier and manufacturing method thereof |
| WO2023125890A1 (en) * | 2021-12-30 | 2023-07-06 | 安集微电子科技（上海）股份有限公司 | Method for synthesizing cerium oxide, cerium oxide, and chemical mechanical polishing solution |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805007A (en) * | 2010-03-31 | 2010-08-18 | 云南大学 | Preparation method of rare earth hydroxide nanorod |
-
2011
- 2011-01-06 CN CN 201110001703 patent/CN102115146A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101805007A (en) * | 2010-03-31 | 2010-08-18 | 云南大学 | Preparation method of rare earth hydroxide nanorod |
Non-Patent Citations (1)
| Title |
|---|
| 《Journal of Alloys and Compounds》 20091216 Guofeng Wang et al. "Synthesis, characterization and photoluminescence of CeO2 nanoparticles by a facile method at room temperature" 202-207 1-2 第493卷, * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102515567A (en) * | 2011-12-14 | 2012-06-27 | 渤海大学 | Method for preparing nano CeO2 film having UV shielding property |
| CN103214015A (en) * | 2013-04-12 | 2013-07-24 | 内蒙古科技大学 | Method for regulating and controlling synthesized petaloid cerium oxide by utilizing cationic polyelectrolyte template |
| CN103214015B (en) * | 2013-04-12 | 2014-11-26 | 内蒙古科技大学 | Method for regulating and controlling synthesized petaloid cerium oxide by utilizing cationic polyelectrolyte template |
| CN107335422A (en) * | 2017-06-06 | 2017-11-10 | 浙江师范大学 | A kind of preparation method of carbon functionalization cerium oxide |
| CN107335422B (en) * | 2017-06-06 | 2020-07-31 | 浙江师范大学行知学院 | Preparation method of carbon functionalized cerium oxide |
| CN111302381A (en) * | 2020-03-04 | 2020-06-19 | 巢湖学院 | Magnetic cerium oxide and preparation method thereof |
| CN114149021A (en) * | 2021-12-09 | 2022-03-08 | 柯子星 | Method for preparing nano cerium from oriental beauty tea extract and application |
| CN114149021B (en) * | 2021-12-09 | 2024-02-06 | 柯子星 | Method for preparing nano cerium from eastern beauty tea extract and application of nano cerium |
| WO2023125890A1 (en) * | 2021-12-30 | 2023-07-06 | 安集微电子科技（上海）股份有限公司 | Method for synthesizing cerium oxide, cerium oxide, and chemical mechanical polishing solution |
| CN115215499A (en) * | 2022-07-18 | 2022-10-21 | 北京师范大学 | Household multi-effect ceramic water purifier and manufacturing method thereof |
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Application publication date: 20110706 |