CN107597130A - Different scale high-specific surface area cerium oxide cupric oxide composite mesopore ball and preparation method - Google Patents
Different scale high-specific surface area cerium oxide cupric oxide composite mesopore ball and preparation method Download PDFInfo
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- CN107597130A CN107597130A CN201710905713.6A CN201710905713A CN107597130A CN 107597130 A CN107597130 A CN 107597130A CN 201710905713 A CN201710905713 A CN 201710905713A CN 107597130 A CN107597130 A CN 107597130A
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- ceo
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
Abstract
The present invention relates to a kind of different scale high-ratio surface CeO to carbon monoxide with efficient cryogenic catalytic oxidation activity2/ CuO composite mesopore balls and preparation method thereof.CeO2/ CuO composite mesopore ball preparation processes include：(1) using cerous nitrate as cerium source, the ceria Mesoporous Spheres of different scale are obtained first by regulating and controlling the content of water in ethylene glycol solution；(2) it is that copper source, sodium carbonate do pH value adjusting control agent, different scale ceria Mesoporous Spheres as carrier using copper nitrate, passes through and precipitate deposition calcination method and obtain CeO2/ CuO composite mesopore balls.This method has that technique is simple, easily operated, low cost and other advantages, is especially suitable for industrial scale production and prepares.The CeO that the present invention obtains2/ CuO composite mesopore balls yardstick can in 30 150 nanometer ranges Effective Regulation, specific surface area is 100 200 meters squared per grams, have the characteristics that complete conversion temperature is low, efficient, long lifespan to catalyzing carbon monoxide oxidation, it is following that there is significant application value in catalyzing carbon monoxide oxidation, vehicle exhaust, industrial waste gas purifying etc..
Description
Technical field
The present invention relates to a kind of different scale high-specific surface area to carbon monoxide with efficient cryogenic catalytic oxidation activity
CeO2/ CuO composite mesopore balls and preparation method thereof, belong to nano composite material preparation field.
Background technology
Carbon monoxide is that one kind can be combined with human body hemoglobin, and serious health of damaging even results in the colourless of death
Odorless gas pollutant.As industrial development is continuously increased with car ownership so that coal, oil, natural gas etc.
The carbon monoxide of fossil fuel imperfect combustion release is more and more, in recent years especially winter carbon monoxide pollution and poisoning problem
Getting worse, therefore it is one of people's critical environments pollution problem urgently to be resolved hurrily to reduce carbon monoxide emission.By being catalyzed oxygen
Changing reaction makes carbon monoxide be converted to the effective ways that carbon dioxide is a kind of removal/reduction carbon monoxide emission.Ceria
Because its excellent lattice structure for storing oxygen ability, cheap price and uniqueness is widely used in high temperature catalyzing carbon monoxide
In oxidation, however, simple ceria is in cryogenic conditions（Less than 300 degree）It is difficult to carbon monoxide oxidation.Research shows, with
Copper can not only effectively improve the catalytic activity and catalysis stabilization of ceria as the cu-ce composite oxidation that co-catalyst is constructed
Property, and catalyzing carbon monoxide oxidizing reaction temperature can be reduced, improve catalyzing carbon monoxide efficiency.Therefore, closely
It is always one of people's study hotspot that over year prepared by low temperature, efficient, long-life cu-ce composite oxidation catalyst.People are using altogether
The methods of precipitation method, infusion process, precipitation-sedimentation, ion-exchange, chemical vapour deposition technique, is prepared for spherical, bar-shaped, line
The cu-ce composite oxidation of the different morphologies structure such as shape, tubulose, flower-shaped.It is known that mesoporous material has, specific surface area is big, hole
The advantages that gap rate is high, density is low, good penetrability, therefore, constructs cu-ce composite oxidation mesoporous material and is expected to further to improve
Catalyzing carbon monoxide efficiency.However, need addition poly- in cu-ce composite oxidation mesoporous material preparation process at present
It is vinylpyrrolidone, cetyl trimethylammonium bromide, alkylamine, acrylic acid, acetic acid, amino acid, block copolymer, mesoporous
Carbon, mesoporous silicon oxide, carbon containing poly sugar ball etc. make surfactant, derivant, stabilizer or template, make its prepare and after
Continuous handling process very complicated, it is clear that be unfavorable for large-scale production and application.Meanwhile using current synthesis technique same anti-
Answer and be difficult to carry out Effective Regulation to the yardstick of cu-ce composite oxidation mesoporous material in system, therefore, copper cerium combined oxidation at present
Thing mesoporous material is rarely reported to the yardstick structure-activity relationship that catalyzing carbon monoxide aoxidizes.
The content of the invention
The technical problem to be solved in the present invention is to overcome the weak point of existing cu-ce composite oxidation material preparation technology, there is provided
It is a kind of easy, quick, without preparing different scale high-specific surface area CeO under conditions of stabilizer and derivant2/ CuO composite mesopores
The method of ball.It is another object of the present invention to prepare to catalyzing carbon monoxide oxidation with low temperature, efficient, long-life superiority
The CeO of energy2/ CuO composite mesopore balls, it is catalyzing carbon monoxide oxidation, vehicle exhaust, industrial waste gas purifying etc. practical application
Material base is provided.
CeO in the present invention2/ CuO composite mesopore balls are using cerous nitrate as cerium source, are not adding any surfactant, are luring
Lead the method under conditions of agent or stabilizer using solvent heat in aqueous ethylene glycol solution and obtain different scale ceria and receive
It is that copper source, sodium carbonate do pH value adjusting control agent, different scale cerium dioxide nano ball as carrier using copper nitrate on the basis of rice ball,
Obtained by precipitation-deposition-calcination method, its preparation process includes step in detail below：
(1) prepared by ceria Mesoporous Spheres carrier：After a certain amount of cerous nitrate stirring and dissolving to aqueous ethylene glycol solution, place
Reacted 0.5 to 6 hour in 180 degree oil bath, after room temperature is naturally cooled to, centrifuged with supercentrifuge, use deionization
After water or alcohol washes 3-5 times, ceria Mesoporous Spheres powder is obtained in 300-500 degree calcining 2-6 hours, wherein in ethylene glycol
The content of water is 1 %-7 %, and the concentration of cerous nitrate is 0.01-0.20 mol/Ls；
(2) the ceria Mesoporous Spheres powder that 0.1-0.3 grams of step (1) obtains is distributed in 10-30 ml deionized waters,
It is uniformly mixing to obtain ceria Mesoporous Spheres colloidal solution；
(3) under agitation, 5-30 milliliters concentration is slowly added dropwise to step for the copper nitrate solution of 0.01 mol/L
Suddenly in the ceria Mesoporous Spheres colloidal solution that prepared by (2), adjusted in adding procedure using the sodium carbonate liquor of 0.5 mol/L
PH value, the pH value for remaining solution are 8.5-9.5, and solution colour is gradually changed into brown-green from yellow, after 1-5 hours, are being turned
After fast 8000-14000 revs/min of centrifugation 10-30 minute, colorless supernatant liquid in centrifuge tube is removed, obtains brown-green precipitated product；
(4) the brown-green precipitated product for being obtained step (3) with deionized water or alcohol is cleaned by ultrasonic 3-5 times, then 100
Spend and 2-3 hours are dried in baking oven, 2-6 hours are calcined at 400 degree after being fully ground, obtain CeO2/ CuO composite mesopore ball powders.
Beneficial effects of the present invention：
(1) the invention provides it is a kind of easy, quick, without preparing different scale Gao Bibiao under conditions of stabilizer and derivant
Area CeO2The method of/CuO composite mesopore balls；
(2) CeO that the present invention obtains2/ CuO composite mesopore balls yardstick can in 30-150 nanometer ranges Effective Regulation, compare surface
Product is 100-200 meters squared per grams, and has the characteristics that yield is high, monodispersity is good, stability is good；
(3) CeO that the present invention obtains2/ CuO composite mesopores ball has complete conversion temperature low, high catalyzing carbon monoxide oxidation
The excellent properties such as effect, long-life；
(4) by testing different scale CeO2/ CuO composite mesopores ball obtains it to one to catalyzing carbon monoxide oxidation susceptibility
The yardstick structure-activity relationship of carbonoxide catalysis oxidation；
(5) present invention need not add any surfactant, derivant or stabilizer, prepare the conventional equipment that need to only commonly use, because
This, is adapted to magnanimity, low cost, large-scale production, be content with very little following commercial applications demand.
Brief description of the drawings
Fig. 1 is the ceria Mesoporous Spheres powder and CeO obtained after centrifugal drying2/ CuO composite mesopore ball powders are with the naked eye observed
The optical photograph shot afterwards with digital camera, wherein, Fig. 1 a are the optical photographs of ceria Mesoporous Spheres powder, and its color is light
Yellow, Fig. 1 b are the CeO obtained2/ CuO composite mesopore ball powder photos, color is brown-green, is illustrated in cerium oxide particles
CuO particles are loaded.
Fig. 2 is the ceria Mesoporous Spheres and CeO to acquisition2/ CuO composite mesopores ball is seen with JEOL-1400 transmission electron microscopes
One of multiple transmission electron microscope (TEM) photos shot after examining, wherein, Fig. 2 a are the TEM image of ceria Mesoporous Spheres, and Fig. 2 b are
CeO2The TEM image of/CuO composite mesopore balls, TEM results show that product is 60 nanometers of monodisperse mesoporous ball, and CuO is born
Particle scale is unchanged after load, and its reason is that CuO particle scale is small and load capacity is few, and all scales are 20 nanometers in figure.
Fig. 3 is by obtained CeO2After/CuO composite mesopore balls are evenly spread on slide, with Bruker D8-
Advance types x-ray diffractometer carries out testing X-ray diffraction (XRD) style of acquisition to it, wherein, ordinate is relative
Intensity, abscissa are the angle of diffraction, XRD data and ceria standard spectrogram（JCPDS cards No.34-0394）Unanimously, but do not observe
To the diffraction maximum of cupric oxide, main cause is that cupric oxide load capacity is few, particle is small.
Fig. 4 is to be with the yardsticks automatically tested than surface and lacunarity analysis instrument under 77 K of TriStar II 3020
60 nanometers of ceria Mesoporous Spheres and CeO2Isothermal nitrogen adsorption-desorption curve of/CuO composite mesopore balls, wherein, before measurement
Sample first carries out 4 hours degassing process under 200 degree of vacuum conditions, and curve is respectively that the absorption of ceria Mesoporous Spheres takes off in figure
Attached curve and CeO2The adsorption/desorption curve of/CuO composite mesopore balls, as a result shows, yardstick is that 60 nanometers of ceria is mesoporous
Ball and CeO2The specific surface area of/CuO composite mesopore balls is respectively 176 meters squared per grams, 160 meters squared per grams.
Fig. 5 is to be oxidized to model with catalyzing carbon monoxide, continuously flows on fixed-bed micro-reactor in normal pressure and is received to 60
Rice ceria Mesoporous Spheres and CeO2The catalytic performance test curve of/CuO composite mesopore balls, wherein, the dosage of catalyst is
50 milligrams, be CO, O in reaction gas2、N2Mixed gas, CO, O2、N2Volume ratio is 1:10:89, flow velocity is 50 ml/mins,
Whole device gas circuit is continuously purged with High Purity Nitrogen before test every time, residual gas is removed, infrared gas analysis is used in test process
Instrument (Gasboard-3100) on-line checking product forms, and then calculates catalyzing carbon monoxide conversion rate of oxidation, the results showed that,
CeO2The catalytic activity of/CuO composite mesopore balls is not only substantially better than ceria Mesoporous Spheres, and carbon monoxide converts temperature completely
Degree is below 100 degree.
Fig. 6 is different scale CeO2The transmission electron microscope photo of/CuO composite mesopore balls, wherein, CeO in Fig. 6 a-6d2/ CuO is multiple
The yardstick for closing Mesoporous Spheres is followed successively by 30,60,110 and 150 nanometers, and all scales are 20 nanometers in figure.
Fig. 7 is the different scale CeO under conditions of Cu load capacity is 5 %2/ CuO composite mesopore ball catalyzing carbon monoxides
Oxidation susceptibility test curve, it can be seen that CeO2The catalytic activity of/CuO composite mesopore balls changes as particle scale changes.
Embodiment
From market, purchase prepares different scale CeO first2Six water cerous nitrates of raw material used in/CuO composite mesopore balls, three
Water copper nitrate, sodium carbonate, ethylene glycol, 18 megaohms of deionized waters are as made from founding pure LCT-I-10T water purifiers.
Present disclosure is described in further detail with reference to specific embodiment, but the invention is not restricted to following
The specific examples of act.
Embodiment 1
30 nano Ce O2The preparation of/CuO composite mesopore balls
Under agitation, 1.4 ml deionized waters are added in 68.6 milliliters of ethylene glycol solutions, be uniformly mixing to obtain aqueous
Ethylene glycol solution, 1.52 gram of six water cerous nitrate is then added, after stirring is completely dissolved cerous nitrate in 30 minutes, is placed on 180 degree
Reacted 1 hour in oil bath, naturally cool to room temperature, it is the two of 30 nanometers to calcine 4 hours acquisition yardsticks after centrifugal drying at 400 degree
Cerium oxide Mesoporous Spheres powder, the wherein content of ethylene glycol reclaimed water are 2 %, and the concentration of cerous nitrate is 0.05 mol/L；By 0.1 gram
The ceria Mesoporous Spheres powder of preparation is distributed in 10 ml deionized waters, then under agitation, by 7.5 milliliters of concentration
Slowly it is added dropwise in ceria Mesoporous Spheres colloidal solution for the copper nitrate solution of 0.01 mol/L, makes in adding procedure
PH value is adjusted with the sodium carbonate liquor of 0.5 mol/L, the pH value for remaining solution is 8.5-9.5, after persistently stirring 1 hour,
Centrifuged with supercentrifuge, after deionization or alcohol washes 3-5 times, obtained in 400 degree of calcinings such as Fig. 6 a institutes within 4 hours
Show, yardstick is 30 nanometers of CeO2/ CuO composite mesopore ball powders.
Embodiment 2
60 nano Ce O2The preparation of/CuO composite mesopore balls
Under agitation, 2.45 ml deionized waters are added in 67.55 milliliters of ethylene glycol solutions, are uniformly mixing to obtain and contain
Water glycol solution, 1.52 gram of six water cerous nitrate is then added, after stirring is completely dissolved cerous nitrate in 30 minutes, is placed on 180
Reacted 1 hour in degree oil bath, naturally cool to room temperature, it is 60 nanometers to obtain within 4 hours yardstick in 400 degree of calcinings after centrifugal drying
Ceria Mesoporous Spheres powder, the wherein content of ethylene glycol reclaimed water are 3.5 %, and the concentration of cerous nitrate is 0.05 mol/L；Will
0.1, which restrains standby ceria Mesoporous Spheres powder, is distributed in 10 ml deionized waters, then under agitation, by 7.5 millis
Rise concentration to be slowly added dropwise in ceria Mesoporous Spheres colloidal solution for the copper nitrate solution of 0.01 mol/L, added
Using the sodium carbonate liquor regulation pH value of 0.5 mol/L in journey, the pH value for remaining solution is 8.5-9.5, persistently stirs 1
After hour, centrifuged with supercentrifuge, after deionization or alcohol washes 3-5 time, acquisition in 4 hours is calcined at 400 degree such as
Shown in Fig. 2 b, 6b, yardstick is 60 nanometers of CeO2/ CuO composite mesopore ball powders.
Embodiment 3
110 nano Ce O2The preparation of/CuO composite mesopore balls
Under agitation, 3.5 ml deionized waters are added in 66.5 milliliters of ethylene glycol solutions, be uniformly mixing to obtain aqueous
Ethylene glycol solution, 1.52 gram of six water cerous nitrate is then added, after stirring is completely dissolved cerous nitrate in 30 minutes, is placed on 180 degree
Reacted 1 hour in oil bath, naturally cool to room temperature, it is 110 nanometers to obtain within 4 hours yardstick in 400 degree of calcinings after centrifugal drying
Ceria Mesoporous Spheres powder, the wherein content of ethylene glycol reclaimed water are 5 %, and the concentration of cerous nitrate is 0.05 mol/L；By 0.2
Restrain standby ceria Mesoporous Spheres powder to be distributed in 20 ml deionized waters, it is then under agitation, dense by 15 milliliters
The copper nitrate solution spent for 0.01 mol/L is slowly added dropwise in ceria Mesoporous Spheres colloidal solution, in adding procedure
PH value is adjusted using the sodium carbonate liquor of 0.5 mol/L, the pH value for remaining solution is 8.5-9.5, is persistently stirred 1 hour
Afterwards, centrifuged with supercentrifuge, after deionization or alcohol washes 3-5 times, such as Fig. 6 c are obtained within 4 hours in 400 degree of calcinings
Shown, yardstick is 110 nanometers of CeO2/ CuO composite mesopore ball powders.
Embodiment 4
150 nano Ce O2The preparation of/CuO composite mesopore balls
Under agitation, 4.9 ml deionized waters are added in 65.1 milliliters of ethylene glycol solutions, be uniformly mixing to obtain aqueous
Ethylene glycol solution, 1.52 gram of six water cerous nitrate is then added, after stirring is completely dissolved cerous nitrate in 30 minutes, is placed on 180 degree
Reacted 1 hour in oil bath, naturally cool to room temperature, it is 150 nanometers to obtain within 4 hours yardstick in 400 degree of calcinings after centrifugal drying
Ceria Mesoporous Spheres powder, the wherein content of ethylene glycol reclaimed water are 7 %, and the concentration of cerous nitrate is 0.05 mol/L；By 0.3
Restrain standby ceria Mesoporous Spheres powder to be distributed in 30 ml deionized waters, then under agitation, by 22.5 milliliters
Concentration is slowly added dropwise in ceria Mesoporous Spheres colloidal solution for the copper nitrate solution of 0.01 mol/L, adding procedure
The middle sodium carbonate liquor regulation pH value using 0.5 mol/L, the pH value for remaining solution is 8.5-9.5, and it is small persistently to stir 1
Shi Hou, centrifuged with supercentrifuge, after deionization or alcohol washes 3-5 times, obtained in 400 degree of calcinings as schemed within 4 hours
Shown in 6d, yardstick is 150 nanometers of CeO2/ CuO composite mesopore ball powders.
Obviously, those skilled in the art can be to CeO of the present invention2/ CuO composite mesopore balls and preparation method thereof
Carry out various changes and modification without departing from the spirit and scope of the present invention.So, if these modifications and variations of the present invention
Belong within the scope of the claims in the present invention and its equivalent technologies, then the present invention is also intended to exist comprising these changes and modification
It is interior.
Claims (3)
- A kind of 1. different scale high-specific surface area CeO2The preparation method of/CuO composite mesopore balls, it is characterized in that comprising the following steps：(1) prepared by ceria Mesoporous Spheres carrier：After a certain amount of cerous nitrate stirring and dissolving to aqueous ethylene glycol solution, place Reacted 0.5 to 6 hour in 180 degree oil bath, after room temperature is naturally cooled to, centrifuged with supercentrifuge, use deionization After water or alcohol washes 3-5 times, ceria Mesoporous Spheres powder is obtained in 300-500 degree calcining 2-6 hours, wherein in ethylene glycol The content of water is 1 %-7 %, and the concentration of cerous nitrate is 0.01-0.20 mol/Ls；(2) the ceria Mesoporous Spheres powder that 0.1-0.3 grams of step (1) obtains is distributed in 10-30 ml deionized waters, It is uniformly mixing to obtain ceria Mesoporous Spheres colloidal solution；(3) under agitation, 5-30 milliliters concentration is slowly added dropwise to two for the copper nitrate solution of 0.01 mol/L In cerium oxide Mesoporous Spheres colloidal solution, using the sodium carbonate liquor regulation pH value of 0.5 mol/L in adding procedure, remain The pH value of solution is 8.5-9.5, and after reacting 1-5 hours, eccentric cleaning obtains brown-green product after drying, and is then forged at 400 degree 2-6 hours are burnt, obtain CeO2/ CuO composite mesopore ball powders；(4) the brown-green precipitated product for being obtained step (3) with deionized water or alcohol is cleaned by ultrasonic 3-5 times, then 100 Spend and 2-3 hours are dried in baking oven, 2-6 hours are calcined at 400 degree after being fully ground, obtain CeO2/ CuO composite mesopore ball powders.
- 2. the CeO that preparation method described in claim 1 obtains2/ CuO composite mesopore balls yardstick can have in 30-150 nanometer ranges Effect regulation and control, specific surface area is 100-200 meters squared per grams, and has the characteristics that yield is high, monodispersity is good, stability is good.
- 3. the CeO that preparation method described in claim 1 obtains2/ CuO composite mesopores ball is obvious to catalyzing carbon monoxide oxidation activity Better than ceria Mesoporous Spheres, especially work as CeO2When the yardstick of/CuO composite mesopore balls is less than 100 nanometers, a corresponding oxidation The complete conversion temperature of carbon is below 100 degree.
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| CN111592027A (en) * | 2020-05-29 | 2020-08-28 | 淮阴师范学院 | Preparation method of high specific surface area cerium dioxide |
| CN112517016A (en) * | 2020-11-17 | 2021-03-19 | 上海应用技术大学 | Carbon monoxide catalytic oxidation catalyst and preparation method and application thereof |
| CN112657501A (en) * | 2020-12-23 | 2021-04-16 | 上海应用技术大学 | CO oxidation catalyst and preparation method and application thereof |
| CN112844394A (en) * | 2019-11-27 | 2021-05-28 | 中国科学院大连化学物理研究所 | CuO-CeO2Preparation method of supported catalyst and application of supported catalyst in tail gas NOxAnd application in anaerobic elimination of CO |
| CN113731428A (en) * | 2021-09-08 | 2021-12-03 | 常州大学 | CeO (CeO)2Preparation method and application of nano triangular plate supported CuO catalyst |
| CN113996304A (en) * | 2021-11-19 | 2022-02-01 | 扬州大学 | Cobalt-based composite oxide catalyst for CO low-temperature oxidation and preparation method thereof |
| CN114806072A (en) * | 2022-06-17 | 2022-07-29 | 山东海科创新研究院有限公司 | Low-VOC flame-retardant filler, flame-retardant ABS composite material and preparation method thereof |
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| CN113996304A (en) * | 2021-11-19 | 2022-02-01 | 扬州大学 | Cobalt-based composite oxide catalyst for CO low-temperature oxidation and preparation method thereof |
| CN114806072A (en) * | 2022-06-17 | 2022-07-29 | 山东海科创新研究院有限公司 | Low-VOC flame-retardant filler, flame-retardant ABS composite material and preparation method thereof |
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