CN109174096A - A kind of Au@CeO2The preparation method and applications of/HATP composite photo-catalyst - Google Patents
A kind of Au@CeO2The preparation method and applications of/HATP composite photo-catalyst Download PDFInfo
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- CN109174096A CN109174096A CN201810895310.2A CN201810895310A CN109174096A CN 109174096 A CN109174096 A CN 109174096A CN 201810895310 A CN201810895310 A CN 201810895310A CN 109174096 A CN109174096 A CN 109174096A
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- hatp
- ceo
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- PUXBEKLSMBVFNW-UHFFFAOYSA-N triphenylene-2,3,6,7,10,11-hexamine hexahydrochloride Chemical compound Cl.Cl.Cl.Cl.Cl.Cl.NC1=CC=2C3=CC(=C(C=C3C3=CC(=C(C=C3C2C=C1N)N)N)N)N PUXBEKLSMBVFNW-UHFFFAOYSA-N 0.000 title claims abstract description 133
- 239000002131 composite material Substances 0.000 title claims abstract description 79
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 79
- 238000002360 preparation method Methods 0.000 title claims abstract description 48
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 58
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 69
- 239000010931 gold Substances 0.000 claims description 68
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 64
- 239000000243 solution Substances 0.000 claims description 60
- 238000003756 stirring Methods 0.000 claims description 35
- 229910052625 palygorskite Inorganic materials 0.000 claims description 34
- 229960000892 attapulgite Drugs 0.000 claims description 33
- 239000008367 deionised water Substances 0.000 claims description 32
- 229910021641 deionized water Inorganic materials 0.000 claims description 32
- 229910001868 water Inorganic materials 0.000 claims description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 24
- 239000007787 solid Substances 0.000 claims description 24
- SJUCACGNNJFHLB-UHFFFAOYSA-N O=C1N[ClH](=O)NC2=C1NC(=O)N2 Chemical compound O=C1N[ClH](=O)NC2=C1NC(=O)N2 SJUCACGNNJFHLB-UHFFFAOYSA-N 0.000 claims description 22
- 239000003054 catalyst Substances 0.000 claims description 22
- 238000001035 drying Methods 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 20
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 claims description 15
- 239000002105 nanoparticle Substances 0.000 claims description 15
- 238000007306 functionalization reaction Methods 0.000 claims description 14
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 claims description 13
- 239000011259 mixed solution Substances 0.000 claims description 13
- 239000001509 sodium citrate Substances 0.000 claims description 12
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N EtOH Substances CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000002156 mixing Methods 0.000 claims description 11
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 claims description 3
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 3
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical class Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 14
- 229910002091 carbon monoxide Inorganic materials 0.000 description 14
- 229910002092 carbon dioxide Inorganic materials 0.000 description 11
- 230000001699 photocatalysis Effects 0.000 description 10
- 229910001220 stainless steel Inorganic materials 0.000 description 10
- 239000010935 stainless steel Substances 0.000 description 10
- 238000010531 catalytic reduction reaction Methods 0.000 description 9
- 238000005119 centrifugation Methods 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 9
- 239000007788 liquid Substances 0.000 description 9
- 239000000203 mixture Substances 0.000 description 9
- 238000005303 weighing Methods 0.000 description 9
- 239000007789 gas Substances 0.000 description 5
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 235000019253 formic acid Nutrition 0.000 description 3
- 229910000510 noble metal Inorganic materials 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 239000002114 nanocomposite Substances 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- OQUFOZNPBIIJTN-UHFFFAOYSA-N 2-hydroxypropane-1,2,3-tricarboxylic acid;sodium Chemical compound [Na].OC(=O)CC(O)(C(O)=O)CC(O)=O OQUFOZNPBIIJTN-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 241001464837 Viridiplantae Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- -1 carbon water Compound Chemical class 0.000 description 1
- 229910000420 cerium oxide Inorganic materials 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000029553 photosynthesis Effects 0.000 description 1
- 238000010672 photosynthesis Methods 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/66—Silver or gold
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2523/00—Constitutive chemical elements of heterogeneous catalysts
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2523/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00
- C07C2523/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals
- C07C2523/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group C07C2521/00 of noble metals combined with metals, oxides or hydroxides provided for in groups C07C2523/02 - C07C2523/36
- C07C2523/66—Silver or gold
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Catalysts (AREA)
Abstract
The invention belongs to energy conversion technical field of material, provide a kind of Au@CeO2The preparation method and applications of/HATP composite photo-catalyst.The present invention includes (1) CeO2The preparation of/HATP composite photo-catalyst: (2) Au@CeO2The preparation of/HATP composite photo-catalyst.The Au@CeO that the present invention obtains2/ HATP is compound to be used for CO under ultraviolet light2It is converted into the purposes of methane；The formation that preparation method of the present invention is simple, will not result in waste of resources with secondary pollution is alleviating energy crisis, provides a kind of technology.
Description
Technical field
The invention belongs to energy conversion technical field of material, are related to a kind of Au@CeO2/ HATP composite photo-catalyst
Preparation method and applications.
Technical background
Environmental pollution and energy crisis are the two big main crises and challenge that human social is faced.From
Semiconductor TiO was utilized for the first time from Fujishima and Honda in 19722After decomposing water, semiconductor light-catalyst is by solar energy
It is considered as promising method in terms of being converted to hydrogen energy source.With CO2 emissions caused by combustion of fossil fuels
Be continuously increased, carbon dioxide is reduced to chemical raw material and has become a vital task, will to Global carbon balance and
Energy crisis generates positive influence.In nature, the photosynthesis of green plants in the sun is by CO2With H2O is converted into carbon water
Compound and O2.By the inspiration of this natural process, many research activities are dedicated to developing artificial or synthesis photochemical catalyst, use
In by CO2It is reduced into organic compound and CH4Equal hydrocarbon fuels.
As the important member of rare earth semiconductor, CeO2It is non-toxic due to its high activity, high stability.In addition, nano junction
Ceria (the CeO of structure2) state that is easily achieved in Ce (IV)-Ce (III) redox cycle due to it, because it has
High oxygen transfer ability receives significant attention in solar battery and solid oxide fuel cell so that it is being catalyzed.CeO2
The position of conduction band is conducive to CO2It is reduced to methanol (CH3OH), methane (CH4), carbon monoxide (CO) and formic acid (HCOOH) etc. are changed
Work material.But since its partial size is small, it is easy to reunite the disadvantages of, cannot preferably and CO2Contact, therefore, by introduce carrier come
Improve CeO2Dispersibility.
The external surface area and inner ratio surface area of attapulgite (ATP) are all very big, therefore, with excellent adsorptivity and
Catalytic can be used as the carrier of catalyst, catalyst of olefinic polymerization etc..The catalytic performance of attapulgite is shown as, when certain
When reactive material is posted on the big hole surface for invest attapulgite crystals, reaction speed is accelerated, and reacts and generate
Novel substance dispersal events can come out inside the palygorskite clay again, and attapulgite crystalline framework is not destroyed.By right
ATP carries out acid processing and obtains the attapulgite of functionalization, makes the more active groups of attapulgite exposure, CeO2By loading function
The ATP of energyization reduces its agglomeration, by CO2Be converted to CH4Reduction current potential be -0.24V (V vs NHE, H=7).Pass through
Noble metal is introduced, the transfer rate of electronics is on the one hand increased, reduces photoexcited electron-hole pair recombination fraction；On the other hand, it utilizes
The local surface plasma resonance effect of noble metal improves light source utilization rate.
Currently, the research that cerium oxide and attapulgite combine, yet there are no relevant report.
Summary of the invention
The present invention uses the means of hydro-thermal, prepares Au@CeO2/ HATP composite photo-catalyst.
The present invention is to realize above-mentioned technical purpose by following technological means.
A kind of Au@CeO2The preparation method of/HATP composite photo-catalyst, includes the following steps:
(1)CeO2The preparation of/HATP composite photo-catalyst:
It weighs ATP and is dissolved in stirring in water bath in hydrochloric acid solution, be centrifuged, wash, it is dry, obtain the attapulgite of functionalization
HATP；
Respectively by cerium nitrate hexahydrate Ce (NO3)3In the deionized water that 6H2O and sodium hydroxide are dissolved in, after the two mixing, add
Enter HATP stirring, mixed solution be then put into vacuum reaction kettle, after baking oven hydro-thermal process, takes out cooled to room temperature,
Obtained catalyst is multiple with deionized water ethanol washing, dry to get CeO2/ HATP composite photo-catalyst；
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
Four water gold chlorides are dissolved in pure water, chlorauric acid solution is obtained；CeO prepared by step (1)2/ HATP is compound
Photochemical catalyst is dissolved in pure water, stirring, then toward CeO2Chlorauric acid solution is added dropwise inside/HATP solution, then uses citric acid
Sodium solution restores Au nanoparticle, and after mixed solution is then poured into autoclave baking oven hydro-thermal process, it is cold to take out nature
But to room temperature, centrifugal drying obtains solid, and obtained solid abrasive is arrived Au@CeO2/ HATP composite photo-catalyst.
In step (1), the temperature of stirring in water bath is 80 DEG C, time 10-24h, and the concentration of hydrochloric acid solution is 1M.
In step (1), the molar ratio of the cerium nitrate hexahydrate and sodium hydroxide is 1:(2.770-11.084).
In step (1), the mass ratio of the cerium nitrate hexahydrate and HATP are 1:(0.2886-1.154).
In step (1), the hydro-thermal process temperature is 160-200 DEG C；The hydro-thermal time is 16-30h.
In step (2), the concentration of the gold chloride is 0.02564mol/L；The mass percentage concentration of sodium citrate solution is
2wt%.
In step (2), the four water gold chloride and CeO2The mass ratio of/HATP is 1:(55.55-500).
In step (2), the hydrothermal temperature is 100-160 DEG C；The hydro-thermal time is 6-20h.
Au@CeO of the present invention2The pattern of/HATP is the Au@CeO2/ HATP pattern is the titanium dioxide of cubic
Cerium (CeO2) and spherical gold (Au) nanoparticle be dispersed in above the HATP of club shaped structure, wherein CeO2Size is about 10-
35nm。
By Au@CeO prepared by the present invention2/ HATP nano composite photo-catalyst is used for CO under ultraviolet light2Be converted to methane
Purposes.
Deionized water dosage is that soluble solids can be made to be completely dissolved in above-mentioned technical proposal.
CO2For high-purity gas, it is purchased from Shanghai Pujiang Specialty Gases Co., Ltd..
Beneficial effects of the present invention:
(1) present invention improves catalyst to the sound of visible light using the local surface plasma resonance effect of noble metal Au
Should be able to power, improve composite catalyst to the utilization rate of visible light.
(2) attapulgite exposure more active sites of the attapulgite (HATP) of functionalization relative to non-functionalization
(3) present invention is realized with Au@CeO2/ HATP nanocomposite is as photochemical catalyst for restoring CO2It produces hydrocarbon
The purpose of compound.Semiconductor excites under visible light as photochemical catalyst, according to different reduction potentials by CO2It is reduced to
HCOOH, CH4And CH3The substances such as OH.To realize the part CO in air2Gas is converted to the purpose of the energy, and this method is not
It will cause the formation of the wasting of resources and secondary pollution, and easy to operate, be a kind of environmentally protective processing technique.
Detailed description of the invention
Fig. 1 is HATP, CeO2、CeO2/HATP、Au@CeO2The UV-vis of/HATP composite photo-catalyst schemes.
Fig. 2 is HATP, CeO2、CeO2/HATP、Au@CeO2The XRD diagram of/HATP composite photo-catalyst.
Fig. 3 is Au@CeO2The TEM of/HATP composite photo-catalyst schemes.
Specific embodiment
With reference to the accompanying drawings of the specification and specific implementation example the present invention will be further described.
The photocatalytic activity evaluation of prepared photochemical catalyst in the present invention: anti-in CY-XD300Q type photochemistry stainless steel
It answers and is carried out in kettle (purchased from Shanghai Lan Yi Industrial Co., Ltd.), irradiated with ultraviolet lamp, the NaOH solution of 100mL 0.1M is added
Enter in reactor, obtained photochemical catalyst is added, high-purity CO of 30min is then led in reaction kettle2Gas, is then shut off out
Air valve continues logical CO2Gas makes the pressure of reaction kettle in 1.4MPa, is then shut off intake valve.Lamp source is opened, is used at interval of 1h
Gas sample needle takes a sample, is then detected by FID, obtains the concentration of methane according to the mark song established before, then root again
The yield of methane is obtained according to formula.
Embodiment 1:
(1)CeO2The preparation of/HATP composite photo-catalyst:
The ATP for weighing 6g is dissolved in the hydrochloric acid solution of 300mL 1M, 80 DEG C of stirring in water bath 10h, and centrifugation, washing is dried to obtain
The attapulgite (HATP) of functionalization；
Cerium nitrate hexahydrate (Ce (the NO of 1.7362g will be weighed respectively3)3·6H2O it) is dissolved in 4.8g sodium hydroxide (NaOH)
In the deionized water of 30mL, after the two mixing, 0.5g HATP stirring is added, mixed solution is then put into 160 DEG C of vacuum reactions
Kettle reacts 16h, after baking oven hydro-thermal process, takes out cooled to room temperature, obtained catalyst deionized water ethanol washing
Repeatedly, it is drying to obtain CeO2/ HATP composite photo-catalyst.
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
The gold chloride of 1g is dissolved in the Wahaha Pure Water of 100mL, chlorauric acid solution is obtained；Weigh 0.5g step (1)
The CeO of preparation2/ HATP composite photo-catalyst is dissolved in the deionized water of 30mL, stirring, then toward CeO2Drop inside/HATP solution
Add the chlorauric acid solution of 0.5mL, then restores Au nanoparticle with the sodium citrate solution of 5mL 2wt%, then will mix molten
Liquid pours into autoclave with after 100 DEG C of baking oven hydro-thermal process 6h, takes out cooled to room temperature, and centrifugal drying obtains solid,
By obtained solid abrasive to get arrive Au@CeO2/ HATP composite photo-catalyst.
(3) sample 0.1g in (2) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield of the methane measured are 2.63 μm of mol/ (gh)
Embodiment 2:
(1)CeO2The preparation of/HATP composite photo-catalyst:
The ATP for weighing 6g is dissolved in the hydrochloric acid solution of 300mL 1M, 80 DEG C of stirring in water bath 16h, and centrifugation, washing is dried to obtain
The attapulgite (HATP) of functionalization；
Cerium nitrate hexahydrate (Ce (the NO of 1.7362g will be weighed respectively3)3·6H2O it) is dissolved in 4.8g sodium hydroxide (NaOH)
In the deionized water of 30mL, after the two mixing, 0.5g HATP stirring is added, mixed solution is then put into 180 DEG C of vacuum reactions
Kettle reacts 16h, after baking oven hydro-thermal process, takes out cooled to room temperature, obtained catalyst deionized water ethanol washing
Repeatedly, it is drying to obtain CeO2/ HATP composite photo-catalyst.
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
The gold chloride of 1g is dissolved in the Wahaha Pure Water of 100mL, chlorauric acid solution is obtained；Weigh 0.5g step (1)
The CeO of preparation2/ HATP composite photo-catalyst is dissolved in the deionized water of 30mL, stirring, then toward CeO2Drop inside/HATP solution
Add the chlorauric acid solution of 0.5mL, then restores Au nanoparticle with the sodium citrate solution of 5mL 2wt%, then will mix molten
Liquid pours into autoclave with after 100 DEG C of baking oven hydro-thermal process 6h, takes out cooled to room temperature, and centrifugal drying obtains solid,
By obtained solid abrasive to get arrive Au@CeO2/ HATP composite photo-catalyst.
(3) sample 0.1g in (2) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield of the methane measured are 2.48 μm of mol/ (gh)
Embodiment 3:
(1)CeO2The preparation of/HATP composite photo-catalyst:
The ATP for weighing 6g is dissolved in the hydrochloric acid solution of 300mL 1M, 80 DEG C of stirring in water bath 20h, and centrifugation, washing is dried to obtain
The attapulgite (HATP) of functionalization；
Cerium nitrate hexahydrate (Ce (the NO of 1.7362g will be weighed respectively3)3·6H2O it) is dissolved in 4.8g sodium hydroxide (NaOH)
In the deionized water of 30mL, after the two mixing, 0.5g HATP stirring is added, mixed solution is then put into 200 DEG C of vacuum reactions
Kettle reacts 16h, after baking oven hydro-thermal process, takes out cooled to room temperature, obtained catalyst deionized water ethanol washing
Repeatedly, it is drying to obtain CeO2/ HATP composite photo-catalyst
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
The gold chloride of 1g is dissolved in the Wahaha Pure Water of 100mL, chlorauric acid solution is obtained；Weigh 0.5g step (1)
The CeO of preparation2/ HATP composite photo-catalyst is dissolved in the deionized water of 30mL, stirring, then toward CeO2Drop inside/HATP solution
Add the chlorauric acid solution of 0.5mL, then restores Au nanoparticle with the sodium citrate solution of 5mL 2wt%, then will mix molten
Liquid pours into autoclave with after 100 DEG C of baking oven hydro-thermal process 6h, takes out cooled to room temperature, and centrifugal drying obtains solid,
By obtained solid abrasive to get arrive Au@CeO2/ HATP composite photo-catalyst.
(3) sample 0.1g in (2) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield of the methane measured are 1.86 μm of mol/ (gh)
Embodiment 4:
(1)CeO2The preparation of/HATP composite photo-catalyst:
The ATP for weighing 6g is dissolved in the hydrochloric acid solution of 300mL 1M, 80 DEG C of stirring in water bath 10h, and centrifugation, washing is dried to obtain
The attapulgite (HATP) of functionalization；
Cerium nitrate hexahydrate (Ce (the NO of 1.7362g will be weighed respectively3)3·6H2O it) is dissolved in 4.8g sodium hydroxide (NaOH)
In the deionized water of 30mL, after the two mixing, 0.5g HATP stirring is added, mixed solution is then put into 200 DEG C of vacuum reactions
Kettle reacts 20h, after baking oven hydro-thermal process, takes out cooled to room temperature, obtained catalyst deionized water ethanol washing
Repeatedly, it is drying to obtain CeO2/ HATP composite photo-catalyst.
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
The gold chloride of 1g is dissolved in the Wahaha Pure Water of 100mL, chlorauric acid solution is obtained；Weigh 0.5g step (1)
The CeO of preparation2/ HATP composite photo-catalyst is dissolved in the deionized water of 30mL, stirring, then toward CeO2Drop inside/HATP solution
Add the chlorauric acid solution of 0.5mL, then restores Au nanoparticle with the sodium citrate solution of 5mL 2wt%, then will mix molten
Liquid pours into autoclave with after 120 DEG C of baking oven hydro-thermal process 6h, takes out cooled to room temperature, and centrifugal drying obtains solid,
By obtained solid abrasive to get arrive Au@CeO2/ HATP composite photo-catalyst.
(3) sample 0.1g in (2) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield of the methane measured are 2.53 μm of mol/ (gh)
Embodiment 5:
(1)CeO2The preparation of/HATP composite photo-catalyst:
The ATP for weighing 6g is dissolved in the hydrochloric acid solution of 300mL 1M, 80 DEG C of stirring in water bath 10h, and centrifugation, washing is dried to obtain
The attapulgite (HATP) of functionalization；
Cerium nitrate hexahydrate (Ce (the NO of 1.7362g will be weighed respectively3)3·6H2O it) is dissolved in 10g sodium hydroxide (NaOH)
In the deionized water of 30mL, after the two mixing, 1.0g HATP stirring is added, mixed solution is then put into 180 DEG C of vacuum reactions
Kettle reacts for 24 hours, after baking oven hydro-thermal process, takes out cooled to room temperature, obtained catalyst deionized water ethanol washing
Repeatedly, it is drying to obtain CeO2/ HATP composite photo-catalyst.
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
The gold chloride of 1g is dissolved in the Wahaha Pure Water of 100mL, chlorauric acid solution is obtained；Weigh 0.5g step (1)
The CeO of preparation2/ HATP composite photo-catalyst is dissolved in the deionized water of 30mL, stirring, then toward CeO2Drop inside/HATP solution
Add the chlorauric acid solution of 0.1mL, then restores Au nanoparticle with the sodium citrate solution of 5mL 2wt%, then will mix molten
Liquid pours into autoclave with after 120 DEG C of baking oven hydro-thermal process 6h, takes out cooled to room temperature, and centrifugal drying obtains solid,
By obtained solid abrasive to get arrive Au@CeO2/ HATP composite photo-catalyst.
(3) sample 0.1g in (2) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield of the methane measured are 2.16 μm of mol/ (gh)
Embodiment 6:
(1)CeO2The preparation of/HATP composite photo-catalyst:
The ATP for weighing 6g is dissolved in the hydrochloric acid solution of 300mL 1M, 80 DEG C of stirring in water bath 10h, and centrifugation, washing is dried to obtain
The attapulgite (HATP) of functionalization；
Cerium nitrate hexahydrate (Ce (the NO of 1.7362g will be weighed respectively3)3·6H2O it) is dissolved in 10g sodium hydroxide (NaOH)
In the deionized water of 30mL, after the two mixing, 1.0g HATP stirring is added, mixed solution is then put into 200 DEG C of vacuum reactions
Kettle reacts 30h, after baking oven hydro-thermal process, takes out cooled to room temperature, obtained catalyst deionized water ethanol washing
Repeatedly, it is drying to obtain CeO2/ HATP composite photo-catalyst.
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
The gold chloride of 1g is dissolved in the Wahaha Pure Water of 100mL, chlorauric acid solution is obtained；Weigh 0.5g step (1)
The CeO of preparation2/ HATP composite photo-catalyst is dissolved in the deionized water of 30mL, stirring, then toward CeO2Drop inside/HATP solution
Add the chlorauric acid solution of 0.3mL, then restores Au nanoparticle with the sodium citrate solution of 5mL 2wt%, then will mix molten
Liquid pours into autoclave with after 140 DEG C of baking oven hydro-thermal process 10h, takes out cooled to room temperature, and centrifugal drying obtains solid,
By obtained solid abrasive to get arrive Au@CeO2/ HATP composite photo-catalyst.
(3) sample 0.1g in (2) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield of the methane measured are 2.07 μm of mol/ (gh)
Embodiment 7:
(1)CeO2The preparation of/HATP composite photo-catalyst:
The ATP for weighing 6g is dissolved in the hydrochloric acid solution of 300mL 1M, 80 DEG C of stirring in water bath 10h, and centrifugation, washing is dried to obtain
The attapulgite (HATP) of functionalization；
Cerium nitrate hexahydrate (Ce (the NO of 1.7362g will be weighed respectively3)3·6H2O it) is dissolved in 10g sodium hydroxide (NaOH)
In the deionized water of 30mL, after the two mixing, 2.0g HATP stirring is added, mixed solution is then put into 200 DEG C of vacuum reactions
Kettle reacts for 24 hours, after baking oven hydro-thermal process, takes out cooled to room temperature, obtained catalyst deionized water ethanol washing
Repeatedly, it is drying to obtain CeO2/ HATP composite photo-catalyst.
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
The gold chloride of 1g is dissolved in the Wahaha Pure Water of 100mL, chlorauric acid solution is obtained；Weigh 0.5g step (1)
The CeO of preparation2/ HATP composite photo-catalyst is dissolved in the deionized water of 30mL, stirring, then toward CeO2Drop inside/HATP solution
Add the chlorauric acid solution of 0.7mL, then restores Au nanoparticle with the sodium citrate solution of 5mL 2wt%, then will mix molten
Liquid pours into autoclave with after 140 DEG C of baking oven hydro-thermal process 14h, takes out cooled to room temperature, and centrifugal drying obtains solid,
By obtained solid abrasive to get arrive Au@CeO2/ HATP composite photo-catalyst.
(3) sample 0.1g in (2) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield of the methane measured are 3.14 μm of mol/ (gh)
Embodiment 8:
(1)CeO2The preparation of/HATP composite photo-catalyst:
The ATP for weighing 6g is dissolved in the hydrochloric acid solution of 300mL 1M, and for 24 hours, centrifugation, washing is dried to obtain 80 DEG C of stirring in water bath
The attapulgite (HATP) of functionalization；
Cerium nitrate hexahydrate (Ce (the NO of 1.7362g will be weighed respectively3)3·6H2O it) is dissolved in 19.2g sodium hydroxide (NaOH)
In the deionized water of 30mL, after the two mixing, 1.5g HATP stirring is added, mixed solution is then put into 180 DEG C of vacuum reactions
Kettle reacts for 24 hours, after baking oven hydro-thermal process, takes out cooled to room temperature, obtained catalyst deionized water ethanol washing
Repeatedly, it is drying to obtain CeO2/ HATP composite photo-catalyst.
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
The gold chloride of 1g is dissolved in the Wahaha Pure Water of 100mL, chlorauric acid solution is obtained；Weigh 0.5g step (1)
The CeO of preparation2/ HATP composite photo-catalyst is dissolved in the deionized water of 30mL, stirring, then toward CeO2Drop inside/HATP solution
Add the chlorauric acid solution of 0.8mL, then restores Au nanoparticle with the sodium citrate solution of 5mL 2wt%, then will mix molten
Liquid pours into autoclave with after 160 DEG C of baking oven hydro-thermal process 16h, takes out cooled to room temperature, and centrifugal drying obtains solid,
By obtained solid abrasive to get arrive Au@CeO2/ HATP composite photo-catalyst.
(3) sample 0.1g in (2) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield of the methane measured are 1.26 μm of mol/ (gh)
Embodiment 9:
(1)CeO2The preparation of/HATP composite photo-catalyst:
The ATP for weighing 6g is dissolved in the hydrochloric acid solution of 300mL 1M, and for 24 hours, centrifugation, washing is dried to obtain 80 DEG C of stirring in water bath
The attapulgite (HATP) of functionalization；
Cerium nitrate hexahydrate (Ce (the NO of 1.7362g will be weighed respectively3)3·6H2O it) is dissolved in 19.2g sodium hydroxide (NaOH)
In the deionized water of 30mL, after the two mixing, 2.0g HATP stirring is added, mixed solution is then put into 180 DEG C of vacuum reactions
Kettle reacts for 24 hours, after baking oven hydro-thermal process, takes out cooled to room temperature, obtained catalyst deionized water ethanol washing
Repeatedly, it is drying to obtain CeO2/ HATP composite photo-catalyst.
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
The gold chloride of 1g is dissolved in the Wahaha Pure Water of 100mL, chlorauric acid solution is obtained；Weigh 0.5g step (1)
The CeO of preparation2/ HATP composite photo-catalyst is dissolved in the deionized water of 30mL, stirring, then toward CeO2Drop inside/HATP solution
Add the chlorauric acid solution of 0.9mL, then restores Au nanoparticle with the sodium citrate solution of 5mL 2wt%, then will mix molten
Liquid pours into autoclave with after 160 DEG C of baking oven hydro-thermal process 20h, takes out cooled to room temperature, and centrifugal drying obtains solid,
By obtained solid abrasive to get arrive Au@CeO2/ HATP composite photo-catalyst.
(3) sample 0.1g in (2) is taken to carry out photo catalytic reduction CO in CY-XD300Q type photochemistry stainless steel cauldron2
Experiment, the yield of the methane measured are 1.45 μm of mol/ (gh)
Fig. 1 is Au@CeO2The UV-vis of/HATP composite photo-catalyst schemes, and illustrates Au@CeO in figure2/ HATP complex light is urged
Agent photoresponse ability compares not compound CeO2And CeO2/ HATP presoma, which has, to be greatly enhanced.
Fig. 2 is Au@CeO2The XRD diagram of/HATP composite photo-catalyst presents CeO with being apparent in figure2, the feature of HATP
Peak, but fail to detect the characteristic peak of Au, it may be possible to because caused by the few reason of Au nano-particle content.
Fig. 3 is Au@CeO2The TEM of/HATP composite photo-catalyst schemes, it can be seen from the figure that the titanium dioxide of cubic
Cerium (CeO2) and spherical gold (Au) nanoparticle be dispersed in above the HATP of club shaped structure, wherein CeO2Size is about 10-
35nm。
The embodiment is a preferred embodiment of the present invention, but present invention is not limited to the embodiments described above, not
In the case where substantive content of the invention, any conspicuous improvement that those skilled in the art can make, replacement
Or modification all belongs to the scope of protection of the present invention.
Claims (10)
1. a kind of Au@CeO2The preparation method of/HATP composite photo-catalyst, which comprises the steps of:
(1)CeO2The preparation of/HATP composite photo-catalyst:
It weighs ATP and is dissolved in stirring in water bath in hydrochloric acid solution, be centrifuged, wash, it is dry, obtain the attapulgite HATP of functionalization；
Respectively by cerium nitrate hexahydrate Ce (NO3)3·6H2In the deionized water that O and sodium hydroxide are dissolved in, after the two mixing, it is added
HATP stirring, is then put into vacuum reaction kettle for mixed solution, after baking oven hydro-thermal process, takes out cooled to room temperature, obtains
The catalyst arrived is multiple with deionized water ethanol washing, dry to get CeO2/ HATP composite photo-catalyst；
(2)Au@CeO2The preparation of/HATP composite photo-catalyst:
Four water gold chlorides are dissolved in pure water, chlorauric acid solution is obtained；CeO prepared by step (1)2/ HATP composite photocatalyst
Agent is dissolved in pure water, stirring, then toward CeO2Chlorauric acid solution is added dropwise inside/HATP solution, then uses sodium citrate solution
Au nanoparticle is restored, after mixed solution is then poured into autoclave baking oven hydro-thermal process, taking-up naturally cools to room
Temperature, centrifugal drying obtain solid, and obtained solid abrasive is arrived Au@CeO2/ HATP composite photo-catalyst.
2. a kind of Au@CeO according to claim 12The preparation method of/HATP composite photo-catalyst, which is characterized in that step
Suddenly in (1), the temperature of stirring in water bath is 80 DEG C, time 10-24h, and the concentration of hydrochloric acid solution is 1M.
3. a kind of Au@CeO according to claim 12The preparation method of/HATP composite photo-catalyst, which is characterized in that step
Suddenly in (1), the molar ratio of the cerium nitrate hexahydrate and sodium hydroxide is 1:(2.770-11.084).
4. a kind of Au@CeO according to claim 12The preparation method of/HATP composite photo-catalyst, which is characterized in that step
Suddenly in (1), the mass ratio of the cerium nitrate hexahydrate and HATP are 1:(0.2886-1.154).
5. a kind of Au@CeO according to claim 12The preparation method of/HATP composite photo-catalyst, which is characterized in that step
Suddenly in (1), the hydro-thermal process temperature is 160-200 DEG C；The hydro-thermal time is 16-30h.
6. a kind of Au@CeO according to claim 12The preparation method of/HATP composite photo-catalyst, which is characterized in that step
Suddenly in (2), the concentration of the gold chloride is 0.02564mol/L；The mass percentage concentration of sodium citrate solution is 2wt%.
7. a kind of Au@CeO according to claim 42The preparation method of/HATP composite photo-catalyst, which is characterized in that step
Suddenly in (2), the four water gold chloride and CeO2The mass ratio of/HATP is 1:(55.55-500).
8. a kind of Au@CeO according to claim 12The preparation method of/HATP composite photo-catalyst, which is characterized in that step
Suddenly in (2), the hydrothermal temperature is 100-160 DEG C；The hydro-thermal time is 6-20h.
9. Au@CeO made from preparation method described according to claim 1~any one of 82/ HATP composite photo-catalyst,
It is characterized in that, the Au@CeO2/ HATP pattern is the ceria (CeO of cubic2) and spherical gold (Au) nanoparticle
It is dispersed in above the HATP of club shaped structure, wherein CeO2Size is about 10-35nm.
10. by Au@CeO as claimed in claim 92/ HATP composite photo-catalyst is used for CO under ultraviolet light2Be converted to the use of methane
On the way.
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| CN114870857B (en) * | 2022-06-21 | 2023-07-25 | 南京信息工程大学 | Spherical MnFeOx-CeO 2 Composite oxide integrated catalyst and preparation method thereof |
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