CN110090640A - Monodisperse platinum base two-dimensional metallic hydroxide and its in-situ synthetic method and the application in the oxygen-containing hydro carbons purification of volatility - Google Patents
Monodisperse platinum base two-dimensional metallic hydroxide and its in-situ synthetic method and the application in the oxygen-containing hydro carbons purification of volatility Download PDFInfo
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- CN110090640A CN110090640A CN201910299153.3A CN201910299153A CN110090640A CN 110090640 A CN110090640 A CN 110090640A CN 201910299153 A CN201910299153 A CN 201910299153A CN 110090640 A CN110090640 A CN 110090640A
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- Prior art keywords
- dimensional metallic
- metallic hydroxide
- platinum base
- polyethylene oxide
- monodisperse
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 229910052697 platinum Inorganic materials 0.000 title claims abstract description 56
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 title claims abstract description 37
- 239000001301 oxygen Substances 0.000 title claims abstract description 25
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 25
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 24
- 229930195733 hydrocarbon Natural products 0.000 title claims abstract description 19
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 18
- 150000002430 hydrocarbons Chemical class 0.000 title claims abstract description 17
- 238000010189 synthetic method Methods 0.000 title claims abstract description 13
- 238000000746 purification Methods 0.000 title claims abstract description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000000243 solution Substances 0.000 claims abstract description 46
- 238000003756 stirring Methods 0.000 claims abstract description 40
- -1 polyethylene Polymers 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims abstract description 17
- 239000004698 Polyethylene Substances 0.000 claims abstract description 17
- 229920000573 polyethylene Polymers 0.000 claims abstract description 17
- 229920000428 triblock copolymer Polymers 0.000 claims abstract description 17
- 239000004743 Polypropylene Substances 0.000 claims abstract description 16
- 229920001155 polypropylene Polymers 0.000 claims abstract description 15
- VKYKSIONXSXAKP-UHFFFAOYSA-N hexamethylenetetramine Chemical compound C1N(C2)CN3CN1CN2C3 VKYKSIONXSXAKP-UHFFFAOYSA-N 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 11
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 230000036571 hydration Effects 0.000 claims abstract description 10
- 238000006703 hydration reaction Methods 0.000 claims abstract description 10
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- 239000004312 hexamethylene tetramine Substances 0.000 claims abstract description 7
- 235000010299 hexamethylene tetramine Nutrition 0.000 claims abstract description 7
- 150000000703 Cerium Chemical class 0.000 claims abstract description 6
- 150000001868 cobalt Chemical class 0.000 claims abstract description 6
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 30
- 238000002360 preparation method Methods 0.000 claims description 5
- AGGKEGLBGGJEBZ-UHFFFAOYSA-N tetramethylenedisulfotetramine Chemical compound C1N(S2(=O)=O)CN3S(=O)(=O)N1CN2C3 AGGKEGLBGGJEBZ-UHFFFAOYSA-N 0.000 claims description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 125000001434 methanylylidene group Chemical group [H]C#[*] 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000001354 calcination Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 56
- 238000006555 catalytic reaction Methods 0.000 abstract description 39
- 239000003054 catalyst Substances 0.000 abstract description 12
- 230000008569 process Effects 0.000 abstract description 6
- 239000006185 dispersion Substances 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000010992 reflux Methods 0.000 abstract description 2
- 238000010438 heat treatment Methods 0.000 abstract 1
- 230000000694 effects Effects 0.000 description 18
- 238000012360 testing method Methods 0.000 description 14
- 229910000510 noble metal Inorganic materials 0.000 description 12
- 239000007789 gas Substances 0.000 description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 10
- 230000003197 catalytic effect Effects 0.000 description 10
- 230000006872 improvement Effects 0.000 description 8
- 239000012855 volatile organic compound Substances 0.000 description 8
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- SMKFCFKIYPLYNY-UHFFFAOYSA-K cerium(3+);trichloride;hydrate Chemical compound O.Cl[Ce](Cl)Cl SMKFCFKIYPLYNY-UHFFFAOYSA-K 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- 239000007788 liquid Substances 0.000 description 5
- 229910052757 nitrogen Inorganic materials 0.000 description 5
- 239000007787 solid Substances 0.000 description 5
- 238000005406 washing Methods 0.000 description 5
- 239000004215 Carbon black (E152) Substances 0.000 description 4
- 125000004429 atom Chemical group 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 229960000935 dehydrated alcohol Drugs 0.000 description 4
- 238000002242 deionisation method Methods 0.000 description 4
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 4
- COTNUBDHGSIOTA-UHFFFAOYSA-N meoh methanol Chemical compound OC.OC COTNUBDHGSIOTA-UHFFFAOYSA-N 0.000 description 4
- 239000000523 sample Substances 0.000 description 4
- 238000007873 sieving Methods 0.000 description 4
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 3
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 150000003839 salts Chemical class 0.000 description 3
- 230000004913 activation Effects 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 description 2
- 239000007795 chemical reaction product Substances 0.000 description 2
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000011109 contamination Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000004949 mass spectrometry Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 150000002894 organic compounds Chemical class 0.000 description 2
- 239000010970 precious metal Substances 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000007790 solid phase Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 229910004664 Cerium(III) chloride Inorganic materials 0.000 description 1
- 229910021580 Cobalt(II) chloride Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical group [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
- QYSYEILYXGRUOM-UHFFFAOYSA-N [Cl].[Pt] Chemical compound [Cl].[Pt] QYSYEILYXGRUOM-UHFFFAOYSA-N 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 239000000926 atmospheric chemistry Substances 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 150000008282 halocarbons Chemical group 0.000 description 1
- 230000011132 hemopoiesis Effects 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 210000003734 kidney Anatomy 0.000 description 1
- 210000002751 lymph Anatomy 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000007144 microwave assisted synthesis reaction Methods 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 210000000496 pancreas Anatomy 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000007639 printing Methods 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 210000002784 stomach Anatomy 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011593 sulfur Chemical group 0.000 description 1
- 210000001519 tissue Anatomy 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
-
- 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
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
-
- 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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8913—Cobalt and noble metals
-
- B01J35/23—
-
- B01J35/615—
-
- B01J35/633—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/344—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy
- B01J37/346—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of electromagnetic wave energy of microwave energy
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/702—Hydrocarbons
Abstract
Monodisperse platinum base two-dimensional metallic hydroxide and its in-situ synthetic method and the application in the oxygen-containing hydro carbons purification of volatility, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer are dissolved in deionized water, stirring forms transparent clear solution；Then hexamethylenetetramine is added, it stirs evenly, adds cerium salt or cobalt salt, stir evenly, ethylene glycol is added, it is stirring evenly and then adding into six hydration chloroplatinic acids-ethylene glycol solution, stirs evenly, obtains mixed solution, then mixed solution is carried out to heating reflux reaction in microwave generator, it is centrifuged after fully reacting, roasts, obtain monodisperse platinum base two-dimensional metallic hydroxide.Catalysis material prepared by the invention possesses the platinum active site of atom level dispersion and shows the oxygen-containing hydro carbons low-temperature purifying ability of excellent volatility.Meanwhile process for synthetic catalyst involved in the present invention is simple, the prices of raw materials are cheap, there is good industrial applications prospect.
Description
Technical field
The invention belongs to technical field of atmospheric pollution control, are related specifically to a kind of monodisperse platinum base two-dimensional metallic hydroxide
Object and its in-situ synthetic method and the application in the oxygen-containing hydro carbons room temperature purification of volatility.
Background technique
Volatile organic contaminant (Volatile Organic Compounds, VOCs) refers to that boiling point is lower than under normal pressure
260 DEG C of organic compound, or saturated vapour pressure is more than 133.32Pa under room temperature (25 DEG C), is discharged into the form of gaseous molecular
The general name of all organic compounds in air.VOCs is many kinds of, includes mainly aliphatic hydrocarbon, oxygen-containing hydrocarbon, aromatic hydrocarbon and its spreads out
Biology, containing halocarbon, nitrogen-containing hydrocarbons, sulfur-bearing hydrocarbon etc..VOCs has very high Atmospheric Chemistry reactivity, is that oxidizing capacity enhances
Key factor.In recent years, VOCs total emission volumn in China gradually increases, and photochemical fog, city gray haze caused etc. is compound big
Gas pollution problem is got worse.A large amount of VOCs discharges not only cause air quality to decline, but also to the immune system of human body, kidney
Great harm is also generated with the function of respiratory system, increases human body (tissues such as brain, pancreas, lymph, hematopoiesis and stomach and device
Official) carcinogenic risk.After the improvement of dedusting, desulphurization and denitration and tail gas pollution of motor-driven vehicle, it is big that VOCs contamination control has become China
One of gas contamination control privileged direction.According to related request, China carries out key industry (garden) discharge volatile hydrocarbon at present
It is reduced emission reduction, emphasizes the Mitigation options for carrying out the discharge process for combining source, and form efficient control technology and process equipment.
Therefore, the control of VOCs efficient emission-reducing is of great significance to China's atmosphere quality is improved.Oxygen-containing volatile organic contaminant
The representative of (such as formaldehyde, acetone, ethyl acetate) as hetero atom hydro carbons, can be by upholstery, coating, packages printing, electronics
The number of ways such as chemical industry are discharged into environment, cause extremely serious negative effect to the production and living of the mankind.Catalytic oxidation technologies
It is one of the most effective means of current purifying low-concentration volatile hydrocarbon due to having many advantages, such as efficient, energy-saving and environmental protection.Support type
Noble metal catalyst is widely adopted in the removal of oxygen-containing hydro carbons since its activity is good, renewable is strong.But due to your gold
Belong to the prospect that expensive and factors such as activated centre easy in inactivation easy to reunite limit its further industrial applications.Therefore it is badly in need of root
A kind of monatomic catalyst with high activity, high stability is researched and developed according to the Drainage feature and characterization of molecules of the oxygen-containing hydro carbons of volatility
To improve the pollutant conversion ratio on unit pt atom, higher activity is still able to maintain while reduction catalysis material is at low cost
And stability.
Summary of the invention
The object of the present invention is to provide a kind of monodisperse platinum base two-dimensional metallic hydroxide and its in-situ synthetic method and
Application in the oxygen-containing hydro carbons room temperature purification of volatility.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of in-situ synthetic method of monodisperse platinum base two-dimensional metallic hydroxide, by polyethylene oxide-polypropylene oxide-
Polyethylene oxide triblock copolymer is dissolved in deionized water, and stirring forms transparent clear solution；Then six methines four are added
Amine stirs evenly, and adds cerium salt or cobalt salt, stirs evenly, and ethylene glycol is added, is stirring evenly and then adding into six hydration chloroplatinic acids-
Ethylene glycol solution stirs evenly, and obtains mixed solution, then carries out mixed solution in microwave generator being heated to reflux anti-
It answers, is centrifuged after fully reacting, roast, obtain monodisperse platinum base two-dimensional metallic hydroxide.
A further improvement of the present invention lies in that polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer with
The ratio of deionized water is 0.27g:(30-45) mL.
A further improvement of the present invention lies in that polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer,
Hexamethylenetetramine, cerium salt, six hydration chloroplatinic acid-ethylene glycol solution ratio 0.27g:(4.0-5.3) g:(5-35) mmoL:3mL；
Or polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, hexamethylenetetramine, cobalt salt, six hydration chlorine platinum
Acid-ethylene glycol solution ratio 0.27g:(4.0-5.3) g:(5-35) mmoL:3mL.
A further improvement of the present invention lies in that, wherein six hydration chloroplatinic acid-ethylene glycol solution concentration are 1.5mgPt/
mL。
A further improvement of the present invention lies in that polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer with
The ratio of ethylene glycol is 0.27g:(180-220) mL.
A further improvement of the present invention lies in that the power setting of microwave generator is 900W, the temperature of back flow reaction is
140-150 DEG C, time 20-40min.
A further improvement of the present invention lies in that roasting carries out under nitrogen atmosphere, the temperature of roasting is 200 DEG C, when roasting
Between be 2-3.5h.
A kind of monodisperse platinum base two-dimensional metallic hydroxide prepared according to the above method, specific surface area 134.2-
156.7m2/ g, Micropore volume 0.11-0.24cm3/g。
A kind of monodisperse platinum base two-dimensional metallic hydroxide according to above method preparation is purified in the oxygen-containing hydro carbons of volatility
In application.
A further improvement of the present invention lies in that monodisperse platinum base two-dimensional metallic hydroxide is in 120 DEG C, air speed 36000h-1,
Under conditions of oxygen volumetric concentration 20%, the deep purifying for being 0.08% to methanol volumetric concentration is realized.
Compared with prior art, the invention has the benefit that
In the present invention using polycyclic miscellaneous aminated compounds in reproducibility solvent ethylene glycol easily with after hydrolysis cerium salt or
The metal salt presoma for being quickly complexed and being formed two-dimensional material occurs for cobalt salt.And by adding polyethylene oxide-polycyclic oxygen third in advance
Alkane-polyethylene oxide triblock copolymer promotes the complexing degree of metal salt presoma and increases the Kong Rong of two-dimentional hydroxide
And specific surface area.The two-dimensional material metal salt presoma that this step is formed compared with prior art, possesses more stable complexing side
Formula, and possess richer surface hydroxyl functional group.In the present invention with in-situ method introduce active component platinum presoma, make its with
Two-dimentional hydroxide precursor surface hydroxyl is converted by strong electronics and is combined, this combination and common adsorption activity
Site is compared, and has superior stability.Existing water and synthesis are replaced by the method for Microwave-assisted synthesis in the present invention
Method and solvent-thermal process method highly shortened generated time and energy consumption, solve carried noble metal to a certain extent
Expensive problem overcomes existing monatomic catalysis material preparation process complexity, the technological deficiency of low output.
The present invention passes through two by microwave assisting method fabricated in situ monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material
The feature of low Surface Polarization and Atomic coordinate number specific to Vygen category hydroxide makes it easier to and monatomic noble metal
Active component forms the active interface of " platinum-hydroxyl-carrier ", accelerates the electronics transfer between carrier and noble metal, passes through table
The effect of face hydroxyl obtains the monatomic catalyst of highly stable noble metal.
Monodisperse platinum base two-dimensional metallic hydroxide prepared by the present invention being capable of answering in the oxygen-containing hydro carbons purification of volatility
With in 120 DEG C, air speed 36000h-1, under conditions of oxygen volumetric concentration 20%, can be realized and be to methanol volumetric concentration
0.08% deep purifying, the present invention are with important application prospects in volatile organic contaminant low temperature purification field.
Detailed description of the invention
Fig. 1 is Pt in the present invention1-Ce(OH)xThe field emission scanning electron microscope and high resolution TEM of two-dimentional catalysis material
Image；Wherein, (a) is Pt1-Co(OH)xThe field emission scanning electron microscope of two-dimentional catalysis material (b) is high resolution TEM figure
Picture.
Fig. 2 is Pt in the present invention1-Co(OH)xThe field emission scanning electron microscope and high resolution TEM of two-dimentional catalysis material
Image；Wherein, (a) is Pt1-Ce(OH)xThe field emission scanning electron microscope of two-dimentional catalysis material (b) is high resolution TEM figure
Picture.
Fig. 3 is Pt in the present invention1-Co(OH)xThe spherical aberration of two-dimentional catalysis material corrects electron microscope image；Wherein, (a)
It (b) is high magnification numbe for low power number.
Fig. 4 is monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material in the present invention1H solid phase nmr spectrum；
Fig. 5 is the active testing of monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material catalytic degradation methanol in the present invention
Curve.
Fig. 6 is the water-resistance test chart of monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material in the present invention；
Fig. 7 is the anti-CO of monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material in the present invention2Impact property test chart.
Specific embodiment
With reference to the accompanying drawing and embodiment the present invention is described in detail.
This hair is by microwave assisting method fabricated in situ monodisperse platinum base two-dimensional metallic hydroxide, by two-dimensional metallic hydroxide
Ultra-thin two-dimension hydroxide materials specific to object can greatly reduce Surface Polarization and Atomic coordinate number, it is easier to single original
Sub- noble metal active component forms the active interface of " platinum-hydroxyl-carrier ", and the electronics accelerated between carrier and noble metal turns
It moves, by the effect of surface hydroxyl, obtains highly stable precious metal catalytic material.
The present invention the following steps are included:
(1) 0.27g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) is dissolved in 30-
In 45mL deionized water, and continue to stir 15min with 500-800rpm revolving speed, forms transparent clear solution；
(2) 4.0-5.3g hexamethylenetetramine is added into transparent clear solution obtained by step (1), turns in 500-800rpm
The lower sufficiently dissolution of speed stirring；
(3) the seven chloride hydrate cerium (CeCl of 5-35mmoL are added into step (2) acquired solution3·7H2O)/six it is hydrated chlorine
Change cobalt (CoCl2·6H2O), stirring dissolves it sufficiently energetically；
(4) it is slowly added to the ethylene glycol solution of 180-220mL into step (3) acquired solution, and continues to stir 15min；
On the one hand ethylene glycol plays the role of dispersing agent, on the one hand play reducing agent.
(5) 3mL six is added dropwise into step (4) acquired solution and is hydrated chloroplatinic acid-ethylene glycol solution (1.5mgPt/ mL),
And continue to stir 30min with 800-1000rpm revolving speed；
(6) step (5) acquired solution is placed in the three-neck flask of microwave generator, power setting 900W will be mixed
Solution is heated to 140-150 DEG C；
(7) step (6) acquired solution is condensed back 20-40min under the conditions of 140-150 DEG C；
(8) liquid obtained by (7) that will be flowed back is cooled to room temperature, and is centrifuged under the conditions of 8000rpm, and obtained solid is with anhydrous
Ethyl alcohol and deionized water washing, drying at room temperature 12-21h, roast 2-3.5h under 200 DEG C of nitrogen atmospheres in Muffle furnace.Roasting
Purpose is the organic matter for removing surface, forms more firm two-dimensional framework, monodisperse platinum base two-dimensional metallic hydrogen is obtained after roasting
Oxide.
Monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material prepared by the present invention has the platinum activity of atom level dispersion
Site；Its specific surface area (134.2-156.7m with higher2/ g) and Micropore volume (0.11-0.24cm3/g)；Monodisperse platinum
Base two-dimensional metallic hydroxide can be in the application in the oxygen-containing hydro carbons purification of volatility.Specifically, in 120 DEG C, air speed 36000h-1, it can be achieved that deep purifying to volumetric concentration 800ppm methanol under conditions of oxygen volumetric concentration 20%；Of the invention is made
Standby catalysis material possesses good stability and anti-poisoning capability.
It is below specific embodiment.
Embodiment 1 uses Microwave Assisted Process fabricated in situ monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material
0.27g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) is dissolved in 30-45mL
In deionized water, and continue to stir 15min with 500-800rpm revolving speed, forms transparent clear solution.It is added into above-mentioned solution
4.0-5.3 g hexamethylenetetramine sufficiently dissolves under the stirring of 500-800rpm revolving speed.Seven hydrations of 5-35mmoL are then added
Cerium chloride (CeCl3·7H2O), stirring dissolves it sufficiently energetically.The second of 180-220mL is slowly added into above-mentioned acquired solution
Glycol solution, and continue to stir 15min.And then 3mL six is added dropwise and is hydrated chloroplatinic acid-ethylene glycol solution (1.5mgPt/ mL),
And continue to stir 30min with 800-1000rpm revolving speed.Solution is placed in the three-neck flask of microwave generator, power setting is
Mixed solution is heated to 150 DEG C and is condensed back 20min with this condition by 900W.
It is cooled to room temperature to liquid, is centrifuged under the conditions of 8000rpm, obtained solid dehydrated alcohol and deionization washing
It washs, drying at room temperature 12-21h, roasts 2-3.5h under 200 DEG C of nitrogen atmospheres in Muffle furnace, obtain monodisperse platinum base two-dimensional metallic
Hydroxide, i.e. monodisperse Pt1-Ce(OH)xTwo-dimentional catalysis material.
Embodiment 2
By seven chloride hydrate cerium (CeCl in embodiment 13·7H2O cobalt chloride hexahydrate (CoCl) is replaced with2·6H2O),
Obtain monodisperse platinum base two-dimensional metallic hydroxide, i.e. monodisperse Pt1-Co(OH)xTwo-dimentional catalysis material.Other and 1 phase of embodiment
Together.
Monodisperse Pt1-Ce(OH)xThe activity of two-dimentional catalysis material catalytic degradation methanol
Catalysis reaction carries out in fixed bed, accurate to claim by the tabletting of gained catalyst, sieving (40-60 mesh) in embodiment 1
Catalysis material after taking 0.3mL to be sieved, in 200 DEG C of activation 1.5h, using methanol (methanol) as probe gas, reactant
Concentration control in 800ppm, reaction velocity 36000h-1, oxygen volumetric concentration be 20%, respectively test catalyst 40 DEG C,
Catalysis at a temperature of 60 DEG C, 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C is anti-
Activity is answered, reaction product passes through gas-chromatography and on-line mass spectroscopy monitoring analysis.
Monodisperse Pt1-Co(OH)xThe activity of two-dimentional catalysis material catalytic degradation methanol
Catalysis reaction carries out in fixed bed, accurate to claim by the tabletting of gained catalyst, sieving (40-60 mesh) in embodiment 2
Catalysis material after taking 0.3mL to be sieved, in 200 DEG C of activation 1.5h, using methanol (methanol) as probe gas, reactant
Concentration control in 800ppm, reaction velocity 36000h-1, oxygen volumetric concentration be 20%, respectively test catalyst 40 DEG C,
Catalysis at a temperature of 60 DEG C, 80 DEG C, 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C, 130 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, 170 DEG C is anti-
Activity is answered, reaction product passes through gas-chromatography and on-line mass spectroscopy monitoring analysis.
Fig. 1 is the Pt that in the present invention prepared by embodiment 21-Co(OH)xThe field emission scanning electron microscope and height of two-dimentional catalysis material
Resolution Transmission sem image, as can be seen from Figure 1 Pt1-Co(OH)xThe microcosmic ultrathin nanometer that rule is presented of two-dimentional catalysis material
Piece pattern.
Fig. 2 is the Pt that in the present invention prepared by embodiment 11-Ce(OH)xThe field emission scanning electron microscope and height of two-dimentional catalysis material
Resolution Transmission sem image, as can be seen from Figure 2 Pt1-Ce(OH)xThe microcosmic ultrathin nanometer that rule is presented of two-dimentional catalysis material
Piece pattern, and rough surface and have a large amount of hole.
Fig. 3 is the Pt that in the present invention prepared by embodiment 21-Co(OH)xThe spherical aberration of two-dimentional catalysis material corrects electron microscope
Image, as can be seen from Figure 3 Pt1-Co(OH)xAtom and dispersity is mutually presented (in figure in two-dimentional catalysis material surface platinum activity
Bright spot in circle).
Fig. 4 is the monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material that in the present invention prepared by embodiment 1 and embodiment 2
's1H solid phase nmr spectrum contains according to analysis monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material surface
A large amount of hydroxyl accelerates the electronics transfer between carrier and noble metal, by the effect of surface hydroxyl, obtains highly stable
Precious metal catalytic material.
Fig. 5 is the monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material that in the present invention prepared by embodiment 1 and embodiment 2
The active testing curve of catalytic degradation methanol, as can be seen from the figure monatomic monodisperse platinum base two-dimensional metallic hydroxide-catalyzed
Material shows excellent low-temperature methanol detergent power.Wherein Pt1-Ce(OH)xCatalysis material is achievable pair under the conditions of 106 DEG C
The removal rate of 800ppm methanol 90%.
The stability of monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material and the test of anti-poisoning capability include following side
Face:
1. the water-resistance of monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material is tested
Catalysis material after accurately weighing 0.3mL sieving is placed in the fixed bed of evaluating apparatus, is activated at 200 DEG C
1.5h, using methanol (methanol) as probe gas, the concentration of reactant is controlled in 800ppm, and reaction velocity is
36000ml·g-1h-1, oxygen concentration 20%, wait be catalyzed reaction 100 DEG C stablize after, be passed through the H of 3vol.%2O gas, holds
Catalytic reaction activity of the continuous test catalyst under mixed component atmospheric condition.H is cut off after 75min2O gas continues test and urges
Change the catalytic activity of material until stablizing.
2. the anti-CO of monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material2Shock-testing
Catalysis material after accurately weighing 0.3mL sieving is placed in the fixed bed of evaluating apparatus, is activated at 200 DEG C
1.5h, using methanol (methanol) as probe gas, the concentration of reactant is controlled in 800ppm, and reaction velocity is
36000ml·g-1h-1, oxygen concentration 20%, wait be catalyzed reaction 100 DEG C stablize after, be passed through the CO of 5vol.%2Gas is held
Catalytic reaction activity of the continuous test catalyst under mixed component atmospheric condition.CO is cut off after 40min2Gas continues test and urges
Change the catalytic activity of material until stablizing.
Fig. 6 is the monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material that in the present invention prepared by embodiment 1 and embodiment 2
Water-resistance test chart, as can be seen from Figure 6 when being passed through H in reactant composition2Catalytic activity slightly declines and works as H when O2O cutting
When monatomic catalysis material can restore starting efficiency rapidly.Confirm the monodisperse platinum base two dimension hydroxide-catalyzed material in the present invention
Material possesses stronger water-resistance.
Fig. 7 is the monodisperse platinum base two-dimensional metallic hydroxide-catalyzed material that in the present invention prepared by embodiment 1 and embodiment 2
Anti- CO2Impact property test chart, as can be seen from Figure 7 when being passed through CO in reactant composition2When catalytic activity slightly decline and
Work as CO2Monatomic catalysis material can restore rapidly starting efficiency when cutting.Confirm the monodisperse platinum base two dimension hydrogen-oxygen in the present invention
Compound catalysis material possesses stronger stability and anti-low concentration CO2Impact capacity.
Embodiment 3
By 0.27g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) be dissolved in 30mL go from
In sub- water, and continue to stir 15min with 800rpm revolving speed, forms transparent clear solution.It is added 4.0g six times into above-mentioned solution
Tetramine sufficiently dissolves under the stirring of 800rpm revolving speed.The seven chloride hydrate cerium (CeCl of 35mmoL are then added3·7H2O),
Stirring dissolves it sufficiently energetically.It is slowly added to the ethylene glycol solution of 180mL into above-mentioned acquired solution, and continues to stir
15min.And then 3mL six is added dropwise and is hydrated chloroplatinic acid-ethylene glycol solution (1.5mgPt/ mL), and turned with 800-1000rpm
Speed continues to stir 30min.Solution is placed in the three-neck flask of microwave generator, power setting 900W, by mixed solution plus
Heat is condensed back 20min to 150 DEG C and with this condition.
It is cooled to room temperature to liquid, is centrifuged under the conditions of 8000rpm, obtained solid dehydrated alcohol and deionization washing
It washs, drying at room temperature 12h, roasts 3.5h under 200 DEG C of nitrogen atmospheres in Muffle furnace, obtain monodisperse platinum base two-dimensional metallic hydroxide
Object.
Embodiment 4
By 0.27g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) be dissolved in 40mL go from
In sub- water, and continue to stir 15min with 700rpm revolving speed, forms transparent clear solution.It is added 5.3g six times into above-mentioned solution
Tetramine sufficiently dissolves under the stirring of 700rpm revolving speed.The seven chloride hydrate cerium (CeCl of 20mmoL are then added3·
7H2O), stirring dissolves it sufficiently energetically.It is slowly added to the ethylene glycol solution of 220mL into above-mentioned acquired solution, and continues to stir
Mix 15min.And then 3mL six is added dropwise and is hydrated chloroplatinic acid-ethylene glycol solution (1.5mgPt/ mL), and with 900rpm revolving speed after
Continuous stirring 30min.Solution is placed in the three-neck flask of microwave generator, mixed solution is heated to by power setting 900W
140 DEG C and it is condensed back 40min with this condition.
It is cooled to room temperature to liquid, is centrifuged under the conditions of 8000rpm, obtained solid dehydrated alcohol and deionization washing
Wash, drying at room temperature for 24 hours, roast 2h under 200 DEG C of nitrogen atmospheres in Muffle furnace, obtain monodisperse platinum base two-dimensional metallic hydroxide
Object.
Embodiment 5
By 0.27g polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer (P123) be dissolved in 45mL go from
In sub- water, and continue to stir 15min with 500rpm revolving speed, forms transparent clear solution.It is added 4.5g six times into above-mentioned solution
Tetramine sufficiently dissolves under the stirring of 500rpm revolving speed.The seven chloride hydrate cerium (CeCl of 5mmoL are then added3·7H2O),
Stirring dissolves it sufficiently energetically.It is slowly added to the ethylene glycol solution of 180mL into above-mentioned acquired solution, and continues to stir
15min.And then 3mL six is added dropwise and is hydrated chloroplatinic acid-ethylene glycol solution (1.5mgPt/ mL), and with 800-1000rpm revolving speed
Continue to stir 30min.Solution is placed in the three-neck flask of microwave generator, power setting 900W heats mixed solution
It is condensed back 20min to 150 DEG C and with this condition.
It is cooled to room temperature to liquid, is centrifuged under the conditions of 8000rpm, obtained solid dehydrated alcohol and deionization washing
It washs, drying at room temperature 12h, roasts 3.5h under 200 DEG C of nitrogen atmospheres in Muffle furnace, obtain monodisperse platinum base two-dimensional metallic hydroxide
Object.
The two-dimensional metallic hydroxide with atom level dispersion platinum site can be achieved in the present invention under conditions of microwave-assisted
The efficient green fabricated in situ of catalysis material.The purpose of the present invention is pass through microwave assisting method one-step synthesis monodisperse platinum base two dimension
Metal hydroxides is made by the feature of low Surface Polarization specific to two-dimensional metallic hydroxide and low Atomic coordinate number
It is easier active interface that " platinum-hydroxyl-carrier " is formed with monatomic noble metal active component, accelerate carrier and noble metal it
Between electronics transfer the monatomic catalysis material of highly stable noble metal is obtained, to a certain extent by the effect of surface hydroxyl
It solves the problems, such as that loaded noble metal catalyst is expensive, overcomes existing monatomic catalysis material preparation process complexity,
The technical problem of low output.Catalysis material prepared by the invention possesses the platinum active site of atom level dispersion and shows excellent
The oxygen-containing hydro carbons low-temperature purifying ability of volatility.Meanwhile process for synthetic catalyst involved in the present invention is simple, the prices of raw materials are low
It is honest and clean, there is good industrial applications prospect.
Claims (10)
1. a kind of in-situ synthetic method of monodisperse platinum base two-dimensional metallic hydroxide, which is characterized in that polyethylene oxide-is poly-
Propylene oxide-polyethylene oxide triblock copolymer is dissolved in deionized water, and stirring forms transparent clear solution；Then six are added
Methine tetramine, stirs evenly, and adds cerium salt or cobalt salt, stirs evenly, and ethylene glycol is added, is stirring evenly and then adding into six hydrations
Chloroplatinic acid-ethylene glycol solution, stirs evenly, and obtains mixed solution, then heats mixed solution in microwave generator
Back flow reaction is centrifuged after fully reacting, and roasting obtains monodisperse platinum base two-dimensional metallic hydroxide.
2. a kind of in-situ synthetic method of monodisperse platinum base two-dimensional metallic hydroxide according to claim 1, feature
It is, the ratio of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer and deionized water is 0.27g:(30-
45)mL。
3. a kind of in-situ synthetic method of monodisperse platinum base two-dimensional metallic hydroxide according to claim 1, feature
It is, polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer, hexamethylenetetramine, cerium salt, six hydration chlorine
Platinic acid-ethylene glycol solution ratio 0.27g:(4.0-5.3) g:(5-35) mmoL:3mL；Or polyethylene oxide-polypropylene oxide-
Polyethylene oxide triblock copolymer, hexamethylenetetramine, cobalt salt, six hydration chloroplatinic acid-ethylene glycol solution ratio 0.27g:
(4.0-5.3) g:(5-35) mmoL:3mL.
4. a kind of in-situ synthetic method of monodisperse platinum base two-dimensional metallic hydroxide according to claim 3, feature
It is, wherein six hydration chloroplatinic acid-ethylene glycol solution concentration are 1.5mgPt/mL。
5. a kind of in-situ synthetic method of monodisperse platinum base two-dimensional metallic hydroxide according to claim 1, feature
It is, the ratio of polyethylene oxide-polypropylene oxide-polyethylene oxide triblock copolymer and ethylene glycol is 0.27g:(180-
220)mL。
6. a kind of in-situ synthetic method of monodisperse platinum base two-dimensional metallic hydroxide according to claim 1, feature
It is, the power setting of microwave generator is 900W, and the temperature of back flow reaction is 140-150 DEG C, time 20-40min.
7. a kind of in-situ synthetic method of monodisperse platinum base two-dimensional metallic hydroxide according to claim 1, feature
It is, roasting carries out under nitrogen atmosphere, and the temperature of roasting is 200 DEG C, calcining time 2-3.5h.
8. a kind of monodisperse platinum base two-dimensional metallic hydroxide of the preparation of any one of -7 methods according to claim 1, special
Sign is, specific surface area 134.2-156.7m2/ g, Micropore volume 0.11-0.24cm3/g。
9. a kind of monodisperse platinum base two-dimensional metallic hydroxide of the preparation of any one of -7 methods according to claim 1 is volatilizing
Property the purification of oxygen-containing hydro carbons in application.
10. application according to claim 9, which is characterized in that monodisperse platinum base two-dimensional metallic hydroxide 120 DEG C,
Air speed 36000h-1, under conditions of oxygen volumetric concentration 20%, realize the deep purifying for being 0.08% to methanol volumetric concentration.
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