TWI442972B - 金-鈀承載於二氧化鈰觸媒之製法及其在去除有機氣體之應用 - Google Patents
金-鈀承載於二氧化鈰觸媒之製法及其在去除有機氣體之應用 Download PDFInfo
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- TWI442972B TWI442972B TW100144587A TW100144587A TWI442972B TW I442972 B TWI442972 B TW I442972B TW 100144587 A TW100144587 A TW 100144587A TW 100144587 A TW100144587 A TW 100144587A TW I442972 B TWI442972 B TW I442972B
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- palladium
- gold
- temperature
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- 239000003054 catalyst Substances 0.000 title claims description 75
- 238000000034 method Methods 0.000 title claims description 26
- BBKFSSMUWOMYPI-UHFFFAOYSA-N gold palladium Chemical compound [Pd].[Au] BBKFSSMUWOMYPI-UHFFFAOYSA-N 0.000 title claims description 18
- 229910000420 cerium oxide Inorganic materials 0.000 title claims description 9
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 title claims description 9
- 239000012855 volatile organic compound Substances 0.000 title description 11
- 238000002360 preparation method Methods 0.000 title description 3
- 230000006378 damage Effects 0.000 title description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 claims description 94
- 229910052763 palladium Inorganic materials 0.000 claims description 43
- 239000010931 gold Substances 0.000 claims description 30
- 229910052737 gold Inorganic materials 0.000 claims description 29
- 239000007789 gas Substances 0.000 claims description 25
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 22
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 claims description 15
- 229910001925 ruthenium oxide Inorganic materials 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000010815 organic waste Substances 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 8
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000005470 impregnation Methods 0.000 claims description 7
- 238000001354 calcination Methods 0.000 claims description 6
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 230000008021 deposition Effects 0.000 claims description 4
- 239000012153 distilled water Substances 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 4
- 229910001252 Pd alloy Inorganic materials 0.000 claims description 3
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 3
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 claims description 3
- GPNDARIEYHPYAY-UHFFFAOYSA-N palladium(ii) nitrate Chemical compound [Pd+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O GPNDARIEYHPYAY-UHFFFAOYSA-N 0.000 claims description 3
- 238000004062 sedimentation Methods 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 claims 1
- 239000002184 metal Substances 0.000 claims 1
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 67
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 18
- 238000006243 chemical reaction Methods 0.000 description 18
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- 229910002710 Au-Pd Inorganic materials 0.000 description 10
- 238000007254 oxidation reaction Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 229910010413 TiO 2 Inorganic materials 0.000 description 7
- 238000006555 catalytic reaction Methods 0.000 description 7
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 5
- 239000010970 precious metal Substances 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 3
- 239000001569 carbon dioxide Substances 0.000 description 3
- 229910002092 carbon dioxide Inorganic materials 0.000 description 3
- 238000002485 combustion reaction Methods 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011572 manganese Substances 0.000 description 3
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- 229910052760 oxygen Inorganic materials 0.000 description 3
- 229910003445 palladium oxide Inorganic materials 0.000 description 3
- 239000002957 persistent organic pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 238000001556 precipitation Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910052703 rhodium Inorganic materials 0.000 description 3
- 239000010948 rhodium Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 2
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000711 cancerogenic effect Effects 0.000 description 2
- 231100000315 carcinogenic Toxicity 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 2
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000009841 combustion method Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- -1 nitrogen-containing amines Chemical class 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000010944 silver (metal) Substances 0.000 description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 230000010718 Oxidation Activity Effects 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- 239000006004 Quartz sand Substances 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 238000007743 anodising Methods 0.000 description 1
- 229910052786 argon Inorganic materials 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical group 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007084 catalytic combustion reaction Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000005274 electronic transitions Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 150000002118 epoxides Chemical class 0.000 description 1
- 239000010436 fluorite Substances 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 238000001889 high-resolution electron micrograph Methods 0.000 description 1
- 238000001239 high-resolution electron microscopy Methods 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- SIWVEOZUMHYXCS-UHFFFAOYSA-N oxo(oxoyttriooxy)yttrium Chemical compound O=[Y]O[Y]=O SIWVEOZUMHYXCS-UHFFFAOYSA-N 0.000 description 1
- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 125000000864 peroxy group Chemical group O(O*)* 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 231100000572 poisoning Toxicity 0.000 description 1
- 230000000607 poisoning effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- MHOVAHRLVXNVSD-UHFFFAOYSA-N rhodium atom Chemical compound [Rh] MHOVAHRLVXNVSD-UHFFFAOYSA-N 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 229910052712 strontium Inorganic materials 0.000 description 1
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- JLQFVGYYVXALAG-CFEVTAHFSA-N yasmin 28 Chemical compound OC1=CC=C2[C@H]3CC[C@](C)([C@](CC4)(O)C#C)[C@@H]4[C@@H]3CCC2=C1.C([C@]12[C@H]3C[C@H]3[C@H]3[C@H]4[C@@H]([C@]5(CCC(=O)C=C5[C@@H]5C[C@@H]54)C)CC[C@@]31C)CC(=O)O2 JLQFVGYYVXALAG-CFEVTAHFSA-N 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 1
Classifications
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- B01J2235/15—X-ray diffraction
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Description
本發明揭示一種製備承載於氧化鈰擔體之金-鈀觸媒之製造方法，及一種在奈米金-鈀承載於氧化鈰觸媒催化下，在空氣中有機廢氣與氧氣反應以去除有機廢氣之方法；本發明以含有金-鈀/氧化鈰觸媒在有機廢氣於空氣中，使用填充床反應器，以去除有機廢氣。
近年由於工業發展迅速帶動經濟成長，相對也造成環境的污染，特別是半導體產業在製造過程中易造成大量揮發性有機物(Volatile Organic Compounds,VOCs)逸散於空氣中，伴隨而來的污染是業界無法避免的課題。VOCs是指含碳(C2
~C6
)之非甲烷碳氫的揮發物質，如苯、甲苯、含氮之胺類等等，在正常情況下，沸點在250℃以下。而VOCs大部分屬於有害性空氣污染物，人體長期曝露於VOCs的環境中，即使在低濃度下，也會產生中毒或致癌性腫瘤等現象。此外，大氣中的VOCs具高度光化學活性，經由紫外光照射產生臭氧、PAN(peroxy acethyl nitrate)、PBN(peroxy benzene nitrate)等高氧化性污染物，對人體的刺激性與危害性甚劇，因此，如何降低這些污染物對環境及人體的傷害，是研究者須努力的目標。
VOCs的處理方法大致可分為以下兩種：一為去除，它包括高溫與觸媒氧化或還原，以及生物濾床法，在此機制下將有機污染物轉化為二氧化碳和水；另一為回收，利用吸收、吸附、冷凝與薄膜分離等方法，將污染物自排放廢氣中轉移或回收，使其成為乾淨氣體。早期對VOCs大多使用高溫燃燒法處理，且在氧氣充足、溫度和反應時間均足夠時，任何碳氫化合物皆可經由燃燒過程而氧化成二氧化碳和水，惡臭的氣體均能經燃燒成為無味無害的氣體，而排放至大氣中，但有機揮發性氣體種類繁多，各種氣體燃點不同，因此以燃燒方式處裡有機揮發性氣體所需達到的爐內溫度亦不
同，若有多種有機揮發性氣體混合，操作溫度及條件則更加複雜，一般直燃爐的操作溫度需達攝氏七百到九百℃甚至更高才能去除大部份的VOCs，但加熱同時也需耗去大量能源(電熱、柴油)，因此造成處理成本的增加。所以目前工業上大多採用觸媒燃燒法去除VOCs，觸媒燃燒法比直接燃燒法的優點為：(1)可低溫處理有機污染物(2)能源效率高(3)產物對環境無污染(產物為二氧化碳和水)。
處理有機污染物之觸媒主要分為(1)低活性但是價位便宜的金屬氧化物(CuO、Cr2
O3
、MnOx
、V2
O5
)及(2)高活性，但是價位也高的貴重金屬(Pt、Rh、Pd、Ag、Au)，本報告選擇鈀觸媒是因為相較於其他貴重金屬(Pt、Ag、Au、Rh)，鈀觸媒擁有(1)較低價格，(2)好的氧化活性，(3)高溫耐久性。鈀為貴重金屬，原子序46，週期表上和鉑、鎳同族，與銠、銀同列，鈀是一種過渡金屬，灰白色，延展性極好，易於加工，其性質像鉑，但比鉑系金屬中其他元素更易受酸腐蝕，鈀的熔點達1828K，可耐高溫。擔體觸媒的研究是觸媒催化反應中極為重要的主題，藉由擔體的支撐可以增加觸媒活性成分的表面積，改變觸媒的性質，增加反應的活性及選擇性，大大降低貴重金屬觸媒的製備成本。
甲苯是一種澄清、無色的液體，具有明顯的味道，與苯同為芳香族碳氫化合物，在現今實際應用中常常代替有相當毒性的苯作為有機溶劑使用，他的許多性質跟苯很相像，但與苯的氧化反應不同，甲苯的氧化反應並不在苯環上，而在甲基上發生。因此甲苯的氧化產物中只有極少量在苯的氧化反應中經常出現的副產品(具有強致癌性的環氧化物)。Wu等人[Catalysis Today，第63卷(2000)第419頁至426頁]發現以活性碳作為擔體的白金觸媒，可將甲苯完全氧化於低溫200℃以下，其中活性碳可於氮氣流中加熱至400℃或800℃，並且用氫氟酸清洗去除表面雜質或礦物質。Luo等人[Applied Catalysis B：Environmental，第69卷，2007，第213頁至218頁]以CeO2
-Y2
O共氧化物做為擔體製備鈀觸媒，並將觸媒以水洗塗佈附著於蜂窩狀陶瓷上，發現以500℃鍛燒的觸媒可於210℃將甲苯完全氧化，觸媒除了要活性好之外其耐久性也是很重要的因素，研究者將觸媒在200至240℃之間重複升溫降溫10℃共8次，在此30小時內發現觸媒活性並無明顯的改變，顯示出其重複性與穩定性。Hosseini[Catalysis Today，第122卷2007，第391頁至396頁]等人則分別利用沉積沉澱法與含浸法，將金與鈀擔載於具多孔性結構的高表面積二氧化鈦擔體上，其活性順序為0.5%Pd-1%Au/TiO2
>1.5% Pd/TiO2
>0.5% Pd/TiO2
>1% Au-0.5% Pd/TiO2
>1% Au/TiO2
>TiO2
，活性最佳的0.5%Pd-1%Au/TiO2
能在230℃將甲苯完全氧化。Liu等人[Journal of Hazardous Materials，第149卷，2007，第742頁至746頁]將氧化鋁與利用共沉澱法製備的二氧化鈰與二氧化鋯共氧化物做為混合擔體，並摻雜釔與錳做為添加物，利用含浸法製備白金觸媒，實驗證明以釔與錳做為添加物的Pt/γ-Al2
O3
/Ce0.4
Zr0.4
Y0.1
Mn0.1
Ox觸媒有較高的活性，於216℃時甲苯完全氧化的轉化率能達到90%。Zheng等人[Catalysis Communications，第9卷(2008)，第990頁至994頁]利用不鏽鋼作為擔體，以陽極氧化程序做製備，並且鍛燒於1000℃下，可得活性最佳觸媒，對甲苯完全轉化溫度為210℃。Qingbao等人[Chinese Journal of Catalysis，第29卷(2008)，第373頁至378頁]利用ZrO2
易於交換氧原子的四方相以及耐磨損、耐高溫、耐腐蝕等特性，將之與CeO2
做適當比例的結合，結果顯示以Pd/Ce0.8
Zr0.2
O2
/substrate單石型觸媒，鍛燒溫度於400℃，反應溫度為210℃下可得97%的甲苯轉化率。
國內現有的專利，公開號200304850揭露一種利用冷卻冷凝技術的有機廢氣之處理方法及裝置，美國專利5753583揭露一種鈀觸媒之製造方法。由已公開專利中，未有如本發明所揭示利用奈米金-鈀觸媒承載於氧化鈰，應用在有機廢氣去除的方法。
本發明揭示一種製備承載於氧化鈰擔體之金-鈀觸媒之製造方法，及一種在奈米Au-鈀承載於氧化鈰之觸媒催化下，在空氣中有機廢氣與氧氣反應以去除有機廢氣之方法。本發明以含有金-鈀/氧化鈰觸媒在有機廢氣於空氣中，使用填充床反應器，以去除有機廢氣。本發明使用初濕含浸法將硝酸鈀水溶液含浸在二氧化鈰擔體觸媒上，在200至500℃之間任一溫度煅燒2至10小時，將鈀觸媒於60至200℃之間任一溫度先通氮氣以去除水氣，再通氫氣於300至400℃之間任一溫度還原2小時；利用沉積沉澱的方法將金負載在上述製備完成之鈀觸媒上，稱取欲配製之等重之四氯金酸，金的含量為重量百分比0.1至1wt.%，配成濃度為1至4M的四氯金酸溶液，將其以每分鐘5至20毫升的速率滴入均勻混合的鈀觸媒中，用氨水控制酸鹼值在6至8之間，並控制其溫度在50至80℃之間任一溫度熟化1至4小時，其後將濾餅過濾出來，用50至60℃之間任一溫度蒸餾水洗去氯離子，並用1M硝酸銀溶液測試其濾液至不會產生白色沉澱為止。再於60至100℃之間的任一溫度乾燥2至20小時，於100至200℃之間之任一溫度煅燒1至8
小時，即可得到奈米金-鈀觸媒。
使用初濕含浸法將硝酸鈀水溶液含浸在二氧化鈰擔體觸媒上，在200至500℃之間任一溫度煅燒2至10小時，將鈀觸媒於60至200℃之間任一溫度先通氮氣以去除水氣，再通氫氣於300至400℃之間任一溫度還原2小時；利用沉積沉澱的方法將金負載在上述製備完成之鈀觸媒上，稱取欲配製之等重之四氯金酸，金的含量為重量百分比0.1至1wt.%，配成濃度為1至4M的四氯金酸溶液，將其以每分鐘5至20毫升的速率滴入均勻混合的鈀觸媒中，用氨水控制酸鹼值在6至8之間，並控制其溫度在50至80℃之間任一溫度熟化1至4小時，其後將濾餅過濾出來，用50至60℃之間任一溫度蒸餾水洗去氯離子，並用1M硝酸銀溶液測試其濾液至不會產生白色沉澱為止。再於60至100℃之間的任一溫度乾燥2至20小時，於100至200℃之間之任一溫度煅燒1至8小時，即可得到奈米金-鈀觸媒。
以初濕含浸法製備Pd/CeO2
觸媒，其中擔體由Nikki公司取得之氧化鈰使用初濕含浸法將硝酸鈀水溶液含浸在二氧化鈰擔體觸媒上，在400℃煅燒6小時，將鈀觸媒於100℃先通氮氣以去除水氣，再通氫/氬混合氣以50ml/min之速率於300℃還原2小時；利用沉積沉澱的方法將金負載在上述製備完成之鈀觸媒上，稱取欲配製之等重之四氯金酸(1wt.%Au)，配成濃度為2.25×10-3
M的金溶液，將其以每分鐘10毫升的速率滴入200毫升均勻混合的鈀觸媒中，用28%氨水控制酸鹼值在7，並控制其溫度在65℃熟化2小時，其後將濾餅過濾出來，用50-60℃蒸餾水洗去氯離子，並用1M硝酸銀溶液測試其濾液至不會產生白色沉澱為止，再以80℃乾燥16小時，200℃煅燒4小時，即可得到金-鈀觸媒。
由X光粉末繞射峰，可利用其半高寬求得鈀顆粒在擔體上的平均大小及擔體晶粒大小。經JCPDS資料庫找出CeO2
的主要特徵峰2θ為28.6°(111)，及數個較小之特徵峰為33.1°(200)、47.5°(220)56.3°(311)及59.1°(222)比對後，得知氧化鈰為Fluorite立方體心結構，圖1顯示引入不同含量的金至Pd/CeO2
觸媒於180℃鍛燒溫度鍛燒4小時，圖中並未觀察到金之繞射峰(2θ=38.2°、44.4°、64.6°、77.5)°，證實金均勻的分散在氧化鈰擔
體上，或是金顆粒小於XRD偵測極限4奈米。
從XRD圖譜可觀察到擔體皆為結晶良好的二氧化鈰，XRD分析圖譜中偵測不到鈀及金的波峰，代表鈀與金的顆粒太小，小於儀器的偵測限制(4奈米)。
高解析度電子顯微鏡圖中則可看出鈀粒子在氧化鈰擔體上，粒徑約為2奈米，適當地將金引入鈀/氧化鈰觸媒中，會有部分金鈀合金的形成，可有效降低甲苯完全轉化溫度
由X-光光電子能譜儀可求知鈀觸媒中鈀粒子的鍵結能。其中所有圖譜皆用Cls
的鍵結能284.5eV做校正。0.5N-wt.% Pd/CeO2
鍛燒400℃ 8小時觸媒的鈀束縛能偏移比其他高，表示鈀和CeO2
表面之間有很強的金屬與擔體交互作用力，可以增加鈀的穩定性，進而提高觸媒的活性。若將訊號峰值作解析，鈀主要參考其3d5/2
及3d3/2
兩個軌域的電子躍遷，其中元素態位置在336.5eV及341.6eV；二價鈀的鍵結能位於337.8eV及343.4eV，XPS分析可取得Pd/CeO2
觸媒上鈀的表面狀態，由圖2可發現將金引入鈀/氧化鈰觸媒後，Pd 3d5/2
波峰會往低束縛能方向偏移；由圖3可發現將金引入鈀/氧化鈰觸媒後，Au 4f7/2
波峰會往高束縛能方向偏移。金、鈀束縛能相反方向的偏移，是因為部分的金、鈀會形成合金。
將Au-Pd/CeO2
觸媒置於填充反應床反應器內，進行在空氣中完全氧化有機廢氣的反應，以連續式觸媒填充床反應器進行實驗；控制流量，並在190℃下，進行反應。
將觸媒置於U型觸媒填充反應床內，進行在空氣中氧化甲苯的反應，以連續式觸媒填充床反應器進行實驗；控制流量為每分鐘40毫升，在室溫下通入反應器中，管子內外直徑為0.9公分及1.3公分，長度21公分，中間有0.5公分之融熔石英砂，以擔載反應之觸媒，但可以透氣；秤取觸媒重量0.2g置入U型石英管中，甲苯的飽和器置水浴中控制溫度為30℃，觸媒反應溫度由室溫升溫至250℃，以4℃/min的速率升溫5分鐘後，到達反應溫度時，控制在此溫度，10分鐘後進行反應測試；進料流速經由流量
控制器控制，先以少量空氣經裝有進料甲苯的錐形瓶帶出進料的蒸氣後，再藉由另一空氣稀釋調整進料濃度，通過U型觸媒填充反應床，反應後的氣體流經氣相層析儀，再由火焰游離偵測器分析，反應結果如圖4所示，其中甲苯轉化率定義如下：甲苯轉化率=(進口甲苯濃度-出口甲苯濃度)÷進口甲苯濃度。
由這些結果證實本發明之觸媒能於190℃能有效去除空氣中之甲苯。金引入鈀觸媒的量對甲苯完全氧化反應之結果如圖4所示。僅需0.1wt.%的金即可提高觸媒活性，於180℃煅燒下即可獲得活性最佳之金-鈀觸媒觸媒，可於190℃將甲苯完全轉化。
圖1. XRD圖譜(a)Pd/CeO2
(b)0.1wt.% Au-Pd/CeO2
(c)0.5wt.% Au-Pd/CeO2
(d)1.0wt.% Au-Pd/CeO2
.
圖2. XPS Pd 3d圖譜(a)Pd/CeO2
(b)0.1wt.% Au-Pd/CeO2
(c)0.5wt.% Au-Pd/CeO2
(d)1.0wt.% Au-Pd/CeO2
.
圖3. XPS Au 4f圖譜(a)0.1wt.% Au-Pd/CeO2
(b)0.5wt.% Au-Pd/CeO2
(c)1.0wt.% Au-Pd/CeO2
(d)1.0wt.% Au/CeO2
.
圖4. 引入不同比例的金對甲苯完全氧化反應之影響
Claims (3)
- 一種承載於氧化鈰之金-鈀觸媒，金的含量為重量百分比0.05至1wt.%，鈀的含量為重量百分比0.5wt.%；其中金屬包含金-鈀合金，其粒徑小於10nm；用於承載金-鈀之氧化鈰顆粒，其比表面積大於100m2 /g。
- 一種承載於氧化鈰之金-鈀觸媒的製造方法，使用初濕含浸法將硝酸鈀水溶液含浸在二氧化鈰擔體觸媒上，在200至500℃之間任一溫度煅燒2至10小時，將鈀觸媒於60至200℃之間任一溫度先通氮氣以去除水氣，再通氫氣於300至400℃之間任一溫度還原2小時，利用沉積沉澱的方法將金負載在上述製備完成之鈀觸媒上，稱取欲配製之等重之四氯金酸，金的含量為重量百分比0.1至1wt.%，配成濃度為1至4M的四氯金酸溶液，將其以每分鐘5至20毫升的速率滴入均勻混合的鈀觸媒中，用氨水控制酸鹼值在6至8之間，並控制其溫度在50至80℃之間任一溫度熟化1至4小時，其後將濾餅過濾出來，用50至60℃之間任一溫度蒸餾水洗去氯離子，並用1M硝酸銀溶液測試其濾液至不會產生白色沉澱為止，再於60至100℃之間的任一溫度乾燥2至20小時，於100至200℃之間之任一溫度煅燒1至8小時，即可得到奈米金-鈀觸媒。
- 一種去除空氣中含有有機廢氣的方法，其係以含有金-鈀承載於氧化鈰之觸媒，在空氣中，於200至400℃之間之任一溫度下反應，使空氣中有機廢氣完全氧化，觸媒為申請專利範圍第1.項之承載於氧化鈰之金-鈀觸媒。
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| TW100144587A TWI442972B (zh) | 2011-12-05 | 2011-12-05 | 金-鈀承載於二氧化鈰觸媒之製法及其在去除有機氣體之應用 |
| US13/444,165 US20130142720A1 (en) | 2011-12-05 | 2012-04-11 | The method of preparation of cerium oxide supported gold-palladium catalysts and its application in destruction of volatile organic compounds |
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| TW100144587A TWI442972B (zh) | 2011-12-05 | 2011-12-05 | 金-鈀承載於二氧化鈰觸媒之製法及其在去除有機氣體之應用 |
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| TWI458549B (zh) * | 2012-01-13 | 2014-11-01 | Univ Nat Central | 奈米金－銀承載於二氧化鈰觸媒之製法及其在去除空氣中一氧化碳之應用 |
| KR101964275B1 (ko) * | 2015-09-01 | 2019-04-01 | 주식회사 엘지화학 | 아크릴산 제조용 촉매 제조방법 및 이로부터 제조되는 촉매 |
| CN114308029B (zh) * | 2020-09-30 | 2023-01-13 | 中国科学院大连化学物理研究所 | 采用双金属催化剂进行肼还原六价铀制备四价铀的方法 |
| CN113042048B (zh) * | 2021-03-23 | 2024-01-30 | 江苏三一环境科技有限公司 | 一种VOCs治理催化剂及其制备方法与应用 |
| CN113262801A (zh) * | 2021-05-31 | 2021-08-17 | 中国科学院兰州化学物理研究所 | 一种Ce-Mn基固溶体催化剂及其制备方法和应用 |
| CN113797958A (zh) * | 2021-10-19 | 2021-12-17 | 浙江师范大学 | 一种处理含氮有机物的催化剂及其制备方法 |
| CN114713221B (zh) * | 2022-04-25 | 2023-12-08 | 南京工业大学 | 一种用于VOCs处理的高效抗硫中毒催化剂的制备方法 |
| CN115069244A (zh) * | 2022-05-05 | 2022-09-20 | 有研工程技术研究院有限公司 | 一种微孔铈镧固溶体负载Pd-Ag催化剂及其应用 |
| CN115160324A (zh) * | 2022-07-13 | 2022-10-11 | 西安近代化学研究所 | 一种单原子钯催化hbiw氢解脱苄合成tadb的方法 |
| CN115845845B (zh) * | 2022-11-21 | 2024-07-23 | 北京沐秀新能源科技有限公司 | 一种用于低品质油田伴生气无焰燃烧的催化剂及其制备方法与应用 |
-
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| US20130142720A1 (en) | 2013-06-06 |
| TW201323082A (zh) | 2013-06-16 |
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