1. 1 M oo 3-TiO 2gSiO 2. Perk in E lm er2l am bda 35 UV 2V is Spectrom eter : E2m ail: tp ṫ tj. cn
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1 V ol. 25 N o CHEM ICAL JOU RNAL O F CH IN ESE UN IV ERS IT IES M oo 3-TiO 2gSiO 2,,,,, (, ) M oo 32T io 2gSiO 2, XRD, BET, TPR, IR, UVDR S TPD,,,, ; T io 2 SiO 2 M oo 3,,. 100, 2 2, M oo 32T io 2gSiO 2, 85. 6%. M oo 32T io 2gSiO 2; ; ; O 643 A (2004) ,,. CH 4 H 2O, [1 ] ;,, [2 ] ; M oo 3gSiO 2 [3 ] 0. 23% M oo 32 T io 2 [4 ] 2,. M oo 32T io 2gSiO 2, [5 ] (PSSCR ), M oo 32T io 2gSiO 2, M oo 3-TiO 2gSiO 2 ( 3050, ), h. 5. 3% T io 2gSiO 2 [6 ] ( g T io 2 g SiO 2, g T io 2g g SiO 2) [7 ], T io 2gSiO 2,, h, M oo 32T io 2gSiO 2. M oo % [ g M oo 3 g (T io 2gSiO 2), g M oo 3 g (T io 2gSiO 2) ] X (Cu K Α, 36 kv, 20 ma ) ; Q uantach rom CH EM BET 3000 (BET ) ; T PR : 6%H 2294%N 2 ( ), 40 ml gm in, 8 gm in, 900, 200 m g. Perk in E lm er2l am bda 35 UV 2V is Spectrom eter : nm,, nm, 240 nm gm in UVDR S. H i2 : : (: 2001CCAO 23600). : (1938 ),,,,. E2m ail: shzhong@public. tp ṫ tj. cn
2 V ol. 25 tach i IR :, ( Pa),,, CH h, (10-1 Pa),. CKW 2g L ZL 2203 T PD 2M S : 500 m g g 6 mm U, 350, Pa 2 h,, 20 ml,, Pa,, 8 gm in ml (1. 3 kpa, 200, 2 h) 9 ml, ( 1 ), CH 4 (> 99. 9% ), ( N 2 ), [ 300 W (GGZ ) ],,, Perk in2e lm er A utosystem XL Gas Ch rom atograph M oo 3-TiO 2gSiO 2 F ig. 1Schema tic diagram of photoca ta lytic reactor. M oo 32T io 2gSiO 2 XRD M oo 3 T io 2,, M oo 3 T io 2 SiO 2,. 1,,,. Table 1Spec if ic surface area of ca ta lysts and support Samp le SiO 2 T io 2gSiO 2 M oo 3gSiO 2 M oo 32T io 2gSiO 2 SBETg(m 2 g - 1 ) a, 900, T io 2gSiO 2, T io 2 SiO 2. M oo 3gSiO 2 (2 b), M oo 32T io 2gSiO 2 (2 c) 500,, 810, ( Im ). M oo 3 SiO 2, M oo 3 SiO 2, SiO 2 T io 2, SM S I T io 2, M oo 3. T io 2 M oo 3 SiO 2, Im Pm. M oo 32T io 2g SiO 2 IR (3 b), SiO 2 T i (721 cm - 1 ), cm
3 N o. 6 : M oo 32T io 2gSiO 2 M o O M oo M o [9 ] ; 785 cm - 1 M oo 3 T io 2 M oo T i.,, M oo 32T io 2g SiO 2 M oo 3gSiO 2,. 2. 2M oo 3-TiO 2gSiO 2 4, nm, SiO 2, nm. T io 2 M oo 3, T io 2gSiO 2 M oo 3g SiO 2,,. M oo 32T io 2gSiO 2, (M oo T i),. T io 2gSiO 2, M oo 32 T io 2gSiO 2, M o T i( ) T io F ig. 4UV-V is diffusion ref lectance spectra of ca ta lysts. 365 nm (), T io 2gSiO 2 57%, M oo 32T io 2gSiO 2 34%, M oo 3 T io 2gSiO 2 T io nm., T io 2 M oo 3 SiO M oo 3-TiO 2gSiO 2 H2O CH4,., H 2O, T io 2. 5 M oo 32T io 2gSiO 2 H 2O CH 4 T PD. 5 (A ), H 2O 2,,., H 2O M oo 3gSiO 2, T io 2gSiO 2., H 2O,, CH 4. F ig. 5TPD curves of H2O (A) and CH4 (B) from M oo 3-TiO 2gSiO 2 (a), M oo 3gSiO 2 (b) and TiO 2gSiO 2 (c) 3 c, CH 4 M oo 32T io 2gSiO 2, cm - 1,. CH 4, CH 4, M oo 32T io 2gSiO 2, CH 4, CH 4. 5 (B ), CH 4 M oo 32T io 2gSiO 2 2, CH 4 2. CH H L ew is, L ew is. M oo T i, M o O, L ew is, CH 4, CH 4,, CH 4 M oo T i 1117
4 V ol. 25. CH 4 M o O M oo T i (3 c). M oo 3g SiO 2 2 CH 4,,, T io 2gSiO 2, CH 4. M oo 32T io 2gSiO 2 CH M oo 3-TiO 2gSiO 2 2., m in, CH 3OH H 2., 1 200, rgm,,,. T io 2gSiO 2 M oo 3gSiO 2, M oo 32 T io 2gSiO 2, CH 3OH 85. 6%, H 2., %. Catalyst Table 2Photo stimula ted surface ca ta lytic reaction s and con trol tests a Conversion of CH 4 (% ) Yieldgmol H 2 CH 3OH C2H 6 Catalyst b Not detected Not detected Not detected 5 CH3 OH (% ) T io 2gSiO 2 c Not detected M oo 3gSiO 2 c T race M oo 32T io 2gSiO 2 c (85. 6% ) d 1. 8 (14. 4% ) d a. t= 100, stock gas: n (CH 4) n (H 2O ) n (N 2) = 328; b. w ithout irradiation: 90 m in; c. irradiation: 90 m in; UV irradia2 tion: 300 W UV high p ressure Hg2lamp, photon num ber: einsteings at 365 nm; d. selectivity in parentheseṡ , 100.,,, 100 rgm, rs m,., CH 4 CH 4,,.,,, ,,. M oo 3 T io 2 [10, 11 ] (6), M oo 3 T io 2,. SiO 2, M oo 3 T io 2,,,,., CH 4 F ig16 Schema tic diagram of conduction and va lence ev, M oo 3 band energy levels of M oo 3 and TiO 2 and HOMO, CH 4 M o energy level of CH4, T PD IR. M o M oo -, CH 4 CH O - Ρ, CH, L ew is M o 6+ CH 3 OH., H 2O L ew is T i n+ L ew is T io - ; CH 3 CH 3OH,, H + H 2. 7., 2 2,, M oo 3gSiO 2 T io 2gSiO 2, M oo 32 T io 2gSiO
5 N o. 6 : M oo 32T io 2gSiO 2 F ig. 7M echan ism of photo stimula ted ca ta lytic surface reaction over M oo 3-TiO 2gSiO 2 [ 1 ]O gura K., Kataoka M.. J. M ol. Catal. [J ], 1988, 43: [ 2 ]Taylor C. E., Noceti R. P.. Catalysis Today[J ], 2000, 55: [ 3 ]W ada K., Yoshida K., W atanable Y. J.. Chem. Soc. Faraday T ranṡ [J ], 1995, 91 (11) : [ 4 ]Chen X. H., L i S. B.. Chem. L etṫ [J ], 2000, 340 (4) : [ 5 ]CHEN Song2Zhe(), ZHON G Shun2He (). Chem. J. Chinese U niversities( ) [J ], 2003, 24 (1) : [ 6 ]ZHON G Shun2He(), WAN G J ie2hui(), KAN G Q ing2hua () et al.. Petroleum Chem ical Engineering ( ) [J ], 1993, 22 (5) : [ 7 ]DEN G Cun (), DUAN L ian2yun (), XU Xian2P ing () et al.. J. Catal. ( ) [J ], 1992, 14: [ 8 ]A rena F., Parm aliana A.. J. Phyṡ Chem. [J ], 1996, 100: [ 9 ]Desikan A. N., Huang L., O yam a S. T.. J. Phyṡ Chem. [J ], 1991, 95: [ 10 ]M ehandru S. P., A nderson A. B., B razdil J. F. et al.. J. Phyṡ Cbem. [J ], 1987, 91: [ 11 ]WAN G Chuan2Yi(), L IU Chun2Yan (), SHEN Tao (). Chem. J. Chinese U niversities( ) [J ], 1998, 19 (14) : Photo Stimulated Surface Catalytic Syn theses of M ethanol and Hydrogen from M ethane and Water over M oo 3-TiO 2gSiO 2 SAN G L i2x ia, ZHON G Shun2H e 3, X IAO X iu2fen, WAN G X i2t ao, TAN J ian2h ua, ZHOU Zh i2q uan (Colleg e of Chem ical E ng ineering and T echnolog y, T ianj in U niversity, T ianj in , China) AbstractT io 2gSiO 2 w ere p repared by the chem ical modification reaction on SiO 2, and M oo 32T io 2gSiO 2 w ere p repared by isovolum etric imp regnation of T io 2gSiO 2. Based on the characterization of XRD, BET, T PR, UVDR S, IR and T PD, the surface species of supported n2p coup led sem iconductors (M oo 32T io 2g SiO 2) are w ell2dispersed, w h ich have the quantum size effects and m ake the photo absorp tion th reshold blue2sh ifting. T he experim ents also confirm ed that the incorporation of T io 2 can not only enhance the in2 teraction betw een M oo 3 and supports but also imp rove photo absorp tion p roperty. In addition, the reac2 tan ts CH 4 and H 2O can be adso rbed and activated effectively. T he gas2phase pho tocatalytic p roduction of CH 3OH and H 2 from CH 4 and H 2O w as perform ed in the p resence ofm oo 32T io 2gSiO 2 at 100 by using a fixed2bed annular pho to reacto r under U V irradiation, w ith a selectivity of CH 3OH being 85. 6%. T he photo2surface2therm alsynergistic action can be form ed at the reaction temperature, w h ich accelerated the photocatalytic reaction. A nd the reaction m echanism w as p roposed. KeywordsM oo 32T io 2gSiO 2; M ethane; M ethanol; Photo2catalysis (Ed. : V, X) 1119
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