394 2011 12 ( ) J. Jianghan Univ. (Nat. Sci. Ed.) Vol.39 No.4 Dec. 2011 Mg 3 (VO 4 ) 2 * 430056 Mg 3 VO 4 2 1. 2 1 ph 4. 8 550 C 6 h Mg 3 VO 4 2 110 nm 450 2 1 0. 107 mol/h 6. 4% Mg3 VO4 2 O643.3 A 1673-0143 2011 04-0023-05 0 Noyori 1 2 3 Mg3 VO4 2 4 6 Mg3 VO4 2 7 8 9 10 11 Mg3 VO4 2 12 14 Mg3 VO4 2 BET XRD SEM 1 1.1 Mg3 VO4 2 Mg NO 3 2 6H 2O NH 4VO 3 Mg V3 2 70 ph 1 h70 70 120 2 h 400 18h 6h0.5 /min 20 ~ 40 Mg3 VO4 2 1.2 Micromeritics ASAP2010 190 133.32 Pa 6 h BET XRD Rigaku D/MAX 2550 X 2011 05 23 (1973 ) * (1971 ) E-mail:guoxianyu828@yahoo.com.cn
24 39 JCPDS-ICDD SEM Philips XL 30 20 kv 3 000 20 000 1.3 9 mm400 mm 500 mg 1 4 ± 0. 5 30 mm 500 50 ml/min 60 min 450 100 ml/min 0. 2 ml/min 1. 5 h ± 3 % PEG 20000 HP 6890 2 2.1 ph 10 3.13 10 4.76 10 6.40 ph 15 1 Mg 2+ ph 4. 76 ~ 6. 40 C6H6O7 2 ph 10 3 mol/l 16 ph 2.0 6. 0 8 V10O28 6 x x OH x H2VO4 8 4 VOx n n ph 9.0 V 5 5O 15 4 V4O12 V3O9 3 8 M.Tsaramyrsi 17 ph 4. 0 NH4 + NH4 2 VO2 C6H6O7 24 4 1 ph Mg 3 VO 4 2 ph ph 4.8 ph Mg 3 VO 4 2 ph / % / % / % 2 C 6H 8O 7 14. 0 36.0 5. 0 3. 2 C 6H 7O 7 14. 9 36.2 5. 4 4. 8 C 6H 6O 7 2 6. 5 C 6H 5O 7 3 15. 5 41.5 6. 4 16. 6 33.5 5. 6 550 6 h1 1.2 2.2 R Mg3 VO4 2 1 0. 5 SEM 1 (a) Mg3 VO4 2 V2O5 MgO 1. 2 1 (b) 1 (c) 18 2 Mg 3 VO 4 2
2011 4 Mg 3 (VO 4 ) 2 25 (a) (b) (c) 550 6 h (a) 2 1 (b) 1 1.2 (c) 1 2. 1 Mg 3 VO 4 2 2 R 1. 2 Mg3 VO4 2 2 Mg 3 VO 4 2 R / nm / % / % / % 0. 5 110 19. 2 32.1 6. 2 1. 2 110 15. 5 41.5 6. 4 2. 0 130 10. 6 48.0 5. 1 2.3 2 Mg3 VO4 2 XRD 500 Mg 3 VO 4 2 XRD Mg3 VO4 2 3 500 550 / 3 Mg 3 VO 4 2 2 / 6 h 1 1. 2 a. 500 b. 550 c. 600 d. 650. / m 2 g 1 / % / % / % 500 26. 7 20.4 25. 7 5. 2 550 17. 5 15.5 41. 5 6. 4 600 14. 2 13.4 38. 4 5. 1 650 12. 0 10.6 41. 6 4. 4 2 10 20 30 40 50 60 70 80 Mg 3 VO 4 2 XRD 2.4 Mg 3 VO 4 2 XRD 3 4 h 8 h 4
26 39 4 / h Mg 3 VO 4 2 / % /% /% 4 16. 0 37. 0 5. 9 5 15. 6 39. 8 6. 2 6 15. 5 41. 5 6. 4 7 15. 6 39. 2 6. 1 8 14. 9 35. 1 5. 2 3, Mg3 VO4 2 1. 2 ph 4. 8 550 6 h 110 nm Mg3 VO4 2 450 2 1 0. 107 mol/h 15. 5% 41. 5% 6. 4% 10 20 30 40 50 60 70 80 2 / 550 1 1. 2 1 4 h, (2) 5 h, (3) 6 h, (4) 7 h 5 8 h. 3 Mg 3 VO 4 2 XRD [1] Schuchardt U, Cardoso D, Sercheli R,et al. Cyclohexane oxidation continues to be a challenge [J]. Appl Catal A: General, 2001, 211(1): 1-17. [2] Liu S C, Liu Z Y, Wang Z, et al. Characterization and study on performance of the Ru-La-B/ZrO 2 amorphous alloy catalysts for benzene selective hydrogenation to cyclohexene under pilot conditions[j]. Chem Eng J, 2008, 139(1): 157-164. [3] Rias M, Mikhail S. Dehydrogenation of cyclohexane over molybdenum mixed oxide catalysts[j]. Catal Comm, 2008, 9(6): 1398-1403. [4] Jin M, Cheng Z M, Gao Y L, et al, Oxidative dehydrogenation of cyclohexane with Mg 3 (VO 4 2 synthesized by the citrate process [J]. Mater Lett, 2009, 63(23): 2055-2058. [5] Elomestnykh I P, Isaguliants G V. V-Mg-O catalysts for oxidative dehydrogenation of alkylpyridines and alkythiophenes[j]. Catal Today, 2009, 142(3/4): 192-195. [6] Mishakov I V, Vedyagin A A, Bedilo A F, et al. Aerogel VOx/MgO catalysts for oxidative dehydrogenation of propane[j]. Catalysis Today, 2009, 144(3/4):278-284. [7] Balderas-Tapia L, Hernández-Pérez I, Schacht P, et al. Influence of reducibility of vanadium-magnesium mixed oxides on the oxidative dehydrogenation of propane[j]. Catal Today, 2005, 107/108: 371-376. [8],,,. V-Mg-O [J]., 2001, 15(3): 230-235. [9] Klisi ska A, Loridant S, Grzybowska B et al. Effect of additives on properties of V 2O 5/SiO 2 and V 2O 5/MgO catalysts II. Structure and physicochemical properties of the catalysts and their correlations with oxidative dehydrogenation of propane and ethane [J]. Appl Catal A: General, 2006, 309: 17-27. [10] Blanco S, Garrazan S R G, Rives V. Oxidative dehydrogenation of propane on Mg-V-Al mixed oxides [J]. Appl Catal A:General, 2008, 342(1/2):93-98. [11] Chaar M A, Patel D, Kung M C, et al. Selective oxidative dehydrogenation of butane over V-Mg-O catalysts [J]. J Catal 1987, 105: 483-498. [12] Gao X T, Ruiz P, Xin Q, et al. Effect of coexistence of magnesium vanadate phases in the selective oxidation of propane to propene [J]. J Catal, 1994, 148(1): 56-67. [13] Gao X T, Ruiz P, Xin Q. Preparation and characterization of three pure magnesium vanadate phases catalysts for selective oxidation of propane to propene[j]. Catal Lett, 1994, 23: 321-337. [14] Jin M, Cheng Z M. Oxidative dehydrogenation of cyclohexane to cyclohexene over Mg-V-O catalysts [J]. Catal Lett, 2009, 131(1/2): 266-278. [15]. Mg-V-O [D].,2010. [16] Blangenois N, Florea M, Grange P. Influence of the co-precipitation ph on the physico-chemical and catalytic properties of vanadium aluminum oxide catalyst [J]. Appl Catal A: General, 2004, 263: 163-170. [17] Tsaramyrsi M, Kavousanaki D, Raptopoulou C P. Systematic synthesis, structural characterization, and reactivity studies of vanadium(v) citrate anions VO 2 C 6H 6O 7 22 isolated from aqueous solutions in the presence of different cations [J]. Inorg Chim Acta, 2001, 320: 47-59. [18],,. - NiO/Ce 0.8 Gd 0.2 O 1.9 [J]. :, 2006, 36(B03): 79-84.
2011 4 Mg 3 (VO 4 ) 2 27 Oxidative Dehydrogenation of Cyclohexane with Mg 3 VO 4 2 Prepared by Citric Acid Method JIN Mei, XU Zhi, LIU Zhi-min, LU Ping, YU Guo-xian (School of Chemistry and Environmental Engineering, Jianghan University, Wuhan 430056, Hubei, China) Abstract Citric acid method was proposed to prepare Mg 3 VO 4 2 which was used as an active catalyst forthe oxidativedehydrogenation ofcyclohexane to cyclohexene. Effects of the preparation conditions were investigated in details. The experimental results showed that Mg 3 VO 4 2 catalyst calcined at 550 for 6 h with a molar ratio of citric acid metal ion = 1.2 1 and initial ph = 4.8, exhibited the best catalyticperformance with an excellent thermal stability. The yield of cyclohexene was 6.4% under the temperature of 450 C, the molar ratio of cyclohexane to oxygen of 2 1 and the flow of cyclohexane of 0.107 mol/h. Key words: citric acid method; Mg 3 VO 4 2; cyclohexane; oxidative dehydrogenation reaction 22 Study on Composite Flame Retardant Rubber Sheet from SBR / Microwave Activation Crumb Rubber HU Si-qian, YU Guo-xian, ZOU Xin (School of Chemistry and Environmental Engineering, Jianghan University, Wuhan 430056, Hubei, China) Abstract Used crumb rubber with microwave activation treatment, styrene-butadiene rubber (SBR), additives and flameretardants to makemixed glue, then theflame retardant rubber products weremade by sulfuration on hot press machine. The products' mechanical performance, differential thermal analysis, the oxygen index determination, horizontal combustibility determination were discussed. Experimental results showed that as the mass ratio of activated powder / SBR / composite flame retardant / additives is 11 18 16 4, the limited oxygen index (LOI) of flame retardant rubber product reached 24%, horizontal flame performanceachieved to GB standard, tensile strength reached 3.44 MPa, the comprehensive indices were better. Key words: microwave activation crumb rubber SBR flame retardant; mechanical property limited oxygen index