Báo cáo Nghiên cứu tổng hợp vật liệu bentonit biến tính, ứng dụng hấp phụ phốtpho trong nước

Qua quá trình nghiên cứu điều chế vật liệu bentonite biến tính lantan, hỗn hợp AlLa, AlFe và khảo sát ứng dụng hấp phụ phốtpho trong dung dịch. Chúng tôi rút ra một số kết luận sau: 1. Đã nghiên cứu công nghệ làm giàu bentonit Bình Thuận theo phương pháp CE, với phương pháp này để làm giàu bentonit Bình Thuận cần hoà tan bentonit với nước theo tỷ lệ 1 : 100 (1% huyền phù) để yên trong 24 giờ, tiếp tục khuấy 30 phút, sau đó ly tâm. Sản phẩm thu được có hàm lượng montmorillonit tăng lên khoảng 90%, kết quả được chỉ ra trong hình 3.3 và bảng 3.4. 2. Nghiên cứu điều chế thành công hai vật liệu B90-La và B40-La. Đã khảo sát được ảnh hưởng của các yếu tố: tỉ lệ LaCl3/bentonit, thời gian phản ứng, pH, nhiệt độ và phần trăm huyền phù đến các giá trị khoảng cách cơ bản, d001, từ đó xác định được các điều kiện thực nghiệm thích hợp để điều chế vật liệu bentonit biến tính lantan như sau:

pdf173 trang | Chia sẻ: builinh123 | Lượt xem: 1337 | Lượt tải: 0download
Bạn đang xem trước 20 trang tài liệu Báo cáo Nghiên cứu tổng hợp vật liệu bentonit biến tính, ứng dụng hấp phụ phốtpho trong nước, để xem tài liệu hoàn chỉnh bạn click vào nút DOWNLOAD ở trên
225. 99. Pálinkó I, Kiricsi I, Tasi G, Varga K (1993). Thermal behaviour of montmorillonite pillared with different metal oxides. Journal of Thermal Analysis 39, 197–205. 100. Parker W.O, Kiricsi I (1995). Aluminum complexes in partially hydrolyzed aqueous AlCl3 solutions used to prepare pillared clay catalysts. Applied Catalysis A: General 121, L7–L11. 101. Patel H.A, Rajesh S Somani, Hari C Bajaj and Raksh V Jasra (2006). Nanoclays for polymer nanocomposites, paints, inks, greases and cosmetics formulations, drug delivery vehicle and waste water treatment. Bull Mater Sci, vol. 29. No. 2, tr 133-145. 102. Pearsall W.H. (1932) Phytoplankton in the English Lakes, I. The composition of the phytoplankton in relation to the dissolved substances. Journal of Ecology, 20, 241–262. 103. Penetra R.G, Reali M.A.P, Foresti E, Campos J.R (1999). Post-treatment of effluents from anaerobic reactor treating domestic sewage by dissolved-air flotation. Water Sci. Technol. 40, 137–143. 104. Phang S.M, Miah M.S, Yeoh B.G, Hashim M.A (2000). Spirulina cultivation in digested sago starch factory wastewater. J. Appl. Phycol. 12, 395–400. 105. Pinnavaia T.J, Tzou Ming-Shin, Landau S.D and Raythatha R.H (1984), On the pillaring and delamination of smectite clay catalysts by polyoxo cations of aluminum, Journal of Molecular Catalysis, 27, 195 – 212. 106. Poyato J, Tobias M.M and Trillo J.M (1987), Retention of La(III) and Nd(III) by Montmorillonite, Inorganica Chimica Acta, 140, 307 – 308. 107. Rightor E.D, Tzou Ming-Shin and Pinnavaia T.J (1991), Iron oxide pillared clay with large gallery height: Synthesis and properties as a Fischer-Tropsch catalyst, Journal of Catalysis 130, 29 – 40. 123 108. Roulia M (2005), Synthesis and characterization of novel chromium pillared clays, Materials Chemistry and Physics 91, 182 – 288. 109. Sakadevan K, Bavor H.J (1998). Phosphate adsorption characteristics of soils, slags and zeolite to be used as substrates in constructed wetland systems. Water Res. 32, 393–399. 110. Sawayama S, Rao K.K and Hall D.O (1998), Nitrate and phosphate ion removal from water by Phormidium aminosum immobilized on hollow fibres in a photobioreactor, Applied Microbiology and Biotechnology, Volume 49, Number 4, 463-468. 111. Sawayama S, Rao K.K, Hall D.O, (1998). Immobilization of Rhodobacter capsulatus on cellulose beads and water treatment using a photobioreactor. J. Ferment Bioeng. 86, 517–520. 112. Scholten (2005). Eutrophication Management and Ecotoxicology, Springer, page 6. 113. Seida Y, Nakano Y (2002). Removal of phosphate by layered double hydroxides containing iron. Water Res. 36, 1306–1312. 114. Shabtai J, Rosell M and Tokarz M (1984), Cross-linked smectites. III. Synthesis and properties of hydroxyl-aluminum hectorites and fluorhectorites, Clays and Clay minerals, Vol. 32, No. 2, 99 – 107. 115. Shabtai (1980) – Cross-Linked montmorillonite molecular sieves, US Patent 4,216,188. 116. Shin Young-Sub, Oh Seung-Geun and Ha Baik-Hyon (2003), Pore structures and Acidities of Al-pillared montmorillonite, Korean J. Chem. Eng 20 (1), 77 – 82. 117. Skoularikis N.D, Coughlin R.W, Kostapapas A, Carrado K and Suib S.L (1988), Catalytic performance of Iron (III) and Chromium (III) exchanged pillared clays, Applied Catalysis, 39, 61 – 76. 124 118. Smith V.H. (1983), Low nitrogen to phosphorus ratios favor dominance by blue-green algae in lake phytoplankton. Science, 221, 669–671. 119. Song Y, Hahn H.H, Hoffmann E (2002). The effect of carbonate on the precipitation of calcium phosphate. Environ. Technol. 23, 207–215. 120. Staszczuk P, Bazan J.C, Blachnio M, Sternik D and Garcia N.J (2006), Studies of surface properties of Na- and La-montmroillonites. Thermogravimetry Q- TG, sorptometry, porosimetry and AFM methods, Jounal of Thermal Analysis and Calorimetry, Vol. 86 (1), 57 – 68. 121. Sterte J (1990), Preparation and properties of pillared interstratified Illite/Smectite, Clays and Clay minerals, Vol. 38, No. 6, 609 – 616. 122. Sterte J (1991), Preparation and properties of large-pore La-Al-pillared montmoriilonite, Clays and Clay minerals, Vol. 39, No. 2, 167 – 173. 123. Steve J. Chipera and David L. Bish (2001), Baseline studies of the clay minerals source clays: powder X-ray diffraction analyses, Clays and and Clay Minerals, Vol 49, No 5, 398-409. 124. Storaro L, Ganzerla R, Lenarda M, Zanoni R (1995). Vapour phase deep oxidation of chlorinated hydrocarbons catalyzed by pillared bentonites. Journal of Molecular Catalysis A: Chemical 97, 139–143. 125. Storaro L, Lenarda M, Perissinotto M, Lucchini V, Ganzerla R (1998). Hydroxy-Al pillaring of concentrated suspensions of smectites clays. Microporous and Mesoporous Materials 20, 317–331. 126. Stratful I, Brett S, Scrimshaw M.B, Lester J.N (1999). Biological phosphorus removal, its role in phosphorus recycling. Environ. Technol. 20, 681–695. 127. Stumm W and Wollast R (1997), Coordination chemistry of weathering: Kinetics of the Surface-Controlled Dissolution of Oxide Minerals, Reviews of Geophysics, 28, 53 – 69. 128. Suzuki K, Mori T, Kawase K, Samami H and Iida S (1988), Preparation of delaminated clay having a narrow micropore distribution in the presence of hydroxylaluminum cations and polyvinyl alcohol, Clays and Clay mineral, Vol. 36, No. 2, 147 – 152. 125 129. Tang Yan-Kui, Tong Zhang-fa, Wei Guang-tao (2006), Removal of phosphate from aqueous solution with modified bentonite, The Chinese Journal of Process Engineering, Vol. 6, No. 2, 197 – 200. 130. Thomas S.M, Bertrand J.A, Occelli M.L, Huggins F and Gould S.A.C (1999), Microporous montmorillonites expanded with alumina clusters and M( - OH)Cu( -OCH2CH2Net2)]6(ClO4)3, M=Al, Ga and Fe), or Cr[[ -OCH3)(  - OCH2CH2Net2)CuCl]3 Complexes, Inorg. Chem, 38, 2098 – 2105. 131. Thomas S.M and Occelli M.L (2000), Effects of synthesis conditions on the thermal stability of a Texas montmorillonite expanded with [Al13O4(OH)24(H2O)12] 7+ cations, Clays and Clay mineral, Vol. 48, No. 2, 304 – 308. 132. Tian S, Jiang P, Ning P, Su Y (2009), Enhanced adsorption removal of phosphate from water by mixed lanthanum/aluminum pillared montmorillonite, Chemical Engineering Journal, 151, 141 – 148. 133. Timofeeva M.N, Khankhasaeva S.Ts, Chesalov Yu.A, Tsybulya S.V (2009), Synthesis of Fe,Al-pillared clays starting from the Al,Fe-polymer precursor: Effect of synthesis parameters on textural and catalytic properties, Applied Catalysis B: Environmental 88, 127 – 134. 134. Tokarz M and Shabtai J (1985), Cross-linked smectites. IV. Preparation and properties of hydroxylaluminum-pillared Ce- and La-montmorillonites and fluorinated NH4 +-montmorillonites, Clays and Clay minerals, Vol. 33, No.2, 89–98. 135. Tokunaga S, Wasay S.A and Park S-W (1997), Removal of arsenic(V) ion from aqueous solutions by lanthanum compounds, Water Science and Technology, Vol. 35, 7, 71 – 78. 136. Tomul F and Balci S (2008), Synthesis and Characterization of Al-pillared Interlayered Bentonites, G.U. Journal of Science, 21(1), 21-31. 137. Tomul F and Balci S (2009), Characterization of Al, Cr-pillared clays and CO oxidation, Applied Clay Science 43, 13 – 20. 126 138. Trillo J.M, Poyato J, Tobias M.M, Sanchez P.J and Castro M.A (1990), Effect of pre-heating on the thermal dehydration of lanthanide montmorillonites, Thermochimica Acta, 164, 339 – 351. 139. Trillo J.M (1993), Alba M.D, Alvero R, Castro M.A, Muñoz A, Poyato J, Tobías M.M and Lagaly G (1993), Montmorillonite intercalated with Al(III), La(III) and alumina pillars: structural aspects and reactivity, Solid State Ionics 63 – 65, 457 – 463. 140. Tsujimura S (2004), Reduction of germination frequency in Anabaena akinetes by sediment drying: a possible method by which to inhibit bloom formation. Water Research, 38, 4361-4366. 141. Valderrama L.T, Del Campo C.M, Rodriguez C.M, de-Bashan L.E, Bashan Y (2002). Treatment of recalcitrant wastewater from ethanol and citric acid production using the microalga Chlorella vulgaris and the macrophyte Lemna minuscula. Water Research. 36, 4185–4192. 142. Valverde J.L, Cañizares P, Sun Kou M.R and Molina C.B (2000), Enhanced thermal stability of Al-pillared smectites modified with Ce and La, Clays and Clay mineral, Vol. 48, No. 4, 424 – 432. 143. Visser P.M, Ibelings B.W, Van der Veer B, Koedood J, Mur L.R (1996), Artificial mixing prevents nuisance blooms of the cyanobacterium Microcystis in Lake Nieuwe Meer, the Netherlands, Freshwater Biology, 36, 435-450. 144. Voltolina D, Cordero B, Nieves M, Soto L.P (1999). Growth of Scenedesmus sp. in artificial wastewater. Bioresource Technology. 68, 265–268. 145. Wang S, Zhu H.Y and Lu G.Q.(Max) (1998), Preparation, Characterization, and Catalytic Properties of Clay-Based Nickel Catalysts for Methane Reforming, Journal of Colloid and Interface Science, Vol. 204, 1, 128-134. 146. Wang K, Xing B (2002), Adsorption and desorption of cadmium by goethite pretreated with phosphate, Chemosphere, 48(7), 665 – 670. 147. Welch E.B. (1981): The Dilution/Flushing technique in lake restoration. Water Resources Bulletin, 17, 558-564. 127 148. Wu P, Komatsu T, Yashima T (1998), Isomorphorous substitution of Fe3+ in the framework of aluminosilicate mordenite by hydrothermal synthesis, Microporous and Mesoporous Materials, Vol 20, 1-3, 139-147. 149. Wu P, Wu W, Li S, Xing N, Zhu N, Li P, Wu J (2009), Removal of Cd2+ from aqueous solution by adsorption using Fe-montmorillonite, Journal of Hazardous Materials, Vol. 169, 1-3, 824 – 830. 150. Xue Y, Hou H, Zhu S (2009), Characteristics and mechanisms of phosphate adsorption onto basic oxygen furnace slag, Journal of Hazardous Materials, 162(2-3), 973-980. 151. Yamamoto-Ikemoto R, Matsui S, Komori T, Bosque-Hamilton, E.K (1998). Control of filamentous bulking and interactions among sulfur oxidation- reduction and iron oxidation-reduction in activated sludge using an iron coagulant. Water Sci. Technol. 38, 9–17. 152. Yan Liang-gua, Xu Yuan-yuan, Yu Hai-qin, Xin Xiao-dong, Wei Q, Du B (2010), Adsorption of phosphate from aqueous solution by hydroxyl- aluminum, hydroxy-iron and hydroxyl-iron-aluminum pillared bentonites, Journal of Hazardous Materials 179, 244 – 250. 153. Yang Y, Zhao Y.Q, Babatunde A.O, Wang L, Ren Y.X, Han Y (2006), Characteristics and Machanisms of phospate adsorption on dewatered alum sludge, Separation and Purification Technology, 51(2), 193 – 200. 154. Ye H, Fanzhong Chen, Yanqing Sheng, Guoying Sheng, Jiamo Fu (2006), Adsorption of phosphate from aqueous solution onto modified palygorskites, Separation and Purification Technology 50 (2006) 283–290. 155. Yi W.G, Lo K.V (2003). Phosphate recovery from greenhouse wastewater. J. Environ. Sci. Heal. B 38, 501–509. 156. Yuan P, Annabi-Bergaga F, Tao Q, Fan M, Liu Z, Zhu J, He H, Chen T (2008), A combined study by XRD, FTIR, TG and HRTEM on the structure of delaminated Fe-intercalated/pillared clay, Journal of Colloid and Interface Science 324, 142 – 149. 128 157. Zeng Xiu-qiong, Liu Wei-ping (2004), Preparation and characterization of mixed hydroxy-Fe-Al pillared montmorillonite with large basal spacing, Journal of Enivironmental Science, Vol. 16, No. 1, 117 – 119. 158. Zeng Xiu-qiong, Liu Wei-ping (2005), Adsorption of Direct Green B on mixed hydroxy-Fe-Al pillared montmorillonite with large basal spacing, Journal of Enivironmental Science, Vol. 17, No. 1, 159 – 162. 159. Zhao D, Yang Y, Guo X (1993), Preparation and characterization of lanthanum-doped pillared clays, Mat. Res. Bull, Vol. 28, 939 – 949. 160. Zhao D, Wang G, Yang Y, Guo X, Wang Q, Ren J (1993). Preparation and characterization of hydroxy-FeAl pillared clays. Clays and Clay Minerals 41, 317–327. 161. Zhu R, Zhu L and Zhu J (2007), Simultaneous sorption of aqueous phenanthrene and phosphate onto bentonites modified with AlCl3 and CTMAB, Environ. Sci. Engin. China, 1(1), 79 – 82. 162. Zhu L, Ma J (2008), Simultaneous removal of acid dye and cationic surfactant from water by bentonite in one-step process, Chemical Engineering Journal, Vol. 139, 3, 5030509. 163. Zhu Mao-Xu, Ding Kui-Ying, Xu Shao-Hui, Jiang X (2009), Adsorption of phosphate on hydroxyaluminum-and hydroxyiron-montmorillonite complexes, Journal of Harazdous Materials 165, 645-651. 164. Zuo S, Zhou R, Chenze QI (2011), Synthesis and characterization of aluminum and Al/REE pillared clays and supported palladium catalysts for benzene oxidation, Journal of Rare Earthes, Vol. 29, No. 1, 52 – 57. 129 CÁC BÀI BÁO CÔNG BỐ LIÊN QUAN ĐẾN CÔNG TRÌNH 1. Lê Bá Thuận, Bùi Văn Thắng, Nguyễn Mạnh Trường, Trần Văn Sơn, Thân Văn Liên (2010), Nghiên cứu hấp phụ phốtpho trong dung dịch nước bằng vật liệu bentonit biến tính lantan, Tạp chí Hoá học, T.48, 4C, 384 – 389. 2. Lê Bá Thuận, Bùi Văn Thắng, Trần Văn Sơn (2010), Nghiên cứu công nghệ xử lý phú dưỡng nước hồ Hoàn Kiếm bằng vật liệu bentonit biến tính lantan, Tạp chí Hoá học, T.48, 4C, 402 – 407. 3. Lê Bá Thuận, Bùi Văn Thắng, Trần Văn Sơn (2011), Nghiên cứu điều chế, tính chất của vật liệu La/Al chống bentonit và ứng dụng hấp phụ phốtphat trong nước. Phần I. Nghiên cứu điều chế, tính chất của vật liệu, Tạp chí Hoá học, T.49, 3A, 302 – 406. I PHẦN PHỤ LỤC Phụ lục P1. KẾT QUẢ PHÂN TÍCH XRD CỦA B40-La A1. KẾT QUẢ PHÂN TÍCH XRD CỦA MẪU B40-La Ở TỶ LỆ CỦA LaCl3/B40 KHÁC NHAU Fa cul ty o f Che m istry, V NU, D8 A DV ANCE -B ruker - MB 1 O pe ra tion s: Sm o oth 0 .60 0 | Im p o rt 1) F ile : Tha ng V C N X H MB 1. raw - Ty p e: L oc ke d C ou pl ed - S tar t: 1 .00 0 ° - E n d: 1 5.0 00 ° - Ste p: 0 .02 0 ° - S t e p tim e: 0.5 s - Te mp .: 2 5 °C ( R o om ) - T im e Star ted : 13 s - 2-T he ta: 1 .00 0 ° - T h e ta : 0.5 00 ° - C h i: 0.0 0 L ef t A ng le : 3 .40 0 ° - R igh t An g le: 8 .40 0 ° - L e ft I n t.: 1 16 C p s - R ig ht In t. : 8 6.4 C ps - Ob s. M a x : 5.7 73 ° - d ( Ob s. M a x ): 15 . 2 95 - Ma x Int .: 17 0 C p s - N e t H ei gh t: 67 .7 Cp s - FW H M : 1 .87 3 ° - C ho rd M id .: 5.8 L in ( C ps ) 0 10 20 30 40 50 60 70 80 90 10 0 11 0 12 0 13 0 14 0 15 0 16 0 17 0 18 0 19 0 20 0 21 0 22 0 23 0 24 0 25 0 26 0 27 0 28 0 29 0 30 0 2-Theta - Scale 1.1 2 3 4 5 6 7 8 9 10 11 1 2 13 14 d = 1 5 .1 1 7 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-La0.25 B40-L 0.25.raw - Typ : Locked Coupled - Start: 1.000 ° - End: 15.000 ° - Step: 0.020 ° - St p time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 13 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: 0.00 L in ( C ps ) d = 1 5 .1 1 7 Faculty of Chem istry, VNU, D8 ADVANCE-Bruker - MB2 1) File : Thang V CNX H MB 2.raw - Type: Locked Coupled - S tar t: 1 .000 ° - E nd: 15.000 ° - Step: 0 .020 ° - S tep tim e: 0.5 s - Temp .: 2 5 °C (Room ) - Tim e S tar ted : 6 s - 2 -Theta : 1.000 ° - Theta: 0 .500 ° - C hi: 0 .00 ° Left A ng le: 3 .680 ° - R igh t Ang le: 8 .360 ° - Le ft In t.: 125 Cps - Right In t.: 91.5 Cps - Ob s. Max: 5.860 ° - d (Ob s. Max): 15.070 - Max Int.: 181 Cp s - Net Hei ght : 71 .3 Cps - FW HM : 1 .57 5 ° - Chord Mid .: 5.8 L in ( C p s) 0 10 20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280 290 300 2-Theta - Scale 1.1 2 3 4 5 6 7 8 9 10 11 12 13 14 d = 1 5 .3 2 5 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-La0.35 .r - T : ked upled - tart: 1. 00 ° - n : 1 .000 ° - te : t . L in ( C p s) d = 1 5 .3 2 5 II F a c u lty o f C h e m is tr y , V N U , D 8 A D V AN C E -B ru ke r - M B 3 1) F ile : T h a ng V CN X H M B 3 .r aw - T yp e : L o ck e d C ou p l e d - S ta r t: 1 . 00 0 ° - E n d : 1 5 .0 0 0 ° - S te p : 0 .0 2 0 ° - S te p t im e: 0 .5 s - T e m p . : 2 5 ° C ( R o o m ) - T im e S ta r ted : 5 s - 2 -T h e ta : 1 .0 0 0 ° - T he ta : 0 . 50 0 ° - C hi: 0 .0 0 ° L e f t A ng le : 4 .6 2 0 ° - R igh t An g le : 7 .2 4 0 ° - L e ft In t .: 1 0 2 C p s - R ig ht In t. : 7 0 .3 C p s - O b s . M a x : 5. 5 40 ° - d (O b s. M a x ): 1 5 .9 3 9 - M a x In t . : 1 1 7 C p s - N e t H ei gh t : 26 .3 C p s - F W H M : 1 .17 0 ° - C h o rd M id . : 5 .6 Li n (C p s ) 0 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 1 6 0 1 7 0 1 8 0 1 9 0 2 0 0 2 1 0 2 2 0 2 3 0 2 4 0 2 5 0 2 6 0 2 7 0 2 8 0 2 9 0 3 0 0 2 -T h eta - S c a le 1.1 2 3 4 5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 d = 1 6 .0 84 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-La0.50 File: ThangVCNXH B40-La0.50.raw - Type: Locked Coupled - Start: 1.000 ° - End: 15.000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (R om) - Time Started: 5 s - 2-Theta: . 0 ° - - i: .0 ° Li n (C p s ) d = 1 6 .0 84 F aculty o f C hem is try , V NU , D8 A D V AN CE -B ru ke r - M B 4 1) F ile : Tha ng V CN X H M B 4.r aw - T yp e: L ock e d C ou pl ed - S tar t: 1 . 00 0 ° - E n d: 1 5.0 00 ° - S te p: 0 .02 0 ° - S te p t im e: 0.5 s - T e mp .: 2 5 °C ( R o om ) - T im e S tar ted : 5 s - 2 -T h eta : 1.0 00 ° - T he ta: 0 . 50 0 ° - C hi : 0 .00 ° L eft A ng le : 4 .40 0 ° - R igh t An g le: 6 .92 0 ° - L e ft In t.: 1 01 C p s - R ig ht In t. : 7 6.2 C ps - Ob s . M a x : 5. 4 80 ° - d (Ob s. M a x ): 16 .1 14 - M a x Int. : 11 3 C p s - N e t H ei gh t : 22 .2 C p s - F W H M : 1 .17 8 ° - C ho rd M id .: 5 .5 L in ( C p s) 0 10 20 30 40 50 60 70 80 90 10 0 11 0 12 0 13 0 14 0 15 0 16 0 17 0 18 0 19 0 20 0 21 0 22 0 23 0 24 0 25 0 26 0 27 0 28 0 29 0 30 0 2-Theta - S c ale 1.1 2 3 4 5 6 7 8 9 10 11 1 2 13 14 d = 1 6 .2 8 6 Faculty of Chemistry, VNU, D8 ADVANCE-Bruke – B40-La0.75 : n B40-La0.75.raw - Type: Locked Coupled - Start: 1.000 ° - End: 15.000 ° - Step: .020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time S arted: 5 s - 2-Theta: 1.000 ° - Theta: 0.5 0 ° - Chi: 0. 0 ° L in ( C p s) d = 1 6 .2 8 6 F a cu l ty o f C h e m is tr y , V N U , D 8 A D V A N C E -B ru ke r - M B 5 O pe ra t ion s : S m o o th 0 .60 0 | I m p o rt 1 ) F ile : T h a ng V C N X H M B 5 . r aw - T y p e: L oc k e d C ou pl e d - S t ar t: 1 .00 0 ° - E n d: 1 5.0 00 ° - S te p : 0 . 02 0 ° - S te p t im e : 0. 5 s - T e m p . : 2 5 ° C ( R o om ) - T im e S ta r te d : 5 s - 2 -T h e ta : 1 .0 0 0 ° - T h e ta : 0 .5 0 0 ° - C hi : 0 .0 0 ° L e f t A n g le : 4 .1 2 0 ° - R ig h t A n g le : 7 .3 8 0 ° - L e ft I n t .: 1 24 C p s - R ig h t I n t. : 8 2.3 C ps - O b s . M a x : 5 .5 8 0 ° - d ( O b s . M a x ): 15 . 8 25 - M a x Int . : 14 5 C p s - N e t H ei g h t : 40 .1 C p s - F W H M : 1 .66 6 ° - C h o rd M id . : 5 .7 L in ( C p s) 0 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 1 6 0 1 7 0 1 8 0 1 9 0 2 0 0 2 1 0 2 2 0 2 3 0 2 4 0 2 5 0 2 6 0 2 7 0 2 8 0 2 9 0 3 0 0 2 - T h e t a - S c a le 1. 1 2 3 4 5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 d =1 5 .9 5 3 istry, VNU, D8 ADVANCE-Bruker – B40-La1.00 B40-L 1.00.raw - Type: Locked Coupled - Start: 1.000 ° - End: 15.000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 5 s - 2-Theta: 1.000 ° - Theta: .500 ° - Chi: .00 ° L in ( C p s) d= 1 5 .9 5 3 III A2. KẾT QUẢ PHÂN TÍCH XRD CỦA MẪU B40-La ĐƯỢC ĐIỀU CHẾ Ở pH KHÁC NHAU Faculty of Chemistry, VNU, D8 ADVANCE-Bruker - MBpH5 File: ThangVCNXH MBpH 5.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.020 ° - Step time: 0.5 s - Tem p.: 25 °C (Room) - Time Star ted: 6 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: 0.0 L in ( C p s) 0 100 200 300 400 500 2-Theta - Scale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 d = 1 5 .3 75 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-LapH5 B40-LapH5.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: 0.0 L in ( C p s) d = 1 5 .3 75 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker - MBpH6 File: ThangVCNXH MBpH 6.raw - Type: Lo cked Co upled - Start: 1.000 ° - End : 20 .000 ° - Step: 0.020 ° - Step time: 0.5 s - Tem p.: 25 °C (Roo m) - Time Star ted: 5 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: 0 .0 L in ( C p s) 0 100 200 300 400 500 2-Theta - Scale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 2 0 d = 15 .8 4 2 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-LapH6 il : B40-LapH6.raw - Type: Locked Coupled - Start: 1.000 ° - End: 2 .000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 5 s - 2-Theta: 1.000 ° - Theta: .500 ° - Chi: 0.0 L in ( C p s) d = 15 .8 4 2 IV F a c u l ty o f C h e m is tr y , V N U , D 8 A D V A N C E -B ru k e r - M B p H 9 F ile : T h a ng V C N X H M B p H 9 . ra w - T y p e: L o c k e d C o u ple d - S ta rt : 1 . 0 0 0 ° - E n d : 2 0 .0 0 0 ° - S te p : 0 .0 2 0 ° - S te p t im e : 0 . 5 s - T em p. : 2 5 ° C ( R o o m ) - T im e S ta r te d : 6 s - 2 -T h e ta : 1 . 0 0 0 ° - T he ta: 0 .5 0 0 ° - C h i: 0 .0 L in ( C p s) 0 1 0 0 2 0 0 3 0 0 4 0 0 5 0 0 2 - T h e ta - S c a le 1 2 3 4 5 6 7 8 9 10 1 1 1 2 13 1 4 1 5 1 6 17 1 8 1 9 2 0 d =1 5 .4 1 7 aculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-LapH7 B40-LapH7.raw - Type: Locked Coupled - Start: 1.000 ° - End: 2 . 00 ° - Step: 0. 20 ° - Step time: 0.5 s - Temp.: 25 °C (R om) - Time Started: 6 s - 2-Theta: 1.000 ° - : L in ( C p s) d =1 5 .4 1 7 F aculty o f C hem is try , V NU , D8 A D V AN CE -B ru ke r - M B pH 8 File : Tha ng V CN X H M B pH 8.ra w - Typ e: Lo c ke d C o u ple d - S ta rt : 1 .0 0 0 ° - E nd : 20 .00 0 ° - S te p: 0 .0 2 0 ° - S tep t im e : 0.5 s - T em p.: 2 5 °C ( R oo m ) - T im e S tar te d : 1 2 s - 2- The ta: 1 .0 0 0 ° - Th eta : 0.5 00 ° - C h i: 0 . L in ( C p s) 0 10 0 20 0 30 0 40 0 50 0 2-Theta - S c ale 1 2 3 4 5 6 7 8 9 10 11 1 2 13 14 1 5 16 17 1 8 19 2 0 d = 15 .4 5 8 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-LapH8 B40-LapH8.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time S arted: 12 s 2-Theta: 1. 00 ° - Theta: 0.500 ° - Chi: 0. L in ( C p s) d = 15 .4 5 8 F a cu lty o f C h e m is tr y , V N U , D 8 A D V AN C E -B ru ke r - M B pH 7 F ile : T ha ng V CN X H M B pH 7 .ra w - T yp e: Lo c ke d C o u ple d - S ta rt : 1 .0 0 0 ° - E nd : 20 .00 0 ° - S te p : 0 .0 2 0 ° - S tep t im e : 0.5 s - T em p.: 2 5 °C ( R oo m ) - T im e S ta r te d : 7 s - 2 -T h e ta : 1 .00 0 ° - T he ta: 0 .5 0 0 ° - C h i: 0 .0 L in ( C p s) 0 10 0 20 0 30 0 40 0 50 0 2-T h eta - S c ale 1 2 3 4 5 6 7 8 9 10 11 1 2 13 14 1 5 16 17 1 8 19 2 0 d = 1 5 .2 1 2 d = 8 .5 04 d =4 .8 1 0 d = 4. 4 8 7 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-LapH9 B40-LapH7.raw - Type: Locked Coupled - Start: 1.000 ° - End: 2 .000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 7 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: .0 L in ( C p s) d = 1 5 .2 1 2 d = 8 .5 04 d =4 .8 1 0 d = 4. 4 8 7 V A3. KẾT QUẢ PHÂN TÍCH XRD CỦA MẪU B40-La ĐƯỢC ĐIỀU CHẾ Ở NHIỆT ĐỘ KHÁC NHAU Faculty o f Chemistry, VNU, D8 ADVANCE-Bruker - MBT50 File : Tha ng VCNXH MBT50 .ra w - Type : Locked Co uple d - Start : 1.000 ° - E nd : 20 .00 0 ° - S tep: 0.0 20 ° - S tep time : 0.5 s - Tem p.: 2 5 °C (R oom) - Time S ta rte d: 6 s - 2-The ta : 1 .000 ° - T he ta: 0.5 00 ° - Ch i: 0.0 L in ( C p s) 0 100 200 300 400 500 2-Theta - Scale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 d = 1 5 .3 3 4 d = 5 .5 9 4 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-LaT50 B40-LaT50.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time S arted: 6 s 2-Theta: 1. 00 ° - Theta: 0.500 ° - Chi: .0 L in ( C p s) d = 1 5 .3 3 4 d = 5 .5 9 4 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker - MBT70 File: ThangVCNXH MBT70.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.020 ° - Step time: 0.5 s - Tem p.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1 .000 ° - T heta: 0.500 ° - Chi: 0.0 L in ( C p s) 0 100 200 300 400 500 2-Theta - Scale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 d = 1 5 .5 0 0 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker –B40-LaT70 B40-LaT70.raw - Type: Locked Coupled - Start: 1.000 ° - End: 2 .000 ° - Step: .020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: 0.0 VI Faculty o f Chemistry, VNU, D8 ADVANCE-Bruke r - MBT90 File : ThangVCNX H M BT90 .ra w - Type : Locked Coupled - Sta rt: 1.000 ° - E nd : 20 .000 ° - Step: 0.020 ° - S tep time : 0.5 s - Tem p.: 25 °C (R oom) - Time Started: 5 s - 2-The ta : 1 .000 ° - T he ta: 0.500 ° - Ch i: 0.0 L in ( C p s) 0 100 200 300 400 500 2-Theta - Scale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 d = 15 .8 4 2 d = 5. 5 9 4 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-LaT90 il : g XH B40-LaT90.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 5 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: 0.0 L in ( C p s) d = 15 .8 4 2 d = 5. 5 9 4 A4. KẾT QUẢ PHÂN TÍCH XRD CỦA MẪU B40-La ĐƯỢC ĐIỀU CHẾ Ở NỒNG ĐỘ HUYỀN PHÙ KHÁC NHAU Faculty of Chemistry, VNU, D8 ADVANCE-Bruker - MB15% File: ThangVCNXH MB15%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.020 ° - Step time: 0.5 s - Tem p.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: 0. L in ( C p s) 0 100 200 300 400 500 2-Theta - Scale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 d= 1 5 .2 1 2 t f i try, , 8 A A CE-Bruker – B40-La2.5% il : B40-La2.5%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: 0. L in ( C p s) d= 1 5 .2 1 2 VII F a cu l ty o f C he m istr y, V N U , D 8 A D V A N C E -B ru ke r - M B 5% F ile : T h a n g V C NX H M B 5% .r aw - T y p e : L o ck e d C ou pl e d - S ta rt : 1 .0 0 0 ° - E n d: 20 .0 0 0 ° - Ste p : 0 .0 2 0 ° - S te p t im e : 0.5 s - T e m p . : 2 5 ° C ( R oo m ) - T im e S ta r ted : 6 s - 2 -T h eta : 1.0 00 ° - T he t a: 0 . 50 0 ° - C hi: 0 .0 L in ( C p s ) 0 1 0 0 2 0 0 3 0 0 4 0 0 5 0 0 2 -T h eta - S c a le 1 2 3 4 5 6 7 8 9 1 0 1 1 1 2 1 3 1 4 1 5 16 17 1 8 1 9 2 0 d = 1 5 .0 13 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-La5% i B40-La5%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 2 .000 ° - Step: .020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: .500 ° - Chi: 0.0 L in ( C p s ) d = 1 5 .0 13 F a c u l ty o f C h e m is tr y , V N U , D 8 A D V A N C E -B ru ke r - M B 7 . 5% F ile : T ha ng V C N X H M B 7,5 % . ra w - T y p e : Lo c k ed C o up le d - S ta rt : 1.0 0 0 ° - E n d : 2 0.0 0 0 ° - S te p : 0.0 20 ° - S te p t im e : 0 .5 s - T e m p . : 25 ° C (R o o m ) - T im e S ta rte d : 1 7 s - 2 -T h eta : 1.0 0 0 ° - T he ta: 0 .5 0 0 ° - C h i: L in ( C p s) 0 1 0 0 2 0 0 3 0 0 4 0 0 5 0 0 2 - T h e t a - S c a le 1 2 3 4 5 6 7 8 9 10 1 1 1 2 13 14 1 5 1 6 17 1 8 19 2 0 d = 15 .6 69 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-La . File: ThangVCNXH B40-La7,5%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 2 .000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 17 s - 2-Theta: 1. 00 ° - Theta: .500 ° - Chi: L in ( C p s) d = 15 .6 69 F a culty o f C h e m is tr y , V NU , D8 A D V AN CE -B ru ke r - M B 10 % F ile : T ha ng V CN X H M B 10 % .ra w - T y pe : Lo ck e d Co up le d - Sta rt : 1.0 00 ° - E nd : 2 0 .0 0 0 ° - S tep : 0 .0 20 ° - S te p ti m e : 0 .5 s - T em p.: 25 °C (R o o m ) - T im e Sta r te d: 6 s - 2- T he ta : 1 . 00 0 ° - T h e ta : 0.5 00 ° - C h i: 0. L in ( C p s) 0 10 0 20 0 30 0 40 0 50 0 2-Th eta - S c ale 1 2 3 4 5 6 7 8 9 10 11 1 2 13 14 1 5 16 17 1 8 19 2 0 d = 1 5 .5 0 0 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-La10 il : B40-La10%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 2 .000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - Chi: 0. L in ( C p s) d = 1 5 .5 0 0 VIII Faculty of Chemistry, VNU, D8 ADVANCE-Bruker - MB2.5% File : Thang VCNXH MB2,5%.raw - Type : Lo cked Coup led - S tart: 1.000 ° - End : 20.00 0 ° - S tep : 0.020 ° - Step tim e: 0 .5 s - Tem p.: 25 °C (Room) - Time Sta rted: 5 s - 2-Theta: 1 .000 ° - Theta : 0.500 ° - Chi: 0. L in ( C p s) 0 100 200 300 400 500 2-Theta - Scale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 1 5 16 17 18 19 2 0 d = 1 5 .5 0 0 lty of hemistry, VNU, D8 ADVANCE-Bruker – B40-La15% B40-La15%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 2 . 00 ° - Step: 0. 20 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 5 s - 2-Theta: 1. 0 ° - Theta: 0.5 0 ° - Chi: 0. L in ( C p s) d = 1 5 .5 0 0 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker - MMT-La3+ (1:0.25) pH = 8 File: ThangVCNX H MMT-La(1-0,25)pH=8.raw - Type: Locked Coupled - S tar t: 1.000 ° - End: 20.000 ° - S tep: 0 .020 ° - Step tim e: 0.5 s - Temp .: 25 °C (Room ) - Time Sta rted: 6 s - 2-T heta: 1.000 ° - Th eta : 0. L in ( C p s) 0 100 200 300 400 2-Theta - Scale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 d = 1 5 .2 9 7 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B40-La20% l : B40-La30%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: .020 ° - Step time: 0.5 s - T mp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: . L in ( C p s) d = 1 5 .2 9 7 IX PHỤ LỤC 2. KẾT QUẢ PHÂN TÍCH XRD CỦA MỘT SỐ MẪU ĐẶC TRƯNG CỦA B90-La F aculty of Chem istry, VNU , D8 A DVAN CE -Bruke r - La -M MT 0 .35 File : Tha ng V CNX H La -M MT 0 ,35 .ra w - Type : Lo cked Co up le d - S ta rt: 1.0 00 ° - En d : 2 0. 0 0 0 ° - S tep : 0. 0 20 ° - Ste p tim e : 0 .5 s - Te m p.: 25 °C (Ro o m) - Tim e Sta rte d: 6 s - 2- The ta: 1 .0 0 0 ° - Th eta : 0.5 00 ° - C L in ( C p s) 0 10 0 20 0 30 0 40 0 50 0 2-Theta - Sc ale 1 2 3 4 5 6 7 8 9 10 11 1 2 13 14 1 5 16 17 1 8 19 2 0 d= 1 5 .4 42 il B90-La0.35.raw - Type: Locked Coupled - Start: 1.00 ° - End: 20.00 ° - Step: 0.010 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: 0.500 ° Faculty of Chemistry, VNU, D8 DVANCE-Bruker – B90-La0.35 L in ( C p s) d= 1 5 .4 42 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker - MMT:La3+ = 1:0.5 File: ThangVCNXH MMT-La(1-0,5).raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.010 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: 0.500 ° - L in ( C p s) 0 100 200 300 400 2-Theta - Scale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 20 d= 1 5 .1 7 2 ile: ThangVCNXH B90-La0.50.raw - y : oupled - Start: 1. 00 ° - End: 20. 00 ° - Step: 0.010 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: 0.500 ° Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B90-La0.50 L in ( C p s) d= 1 5 .1 7 2 X F a culty o f C he m istr y, V N U , D8 A D V AN CE -B ru ke r - La -M M T 0 .75 F ile : T ha ng V C NX H La -M M T 0, 75 .ra w - T ype : Lo c ked C o up le d - S ta rt : 1 .0 00 ° - En d : 20. 0 00 ° - S tep : 0.0 20 ° - Ste p t im e : 0 .5 s - Te m p.: 25 °C (R o o m ) - T i m e Sta rte d: 6 s - 2 -T he ta : 1 .0 0 0 ° - T h et a : 0 .5 00 ° - C L in ( C p s ) 0 10 0 20 0 30 0 40 0 50 0 2-Theta - S c ale 1 2 3 4 5 6 7 8 9 10 11 12 13 14 1 5 16 17 1 8 19 20 d = 1 5 .0 8 3 Faculty of Chemistry, E-Bruker – B90-LapH7 B90-LapH7.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20. 0 ° - Step: 0.02 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 6 s - 2-Theta: 1.000 ° - Theta: 0.50 ° - C L in ( C p s ) d = 1 5 .0 8 3 F a cu l ty o f C h e m is tr y , V N U , D 8 A D V A N C E -B ru ke r - M M T -L a 3 + (1 : 0 .2 5 )4 0 C F ile : T ha ng V C N X H M M T -L a( 1 -0 ,2 5 )4 0 C .ra w - T yp e : L o ck ed C o up le d - S ta rt : 1 .0 00 ° - En d : 2 0 .0 0 0 ° - S te p : 0 .0 2 0 ° - S te p t im e : 0 . 5 s - T e m p. : 25 ° C (R o o m ) - T i m e Sta rte d: 1 2 s - 2 - T h e ta : 1 .0 0 0 ° - T h e ta : 0 . L in ( C p s) 0 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 1 6 0 1 7 0 1 8 0 1 9 0 2 0 0 2 - T he ta - S c a le 1 2 3 4 5 6 7 8 9 1 0 11 1 2 13 1 4 1 5 16 17 1 8 1 9 2 0 d = 1 4 .8 4 1 Faculty of Chemistry, VNU, D8 ADVANCE Bruker – B90-LaT 0 ile: ThangVCNXH B90-T50.raw - Type: Locked C upled - Start: 1.000 ° - End: 20.000 ° - Step: 0.020 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - Time Started: 12 s - 2-Theta: 1.0 ° - Theta: 0. L in ( C p s) d = 1 4 .8 4 1 F a culty o f C he m istr y, V N U , D8 A DV A N CE -B ru ke r - M M T -La 3+ (1:0 .2 5 )60 C F ile : T ha ng V C N X H M M T -L a( 1-0 ,25 )6 0 C .ra w - T y pe : L o ck ed C o up le d - S ta rt : 1.0 00 ° - E n d : 2 0. 0 0 0 ° - S tep : 0. 0 20 ° - Ste p t im e : 0 .5 s - T e m p.: 25 °C (R o o m ) - T i m e Sta r te d: 6 s - 2- T he ta : 1 .0 0 0 ° - T h eta : 0 .5 L in ( C p s) 0 10 20 30 40 50 60 70 80 90 10 0 11 0 12 0 13 0 14 0 15 0 16 0 17 0 18 0 19 0 20 0 2 -The ta - S c a le 1 2 3 4 5 6 7 8 9 10 11 1 2 13 14 1 5 16 17 1 8 19 2 0 d = 1 5 .2 2 1 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B90-LaT70 : angVCNXH B90-LaT70.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.02 ° - Step time: 0.5 s - Temp.: 25 °C (Room) - i : s - 2-Theta: 1. 0 ° - Theta: 0.5 L in ( C p s) d = 1 5 .2 2 1 XI F a cul ty o f C he m is tr y, V NU , D8 A DV A N CE -B ru ke r - MM T -La 3+ (1-0.2 5 ) 2 .5% File : Tha ng V C N X H M M T-L a( 1-0 ,25 )2 ,5% .raw - Ty p e: L oc k ed C ou p led - S tar t: 1 .00 0 ° - E n d: 2 0.0 00 ° - Ste p: 0 .02 0 ° - S te p t im e: 0 .5 s - Te m p .: 2 5 °C ( R o om ) - T im e S tar ted : 2 s - 2 -Th eta : 1 .0 00 ° - The ta : 0 . L in ( C p s) 0 10 20 30 40 50 60 70 80 90 10 0 11 0 12 0 13 0 14 0 15 0 16 0 17 0 18 0 19 0 20 0 21 0 22 0 23 0 24 0 25 0 26 0 27 0 28 0 29 0 30 0 2 -Theta - Sc ale 1 2 3 4 5 6 7 8 9 10 11 1 2 13 14 1 5 16 17 1 8 19 2 0 d= 1 5. 5 58 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B9-La2.5% gVCNXH B90- 2,5%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.000 ° - Step: 0.02 ° - Step time: 0.5 s - Temp.: 25 °C (Roo ) i rt : s - 2-Theta: 1. 0 ° - Theta: 0. L in ( C p s) d= 1 5. 5 58 F a culty o f C h e m is tr y , V NU , D8 A D V AN CE -B ru ke r - M M T -La 3+ (1-0.2 5 ) 5 % F ile : T ha ng V CN X H M M T -L a(1-0 ,25 )5 % .ra w - T y pe : Lo c ke d C o up le d - S ta rt : 1.0 00 ° - E nd : 2 0 .00 0 ° - S tep : 0 .0 20 ° - S tep ti m e : 0 .5 s - T em p.: 25 °C (R oo m ) - T im e S ta rte d: 6 s - 2- T he ta : 1 .00 0 ° - T h e ta : 0.5 0 L in ( C p s) 0 10 20 30 40 50 60 70 80 90 10 0 11 0 12 0 13 0 14 0 15 0 16 0 17 0 18 0 19 0 20 0 21 0 22 0 23 0 24 0 25 0 26 0 27 0 28 0 29 0 30 0 2-Th eta - S c ale 1 2 3 4 5 6 7 8 9 10 11 1 2 13 14 1 5 16 17 1 8 19 2 0 d = 1 5 .6 1 9 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B90-La5% gVCNXH B90-La5%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.0 0 ° - Step: 0.02 ° - Step time: 0.5 s - Temp.: 25 °C (Roo i rted: 6 s - 2-Theta: 1. 0 ° - Theta: 0.50 L in ( C p s) d = 1 5 .6 1 9 F a c u l ty o f C h e m is tr y , V N U , D 8 A D V A N C E -B ru k e r - M M T -L a 3 + (1 - 0 .2 5 ) 7 .5 % F ile : T h a ng V C N X H M M T -L a ( 1 -0 ,2 5 )7 ,5% . r aw - T y p e : L o c k ed C ou p le d - S ta r t: 1 . 00 0 ° - E n d : 2 0 .0 0 0 ° - S te p : 0 .0 2 0 ° - S te p t im e: 0 .5 s - T e m p . : 2 5 ° C ( R o o m ) - T im e S ta r t ed : 6 s - 2 -T h e ta : 1 .0 0 0 ° - T he ta : 0 . L in ( C p s) 0 1 0 2 0 3 0 4 0 5 0 6 0 7 0 8 0 9 0 1 0 0 1 1 0 1 2 0 1 3 0 1 4 0 1 5 0 1 6 0 1 7 0 1 8 0 1 9 0 2 0 0 2 1 0 2 2 0 2 3 0 2 4 0 2 5 0 2 6 0 2 7 0 2 8 0 2 9 0 3 0 0 2 - T h e ta - S c a le 1 2 3 4 5 6 7 8 9 10 1 1 1 2 13 1 4 1 5 1 6 17 1 8 1 9 2 0 d = 15 .6 2 3 Faculty of Chemistry, VNU, D8 ADVANCE-Bruker – B90-La7. % ile: angVCNXH B90-La7,5%.raw - Type: Locked Coupled - Start: 1.000 ° - End: 20.0 0 ° - Step: 0.02 ° - Step time: 0.5 s - Temp.: 25 ° ( i Started: 6 s - 2-Theta: 1. 00 ° - Theta: 0. L in ( C p s) d= 15 .6 2 3 XII PHỤ LỤC 3. KẾT QUẢ PHÂN TÍCH XRD CỦA MỘT SỐ MẪU BAlLa 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlLa-14d L in ( C p s) File: ThangVCNXH BAlLa-14d.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 8 .8 5 9 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlLa-21d L in ( C p s) File: ThangVCNXH BAlLa-21d.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 8 .7 3 0 XIII 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlLa-OH-1.5 L in ( C p s) File: ThangVCNXH BAlLa-OH-1.5.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 7 .9 8 3 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlLa-OH-2.5 L in ( C p s ) File: ThangVCNXH BAlLa-OH-2.5.raw - Type: Locked Couplet - Start: 1.000o -End: 20.000o- Step: 0,020o - Step time: 0.5 s - Temp: 25oC (Room) - Time started: 12 s - 2-Theta: 1.000o - Theta: 0.500o- Chi: 2 - Theta - Scale d = 1 8 .8 5 9 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlLa-C25 L in ( C p s) File: ThangVCNXH BAlLa-C25.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 8 .8 5 9 XIV PHỤ LỤC 4. KẾT QUẢ PHÂN TÍCH XRD CỦA MỘT SỐ MẪU BAlFe 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlFe-1 L in ( C p s) File: ThangVCNXH BAlFe-1.raw - Type: Locked Couplet - Start: 1.000o -End: 20.000o- Step: 0,020o - Step time: 0.5 s - Temp: 25oC (Room) - Time started: 12 s - 2-Theta: 1.000o - Theta: 0.500o- Chi: 2 - Theta - Scale d = 1 6 .2 6 2 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 1 7 1 8 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chem is try, HU S, V NU , D 8 A DV A NC E -B rucke r - B AlFe -2 L in ( C p s) F ile: ThangVCNXH BAlFe-2.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step tim e: 0.5 s - Tem p: 25 o C (Room ) - Tim e started: 12 s - 2-Theta: 1.000 o - Theta: 0 .500 o - Chi: 2 - T heta - Scale d = 1 8 .1 7 1 XV 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 1 7 1 8 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Facu lty o f C hem istry, H US, VN U, D8 AD VANC E-Brucker - BA lFe-14d L in ( C p s ) File: ThangVCNXH BAlFe-14d.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0 ,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 18 .2 9 9 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlFe-21d L in ( C p s) File: ThangVCNXH BAlFe-21d.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 8 .1 0 1 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlFe-C15 L in ( C p s ) File: ThangVCNXH BAlFe-C15.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 7 .8 4 1 XVI 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chem istry, HUS, VNU, D8 ADVANCE-Brucker - BAlFe-T50 L in ( C p s ) F ile: ThangVCNXH BAlFe-T50.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Tem p: 25 o C (Room) - Tim e started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 8 .3 0 3 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlFe-T70 L in ( C p s) File: ThangVCNXH BAlFe-T70.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 7 .5 0 9 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chemistry, HUS, VNU, D8 ADVANCE-Brucker - BAlFe-OH-1.5 L in ( C p s) File: ThangVCNXH BAlFe-OH-1.5.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 7 .4 9 8 XVII 0 1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17 18 19 0 50 100 150 200 250 300 350 400 450 500 550 600 650 Faculty of Chem istry, HUS, VNU, D8 ADVANCE-Brucker - BAlFe-OH-2.5 L in ( C p s) File: ThangVCNXH BAlFe-OH-2.5.raw - Type: Locked Couplet - Start: 1.000 o -End: 20.000 o - Step: 0,020 o - Step time: 0.5 s - Temp: 25 o C (Room) - Time started: 12 s - 2-Theta: 1.000 o - Theta: 0.500 o - Chi: 2 - Theta - Scale d = 1 8 .0 0 5 Phụ lục P5 PHỔ HỒNG NGOẠI CỦA MỘT SỐ MẪU BENTONIT BIẾN TÍNH Ten mau: B90Date: 10/12/2011 4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400.0 0.000 0.05 0.10 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 1.000 cm-1 A 3698 3626 3445 1638 1431 1035 780 704 639 532 471 Hình P3.1. Phổ hồng ngoại của mẫu B90 XVIII Ten mau: B40Date: 10/12/2011 4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400.0 0.350 0.36 0.38 0.40 0.42 0.44 0.46 0.48 0.50 0.52 0.54 0.56 0.58 0.600 cm-1 A 3633 3424 1646 1435 1037 534 Hình P3.2. Phổ hồng ngoại của mẫu B40 TEN MAU: B40-LaDate: 10/13/2011 4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400.0 0.150 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.600 cm-1 A 3699 3625 3429 1639 1488 1034 775 694 652 538 471 Hình P3.3. Phổ hồng ngoại của mẫu B40-La XIX Mail: sonhuco@yahoo.comResolution: 4cm-1 Ten mau: B90-LaDate: 10/12/2011 4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400.0 0.300 0.35 0.40 0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.95 1.000 cm-1 A 3636 3412 1641 1475 1435 1035 791 711 637 578 529 Hình P3.4. Phổ hồng ngoại của mẫu B90-La TEN MAU: BAlLa-OH-2.spDate: 10/13/2011 4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400.0 0.300 0.32 0.34 0.36 0.38 0.40 0.42 0.44 0.46 0.48 0.50 0.52 0.54 0.56 0.58 0.600 cm-1 A 3622 3471 1640 1491 1040 734 584 552 Hình P3.5. Phổ hồng ngoại của mẫu BAlLa XX TEN MAU: BAlFe-OH-2.spDate: 10/13/2011 4000.0 3600 3200 2800 2400 2000 1800 1600 1400 1200 1000 800 600 400.0 0.100 0.15 0.20 0.25 0.30 0.35 0.40 0.45 0.50 0.55 0.600 cm-1 A 3432 1636 1039 783 693 655 529 470 Hình P3.6. Phổ hồng ngoại của mẫu BAlFe Phụ lục P6 KẾT QUẢ PHÂN TÍCH BET CỦA MỘT SỐ MẪU BENTONIT BIẾN TÍNH SA3100 Serial No. ad48046 Software Version 2.13 Sample ID B40 Start Date 05/24/11 Customer THANG-DHDT Start Time 11:07:53 Operator TIEN Elapsed Time 1 hrs 57 min Sample Wt 0.0973 g Outgas Time 20 min Profile PSD(ADS) Outgas Temperature 150 C Summary Surface Area Report BET Surface area 48.74 sq.m/g Correlation Coefficient 0.98232 Total Pore Volume Report Total Pore Volume 0.1329 ml/g (Ps/Po = 0.9814, Adsorption) Adsorption BJH Pore Size Distribution Pore Dia. Pore Volume % Range(nm) (ml/g) Under 6 0.00320 1.12 6 - 8 0.02214 3.76 8 - 10 0.02357 6.19 10 - 12 0.01283 8.37 12 - 16 0.02234 10.81 16 - 20 0.03431 19.64 20 - 80 0.03469 39.34 Over 80 0.01294 10.77 BJH Total 0.14892 100.00 Page 1 of 13 SA3100 Serial No. ad48046 Software Version 2.13 Sample ID B90 Start Date 10/13/11 Customer THANG-DT Start Time 10:01:42 Operator TIEN Elapsed Time 1 hrs 40 min Sample Wt 0.078 g Outgas Time 20 min Profile PSD(ADS) Outgas Temperature 200 C Summary Surface Area Report BET Surface area 60.724 sq.m/g Correlation Coefficient 0.99953 Total Pore Volume Report Total Pore Volume 0.1644 ml/g (Ps/Po = 0.9814, Adsorption) Adsorption BJH Pore Size Distribution Pore Dia. Pore Volume % Range(nm) (ml/g) Under 6 0.00000 0.00 6 - 8 0.00000 0.00 8 - 10 0.00414 1.06 10 - 12 0.01425 3.66 12 - 16 0.01421 3.65 16 - 20 0.02265 5.81 20 - 80 0.29557 75.87 Over 80 0.03877 9.95 BJH Total 0.38958 100.00 Page 1 of 11 SA3100 Serial No. ad48046 Software Version 2.13 Sample ID B40-LA Start Date 10/12/11 Customer THANG-DT Start Time 11:05:20 Operator TIEN Elapsed Time 1 hrs 40 min Sample Wt 0.1239 g Outgas Time 20 min Profile PSD(ADS) Outgas Temperature 200 C Summary Surface Area Report BET Surface area 79.333 sq.m/g Correlation Coefficient 0.99999 Total Pore Volume Report Total Pore Volume 0.2295 ml/g (Ps/Po = 0.9814, Adsorption) Adsorption BJH Pore Size Distribution Pore Dia. Pore Volume % Range(nm) (ml/g) Under 6 0.01268 5.71 6 - 8 0.00573 2.58 8 - 10 0.00559 2.52 10 - 12 0.00967 4.35 12 - 16 0.01192 5.36 16 - 20 0.01926 8.67 20 - 80 0.12147 54.68 Over 80 0.03582 16.12 BJH Total 0.22214 100.00 Page 1 of 13 SA3100 Serial No. ad48046 Software Version 2.13 Sample ID ALLA-2.0 Start Date 10/12/11 Customer THANG-DT Start Time 13:08:19 Operator TIEN Elapsed Time 1 hrs 24 min Sample Wt 0.1008 g Outgas Time 20 min Profile PSD(ADS) Outgas Temperature 200 C Summary Surface Area Report BET Surface area 181.509 sq.m/g Correlation Coefficient 0.99684 Total Pore Volume Report Total Pore Volume 0.2845 ml/g (Ps/Po = 0.9814, Adsorption) Adsorption BJH Pore Size Distribution Pore Dia. Pore Volume % Range(nm) (ml/g) Under 6 0.00000 0.00 6 - 8 0.00212 0.68 8 - 10 0.00901 2.88 10 - 12 0.02315 7.39 12 - 16 0.02337 7.47 16 - 20 0.03094 9.88 20 - 80 0.18483 59.04 Over 80 0.03963 12.66 BJH Total 0.31305 100.00 Page 1 of 13 SA3100 Serial No. ad48046 Software Version 2.13 Sample ID BALFE-20 Start Date 10/12/11 Customer THANG-DT Start Time 08:28:22 Operator TIEN Elapsed Time 2 hrs 14 min Sample Wt 0.114 g Outgas Time 20 min Profile PSD(ADS) Outgas Temperature 200 C Summary Surface Area Report BET Surface area 131.478 sq.m/g Correlation Coefficient 0.95498 Total Pore Volume Report Total Pore Volume 0.2821 ml/g (Ps/Po = 0.9814, Adsorption) Adsorption BJH Pore Size Distribution Pore Dia. Pore Volume % Range(nm) (ml/g) Under 6 0.00000 0.00 6 - 8 0.00209 0.66 8 - 10 0.00695 2.19 10 - 12 0.01052 3.31 12 - 16 0.02481 7.81 16 - 20 0.02881 9.07 20 - 80 0.19187 60.42 Over 80 0.05252 16.54 BJH Total 0.31758 100.00 Page 1 of 13

Các file đính kèm theo tài liệu này:

  • pdfnghien_cuu_tong_hop_vat_lieu_bentonit_bien_tinh_ung_dung_hap_phu_photpho_trong_nuoc_1303.pdf
Luận văn liên quan