7 2 Vol. 7 No. 2 2016 2 Journal of Food Safety and Quality Feb., 2016 MCM-41 * 李儒, 李冰, 谭佳, 鲁奇林 (, 121013) 摘要 : 目的 MCM-41-(CH 2 ) 3 NH 2 -EDTP, 方法, (CTAB),, MCM-41 3- (APTES) (TEOS) MCM-41, MCM-41 (EDTP) MCM-41-(CH 2 ) 3 NH 2 -EDTP X (XRD) (FT-IR) 结果, MCM-41-(CH 2 ) 3 NH 2 -EDTP, MCM-41 MCM-41 结论, 关键词 : MCM-41; ; ; Synthesis and application of EDTP-modified MCM-41 to remove Cu 2+ from water LI Ru, LI Bing, TAN Jia, LU Qi-Lin * (College of Chemical Engineering and Food Safety, Bohai University, Jinzhou 121013, China) ABSTRACT: Objective To study adsorption properties of Cu 2+ by functionalized mesoporous material MCM-41-(CH 2 ) 3 NH 2 -EDTP. Methods The MCM-41 were synthesized by hydrothermal method under alkaline conditions, using sodium silicate as source of silicon and cetyltrimethyl ammonium bromide as template. The modified MCM-41-(CH 2 ) 3 NH 2 was modified by 3-aminopropyltrimethoxysilane(APTS) and ethylsilicate (TEOS), then reacted with EDTP, which succeeded to obtain MCM-41-(CH 2 ) 3 NH 2 -EDTP. Assemblies were characterized by XRD, FT-IR and the adsorption of Cu 2+ were preliminary investigated. Results The adsorption of Cu 2+ by modified-edtp MCM-41 was better than the adsorption of pure MCM-41. Conclusion After EDTP modified, the adsorption capacity can be improved obviously. The functionalized mesoporous material MCM-41-(CH 2 ) 3 -EDTP has a promising prospect in inspection of water safety. KEY WORDS: MCM-41; EDTP; adsorption; Cu 2+ 基金项目 : (LNSAKF 2011018) Fund: Supported by Key Laboratory Project for Food Safety in Liaoning Province (LNSAKF 2011018) * 通讯作者 :,, E-mail: luqilinn@126.com *Corresponding author: LU Qi-Lin, Professor, Bohai University, No.19, Keji Road, Songshanxin District, Jinzhou 121013, China. E-mail: luqilinn@126.com
2, : MCM-41 775 1 引言,,,, [1,2] : (1), ; (2), H 2 S, ; (3),, 1 g/l ; (4), MCM-41,,,,, MCM-41, [3-6], [7,8] MCM-41, MCM-41 MCM-41, EDTP [9,10] MCM-41-(CH 2 ) 3 NH 2, XRD FT-IR, 2 材料与方法 2.1 主要试剂和仪器 (, ); (CTAB,, ); 3- (APTS,, ); (, ); (, ); (, ); (TEOS)(, ); (, ); (, ); (, ); ( ) (SRJX-8-13, ); (FA2004, ), (DF-101Z, ); Shimadzu XRD-6000 X ( ), Cu, Kα,, 40 kv, 40 ma, 2 ~10, 2 /min; Nicolet Impact410, KBr, 400~4000 cm -1 ; (TAS990ATG, ); (BW-ZKHX-400, ) 2.2 全硅介孔分子筛 MCM-41 的合成 25 g, 50 ml,,, ph 11, 10 min, 6.4 g (CTAB),, 30 min,., 130 72 h,,,,, 260 2 h, 600 6 h, MCM-41 [11-14] 2.3 功能性介孔材料 MCM-41-(CH 2 ) 3 NH 2 的合成 2.0 g (CTAB), 400 ml, 3 mol/l NaOH, ph 12,, 75 40 min,, 2.0 ml 3- (APTS) 4 ml (TEOS),, 75 2.5 h.,,., 20 ml 80 ml, 75 6 h,,, 60 6 h, MCM-41 2.4 功能性介孔材料 MCM-41(CH 2 ) 3 NH 2 -EDTP 的合成 MCM-41, 100 ml 1 mol/l 12 h,,, 60, 100 ml 0.1 mol/l EDTA,
776 7 24 h,, 60, MCM-41-(CH 2) 3 NH 2 -EDTP 2.5 样品表征 XRD(x ):, Cu, Kα,, 40kV, 40mA, 2 ~10, 2 /min FT-IR( ):. KBr, 400~4000 cm -1 2.6 功能性介孔材料 MCM-41(CH 2 ) 3 NH 2 -EDTP 的等温吸附曲线 CuSO 4 50 ml 150 250 350 450 550 mg/l, 0.4 g MCM-41(CH 2 ) 3 NH 2 -EDTP, 40, 2 h,, 3 结果与讨论 3.1 XRD 谱图解析 1 MCM-41 2θ=2 o ~3 o, 100, 2θ=4 o ~7 o, 110 200, MCM-41,,, MCM-41- (CH 2 ) 3 NH 2 -EDTP 2θ=2 o ~3 o, MCM-41 100, -(CH 2 ) 3 NH 2 -EDTP, 2θ=4 o ~7 o, MCM-41 110 200, MCM-41, XRD, MCM-41 [15] ( 2) 2θ=2 o -3 o, 100, 4 o ~7 o, 110 200, MCM-41 1 MCM-41 MCM-41-(CH 2 ) 3 NH 2 -EDTP XRD Fig. 1 XRD pattern of MCM-41 and MCM-41-(CH 2 ) 3 NH 2 -EDTP 2 MCM-41 NH 2 -MCM-41 XRD [15] Fig. 2 XRD pattern of MCM-41 and NH 2 -MCM-41 [15], -NH 2, -EDTP MCM-41, 100 110 200,, MCM-41,,, MCM-41,,, 3.2 FT-IR 谱图解析 3 MCM-41-(CH 2 ) 3 NH 2 -EDTP 3, 1074 cm -1 Si-O-Si ; 790 cm -1 Si-O-Si ; 464 cm -1 Si-O-Si ; 943 cm -1 Si-OH, 4 MCM-41.1631 cm -1 O-H ; 3450 cm -1 -OH ; 2920 cm -1 -CH 2, 3284 cm -1 -NH + 3 1481 cm -1 1631 cm -1
2, : MCM-41 777 -COOH- C-O, 2, EDTP MCM-41 MCM-41 MCM-41 Si-OH MCM-41-(CH 2 ) 3 NH 2 -EDTP EDTP, EDTP [16] 3 MCM-41-(CH 2 ) 3 NH 2 -EDTP Fig. 3 FT-IR spectrum of MCM-41-(CH 2 ) 3 NH 2 -EDTP 3.3 功能性介孔材料 MCM-41-(CH 2 ) 3 NH 2 -EDTP 的等温吸附曲线 Langmuir : C e Q e =1 Q m K+C e Q m (1) Qe, mg/g; Qm, mg/g; Ce mg/ ml (1) 4, r 2 MCM-41-(CH 2 ) 3 NH 2 -EDTP Langmuir 4 Cu 2+ MCM-41-(CH 2 ) 3 NH 2 -EDTP Fig. 4 Adsorption isotherm of Cu 2+ on MCM-41-(CH 2 ) 3 NH 2 -EDTP MCM-41-(CH 2 ) 3 NH 2 -EDTP 32.89 mg/g [15] ( 5) MCM-41 17.54 mg/g, MCM-41 MCM-41-(CH 2 ) 3 NH 2 - EDTP 53.3% 5 Cu 2+ MCM-41 [15] Fig. 5 Adsorption isotherm of Cu 2+ on MCM-41 [15] 4 结论, MCM-41, APTES,, EDTP. MCM-41-(CH 2 ) 3 NH 2 -EDTP XRD FT-IR,, -(CH 2 ) 3 NH 2 -EDTP, MCM-41 Langmuir, MCM-41-(CH 2 ) 3 NH 2 - EDTP Langmuir 32.89 mg/g EDTP, MCM-41, 参考文献 [1]. [D]. :, 2013. Huang J. Preparation of multifunctional mesoporous material for heavy metal removal from aqueous solution [D]. Shanghai: Shanghai Normal University, 2013. [2]. MCM-41
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