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1 7 2 Vol. 7 No Journal of Food Safety and Quality Feb., 2016 MCM-41 * 李儒, 李冰, 谭佳, 鲁奇林 (, ) 摘要 : 目的 MCM-41-(CH 2 ) 3 NH 2 -EDTP, 方法, (CTAB),, MCM (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 , 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 ) Fund: Supported by Key Laboratory Project for Food Safety in Liaoning Province (LNSAKF ) * 通讯作者 :,, luqilinn@126.com *Corresponding author: LU Qi-Lin, Professor, Bohai University, No.19, Keji Road, Songshanxin District, Jinzhou , China. luqilinn@126.com

2 2, : MCM 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,., h,,,,, h, 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,, min,, 2.0 ml 3- (APTS) 4 ml (TEOS),, h.,,., 20 ml 80 ml, 75 6 h,,, 60 6 h, MCM 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.

3 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 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 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, , MCM-41,,, MCM-41- (CH 2 ) 3 NH 2 -EDTP 2θ=2 o ~3 o, MCM , -(CH 2 ) 3 NH 2 -EDTP, 2θ=4 o ~7 o, MCM , MCM-41, XRD, MCM-41 [15] ( 2) 2θ=2 o -3 o, 100, 4 o ~7 o, , 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, ,, 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 cm -1 O-H ; 3450 cm -1 -OH ; 2920 cm -1 -CH 2, 3284 cm -1 -NH cm cm -1

4 2, : MCM 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 mg/g [15] ( 5) MCM 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 mg/g EDTP, MCM-41, 参考文献 [1]. [D]. :, Huang J. Preparation of multifunctional mesoporous material for heavy metal removal from aqueous solution [D]. Shanghai: Shanghai Normal University, [2]. MCM-41

778 7 [D]. :, 2013. Zhu WJ. The study of MCM-41 organic functionalization and heavy metal ionic adsorption performance [D]. Kunming: Kunming University of Science and Technology, 2013. [3].

Bai SS. Study on the modification of mesoporous molecular sieve and thire adsorption properties of heavy metals [D]. Harbin: Harbin Institute of technology, 2011.

5 778 7 [D]. :, Zhu WJ. The study of MCM-41 organic functionalization and heavy metal ionic adsorption performance [D]. Kunming: Kunming University of Science and Technology, [3]. MCM-41 [D]. :, Sun QY. Study on the preparation of mesoporous MCM-41 molecular sieve and its adsorption properties [D]. Jinzhou: Liaoning: Liaoning University of Technology, [4]. [D]. :, Bai SS. Study on the modification of mesoporous molecular sieve and thire adsorption properties of heavy metals [D]. Harbin: Harbin Institute of technology, [5] Vasudevan M, Sakaria PL, Bhatt AS, et al. Effect of concentration of aminopropyl groups on the surface of MCM-41 on Adsorption of Cu 2+ [J]. Ind Eng Chem Res, 2011, 50(19): [6] Wongsakulphasatch S, Kiatkittipong W, Saiswat J, et al. The adsorption aspect of Cu 2+ and Zn 2+ on MCM-41 and SDS-modified MCM-41[J]. Inorg Chem Commun, 2014, 46: [7],,,. MCM-41 MCM-41 [J]., 2011, 06: Cao Y, Li CJ, Huang QY, et al. Study on microwave performance of amino-modified MCM-41 and the application for removal of copper ions from wastewater [J]. Chin Environ Eng, 2011, 06: [8],,,. MCM-41 [J]., 2010, 41(5): Cao Y, Wang X, Bai YH, et al. Study the performance of drug loading and release on aminopropyl modified MCM-41-(CH 2 ) 3 NH 2 [J]. J Funct Mater, 2010, 41(5): [9],,. 5-Cl-PADAB EDTP [J]., 1991, 05: 4 6 Lin RC, Chen HG, Yang Y, et al. Visual Titration of copper with EDTP Using 4-[(5-Chloro-2-Pyridyl)Azo]-1,3-Diamiao-Benzene change laws of rare earth metal mplexes with aminopolycarboxylic acids I, nta, edta and cydta series [J]. Chin J Struct Chem, 2004, 23(10): [11] Xu YQ, Cao Y, Xia ZN. Microwave radiation one-pot synthesis of chloropropyl-functionalized mesoporous MCM-41 [J]. Cent South Univ. 2012, 19: [12]. CH 3 -MCM-41-NH 2 [D]. :, Chu C. Synthesis of functional mesoporous material CH 3 -MCM- 41-NH 2 and its application study in solid phase microextraction of quintozene(pcnb) [D]. Jinzhou: Bohai University, [13]. MCM-41 [D]. :, Yuan C. Study on preparation,organic functional modification and adsorption performance of MCM-41 mesoporous [J]. Wuhan: Wuhan University of Technology, [14]. MCM-41 [J]., 2014, (4): 56. He JX. Synthesis of MCM-41 mesoporous molecular sieve and its catalytic activity at constant pressure [J]. Technol Wind, 2014, (4): 56. [15]. MCM-41 [D]. :, Li CJ. Study on adsorption of functionalized mesoporous material MCM-41 toward copper ion in the wastewater [D]. Chongqing: Chongqing University, [16],,,. EDTA MCM-41 Cu 2+ [J]., 2011, 25(2): Huang CQ, Xu YQ, Cao Y, et al. Synthesis of modified MCM41 with EDTA and adsorption of Cu from an aqueous solution [J]. Mater Rev, 2011, 25(2): 作者简介 ( 责任编辑 : 金延秋 ) 李儒, 硕士, 主要研究方向为分子筛催化剂方向 @qq.com (5-Cl-PADAB)as lndicator [J]. Metall Anal, 1991, 05: 4 6. [10],,,. - I (nta) (edta) -1,2- (cydta) [J]., 2004, 23(10): 鲁奇林, 教授, 主要研究方向为分子筛催化剂方向 luqilinn@126.com Wang J, Wang Y, Zhang XD, et al. Coordinate structures and

ph ph ph Langmuir mg /g Al 2 O 3 ph 7. 0 ~ 9. 0 ph HCO - 3 CO 2-3 PO mg /L 5 p

ph ph ph Langmuir mg /g Al 2 O 3 ph 7. 0 ~ 9. 0 ph HCO - 3 CO 2-3 PO mg /L 5 p 1 2 1 2 3 1 2 1. 100054 2. 100054 3. 100036 ph ph ph Langmuir 166. 67 mg /g Al 2 O 3 ph 7. 0 ~ 9. 0 ph HCO - 4 5. 00 mg /L 5 ph doi 10. 13928 /j. cnki. wrahe. 2017. 03. 017 TV213. 4 + TU991. 26 + 6 A 1000-0860