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Thành phố Huế, ngày 25 tháng năm 2022 Tác giả luận án Đặng Thị Ngọc Hoa ii an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm DANH MỤC CÁC CHỮ VIẾT TẮT, KÝ HIỆU Viết tắt Tiếng Anh Tiếng Việt AdSV Adsorptive anodic stripping Volt-Ampere hấp phụ hòa tan voltammetry anode AO Auramine O Vàng ô ASV Anodic stripping voltammetry Volt-Ampere hòa tan anode BET Brunauer-Emmett-Teller Brunauer-Emmett-Teller B-RBS Britton-Robinson Buffer Solution Dung dịch đệm Britton-Robinson CB Conduction band Vùng dẫn COD Chemical oxygen demand Nhu cầu oxygen hóa học CV Cyclic voltammetry Volt-Ampere vịng DCF Diclofenac Diclofenac DP-ASV Differential pulse anodic stripping Volt-Ampere hòa tan anode xung voltammetry vi phân Energy - dispersive X-ray Phổ tán xạ lượng tia X EDX spectroscopy Eg Energy of band gap Năng lượng vùng cấm EtOH Ethanol Ethanol FTIR Fourier transform infrared Phổ hồng ngoại biến đổi Fourier iii an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm GCE Glassy carbon electrode Điện cực than thủy tinh HmIM 2-methyl imidazolate 2-methyl imidazolate HPLC High performance liquid Sắc ký lỏng hiệu cao chromatography IM Imidazolate Imidazolate M Metal Kim loại MB Methylene blue Methylene blue MeOH Methanol Methanol MG Malachite green Malachite green MOFs Metal-organic frameworks Khung hữu - kim loại MR Methyl red Methyl red MS Mass spectroscopy Phổ khối MyB Methyl blue Methyl blue NHE Normal hydrogen electrode Điện cực hydrogen chuẩn PZC Point of zero charge Điểm đẳng điện RE Relative error Độ lệch tương đối Rev Recovery Độ thu hồi RSD Relative standard deviation Độ lệch chuẩn tương đối SEM Scanning electron microscopy Hiển vi điện tử quét iv an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm SV Stripping voltammetry Volt-Ampere hòa tan TEM Transmission electron microscopy Hiển vi điện tử truyền qua UV-Vis Ultraviolet - Visible absorption Phổ hấp thụ tử ngoại – khả kiến spectroscopy UV-Vis Ultraviolet - Visible diffuse Phổ phản xạ khuếch tán tử ngoại - DRS reflectance spectroscopy khả kiến VB Valance band Vùng hóa trị WE Working electrode Điện cực làm việc XPS X-ray photoelectron spectroscopy Phổ quang điện tử tia X XRD X-ray diffraction Nhiễu xạ tia X ZIFs Zeolitic imidazolate frameworks Khung zeolite imidazole v an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm MỤC LỤC Trang LỜI CAM ĐOAN i LỜI CẢM ƠN ii DANH MỤC CÁC KÍ HIỆU, CÁC CHỮ VIẾT TẮT iii MỤC LỤC vi DANH MỤC CÁC BẢNG, SƠ ĐỒ ix DANH MỤC CÁC HÌNH xi MỞ ĐẦU Chương TỔNG QUAN TÀI LIỆU 1.1 T GQ VỀ VẬT LIỆU g-C3N4 1.1.1 Tính chất cấu trúc tinh thể 1.1.2 Phương pháp tổng hợp 11 1.1.3 ng dụng 14 1.2 VẬT LIỆU B T H g-C3N4 V ZIF-67 15 1.2.1 Vật liệu ZIF-67 15 1.2.2 Vật liệu g-C3N4 với -67, Fe2O3 ứng dụng phân tích điện hóa .19 1.3 VẬT LIỆU B T H g-C3N4 V TiO2 23 1.3.1 Vật liệu TiO2 hòa tan .23 1.3.2 Vật liệu g-C3N4 với TiO2 ứng dụng xúc tác quang hóa 26 1.4 GI I THIỆU VỀ O, DC VÀ MB 30 Chương NỘI DUNG VÀ PHƯƠNG PHÁP NGHIÊN CỨU 34 vi an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm 2.1 Ộ D G GH Ê C 34 2.2 PHƯƠ G PHÁP GH Ê C 34 2.2.1 Các phương pháp nghiên cứu đặc trưng vật liệu 34 2.2.2 Phương pháp sắc ký lỏng hiệu cao (HPLC) 43 2.2.3 Sắc ký lỏng hiệu cao ghép nối khối phổ (HPLC-MS) 44 2.2.4 Phương pháp Volt-Ampere hòa tan (SV) 45 2.3 THỰC NGHIỆM 46 2.3.1 Hóa chất 46 2.3.2 Tổng hợp vật liệu 47 2.3.3 Biến tính điện cực GCE vật liệu ZIF-67/Fe2O3/g-C3N4 để xác định AO, vật liệu ZIF-6/g-C3N4 để xác định DCF 51 2.3.4 ghiên cứu hoạt tính quang xúc tác phân hủy MB TiO2/g-C3N4 54 Chương KẾT QUẢ VÀ THẢO LUẬN .59 3.1 GH Ê C T G H P VẬT LIỆU ZIF-67/g-C3N4 VÀ GD TRO G PHÂ T CH Đ Ệ HÓ XÁC ĐỊNH DCF TRO G Ư C T G 59 3.1.1 Tổng hợp vật liệu ZIF-67/g-C3N4 59 3.1.2 Phân tích điện hóa DC điện cực biến tính ( ) -67/g-C3N4 65 3.1.3 Phân tích mẫu thật 73 3.2 D GH Ê G Đ BI C T T G H P VẬT LIỆU ZIF-67/Fe2O3/g-C3N4 VÀ H Đ ỆN CỰC TRO G PHÂ T CH Đ Ệ HÓ G XÁC ĐỊNH AO TRO G THỰC PHẨM 75 3.2.1 Tổng hợp vật liệu ZIF-67/Fe2O3/g-C3N4 .75 3.2.2 Phân tích O điện cực biến tính -67/Fe2O3/g-C3N4 79 3.2.3 Phân tích mẫu thật 87 vii an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac 3.3 GH Ê C LÝ MB DƯ T G H P VẬT LIỆU TiO2/g-C3N4 VÀ NG D NG XỬ Á H SÁ G KHẢ KI N 88 3.3.1 Tổng hợp phức peroxo­hydroxo titanium tan nước .88 3.3.2 Tổng hợp composite TiO2/g-C3N4 90 3.3.3 Hoạt tính xúc tác quang vật liệu TiO2/g-C3N4 96 KẾT LUẬN VÀ KIẾN NGHỊ 109 DANH MỤC CÁC CƠNG TRÌNH NGHIÊN CỨU 111 TÀI LIỆU THAM KHẢO 112 viii (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac determination of eight illegal dyes in chili products by liquid chromatography–tandem mass spectrometry J Chromatogr B 942:46–52 [104] Li K, Gao S, Wang Q, Xu H, Wang Z, et al (2015), In-situ-reduced synthesis of Ti3+ self-doped TiO2/g-C3N4 heterojunctions with high photocatalytic performance under led light irradiation ACS Appl Mater Interfaces 7(17):9023–30 [105] Li X, Liu C, Wu D, Li J, Huo P, Wang H (2019), Improved charge transfer by size-dependent plasmonic au on C3N4 for efficient photocatalytic oxidation of RhB and CO2 reduction Chinese J Catal 40(6):928–39 [106] Li Y, Li L, Li C, Chen W, Zeng M (2012), Carbon nanotube/titania composites prepared by a micro-emulsion method exhibiting improved photocatalytic activity Appl Catal A Gen 427:1–7 [107] Li Y, Zhou K, He M, Yao J (2016), Synthesis of ZIF-8 and ZIF-67 using mixed-base and their dye adsorption Microporous Mesoporous Mater 234:287–92 [108] Liao Y, Que W, Jia Q, He Y, Zhang J, Zhong P (2012), Controllable synthesis of brookite/anatase/rutile TiO2 nanocomposites and singlecrystalline rutile nanorods array J Mater Chem 22(16):7937 [109] Lin K-YA, Chang H-A (2015), Ultra-high adsorption capacity of zeolitic imidazole framework-67 (ZIF-67) for removal of malachite green from water Chemosphere 139(1):624–31 [110] Lin K-YA, Lee W-D (2016), Self-assembled magnetic graphene supported ZIF-67 as a recoverable and efficient adsorbent for benzotriazole Chem Eng J 284:1017–27 [111] Lin Z, Yu B, Huang J (2020), Cellulose-derived hierarchical g-C3N4/TiO2nanotube heterostructured composites with enhanced visible-light photocatalytic performance Langmuir 36(21):5967–78 [112] Linnemann J, Taudien L, Klose M, Giebeler L (2017), Electrodeposited films to MOF-derived electrochemical energy storage electrodes: a concept of 123 (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac simplified additive-free electrode processing for self-standing, ready-to-use materials J Mater Chem A 5(35):18420–28 [113] Liu DY, Dong JH, Liu FM, Gao XF, Yu Y, et al (2019), Synthesis and photocatalytic performance of g-C3N4 composites J Ovonic Res 15(4):239– 46 [114] Liu Y, Sun K, Jiang J, Zhou W, Shang Y, et al (2021), Metallurgical pyrolysis toward Co@ 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Appl Surf Sci 441:1012–23 [120] Lu N, Wang C, Sun B, Gao Z, Su Y (2017), Fabrication of TiO2-doped single layer graphitic-C3N4 and its visible-light photocatalytic activity Sep Purif Technol 186:226–32 [121] Luo Z, Yao J (2017), Raman investigations of atomic/molecular clusters and aggregates In Raman Spectroscopy and Applications InTech [122] Madsen KG, Skonberg C, Jurva U, Cornett C, Hansen SH, et al (2008), 124 (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac Bioactivation of diclofenac in vitro and in vivo: correlation to electrochemical studies Chem Res Toxicol 21(5):1107–19 [123] Mamakhel , Tyrsted C, Bøjesen ED, Hald P, Iversen BB (2013), Direct formation of crystalline phase pure rutile TiO2 nanostructures by a facile hydrothermal method Cryst Growth Des 13(11):4730–34 [124] Manea F, Ihos M, Remes A, Burtica G, Schoonman J (2010), Electrochemical determination of diclofenac sodium in aqueous solution on Cu‐doped zeolite‐expanded graphite‐epoxy electrode Electroanalysis 22(17‐ 18):2058–63 [125] Matthews JA (2014), 5220 chemical oxygen demand (COD)* In Encyclopedia of Environmental Change, 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Mousavi B, Chaemchuen S, Moosavi B, Luo Z, Gholampour N, Verpoort F 125 (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac (2016), Zeolitic imidazole 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ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac [204] Yan J, Huang X, Liu S, Yang J, Yuan Y, et al (2016), A simple and sensitive method for Auramine O detection based on the binding interaction with bovin serum albumin Anal Sci 32(8):819–24 [205] Yan SC, Li ZS, Zou ZG (2009), Photodegradation performance of g-C3N4 fabricated by directly heating melamine Langmuir 25(17):10397–401 [206] Yan T, Chen H, Wang X, Jiang F (2013), Adsorption of perfluorooctane sulfonate (PFOS) on mesoporous carbon nitride RSC Adv 3(44):22480–89 [207] Yan Z, Liu L, Shu H, Yang X, Wang H, et al (2015), A tightly integrated sodium titanate-carbon composite as an anode material for rechargeable sodium ion 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ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac C3N4 composites for cataluminescence sensing of H2S Sensors Actuators, B Chem 211:370–76 [215] Zhang B, He X, Ma X, Chen Q, Liu G, et al (2020), In situ synthesis of ultrafine TiO2 nanoparticles modified g-C3N4 heterojunction photocatalyst with enhanced photocatalytic activity Sep Purif Technol 247:1-33 [216] Zhang C, Huang K (2017), MOF-derived iron as an active energy storage material for intermediate-temperature solid oxide iron–air redox batteries Chem Commun 53(76):10564–67 [217] Zhang F, Yang H, Xie X, Li L, Zhang L, et al (2009), Controlled synthesis and gas-sensing properties of hollow sea urchin-like α-Fe2O3 nanostructures and α-Fe2O3 nanocubes Sensors Actuators, B Chem 141(2):381–89 [218] Zhang H, Li Z, Chen T, Qin B (2017), Quantitative determination of Auramine O by terahertz spectroscopy with 2DCOS-PLSR model Spectrochim Acta Part 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(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac an tien si luan an tien si1 TIEU LUAN MOI download : skknchat123@gm (LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac(LUAN.an.TIEN.si).tong.hop.vat.lieu.composite.tren.co.so.g.c3n4 ung.dung.trong.dien.hoa.va.quang.xuc.tac [224] Zhang W, Tan Y, Gao Y, Wu J, Hu J, et al (2016), Nanocomposites of zeolitic imidazolate 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