Luận án tiến sĩ nghiên cứu tổng hợp vật liệu từ tính trên nền graphit việt nam ứng dụng trong xử lý môi trường ô nhiễm màu hữu cơ (congo red)

BỘ GIÁO DỤC VÀ ĐÀO TẠO VIỆN HÀN LÂM KHOA HỌC VÀ CÔNG NGHỆ VIỆT NAM HỌC VIỆN KHOA HỌC VÀ CÔNG NGHỆ - PHẠM VĂN THỊNH NGHIÊN CỨU TỔNG HỢP VẬT LIỆU TỪ TÍNH TRÊN NỀN GRAPHIT VIỆT NAM ỨNG DỤNG TRONG XỬ LÝ MÔI TRƯỜNG Ô NHIỄM MÀU HỮU CƠ (CONGO RED) LUẬN ÁN TIẾN SĨ VẬT LIỆU CAO PHÂN TỬ VÀ TỔ HỢP HÀ NỘI – 2019 i VIỆN HÀN LÂM KHOA HỌC VÀ CÔNG NGHỆ VIỆT NAM HỌC VIỆN KHOA HỌC VÀ CÔNG NGHỆ …… ….***………… PHẠM VĂN THỊNH NGHIÊN CỨU TỔNG HỢP VẬT LIỆU TỪ TÍNH TRÊN NỀN GRAPHIT VIỆT NAM ỨNG DỤNG TRONG XỬ LÝ MÔI TRƯỜNG Ô NHIỄM MÀU HỮU CƠ (CONGO RED) LUẬN ÁN TIẾN SĨ VẬT LIỆU CAO PHÂN TỬ VÀ TỔ HỢP Chuyên ngành: Vật Liệu Cao Phân Tử Và Tổ Hợp Mã số: 9440125 Người hướng dẫn khoa học: PGS.TS Bạch Long Giang PGS.TS Lê Thị Hồng Nhan Hà Nội – 2019 ii LỜI CAM ĐOAN Tôi xin cam đoan luận án cơng trình nghiên cứu riêng tơi khơng trùng lặp với cơng trình khoa học khác công bố Kết đề tài phần dự án số: 10/HĐ-ĐT.10.13/ CNMT Trường Đại Học Nguyễn Tất Thành Tôi xin cam đoan giúp đỡ cho việc thực luận án cảm ơn, thơng tin trích dẫn luận án có nguồn gốc rõ ràng TP.Hồ Chí Minh, ngày 10 tháng 12 năm 2019 Tác giả luận án PHẠM VĂN THỊNH iii LỜI CẢM ƠN Tôi xin bày tỏ lịng biết ơn sâu sắc đầy kính trọng đến thầy PGS.TS.Bạch Long Giang cô PGS.TS Lê Thị Hồng Nhan dẫn dắt từ ngày đầu nghiên cứu đầy bỡ ngỡ nhiều thiếu sót, thầy hướng dẫn tận tâm cho suốt chặng đường dài nghiên cứu luận án Thầy cô tạo hội điều kiện tốt để tơi thực hồn thành thí nghiệm điều kiện thiết bị máy móc Việt Nam cịn nhiều khó khăn Tơi xin trân trọng cảm ơn Ban lãnh đạo sở đào tạo, Viện Khoa học Vật liệu ứng dụng, Học viện Khoa học Công nghệ - Viện Hàn lâm Khoa học Công nghệ Việt Nam tạo điều kiện tốt cho tơi hồn thành bảo vệ luận án Tôi xin thành thật biết ơn tới lãnh đạo Trường Đại học Nguyễn Tất Thành, Viện Kỹ Thuật Cơng Nghệ Cao NTT, Phịng Khoa học Công nghệ nhà trường quan tâm giúp đỡ hỗ trợ tối đa để tơi hồn thành khóa học Cuối cùng, tơi bày tỏ lịng biết ơn sâu sắc tới đồng nghiệp, bạn bè gia đình, người chia sẻ, gánh vác công việc giúp động viên vượt qua thử thách, tiếp thêm sức mạnh, nghị lực để hoàn thành luận án iv DANH MỤC CÁC CHỮ VIẾT TẮT AA Axit ascorbic AAS Atomic Absorption Spectrophotometric: Phổ hấp thụ nguyên tử AC Axit citric CR Congo red EG Exfoliated Graphite: Graphit tróc nở USGS United States Geological Survey - Cục Khảo sát Địa chất Hoa Kỳ MG Malachinte Green MB Methylene Blue EDS Energy-dispersive X-ray spectroscopy: Quang phổ X-quang tán xạ lượng EIS Electrochemical Impedance Spectroscopy: Phổ tổng trở điện hóa MO Methyl Orange MG Methyl Green TEG Thermally Exfoliated Graphite - Graphit tróc nở nhiệt Rh B Rhodamine B GIC Graphit Intercalation Compounds – Hợp chất xen chèn graphit THF Tetrhydrofuran EV Exfoliated Volume - Thể tích tróc nở NFG Natural flakes graphite - Graphit vảy tự nhiên FO Fuel Oil: Dầu mazut DO Diesel Oil: Dầu diesel CO Crude Oil: Dầu thơ SEM Scanning Electron Microscope: Kính hiển vi điện tử quét TEM Transmission Electron Microscopy: Kính hiển vi điện tử truyền qua TGA Thermogravimetric analysis: Phân tích nhiệt XRD X-ray Diffraction: Nhiễu xạ tia X XPS X - ray Photoelectron Spectroscopy: Phổ quang điện tử tia X BOD Biochemical oxygen Demand - Nhu cầu oxy sinh hóa v COD Chemical Oxygen Demand - Nhu cầu oxy hóa học TOC Total organic carbon: Tổng cacbon hữu PAC Poly Alumino Clorua RSM Response Surface Method: Phương pháp bề mặt đáp ứng MEG Magnetic Exfoliated Graphit: Graphit tróc nở mang từ tính CAS Chemical Abstracts Service: Tóm tắt dịch vụ hóa chất BET Brunauer – Emmett – Teller VSM Vibrating Sample Magnetometer - Từ kế mẫu rung SCS Solution Combustion Synthesis - Tổng hợp đốt cháy dung dịch CCD Central Composite Design - Thiết kế phức hợp trung tâm FTIR PZC Fourier Transform Infrared spectroscopy - Phổ hồng ngoại khai triển Fourier Point of Zero Charge - Điểm điện tích khơng vi MỤC LỤC VIỆN HÀN LÂM KHOA HỌC VÀ CÔNG NGHỆ VIỆT NAM ii LỜI CẢM ƠN iv DANH MỤC CÁC CHỮ VIẾT TẮT v MỤC LỤC vii DANH MỤC CÁC BẢNG xiv ĐẶT VẤN ĐỀ CHƯƠNG TỔNG QUAN 1.1 Hiện trạng ô nhiễm chất màu 1.2 Vật liệu hấp phụ 1.2.1 Các phương pháp hấp phụ thuốc nhuộm 1.2.2 Các kết nghiên cứu Việt Nam hấp phụ thuốc nhuộm 1.2.3 Nguồn nguyên vật liệu Graphit 10 1.2.4 Tổng quan phương pháp chế tạo vật liệu graphit tróc nở (EG) 13 1.3 Vật liệu từ tính 18 1.3.1 Tổng hợp vật liệu EG@MFe2O4 18 1.3.1.1.Phương pháp vật lý 20 1.3.1.2.Phương pháp hóa học 20 1.3.1.3.Lựa chọn điều kiện tổng hợp MFe2O4 theo phương pháp tự bốc cháy solgel 25 1.3.1.4 Một số nghiên cứu tổng hợp vật liệu MEG phương pháp sol-gel giới 30 1.3.2 Một số kết ứng dụng vật liệu EG@MFe2O4 xử lý ô nhiễm 32 CHƯƠNG PHƯƠNG PHÁP NGHIÊN CỨU 35 2.1 Ngun vật liệu, hóa chất, thiết bị thí nghiệm phân tích 35 2.2 Tổng hợp vật liệu EG EG@MFe2O4 37 vii 2.2.1 Tổng hợp vật liệu EG 37 2.2.2 Tổng hợp vật liệu EG@MFe2O4 38 2.3 Đánh giá tính chất đặc trưng vật liệu EG EG@MFe2O4 40 2.3.1 Phương pháp đo thể tích riêng vật liệu EG 41 2.3.2 Xác định tính chất đặc trưng vật liệu EG vàEG@MFe2O4 41 2.4 Khảo sát khả hấp phụ màu Congo Red vật liệu EG@MFe2O4 43 2.4.1 Khảo sát yếu tố ảnh hưởng đến khả hấp phụ màu CR vật liệu EG@MFe2O4 44 2.4.1.1.Khảo sát ảnh hưởng thời gian 44 2.4.1.2.Khảo sát ảnh hưởng nồng độ 44 2.4.1.3.Khảo sát ảnh hưởng pH dung dịch 45 2.4.1.4.Khảo sát ảnh hưởng khối lượng vật liệu 45 2.4.2 Tối ưu hóa khả hấp phụ màu congo red vật liệu EG EG@MFe2O4 phương pháp đáp ứng bề mặt (RSM) 45 2.4.3.Động học, nhiệt học, đẳng nhiệt hấp phụ 48 2.4.3.1.Động học hấp phụ 49 2.4.3.2.Nhiệt động học hấp phụ 50 2.4.3.3.Đẳng nhiệt hấp phụ 50 2.4.4 Tái sử dụng vật liệu 52 CHƯƠNG KẾT QUẢ VÀ THẢO LUẬN 53 3.1 Kết tổng hợp vật liệu EG hỗ trợ vi sóng 53 3.2 Kết phân tích tính chất đặc trưng vật liệu EG vật liệu EG@MFe2O4 (M=Co, Mn, Ni) 58 3.2.1 Kết phân tích SEM 58 3.2.1.2.Phân tích cấu trúc bề mặt SEM vật liệu EG@MFe2O4 59 3.2.2 Kết phân tích diện tích bề mặt riêng BET 62 viii 3.2.2.1 Phân tích diện tích bề mặt riêng BET vật liệu EG 62 3.2.2.2.Phân tích bề mặt riêng BET EG@MFe2O4 63 3.2.3 Kết phân tích FT-IR 64 3.2.3.1.Phân tích FT-IR vật liệu EG 64 3.2.3.2.Phân tích FT-IR vật liệu EG@MFe2O4 65 3.2.4 Kết phân tích XRD 66 3.2.4.1.Kết phân tích XRD vật liệu EG 67 3.2.4.2.Kết phân tích XRD vật liệu EGMFe2O4 67 3.2.5 Kết phân tích phổ tán sắc lượng tia X (EDX) 68 3.2.6 Kết phân tích phổ tán xạ lượng (XPS) 70 3.2.7 Kết phân tích từ kế mẫu rung (Vibrating Specimen Magne- tometer – VSM) 73 3.2.8 Kết chuẩn độ theo phương pháp Boehm 74 3.3 Kết khảo sát yếu tố ảnh hưởng đến khả hấp phụ màu CR EG@MFe2O4 75 3.3.1 Ảnh hưởng thời gian nồng độ 75 3.3.2 Ảnh hưởng pH dung dịch 77 3.3.3 Ảnh hưởng khối lượng vật liệu 83 3.3.4 Kết phân tích FT-IR vật liệu EG@MFe2O4 sau hấp phụ CR 84 3.4 Kết tối ưu hóa khả hấp phụ thuốc nhuộm congo red vật liệu EG EG@MFe2O4 phương pháp đáp ứng bề mặt 91 3.4.1 Kết tối ưu hóa khả hấp phụ màu congo red vật liệu EG 91 3.4.2 Kết tối ưu hóa khả hấp phụ màu congo red vật liệu vật liệu EG@MFe2O4 96 3.4.2.1 Kết tối ưu hóa vật liệu EG@CoFe2O4 96 3.4.2.2 Kết khảo sát vật liệu EG@NiFe2O4 104 ix Kết mơ hình tối ưu hóa 104 3.4.2.3 Khảo sát vật liệu EG@MnFe2O4 111 Mơ hình tối ưu hóa 111 3.5.1 Kết khảo sát vật liệu EG@CoFe2O4 120 3.5.1.1 Kết động học hấp phụ 120 3.5.1.2 Kết nhiệt động học hấp phụ 123 3.5.1.3 Kết đẳng nhiệt hấp phụ 124 3.5.2 Kết khảo sát vật liệu EG@NiFe2O4 125 3.5.2.1 Kết động học hấp phụ 125 3.5.2.2 Kết nhiệt động học hấp phụ 128 3.5.2.3 Kết đẳng nhiệt hấp phụ 129 3.5.3 Kết khảo sát vật liệu EG@MnFe2O4 130 3.5.3.1 Kết động học hấp phụ 130 3.5.3.2 Kết nhiệt động học hấp phụ 133 3.5.3.3 Kết đẳng nhiệt hấp phụ 133 3.6 Khả tái sử dụng 134 CHƯƠNG KẾT LUẬN VÀ KIẾN NGHỊ 136 4.1 Kết luận 136 4.2 Kiến nghị 137 NHỮNG ĐÓNG GÓP MỚI CỦA LUẬN ÁN 138 DANH MỤC CÁC CÔNG TRÌNH ĐÃ CƠNG BỐ 139 TÀI LIỆU THAM KHẢO 141 x waste water by ceramic membrane in crossflow microfiltration,” Desalination, vol 149, no 1–3, pp 199–203, 2002 [46] J C Diogo, A Morão, and A Lopes, “Persistent aromatic pollutants removal using a combined process of electrochemical treatment and reverse 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