Nghiên cứu chế tạo cellulose aerogel từ sinh khối ứng dụng trong hấp phụ

IăH CăQU CăGIAăTHÀNHăPH ăH ăCHệăMINH TR NGă IăH CăBÁCHăKHOA -o0o - TR NăQU CăHUY NGHIÊN C U CH T O CELLULOSE AEROGEL T SINH KH I NG D NG TRONG H P PH FABRICATION OF CELLULOSE AEROGEL FROM BIOMASS FOR ADSORPTION APPLICATION ChuyênăngƠnh:ăK ăTHU TăHịAăH C Mưăs :ă8520301 LU NăV NăTH CăS TP.ăH ăCHệăMINH,ăthángă07ăn mă2022 Cơng trình đ c hoàn thành t iμ Tr ng i H c Bách Khoa – i h c Qu c gia Thành ph H Chí Minh Cán b h ng d n khoa h cμ PGS TS LÊ TH KIM PH NG Cán b ch m nh n xét 1μ PGS.TS Lê Anh Kiên Cán b ch m nh n xét β: TS Tr n T n Vi t Lu n v n th c s đ c b o v t i Tr ng i H c Bách Khoa – i h c Qu c gia Thành ph H Chí Minh, ngày 14 tháng 08 n m β0β2 Thành ph n H i đ ng đánh giá lu n v n th c s g mμ PGS TS Nguy n Tr ng S n - Ch t ch PGS.TS Lê Anh Kiên - y viên ph n bi n γ TS Tr n T n Vi t - y viên ph n bi n β TS Tr n Ph c Nh t Uyên - y viên TS Ph m Hoàng Huy Ph c L i - Th kỦ Xác nh n c a Ch t ch H i đ ng đánh giá Lu n v n Tr ngành sau lu n v n đ CH ăT CHăH Iă ng Khoa qu n lỦ chuyên c s a ch a (n u có) NGăăăăăăăăăăăăTR NGăKHOAăK ăTHU TăHịAăH C (H tên ch kỦ) (H tên ch kỦ) i IăH CăQU CăGIAăTP.ăHCM TR NGă C NGăHọAăXẩăH IăCH ăNGH AăVI TăNAM căl pă- T ădoă- H nhăphúc IăH CăBÁCHăKHOA NHI M V LU NăV NăTH CăS H tên h c viênμ TR N QU C HUY MSHV: 1970646 Ngày, tháng, n m sinhμ β4/10/1λλγ N i sinhμ L t Chuyên ngànhμ K thu t Hóa h c Mã s μ 85β0γ01 I TÊNă TÀI: Tên ti ng Vi t: Nghiên c u ch t o cellulose aerogel t sinh kh i ng d ng h p ph Tên ti ng Anh: Fabrication of cellulose aerogel from biomass for adsorption application II NHI M V VÀ N I DUNG: - T ng h p Micro nano cellulose fiber (MNCF) t s i d a - T ng h p Cellulose fiber-lignin aerogel (CFLA) - Kh o sát c u trúc – hình thái – đ c tính c a v t li u CFLA - Kh o sát ng d ng h p ph Cu (II), Ni (II) Pb (II) CFLA III NGÀY GIAO NHI M V : 14/02/2022 IV NGÀY HOÀN THÀNH NHI M V : 06/06/2022 V CÁN B H NG D N: PGS TS LÊ TH KIM PH NG TP HCM, ngày ầ thángầ n m 2022 CÁNăB ăH NGăD N CH ăNHI MăB ăMỌNă ÀOăT O (H tên ch kỦ) TR (H tên ch kỦ) NGăKHOAăK ăTHU TăHịAăH C (H tên ch kỦ) ii L IC M N L i đ u tiên tác gi c m n chân thành s tri ân sâu s c đ n ng i thân gia đình dành s quan tâm t o m i u ki n thu n l i cho tác gi su t th i gian th c hi n lu n v n Tác gi xin chân thành c m n PGS TS Lê Th Kim Ph ng t n tình h ng d n, t o u ki n thu n l i cho tác gi su t trình h c t p, th c hi n lu n v n Tác gi xin g i l i c m n đ n anh ch nghiên c u sinh, h c viên, nghiên c u viên b n sinh viên i H c Bách Khoa – Trung Tâm Nghiên C u Cơng Ngh L c Hóa D u, Tr ng i H c Qu c Gia TP.HCM h tr tác gi su t trình h c t p nghiên c u Tác gi Tr năQu căHuy iii TÓM T T LU NăV N Trong lu n v n, s i micro nano cellulose (MNCF) đ ph c t ng h p t s i d a theo ng pháp ki m hóa k t h p q trình x lỦ c h c đ ng hóa rotor stator siêu âm Cellulose fiber-lignin aerogel (CFLA) đ c t ng h p t h n h p s i micro nano cellulose (MNCF) natri lignosulphonate (LS) s d ng ch t t o liên k t chitosan (CS) nh h ng c a y u t t ng h p CFLA bao g mμ hàm l natri lignosulphonate (LS), hàm l ng MNCF, hàm l ng chitosan (CS) n ng đ huy n phù đ kh o sát C u trúc - hình thái - đ c tính c a v t li u CFLA phù h p đ ph ng phápμ Kh i l h c xác đ nh b ng ng c ng d ng làm v t li u h p ph Cu (II), Ni (II) Pb (II) ng c a th i gian n ng đ ban đ u đ n dung l nghiên c u c ng riêng, kính hi n vi n t quét, ph h ng ngo i chuy n hóa Fourier, nhi u x tia X phân tích nhi t tr ng l V t li u CFLA đ ng ng h c trình h p ph đ ng h p ph c a CFLA đ nh c c kh o sát v i mơ hình đ ng h c bi u ki n b c m t b c hai Quá trình h p ph đ ng nhi t đ c đánh giá v i mô hình đ ng nhi t Langmuir Freundlich Quá trình h p ph Cu (II), Ni (II) Pb (II) phù h p v i mơ hình đ ng h c b c hai mơ hình đ ng nhi t langmuir Dung l đ c xác đ nh c a Cu (II), Ni (II) Pb (II) t ng h p ph c c đ i ng ng v i 158,73 mg/g; 72,99 mg/g 276,24 mg/g V t li u CFLA cho th y kh n ng h p ph ion kim lo i Pb (II) t t h n V t li u CFLA có ti m n ng ng d ng làm s ch n iv c ô nhi m kim lo i n ng ABSTRACT In this study, micro nano cellulose fiber (MNCF) was syntheiszed from pineapple leaf fiber by alkali treatment method Cellulose fiber lignin aerogel (CFLA) samples were syntheisze from MNCF by cross-linking method Effect of conditions on CFLA synthesis including suspensions concentration, cellulose fiber concentration, chitosan concentration and sodium lignosulphonate concentration were investigated The structure - morphology - characterization of CFLA samples were studied by density, scanning electron microscope, Fourier transform infrared spectroscopy, X-ray diffraction and thermogravimetric analysis The synthesized CFLA was applied as adsorbent for removal of Cu (II), Ni (II) and Pb (II) from water The effect factors including contact time and initial concentration on the adsorption ablity of CFLA were studied The adsorption kinetics was examined pseudo-first-order and pseudo-secondorder kinetic models The experimental data was studied by using Langmuir and Freundlich isotherm models The asobtained adsorbent showed the maximum adsorption capacity for Cu (II), Ni (II) and Pb (II) of 158.73 mg.g-1, 72.99 mg.g-1 and 276.24 mg.g-1 respectively Furthermore, the adsorption isotherm and kinetics models were in accord with the Langmuir and pseudo-second-order models, indicating that the adsorption behavior was dominated by monolayer chemisorption The CFLA adsorbent had better affinity for Pb (II) than other coexisting ions in wastewater Such a CFLA adsorbent holds great potential in the application of contaminant cleaning v L IăCAMă OAN Tác gi xin cam đoan lu n v n cơng trình nghiên c u th c s c a cá nhân tác gi đ c th c hi n d is h ng d n c a PGS TS Lê Th Kim Ph ng Trung Tâm Nghiên C u Cơng Ngh L c Hóa D u, Tr ng i h c Bách Khoa - HQG TP HCM Các s li u, k t qu nghiên c u lu n v n hoàn toàn trung th c, ch a t ng đ c công b b t c m t cơng trình khác tr vi c hoàn thành lu n v n đ u đ v n đ u đ c M i s giúp đ cho c c m n, thơng tin trích d n lu n c ch rõ ngu n g c Tác gi xin ch u trách nhi m v nghiên c u c a Tác gi Tr năQu căHuy vi M CL C TÓM T T LU NăV N .iv ABSTRACT v M C L C vii DANH M C HÌNH ix DANH M C B NG .xi DANH M C CÁC T T V Nă CH VI T T T xii NGă1:ăT NG QUAN 1.1 Ô nhi m kim lo i n ng 1.2 Kim lo iăđ ng, niken chì 1.2.1 Ngu n g c ô nhi m 1.2.2 c tính 1.3 M t s ph ngăphápăx lý ô nhi m kim lo i n ng 1.3.1 Ph ng pháp k t t a 1.3.2 Ph ng pháp n hóa 1.3.3 Ph ng pháp sinh h c 1.3.4 Ph ng pháp trao đ i ion h p ph 1.4 Cellulose fiber-lignin aerogel (CFLA) 1.4.1 Nguyên li u t ng h p 1.4.2 Ph ng pháp t ng h p 10 1.4.3 C u trúc tính ch t 13 1.5 Tình hình nghiên c uătrongăn căvƠăngoƠiăn c, tính c p thi t tính m i c aăđ tài 14 1.5.1 Tình hình nghiên c u n c n c 14 1.5.2 Tính c p thi t tính m i c a đ tài 16 CH NGă2:ăTH C NGHI M 17 2.1 M c tiêu n iădungăvƠăph ngăphápănghiênăc u 17 2.1.1 M c tiêu nghiên c u 17 2.1.2 N i dung nghiên c u 17 2.1.3 Ph ng pháp nghiên c u 17 vii 2.2 Hóa ch t, d ng c , thi t b vƠăđ aăđi m th c hi n 18 2.2.1 Hóa ch t 18 2.2.2 D ng c thi t b 18 2.2.3 a m th c hi n 18 2.3 N i dung nghiên c u 19 2.3.1 T ng h p v t li u 19 2.3.2 Kh o sát kh n ng h p ph kim lo i c a v t li u 23 2.3.3 Các ph ng pháp đánh giá hình thái c u trúc 24 2.3.4 Kh o sát h p ph kim lo i 29 CH NGă3ăK T QU VÀ BÀN LU N 33 3.1 S i micro nano cellulose 33 3.1.1 Phân tích hình thái c u trúc SEM 33 3.1.2 Phân tích phân b kích th c DLS 34 3.1.3 Nhi u x tia X 34 3.1.4 Quang ph h ng ngo i FT-IR 36 3.2 Cellulose fiber-lignin aerogel 37 3.2.1 nh h ng u ki n t ng h p 37 3.2.2 Phân tích hình thái c u trúc SEM 43 3.2.3 Nhi u x tia X 44 3.2.4 Quang ph h ng ngo i FT-IR 44 3.2.5 Phân tích nhi t tr ng l ng TGA 46 3.3 Kh o sát ng d ng h p ph kim lo i Cu (II), Ni (II) Pb (II) 47 3.3.1 nh h ng c a th i gian 47 3.3.2 nh h ng c a n ng đ đ u 49 CH NGă4:ăK T LU NăVÀă XU T 55 4.1 K t lu n 55 4.2.ă xu t 55 TÀI LI U THAM KH O 57 viii DANH M C HÌNH Hình 1.1: Q trình h p ph v t lý hóa h c Hình 1.2: Quy trình s n xu t s i d a Hình 1.3: C u trúc hóa h c c a natri lignosulphonate Hình 1.4: C u trúc c a chitosan 10 Hình 1.5: Quá trình hình thành sol gel 10 Hình 1.6μ Các ph ng pháp s y nh h ng đ n c u trúc .11 Hình 1.7μ S đ mơ t q trình s y siêu t i h n 12 Hình 1.8: Quá trình s y th ng hoa 12 Hình 1.9: Các liên k t ngang có th hình thành gi a chitosan natri lignosulphonate .13 Hình 1.10μ C ch t o ph c c a kim lo i v i chitosan 14 Hình 2.1: Quy trình x lý s i d a 19 Hình 2.2: Quy trình t ng h p CFLA .20 Hình 2.3: Quy trình kh o sát h p ph Cu (II), Ni (II) Pb (II) 23 Hình 2.4: C u t o thi t b quang ph FTIR 25 Hình β.5μ Nguyên lỦ đo nhi u x tia X 26 Hình 2.6: C u t o máy SEM 27 Hình 2.7: Các thành ph n c b n ph Hình 2.8: Thi t b đo s phân b kích th ng pháp đo TGA .28 c h t (Model: Zetasizer Nano ZS90) 29 Hình 2.9: C u t o thi t b quang ph h p thu phân t UV-VIS 30 Hình 3.1: nh SEM c a s i d a ki m hóa x lỦ c h c 33 Hình 3.2: K t qu phân b kích th c DLS 35 Hình 3.3: Gi n đ XRD c a : a) s i d a b) s i d a ki m hóa 35 Hình 3.4: Ph FTIR c a: a) s i d a ki m hóa b) s i d a 36 Hình 3.5: Cellulose fiber-lignin aerogel (CFLA) 37 Hình 3.6: Kh i l ng riêng đ x p c a CFLA 0,50; 0,75 1,00% .38 Hình 3.7: Kh i l ng riêng đ x p theo kh i l ng s i cellulose 39 Hình 3.8: nh SEM c a (a) CFLA-F1, (b) CFLA-F2, (c) CFLA-F3 (d) CFLA-F4 40 Hình 3.9: Kh i l Hình 3.10: Kh i l ng riêng đ x p c a CFLA theo t l kh i l ng riêng đ x p theo t l kh i l ng chitosan 41 ng lignosulphonate 42 Hình 3.11: nh SEM c a CFLA 43 ix CH NGă4: K T LU N VÀ XU T 4.1 K t lu n S i micro nano cellulose (MNCF) đ c t ng h p thành công b ng ph ng pháp ki m hóa x lỦ c h c đ ng hóa rotor-stator k t h p siêu âm Bên c nh đó, CFLA đ c t ng h p thành công b ng ph u đ ng pháp t o liên k t ngang i u ki n t ng h p t i c xác đ nh v i: n ng đ huy n phù % t l MNCF:CS:LS 1μ1μ1 t ng v i m u CFLA K t qu phân tích: kh i l ng ng riêng, FTIR, XRD, TGA c a CFLA cho th y nhóm ch c ch a oxy, amine sulfua c a MNCF, CS LS liên k t v i hình thành c u trúc aerogel K t qu phân tích SEM cho th y v t li u CFLA có kích th nh h c kênh mao qu n đ t 40 – 80 m ng c a y u t nh th i gian ti p xúc n ng đ ban đ u đ n kh n ng h p ph c a CFLA đ i v i: Cu (II): th i gian h p ph đ t cân b ng sau 30 phút Quá trình h p ph ph thu c vào giai đo n cân b ng h p ph , phù h p v i mơ hình đ ng h c b c hai h p ph đ ng nhi t Langmuir Dung l ng h p ph Cu (II) c c đ i đ c xác đ nh 158,73 mg/g Ni (II): th i gian h p ph đ t cân b ng sau 30 phút Quá trình h p ph ph thu c vào giai đo n cân b ng h p ph , phù h p v i mơ hình đ ng h c b c hai h p ph đ ng nhi t Langmuir Dung l ng h p ph Ni (II) c c đ i đ c xác đ nh 72,99 mg/g Pb (II): th i gian h p ph đ t cân b ng sau 15 phút Quá trình h p ph ph thu c vào giai đo n cân b ng h p ph , phù h p v i mô hình đ ng h c b c hai h p ph đ ng nhi t Langmuir Dung l ng h p ph Pb (II) c c đ i đ c xác đ nh 276,24 mg/g C ch h p ph c a CFLA đ i v i Cu (II), Ni (II) Pb (II) c ng đ c nghiên c u Quá trình h p ph ph thu c vào s t o ph c gi a nhóm –OH, N-H SO3 c a CFLA v i ion kim lo i Cu (II), Ni (II) Pb (II) Qua k t qu nghiên c u c a lu n v n cho th y v t li u CFLA phù h p đ h p ph ion kim lo i Cu (II), Ni (II) Pb (II) n đ x lý ion kim lo i n ng n 4.2 c V t li u CFLA có kh n ng ng d ng c xu t Tác gi đ xu t h ng nghiên c u ti p theo kh o sát trình h p ph ion kim lo i c a CFLA mơ hình lõi l c đ xác đ nh đ 55 c thông s k thu t áp d ng vào ng d ng làm lõi l c lo i b kim lo i n ng Quy trình thí nghi m mơ hình c t h p ph đ ng đ c th hi n hình 4.1 Hình 4.1: Quy trình thí nghi m c t h p ph kim lo i n ng CFLA Thuy t minh quy trình: V t li u CFLA đ c nh i c t h p ph đ c ng n cách v i đ u b ng m t l p màng l c micro Sau đó, m u dung d ch ch a ion kim lo i n ng đ th đ c b m qua c t h p ph Dung d ch sau h p ph đ c xác đ nh n ng đ b ng ph c t o ph c v i thu c ng pháp quang ph UV-Vis 56 TÀI LI U THAM KH O [1] G A Engwa et al., "Mechanism and health effects of heavy metal toxicity in humans," Intechopen, vol 10, pp 70-90, 2019 [2] C Aydinalp and S Marinova, "The effects of heavy metals on seed germination and 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CFLA_1,00 0,2838 24,99 32,21 64 nhăh  Kim lo i STT ng c a th i gian Cu (II) t (phút) Ni (II) qe (mg/g) Pb (II) t (phút) qe (mg/g) t (phút) qe (mg/g) 0,25 47,18 0,25 7,46 0,25 40,11 1,00 75,44 1,00 11,85 1,00 69,50 2,50 80,69 2,50 15,67 2,50 116,86 3,00 83,84 3,00 17,58 5,00 121,13 4,50 84,09 5,00 32,44 7,00 123,23 7,00 89,01 7,00 32,87 15,0 121,45 15,0 94,24 15,0 35,00 30,0 122,05 30,0 96,42 30,0 38,37 60,0 122,41 60,0 96,15 60,0 39,56 65 nhăh  ng c a n ngăđ banăđ u Cu (II) Kim lo i STT Ni (II) Ce qe (mg/L) (mg/g) Pb (II) Ce (mg/L) qe (mg/g) Ce (mg/L) qe (mg/g) 15,63116 50,30568 29,61474 18,15574 25,03115 43,07945 96,06791 91,72125 103,8995 50,81625 94,31818 95,15007 177,8608 112,9999 207,5739 56,74972 170,0661 139,2576 258,5281 139,6092 314,0974 59,91747 260,4351 172,9051 377,6292 145,2062 411,8526 64,87661 363,3775 199,591 456,9909 143,7989 491,7052 64,65702 445,1282 204,6678 552,5965 143,7477 603,0509 64,73948 548,5316 211,9223 66 ng chu n y = 0.2288x - 0.0055 R² = 0.9955 0.25 h p thu 0.2 0.15 0.1 0.05 0 0.2 -0.05 0.4 0.6 0.8 1.2 N ng đ ph c Cu (ppm) ng chu n Cu (II) 0.5 y = 0.6978x + 0.0111 R² = 0.9917 0.4 h p thu  0.3 0.2 0.1 0 0.2 0.4 0.6 N ng đ ph c Ni (ppm) ng chu n Ni (II) 67 0.8 h p thu 0.09 0.08 0.07 0.06 0.05 0.04 0.03 0.02 0.01 y = 0.0385x + 0.0016 R² = 0.9906 0.5 1.5 N ng đ ph c Pb (ppm) ng chu n Pb (II) 68 2.5 LÝ L CH TRÍCH NGANG H tên: Tr n Qu c Huy NgƠy,ătháng,ăn măsinh: 24/10/1993 a ch liên l cμ ng Cao Th ng-Ph N iăsinhμ L t ng 7-Thành ph àL t TDD: 0915125909 Email: Quochuytran2410@gmail.com QUÁăTRỊNHă ÀOăT O 2014-2018: Sinh viên chuyên nghành Hóa h u c , khoa K thu t Hóa H c, tr ng đ i h c Công Nghi p Th c Ph m TP.HCM 2019-2022: H c viên cao h c chuyên nghành K thu t Hóa H c, tr Khoa, đ i h c Qu c Gia TP.HCM 69 ng i h c Bách ... n v n nghiên c u tách s i micro nano cellulose t s i d a s d ng đ gia c c u trúc cho aerogel  Natri lignosulphonate Ngu n tài nguyên tái t o d i nh t th gi i sinh kh i Trong sinh kh i, cellulose. .. m hóa Cellulose, hemicellulose, Lignin Lignin, cellulose, Hemicellulose 3334,55 3335,75 2917,54 2898,89 C=O Hemicellulose, lignin 1728,96 - C=O Hemicellulose, lignin 1605,24 - C-O-C Hemicellulose,... cellulose c ng b gi m m t ph n Cho th y, lo i b lignin hemicelluse NaOH c ng lo i b m t ph n cellulose 3.2 Cellulose fiber-lignin aerogel 3.2.1 nh h ng u ki n t ng h p Trong nghiên c u này, cellulose