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Nghien cuu che tao carbon cellulose aerogel tu hon hop soi la dua va soi cotton ung dung trong hap phu pgs Nghien cuu che tao carbon cellulose aerogel tu hon hop soi la dua va soi cotton ung dung trong hap phu pgs
IăH CăQU CăGIAăTHÀNHăPH ăH ăCHệăMINH TR NGă IăH CăBÁCHăKHOA TR Nă ỊNH LÂM NGHIÊN C U, CH T O CARBON CELLULOSE AEROGEL T H N H P S I LÁ D A VÀ S I COTTON NG D NG TRONG H P PH CARBON CELLULOSE AEROGEL PRODUCTION FROM COMPOSITES OF PINEAPPLE LEAF AND COTTON FIBERS FOR APPLICATION IN ADSORTION ChuyênăngƠnh:ăK ăTHU TăHịAăH C Mưăs :ă8520301 LU NăV NăTH CăS TP.ăH ăCHệăMINH,ăthángă07 n mă2022 Cơng trình đ c hồn thành t i: Tr Thành ph H Chí Minh Cán b h ng i H c Bách Khoa ậ i h c Qu c gia ng d n khoa h c: PGS TS LÊ TH KIM PH NG PGS.TS LÊ ANH KIÊN Cán b ch m nh n xét 1: PGS.TS PH M TRUNG KIÊN Cán b ch m nh n xét 2: TS PH M TH H NG PH NG Lu n v n th c s đ c b o v t i Tr ng i H c Bách Khoa ậ Thành ph H Chí Minh, ngày 25 tháng 07 n m 2022 i h c Qu c gia Thành ph n H i đ ng đánh giá lu n v n th c s g m: PGS.TS Nguy n Tr ng S n - Ch t ch PGS.TS Ph m Trung Kiên - y viên ph n bi n TS Ph m Th H ng Ph TS.Tr n Ph ng - y viên ph n bi n 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 ng Khoa qu n lỦ chuyên ngành sau lu n v n đư đ c s a ch a (n u có) CH T CH H I NG TR NG KHOA K THU T HịA H C IăH CăQU CăGIAăTP.ăHCM TR NGă C NGăHọAăXẩăH IăCH ăNGH AăVI TăNAM IăH CăBÁCHăKHOA căl pă- T ădoă- H nhăphúc NHI M V LU NăV NăTH CăS H tên h c viên: Tr n ình Lâm MSHV: 1970065 Ngày, tháng, n m sinh: 16/05/1995 N i sinh: Qu ng Ngưi Chuyên ngành: K thu t Hóa h c Mư s : 8520301 I.ăTÊNă TÀI: Nghiên c u, ch t o carbon cellulose aerogel t h n h p s i d a s i cotton ng d ng h p ph Carbon cellulose aerogel production from composites of pineapple leaf and cotton fiber for application in adsortion II NHI M V VÀ N I DUNG: Nghiên c u quy trình đ t ng h p v t li u carbon cellulose aerogel Kh o sát c u trúc ậ hình thái ậ đ c tính c a v t li u carbon cellulose aerogel Th nghi m kh n ng h p ph methylene blue Cu2+c a v t li u carbon cellulose aerogel III NGÀY GIAO NHI M V : 14/02/2022 IV NGÀY HOÀN THÀNH NHI M V : 17/06/2022 V CÁN B H NG D N: PGS TS LÊ TH KIM PH NG PGS.TS LÊ ANH KIÊN TP HCM, ngày 25 tháng 07 n m 2022 CÁNăB ăH NGăD N TR CH NHI MăB ăMỌNă ÀOăT O NGăKHOAăK ăTHU TăHịAăH C i L I C Mă N đ tđ c k t qu nh hôm nay, bên c nh nh ng n l c c g ng c a b n thân không th không k đ n s h ng d n giúp đ t n tình c a q Th y Cơ c ng nh s đ ng viên, khích l c a gia đình b n bè su t th i gian th c hi n đ tài lu n v n V i lòng bi t n sâu s c, tr c h t em xin g i l i c m n chân thành đ n PGS TS Lê Th Kim Ph ng PGS TS Lê Anh Kiên đư giao đ tài nhi t tình giúp đ Th y Cô đư t o u ki n, t n tình d y b o truy n đ t nh ng ki n th c quý báu su t trình nghiên c u đ giúp em hoàn thành lu n v n c bi t g i l i c m n sâu s c đ n PGS TS Lê Th Kim Ph ng ng tr c ti p h i đư ng d n giúp em có th hồn thành lu n v n m t cách hoàn thi n Không ch h c h i t cô nh ng ki n th c chun mơn mà cịn h c h i đ c tác phong làm vi c nghiêm túc, khoa h c c n tr ng C m n phịng thí nghi m Q Trình & Thi t B c a Vi n KH-CN Quân s Vi n Nhi t i Môi Tr ng đư t o u ki n đ em có d ng c thi t b giúp em hoàn thành đ tài Chân thành c m n anh Ph m Qu c Nghi p c a Vi n KH-CN Quân s -Vi n Nhi t i Môi Tr ng đư giúp đ em su t q trình làm thí nghi m Em xin chân thành c m n Sinh viên th c hi n Tr n ình Lâm ii TĨM T T LU NăV N Trong lu n v n này, carbon cellulose aerogel đ aerogel b ng trình carbon hóa mơi tr c t ng h p t cellulose ng khí N2 Q trình carbon hóa g m hai giai đo n: than hóa ho t hóa, đ u di n mơi tr ng khí tr Q trình ho t hóa có th s d ng tác nhân ho t hóa v t lý ho c hóa h c, th ng s d ng CO2 KOH Trong nghiên c u này, quy trình ho t hóa b ng tác nhân ho t hóa v t lý CO2 tác nhân ho t hóa h c KOH đ gian ho t hóa đ ng ch t ho t hóa th i c kh o sát C u trúc - hình thái - đ c tính c a v t li u carbon cellulose aerogel đ vi n t c nghiên c u, l c xác đ nh b ng ph ng pháp: Kh i l ng riêng, kính hi n quét, ph h ng ngo i chuy n hóa Fourier di n tích b m t riêng Brunauer - Emmett - Teller Carbon cellulose aerogel t ng h p có kh i l 0.0236 g/cm3 t ng ng v i m u ho t hóa v t lý m u ho t hóa hóa h c đ nh h d ng làm v t li u h p ph n ng đ ban đ u đ n dung l đ ny ut ng c a th i gian, kh i l ng h p ph đư đ ng h c trình h p ph đ ki n b c m t b c hai v i m u ho t hóa hóa h c 886.58 ph methylene blue t i đa t c ng ng ch t h p ph , c nghiên c u thông qua kh o sát c kh o sát v i mơ hình đ ng h c bi u ng nhi t h p ph đ Langmuir Freundlich S n ph m thu đ t ng riêng th p 0.0212 g/cm3 c đánh giá v i mơ hình đ ng nhi t c có di n tích b m t riêng 970,20 /g /g v i m u ho t hóa v t lý, kh n ng h p ng ng 263 mg/g 250 mg/g, h p ph Cu2+ t i đa ng ng 69.44mg/g 62.11 mg/g ng h c h p ph methylene blue thích h p v i mơ hình h p ph bi u ki n b c 1, đ ng h c h p ph Cu2+ thích h p v i mơ hình h p ph bi u ki n b c H p ph đ ng nhi t thích h p v i mơ hình đ ng nhi t Langmuir K t qu ch ng t v t li u t ng h p carbon cellulose aerogel t s i d a s i cotton thích h p đ làm v t li u h p ph ng th i, u ki n thí nghi m s c s đ xây d ng quy trình s n xu t quy mô công nghi p iii ABSTRACT In this thesis, carbon cellulose aerogel is synthesized from cellulose aerogel by carbonization under a N2 atmosphere The carbonization process consists of twostages: heat treatment and activation, both taking place in an inert atmosphere Activation can use a physical or chemical activating agent, often using CO2 and KOH The activation process by physical agent CO2 and chemical agent KOH were studied in this work KOH impregnation ratio and activation time were investigated The structure - morphology - properties of carbon cellulose aerogel were determined by the following methods: Density, scanning electrone microscopy, Fourier Transform Infrared Spectroscopy, and Brunauer - Emmett - Teller specific surface area The synthesized carbon cellulose aerogel has a low density of 0.0212 g/cm3 and 0.0236 g/cm3, respectively, for physical and chemically activated samples, which are used as adsorbents material The effects of time, amount of adsorbent, and initial concentration on adsorption capacity were studied through single-factor survey The adsorption kinetics was investigated with the pseudo-first-order model and pseudo-second-order model The adsorption isotherm was evaluated with Langmuir and Freundlich isotherm models The product has a specific surface area of 970.20 m2/g with the chemically activated sample and 886.58 m2/g with the physically activated sample, the maximum adsorption capacity of methylene blue corresponding to 263 mg/g and 250 mg/g, maximum Cu2+ adsorption 69.44mg/g and 62.11 mg/g respectively The adsorption kinetics for methylene blue is suitable for the pseudo-first-order model and the Cu2+ adsorption kinetics is suitable for the pseudo-second-order model The adsorption isotherm comply with the Langmuir isotherm model These results show that carbon cellulose aerogel was synthesized from pineapple leaf and cotton fibers can be used as adsorbents material iv 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 cô PGS TS LÊ TH KIM PH NG th y PSG TS LÊ ANH KIÊN 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 giúp đ cho vi c hoàn thành lu n v n đ u đư đ d n lu n v n đ u đư đ c M i s c c m n, thơng tin trích c ch rõ ngu n g c Tác gi xin ch u trách nhi m v nghiên c u c a Tác gi Tr n ình Lâm v M CL C L I C Mă N ii TÓM T T LU NăV N iii L IăCAMă OAN v M C L C vi DANH M C HÌNH viii DANH M C B NG x DANH M C CH VI T T T xi M U CH NGă1:T NG QUAN 1.1 Carbon cellulose aerogel 1.1.1 T ng quan 1.1.2 Ph ngăpháp t ng h p carbon cellulose aerogel .7 1.1.2.1 Quá trình Sol- Gel 1.1.2.2 S y khô gel 1.1.2.3 S y khô CO2 siêu t i h n 10 1.1.2.4 S yăth ngăhoa .11 áp su tămôiătr 1.1.2.5 S y 1.1.3 ng 12 Q trình carbon hóa 12 1.1.3.1 Ph ngăphápăho t hóa v t lý 13 1.1.3.2 Ph ngăphápăho t hóa hóa h c 14 1.2 ng d ng c a carbon cellulose aerogel 15 1.3 Các nghiên c u t ng h p carbon aerogel ng d ng h p ph 18 1.3.1 1.3.2 ng d ng h p ph khí 18 ng d ng x lỦăn c 21 1.4 Lý thuy t v h p ph 23 1.4.1 Khái ni m phân lo i h p ph 23 1.4.2 Cácăd ngăđ ngăh păph ăđ ngănhi t 26 1.4.3 Cácăy uăt ă nhăh CH NGă2:ăPH ngăđ năkh ăn ngăh păph .30 NGăPHÁPăTH C NGHI M 31 2.1 T ng h p v t li u 31 2.1.1 T ng h p Carbon cellulose aerogel .31 vi 2.1.2 Kh o sát y u t nhăh ngăđ n trình ho t hóa .33 2.2 Kh oăsátăcácăđ cătr ngălỦ- hóa 34 2.2.1 Xácăđ nh ch s h p ph 34 2.2.1.1.ăXácăđ nh ch s h p ph methylene blue .34 2.2.1.2.ăXácăđ nh ch s h p ph Cu2+ 37 2.2.2.ăPhépăđoăph h ng ngo i (FTIR) 39 2.2.3 K thu t phân tích thành ph n v t ch t EDX .40 2.2.4 PhépăđoăSEM 41 2.2.5.ăPhépăđoăBET 42 CH NGă3:ăK T QU VÀ BÀN LU N 43 3.1 c tính c u trúc c a v t li u 43 3.1.1 Hình thái phân tích c u trúc 43 3.1.2 Di n tích b m tăriêngăvƠăđ cătr ngăl x p 48 3.1.3 Phơnătíchăb ăm tăhóaăh c .50 3.2 Quá trình h p ph c a carbon cellulose aerogel 51 3.2.1 nhăh ng c a t l r n ậ l ng lên kh n ngăh p ph 51 3.2.2 nhăh ng c aăđi u ki n ho t hóa lên q trình h p ph 53 3.2.3 nhăh ng c a th i gian h p ph lên trình h p ph 56 3.2.4 nhăh ng c a n ngăđ banăđ u lên kh n ngăh p ph 63 CH NG K T LU NăVÀă XU T .71 4.1 K t lu n 71 4.2 xu t 71 TÀI LI U THAM KH O 72 vii DANH M C HÌNH Hình 1.1 Q trình h p ph v t lỦ 23 Hình 1.2 N m lo i đ ng h p ph theo Brunauer 25 Hình 1.3 D ng đ th đ Hình 1.4 ng h p ph đ ng nhi t BET 27 ng đ ng nhi t h p ph BET 28 Hình 2.1: Quy trình t ng h p cellulose aerogel 29 Hình 2.2 S đ quy trình than hóa ho t hóa .31 Hình 2.3 ng làm vi c chu n c a Methylen Blue Hình 2.4 ng làm vi c chu n c a Cu2+ b b c sóng 664 nm 33 c sóng 550 nm 35 Hình 2.5: Máy đo ph h p ph phân t UV-vis SP-2000UV…………………… 37 Hình 2.6: Thi t b đo ph h ng ngo i bi n đ i Fourier (Model: Alpha II)……… 38 Hình 2.7: Thi t b FE-SEM Tescan Mira 3…………………………………… .39 Hình 2.8: Thi t b BET 201A………………………………………………………40 Hình 3.1 nh SEM c a CA (a), C (b), CCACO2(c) CCAKOH (d) 41 Hình 3.2 Ph EDX c a CA (a), C (b), CCACO2(c) CCAKOH (d) 42 Hình 3.3 nh SEM c a CAT(a), CCAKOH 0.5(b) CCAKOH 2(c) 43 Hình 3.4 nh SEM c a CAT(a), CCACO2 100(b) CCACO2 400(c) 44 Hình 3.5 t=10 (d), nh SEM c a CCAKOH t=0.5(a), CCAKOH t=1.5(b), CCAKOH t=2(c), CCACO2 CCACO2 t=15 (e), CCACO2 t=30 (f) 45 Hình 3.6 th th hi n s phân b kích th c l x p c a carbon cellulose aerogel .47 Hình 3.7 Ph FTIR c a CA (a), C (b), CCACO2(c) CCAKOH (d) 48 Hình 3.8: Hi u su t h p ph theo kh i l Hình 3.9: Dung l Hình 3.10: Dung l ng h p ph theo kh i l ng 50 ng .50 ng h p ph c a m u ho t hóa hóa h c th i gian ho t hóa khác nhau……………… 51 Hình 3.11: Dung l ng h p ph c a m u ho t hóa v t lý th i gian ho t hóa khác 51 viii B ng 3.5 H ng s đ ng nhi t Langmuir, Freundlich, trình h p ph MB Langmuir Ho tăhóaăv tălỦ Ho tăhóaăhóaăh c Than hóa T b ng 3.5, d Freundlich RL qmax (mg/g) R2 n kF R2 0.058-0.30 250 0.9984 1.60 6.57 0.7625 0.057-0.30 263 0.9997 1.66 8.19 0.7730 0.076-0.37 166 0.9988 2.21 11.58 0.8063 li u th c nghi m c a trinh h p ph thích h p v i mơ hình đ ng nhi t Langmuir h n so v i mơ hình đ ng nhi t Freundlich i u th hi n tính ch t đ ng nh t c a b m t carbon cellulose aerogel m i phân t methylene blue b m t h p ph có n ng l ng h p ph b ng T giá tr RL cho th y carbon cellulose aerogel ch t o đ c thích h p đ h p ph dung d ch methylene blue giá tr RL n m kho ng t đ n K t qu c ng cho th y s hình thành l p ph đ n l p c a phân t methylene blue b m t c a carbon aerogel Theo lỦ thuy t qm đ c tính tốn t mơ hình Langmuir, carbon aerogel có kh n ng h p ph t i đa 263 mg/g đ i v i m u đ đ iv im uđ th y đ c ho t hóa hóa h c, 250 mg/g c ho t hóa v t lỦ 166 mg/g đ i v i m u than hóa k t qu cho c dung l ng h p ph c a carbon cellulose aerogel t ng lên đáng k so sánh v i k t qu h p ph đ t đ c c đ i v i cellulose aerogel ch a ho t hóa (23.20 mg/g) [111] K t qu h p ph methylene blue đ t đ khác đ đ c t v t li u quy trình c t ng h p đ so sánh v i k t qu đ t đ c t nghiên c u th hi n b ng 3.6 B ng 3.6 Kh n ng h p ph methylene blue t i đa t nguyên li u khác Nguyên li u Tác nhân ho t hóa Kh n ng h p ph (mg/g) aerogels t Carboxymethyl KOH 249.6 [57] Than ho t tính t b cà phê ZnCl2 188.7 [122] Than ho t tính t r m (NH4)3PO4 129.5 [123] KOH 263 Carbon cellulose Carbon cellulose aerogels t s i d a s i cotton 66 Carbon cellulose aerogels t s i d a s i cotton CO2 250 Quá trình h p ph Cu2+ K t qu thí nghi m h p ph Cu2+ n ng đ khác đ c trình bày hình 3.24 Hình 3.24 th th hi n dung l Hình 3.24 cho th y đ ng h p ph Cu2+ n ng đ khác c, m u cellulose aerogel không h p ph Cu2+ b t kì n ng đ i u th hi n r ng b m t c a cellulose aerogel khơng có n tích âm c ng nh n th liên k t đ có th t o thành q trình h p ph hóa h c v i Cu2+ i v i m u ho t hóa, t ng t q trình h p ph methylene blue, t ng n ng đ Cu2+ ban đ u d n đ n t ng kh n ng h p ph V i vi c t ng n ng đ ban đ u t 20 đ n 150mg/L, kh n ng h p ph t ng t 23.31 lên 60.69 mg/g đ i v i m u ho t hóa v t lý, t 25.73 lên 66.78 mg/g đ i v i m u ho t hóa hóa h c S h ng c a n ng đ đ u có th đ c gi i thích nh sau: nh n ng đ ion kim lo i ban đ u th p, có đ v trí h p ph đ h p ph ion kim lo i n ng Do đó, s h p 67 ph không ph thu c vào n ng đ ion kim lo i ban đ u Tuy nhiên, h n, v trí h p ph c a carbon cellulose đư đ t ng ch m có xu h ng n m ngang, s l c n đ y, dung l n ng đ cao ng h p ph ng ion kim lo i n ng t ng đ i cao h n so v i s s n có c a v trí h p ph [120,121] K t qu c ng cho th y r ng m c dù cân b ng h p ph t ng lên n ng đ ion kim lo i t ng, m c đ t ng không t l v i n ng đ ion kim lo i ban đ u, t c n ng đ ion kim lo i c a ion kim lo i t ng lên hai l n không d n đ n t ng g p đôi kh n ng h p ph cân b ng Kh o sát d ng đ Cu2+ k t qu đ Hình 3.25 ng đ ng nhi t Freundlich Langmuir trình h p ph c th hi n b ng 3.7 hình 3.25, 3.26 th h p ph đ ng nhi t theo Langmuir, trình h p ph Cu2+ 68 Hình 3.26 th h p ph đ ng nhi t theo Freundlich, trình h p ph Cu2+ B ng 3.7 H ng s đ ng nhi t Langmuir, Freundlich, trình h p ph Cu2+ Langmuir Ho tăhóaăv tălỦ Ho tăhóaăhóaăh c Freundlich kL qmax (mg/g) RL2 n 0.030-0.186 62.11 0.9952 3.27 16.28 0.8793 0.040-0.225 69.44 0.9891 4.27 23.92 0.9618 kF RF2 T b ng 3.7, d li u th c nghi m c a q trình h p ph Cu2+ thích h p v i mơ hình đ ng nhi t Langmuir h n so v i mơ hình đ ng nhi t Freundlich i u th hi n tính ch t đ ng nh t c a b m t carbon cellulose aerogel m i ion Cu2+ b m t h p ph có n ng l ng h p ph b ng T giá tr RL cho th y carbon cellulose aerogel ch t o đ c c ng thích h p đ h p ph kim lo i Cu2+vì giá tr RL n m kho ng t đ n K t qu c ng cho th y s hình thành l p ph đ n l p c a ion Cu2+ Theo lý thuy t qm đ b m t c a carbon aerogel c tính tốn t mơ hình Langmuir, carbon aerogel có kh n ng h p ph Cu2+ t i đa 69.44 mg/g đ i v i m u đ 62.11 mg/g đ i v i m u đ c ho t hóa hóa h c c ho t hóa v t lý M t s k t qu h p ph Cu2+ đ t 69 đ c t v t li u quy trình khác đ đ tđ c t ng h p đ so sánh v i k t qu c t nghiên c u th hi n b ng 3.8 B ng 3.8 Kh n ng h p ph Cu2+ t i đa t nguyên li u khác Nguyên li u Tác nhân ho t hóa Kh n ng h p ph (mg/g) Carbon aerogels ph N Tác nhân nhi t đ 19.06 [124] 1300 oC Ho t hóa h i n c t i nhi t đ 900oC, Than ho t tính t h t oliu 25.38 [125] t=3.5h Carbon cellulose aerogels t s i d a s i cotton KOH 69.44 CO2 62.11 Carbon cellulose aerogels t s i d a s i cotton T đó, có th th y đ c q trình ho t hóa nh h ng l n đ n c u trúc c a v t li u Ho t hóa v i tác nhân v t lỦ ho c hóa h c y u t quan tr ng tác đ ng đ n ch t l ng c a carbon cellulose aerogel 70 CH NG K T LU N VÀ XU T 4.1 K t lu n T k t qu nghiên c u c a đ tài, có th rút m t s k t lu n nh sau: - V i nguyên li u s i d a s i bông, carbon cellulose aerogel đ c t ng h p s d ng trình ho t hóa hóa h c mang l i hi u qu h p ph cao h n nhi u so v i cellulose aerogel Do đó, đ tài nghiên c u t p trung vào giai đo n ho t hóa - Trong giai đo n ho t hóa th i gian tác nhân ho t hóa đ u nh h ch t l ng s n ph m u ki n nhi t đ 800°C, th i gian 1.5h t l KOH/C = đ i v i q trình ho t hóa hóa h c và l u l ng đ n u ki n nhi t đ 800°C, th i gian 15 phút ng CO2 100ml/phút đ i v i trình ho t hóa v t lý carbon cellulose aerogel có kh n ng h p ph methylene blue cao nh t - Carbon cellulose aerogel t ng h p đ c có SBET = 970.20 m2/g đ i v i m u ho t hóa hóa h c SBET =886.58 m2/g đ i v i m u ho t hóa v t lý Thích h p đ làm v t li u h p ph m t s ch t h u c nh methylene blue m t s kim lo i n ng nh Cu2+ K t qu h p ph c methylene blue Cu2+ phù h p v i h p ph đ ng nhi t Langmuir Kh n ng h p ph t i đa t ng ng 263 mg/g 250 mg/g đ i v i methylene blue, 69.44 mg/g 62.11 mg/g đ i v i Cu2+ 4.2 xu t - C n ti p t c nghiên c u, tính tốn nh m t i u c chi phí quy trình ho t hóa ng th i nghiên c u, s d ng tác nhân ho t hóa khác ngồi KOH CO2 - C n ph i nghiên c u đánh giá m t s ch tiêu đ m r ng vi c ng d ng carbon cellulose aerogel t ng h p đ c t s i d a s i - Các k t qu nghiên c u cho th y carbon cellulose aerogel t ng h p đ ct s i d a s i bơng có th s d ng nh v t li u h p ph giá thành th p, hi u qu thân thi n v i mơi tr ng Vì v y, c n đ c ti p t c nghiên c u ng d ng quy mô l n 71 TÀI LI U THAM KH O [1] [2] [3] [4] [5] [6] [7] [8] [9] [10] [11] [12] [13] [14] [15] [16] [17] D 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