Tổng hợp nanocellulose từ phụ phẩm nông nghiệp và ứng dụng

I H C QU C GIA TP HCM TR NGă I H C BÁCH KHOA NGUY N TH XUÂN CHI T NG H P NANOCELLULOSE T NÔNG NGHI P VÀ PH PH M NG D NG SYNTHESIS OF NANOCELLULOSE FROM BIOMASS AND APPLICATION Chuyên ngành: K THU T HÓA H C Mã s : 8520301 LU NăV NăTH CăS TP H CHÍ MINH, tháng n mă2022 i CỌNG TRỊNH C HOÀN THÀNH T I TR NG I H C BÁCH KHOA ậ HQG -HCM Cán b h ng d n khoa h cμ PGS.TS Lê Th Kim Ph ng Cán b ch m nh n xét 1μ TS Tr n Ph c Nh t Uyên Cán b ch m nh n xét 2μ PGS.TS Ph m Trung Kiên Lu n v n th c s đ c b o v t i Tr ng i h c Bách Khoa, HQG Tp HCM, ngƠy 14 tháng 08 n m 2022 ThƠnh ph n H i đ ng đánh giá lu n v n th c s g mμ PGS.TS Nguy n Tr TS Tr n Ph ng S n - Ch t ch c Nh t Uyên - Ph n bi n PGS.TS Ph m Trung Kiên - Ph n bi n TS Ph m HoƠng Huy Ph TS Ph m Th H ng Ph cL i ng - Th kỦ - y viên Xác nh n c a Ch t ch H i đ ng đánh giá LV vƠ Tr sau lu n v n đư đ ng Khoa qu n lỦ chuyên ngƠnh c s a ch a (n u có) CH ăT CHăH Iă PGS.TS.ăNguy năTr NG TR NGăKHOAăK ăTHU TăHịAăH C ngăS n ii C NG HOÀ XÃ H I CH NGH AăVI T NAM I H C QU C GIA TP.HCM TR NGă c l p ậ T ậ H nh phúc I H C BÁCH KHOA NHI M V LU NăV NăTH CăS H tên h c viên: Nguy n Th Xuân Chi MSHV: 2070164 NgƠy, tháng, n m sinhμ 28/03/1λλ5 N i sinhμ V nh Long Chuyên ngành: K thu t Hóa h c Mã s : 8520301 I TểNă TÀI: Tên ti ng Vi t: ắT ng h p nanocellulose t ph ph m nông nghi p ng d ng” Tên ti ng Anh: ắSynthesis of nanocellulose from biomass and application” II N I DUNG TH C HI N:  nh h ng c a ph ng pháp c h c tách s i đ n trình thu h i cellulose t d a  Kh o sát nh h ng c a ph thu h i cellulose t d a ng pháp hóa h c ki m hóa vƠ t y tr ng đ n q trình  Kh o sát nh h b ng ph ng c a thông s công ngh đ n trình t ng h p nanocellulose ng pháp th y phơn acid  T ng h p mƠng biocomposite III NGÀY GIAO NHI M V : 1/2022 IV NGÀY HOÀN THÀNH NHI M V : 6/2022 V CÁN B H CÁN B NG D N: PGS.TS LÊ TH KIM PH NG TP.HCM, ngƠyầthángần m 2022 H NG D N CH NHI M B MỌNă ẨOăT O PGS.TS Lê Th Kim Ph ng PGS.TS Lê Th Kim Ph ng TR NG KHOA K THU T HÓA H C iii L I C Mă N hoàn thành lu n v n nƠy, đ u tiên tác gi xin trân tr ng g i l i c m n sơu s c chơn thƠnh đ n PGS.TS Lê Th Kim Ph ng đư tr c ti p h ng d n, h tr r t nhi u cho tác gi v ki n th c c ng nh tinh th n 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 Trung tâm Nghiên c u Cơng ngh L c Hóa D u (RPTC), Tr ng i H c Bách Khoa - HQG TP.HCM đư h tr tác gi su t trình h c t p nghiên c u Bên c nh đó, tác gi xin g i l i c m n đ n gia đình, ng i thân đư quan tơm, đ ng viên, 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 nƠy Cu i cùng, tác gi xin c m n Trung tơm Nghiên c u Cơng ngh L c Hóa D u đư h tr kinh phí hóa ch t phân tích, xin c m n Tr ng i h c Bách Khoa ậ TPHCM đư h tr trang thi t b cho nghiên c u Tác gi Nguy n Th Xuân Chi iv HQG ậ TÓM T T Trong lu n v n nƠy, nanocellulose (NC) đ c t ng h p t d a v i ph ti n x lỦ c h c k t h p hóa h c (ki m hóa, t y tr ng) vƠ ph m i giai đo n t ng h p đ u đ nh h ki n t ng h p phù h p ng pháp th y phân acid c ti n hành kh o sát luân phiên t ng bi n đ tìm u ng c a y u t thu h i cellulose bao g m q trình ki m hóa v i NaOH t y tr ng H2O2 đư đ ng, t l r n ậ l ng T ng pháp ng t , nh h ng c a y u t t ng h p NC bao g m: th i gian, nhi t đ t l r n ậ l ng c ng đ v t li u cellulose NC phù h p đ c kh o sát nh μ n ng đ , th i gian ph n c kh o sát C u trúc - hình thái - đ c tính c a c xác đ nh b ng ph ng phápμ đ nh l ng carbonhydrate NREL, kính hi n vi n t quét, ph h ng ngo i chuy n hóa Fourier, phân tích nhi t tr ng l b kích th l ng TGA, nhi u x tia X, kính hi n vi n t truy n qua, phân c h t DLS K t qu t ng h p NC cho th y, d a sau ti n x lý có hàm ng cellulose lên đ n λ8,0λ%, đ k t tinh lên đ n 76,95% Sau thu phơn, NC có đ k t tinh t ng lên 84,31%, NC có chi u dài kho ng 100 - 300 nm chi u r ng t 10 - 50 nm S n ph m NC t ng h p đ vƠo gia c tr c k t h p v i polyvinyl alcohol chitosan ng d ng ng v t li u biocomposite MƠng biocomposite đ ng mƠng vƠ ph ng pháp xác đ nh c u trúc, đ c tính nh ph h ng ngo i chuy n hóa Fourier, phân tích nhi t tr ng l tr ng n c đánh giá đ b n kéo, đ ng K t qu cho th y, b sung thêm NC đ c gi m đ n 160% trì m c 280% gi g n l n so v i màng khơng có NC D a vào nh ng k t qu thu đ b n kéo t ng c, ph ng pháp có th phát tri n đ thu h i NC có giá tr cao t ngu n nguyên li u d a th i, NC có ti m n ng l n gia c ng c u trúc màng biocomposite v ABSTRACT In this study, nanocellulose (NC) is synthesized from pineapple leaves (PLs) with mechanical and chemical pretreatment methods (alkaliization, bleaching) and an acid hydrolysis method At each synthesis stage, each variable is alternately surveyed to find suitable synthesis conditions The influence of cellulose extract factors including alkalization with NaOH and bleaching by H2O2 were investigated, such as concentration, reaction time, and solid-liquid ratio Similarly, the effects of NC synthesis variables such as time, temperature, and solid-liquid ratio were studied The structure - morphology characterization of cellulose and NC samples were studied by determination of structural carbohydrates and lignin in biomass (NREL), scanning electron microscope, Fourier transform infrared spectroscopy, thermogravimetric analysis (TGA), X-ray diffraction, transmission electron microscopy, Analysis of Particle size distribution (DLS) The results of NC synthesis showed that PLs after pretreatment had cellulose content up to 98.09%, and the crystallinity (CrI) reaches 76.95% After hydrolysis, CrI increases to 84.31%, the length of NC was about 100-300 nm and a width of 10 - 50 nm Synthetic NC products are mixed with polyvinyl alcohol and chitosan applied to strengthen biocomposite materials Biocomposite films were evaluated for tensile strength, film swelling and structural determination methods, such as Fourier transform infrared spectroscopy and thermogravimetric analysis The results showed that, when adding NC, the swelling in the water of the biocomposite membrane decreased to 160% and remained at 280% for hours Tensile strength is increased by almost times compared to films without NC Based on the obtained results, methods can be developed to recover high-value NC from waste pandan leaf material NC has great potential for structural reinforcement for biocomposite films vi L IăCAMă OAN Tác gi xin cam đoan lu n v n nƠy lƠ cơng trình nghiên c u th c s c a cá nhân tác gi vƠ 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 (RPTC), Tr ng i H c Bách Khoa - HQG TP.HCM Các s li u, k t qu nghiên c u lu n v n nƠy lƠ hoƠn toƠn trung th c, ch a t ng đ c công b b t c m t công trình nƠo khác tr hồn thành lu n v n nƠy đ u đư đ đ u đư đ c đơy M i s giúp đ cho vi c c c m n, thơng tin trích d n lu n v n nƠy c ch rõ ngu n g c Tác gi xin ch u trách nhi m v nghiên c u c a Tác gi Nguy n Th Xuân Chi vii M CL C L I C M N iv TÓM T T v ABSTRACT vi L I CAM OAN vii DANH M C HÌNH xi DANH M C B NG xiv DANH M C CH L IM VI T T T xv U T NG QUAN V t li u nano 1.1.1 Khái ni m 1.1.2 Phân lo i T ng quan nanocellulose 1.2.1 S l 1.2.2 Phân lo i nanocellulose 1.2.3 c tính nanocellulose c nanocellulose 1.2.4 Ph ng pháp thu h i cellulose 1.2.5 Ph ng pháp t ng h p nanocellulose 14 ng d ng nanocellulose vào v t li u composite 21 T ng quan d a 23 1.4.1 Tình hình phát tri n, s n l 1.4.2 Thành ph n c a d a 24 ng khai thác d a viii Vi t Nam 23 1.4.3 Ph ng pháp ti n x lỦ c h c d a 25 Tình hình nghiên c u vƠ ngoƠi n c 27 TH C NGHI M 32 it ng, n i dung nghiên c u 32 Hóa ch t, d ng c , thi t b , đ a m th c hi n 32 2.2.1 Hóa ch t 32 2.2.2 D ng c thi t b 32 2.2.3 a m th c hi n 33 Ph ng pháp nghiên c u 33 2.3.1 Thu h i cellulose 34 2.3.2 T ng h p nanocellulose 39 2.3.3 T ng h p màng biocomposite 41 Ph ng pháp phơn tích đ c tính, hình thái, c u trúc v t li u 42 K T QU VÀ BÀN LU N 50 K t qu thu h i cellulose 50 3.1.1 ánh giá nh h ng trình ti n x lỦ c h c (tách s i) 50 3.1.2 K t qu kh o sát q trình ki m hóa 54 3.1.3 K t qu kh o sát trình t y tr ng 58 K t qu t ng h p nanocellulose 65 3.2.1 Kh o sát th i gian th y phân 65 3.2.2 Kh o sát t l r n ậ l ng 67 3.2.3 Kh o sát nhi t đ ph n ng 69 K t qu t o màng biocomposite 75 ix 3.3.1 Phân tích hình thái b m t SEM 75 3.3.2 Phân tích FTIR 76 3.3.3 Phân tích TGA 77 3.3.4 Kh i l 3.3.5 tr ng ng su t kéo 78 ng n c 79 K T LU N 81 DANH M C CÁC CƠNG TRÌNH KHOA H C 82 TÀI LI U THAM KH O 83 PH L C 94 LÝ L CH TRÍCH NGANG 99 x [23] A A Elgharbawy et al., "Ionic liquid pretreatment as emerging approaches for enhanced enzymatic hydrolysis of lignocellulosic biomass," Biochemical Engineering Journal, vol 109, pp 252-267, 2016 [24] S H Mood et al., "Comparison of different ionic liquids pretreatment for corn stover enzymatic saccharification," (in eng), Prep Biochem Biotechnol, vol 44, no 5, pp 451-63, 2014 [25] H P S Abdul Khalil et al., "Green composites from sustainable cellulose nanofibrils: A review," Carbohydrate Polymers, vol 87, no 2, pp 963-979, 2012 [26] H Sangian et al., "Preparation of Reducing Sugar Hydrolyzed from High-Lignin Coconut Coir Dust Pretreated by the Recycled Ionic Liquid [mmim][dmp] and Combination with Alkaline," Bulletin of Chemical Reaction Engineering & Catalysis, vol 10, 2015 [27] F G Calvo-Flores et al., "Structure and Physicochemical Properties," in Lignin and Lignans as Renewable Raw Materials: Chemistry, Technology and Applications, V Stevens, Ed Belgium: Wiley, 2015, pp 9-48 [28] A P Abbott et al., "Deep Eutectic Solvents formed between choline chloride and carboxylic acids: Versatile alternatives to ionic liquids," Journal of the American Chemical Society, Article vol 126, no 29, pp 9142-9147, 2004 [29] A Satlewal et al., "Natural deep eutectic solvents for lignocellulosic biomass pretreatment: Recent developments, challenges and novel opportunities," Biotechnology Advances, vol 36, no 8, pp 2032-2050, 2018 [30] C Capello et al., "What is a Green Solvent? 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HQG Tp.HCM Chuyên ngành: K thu t Hóa h c Q TRÌNH CƠNG TÁC  T 04/2019-05/2020: Nhân viên R&D t i công ty TNHH S n xu t vƠ Th ng m i T ng h p Vi t My  T 11/2020-05/2022: Nghiên c u viên t i Trung tâm Nghiên c u Cơng ngh L c hóa d u 99 ... 1.1.2 Phân lo i T ng quan nanocellulose 1.2.1 S l 1.2.2 Phân lo i nanocellulose 1.2.3 c tính nanocellulose c nanocellulose 1.2.4 Ph ng pháp... m u nanocellulose 72 Hình 3.23 Hình nh TEM m u nanocellulose 72 Hình 3.24 Ph FTIR Cellulose nanocellulose (NC) 73 Hình 3.25 Gi n đ nhi u x tia X c a m u Cellulose nanocellulose. .. diffraction Nhi u x tia X CNF Cellulose Nanofibers S i Nanocellulose CNC Cellulose Nanocrystals Tinh th Nanocellulose NC Nanocellulose Nanocellulose PL Pineapple leaf Lá d a thô PF Pineapple