I H C QU C GIA HÀ N I TR NG I H C KHOA H C T NHIÊN _ NGÔ H NG ÁNH THU NGHIÊN C U BI N TÍNH B M T MÀNG L C COMPOSIT POLYAMID L P M NG (TFC-PA) VÀ KH N NG NG D NG MÀNG TRONG X LÝ N LU N ÁN TI N S HÓA H C HƠ N i - 2017 C Ô NHI M I H C QU C GIA HÀ N I TR NG I H C KHOA H C T NHIÊN _ NGÔ H NG ÁNH THU NGHIÊN C U BI N TÍNH B M T MÀNG L C COMPOSIT POLYAMID L P M NG (TFC-PA) VÀ KH N NG NG D NG MÀNG TRONG X Chun ngành: Hóa Mơi tr LÝ N C Ơ NHI M ng Mư s : 62440120 LU N ÁN TI N S HịA H C NG IH NG D N KHOA H C: PGS.TS TR N TH DUNG PGS.TS SHINSUKE MORI HƠ N i - 2017 L I CAM OAN Tác gi xin cam đoan công trình nghiên c u c a b n thân tác gi Các k t qu nghiên c u k t lu n lu n án trung th c, không chép t b t k m t ngu n tài li u d ngu n tài li u đư đ i b t k hình th c Vi c tham kh o c th c hi n trích d n ghi ngu n tài li u tham kh o quy đ nh Tác gi lu n án Ngô H ng Ánh Thu i L IC M N V i lòng bi t n sâu s c, xin cho phép em dành nh ng dòng đ u tiên c a lu n án g i l i c m n chân thành nh t t i PGS.TS Tr n Th Dung, ng giao đ tài, t n tình h ng d n t o m i u ki n thu n l i nh t cho em su t trình th c hi n lu n án Em xin đ V i th y h n th y b i s h i đư ti p nh n, c g i l i tri ân chân thành nh t đ n cô ng d n th hai, PGS.TS Shinsuke Mori, em xin chân thành c m ng d n t n tình c a th y, đ c bi t th i gian em sang Nh t th c t p Em xin c m n th y v quà c a th y dành cho em Em c ng xin g i l i c m n chân thành t i th y khoa Hố h c, th y B mơn Cơng ngh Hóa h c, th y phịng thí nghi m Hóa Mơi tr ng đư truy n th cho em nh ng ki n th c quý báu, c ng nh đ ng viên, giúp đ , đóng góp giúp em nhi u ý ki n su t q trình em h c t p cơng tác Tác gi xin đ c c m n TS inh Hùng C ng, TS Tr nh Xuơn giúp tác gi đo đ c m u phân tích; xin c m n ThS i đư ình Kh i đư giúp tác gi r t nhi u v m t k thu t đ tác gi có th hồn thi n cơng trình Tác gi c ng xin đ c g i l i c m n t i Qu Phát tri n Khoa h c Công ngh qu c gia (NAFOSTED), ch ng trình 911 c a Chính ph Vi t Nam, Qu Ryoichi Sasakawa Young Leaders Fellowship Fund (Sylff), N i (VNU) Tr ng i h c Qu c gia Hà i h c Khoa h c T nhiên (HUS) đư giúp r t nhi u su t th i gian h c t p Cu i cùng, xin đ dõi theo t ng b c bày t lòng bi t n t i gia đình tơi, đ c bi t ng c đi, ng i m ch ng đư giúp đ r t nhi u, ng im i ch ng m t a v ng ch c, chia s m i khó kh n cu c s ng, gái đáng yêu t i ch em thân thi t, b n bè thân yêu c a Ngô H ng Ánh Thu ii TÓM T T LU N ÁN Màng l c composit polyamid l p m ng (TFC-PA) m t lo i màng đ c s d ng r ng rưi có tính n ng l c tách v h c, b nh h t tr i có đ b n c ng b i sinh v t Tuy nhiên, màng TFC-PA có nh c m d b t c ngh n trình l c tách, làm gi m hi u qu c a tồn b q trình màng Cho đ n nay, vi c nâng cao kh n ng ch ng t c mà khơng làm gi m tính n ng l c tách c a màng nói chung màng TFC-PA nói riêng v n m t thách th c l nh v c nghiên c u ch t o ng d ng màng l c Lu n án đư ti n hành nghiên c u bi n tính b m t màng l c composit TFC-PA b ng m t s ph ng pháp nh trùng h p ghép quang hóa d h p ghép kh i mào oxy hóa kh ph l p h t TiO2 kích th i b c x t ngo i, trùng c nanomet lên b m t màng, nh m nâng cao tính n ng l c tách kh n ng ch ng t c cho màng Các đ c tính b m t đ c tính tách l c c a màng đ t c kh o sát đánh giá, v i đ i ng tách l c m t s ch t h u c , vô c ion kim lo i n ng đ c h i n c Các k t qu nghiên c u cho th y q trình bi n tính b m t màng l c composit TFC-PA đư làm thay đ i rõ r t đ c tính b m t tính n ng tách l c c a màng Các u ki n bi n tính b m t màng nh n ng đ tác nhân ghép, th i gian trùng h p ghép, n ng đ ch t kh i mào, hàm l ng huy n phù TiO2 kích th kích thích b c x t ngo i (UV)… có nh h c nanomet, th i gian ng m nh đ n đ c tính c a màng T k t qu th c nghi m, có th rút u ki n bi n tính b m t màng thích h p cho hi u qu tách l c t t nh t màng trùng h p ghép quang hóa v i acid acrylic 10 g/L phút, màng trùng h p ghép kh i mào oxy hóa kh v i acid acrylic 10 g/L phút, màng trùng h p ghép quang hóa v i poly (ethylen glycol) 30 g/L 10 phút màng ph l p h t TiO2 kích th c nanomet 15 ppm, chi u b c x t ngo i 30 giây Ph h ng ngo i ph n x cho th y s xu t hi n nhóm ch c carbonyl, hydroxyl TiOH a n c b m t màng sau bi n tính, t iii ng ng v i tác nhân s d ng acid acrylic (AA), poly (etylen glycol) (PEG) TiO2 B m t màng tr nên a n c h n v i góc th m t gi m m nh, t 51o c a màng n n ban đ u xu ng kho ng 25o cho màng trùng h p ghép v i AA, kho ng 15o cho màng trùng h p ghép v i PEG, kho ng 33o cho màng ph TiO2 tr nên siêu a n th m t nh h n 10o cho màng ph TiO2 đ c v i góc c chi u b c x UV nh ch p hi n vi n t quét hi n vi l c nguyên t cho th y b m t màng sau trùng h p ghép tr nên ch t sít h n tr n nh n h n s hình thành l p polyme ghép, đ thô nhám b m t màng gi m xu ng rõ r t K t qu đánh giá đ c tính l c tách c a màng bi n tính b m t ch ng t s t ng lên đ ng th i c a c ba thông s g m đ l u gi , n ng su t l c kh n ng ch ng t c l u gi t ng kho ng %, n ng su t l c c a màng t ng t 35 đ n 60 %, m c đ trì n ng su t l c cao h n t 20 đ n 40 % so v i màng n n Màng sau bi n tính b m t có đ l u gi n đ nh kho ng pH t đ n 11, đ c bi t kh n ng ch u chlor ho t đ ng c a màng trùng h p ghép b m t tr nên t t h n nhi u so v i màng ban đ u Màng sau bi n tính b m t v i AA, PEG TiO2 kích th kh n ng tách lo i tri t đ ch t h u c t nhiên tan n c nanomet có c, c ng nh ion kim lo i n ng, amoni, cromat K t qu đánh giá v i m t s m u n c th i th c t cho th y, màng TFC-PA bi n tính b m t có th lo i b g n nh hồn toàn thu c nhu m d n c th i d t nhu m, protein ch t h u c d ch th i bia sau lên men, ion kim lo i n ng n đ c nâng lên đáng k so v i màng n n iv c th i m , v i tính n ng tách l c ABSTRACT The polyamide thin film composite (TFC-PA) membranes exhibit superior water flux and good resistance to pressure compaction They have wide operating pH range and good stability to biological attack Therefore, the TFC-PA membranes are widely accepted as the relevant choice for water treatments, especially for producing of the pure and ultrapure water However, the poor fouling restrain the filtration capacity and lifetime of the TFC-PA membranes, leading to an appreciable increase for operational costs of membrane processes Therefore, the simultaneous improvement of fouling resistance, flux and retention is still very challenging for the development of membrane applications In this work, the UV-photo-induced grafting, the redox-initiated grafting and the coating of titanium dioxide nanoparticles onto the surface of commercial TFC-PA membrane have been carried out to enhance the membrane separation performance and antifouling property The changes of the membrane surface characteristics were evaluated and the membrane separation performance were determined through the possibility for removal of organic and inorganic compounds, heavy metal ions in water The experimental results demonstrated that the grafting polymerizations and the coating of titanium dioxide nanoparticles led to changes in the membrane surface characteristics and membrane filtration performance The conditions of the modification of membrane surface such as monomer concentration, graft polymerization time, TiO2 concentration and UV irradiation time highly influenced on membrane characteristics From the experimental results, the most suitable modification conditions using acid acrylic (AA), poly (ethylene glycol) (PEG) and TiO2 nanoparticles for the membrane characteristics could be obtained: 10 AA-UV 7min, 10 AA-Redox 5min, 30 PEG-UV 10min and TFC-PA/TiO2,UV The FTIR-ATR analysis verified the appearances of hydrophilic groups such as carbonyl, hydroxyl and Ti-OH after grafting of AA, PEG or coating of TiO2 nanoparticles onto membrane surface The formation of the hydrophilic layer increased the hydrophilicity of membranes with the strongly reduced water contact angles, from v 51o of unmodified membrane to about 25o, 15o and 33o for the AA-grafted, PEG-grafted and TiO2-coated membranes, respectively The TiO2-coated membrane surface became super-hydrophilic with the contact angles are less than 10o The SEM and AFM images demonstrated that the grafted membrane surface is more relative compact and smoother after grafting The filtration experiments illustrated the improved separation performance of the modified membranes with the simultaneous enhancement of membrane flux and retention and antifouling property for separation of the different organic and inorganic substances in an aqueous feed solution The retention increased about %, while the membrane flux increased from 35 to 60 %, the antifouling property increased from 20 to 40 % compared to the unmodified one The modified membranes showed the stable retention for a wide range of pH from to 11, especially the chlorine resistance of the grafted membranes was significantly improved compared to the unmodified one The modified membranes using AA, PEG and TiO2 nanoparticles showed the good possibility for removal of the polluted substances such as the natural organic matter dissolved, heavy metal ions, ammonium, chromate in water The experimental results for the wastewater treatments indicated that the modified membranes could remove well the residual dyes, organic substances and metal ions in water, with the much better filtration performance compared to the unmodified one vi M CL C Trang L I CAM OAN i L IC M N ii TÓM T T LU N ÁN iii ABSTRACT v M CL C vii DANH M C T VI T T T x DANH M C HÌNH xii DANH M C B NG xvii M CH 1.1 U NG I ậ T NG QUAN Gi i thi u v màng l c trình tách b ng màng 1.1.1 Các trình màng đ ng l c áp su t 1.1.2 C ch tách qua màng 1.1.3 Màng composit polyamid l p m ng (TFC-PA) 1.2 ng d ng c a màng l c x lỦ n 1.2.1 ng d ng c a màng x lý n c ô nhi m b i m t s h p ch t h u c 10 1.2.2 ng d ng c a màng x lý n c ô nhi m b i ion kim lo i n ng 13 c ô nhi m m t s ion vô c khác 1.3 Hi n t ng t c màng trình tách l c 16 1.3.1 Hi n t ng t c màng 16 1.3.2 Hi n t ng t c màng tách l c dung d ch h u c 18 1.3.3 Hi n t ng t c màng tách l c dung d ch mu i vô c 20 vii 1.3.4 Các tính ch t b m t nh h 1.4 ng đ n m c đ t c màng 22 Bi n tính b m t màng l c 24 1.4.1 Bi n tính b m t màng l c b ng ph ng pháp trùng h p ghép 1.4.2 Bi n tính b m t màng l c b ng ph 27 ng pháp ph l p h t kích th c 39 nanomet 1.5 M c tiêu n i dung nghiên c u c a Lu n án 45 1.5.1 M c tiêu nghiên c u 45 1.5.2 N i dung nghiên c u 45 CH 47 NG II ậTH C NGHI M 2.1 Thi t b , hóa ch t, v t li u 47 2.1.1 Thi t b 47 2.1.2 Hóa ch t, v t li u 48 2.2 Ph 50 ng pháp nghiên c u 2.2.1 Bi n tính b m t màng 50 2.2.2 ánh giá đ c tính b m t màng 53 2.2.3 ánh giá đ c tính tách l c c a màng 54 2.2.4 ánh giá kh n ng ch ng t c ngh n c a màng 58 2.2.5 ánh giá kh n ng ch u pH, chlor ho t đ ng, nhi t đ , đ n đ nh c a 58 màng theo th i gian b o qu n 2.2.6 ánh giá kh n ng tách lo i thành ph n gây ô nhi m n CH 3.1 3.1.1 c c a màng NG III ậ K T QU NGHIÊN C U VÀ BÀN LU N Trùng h p ghép bi n tính b m t màng l c TFC-PA ánh giá đ c tính b m t màng TFC-PA tr c sau trùng h p ghép 59 60 60 60 3.1.2 Kh o sát đ c tính tách l c c a màng 75 3.1.3 Kh o sát kh n ng ch ng t c c a màng 81 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poly(-caprolactone) films using acrylic acid and collagen”, Biomaterials 25, pp 1991-2001 139 THÔNG TIN V TÁC GI Tác gi Ngô H ng Ánh Thu sinh ngày 17 tháng 04 n m 1987, t i Hà N i N m 2009, tác gi nh n b ng C nhân Cơng ngh Hóa h c n m 2012, tác gi nh n b ng Th c s Hóa h c t i khoa Hóa h c, tr i h c Khoa h c T nhiên – i h c Qu c gia Hà N i d d n c a PGS.TS Tr nh Lê Hùng Sau t t nghi p is h ng ng i h c, tác gi v làm công tác gi ng d y t i B mơn Cơng ngh Hóa h c, Khoa Hóa h c, Tr ng i h c Khoa h c T nhiên Hà N i Tác gi b t đ u làm nghiên c u sinh t tháng 09 n m 2013 th c hi n Lu n án d d n c a PGS.TS Tr n Th Dung PGS.TS Shinsuke Mori Email: anhthu@hus.edu.vn 140 is h ng ... ch t o màng V i tiêu đ "Nghiên c u bi n tính b m t màng l c composit polyamid l p m ng (TFC- PA) kh n ng ng d ng màng x lý n c ô nhi m“, Lu n án đ c p đ n vi c nghiên c u bi n tính b m t màng l... ng pháp nghiên c u 2.2.1 Bi n tính b m t màng 50 2.2.2 ánh giá đ c tính b m t màng 53 2.2.3 ánh giá đ c tính tách l c c a màng 54 2.2.4 ánh giá kh n ng ch ng t c ngh n c a màng 58 2.2.5 ánh giá... NGÔ H NG ÁNH THU NGHIÊN C U BI N TÍNH B M T MÀNG L C COMPOSIT POLYAMID L P M NG (TFC- PA) VÀ KH N NG NG D NG MÀNG TRONG X Chun ngành: Hóa Mơi tr LÝ N C Ô NHI M ng Mư s : 62440120 LU N ÁN TI N S