TAP CHI HOA HQC DOI: 10.15625/0866-7144.2015-00137 T 53(3) 322-326 THANG NAM 2015 NGHIEN COU PHAN U'NG TRANS-ESTE HOA TRONG Sly CO MAT CUA XOC TAC CHAT LONG ION Pham Thi Nam Binh*, Ding Thi Thuy Hanh, Vfi Thi Thu Hi, DO Thanh Hai, Trtin Van Hien Phong TNTD Qudc gia ve Cling nghe 1QC - haa dazi, Vien Haa hQc Cong nghi Op Viet Nam Den Tea soan 17-11-2014; Chip nhan clang 20-6-2015 Abstract Transesterification reaction between refined coconut oil and methanol was investigated in the present of ionic liquid 1-(4-sulfonic acid) butyl-3-methylimidazolium methane sulfonate as catalyst The results show that the methyl esters content of product exceeds 88 % at 75 °C for hours with methanol/oil/catalyst molar ratio of 12:1:0.15 This catalyst can be recovered and reused So it has potential application in transesterification process Keywords FAMEs, ionic liquid, transesterification, coconut oil I MO DAU Ilea not tren Bai bao glen thiau cac kat qui nghien ciru Cong nghe truyen dicing san xuat metyleste tong hop, dac trtrng vi thir nghiam hoat tinh Vic tac cita cac axit beo (FAMEs) irng dung san xuat dm met se IL ten ca sec imidazolium tong phan nhien lieu sinh hoc di tir nguon dau men d6ng, thuc ting trans-este hoa nguyen lieu triolein va dau dira vat cong nghe' sir dung Vic tae kiem deng the tinh luyen Cling ngh'e rat phut hop vai nhang nguon nguyen lieu co ham *mg nu& va axit beo W thfip Vai THVC NGHIEM cac nguyen lieu ca ham ltrqng axit beo cao (thuang la cac nguyen lieu re tien, khong canh tranh yeti 2.1 H6a chat va thiet bi nguon lacing th,rc), ding nghe cho hieu qua khong cao Ben canh do, 'dm tac ding the co nhtrqc Cac Ma chit dung tong hqp IL, triolein va diem la kh6ng thu h6i duct sau phin img, an mon metanol co nguon gOc tir Sigma-Aldrich va thiet bi va gfiy o nhiem mei twang nen khOng dap Spectrum China duqc sir dung uvc tiep, kh6ng qua ling &roc cac tieu chi dm Floa hoc xanh Vi vay, btrac tinh che viec fiat kiem cac cong nghe va Vic tic mai, co kha DAu dira tinh luyen (tri s6 axit 0,25 mg KOH/g) nang chuyen hoa clang thai Ca axit beo tar va co nguon gee tir Cong ty Dalt Ttr?yng An, Viet Nam triglyxerit thinh FAMEs tra nen rat can thiet: Theo Cac IL sau tong hop dtrqc dac tnmg cau true do, cac qua trinh sir dung xfic tac axit di the dtrqc bang phtrang phap ph6 cong huang tir hat nhfin tren quan tam nghien ciru chfing di the xfic tac cho ca may Brucker AVANCE-500 MHz va Brucker AVANCE-250 MHz va dac trung tinh chAt nhiet hai phan fing este Ma va trans-este h6a [1-7] Cac nghien ciru tren the giai cho thAy chit long troll may DTG-60H Shimadzu ion (IL) vai vai tro Vic tac c6 rat nhieu tru diem nhtr khong yeu au chat che ve tri se axit nguyen 2.2 'ding hop ILs lieu ban diu, tach khoi san phfim sau phan tang va co kha nang tai sir dung nhieu Fan [3-7] (3 Viet Nam 2.2.1 Tang h9p 1-metylimidazolium hydro sulfat co met s6 nghien ciru trien khai ve qua trinh san xuat Nho giQt dung dich ntrac china 0,2 mol FAMEs sir dung xfic tac di the tren ca ser ding nghe gOc dm Han Quoc [8, 9] ve IL, co the ke den met H2Sa4vao 0,2 mol N-metylimidazol (mim) da dtrqc so nhorn Lie gia nghien ciru tong hop, dac va lam lanh san ye °C dieu kien co khufiy Sau img dung cila IL nhu P T S Nam [10], L N Thach de khuAy hiln hop phan img trong, gia a nhiet de [11, 12], B T L Thiry [13, 14] Tuy nhien chtra ca phong Ket tit& phin img, san phfim duqc say a 90 nghien ciru naolien quan den tang hqp va img dung °C dtrai ap suAt 0,1 Bar 12 gia de loai be mat cac )(ix the IL cho phan (mg este Ilea va trans-este San phfim thu ducc la cac chat long khong mau hoac 322 Pham Thi Nam Binh va Ong sy- TCHH, T 53(3), 2015 yang nhat, sanh 2.2.2 Tong hop 1-ankyl-3-metylimidazolium hydro sulfa! (C„miniHSO4) Ket qua khao sat hoot tinh xUc tic cua cac ILduqc trinh bay teen hinh Ham lucrng metyl este cua san pham cang Ion thi hoat tinh cua Vic tac IL ttrang ling cang cao 30 Phucrng phap tong hop CnmimHSO4 ducrc thvc hien nhu mo to [15] 2.2.3 Tdng hop 1-(4-sulfonic axit)buty1-3metylimidazolium metanesulfonat mimC4H8S03H.CH3S03va 1-(4-sulfonic axi0butyl3-nietylimidazolium hydrogen sulfat mimC414503H.HSO4 CA 20 E ft 10 04 Nho gipt 1,4-butan sulton vao mim theo ty le mol 1:1 nhiet dO phang, sau khuay hon hcrp phan ling a 50 °C cho den (long ran hoan toan Rim chat ran thu throe bang dietyl ete va sAy chan khOng a 60 °C gia Nh6 tir tir dung djch axit CH3S03H (99,5 %) hoac H2SO4 (98 %) vao chAt ran thu duqc theo ty le mol 1:1 a °C, sau khuAy lion hop u 80 °C cho den hoa long hoan toan Rira san phAm bang dietyl etc va sAy tit say a 60 °C dual ap suAt 0,1 Bar San pham thu dtrqc la cac chat long co mau yang nhat, sanh 2.2 Phan irng trans-este hoa Phan ling dirge tien hanh binh eau ea' dun* tich 100 ml co trang bi sinh han, nhiet ke va khuay tir Tec de khuay duqc giir kh6ng doi (500 yang/phut) mpi thvc nghiem Nguyen lieu triolein duqc sir dung phan ling trans-este h6a de danh gia hoot tinh cua cac xuc tac a cling met diet' kien phan ling (75 °C, gia, ty le mol metanol/triolein/xiic tac = 9/1/0,15) Nguyen lieu dAu diva tinh luyen &roc sir dung de nghien ciru phan 1mg trans-este hoa sir c6 mat dm IL co hoot tinh mac tac cao nhat Thy trang thirc nghiem ma mau duqc lAy.dinh kY Ham metyl este cita cac mau san pham duqc xac dinh bang GC-MS theo tieu chuan EN-14103 Tnrirc phan tich, mau san pham &roc xli IY bang phuong phap chiet vai hon hop ntrac va n-hexan theo tY le the tich 1:1 Doi vai cac thkrc nghiem nghien c(ru kha nang tai sir dung dm xiic tic, x6c tac se' &rot thu hai, tinh the va sir dung quay yang cho phan ling a cling diet' kien KET QUA VA THAO LUAN 3.1 Sing luc vac tic IL cho phin irng trans-este hoa E cb,s s Looi 'dm Co s', , Hinh 1: Ket qua khao sat hoot tinh Vic tac cita IL Co the thAy rang hoat tinh )(Ix tac cua mimC4H8SO3H.CH3SO3 cao nhAt, sau den mimC4H8S03H.HSO4 Cie IL c6 hoot tinh cao hon han so vai cac xac tac IL can loi Dieu c6 the giai thich la chang dtrqc "bo sung" tam axit cation (nhom SO3H), dan tai lam tang manh hoot tinh xtic tac Doi vai nhom IL co cling anion HSO4 nhtmg khac ve d6 dai mach ankyl nhom the a cation, quan sat thAy sir tang hoot tinh xtic tac theo trot tir dm day sau: HmimHSO4 < C4mimHSO4 < C6mimHSO4 < C8mimHSO4 < ClomimHSO4 Nguyen nhan sir tang hoot tinh xuc tac a day hilt la sir tang d6 axit de dal mach ankyl tang [3] Nhu vay, s6 cac IL dtrac khao sat, mimC4H8SO3H.CH3SO3 co hoat tinh x6c tac cao nhat, ham Itrang metyl este dm san pham dot 26,95 % thai gian gia X6c tac dirge lira chpn de nghien ciru phan ang chuyen Ma este tir dau dira tinh luyen 3.2 Cic yeu to inh hurting den phin ling trans- este h6a dttu dira sir dung 'cue tic mim C4H8SO3H.CH3SO3 3.2.1 T.)) le mol xuc tac/ddu Ket qua khao sat dtrac bieu din hinh Hieu qua phan 1mg thay doi r6 ret tang Itrang xuc tac Khi ti le )(lie tac/dau tang tir 0,05 len 0,15, ham Wang metyl este dm san pham tang tir 32,35.% len 74,60 % Ham Itrang metyl este dm san pham khong tang nhieu tang t3 le xac tacklAu len tren 323 TCHH, T 53(3), 2015 Nghien caw ',hem zing trans-este h6a gia trj 0,15 Do do, ti lg mac tic/6'u duqc Iva chon IA 0,15 _ 3.2.3 Nhiet d() Anh twang cua nhiet d$ den phin (mg &Km the hien tren dO thi hinh 100 80 4.) 100 64 ▪ 80 al p 60 E.