4 CATtech-3 Dac trung xuc tac NOi dung a 1. Gidi thigu 2. Cac tinh chat héa ly téng quat 3. Cac tinh chat bé mat va Id xép 4, Ham lugng tam hoat tinh xuc tac o Catalyst characterization 1. GIO! THIEU a 1. GIO! THIEU a Vat ligu = “chat xc tac tot” néu: Vat ligu = “chat xc tac tot” néu: (0. Thé hign 46 chon Igc cao déi voi sn phim mong musn va ‘idm thiéu sy tao thanh céc san phém phu. (Selectivity) (i):Th8 hin a bén (tub the) a Ku trong du kign phan ong hhoge co iné ta sinh wo fal sau mi mot thot gian nga sr dung. (Stability) (i) Tée ag phan ang trén chét xac tae pha 30 nhanh trong {Bu Kiba eda quy rink phan ng (Aetivity) (iv) Céu trac vat ligu cho phép qua trinh di chuyén clia tac chat va sn pham dén cac. tam hoat tina d& dang, tir dé cé thé thu duoc téc 46 phan ng cao cho méi thé tich thiét bi phan tng.1. GIO! THIEU a Die trung cua chat xc tic (cotalyst charactorization) (0) Céc tinh chat héa ly t8ng quat: thanh phan, edu trde pha, KhSi lugng riéng, dé ber co. (ii) Cac tinh chat b& mat va 18 xép: hinh thai, bB mat ring, thé tich 15 x6p, phan bé kich thc 16 xép (ii) Ham lremng ede eu tit hoat tinh: TPR, TPD 2. Cac tinh chat héa ly tang quat ‘Thanh phan (composition) * Phan tich hoa hoc hay héa ly + Phan tich pha hily hay khong pha hay mau 2. Cac tinh chat héa ly tang quat ‘Thanh phan (composition) (0 XRF (X-rey Fluorescence) (ii) AAS (Atomic Absorption Spectroscopy) (iil) AES (Atomic Emission Spectoscopy) ICP AEE (Inductively Coupled Picoma -AEB) 2. Cac tinh chat héa ly tang quat ‘Cau tric pha Phuong phap XRD (X-ray diffraction) ees) a as2. Cac tinh chat héa ly tang quat ‘Cu trac pha ‘eof 0 Phuong phap chuong trinh nhigt do i (Temperature Programmed methods) g TGA hay TG (Thermal Gravimetric analysis): 3 Ghi nhan sy gidm hoac tang khéi lng Khi gia 0 | nhigt mau theo mét t6c 46 xac dinh trong dong a hi tror (Np, He,...) a So sanh voi mu chun dé dinh danh cu truc. a aan eee 2. Cac tinh chat héa ly tng quat 2. Cac tinh chat héa ly tang quat Khéi lwgng riéng [kndI lng riéag = Khéi lwongidon vi thé tich (") 04 loai khéi lurgng riéng cuia chat rén (ASTM): (i) KLR ly thuyat (theoretical density) (d,) TiIé khéi lng cla cac phan ri rac voi tng thé cac mau do. KLR nay thu@ng dugc xac dinh dya vao thong s6 mang tinh thé xac dinh tu phan tich XRD Cén goi la KLR XRD hay KLR 6 co 50 (unit cell) It 06 ting dung trong thyre 18 2. Cac tinh chat héa ly tng quat Khéi long riéng KLR khung (skeletal density) (d,) Thé tich dug dinh nghia bao gém tong thé +h clia vat ligu ran va cac 16 x6p bén trong vat liéu (closed pores). Khéng cé Iwu chat nao cé thé di vao cac 16 x6p nay. Cac 8 nay tro thanh mét phan cia vat lieu.2. Cac tinh chat héa ly tng quat Khéi long riéng (i) KLR khung (skeletal density) (,) ach do ‘ ~ Met kh6i trang xt te cho vao trong binh dong thé ‘i = Xae dinh thé tich He can thiét a6 didn gay binh dong 2 The tich hat rn Ta higu thé tich binh va thé tich He (Cho ld phai losi hét hoi Am trong mau Con goi la KLR theo He (He density) 2. Cac tinh chat héa ly tng quat Khéi long riéng (ii) KLR hat (particle density) (4,) Thé tich [a thé tich cla vat ligu ran, 18 x6p ben trong, va bén agoai cia hat xtic tac. Thuéng goi la KLR theo Hg (Mercury density) 2. Cac tinh chat héa ly tng quat Khéi long riéng (i) KLR nat (particle density) (4) Cach do: ne - Su dung Juru chat bu thé tich la loal 6 kich thude ion, khong di vaw bén tony Gat 16 x6p eta hat xc tac. ~ Cling c6 thé hp phu true mot chdt khac (vi dy methanol), rdi mdi tién hanh do thé tich ~ Hg thueng ding lam luu chat bu thé tich trong trong hgp nay. (Hg khong vao dug cac 16 x6p kich thuéc <1,2 um 6 didu kién ap suat thong) 2. Cac tinh chat héa ly tong quat Knéi lwong riéng KLR hat (particle density) (d,) D6 x6p (porosity): B= (1- df) = Vpoe! Victat 42. Cac tinh chat héa ly tng quat Khéi long riéng (iv) KLR kh6i (bulk density) (4,) Thé tich bao gdm cA thé tich cac ahan tréng gira cc hat. Thé tich nay phy thudc nhiéu yéu 6: loai binh chira, phurong phép 46 déng (packing), ... Wat TG ete) Ti lé khoang tréng (void fraction): z a gi a 7a gen ood) a (1-d/d,) oroa e049 rms » rms a 2. Cac tinh chat héa ly tng quat Khéi long riéng Vi ou: vi du ve RuReba nic tae 7.6 MUA KLR Gist Lythuyét | 5.89 g/cm (sole) Khung 2.99 g/cm? (solid + closed pores) 2. Cac tinh chat héa ly tng quat 186 bin co (crushing strength) Kha nang chiu lye ép cua vat ligu xic tac. Bi véi hat xtc tac (pellets): idm tra chiéu doc truc (axial crushing test) Kiém tra chiéu huéng kinh (radial crushing test) 2. Cac tinh chat héa ly tng quat ‘D6 bin co (crushing strength) Théng ke tile nat b| vé theo chiéu doc truc hay chiéu huéng kinh voi cdc Ic ép (ap suat ép) rndo do (ti yeu cu dat ra) Knoang old tr ap sudt ep: Axial test: 10 100 kglom? Radial test: 1 ~ 10 kglom?2. Cac tinh chat héa ly tng quat 6 bin co (crushing strength) -khdi hat xc tdc (bulk): = Kh6i hat dat trorg binh chifa hinh try (t em) (=100 cm) ~ Logi hai ém bang nung trong Khong, ki 200° trong 3 3i6 Duy tr dp sua c6 dinh (tue 3 ~ 30 atm) trong 1 phit. = Ray qua ray tiy theo kich thud hat: (0.8 mm (40 mesh), 1.6 mm (20 mesh) 2.5 mm (12 mesh); 6.5 mm (4 mesh) 2. Cac tinh chat héa ly tong quat ‘D6 bin co (crushing strength) ‘Béi v6i khéi hat xie tae (bulk): (4) -Phén tram kot qua ray duige ghi nhan 6 ting gia tr ap sudt ép khac nhau. + Gia tri d6 bén co ( crushing strength) la ap sudt ép cn 48 tao b6t chiém 1% khdi long kndi xtc tc 4 2. Cac tinh chat héa ly tng quat ‘6 bin co (crushing strength) 2. Cac tinh chat héa ly tong quat Hinh thai (Morphology) - Hinh dang va kich thuée ctia cc tinh thé chat xuc tac - Sy phan bé kich thuec hat tinh thé 42. Cac tinh chat héa ly tng quat inh thai (Morphology) Phan tich kinh hign vi ign wu quét SEM {Scanning Electron Microscopy) 2. Cac tinh chat héa ly tng quat ih thai (Morphology) Phan tich kinh hién vi dién té truyén qua TEM (Transmission Electron Microscopy) 2. Cac tinh chat héa ly tng quat inh thai (Morphology) Phuong phép XRD XRD cén ding trong xac dinh kich thc hat tinh thé hoat tinh néu néng 46 cac hat nay Ia dui len, Phuong trinh Scherror: KA 080 4: kichthuge trung bah K: hdng s6 (0.9-.0) : 2: bude séng X-ray (0.154 am- ‘Cuka) ;f (rad): bé rong peak tai % ciu cao max, 6 (rad): g6c nhieu xa 3. Cac tinh chat bé mat va 6 xép fH Dién tich bé mat (Surface area) ¥ DTBM dug do bang phuong phao hap phy vat ly (khac voi hdo phy héa hoc) ¥ Twong tac do lye Van der Waals gia céc phan tr luu ch&t w6i b& mat ¥ Sy bao phii 98 mat co thé tao ra nhibu lop ~ Qua trinh la sa nhiét va lugng chat hap phy & trang thai cn bang giam khi tang nhiét 46 ¥ Thuong do tai nhiét dO gan nhiét ¢6 sdi cua luu chat3. Cac tinh chat bé mat va 6 xép fH ign tich bé mat (Surface area) Dién tich bé mat (Surface area) Duong ding nhigt can kang © ap sudt thdp. sy hint Urant don lop theo phugng . trinh Langmuir: i ave /po) i Ta + Kell j =o Vy: thé tch eta lp du tién (monolayer) . K: hang sé P: ap suat ca kni Po: Ap sudt bao hoa cia khi tai nhigtdd do orm » rms » 3. Cac tinh chat bé mat va 6 xép fH 3. Cac tinh chat bé mat va 6 xép fH ign tich bé mat (Surface area) Kh &p sudt ting (ppy > 0-1) sy ngung ty da lop (multilayer) tang dan. Mé hinh cho twéng hop nay la BET (Brunauer, Emmett, va Teller) voi phuong trinh BET: 2. Cac tinh chat bé mat va 6 xdp fH Dién tich bé mat (Surface area) ep Van [po = plll +(e = 1) pipo) se 2 1-1) Vim=p) Vue? Vue too) fet torn ry con sa gh ee tothe faut vm 2 (ip)3. Cac tinh chat bé mat va 6 xép fH Dign tich bé mat (Surface area) conn ana et E tet i ono rate hy we Te ic 3. Cac tinh chat bé mat va 6 xép fH Dién tich bé mat (Surface area) 3. Cac tinh chat bé mat va 6 xép fH ‘Sur phan b6 1d x6p 3. Cac tinh chat bé mat va 6 xép fH ‘Sur phan b6 1d x6p 'Sé cung cp théng tin vé: mirc d6 tro’ irc khuéch tan, ee) oun Gidu khién qua tinh dau doc xc tac. a = Macroporethuting dure do bang hap phs Ho a=! “ (Mecury Porosity) = Mesopore thuéng durge do bing hap physi hp Ne woe —— rms ss yma »3. Cac tinh chat bé mat va I6 x6p sur phan b6 18 x6p Hg Porosimetry CCT 1 ex 3310 165 rT é 410) s (te: Rehan fe Pec tt eet Sein 1989) vm. 3. Cac tinh chat bé mat va I6 x6p Sur phan b6 18 x6p ‘B6i véi mesopore: (2-50 nm) St dung phuong php ngung ty mao quin trong phan tich hip phu/eiai hip N. Phuong phap churdng dung la BIH (Barre -leynerHalenda), OFT, 4, Ham luong tam hoat tinh xtc tac GY 7am host tinh 18 kim logi Thuong ding phurong —Seewinw weet Fee) phdp TPD en cra S| (Temperature Programmed ca a0 Desorption) co om oo 6% chat dd la see CO/H,/0,/N,C ae lieu yen hiya chon chat dd % NS diing 8 tranh céc phan img SE hhéa hoc xay ra yma Low dapersion Mh dispersion a se Tyee nen Sa4, Ham luong tam hoat tinh xtc tac GY “im hoat tinh fa kim oat Vi dy: ding CO-TPD d@ xéc dinh s6 long tam Pt ‘rn xtic téc PH/AL,O, 1 Lam Pte 4 phan te CO Xéc dinh lugng CO => Sé lugng tam Pt giai hap phy 4, Ham luong tam hoat tinh xtc tac GY Tam hoat tinh fa oxt kim tai ‘Thuong ding phurong phdp TPR (Temperature Programmed Reduction) Dang khi la : H,/He (N,, Ar) Phan ting héa hoe: xH, +M,0, “> 2M +xH,0 Xéc dinh lang H, $6 wong tam phan ting hoat tinh 4, Ham luong tam hoat tinh xtc tac GY Tim hoat toh Ia HY (xe din 9 acid) Thuéng ding phwong phap NH,-TPD os 2 bd rose 39 co 4, Ham luong tam hoat tinh xtc tac GY Tim hoat toh Ia HY (xe din 9 acid) Phuong phap NH,-TPD Luu y: (i) 86 long tam = Iugng NH, gidi ho phy (i) Tay theo digu kign gidi Rp phu ma cé thé bao gm mot phan NH, hép phy vat I (i) 86 manniyéu cia cdc tam acid thé hign qua gia tr nhiét d6 cia céc peak trong dung gidi hap phy. (iv) Kho phan biét tam acid Lewis va Bronsted