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TNG HP ZEOLITE A T KAOLIN BNG PHNG PHP THY NHIT

L Thanh Phc1 v La Vn Thi1

ABSTRACT
Zeolite A, a white powder, was synthesized by the hydrothermal reaction of activated kaolin (metakaolin) derived from commercial kaolin, a low cost mineral, with sodium aluminate. In this study, the effects of added quantity of sodium aluminate, concentrations of sodium hydroxide solutions on the characteristics of zeolite A and the yield of the product have been studied. The morphology of zeolite A crystals was determined using scanning electron microscopy (SEM) and it was shown that particles had a cubic shape, characteristics of standard zeolite A. Keywords: Zeolite A, kaolin, metakaolin Title: Synthesis of zeolite A from Kaolin

TM TT
Zeolite A, l sn phm bt mu trng, c tng hp bng phn ng thy nhit kaolin hot ha (metakaolin), sn phm chuyn ha ca kaolin thng mi, mt loi khong c gi r, c b sung sodium aluminate. Trong nghin cu ny, nh hng ca lng sodium aluminate thm, nng dung dch sodium hydroxide trn hnh dng v hiu sut sn phm c nghin cu. Hnh dng ca zeolite A c xc nh bng nh hin vi in t qut (SEM). Kt qu cho thy chng c hnh lp phng u, c trng ca zeolite A chun. T kha: Zeolite A, kaolin, metakaolin

1 T VN Zeolite l mt dng vt liu xp c thnh phn ch yu l cc khong cht alumino-silicat c kh nng hp th cc ion kim loi nng cng nh cht hu c c hi, c ng dng trong rt nhiu lnh vc quan trng nh du kh, x l mi trng, lc du, y t, trng trt, chn nui, lm cht ty ra,... Mc d vy nhng trong nhiu nm qua, Vit Nam vn phi nhp ngoi zeolite vi gi t. V th, ngy nay c rt nhiu nghin cu tng hp zeolite t cc nguyn liu r tin c sn, p ng c nhu cu s dng ngy cng cao ca x hi. Trong s nhng ngun nguyn liu , kaolin (t st) l mt loi nguyn liu rt di do v y tim nng. Kaolin l mt loi khong st c thnh phn xp x Al2O3.2SiO2.2H2O, t l Si/Al 1 (L Tr et al., 2008), trong khi zeolite A c thnh phn 2.04 Na2O:1.00 Al2O3:1,75 SiO2:70 H2O hay Si/Al 0.75 (Hellmut G. K. et al., 1999), do vy c th tng hp zeolite A t ngun kaolin bng cch b sung aluminum di dng sodium aluminate c iu ch t aluminium sulfate (Al2(SO4)3.18H2O).

Khoa Khoa hc T nhin, Trng i hc Cn Th

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Ni dung ca bi bo ny s ch yu trnh by phng php thy nhit tng hp zeolite A t kaolin, kho st cc yu t nh hng n hnh dng v kch thc ht. 2 PHNG TIN V PHNG PHP 2.1 Nguyn liu Kaolin, sodium hydroxide, nhm sulfate, hydrochloric acid s dng cho tng hp c xut x t Trung Quc. Mu kaolin c phn tch thnh phn ha hc v hnh nh chp SEM ca cc mu zeolite A tng hp c thc hin Phng th nghim Chuyn su, i hc Cn Th. 2.2 Phng php Qui trnh tng hp nh sau: Hot ha kaolin nhit cao to metakaolin, sau b sung sodium aluminate v sodium hydroxide, ri em kt tinh trong iu kin nhit v thi gian thch hp s thu c zeolite A. Kt qu phn tch thnh phn ha hc cho thy mu kaolin nguyn liu c hm lng silic kh cao (Si: 24.5%, Al: 16.2%; Si/Al 1.46) nn qu trnh tng hp zeolite A cn b sung thm nhm di dng sodium aluminate (dng aluminium sulfate hoc Al2(SO4)3). iu ch metakaolin Kaolin ban u c ngm vi dung dch HCl 6M trong mt ngy m, sau lc v ra nhiu ln vi nc ct loi st. Kaolin sau khi ra st c sy kh v nghin thnh bt mn. Sau c cho vo cc s v nung 900-950C trong 2 gi chuyn ha thnh metakaolin. Chuyn ha metakaolin thnh zeolit A c s dng lng nhm b sung To dung dch NaAlO2 Cn mt lng cn thit aluminium sulfate ri ha tan vo nc ct cho tan hon ton. Dung dch thu c cho tc dng vi mt lng NaOH va to kt ta Al(OH)3. Sau em lc v ra vi nc ct ta thu c Al(OH)3. Ri ha tan Al(OH)3 vi lng va dung dch NaOH 4M thu c dung dch NaAlO2 trong sut. Tng hp Cn khi lng 10 g metakaolin, cho vo dung dch NaAlO2 iu ch trn (c hoc khng), thm vo dung dch NaOH c nng xM cho va 200 ml. Dng my khuy t khuy u trong 1 gi v gi ha trong thi gian 1 tun. Tip theo tin hnh un hn hp trn nhit 100C cc thi gian khc nhau. Sau khi un, ngui, lc, ra v sy kh thu c sn phm. Sn phm c chp nh SEM xc nh hnh dng tinh th to thnh.

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3 KT QU V THO LUN 3.1 nh hng ca nng NaOH ln hiu sut tng hp zeolite A
Bng 1: Kt qu ca s thay i nng NaOH ln lng zeolite A thu c

Khi lng metakaolin (g)

10

Nng NaOH (M) 1 2 3 4 5

Khi lng sn phm (g) 5.81 6.27 7.86 8.65 8.45

Khi nng dung dch NaOH tng dn, lng sn phm tng dn. Tuy vy, khi nng NaOH cao, khi lng zeolite A thu c c khuynh hng gim. Hn na lng NaOH d trong nc thi nhiu. Do , nng NaOH 4M c chn cho cc kho st tip theo. 3.2 Kho st nh hng ca thi gian thy nhit Khi thay i thi gian thy nhit t 2 n 5 gi cho thy rng sau 4 gi un khi lng sn phm thu c nhiu nht (Bng 2). Tuy vy, tinh th zeolite A thu c c kch thc rt nh v cn ln nhiu silic oxide (Hnh 1).
Bng 2: Kt qu ca s thay i thi gian thy nhit ln lng zeolite A thu c

Khi lng metakaolin (g) ((g)metakaolin

Thi gian un (gi) 2 3 4 5

Khi lng sn phm (g) 8.10 8.41 9.16 9.01

10

Hnh 1: nh SEM sn phm khng b sung Al2(SO4)3

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3.3 Kho st nh hng ca lng nhm b sung

Bng 3:Kt qu ca s b sung lng aluminium sulfate ln khi lng sn phm thu c

Khi lng metakaolin (g) metakaolin 10

Khi lng Al2(SO4)3 (g) 7.5 10 15 20

Khi lng sn phm (g) 10.45 15.29 9.45 15.95

Hnh 2: nh SEM sn phm b sung 10 g Al2(SO4)3 (hnh gc v hnh phng ln)

Kt qu cho thy khi lng aluminium sulfate b sung tng dn t 7.5 g n 15 g th khi thm 10 g khi lng sn phm thu c l cao nht, tinh th c hnh khi lp phng kh ng u, kch thc ca ht zeolite A vo khong 1-1.3 m (Hnh 2) rt l tng cho s phn tn trong nc, c nhiu ng dng trong sn xut cht ty ra. Khi lng aluminium sulfate tng ln (20 g) th khi lng sn phm c tng nhng bn cnh tinh th zeolit A c nhiu loi tinh th khc pht sinh (Hnh 3), ng thi cc tinh th nhm oxide cng hin din (hnh cun len) do lng nhm d to thnh, c th thy r trn hnh phng ln (Hnh 4). Do vy khi lng aluminium sulfate b sung c khi lng tng ng vi lng metakaolin s cho zeolite A thu c c tnh cht mong mun tt nht.

Hnh 3:nh SEM sn phm b sung 15 g (a - tri) v 20 g Al2(SO4)3 (b phi)

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Hnh 4: nh SEM sn phm b sung Al2(SO4)3 phng ln

Tng kt cc kt qu th nghim cho thy rng sn phm zeolit A tng hp c c dng bt mu trng, ht mn, khng tan trong nc, c dng hnh tinh th lp phng ca zeolit A chun, ht vung vc rt u, hiu sut hnh thnh tinh th cao. 4 KT LUN tng hp c zeolite A bng phng php thy nhit t kaolin c b sung aluminum di dng sodium aluminate, cc yu t nh hng n tinh khit, hnh dng v kch thc ht c kho st. iu kin ti u cho tng hp zeolite A t kaolin c tm thy l dung dch NaOH c nng thch hp khong 4M, thi gian thy nhit khong 4 gi v lng nhm sulfate b sung thch hp tng ng vi lng metakaolin vi nhit ca phn ng thy nhit c gi c nh l 100C. Hnh dng v kch thc ht c xc nh bng phng php chp hnh SEM. iu kin tin hnh tng hp kh m du. Ha cht dng cho tng hp kh ph bin v d mua. Hy vng trong tng lai th nghim c th tin hnh vi qui m ln hn v tin ti nghin cu sn xut p ng c nhu cu zeolite A cho cng nghip v i sng ngy cng tng nc ta. TI LIU THAM KHO
Hellmut G. K., Jens W., Zeolite - Structures and Structure Determination, Molecular Sieves, Vol. 2, 174-177, 1999. L Tr, Nguyn Phng, Nguyn Trng Ton, Tim nng kaolin Vit Nam v nh hng cng tc thm d, khai thc phc v pht trin kinh t x hi, Tp ch a cht, lot A, s 307, 7-8/2008.

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