Tổng hợp và đặc trưng vật liệu Mil - 53(Fe)

TAP CHi HOA HOC T.51(6)765-769 THANG 12 NAM 2013

T6N G Hgp VA DAC TRD'NG VAT LIEU MIL-53{Fe)

Dang Thj Quynh Lan', Le Thi Quynh Nhi^, Ho Van Thanh', Duomg Tuan Quang^", Vii Anh Tuan^

'Truang Cao ddng Suphgm Thira Thien Hue

^Truang Dgi hgc Sir phgm Hui

Vien Hoa hoc, Viin Hdn ldm Khoa hgc vd Cdng nghe Viet Nam

D i n Tda soan 02-10-2013

Abstract

MIL-53(Fe) material has been successfully synthesized by the hydrothermal method from FeCl,-6H,0 combined

with terephlhalic acid organic linker in the presence of DMF. The material was characterized by a vanety of modem

methods including X-ray diffraction (XRD), infrared (IR), transmission eleptron microscopy (TEM). thermo

gravimetric analysis (TGA) and Adsorpuon-Desorption isotherms method. The XRD patterns represented that MIL￾53(Fe) had well crystalline strucUires. The material was a highly crystallized yellow powder with a very large surface

area of about 3000 mVg The vapor-phase adsorpnon of benzene and the liquid-phase adsorpUon of arsenic were

investigated. The results showed that the maximum adsorption capacity for benzene al the relative pressure P/P^ - 1 was

about 500 mg/g, the saturated adsorption capacity for arsenic (C^„,^ = 100 ppm) was about 50 mg/g

Keywords: MIL-53(Fe), hydrothermal method, adsorption.

l.DATVANDE

Vat lieu khung kim loai hQ-u co (MOFs) da dugc

phat trien thanh mdt Idp quan trpng trong hp vat lieu

xdp. Nhiing vat lieu xdp micro nay bao gdm cum

kim loai lien ket vdi nhau bdi mdi lien ket hii"u co da

chirc tao nen mang ludi khdng gian 3 chieu xdp vol

thi tich rdng ldn va dien tich be mat ldn Ien den

5500 m'/g [1-4]. Do cac tinh chat dd, MOFs dugc

danh gia la vat lieu cd nhieu tiem nang irng dung

trong ITnh vuc phan tach khi, luu tru, xiic tac... [3,

4]. Trong nhiing nam gan day, da sd nghien ciru ve

MOFs chii yiu tap trung vao tong hgp cac vat lieu

chiia Cr(in) hoac Al(ni), tdng hgp cac vat lieu

khung kim loai hu'u co cd chira Fe(lll) it dugc

nghien ciru bdi cac anh hudng ciia thdng sd qua

trinh. Vat lieu MlL-53-Fe rit thii vi vi hieu irng "hit

thd" va diiu nay dugc img dung rdng rai trong ITnh

virc hap phu va dan thudc [5-7]. MIL-53(Fe) cd dien

tich bl mat va dien tich Id xop ldn dugc tdng hgp tir

sai(lll) clorua va axit terephtalic (H2BDC) vdi su cd

mat ciia DMF d nhiet do cao, MlL-53(Fe) cd cau

triic hinh thoi va dien tich bl mat BET cd the Ien tdi

4000 mVg, ki'ch thudc lo khoang 0,85 nm [7-10].

Trong bai bao nay, chiing tdi nghien ciiu anh hudng

ciia nong do axit H,BDC, muoi FeCb, anh hudng

ciia dung mdi DMF va chl dp nia din qua trinh tong

hgp va budc dau nghien ciru kha nang hap phu trong

pha hat va pha Idng tren vat lieu tdng hgp.

2. THUC NGHIEM

2.1. Tong hgp vat lieu

Qua trinh tdng hgp MIL-53-Fe dugc lien hanh

bang each hoa tan FeCl3.6H20 vao

dimetylformamid (DMF), sau dd cho tir tir axit

terephtalic (HiBDC) khuay cho tan thanh hdn hgp

trong sudt mau vang. Sau dd cho hdn hpp vao binh

teflon va cho vao autoclave gia nhiet d 150 "C trong

16 gid. Lpc hdn hgp bing giay lpc whatman, say san

phdm ta thu dugc vat lieu MIL-53-Fe cd mau vang.

San pham sau khi say dugc riia lai bang MeOH 95%i

trong binh teflon trong 12 gid d 100 °C vdi ti le 200

ml MeOH rira 1 g MIL-53. Sau dd lpc va rira san

pham bang 100 mi MeOH rdi say qua dem d

100 "0(4].

2.2. Dac trung cau true

cau true vat ligu dugc xac djnh bang phuong

phap nhieu xa tia X th\rc hipn tren may Simen D500

(Due), ong phat tia Ranghen bang Cu vdi budc sdng

Ka ^ 1,5406 A, gdc quet 29 thay doi tir 0,5^10°.

Phd hong ngoai IR dugc ghi theo ky thu^I 6p vien