I HC QUC GIA H NI

TRNG I HC KHOA HC T NHIN

---------------------

V Mai Phng

TNG HP VT LIU HP PH C T TNH V KHO ST KH

NNG TCH LOI PHM MU AZO TRONG MI TRNG
NC

TM TT LUN VN THC S KHOA HC

Chuyn ngnh: Ha Mi Trng

M s: 60440120

NGI HNG DN KHOA HC:

1. TS. CHU XUN QUANG
2. PGS.TS. QUANG TRUNG

H Ni 2015
 Cng trnh c hon thnh ti:
Trng i hc Khoa hc T nhin, HQGHN.

Ngi hng dn khoa hc:

1. TS. Chu Xun Quang
2. PGS.TS. Quang Trung

Phn bin 1: TS Phng Tho

Phn bin 2: PGS.TS Khc Un

Lun vn c bo v trc Hi ng chm Lun vn tt nghip thc s

hp ti Khoa Ho hc Trng i hc Khoa hc T nhin, HQGN vo
13h30 ngy 11 thng 01 nm 2016.

C th tm hiu lun vn ti:

- Trung tm th vin i hc Quc gia H Ni.
 M U

Hin nay, trc s pht trin ngy cng ln mnh ca t nc v kinh t v x

hi, c bit l s pht trin mnh m ca cc ngnh cng nghip nh hng rt
ln n mi trng sng ca con ngi. Bn cnh s ln mnh ca nn kinh t t
nc l hin trng cc c s h tng xung cp trm trng v s nhim mi trng
ang mc bo ng. Mt trong nhng ngnh cng nghip gy nhim mi
trng ln l ngnh dt nhum. Bn cnh cc cng ty, nh my cn c hng ngn
c s nh l t cc lng ngh truyn thng. Vi quy m sn xut nh, l nn lng
nc thi sau sn xut hu nh khng c x l, m c thi trc tip ra h thng
cng rnh v thng xung h ao, sng, ngi gy nhim nghim trng tng nc
mt, mch nc ngm v nh hng ln n sc khe con ngi.
Vi dy chuyn cng ngh phc tp, bao gm nhiu cng on sn xut khc
nhau nn nc thi sau sn xut dt nhum cha nhiu loi hp cht hu c c hi,
c bit l cc cng on ty trng v nhum mu. Vic ty, nhum vi bng cc
loi thuc nhum khc nhau nh thuc nhum hot tnh, thuc nhum trc tip, thuc
nhum hon nguyn, thuc nhum phn tn khin cho lng nc thi cha nhiu
cht nhim khc nhau (cht to mu, cht lm bn mu...) [7,8]. Bn cnh nhng li
ch ca cht to mu h azo trong cng nghip nhum, th tc hi ca n khng nh
khi m cc cht ny c thi ra mi trng. Gn y, cc nh nghin cu pht
hin ra tnh c hi v nguy him ca hp cht h azo i vi mi trng sinh thi v
con ngi, c bit l loi thuc nhum ny c th gy ung th cho ngi s dng sn
phm [19,30].
Vi mc ch hiu r hn v c im qu trnh x l cc hp cht hu c c
hi, c bit l hp cht to mu h azo bng vt liu hp ph c t tnh, qua
xc nh c iu kin thch hp x l nc thi dt nhum thc t nn ti
lun vn Tng hp vt liu hp ph c t tnh v kho st kh nng tch loi phm mu
azo trong mi trng nc c thc hin.

1
 CHNG 1: TNG QUAN
1.1. Chitosan
1.1.1. Khi qut v chitosan
Chitosan l polyme khng c, c kh nng phn hu sinh hc v c tnh tng
thch v mt sinh hc. Trong nhiu nm qua, cc polyme c ngun gc t chitin c
bit l chitosan c ch c bit nh l mt loi vt liu mi c ng dng bit
trong cng nghip dc, y hc, x l nc thi v trong cng nghip thc phm nh l
tc nhn kt hp, gel ho, hay tc nhn n nh ...
Trong cc loi thu sn c bit l trong v tm, cua, gh, hm lng chitin
chitosan chim kh cao dao ng t 14-35% so vi trng lng kh. V vy v tm,
cua, gh l ngun nguyn liu chnh sn xut chitin chitosan.

Hnh 1.1: Cng thc cu to chitin, chitosan v xenlulozo a

Chitosan v cc dn xut ca n c hot tnh khng nm, khng khun, c kh
nng t phn hy sinh hc cao, khng gy d ng. Khng gy c hi cho ngi v gia
sc, c kh nng to phc vi mt s kim loi chuyn tip nh Co(II), Ni(II), Cu(II)...
do vy chng c ng dng rng ri trong nhiu lnh vc nh: x l nc thi v bo
v mi trng, dc hc v y hc, nng nghip, cng nghip, cng ngh sinh hc....
Chitosan c cu trc c bit vi cc nhm amin trong mng li phn t c kh
nng hp ph to phc vi kim loi chuyn tip: Cu(II), Ni(II), Co(II).... trong mi

2
trng nc. V vy chitosan ang c nghin cu kt hp vi mt s cht khc
ng dng x l kim loi nng trong nc.
1.1.2. Tnh cht ca chitosan
- Khng c, tnh tng ng sinh hc cao v c kh nng phn hy sinh hc nn
khng gy d ng v khng gy phn ng ph, khng gy tc hi n mi trng.
- Cu trc n nh
- Tan tt trong dung dch acid long (pH<6,3) v kt ta nhng gi tr pH cao
hn, ha tm trong dung dch iot.
- C tnh khng khun tt.
- L hp cht cao phn t nn trng lng phn t ca n gim dn theo thi
gian do phn ng t ct mch. Nhng khi trng lng phn t gim th hot tnh
khng khun v khng nm khng b gim i.
- C kh nng hp ph cao i vi cc kim loi nng.
- pH<6,3, chitosan c tnh in dng cao.
- Trong phn t chitosan c cha nhm OH, -NHCOCH 3 trong cc mt xch
N-acetyl-D-glucosaminc c ngha chng va l ancol va l amine, va l amide.
Phn ng ha hc c th xy ra v tr nhm chc to ra dn xut th O-, dn xut th
N-.
1.2. Oxit st t
1.2.1. Cu trc tinh th ca Fe3O4
Oxit st t c cng thc Fe3O4 l vt liu t tnh u tin m con ngi bit n.
T th k IV ngi Trung quc bit rng Fe 3O4 tm thy trong cc khong vt t
nhin c kh nng nh hng theo phng Bc - Nam a l. n th k XII, h
s dng vt liu Fe3O4 l la bn, mt cng c gip xc nh phng hng rt c ch.
Trong t nhin, oxit st t khng nhng c tm thy trong khong vt m n cn
c tm thy trong c th cc sinh vt nh ong, kin, b cuChnh s c mt ca
Fe3O4 trong c th nhng sinh vt to nn kh nng xc nh phng hng mang
tnh bm sinh ca chng.
Trong phn loi vt liu t Fe3O4 c xp vo nhm vt liu ferit c cng thc
tng qut MO. Fe3O4 c cu trc spinel (M l kim loi ha tr II nh : Fe, Ni, Co, Mn,
Mg hoc Cu)

3
 Hinh Hnh 1.2 : Cu trc spinel ca Fe3O4b
Mi phn t Fe3O4 c momen t tng cng l 4 ( l magneton bohr nguyn
t, = 9,274.10-24 J/T trong h SI)
1.2.2. Tnh cht
Mt vi oxit st c chung cu trc tinh th vi cc tng ng khong cht khc
nhau. VD: goc-thie c cu trc ging vi diaspore ( -ALOOH), qung st t ging
vi spinel (MgAl2O3). Cc cu trc ca oxit st c xc nh bi s sp xp ca cc
ion oxy hay hydroxide. Cc ion dng chim cc v tr so le i vi lp cc ion m.
Bt c vt liu no u c s nh hng vi t trng ngoi (H), th hin bng
t ha ( t - M). T s C = M/N c gi l cm t. Ty thuc vo gi tr,
cm t c th phn ra lm cc loi vt liu t khc nhau. Vt liu c C < 0 (~10-6) c
gi l vt liu nghch t. Vt liu c C > 0 (~10-6) c gi l vt liu thun t. Vt
liu c C > 0 vi gi tr rt ln c th l vt liu st t, ferit t.
Ngoi cm t, mt s thng s khc cng rt quan trng trong vic xc nh
tnh cht ca vt liu. VD: t bo ha M s ( t t cc i ti t trng ln), cm
ng t d Br ( t cn d sau khi t ha n bo ha v a mu ra khi t
trng), lc khng t Hc ( t trng ngoi cn thit mt h, sau khi t trng thi
bo ha t, b kh t).
1.3. Vt liu t tnh ng dng x l nc thi
Trong phng php hp ph loi b trit cc cht nhim trong nc thi
thng s dng k thut hp ph tng c nh vi cc ct c ng knh t 0,1 n 1,5
m v chiu cao c th ln n hn 10 m. Cc ct thng c nhi cc vt liu nh
than hot tnh, zeolit...Dung dch nc thi c dn ln u ct, khi i qua vt liu
hp ph cc cht nhim b gi li, nc sch c x l i ra ngoi. Tuy nhin nhc
4
im ca phng php ny l thi gian ti sinh vt liu hp ph lu, qu trnh vn
hnh hay b hin tng tc ct phi np li, tn v thi gian v kinh ph. i vi k
thut hp ph tng ng, nhiu trng hp qu trnh lng ko di lm nh hng n
tc x l nc thi. khc phc nhc im ny, nhiu nh khoa hc nghin
cu ch to nha trao i ion c t tnh v nghin cu ng dng trong x l nc thi
[31,32]. Khi c tc dng ca t trng cc vt liu hp ph s tch ra khi hn hp
huyn ph nhanh hn do vy lm tng tc qu trnh x l v ti sinh vt liu. Tuy
nhin, vic s ng vt liu polyme tng hp c th to ra cc monome kh phn hy,
gy nhim th cp cho mi trng. Do , xu hng x dng cc loi polyme c sn
trong thin nhin c cc nh khoa hc rt quan tm, trong chitosan l vt liu
c ch nhiu nht do c cu trc v tnh cht ha l c bit, hot tnh cao v kh
nng la chn rt tt i vi cc hp cht v kim loi nng. Chnh v th, chng ti
nghin cu v ch to ra vt liu chitosan c nh cc ht Fe 3O4 x l nc thi dt
nhum.
1.4. c tnh v mt s phng php x l nc thi dt nhum
1.4.1. c tnh v cc ngun pht sinh nc thi dt nhum
Ngun nc thi pht sinh trong cng nghip dt nhum t cc cng on h
si, gi h, nu, ty, nhum v hon tt. Trong lng nc thi ch yu do qu
trnh git sau mi cng on. Nhu cu s dng nc trong nh my dt nhum rt ln
v thay i ty theo mt hng khc nhau. Theo phn tch ca cc chuyn gia, lng
nc c s dng trong cc cng on sn xut chim 72,3%, ch yu l t cc cng
on nhum v hon tt sn phm. Ngi ta c th tnh s lc nhu cu s dng nc
cho 1 mt vi nm trong phm vi t 12 -65 lt v thi ra 10 -40 lt nc [7,8].
i vi con ngi, thuc nhum c th gy ra cc bnh v da, ng h hp,
ng tiu ha. Ngoi ra, mt s thuc nhum hoc cht chuyn ha ca chng rt c
hi c th gy ung th (nh thuc nhum Benzidin, 4 amino azo benzen). Cc
nh sn xut Chu u cho ngng sn xut cc loi thuc nhum ny nhng trn
thc t chng vn c tm thy trn th trng do gi thnh r v hiu qu nhum
mu cao .
1.4.2. Cc loi thuc nhum thng thng
Thuc nhum l cc hp cht mang mu dng hu c hoc dng phc ca cc
kim loi nh Cu, Co, Ni, CrTuy nhin, hin nay dng phc kim loi khng cn s
5
dng nhiu do nc thi sau khi nhum cha hm lng ln cc kim loi nng
gy nhim mi trng nghim trng. Thuc nhum dng hu c mang mu hin
rt ph bin trn th trng.
1.4.3. Mt s phng php x l nc thi dt nhum
1.4.3.1. Phng php keo t
y l phng php thng dng x l nc thi dt nhum. Nc thi dt
nhum c tnh cht nh mt dung dch keo vi cc tiu phn c kch thc ht 10 -7
10-5 cm, cc tiu phn ny c th i qua giy lc.
Qu trnh lng ch c th tch c cc ht rn huyn ph nhng khng th tch
c cc cht gy nhim bn dng keo v ha tan, v nhng ht rn c kch thc
qu nh. tch cc ht rn mt cch c hiu qu, cn chuyn cc tiu phn nh
thnh cc tp hp ln hn.Vic kh cc ht keo i hi trc ht cn trung ha in
tch ca chng, tip n l lin kt chng vi nhau bng cc cht ng t. Cc khi kt
ta bng ln chu nh hng ca lc trng trng b sa lng xung, trong qu trnh sa
lng s ko theo cc ht l lng v cc ht tp cht khc. tng tc keo t, tc
sa lng, tc nn p cc bng keo v c bit lm gim lng cht keo t c th
dng thm cc cht tr keo, cht ny c vai tr lin kt gia cc ht keo vi nhau [1].
1.4.3.2. Phng php oxy ha tng cng AOP
y l phng php c kh nng phn hy trit nhng cht hu c c cu
trc bn, c tnh cao cha b loi b hon ton bi qu trnh keo t v khng d b oxy
ha bi cc cht oxy ha thng thng, cng nh khng hoc t b phn hy bi vi sinh
vt.
Bn cht ca phng php l xy ra cc qu trnh oxi ha to ra cc gc t do
nh OH c hot tnh cao, c th khong ha hon ton hu ht cc hp cht hu c bn
thnh cc sn phm bn vng nh CO 2 v cc axit v c khng gy kh thi. Mt s v
d v phng php oxi ha tng cng nh Fenton, Peroxon, catazon, quang fenton v
quang xc tc bn dn.
1.4.3.3. Phng php hp ph
Hp ph l qu trnh t tp (cht cha, thu ht) cc phn t kh, hi hoc cc
phn t, ion ca cht tan ln b mt phn chia gia cc pha. B mt phn chia pha c
th l lng rn, kh rn. Cht m trn b mt ca n c s hp ph xy ra gi l cht

6
 hp ph, cn cht m c hp ph trn b mt phn chia pha c gi l cht b hp
ph. Qu trnh ngc li ca hp ph gi l qu trnh gii hp ph hay nh hp ph.
Phng php hp ph l mt phng php tch trc tip cc cu t tan trong
nc, c s dng rng ri trong k thut x l nc thi nh c cc u im sau:
C kh nng lm sch nc mc cao, p ng nhiu cp cht lng.
Quy trnh x l n gin, cng ngh x l khng i hi thit b phc tp.
Vt liu hp ph c bn kh cao, c kh nng ti s dng nhiu ln nn chi ph thp
nhng hiu qu x l cao.
Vt liu ng dng trong phng php hp ph rt a dng : than hot tnh,
zeolite, composit, t st, silicagel... Vi mi loi vt liu c c im v tnh chn lc
ring ph hp vi tng mc ch nghin cu v s dng thc tin.
1.5. Khi nim chung v hp cht mu azo
1.5.1. c im cu to
Hp cht azo l nhng hp cht mu tng hp c cha nhm azo - N= N-. Hu
ht cc loi hp cht mu azo ch cha mt nhm azo (gi l monoazo), mt s t
cha hai nhm hoc nhiu hn. Hp cht azo thng c cha mt vng thm lin
kt vi nhm azo v ni vi mt naphtalen hay vng benzen th hai. S khc
nhau gia cc hp cht azo ch yu vng thm, cc nhm quanh lin kt azo gip
n nh nhm N = N bi chnh nhng nhm ny to nn mt h thng chuyn
ng, l yu t quan trng nh hng ti mu sc ca hp cht azo. Khi h thng
chuyn v v phn chia s xy ra hin tng hp th thng xuyn nh sng vng
kh kin [12,13].
1.5.2. Tnh cht
Hp cht mu azo bn hn tt c cc phm mu thc phm t nhin. c
bit, phm mu azo bn trong phm vi pH kh rng ca thc phm, bn vi nhit khi
phi di nh sng v oxy, rt kh b phn hy bi cc vi sinh vt. Chnh v vy, cc
hp cht mu azo c ng dng ph bin trong nhiu ngnh cng nghip (thc
phm, in, nhum...) [2,21].

7
 CHNG 2 THC NGHIM
2.1. Mc tiu v ni dung nghin cu
Mc tiu nghin cu l tng hp vt liu c t tnh Chitosan/Fe 3O4 nhm nh
gi hiu qu x l phm mu azo c trong nc thi dt nhum. thc hin c
mc tiu ny ni dung nghin cu c thc hin nh sau:
- Tng hp Chitosan/ Fe3O4 cc iu kin nng v thi gian phn ng khc
nhau.
- Kho st v nh gi kh nng s dng chitosan thng mi v oxit st t
thng mi.
- Kho st v nh gi b mt vt liu v kh nng hp ph hai loi phm mu
azo.

2.2. Thit b, ha cht cn thit cho nghin cu

2.2.1 Ha cht v Vt liu nghin cu

- Dung dch Alizrin vng G 1000 mg/l : Cn chnh xc 1,0 gam Alizarin vng G
vo cc 250 ml cha nc ct, un nng 40 0C, ngui, nh mc bng nc ct
n 1000 ml. Cc dung dch c nng khc s dng trong thc nghim s c pha
long trc tip t dung dch ny.
-Dung dch Methyl 1000 mg/l : Cn chnh xc 0,1 gam Methyl vo cc
500 ml nc ct, un cch thu 40 0C, ngui, nh mc bng nc ct n 1000
ml. Cc dung dch c nng khc s dng trong thc nghim s c pha long trc
tip t dung dch ny.
- Dung dch HCl, NaOH, CH3COOH, glutaralehyt.
- Cc dung dch mui clorua, cc dung dich mui natri.
2.2.2. Thit b
- My trc quang UV-Vis THERMO ELECTRON COVPORATION
- in cc o pH THERMO SCIENTIFIC
- My o c (HI 98703)
- My phn tch a ch tiu (DR600)
- Cn phn tch HR200 SHIMMADZU
- B my khuy Jar tester
- T sy MENMERT - c
- My khuy t MSH 20 D/MS MP4
8
 - My ht chn khng LAB LABOPORT
2.3. Phng php phn tch trc quang xc nh nng phm mu trong
dung dch
phc v cho qu trnh nghin cu, xc nh hm lng phm mu cn li
sau qu trnh hp ph ca chitosan, Fe3O4 v cc vt liu chng ti kho st li kh
nng hp th nh sng ca 2 loi phm mu (Methyl , Alizarin vng G) cc pH
khc nhau.
Chun b cc dung dch phm mu (Methyl , Alizarin vng G) c nng 5
mg/l trong cc pH khc nhau(2, 4, 6, 8, 10). Kho st hp th nh sng trong
khong bc sng t 200 800 nm. Tm khong bc sng ti a v n nh, kho st
tip vi khong cch 2nm tm bc sng ti u. Cc kt qu c th hin trn
hnh 2.1, 2.2 :
0.35

0.3

0.25

0.2
pH 2
Abs 0.15 pH 4
pH 6
0.1 pH 8
pH 10
0.05

0
100 200 300 400 500 600 700 800 900
-0.05

Bc sng nm

Hnh cHnh 2.1. th s ph thuc hp th quang Methyl vo pH

9
 0.7

0.6

0.5

0.4
Abs pH 7
0.3
pH 8
0.2 pH 12

0.1

0
100 200 300 400 500 600 700 800 900

Bc sng nm

Hnh d Hnh 2.2. th s ph thuc hp th quang Alizarin vng G vo pH

T cc s liu biu din trn th cho thy hp th quang ca cc phm
mu n nh v t cc i ti : bc sng 524 nm ti pH ca dung dch l 4 i vi
Methyl , bc sng 352 nm ti pH ca dung dch l 7 i vi Alizarin vng G. Trn
c s ny chng ti xy dng ng chun i vi tng phm mu. Kt qu c th
hin trn bng 2.1, 2.2 v hnh 2.3, 2.4.
Bng 1Bng 2.1 S liu xy dng ng chun xc nh nng Methyl
C (mg/L) 2 4 6 8 10 20 40 60 80
Abs 0,045 0,08 0,12 0,15 0,19 0,37 0,74 1,1 1,56

ng chun dung dch metyl

2

1.5
f(x) = 0.02x - 0
R = 1
1
Abs

0.5

0
0 10 20 30 40 50 60 70 80 90

Co(ppm)

Hnh eHnh 2.3 ng chun xc nh nng Methyl

10
Bng 2Bng 2.2 S liu xy dng ng chun xc nh nng Alizarin vng G

C (mg/l) 10 20 30 40 60 80 100
Abs 0,065 0,14 0,192 0,256 0,383 0,490 0,637

0.7

0.6

0.5

0.4
Abs 0.3

0.2

0.1

0
0 20 40 60 80 100 120

C (mg/l)

fHnh 2.4 ng chun xc nh nng alizarin vng G

11
 CHNG 3 - KT QU V THO LUN
3.1. Cc c trng c bn ca vt liu
3.1.1. Hnh thi hc ca vt liu
Vt liu Fe3O4, FMM-C11, FMM-C21 v FMM-C31 c chn la so snh
hnh thi b mt. Kt qu c th hin trn hnh 3.1.

gHnh 3.1: Kt qu chp SEM ca vt liu a. Fe3O4; b. FMM-C11; c. FMM-C21; d.

FMM-C31
T kt qu chp SEM ca vt liu Fe3O4, ta thy Fe3O4 tn ti di dng hnh cu
v phn b khng ng u.
Kt qu chp SEM ca cc mu vt liu FMM-C11, FMM-C21, FMM-C31 c
th thy cc ht Fe3O4 c t hp vo trong cu trc mng chitosan polime, phn
b ng u trn b mt vt liu.
3.1.2. Kt qu phn tch ph hng ngoi
Cu trc ca vt liu chitosan, FMM-C11, FMM-C21 v FMM-C31 c phn
tch qua ph hng ngoi IR. Kt qu c th hin trong hnh 3.2.

Hinhh Hnh 3.2: Ph IR ca vt liu a. Chitosan, b. FMM-C11, c. FMM-C21, d.

FMM-C31
Vi kt qu ph IR ca vt liu, ta thy xut hin pic hnh a,b,c,d ln lt
3411; 3427; 3413; 3399 cm-1 vi chn pic rng c trng cho dao ng ca lin kt O-

12
H. Pic 1644 v 1379; 1633 v 1416; 1633 v 1376; 1645 v 1376 cm -1 c trng cho
dao ng ca lin kt C=O v N-H. Pic 1086; 1061; 1068; 1067 cm-1 c trng cho
dao ng lin kt C-O trong (O-C-O). hnh b,c,d c pic 572; 580; 579 cm -1 l pic
c trng cho dao ng ca lin kt Fe-O.
T kt qu chp ph IR cho thy, ta t hp c vt liu chitosan/ oxit st t.
3.1.3. Kt qu phn tch nhiu x tia X

i Hnh 3.3: Gin nhiu x tia X ca vt liu a. Chitosan; b. Fe3O4; c. FMM-C11; d.

FMM-C21; e. FMM-C31
T gin trn, ta thy vt liu chitosan tn ti di dng v nh hnh. Cc vt
liu cn li tn ti di dng tinh th, c thnh phn phn trm Fe 3O4 ln lt l 90%;
65%; 68% v 70%.

3.1.4. Xc nh ng cong t ha v t bo ha
Cc mu vt liu Fe3O4, FMM-C11, FMM-C21 v FMM-C31 c phn tch
bng phng php t k mu rung. Cc kt qu c th hin trong hinh 3.4.

jHnh 3.4: ng cong tr t ca vt liu a. Fe3O4; b.FMM-C11; c.FMM-C21;d.

FMM-C31
T kt qu chp ph cho thy t bo ha ca cc vt liu Fe 3O4, FMM-C11,
FMM-C21 v FMM-C31 ln lt l 72; 37.8; 24; 16 emu/g.
Khi t bo ha thp, vt liu s kh lng, khi t bo ho cao cn s dng
lc khuy ln phn tn cc ht trong mi trng nc. Do , t thch hp nm

13
trong khong 10-20 emu/g. Do , chng ti chn vt liu FMM-C31 lm vt liu hp
ph.
3.1.5. Din tch b mt ring ca vt liu

Hinh kHnh 3.5: Kt qu chp BET ca vt liu a. FMM-C11; b. FMM-C21; c. FMM-

C31.
Din tch b mt ring vt liu FMM-C11, FMM-C21v FMM-C31 ln lt l
3,89; 0,645; 0,081 m2/g.
D nhn thy ng ng nhit hp ph (vi thang p/po tuyn tnh) ca vt liu
c dng ging vi kiu IV theo IUPAC.
iu ny cho php d on tt c cc vt liu nghin cu trn thuc loi vt liu
c kch thc mao qun trung bnh.
3.1.6. nh gi kh nng lng ca vt liu
Cn 5 g vt liu, cho vo ng ong hnh tr 150 ml nc ct, lc u. Sau cc
khong thi gian nh trc th ly 10 ml mu khong gia dung dch o c
v xc nh lng. Lp li th nghim cho n khi vt liu gn nh lng ht. Lm th
nghim ln lt vi cc vt liu .
Kt qu c biu din bng 3.2 v hnh 3.6.
Bng 3Bng 3.2. Bng kho st thi gian lng ca vt liuu

Thi gian Chitosan Chitosan Chitosan

FMM11 FMM21 FMM31
(pht) th oligome polime

0 548 108 132 968 864 1410

1 282 34,8 34,9 508 524 336
5 90,3 13,3 9,02 264 486 235
10 45,4 7,2 6,71 180 466 177
15 32,5 6,04 6,03 166 451 169
20 23,5 5,15 5,9 155 425 152
30 12,8 3,31 4,86 123 408 91,9
60 3,95 1,75 3,36 77 359 43,4

14
 1500

c (NTU)
1000 FMM11 FMM21
FMM31 Chitosan th
500 chitosan chitosan polime
oligome

0
0 50100

Thi gian lng (pht)

Hinh lHnh 3.6: Kho st thi gian lng ca vt liu ca vt liu

T nhng kt qu trn, ta c th kt lun c vt liu FMM-C31 c c thp
v thi gian lng nhanh.
3.1.7. So snh tnh nng hp ph ca cc vt liu
Tin hnh lc hn hp 1 g vt liu vi 100 ml dung dch alizarin vng G 500
mg/L ln lt trong 3 bnh tam gic vi 3 loi vt liu l FMM-C11, FMM-21 v
FMM-C31 trong vng 180 pht. Gi nguyn pH, o v ghi li gi tr pH. Ly mt
lng mu nht nh em i lc, o hp ph quang.
Kt qu c trnh by bng 3.1
Bng Bng 4Bng 3.1. So snh s hp ph alizarin vng ca 3 loi vt liu FMM-
C11, FMM-C21 v FMM-C31
Co(mg/l) Ct(mg/l) Qt (mg/g)
FMM-C11 500 322 17,8
FMM-C21 500 129,6 37,04
FMM-C31 500 42,4 45,76
T phng trnh ng chun, ta tnh c nng alizarin vng G cn li ln
lt l 322 mg/L; 129,6 mg/L v 42,4 mg/L. Kt qu trn cho thy, vt liu FMM-C31
c kh nng hp ph alizarin vng G tt nht.
3.2. Kho st mt s iu kin hp ph c bn s dng vt liu chitosan/oxit
st t FMM-C31
Trn c s thc nghim la chn v bin lun trong mc 3.1. Chng ti tin
hnh tng hp vt liu vi quy trnh v cch tin hnh nh nu trn v dng vt
liu FMM-C31 kho st kh nng hp ph phm mu alizarin vng G v metyl .

15
 3.2.1. Kho st mt s iu kin hp ph phm mu metyl i vi vt liu
hp ph FMM-C31
a. Kho st thi gian cn bng hp ph ca vt liu FMM-C31 i vi phm
mu metyl
Bng 56Bng 3.6. Kho st thi gian cn bng hp ph ca vt liu FMM-C31 i
vi phm mu metyl
T (pht) Co (mg/L) Ct (mg/L) Qt (mg/g)
0 20 19,9 0,001
15 20 11,5 0,85
30 20 6,1 1,39
60 20 3,87 1,61
90 20 3,77 1,62
120 20 3,66 1,63
180 20 3,45 1,66
240 20 3,4 1,66

1.5

qt(mg/g) 1

0.5

0
0 50 100 150 200 250 300
Thi gian(pht)

Hinh mHnh 3.13: th biu din thi gian cn bng hp ph metyl ca vt liu
T th hnh ta thy, i vi vt liu FMM-C31 thi gian t 0 n 180 pht.
Dung lng hp ph metyl tng dn, sau 180 pht dung lng hp ph hu nh
khng i.
b. Kho st nh hng ca pH n kh nng hp ph metyl ca vt liu
78Bng 3.7. Kho st nh hng ca pH n kh nng hp ph metyl va vt liu
pH pH sau Co(mg/L) Ct(mg/L) qt(mg/g)
2 2,36 50 7,05 4,29
4 6,41 50 6,9 4,31
6 7,54 50 8,6 4,1
8 7,79 50 14,35 3,56
10 8,17 50 14,29 3,57
16
 Qua bng cho thy i vi metyl , pH sau khi x l i vi pH thp c xu
hng tng nh. i vi pH cao > 6 th c xu hng gim, dao ng xung quanh pH =
7. Qu trnh hp ph mu xy ra mnh nht pH = 4. pH cao, hiu sut x l
mu thp.
c. Kho st dung lng hp ph metyl cc i ca vt liu FMM-C31
910Bng 3.8. Kho st dung lng hp ph metyl cc i ca vt liu FMM-C314
Co(mg/L) Ct(mg/L) qt(mg/g) Ct/qt logCt logqt
0 0 0 0 0 0
10 1,56 0,84 1,85 0,19 0
20 3,45 1,65 2,08 0,54 0,22
30 10,5 1,95 5,38 1,02 0,29
40 20,12 1,99 10,12 1,30 0,30
60 40,11 1,99 20,16 1,60 0,30

25
20
f(x) = 0.49x + 0.42
15 R = 1
Ct/qt 10

5
0
0 5 10 15 20 25 30 35 40 45
Ct(ppm)

Hinh nHnh 3.14: th biu din s ph thuc ca Ct/qt vo Ct ca metyl

T th ta tnh c vt liu FMM-C31 c dung lng hp ph metyl cc
i: qmax=1/0,4898= 2,04 (mg/g).
3.2.2. Tin hnh kho st kh nng hp ph alizarin vng G ca vt liu
FMM-C31
a. Kho st thi gian cn bng hp ph
Bng 11Bng 3.3. Kho st thi gian cn bng hp ph alizarin vng G
T (pht) Co (mg/L) Ct (mg/L) Qt (mg/g)
0 200 197,43 0,26
15 200 188,71 1,13
30 200 176,54 2,35
60 200 149,67 5,03
90 200 140,21 5,98
120 200 125,23 7,48
17
 180 200 113,7 8,63
240 200 113,7 8,63
360 200 113,7 8,63

10
8
6
qt(mg/g) 4
2
0
0 50 100 150 200 250 300 350 400
Thi gian

Hinh oHnh 3.9: th biu din thi gian cn bng hp ph alizarin vng G ca vt
liu
T th hnh, cho ta thy i vi vt liu FMM-C31 thi gian t 0 n 180
pht, dung lng hp ph alizarin vng G tng dn, sau 180 pht th dung lng hp
ph gn nh khng tng.
b. Kho st nh hng ca pH n kh nng hp ph alizarin vng G ca vt
liu FMM-C31.
12Bng 3.4. Kho st nh hng ca pH n kh nng hp ph alizarin vng G ca
vt liu FMM-C31.
pH pH sau Co(mg/L) Ct(mg/L) qt(mg/g)
2 2,39 500 40,28 45,97
4 5,18 500 147,28 35,72
6 5,7 500 190,28 30,97
8 6,3 500 397,44 10,26
10 6,66 500 418,86 8,11

Qua bng 3.4 nhn thy: i vi dung dch alizarin vng, pH sau khi x l i
vi pH thp c xu hng tng nh. i vi pH cao > 6 th c xu hng gim, dao
ng xung quanh pH = 6. Qu trnh hp ph mu xy ra mnh nht pH = 2 . pH
cao, hiu sut x l mu rt thp.
c. Kho st dung lng hp ph cc i.
13Bng 3.5. Kho st dung lng hp ph alizarin vng G cc i ca vt liu FMM-
C31
Co(mg/L) Ct(mg/L) qt(mg/g) Ct/qt logCt Logqt
18
 0 0 0 0 0 0
100 1,07 9,89 0,11 0,03 0,99
200 1,16 19,88 0,06 0,06 1,30
400 2 39,8 0,05 0,30 1,60
600 10,13 58,99 0,17 1,00 1,77
800 45,08 75,49 0,60 1,65 1,88
1000 157,7 84,23 1,87 2,20 1,92
2
f(x) = 0.01x + 0.05
1.5
R = 1
1
Ct/qt
0.5

0
0 20 40 60 80 100 120 140 160 180
Ct

Hinh pHnh 3.10: th biu din s ph thuc ca Ct/qt vo Ct ca alizarin vngG

KT LUN

Qua qu trnh thc hin ti lun vn nghin cu Tng hp vt liu hp ph

c t tnh v kho st kh nng tch loi phm mu azo trong mi trng nc, ti
thu c nhng kt qu chnh nh sau:
- t hp c vt liu Chitosan/Fe3O4 t 3 loi chitosan thng mi c bn trn
th trng Vit Nam (c deaxetyl ha v phn t lng khc nhau) v oxit st t
thng mi. Vt liu c t tnh v c kh nng hp ph phm mu trong mi trng
nc. Vt liu t hp t chitosan c deaxetyl ha cao v phn t lng cao
(chitosan polyme) l ph hp nht.
- s dng cc phng php phn tch nh ph hng ngoi (IR), knh hin vi
in t qut (SEM), din tch b mt ring (BET) ... xc nh c trng vt liu. Kt
qu cho thy Fe3O4 c phn tn tt vi chitosan, do vt liu c kh nng lng tt
hn vt liu chitosan thng thng. Thi gian lng t c thp hn 10 NTU l
1 pht.
- kho st iu kin v tnh nng hp ph ca vt liu Chitosan/Fe 3O4 FMM-31
i vi phm mu azo t tan trong nc l Methyl . Kt qu cho thy thi gian t

19
cn bng hp ph l 60 pht; khong pH ph hp l pH = 2 - 6; ti trng hp ph cc
i l 2 mg/g.
- kho st iu kin v tnh nng hp ph ca vt liu Chitosan/Fe 3O4 FMM-31
i vi phm mu azo d tan trong nc l Alizarin vng G. Kt qu cho thy thi
gian t cn bng hp ph l 180 pht; khong pH ph hp l pH = 2 - 4; ti trng hp
ph cc i l 86 mg/g.
Nh vy, cc kt qu nghin cu cho thy t hp c vt liu hp ph c t
tnh v kh nng ng dng kh tt. Tuy nhin, cc nghin cu tip theo cn i su
nh gi, l gii v kho st cc yu t nh hng n c ch hp ph, kh nng ti s
dng cng nh tng bc hon thin iu kin ch to vt liu nhm nng cao hiu
qu hp ph ca vt liu.

20