Tổng hợp nano vàng trên hệ chất mang Alginate/Lactose và ứng dụng xúc tác phản ứng phân hủy chất

i

N T T NGHI P

U T NG H P NANO CH T MANG NG D NG PH N

NG CH

M

iii

ii

L

M CL C L IC

T

IH

....................................................................................................... ii

L

C TH NG

............................................................................................................. i

DANH M C B NG ................................................................................................. vi u c

c s

ng d n khoa h c c a Th.S

DANH M

................................................................................................. vii

u, k t qu DANH M C PH L C ........................................................................................... ix

i b t k Nh ng s li u trong b ng bi u ph c v cho vi

nh

DANH M C THU T NG

c

thu th p t

u tham

L IM

kh o.

VI T T T ................................................................... x

U ........................................................................................................... xi NG QUAN....................................................................................... 1

n lu

d ng m t s nh

li u c

ch

I.1. T ng quan v h t nano kim lo i ....................................................................... 1 n

t c a h t nano kim lo i ................................................................. 1

ngu n g c.

N

ng h p v t li u nano .......................................................... 2 t k s gian l

n i dung lu

.

nh ng vi ph

n, b n quy

mv ih

c Th

I.1.3.

n c hi n (n

.

ng d ng .................................................................................................... 4

I.2. Nanocomposite kim lo i polymer.................................................................. 5 I.3. H

................................................................................................... 6

TP. H .................................................................................................... 6 t ................................................................................. 7 ng h p ........................................................................ 7 I.3.4.

ng d ng .................................................................................................... 9

I.4. Alginate........................................................................................................... 10 .................................................................................................. 10 I.4.2. C

.................................................................................................... 10 ng d ng .............................................................................. 11

iv

v

ng gel so v i ion Au3+ ......... 27

I.5. Canxi-axetate .................................................................................................. 12

III.1.1. K t qu kh

ng t l kh

I.6. Lactose ............................................................................................................ 12

III.1.2. K t qu kh

ng nhi

.................................................................................................. 12

III.1.3. K t qu kh

ng th i gian ................................................... 30

I.6.2. C

.................................................................................................... 13 ng d ng .............................................................................. 13 gi i .......................................... 15 gi i ........................................................... 15

III.2. K t qu III.2.1. K t qu

.............................................................. 32 ......................................................................... 32

III.2.2. K t qu TEM ......................................................................................... 33 III.2.3. Th

c ............................................................. 16 m m i c a lu

.................................................... 28

ng Zeta ................................................................................ 36 c h t ....................................................................................... 38

................................................................................... 17

III.2.5. K t qu

FT-IR ........................................................................... 39

C NGHI M ............................................................................... 18

III.2.6. K t qu

t TGA ................................................................. 41

t, d ng c

t b th c nghi m .................................................... 18

III.2.7. Kh

..................................................................................... 44

t .................................................................................................. 18

K T LU N .............................................................................................................. 52

II.1.2. D ng c ................................................................................................... 18

KI N NGH ............................................................................................................. 54

II.1.3. Thi t b .................................................................................................... 19

U THAM KH O ........................................................................................ 55

II.2. Th c nghi m.................................................................................................. 20

PH L C ................................................................................................................. 59

II.2.1. Pha ch

t chu n b

ng h p.................................. 20

o ch t mang Alginate/Lactose ............................................. 21 t mang Alginate/Lactose .................... 22 II.2.4. Kh ph UV-Vis........................................................................................................ 23 ..................................................................... 25 u ng d T QU III.1. K t qu

................................................................. 25 N LU N ........................................................... 27

m kh

ng ph Uv-Vis ............................................ 27

vii

vi

DANH M C B NG B ng 2. 1 B ng s li

m kh

ng h p nano

ch B ch

t o h t nano.................................................................... 2

m kh

ng c a nhi

ng c

.................................................................... 7

ng d ng c

..................................................................... 9

................................................................................................. 24

B ng 3. 1 S li u k t qu B

3+

.......................................................................................... 23

B ng 2. 2 B ng s li t ng h

ng t l

DANH M C

TGA c

....................................................................... 10

t ..................................... 41

...................................................................................... 13

n Alginate/Lactose v

o ch t mang Alginate/Lactose ..................................... 21

a ph n ng kh NaBH4 v i Metyl Orange ............................... 48

ng h

n Alginate/Lactose v

c bi

a ph n ng kh NaBH4 v i Rhodamine B ............................... 51

ch t mang. .......................... 22

i ph thu c t l kh

ng. ........................................... 27

t qu ph UV-Vis bi u di +

l

h p th

t

. .................................................................................................... 27

t qu ph UV-

h p th

ng b i nhi

.

.................................................................................................................................. 28 th bi u di n m

h p th

p th khi

. ............................................................................................................ 29 3. 5 K t qu ph UV-

h p th

ng b i th i

gian. .......................................................................................................................... 30 th bi u di n m

a th i gian ph n ng v

h p th

p th . ............................................................................................... 30 t qu

u x tia X m u T3-

-AuNPs. .................... 32

t qu ch p TEM m u T3-AuNPs. ........................................................ 33 th

h t nano t

i 20nm c a m u

T3-AuNPs................................................................................................................. 34 t qu ch p TEM m u T4- AuNPs. ..................................................... 34 th

h

i 20nm m u T4-

AuNPs. ..................................................................................................................... 35 t qu t qu

th

ng Zeta......................................................... 36 h

trong dung d ch ........................... 38

viii

3. 14 K t qu ph FTt qu

ix

t. .................................................................. 39 TGA c

n ng kh gi c ch t qu ph UV-Vis ph n ng kh Metyl Orange v i NaBH4

........ 44

Ph l

c h t m u T3-AuNps. ............................................................... 59

.... 45

Ph l

c h t m u T4-AuNPs. ............................................................... 60

t

Ph l

c h t m u nano tr ng. ............................................................... 61

- AuNPs theo th i gian. .......................................................................... 46 th bi u di n h ng s t

DANH M C PH L C

t. .............................................. 41

ph n ng kh

Ph l c 4 Th Zeta m u T3-AuNPs. ........................................................................ 62

-

Ph l c 5 Th Zeta m u T4-AuNps.......................................................................... 63

AuNPs. ..................................................................................................................... 46

Ph l c 6 Th Zeta m u nano tr ng. ........................................................................ 64

3. 21 K t qu ph UV-Vis ph n ng kh Metyl Orange v i NaBH4

t

- AuNPs theo th i gian. .......................................................................... 47 th bi u di n h ng s t

ph n ng kh

-

AuNPs. ..................................................................................................................... 47 t qu ph UV-Vis ph n ng kh Rhodamine v i NaBH4

t

- AuNPs theo th i gian. .......................................................................... 49 t qu ph UV-Vis ph n ng kh Rhodamine v i NaBH4

Ph l c 7 nh ch

-AuNPs............................................................... 65

Ph l c 8 nh ch p TEM m u T4-AuNPs............................................................... 66 Ph l c 9 Ph nhi u x XRD m u T4

AuNPs. ...................................................... 67

Ph l c 10 Ph nhi u x XRD m u T3-AuNPs. ...................................................... 68 Ph l c 11 K t qu

t tr

ng TGA c a m u T3-

-

AuNPs. ..................................................................................................................... 69

t

Ph l c 12 K t qu

t tr

ng TGA c a m u nano tr

c T3 - AuNPs theo th i gian. .......................................................................... 49

Ph l c 13 K t qu

t tr

ng TGA c a Lactose.......................... 71

t qu ph UV-Vis ph n ng kh Rhodamine v i NaBH4

70

t

Ph l c 14 K t qu ph IR c a Alginate sodium. .................................................... 72

- AuNPs theo th i gian. .......................................................................... 50

Ph l c 15 K t qu ph IR c a Lactose. ................................................................. 72

t qu ph UV-Vis ph n ng kh Rhodamine v i NaBH4

t

Ph l c 16 K t qu ph IR m u tr ng. ..................................................................... 73

c T4 - AuNPs theo th i gian. .......................................................................... 50

Ph l c 17 K t qu ph IR m u T3-AuNPs. ............................................................ 73 Ph l c 18 K t qu ph IR m u T4-AuNPs. ............................................................ 74

xi

x

L IM DANH M C THU T NG

VI T T T

v t li

U

nm

u cho

i nh FT-IR

Fourier transform infrared radiation

Alg

Sodium Alginate

TEM

Transmission Electron Microscopy

c nh v n vi

u, t ng h

ng d

quan

ng d ng trong nhi

m bi n sinh h c, kh

u, ch

n t truy n qua

c bi

u tr

n truy n thu c, ch p nh sinh h c nh

c bi TGA

Thermogravimetry analysis

XRD

X-ray powder diffraction

UV-Vis

UltraViolet-Visible Spectroscopy - Ph t ngo

NaBH4

Sodium Borohydride

t ng h p nano om

h

ux

sinh i nhi

nhau. ki n Hi n nay khi n n kinh t

Abs

Absorptance

AuNPs

Au nanoparticles

MO

Metyl Orange

n g n li n v i v

cs Vi

c bi

ch it n

RH

Rhodamine

T4-AuNPs

M

ng h p

t l kh

ng 0.04

T3-AuNPs

M

ng h p

t l kh

ng 0.03

ng

t trong nh ng v

i thi

n v i nhi

ti

i

ct

t

p d t nhu m, gi y, da,

ng s d

nh ng ch

t ra cho

m ngu

p th i ra

th c ph m, m ph

b ov

ng ch cx

ng tr m tr

trong s

hay x tr c

n ngu

t

c s d ng r

nhu

t

p v i s

ch

nhu m t Trong nh

c ng d ng v t li

m

c ng d ng r

n nh

n ng d

y ch i l so v

ng

xu t hi n d ng kh i. Ho

lo

a h t nano kim

n so v i h

ch

t nano t ng h i b m t ti

n. Nh ng ch t mang

t mang, m ng d ng polymer sinh h

1

xii

c u nh

c ng d ng trong

s

T NG QUAN

n d ng kh c

kh

kh

n ti t ki Xu

I.1. T ng quan v h t nano kim lo i c h i.

nh ch

h y ch

i m ra m t k

T ng h p ng d

ng d ng, v i nh

n

nano. H

m

.

M

c, quang h

I.1.1.

n

v i v t li u kh i do hai hi li

ch t mang Alginate/Lactose

c nh

c nano cho th y nh ng: hi u ng b m

u ki n t l , nhi

i gian t

ng h p nano

hi u ng b m

ra

d

ng t c

c nh d

n hi

ib cx

ng h

ng nh t Alginate/lactose, s d n d ng kh kh

b m c. T o h ch t mang us

ng t m i. H t nano kim lo i t quang[3][1]. ng t p th c nt

c

ng c

ir cc lu t v

ng plasmon

ut

h t nano. c v t li u gi m d n, hi u

n trong ch t mang.

nt

ns

ah l n c a h t nano, m

n

nt d

n t t do c a h t nano h p th

c a lactose g n k t s n trong ch t mang Alginate gi

n t bi u hi n

t nhi

c ti n c

c h i. Hi

iv i

c

t quang h c: do s

u ki n t ng h

c a

c bi t c a h

n ng c a NaBH4

u hi

ng s cl

chuy n th ng trong ch t d t

c. Khi v t

m hi u ng b m

hi u

Kh

i l so

u

s gi

v t li Kh

n t . [4]

t c a h t nano kim lo i kim lo

T ng h

ng, c u

u khoa h

ng d

N

c

c t 1nm t i 100nm

nhi u ng d ng ti

T ng h

u

c bi t khi v t li

d

ng

ng t do giam s tuy

nh

n so v i v t li u kh i.

SVTH: H Th Thu Trang

3

2

tt

o

do s

c

ch t

nt

c thu nh

im

Theo

i

-

b ng b

t li

-down

c nh

y nhi t, sol-

ng, t

ch

ng). cc ah

m, nhi

t li c, s

ys

gi m.

i

o h t nano t

b ng

ng l n v t li

p ch -gel hi u

d ng k thu t nghi n,

ho c kh ion.

t nano kim lo i

c d

t n

su

cl

oh tt

iv

tv

t ng h p h t nano kim lo i

t

ng c a

ng t t o m t kh

ng h p v t li u nano

ch

c k t t a t dung d

c v t li

li u t o ra r

I.1.2.

c

tt

c tr n v i nhau theo t l t

nhi

t nhi t:

thu

t o v t li

n sang tr

nt

t li

bi n:

i v i kim lo

t, niken, coban khi

t

tr

-up,

c kh

t v i nhau

h

t li u

ph c t

ch y

c nghi ch t

t o ra m

t v

ng t .[18]

d ng b

t ng v t li u l

td b k t

ch

u, d b nhi m b n,

ch t o v t li

h

i.

c bay: g

c, b

V t li u kh i

ng hi u qu ch t o

Top-down

ng ho c l p bao ph b m t c o v t li u t

c h t nano

o h t nano b

g hi u qu

ng

i.

(1-100nm) Bottom up

t laser, b c bay nhi t li u t

Phân t

cao, plasma d ch t

t li t

HĂŹnh 1. 1

t o h t nano.

gi i h

nn

c nhi u lo i v t li u

m b i hi u su t th

4

5

t chi

t o nhi u v t li u

ch c

nh

t o v t li u h n 9000

t o l ng carbon,

is u kh

nh c a ng d ng trong y, sinh h c

c v

c c a t

virus(20-450nm), protein(5-50nm), gen(2nm r n gi ng v

ng

I.2. Nanocomposite kim lo i

cs d

c, h tr

tt

n

i thu

tc cb

m, vi

nh h t kim lo

ah t

nanocompozit polyme/kim lo

ng t

c nano -

c, nhi t hay b c x

t nano trong m

i polyme. Ho

n, ho n v t li

TiO2 t ng h p b

-

c

: h t nano

t nano kim lo u.

-

y nhi t kh

i k tt

t nano kim

c v t li

c ng

u.

ng ug

Hi

ng minh r ng, s d ng v t li u nano C, Ag, Cu, TiO2, ch t k

ng h u

u ki n khu y tr

ho

tc

c ch t

ng b m t l

lo m...[30][24][23]

c p

n ph

n

t

c) Ph gia trong v t li

t nano kim lo

ch ch t

th bao g

i

[19]

m t ti

t o

kh b

b) c nano di

t t bao b

-

nt

tt

n cho nh c

t li

c bi t,

a h t nano kim

t t , truy

polymer

Nanocomposite polyme/kim lo tr i nh

n truy n thu c, t n d ng kh

nc

li u, pin Li-ion,

-100nm chi

t nano kim lo

t

c

-100nm),

c th sinh h

t

lo

b n

l p ph nano ch

nano, v t li u nano

khu

ch

ng trong chuy

u

c nh

c c i thi

.

ng d ng

S ti n b c a Khoa h c k thu

c

tt

d)

a) Y sinh- sinh h c

T nd

cl

nt

ng nano carbon.

I.1.3.

tc

b

o

th

n ti

b n

i trong polyme t

c s d ng ph bi ng nanocompozit

c h c, nanocompozit polyme/kim lo i ng d ng trong

7

6

h th ng d n truy n thu

c lo i c m bi n sinh h

I.3.2.

th nghi m mi n d ch.

i

t

ch

1nm-8

u,

ng s

I.3. H

t nano kim lo

n gi ng nano kim lo

I.3.1.

ch

c

10

1

4f 5d 6s

Kh

t 196,9665g.

d ng kh ng ng

u

n, d n

ng b i nhi ch keo t

m trong kho ng th

c t o ra b i t n s plasmon c a c, t

p th . Tr

khi ph n x

-

ch t n t i

hai d ng + 1(auro) n

t c kim lo

.

(axit cloroauric) kh v d

c kh

i

i v i dung d

clorua

ch t

dung

e hay ascorbat

v

u.[9] u ng d ng trong y h

dung d

ch s

cs d

c li u t th i Trung c

b nh tim, hoa li

n, huy ng cho y h c, sinh h nt .H

thay th cho h m

tr

i s ti n b c a khoa h c k thu t

th

h

c,

79 trong b ng tu

c c t nhuy nhi t t t, h

t nhi c.[29]

d

i chuy n ti 14

n,

t quang h

2 ng

I.3.3.

ng h p

ng

c

p trung v S d

t thay th t

thu cho nhi u ng d

kh ion kim lo

d ng l

a h p ch t cadmium k th pv

mu

sinh h [16]

ng c

cg 4

i. t. Dung d

v

NaBH4

c kh : Au3+ + B

Auo + nAuo

nano Au.

d ng

8

9

ng c a ch t kh B, ion Au3+ b kh t th pv

t

I.3.4.

t nano Au.

kh s

c ng d ng r

t

ng h t,

h c u, c

ng ng d n vi c l a ch

nt

m t l

d

sinh h n t cao. Vi c ki

nanomet c a h

p.

S d

ng d ng

ng v i m

sinh h c

c

t nano v n truy n thu

nt

, biosensor, kh

[29]

nt

, tia t ngo i, tia laser kh

3+

c ti

: Au

o

Au

c sinh h n m

m Furasium Oxysporum, Bacillis licheniformic, khu n Lactobacillus,

khu

ion kim lo

t nano

nv

t o ra v i s

ng l

d

lo i n m m c, d ch chi t t

,c t ng h

d ng nhi 3

d h ng ngo

ns t kh ion Au3+

Au3+

o

t tr kh s t kh

nh

n 300GHz, s d ng

c bi

m r ng b m t ti

c ng d ng trong m ph m,

ng c ng c a nhi

n

c s d ng

p ch t polyol : t nano t

gi n, d s d ng, t

ng d ng c

u nhanh, th i gian kh nhanh.

n ng oxi2O3

nhi 2/Al2O3.

th p, oxi-

cho nhi u ph n

10

11

I.4.3.

I.4. Alginate

ng d ng

a)

I.4.1.

t ,c

6H7O6

t

, d ng h

y sinh h sodium

i c a acid alginic

ng ho nghi

c t o dung d

ho c acid khi

nhi

o gel v

k t

c ng d ng trong nhi

b n,

c.

nh t ph thu c

chi

,

i, r t b n, ch u d

n 10

n ngh ch khi n

t.

t o keo t v

n

Ca2+ cao b)

n qua c u n i Ca2+ n ngh ch v i nhi

chi t xu

,

Ca2+

thu n ngh

hay th p.

n so v i kh

cs iv i

c ng d ng trong nhi o ra

h p th

t 32000-400000g/mol, trong

nh 2+

c ch

ng v t. Alginate

copolymer sinh h c

n

t

Alginate, c n chuy

d

th c ph m:

i.

ng trong th c ph m

h n ch

t o

cung c p 1.4kcal; t o l p ph

phim alginate

bi n nh s d ng dung d

ng d ng

c ns

2SO4.[2]

c ph m nh p c a vi khu n

t ph gia quan tr ng trong th c ph m

n xu

c gi

I.4.2. C

ph

nh c a s n ph m c c u t o t g c -D-mannuronate (M)

b ng lien k t 1-4 glucoside

g

M-M), polyG (G-G-G), polyGM (M-M-G).

-Lguluronate (G)

c

trong th c ph m.

polyM (M-

m, d

cs d

thu c nhu m, c i thi r

a Alg thay th

Trong y h

a

dai c a s i v i khi ch c n m

ng

ng l n tinh b t trong quay s i

c h c: Alg

cs d

b nhi

p ch t ch a tr

i

u qu nt

ch thu t

c cho dung d

cs d

t

nh,

t mang trong k thu t 4C

t

b c thu c. S n xu o

, protein v i t

12

13

342.2965g, chi m kho ng 2-8% v kh

d n truy n thu c; ch t mang nano ng d h c.[12]

ng trong s a.

galactopiranozyl-(1 - 4) -Dtt

g

m t -D-

oc

c

-Dm m t -D-

nk tv

t 1-4 glicozit.[20]

I.6.2. C

c,

I.5. Canxi-axetate Canxi-

3COO)2.

u ch b ng

m: CaCO3 + 2CH3COOH

Ca(CH3COO)2 + H2O + CO2

Ca(OH)2 + 2CH3COOH tr c

Ca(CH3COO)2 + 2H2O

ng

y

160o

20o 5C

ng d ng:

I.6.3.

S d

t ph gia trong th c ph m, ch y u s

ng d ng

n ph m k o; a)

cho canxi sunfat.

t c

t photphat trong ch

ng

m th ho

2+

un

tm

kim t Th

I.6.1.

Lac

galactose. ng s

th c ph Lactose

thi u cho s t lo i disaccharide,

n th ch t c c C12H22O11, kh

i.

n

c t t.

Lactose k t tinh ch m, tinh th c

I.6. Lactose

h ph n

ng t th tv

i

polymer Alginate.

u ki n nhi

B2 i ezyme

u d ng tinh th c ch s k t tinh c a lactose.

nh

15

14

S bi

a Lactose: khi gia nhi

lactose. Khi

i

nhi

Trong

c s n xu t t

i m t ph n t

d ng trong th

acid lactide, acid formide

gi i

I.7. c a Lactose:

OH hemiacetal c a

monosaccaricd th nh monosccarid th

tv

y disccarid t

monosccarid th

I.7.1.

OH ancol c OH hemiacetal

ng h

h bi n sang d ng m ch h

t do)

r

ng th

-CHO + 2[Ag(NH3)2]OH=> R-COONH4 + 2Ag+

3NH3+ H2O.

ng c a nhi ng d

ng: lactose th c ph

c ph m, lactose

ng. Chitosan

t kh

, kh

ng mu -aminophenol. K t

u qu

nanocomposite sinh h c

p.

[27] ng h

xanh l y d ch chi t t

Trong th c ph ngu n gi ch t h t

n v

n ng kh 4-

qu ch ra t

ng d ng

Lactose ng d

trong pha

ng h p in-situ

-

ph n

b)

gi i

s n xu

kh mu

b o qu

kh

k

phosphate; ch t v n chuy

a mu i,

, h p ch t t

t t o ng

xu t hi ng d ng tron

c ch s

n c a vi khu n, n

87.64%. [11]

ng; ph p ch t

d ng chi t xu t t

d

t kh c s n xu t b

c whey ho

a

ng h

c tinh ch

tB c s n xu

a hai lo

kobus

t ng h p ngo

n thi n v c

t

m

i t l ph

o

c ph m d ng b

c ph

t nhu

chuy

ng h p di n ra nhi

95oC nhanh

c ki

n Hoa K ,

ch nh p

cs d o kh i t v n chuy

ch

y trong c ch

p.

t 5-300nm.[15]

c

17

16

I.7.2.

c

c ng h p nano b

ch t mang 2-

hydroxylpropyl- -cyclodextrin (HPCD)/Alginate s d ng ch t kh chi t t

ng d

n ng kh

u t ng h

ch m. Qua

ng h p cho th y hi u qu ch

gi

t nano

t d ch chi t c a th c v t AuNPs/Chitosan, AuNps/Than ho b

ng d c

n

-

ng Au 1% cho k t qu t t nh t ph n ng oxy

ph i s d

o

u t ng h

t

ng h c s d ng mu

c h

4

10-

c

nh g n k t t ng th i c

Au3+:d ch chi t chanh 1:1, nhi

u ki n t ph n ng

nh

t t ng h p, t l

65oC, th i gian ph n c h t nano trung

5.48nm.[8]

tn i 3+

o

trong

c hi

r ng

ng nano t ng h

d ch chi

-CD tan t t trong

t ki m th

nh ch ng h

u t ng h cs d

n th

ng kh ion Au

vi khu n E.Coli.[7]

c, ch t kh

ng gel c a Alginate

t kh t d ch chi t c

ch t o h

UV-Vis cho th y s g n k

kh

gel d

c, g

c, gi thuy

n

k tv

polyvinylpyrrolidone (PVP)

t ch

td

250 C.[6]

dung d ch mu

yc ns d c. Nh

ng h p th N2, XRD, TEM. K t qu

cho th y m

nano

2+

. Alginate t o gel t

ng

c ud

ug

d ng d ch chi t t

ng h

u t ng h t mang than ho

ng

n ch

hay nh

ch t mang

c nh HPCD. [23]

ng h

m m i c a lu

I.8.

yv i u v i n i dung: thi.

19

18

II.1.3. Thi t b

TH C NGHI M

Thi t b s d

t, d ng c

II.1.

II.1.1.

t

-

t b th c nghi m

p: CH3COCH3 c c t hai l n

(UtralSonic Center), t s y

-

y t (Magnetic stirrer hot plate 78-1) M

y t gia nhi t MSH 20D

-

Sodium Alginate(Alg): (C6H7NaO6)n, xu t x Trung Qu c.

-

Calcium Axetate Hydrate, 99%: Ca(CH3COO)2.H2O, xu t x Netherlands.

-

Lactose: C12H22O11

-

Tetra Chlorauric(III) acid: HAuCl4.3H2O t

B

-

-

-

-

n

: 4-Nitrophenol, 99%: C6H5NO3; Methyl Orange 99%,

ng h p AuNps

(Centrifuge Machine Model EBA 20)

-

nt Thi t b s d

thu t t ng h p AuNps:

-Equinox-55cd

h ng ngo i IR Spectroscopy ho h p th b c x h ng ngo i c a ch t c

ghi l

Rhodamine B, 98%.

cc

, cho

a v t ch

i Trung

(Transmission electron microscope)

-

truy n qua - thi t b

-

Bercher 100mL, 250mL, 500mL

-

Micropipet 100-1000 l, pipet 0.5 mL, 1mL, 10mL

u vi c

n t

a v t r n nh

ng cao

nt

c h t nano, m

h t. Th c hi

iH

TGA (Thermogravimetry Analysis) -

-

t tr

nh kh ho c nh

Milipore 0.45 m

ng c a m -

u,

t b khoa h

II.1.2. D ng c

-

ng

, ng m u 3, 5, 10, 20mL

i c a nhi

iv thay v

ng c a m u v t r n b m

n pha, ghi nh n s t is

ng,

,

i

c kh i

cs d

cv is

nh

i v kh

ng

m

i p th , kh h p th .

ng s d Thermogravimetric

21

20

Analyzer with high temperature furnace (HT). Th c hi

t

Dung d

b khoa h

Ca(CH3COO)2

cc t2l

XRD

ng d

ux

n pha c

ch t r n. Trong gi

nhi u x

trong c

. Hi ih

c, v

peak ph

i u x t m i m t ph ng trong pha tinh th

Th c hi

c 100mL dung d ch Canxi Acetate.

nh c

i x ng c c

yt v it

Dung d ch Lactose ng

yt v it

thu c tr c ti p

c 200mL dung d ch Lactose.

D2-PHARSER -

Dung d

p TpHCM.

AuCl4.3H2

l

c x t ngo i g n hay kh ki n ng v

cc t2

a dung d

h p th UV-Vis JASCO V-630 Spectrophotometer-USA s d

cc t2l n

c gi y b c.

200-800nm, a h p ch t c n

T l

t s d ng trong ph n ng t ng h

t

l kh

ng

d ng kh

c kh

ng Alg

n:

c ph thu n

h

ch. Th c hi

c t i Vi

c

Vi t Nam.

mAlginate : mCa2+ = 4:1 mAlginate : mLactose = 3:1

Thi t b HORIBA SZ-100 s d

ch

ch td

II.2.2.

ng h nh c a h . Th c hi

i

t b khoa h

o ch t mang Alginate/Lactose Dung d ch

Khu y t

II.2. Th c nghi m II.2.1. Pha ch

t chu n b

Dung d ch Sodium Alginate c t2 l

Dung d ch

ng h p

qua

H gel 1

Dung d ch Lactose

c

Khu y t

yt v

qua

c 100mL dung d ch Sodium Alginate.

H gel 2 1

o ch t mang Alginate/Lactose

22

23

Thuy l cb

tb

ch lactose, alginate, canxi axetate

c h dung d

ion Au

c t ng h

a 100mL dung d ch Alginate, khu y t

t

y t

av

r as

tb

v it

o

nhi

120

nh n

v i s

t

nh 1000 u ki n nhi

,

th i gian t

qua gel l ng xu

ng t l v i n

3+

ng nh t. Nh t t t ng gi t 26.9mL

dung d

l

H

ng v i nhau, s d ng

II.2.4. Kh

c c t th c hi n l p l i 3

UV-Vis

il a)

c h gel 1.

ng t l kh

3+

ng gi

ng dung d Ti p theo cho t t 145,83mL dung d

yt

y

gel 2 sau khi o

nhi

90

c ng gel

nv

c c t, m i l

it

ch

gel 2.

ng ion Au3+

2. T l kh trong dung d kh

II.2.3.

ng n

:

t mang Alginate/Lactose

Kh Dung d ch

Dung d ch

Alginate

Ca(CH COO)

khu y t o nano: 6.002g => m

N

dung d

stock

= 0.0218g

= 3.4394*10-6 mol/mL

Th i gian khu y: 140 H gel 1

Dung d ch Lactose

T H gel 2

Dung d ch HauCl4.3H2O

khu

B ng 2. 1 B ng s li ng h T

Khu y t , gia nhi t 120oC

:120oC

Nhi

Gel 2(g

m kh mAu3+ (g)

nAu3+ ( moL)

ng t l Csample Vsample (mol/ L) (mL)

3+

Vstock (mL)

VH2O (mL)

AuNPs 1:0.02 0.0218 2

ng h

ch t mang.

0.000435

2.208

27.6

8

0.6420

7.3580

25

24

1:0.03 0.0218

0.000653

3.313

41.4

8

0.9630

7.0370

1:0.04 0.0218

0.000870

4.417

55.2

8

1.2840

6.7160

1:0.05 0.0218

0.001088

5.522

69.0

8

1.6060

6.3940

II.2.5. t o

a h

c h t nano t

ch t mang

b n c a h c n th c hi AuNPs

HR-TEM, TEM, EDX,

M

t hi n UV-Vis c a nano h p th c

b)

ic

ch n t l t

Lactose c hai t l kh

hi

ng

Th Zeta-

ng c a nhi

120 C, 130 C, t

nh nhi

B ng 2. 2 B ng s li t ng h (oC)

Nhi

t

c

AuNPs

ng Nanoblank

: 90oC, 100oC,

ch t mang Alginate/Lactose o

c

-

Ch n m t trong hai t l ti p t c kh h

XRD

Alginate

ng nhi

Sau khi kh

o

Nanoblank

TGA, IR

t ng h

m kh

Alginate

ng c a nhi

Th i gian

T l

90 100 110 120 130

T

Lactose

II.2.6.

khu y

u ng d

Kh

a AuNPs v i ph n ng gi a ch t kh NaBH4 sau: Rhodimine, Metyl Orange

1: 0.04

ng ch t nhu m s d ng r ng

p d t nhu m

mh

n s c kh

t th

cx

v i nhu m. c)

Kh

ng th i gian

ng c a th

ch t mang Alginate/Lactose 120p, 140p

c C14H14N3NaO3

ng h c th i gian: 0p, 20p, 40p, 60p, 80p, 100p,

i t l 1: 0.04, nhi -

t nh th i gian t

b

c,

uc

ch

o

C, t t ng h p nano

cacbon ph c t

p

-N=Nng k

. C

ch

nv ng ki

m nh

ch t nhu m monoazo, d ng

cam, h p th

26

Rhodamine B

27

c C28H31ClN2O3

thu c nhu

t nhu m

c khi th

ng.

p th m nh Ph n

c

N LU N

III.1. K t qu

m kh

ng ph Uv-Vis

552-554nm.

c th c hi n theo t l

III.1.1. K t qu kh

t: 2.5mL ch t oxi-

1mM ph n ng v i 0.2mL NaBH4 n

c a ph n

K T QU

nzen b m ngu

AuNP

nh quang,

0.05mL dung d ch AuNps. K t qu t

ng t l kh

ng gel so v i ion

Au3+

u ki ph n ng oxi-

c bi

kh

i ph thu

t l kh

ng

i s gi m peak trong UV-Vis.

1

K t qu

c bi

i ph thu c t l kh

ng.

UV-Vis

2 K t qu ph UV-Vis bi u di l

h p th +

.

t

28

UV-

29

nh

mang Alginate/Lactose.

t c a peak UV-

3.2, k t qu

UV-Vis

ch t mang Alg/Lactose

ng v i t l kh

p th gi ng nhau v

v

t h

ng

c

l

cho

548-549nm. T l

p th 530nm.

c t ng h

500-590nm. Qua

t ng h p

h p th peak UV3.1)

trong h ch t

nh

h p th

nh r ,s

ch

III.1.2. K t qu kh

ng nhi

4

th bi u di n m

h p th

p th khi

.

K t qu kh

UV-Vis

ng h

y r ng:

ng c a nhi o

90

t hi

o

hi

-130

kho

553nm xu t hi t 90-120o

3 K t qu ph UV-

h p th

ng b i nhi

.

C.

p th t 120-130o

ng h o

t

h p th

ng gi t

a nano

c nhi t gel ch t mang Alginate/Lactose

30

III.1.3. K t qu kh

31

K t qu

ng th i gian v

UV-

kh

ng h

th

h p th

p th

h p th

ng th hi n m

a th i gian

i nhi u, n m trong kho h p th

548-550nm khi

n theo th i gian. T

t i kho

peak h p th

t hi

n ra

ho c kh r peak l n nh t t i 140oC. T

t qu kh

u ki n t l kh

b ng ph UV-Vis cho th y 120oC v i t

ng h p t

khu 3+

th

6

th bi u di n m

h p th gian.

a th i gian ph n ng v p th .

ng b i th i

h p th

t tr

ng TGA.

c ch n ng Zeta-

i gian

i th

hai t l kh

Alginate/Lactose v i ion Au 5 K t qu ph UV-

ng, nhi

a gel

c ki ch

FT-IR,

32

33

T3-AuNP

III.2. K t qu o

77.52

III.2.1. K t qu

XRD

38.12o, 44.16o, 64.00o,

4 peak nhi u x o

T4-AuNPs v i

o

o

, 44.16 , 64.88 , 77.56o

ng v i

t [111], [200], [220], [311] c a m ng tinh th l

III.2.2. K t qu TEM ch

ng h

nh TEM. Dung d Alginate/Lactose T3i 20nm

ng h p v

-AuNPs. Kh c bi u di n

nh b

c

ng v i hai m u t nano t ng h p

th

T3-AuNPS

8 K t qu ch p TEM m u T3-AuNPs. 7 K t qu

C

u x tia X m u T3-AuNPs

c

nh b

nhi u x tia X h

c t i hai t l kh

-AuNPs.

bi u di n ph XRD c ng

i

ng r n t ng u T4-

-AuNPs.

nanocomposite.

34

9

th

35

h t nano t i T3-AuNPs.

t ng h h

u

i 20nm c a m u

n Alginate/lactose

.H

h t t 5-25nm, h

c 10ys

y

c

y u. T

i 11

ng h t nano t o ra nhi u.

th

h AuNPs.

So v i m u T3-AuNPs

T4-AuNPs

c h t nh ch nhi So v i T3Ch ng t h

3. 10 K t qu ch p TEM m u T4- AuNPs.

i 20nm m u T4-

nh TEM m u T4-AuNPs

u

cho

n Alginate/Lactose

t 2- 8nm n.

ms i

n

c h t c a T4-

ng u.

c nh ng h p s cho

n. c

36

III.2.3. Th

37

b nc ac

ng Zeta u nano tr ng, dung d o

nhi

a3m

c,

cho kh h keo b n v

n v ng c a t keo ph i l n, t

n. Khi tr s th zeta nh ng co c m l i. H gel b n khi cho th Zeta c a nano tr ng hai t l kh

ng

nh t t.

12 K t qu

th

ng Zeta.

c

s th

>30mV. K t qu th c nghi m

h 04 l

t nano

t trong h gel

u AuNPs t ng h p -102.7mV, -72.8mV, -73.3mV.

gel tr s th Zeta gi m xu ng, ch ng t h trong dung d

u ki n

n th 3.8V.

Th trong h keo

u T3-AuNPs, T4-AuNPs,

c

c hai t l

b nt t b n

38

39

K

ch t

III.2.4.

o

c h t nano c a hai m u T3-AuNPs, T4-AuNPs 90o

25 C m u T3-

III.2.5. K t qu

h

trong dung d ch

a m u nano tr i m u T4-AuNPs v

. K t qu

13 K t qu

c

t qu

nh ch p TEM

FT-IR

14 K t qu ph FT-

t.

c h t trung m c III.2.

41

40

t qu

IR c

u T3-AuNPs, T4-AuNPs,

III.2.6. K t qu

t TGA

Nanoblank, Lactose, Sodium Alginate: IR c a Alginate: ch c CH2

-COOH,

, t n s 1031.57cm c

c ether C-O-

t n s 3436 cm-1, t n s 2926.55cm-1

-OH -1

t n s 1612.77cm-1 ng v i n

ng

i x ng

t glucoside.

K t qu ph IR c a

hi n di n c

t n s 2901.61 cm-1

OH

t n s 3348.69cm-1,

-CH2, t n s 1658.3 cm-1

-1

s 1071.77 cm

ng v

c ether C-O-C.

K t qu ph IR c a nanoblank OH amide l i, 2927 cm-1 cm

t n s 3627.73 cm-1

m -COOH, 1652 cm-1

-CH2

-1

-CHO , t n

-CHO, 1594.41

a Lactose, 1034.77 cm-1

d ch chuy n

ether C-O-C. K t qu ph IR c a T3-AuNPs -CH2

t n s 3401.16 cm-1

-COOH, 1616.05 cm-1

a Alginate, 1082.46 cm-1

, k t qu ph IR c a T4-AuNPs

ether C-O-C. 3423.7cm-1, 2926cm-1 1035.95cm-1

-OH, 2928 cm-1

CH2

ether C-O-C.

cm-1 so v i ph IR-

T3AuNPs so v i m u nanoblank t 1500-1700 cm

c

CHO

t hi n peak c a

n ion Au3+

n2

n3

t

a Alginate ch

ng

n1

u IR-1

t PEAK

peak 1652, 1594

-

TGA c

t.

u

m u nano tr

th hi n s

B ng 3. 1 S li u k t qu

ph TGA c

t n s

COOH, 1621.97cm-1 cho th y r ng,

2+

-OH

15 K t qu

o

l i% 18%

Sodium Alginate

T (oC)/mloss(%)

25-220oC 22%

220-280oC 32%

280-800oC 28%

Lactose

T (oC)/mloss(%)

25-220oC 8%

220-325oC 54%

325-800oC 32%

6%

Nanoblank T (oC)/mloss(%)

25-210oC 16%

210-510oC 48%

510-800oC 15%

21%

T3-AuNPs T (oC)/mloss(%)

25-200oC 18% 25-180oC 18%

200-580oC 26% 180-270oC 30%

580-800oC 36% 270-800oC 40%

20%

.

T4-AuNPs T (oC)/mloss(%)

22%

42

43

36%. T ng kh i

ng m

t

T (oC): Nhi mloss(%): kh

T4-AuNPs

ng m

2,

t

m

Sodium Alginate t TG khi m u oxi-

t 220-280 C m

25-220oC m t 22% kh

ng, 280-800oC m t 28% kh

kh

ng m

ng. T ng kh

ng,

ng. T ng

ng

i k t qu ph nh t, t kho ng 150o

v

i trong h p ch t.

Lactose 25-220oC gi m 8% kh

t TG khi m o

ng, 325-800oC m

t 220-325 C m ng m

ng, ng.

ng tro c a Lactose b

y.

Nanoblank 25-210oC m t

t TG cho th y khi m u b oxio

ng, t 210-510 C m 15% kh

ng, t 270-800oC

ng m

ng. T ng kh

ng, 510-800oC m

ng m

ng.

Ca, Na.

T3-AuNPs t TG cho th y khi m u b oxio

ng, t 200-580 C m

m ib

i

th ub

Sodium Alginate, nano tr ng, T3-AuNPs, T4-

c a Ca.

T ng kh

n 270oC m t 40% kh

22% kh

o

kh

ng, t 180o

18% kh

t qu sau:

ng

25-180oC m

t TG cho th y m u khi b oxi-

u t 25-800oC, t l nhi t 10o

t tr

25-200oC m t

ng, 580-800oC m

o

i 100

b n nhi t cao

y b i nhi

ic a b n nhi t th p

y do s m

cc

44

45

Th c nghi

III.2.7. Kh o s S suy

a ch

ph n ng t sinh nhi n x y ra r t ch m.

m Metyl Orange, Rhodaminet ch t kh NaBH4 . N

b ng s

t ch odamine

c quan sau m

v i NaBH4 v h p th c a ph n

i NaBH4 di

c bi

y ch

AuNPs c a ph n

ch hai ch hi n di n c a ch

t ch

c ki m tra qua

ph UV-Vis

17 S

16 Ph n ng kh gi

[23].

c ch

ng kh

c a c

46

a) Kh

47

T4-AuNPs

ph n ng kh

T3-AuNPs

24 phút

20 K t qu ph UV-Vis ph n ng kh Metyl Orange v i NaBH4 - AuNPs theo th i gian.

18 K t qu ph UV-Vis ph n ng kh Metyl Orange v i NaBH4 - AuNPs theo th i gian.

19

th bi u di n h ng s t ph n ng kh AuNPs.

t

t

-

21

th bi u di n h ng s t ph n ng kh AuNPs.

-

48

K t qu ph UVNaBH4

49

20 c a ph n ng kh a hai m u T3-

peak MO

-

gi m d n

th

b) Kh

h p th c a

ng nb

ng th

c amine n ng t

NH2

ng h ch

c bi t khi T4-

T3-

c

nt

a ph n ng.

b m t ti

ng h c ph n ng th hi n t

ng s t

t o ra h p ch t

ph n

ch

nhanh.

a

t

m

T3-AuNPs

h p

n theo th i gian cho th y ho

AuNPs hi u qu

n ng kh

ph n

ph n -1

c ln (A/Ao) = i gian ph n ng, [Ao

MO t i th

)

h p th c a

h p th t i th i gian t (s) l

t i

ng 464nm.

B ng 3. 2 ch

n Alginate/Lactose v c a ph n ng kh NaBH4 v i Metyl Orange Ch

22 K t qu ph UV-Vis ph n ng kh Rhodamine v i NaBH4 - AuNPs theo th i gian.

t

23 K t qu ph UV-Vis ph n ng kh Rhodamine v i NaBH4 - AuNPs theo th i gian.

t

H ng s ph n ng k (sec-1)

T3-AuNPs(AuNPs/Alg/Lactose)

3.07x10-3

T4-AuNPs(AuNPs/Alg/Lactose)

6.73x10-3

AgNPs/HPCD/Alg(23)

1.79x10-3

PdNCs/HPCD/Alg(24)

2.24x10-3

50

51

K t qu ph UV-

T4-AuNPs

c a ph n ng kh Rhodamine a hai m u T3-

c a peak Rhodamine

h p th

554nm gi m d n theo th i gian cho th y ho

a AuNPs hi u qu Khi T4-

-

Rhodamine t h ng

-

n ng, t

ph n

nh m t l n n a ho T4-

ch

B ng 3. 3 ch

ph n ng x

n Alginate/Lactose v a ph n ng kh NaBH4 v i Rhodamine B Ch

24 K t qu ph UV-Vis ph n ng kh Rhodamine v i NaBH4 - AuNPs theo th i gian.

t

t

H ng s ph n ng k (sec-1)

T3-AuNPs

6.81x10-3

T4-AuNPs

14.39x10-3

d

25 K t qu ph UV-Vis ph n ng kh Rhodamine v i NaBH4 - AuNPs theo th i gian.

a T3-

(13)

5x10-5

AgNPs/HPCD/Alg(23)

2.23x10-3

PdNCs/HPCD/Alg(24)

2.75x10-3

ng

53

52

ch

K T LU N l c hi

m v lu

t ng h

i m u T43-4nm, t

ra:

ch t mang nanocomposite Alginate/Lactose, 3+

kh

nh

ng c a Lactose.

FT-IR

u ki

ch

t

ho

yl Orange c a hai t l kh

ik t

ng 1:0.03

Th Zeta c a m u T4th y s

u ki n t

ng h p AuNPs

T l kh

ng t

gi

ng gel Alginate/Lactose (

Nhi

-72.8mV, -73.3mV cho

nh cao trong h keo.

l

hai kho

t tr t ng kh i l

ng TGA c a T3-

i

Ho

ng h p 120oC.

t

a AuNPs Hai m u AuNPs t ng h p

tt

hai t l kh

-

-

c a ph n ng kh

a AuNPs

t

b ng ph UV-Vis cho th y s

n bi t

ng h

ng 1:0.03(m u T3-AuNPs)

c

hai t l

gi

h p th

Qua h ng s k (sec-1) k c

ch t mang

cc i gian ng n, chuy n t

(T4-AuNPs)

c h t , FT-IR, TGA cho th y: AgNPs t ng h

t

y Na trong Alginate Sodium, Ca trong Canxi axetate.

c ki m tra ho

k

-AuNPs cho th y

ng b m t c a m

khu

Th i gian khu

kh

4 m t [111], [200],

[220], [311].

ng

cc

-AuNPs cho th y s t o

i

c T

b n

-

K t qu ph XRD c a hai m u T3-

3+

v

-

qu ch p TEM.

n ng kh c a NaBH4

m RHodamine

trong dung d ch c a m u T3-

AuNPs

h ch t mang Alginate/Lactose, th c nghi

ng.

c

c nghi m kh

t ng h

u T3-AuNPs c h t nano ch y u t 10-

u,

n ch t mang h nanocomposite Alginate/Lactose.

nt

ph n

x y ra ph n ng c a T3ng trong ph n ng kh

ng h p ch

t

Trong ph n ng kh MO, h ng s t -3

-3

sec-1

-1

-3

sec

-3

ph n -1

sec

sec-1.

54

55

KI N NGH T ng h

U THAM KH O ch t mang nanocomposite

Alginate/Lactose,

t s ki n ngh

Ti ng Vi t:

u ti p theo c a

u ch t

m ts

ng d ng, Lu n

i H c Khoa H c Hu . ng nano t trong h keo.

Ki m tra ho

[

Th y, (2016), Chi t xu t Alginate t s 12, T

Sargassum Policystym b ng m t s

h c DHSP TPHCM.

c c a h nano.

[3] Nguy

ng d ng trong biosensor nh n bi t melamine.

),

c nano, NXB Khoa h c t

i.

Kh

g nv

Kh

ng h p nano kim lo

n.

[4 ch t mang

nano

h c k thu t th k th 21, T

c-

Cu

ng d

ng trong khoa

ih

c Th ng.

Alginate/Lactose.

[5] Ph m Th Qu nh, Ph m Th (2012),

u v c

ih

Alginate

[6]

nh Quy ng d ng c a

p Th c Ph m.

Huy n Trang, Nguy n H

Huy

n Quang Vinh, Ph m Thanh u t ng h

t

T

n

c

. t,

[7] (2013),

u t ng h

nk tv

n E. coli O157, T

[8

ng Thi n, H

Nguy n Vi h

m Nhung, Hu nh Thu H nh,

n Quang Long, (2014), S d ,T

ih cC

ng

56

[9

n, (2011),

hi n nay

n t t nghi

57

uv h

ng ng d ng

ih

-

i h c Qu

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Ph l c 1

c h t m u T3-AuNps.

60

61

Ph l c 3

Ph l c 2

c h t m u T4-AuNPs.

c h t m u nano tr ng.

62

63

Ph l c 5 Th Zeta m u T4-AuNps.

Ph l c 4 Th Zeta m u T3-AuNPs.

64

65

Ph l c 6 Th Zeta m u nano tr ng.

Ph l c 7 nh ch p

-AuNPs.

66

67

Ph l c 9 Ph nhi u x XRD m u T4

Ph l c 8 nh ch p TEM m u T4-AuNPs.

AuNPs.

68

69

Ph l c 10 Ph nhi u x XRD m u T3-AuNPs.

Ph l c 11 K t qu

t tr ng TGA c a m u T3AuNPs.

-

70

71

Ph l c 13 K t qu

Ph l c 12 K t qu

t tr

ng TGA c a m u nano tr

t tr

ng TGA c a Lactose.

72

73

Ph l c 14 K t qu ph IR c a Alginate sodium.

Ph l c 16 K t qu ph IR m u tr ng.

Ph l c 15 K t qu ph IR c a Lactose.

Ph l c 17 K t qu ph IR m u T3-AuNPs.

74

Ph l c 18 K t qu ph IR m u T4-AuNPs.