Tp ch Ha hc, T. 44 (4), Tr.

465 - 470, 2006

tnh cht c hc v hnh thi cu trc

ca polyme blend polyamit/polypropylen
n Ta son 26-9-2005
o Th Minh, Trnh Sn H
Vin K thut Nhit i, Vin Khoa hc v+ Cng ngh Vit Nam
SUMMARY
The aims of this work were to prepare compatibilizers and polymer blends at a pilot scale
served for the railway branch. Firstly, the grafting of maleic anhydride into polypropylene (PP-gAM) was carried out by an industrial single extruder at the temperature zone 165 - 180oC and
was qualitatively and quantitatively characterized by Infrared Spectroscopy. The grafted maleic
anhydride contents were found to be 0.46 - 1%. Afterward, polymer blends of polyamide and
polypropylene were prepared with a industrial injection molding machine in presence of the
maleic anhydride grafted polypropylene as a compatibilizer. It clearly showed that the
mechanical properties of the PA/PP-g-AM/PP blends in term of tensile strength and elongation at
break were 6.43 and 1.34 times higher than those of the PA/PP mixiture without a compatibilizer.
The creep testing results showed that the blend was deformed 1.4% by a load of 9.73 MPa and by
a load of 12.16 MPa the blend was deformed 2.86%, but no break was observed. It proved that
there were no phase separation due to good adhesion between polyamide and polypropylene
thanks to PP-g-AM compatibilizer. The SEM images showed that the blend PA/PP-g-AM/PP had
a fine structure and appeared only the little carckings by imposing a load of 208 MPa while the
grand and long crackings appeared onto the mixture PA/PP only by a load of 56.99 MPa.

I - M u
Vt liu polyme blend c ch to bng
vic trn hp hai hoc nhiu polyme khc nhau
kt hp c nhng tnh cht ni tri ca mi
polyme th2nh phn. Polyamit (PA) v2
polypropylen (PP) l2 hai polyme k thut quan
trng. PA th ng c s dng ch to cc chi
tit: in, c kh v2 cc chi tit cho t do c
tnh cht c hc cao, chu nhit, chu m2i mn,
d gia cng v2 sn xut. Tuy vy, kh nng chu
va p, n nh v kch th c v2 bn i
vi mi tr ng m km, cng thm gi th2nh
ca PA t ng i t, do vy vic ng dng
polyme n2y trong mt s lnh vc b hn ch.
Nhng nh c im trn ca PA c th khc
phc bng vic trn hp vp PP. Nh U bit PP
c tnh cht c hc t ng i cao, chu m v2

gi th2nh thp. ng tic l2 PA v2 PP khng

trn hp c. Do vy, cn phi a thm v2o
t hp vt liu polyme blend nhng cht t ng
hp c kh nng kt dnh gia hai pha nhm to
ra polyme blend c tnh cht c hc tt. Nhiu
nm tr li y, polyme blend PA/PP U c
nhiu tc gi nghin cu [1 - 6]. Trong cng
trnh n2y chng ti trnh b2y kt qu ghp
anhiric maleic (AM) ln PP trn thit b n
cng nghip, tnh cht c hc v2 hnh thi cu
trc ca vt liu polyme blend PA/PP c ch
to trn my phun cng nghip nhm mc ch
ch to mt s ph kin 2n hi phc v cho
ng2nh ng st Vit Nam.
II - thc nghim
1. Nguyn liu v ha cht chnh
465

- PA6: Sn phm th ng mi ca hUng

Toray (Nht Bn) dng ht, t trng 1,13
g/cm3, ch s chy 25 g/10 pht (230oC, ti
trng 2,16 kg), khong nhit nng chy
224oC.
PP: Sn phm th ng mi ca hUng
Samsung (H2n Quc) dng ht, t trng 0,9
g/cm3, ch s chy 3,5 g/10 pht (190oC, ti
trng 2,16 kg), khong nhit nng chy
165oC.
AM: Sn phm th ng mi ca hUng Sigma
Aldrich (M), nhit nng chy 52,8oC,
tinh khit 97%.
DCP (dicumyl peoxit): Sn phm th ng
mi ca hUng Aldrich (M), tinh khit 97%.
Cht t ng hp so snh (copolyme): l2
sn phm ng trng hp gia propylen v2 AM
ca hUng Exxellor (CHLB c), c tn th ng
mi PO 1015, h2m l ng AM l2 0,4%, t trng
0,9 g/cm3.
2. Ghp AM ln PP
Qu trnh ghp AM ln PP ch c tin
h2nh nh sau:
- Trn PP vi AM v2 DCP vi cc t l khc
nhau;
- Ghp trn thit b n ct ht nhit t
165oC n 180oC;
- L2m lnh v2 ct ht ;
- Sy kh.
3. Ch to polyme blend PA/PP-g-AM/PP
Vt liu PA, PP v2 cht t ng hp PP-g-AM
c trn trong thit b trn cc t l khc
nhau, sau phun trn thit b phun Woojin
Selex E-150 ca H2n Quc trong khong
nhit 230 - 255oC v2 p sut 150 MPa. Mu
c phun dng hnh ch2y theo tiu chun
ASTM D 638-99.
4. Cc ph*ng php phn tch
a) Xc nh h+m lKng AM ghp v+o PP
Mu PP sau khi ghp AM c trch ly bng
axeton trong 8 gi loi AM khng phn ng
v2 sy 70oC trong 8 gi. H2m l ng AM c
xc nh dng m2ng c chiu d2y 50 m trn
466

my hng ngoi Perkin Elmmer, da v2o s

xut hin v2 c ng pic dao ng ca nhm
cacbonyl CO thuc vng anhiric maleic di
khong 1786 cm-1. H2m l ng AM c ghp
ln PP (% trng l ng) c tnh da v2o t l
din tch A1786/A1166 (A1786: din tch ca pic ca
nhm CO 1786 cm-1 t ng ng vi l ng AM;
A1166: din tch ca pic ca nhm CH3 1166
cm-1 t ng ng vi nhm CH3 ca PP) v2 ng
chun A1786/A1166 - h2m l ng AM.
- Phn tch nhit DTA
Tin h2nh trn thit b Shimadzu DSC-50,
trong mi tr ng khng kh, t nng t nhit
phng n 400oC vi tc 10oC/pht.
- Kho st hnh thi cu trc ca vt liu
polyme blend
Bng knh hin vi in t qut (SEM). Mu
c ct trn microtone th2nh bn mng 50 m,
ph kim loi v2 c chp bng thit b knh
hin vi in t qut Jeol-5300 (Nht Bn).
- o tnh cht c hc
C ng ko t b v2 giUn d2i t ng
i khi t b c o trn my o tnh cht c
hc ZWICK (CHLB c). Mi blend o 3 mu
ly gi tr trung bnh.
- o rWo theo ko
Trn my STRAINVIS COD. 6800.000 ca
hUng CEAST (), ti Trung tm nghin cu vt
liu polyme, Tr ng i hc Bch khoa H2 Ni.
Mu c th nghim ti trng 40 kg (9,73
MPa), 50 kg (12,16 MPa), nhit 40oC trong
72 gi.
III - Kt qu v tho lun
1. Ghp anhiric maleic ln PP
Hnh 1 trnh b2y ph hng ngoi ca mu
PP v2 mu PP-g-AM. mu PP xut hin pic
1722 cm-1. Pic n2y theo Lion Xavier [7] ng vi
dao ng ca nhm CO thuc nhm hiropeoxit
(COOH) ti nguyn t cacbon bc ba, hnh
th2nh do PP b oxi ha trong qu trnh l u tr
trong kho. Ng c li, mu PP-g-AM, pic n2y
b mt v2 xut hin pic mt pic mi

Transmission, %

PP-g-AM

PP
PP-g-MA

Hnh 1: Ph hng ngoi ca PP v2 PP-g-AM

1786 cm-1, ng vi dao ng ca nhm CO ca
vng anhyric maleic. iu n2y chng t khi
ghp AM v2o PP, nhm hiropeoxit U b phn
hy to th2nh gc v2 cng vi cc cht khi
m2o phn ng DCP U tham gia v2o qu trnh

khi m2o phn ng ghp AM ln PP. Kt qu

xc nh nh l ng cho thy AM ghp v2p PP
l2 0,5 - 1%. PP sau khi ghp AM vn gi c
tnh cht c hc kh tt.
2. Phn tch nhit

DTA, uV
5,00

0,00

-5,00

164,8oC
224,4oC

-10,00
0,00

100

200

300

400
o

Nhit , C
Hnh 2: Gin DTA ca blend PA/PP-g-AM/PP
Kt qu phn tch nhit cho thy polyme
blend PA/PP-g-AM/PP c hai pic thu nhit
164,8oC ng vi nhit chy ca pha PP v2
224,4oC ng vi nhit chy ca pha PA. Gia
hai pic trn khng tn ti pic thu nhit ca pha
hn hp PA/PP. iu n2y cho thy blend
PA/PP-g-AM/PP ch c hai pha v2 cht t ng
hp PP-g-AM tn ti mt phn cch gia cc

pha PA v2 PP ch ng vai tr cht kt ni ch

khng to mt pha ring bit.
bn ko t ca hn hp PA/PP, ca
blend PA/PP-g-AM/PP cng nh ca blend
PA/copolyme/PP c trnh b2y hnh 3. Qua
hnh 3 chng ta c th d d2ng nhn thy khi ch
trn hp n thun PA v2 PP v2 khng c mt
ca cht t ng hp th tnh cht c hc ca hn
467

dnh vi pha PA qua cu lin kt hydro hoc

phn ng ca nhm AM ghp trn mch PP vi
cc nhm amin v2 amit ca PA.
Khi so snh gia blend PA/PP-g-AM/PP s
dng cht t ng hp ch to trn my n do
chng ti t ch to v2 PA/copolyme/PP s
dng cht t ng hp nhp ngoi chng ti nhn
thy khng c s khc bit ln v tnh cht c
hc. Cc ch s v bn t, giUn d2i khi
t v2 do ca hai t hp trn u t ng
ng (xem bng 1).
ng sut, MPa

ng sut, MPa

hp PA/PP rt km, dUn d2i t ng i ch t

46% v2 bn ko t ca hn hp PA/PP cng
ch t 39,04 MPa, thp hn rt nhiu so vi PP
v2 PA ban u. Khi c mt ca PP-g-AM tnh
cht c hc ca blend tng ln rt nhiu (hnh
2b): giUn d2i t ng i khi t t ti 296%
tc l2 cao hn so vi PA ban u. Vai tr ca
cht t ng hp y c th gii thch qua vic
hnh th2nh mt lp chuyn tip gia hai pha PP
v2 PA t PP-g-AM. Nhng on mch ca PPg-AM U kt dnh vi pha PP ng thi cng kt
80
a
60

80
b
60

40

40

20

20

20

40

60

20

40

Bin dng, %

Bin dng, %

Hnh 3: Gin ph thuc ca bn ko t v2o giUn d2i t ng i ca hn hp PA/PP

khng c cht t ng hp (a) v2 blend PA/PP-g-AM/PP (b)

bin dng, mm

4. bn ro ca vt liu
1,5
1,4
1,3
1,2
1,1
1,0
0,9
0,8
0,7
0,6
0,5
0,4
0,3
0,2
0,1
0

10

15

20

25

30

35

40

45

50

Thi gian chu ti, h

Hnh 4: bin dng rUo ko ca blend PA/PP-g-AM/PP
468

55

60

60

Kt qu o rUo theo ko ca vt liu

ng sut 9,73 v2 12,16 MPa, nhit 40oC
trong thi gian 55,42 gi c trnh b2y hnh
4. ng sut 9,73 MPa mu b bin dng 1,4%,
mun rUo gim t 4524,7 xung 555 MPa v2
ng sut 12,16 MPa mu b bin dng 2,86%,
mun rUo gim t 1123,3 MPa xung 340,6

(a) Hn hp PA/PP

MPa. Nh vy, d i tc ng ca ti trng theo

thi gian vt liu blend c b bin dng, song
khng b ph hu do khng b tch pha. iu
chng t PA v2 PP c s kt dnh tt.
5. Hnh thi cu trc ca polyme blend
PA/PP-g-AM/PP

(b) Blend PA/PP-g-AM/PP

Hnh 5: nh SEM ca hn hp PA/PP v2 polyme blend PA/PP-g-AM/PP

Cu trc ca ca hn hp PA/PP v2 vt liu
blend PA/PP-g-AM/PP c th hin hnh 5.
Chng ta d d2ng nhn thy, hn hp PA/PP
(hnh 5a) c cu trc rt th c nhiu cc hc,
cn blend PA/PP-g-AM/PP (hnh 5b) c cu

(a) Hn hp PA/PP 56,99 MPa

trc rt mn, rt kh phn bit c ranh gii

ca cc pha v2 ho2n to2n khng c cc l, cc
hc. R r2ng nh c cht t ng hp cc pha ca
polyme blend phn tn u v2 lin kt vi nhau
cht ch hn.

(b) Blend PA/PP-g-AM/PP 208 MPa

Hnh 6: nh SEM ca hn hp PA/PP v2 polyme blend PA/PP-g-AM/PP khi b ph hy

(chp ph ng song song vi lc tc ng)
Hnh 6 trnh b2y cu trc ca hn hp
PA/PP v2 polyme blend PA/PP-g-AM/PP khi b
ph hu ko t. D d2ng nhn thy khi tc

dng lc c hc v2o vt liu xut hin s bin

dng ca cc pha cng nh s tch ca cc pha.
Mt iu th v l2 hn hp PA/PP do khng c
469

cht t ng hp, cc pha khng c s lin kt

cht ch do chng b tr t rt mnh v2 tch
khi nhau, to ra cc vt nt d2i ln c ng
ko t 56,99 MPa. Trong khi polyme
blend PA/PP-g-AM/PP do c cht t ng hp
PP-g-AM nn cc pha kt dnh vi nhau tt hn,
qu trnh tr t ca cc pha cng xy ra t hn,
ngay c c ng ko t 208 MPa (gp 4 ln
c ng ko t ca hn hp PA/PP), song ch
xut hin cc vt rch rt nh.
IV - Kt lun
- U ch to c cht t ng hp PP-g-AM
c h2m l ng AM l2 0,5 - 1% trn thit b n
cng nghip.
- U s dng PP-g-AM ch to polyme
blend PA/PP-g-AM/PP trn thit b phun cng
nghip. Vt liu polyme blend c tnh cht c
hc cao p ng c vic ch to mt s ph
kin 2n hi cho ng2nh ng st.

470

T i liu tham kho

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3. S. H. Jafari, A. K. Gupta. J. Appl. Polym.
Sci., 71, 11153 - 11161 (1999).
4. RaJ K. Datta, Malcolm B. Polk and Satish
Kumar. J. Polym. Plast. Technol. Eng., 34,
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Ha hc, T. 40, s B, Tr. 165 - 167
(2002).
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