*department of chemistry, korea university, seoul 136-701, korea · 2005-03-29 · plasticoder...

6
Polymer(Korea), Vol. 29, No. 2, pp 166-171, 2005 / 166 1.# g«# ^F W, ZW ú^úÒ Ã q6 Þ &" Ò ÿ ®& Ò WÛ zR& à Îòn Þ:. B ² ® V2þª² ήB :FR Ú& ®² zRÊ óV® 6 ÞÆ, Z{Ö®V V'r K>C VÖÚÊ RÊV Þê ÊC& Z®®6 Þ ¢& ^F® zR& ®² 6V î î6 Þê êÊ:. Ê o rÒ Ê® ZÊ ²R&ê ^F"® 6 û vÊ Rr F ÚÒV n6 Þ:. ß, ^ FJª, VãJª e nÛ ^w v GR o ^F > v « R ® ^F"& Ö¿nê òF ^F 2ú²® r r GÊÆ Ê& Î ² ^F"® rrÊ ²r®â ßn6 Þ:. 1,2 6Z« ^Fÿ 6Úæ "²ê EPDMR :® 6(silicone rub- ber, SR) GÊ R² ÿr:. EPDM &NbR Z²bR j*Ê Þ2¯W² ¿² &g¿²r W , n, J GÊ :Î v 6:J: n®6, ª¯ ÂÆ& OV r è vZ{ e ª²î Z Và l", ÎÖ&r û Z ÿ®V Óâ Jªn vZbV Òò:. 3 :® 6ê Úæ ÂÆV :³(Si-O) ¿Î ² Ê> Þ ¢& :Î v 6& ¦®B , zÊ, â G& ®² ª k, JR ZW Ê : n®:. B² ²Ê&^ê rn û2r ï r®Æî r3 Ò ê² 4 ®&r û2Z Îòn ²Ê® rnÊ ãW² vr:. NBî, VÿÊ 6VÊÆ W Ê î ² >fÊ Þ:. Ê o EPDMR :® 6® >f J®B 6Z« ®& r ÿÊ Vû² ^F ZÊ EPDM/SR jb2& V² FÂV ²rÞ ßn6 Þ:. Kole G 5-7 V²WÎ ÿ jb 2Î EPDM/SR jb2® ÿ û2r n² W Z² ^ F² n&^ÎÊ NîZr EPDM(MAH-g- EPDM) R ÂN2V NîZr :®(acrylamide- g-silicone)® :#¥#HSGP2 ÊnÊ# &# <bÌ# .á# «I# HÞ# `k}¿|·}»6ã }§L # -^¬# ðq(|p/# d(# ^<# # +5337T# 44# 58¼# Q:/#5338T#5# 5;¼# T,# # Lqioxhqfh#ri#Wkhupdo#Djlqj#rq#wkh#Surshuwlhv#ri## HSGP2Vlolfrqh#Uxeehu#Eohqgv# \x0N|rxqj#Fkxqj/#Vxqj0Jrr#Ohh/#Erqj#Udh#Fkr*/#dqg#Nlo0\hrqj#Fkrl # Reliability Assessment Center, Korea Research Institute of Chemical Technology, Daejeon 305-600, Korea *Department of Chemistry, Korea University, Seoul 136-701, Korea (Received November 25, 2004;accepted February 28, 2005) S¨Ü EPDM(ethylene propylene diene monomer)/:® 6 jb2Ò ®6, ÿªr JΪ 2Z& Î ªÒ J®:. EPDMR :® 6(SR)® Æê 90/10&r 10/90 wt% ʲ Æ^®VÆ, Bra- bender® PlasticoderÒ ÿ®B ÿ ¿®6, JZ^ú² V¦®V:. V¦r EPDM/SR jb2® þJ²Ò RZæZN² V®V:. B², jb2Ò 100 ×&r 24, 48, 962Z / JΪ2r , Îû k, 6û e g_W wk®V:. þJ²Ò Ʋ R ÿªrÒ þV² jb2® Ú® ÂV fâ®V:. JΪ 2ZÊ óV¾& Ò, jb2® Îû kê fâ®VÆ, 6ûR g_W óV®V:./ Abstract: EPDM (ethylene propylene diene monomer)/silicone rubber blends were prepared and the influence of a compatibilizer and thermal aging on the properties of the blends was investigated. The blends of which the compositions were varied in the range of 90/10 through 10/90 wt% were melt mixed by using a Brabender Plasticoder (internal mixer) and were vulcanized by a hot press. The morphology of the vulcanized EPDM/SR blends was examined by scanning electron microscopy (SEM). After the thermal Aging for 24, 48, 96 hrs at 100 × in an air oven, hardness, tensile strength, elongation and contact angle of the blends were investigated. From the result of the morphology, it was confirmed that the domain size of the blends containing the compatibilizer was reduced. As the increase of the thermal aging time, hardness and tensile strength of the blends decreased but elongation and contact angle increased. Keywords: EPDM, silicone rubber, compatibilizer, thermal aging, MAH-g-EPDM. / To whom correspondence should be addressed. E-mail: [email protected]

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Page 1: *Department of Chemistry, Korea University, Seoul 136-701, Korea · 2005-03-29 · Plasticoder (internal mixer) and were vulcanized by a hot press. The morphology of the vulcanized

Demo

Polymer(Korea), Vol. 29, No. 2, pp 166-171, 2005 �

166�

1.����

������ ���, ��� ����� �� �� �� �� �

�� �� ��� �� �� ����� �� ���� ��. �

� �� ����� �� ��� ��� �� ��� ���

� ���, ����� ��� ����� ���� ��� ��

����� ���� �� ��� ���� ��� �� ��� �

��� �� ����. �� �� ��� ���� �� ����

����� ��� �� ��� �� �� ��� �� ��. �, �

� �, �� � � �� �� �� �� �� �� �� �� �

�� ���� ����� ���� �� ��� �� ���� �

� ��� �� �� �� ����� ��� ���� ����

��.1,2

��� ��� �� ���� EPDM� ��� ��(silicone rub-

ber, SR) �� �� ����. EPDM� ���� ���� ���

������ ��� ������ ��� ��, ���, � �

�� �� �� ����� ���, � ��� ���� ��

�� ��� � ��� �� ���� ���, ��� ��

� ����� � �� ��� ����� ����.3 ���

��� � ��� ���(Si-O) ��� ���� ��� ��

��� �� ��� ��� �� ��, �, � �� ��

�� ���, � �� ��� ��� � ���. �� ��

������ ���� ���� ���� ����� �� ��

� ����4 �� ��� ��� ����� ��� ����

����� ����. ���, �� ���� ��� ��� �

� ��� ��.

�� �� EPDM� ��� ��� ��� ��� ��� ��

��� ��� ����� �� �� EPDM/SR ���� �

��� ��� ���� ��. Kole ��5-7 ���� ���� ��

�� EPDM/SR ���� ���� ���� �� ��� ���

�� �� �� ��� ������ ����� EPDM(MAH-g-

EPDM)� ������ ����� ���(acrylamide-g-silicone)�

���������������������������������

����������������

��

����������������������������

� ������� ���� �������������� ��� ������

����� ��������������������������������������

�������� �����������������

�������������� ����������������������*��������������������Reliability Assessment Center, Korea Research Institute of

Chemical Technology, Daejeon 305-600, Korea

*Department of Chemistry, Korea University, Seoul 136-701, Korea

(Received November 25, 2004;accepted February 28, 2005)�

��� EPDM(ethylene propylene diene monomer)/��� �� ���� ����, ����� �� ��� ��

�� ��� �����. EPDM� ��� ��(SR)� ���� 90/10� 10/90 wt% ��� ������, Bra-

bender�� Plasticoder� ��� �� ����, ���� ����. �� EPDM/SR ���� �����

�������� ����. ��, ���� 100 �� 24, 48, 96�� �� ���� ��, �� �, ��

� � ��� �����. ����� ��� �� ����� ��� ���� ���� ��� ����.

�� ��� ���� ��, ���� ��� �� �� �����, ���� ��� �����.�

Abstract:�EPDM (ethylene propylene diene monomer)/silicone rubber blends were prepared and the influence of a

compatibilizer and thermal aging on the properties of the blends was investigated. The blends of which the

compositions were varied in the range of 90/10 through 10/90 wt% were melt mixed by using a Brabender

Plasticoder (internal mixer) and were vulcanized by a hot press. The morphology of the vulcanized EPDM/SR

blends was examined by scanning electron microscopy (SEM). After the thermal Aging for 24, 48, 96 hrs at 100 �

in an air oven, hardness, tensile strength, elongation and contact angle of the blends were investigated. From the

result of the morphology, it was confirmed that the domain size of the blends containing the compatibilizer was

reduced. As the increase of the thermal aging time, hardness and tensile strength of the blends decreased but

elongation and contact angle increased.

Keywords: EPDM, silicone rubber, compatibilizer, thermal aging, MAH-g-EPDM.

†To whom correspondence should be addressed. E-mail: [email protected]

Page 2: *Department of Chemistry, Korea University, Seoul 136-701, Korea · 2005-03-29 · Plasticoder (internal mixer) and were vulcanized by a hot press. The morphology of the vulcanized

��� EPDM/��� �� ���� ��� ��� �� 167�

Polymer(Korea), Vol. 29, No. 2, 2005�

��� ��� �� ��� � ��� �����. ��, Kim �

�8 EPDM/SR ���� �� ��� ���� ��� �� ��

��� � ��� ��� � ���, Kang ��9 ����� MAH-

g-EPDM-polydimethylsiloxane� ������, ��� ����� EPDM/

SR ���� ��� ��� ��� �� �� ��� ���

�� � ��.

� ���� ����� EPDM/SR ���� ��� �� �

���� ��� ��� ���� �� � ��� �� �� ��

� ���� ������, ����� �� ��� �� � �

�� ����, ��� ��� ��� ��� �����.

2. ��

2.1 ��

EPDM� 5-ethylene-2-norbornene(ENB)� ��� Du Pont�� Nor-

del IP NDR4640(ethylene/propylene/ENB�55/40/5 wt%; ���0.86;

Mooney viscosity ML1+4, 125 ��40)� ������, SR� Dow Cor-

ning�� Silastic GP437(vinyl methyl based silicone; ���1.1; �

� 190)� �����. ����(compatibilizer�C)� �����

� ����� EPDM� Crompton�� Royaltuf 498(maleic anhydride

1.0 wt%; ���0.89; Mooney viscosity ML1+4, 125 ��30; Tg�46 �)

� �����, ���� di(tert-butylperoxy-isopropyl)benzene� ��

� 40 wt%� Akzo Nobel�� Perkadox 14-40MB� �����.

2.2 ���� �� � ����

� ��� ��� EPDM/SR ���� ��� Table 1� ��

���. ���� Brabender�� Plasticorder� ��� 50 �, 60

rpm�� ��� �� �����. Table 1� ��� ���� �

� �� EPDM� ����� ��� 3�� ��� �� ���

�� SR� ���, ��� � � 5� �� ��� �, ��

� ��� 5� �� ��� EPDM/SR ���� �����. �

�� �� ���� hot press� ��� 170 �� 2000 psi�

���� 10�� ��� ��� 1 mm� ���� ���� �

����. ���� ���� ��� �� �� 150 �� ��

� ��� � ��� 2�� �� �����.

2.3 �� ��

�� �� ���� �� ��� �� �� �� Alpha Tech-

nology�� oscillating disk rheometer(ODR, ODR-2000)� ���

ASTM D 2502� �� ��� 170 �� ���� 3°� ��� �

���� � �� �� �����.

2.4 ����

��� ����� JEOL�� scanning electron microscope(SEM,

JSM-6700F)� ��� ����. ���� ��� ��� �

���, � �� �� ��� �� �� �� 1�1� ���� 2�

� �� ��� EPDM� ��� �, ��� ��� ���

��. �� �� 500 �� ����� 5 kV �����.

2.5 ����

EPDM/SR ���� ��� �� �� ��� ���� ��

KS M 6518� ���� �� � � �� ���� ��� 100 �

� 24, 48, 96�� �����.

2.6 ��� ��

���� � �� � � ���� ��� ��� ��� �

�� ���� �� ��, �� � � ���� �����.

��� KS M 6518� � ��� ��� Shore Instrument�� Shore

A-2� ��� �� � 5�� ��� ����� �����.

�� �� ���� Instron�� �����(UTM, 5567)� ��

� KS M 6518� ��� 3 ���� �����. ���� ��

��� ��� � ������, crosshead speed� 500 mm/min, grip

�� 20 mm� �����.

2.7 ���

�� ��� ���� ���� �� SEO�� contact angle

(300A)� ��� ���(sessile drop)�� �����. ��� �

� � ��� ��� ��� �� 10 µL� ��� ��� ��

���� ���� 5 �� � ��� ���� �����.

3. �� � ��

3.1 �� ��

�� ��� ��� ��� �� ��� �� ��� ��

� ���� � ��� ��� �� � ��� ��� �

� � ����. ��� ��� ��(ts2)� �� � ��(tc90)�

��� �� ��� ����� ����� ��� �� ���

���� �����. �� � ��� �� ���� ����

��� ��� ��� ��� ��� ��� � ��� ���

� �� ����. � ��� EPDM � ��� �� ��� 8�

15� ��� �� ��� ��� ����.10,11

EPDM/SR ���� ��� ����� �� ��� �� ODR

�� ��� Figure 1� 2� ������, �� ��� Table 2�

3� �����. SR� ��� ���� �� ��� ��� ��

� ��� ��� ���� ����� � �� �� ��

�� � ��. �� �� ��� � ��� ���� ��� �

�� �� � ��� EPDM�� ��� ����.

����� ��� � �� �� � ��� ���� �� �

�� ����. �� ����� ��� MAH-g-EPDM� ���

�� ���� �� ��� � �� ����� � ���

����� ��� ����.

3.2 ����

� ��� � ��� ���� � �� ��� �����

�� ��� ��, ��� �� �� ���� ���� �� ��

���� ��. �� ���� � �� �� ��� ��� ��

Table 1. Formulation of EPDM/SR Blends (unit : phr)

Sample EPDM SR Compatibilizer Perkadox Pure EPDM EP90/SR10 EP70/SR30 EP50/SR50 EP30/SR70 EP10/SR90

Pure SR EP90/SR10/C5 EP70/SR30/C5 EP50/SR50/C5 EP30/SR70/C5 EP10/SR90/C5

100 90 70 50 30 10 0

90 70 50 30 10

0 10 30 50 70 90

100 10 30 50 70 90

0 0 0 0 0 0 0 5 5 5 5 5

6 6 6 6 6 6 6 6 6 6 6 6

Page 3: *Department of Chemistry, Korea University, Seoul 136-701, Korea · 2005-03-29 · Plasticoder (internal mixer) and were vulcanized by a hot press. The morphology of the vulcanized

168� ���������������

���, �29� �2�, 2005� �

�� ��� ��� ���� ��� � ��� �����

��� ��, �� ��� ���� ����� ��.12

EPDM/SR ���� ���� ��� ��, ��� �� 1�

1 �� �� ��� ���� EPDM� ��� � SEM�� ���

�� �� Figure 3� �����. ����� ���� �� �

� EPDM� 90�50 wt%� ���� ���� ��� �� EPDM

� ���� ��� SR �� ����, EPDM� �����

SR� ���� ����� �����. EPDM� ��� 30�10

wt%� � �� ��� EPDM� ��� �� ��� ���

�� SR� ����� EPDM� ���� ��� ���� ���-�

�� ����� �����. � ��� ��� ����� co-

continuous ����� ��� ����, �� ����� EPDM

� ��� 31� 49 wt% ��� ���� ���� ����

��� ����.

����� ��� � �� ���� ����� ����� �

��� �� � � ��� ��� �����. �� ���� �

Table 2. Curing Characteristics of EPDM/SR Blends

ODR(170 �) Sample

MH(N�m) ML(N�m) ts2(sec) tc90(sec) Pure EPDM 59.28 5.86 78 750

Pure SR 24.59 2.29 40 502 EP90/SR10 55.74 4.15 64 576 EP70/SR30 50.47 3.63 57 502 EP50/SR50 41.70 2.97 48 512 EP30/SR70 35.70 2.69 47 487 EP10/SR90 27.52 2.45 40 416

*scorch time(ts2), 90% curing time(tc90), maximum torque(MH), minimum torque(ML).�

Figure 1. Rheographs of EPDM/SR blends.�

���

���

���

���

���

���

��

��

Torq

ue(N

�m

)

� �� ���� ���� ���� ��� ���� ���� ���

Time(sec)

0

0

0

0

0

0

0

0

Pure EPDM

EP90/SR10

Pure SR

EP10/SR90

EP30/SR70

EP70/SR30

EP50/SR50

Figure 2. Rheographs of EPDM/SR blends with 5 phr compatibilizer.�

0

0

0

0

0

0

0

0

EP90/SR10/C5

EP70/SR30/C5

EP50/SR50/C5

EP30/SR70/C5

EP10/SR90/C5

Pure EPDM

Pure SR

��

��

��

��

��

��

Torq

ue(N

�m

)

� �� ���� ���� ���� ��� ���� ���� ����

Time(sec)

� � � �

� � � �

� � � �

� � � �

� � � Figure 3. SEM photographs for EPDM/SR blends; (a) EP90/SR10, (b) EP70/SR30, (c) EP50/SR50, (d) EP30/SR70, (e) EP10/SR90, (f) EP90/ SR10/C5, (g) EP70/SR30/C5, (h) EP50/SR50/C5, (i) EP30/SR70/C5, and (j) EP10/SR90/C5.�

Table 3. Curing Characteristics of EPDM/SR Blends with 5 phr of Compatibilizer

ODR (170 �) Sample

MH(N�m) ML(N�m) ts2(sec) tc90(sec) EP90/SR10/C5 60.59 4.62 53 611 EP70/SR30/C5 51.71 3.79 58 599 EP50/SR50/C5 45.89 3.07 49 572 EP30/SR70/C5 36.51 2.86 47 525 EP10/SR90/C5 27.72 2.58 47 493

KRICT SEI 5.0 kV X500 10 µm W D 7.6 mm KRICT SEI 5.0 kV X500 10 µm W D 7.8 mm

KRICT SEI 5.0 kV X500 10 µm W D 7.6 mm KRICT SEI 5.0 kV X500 10 µm W D 7.8 mm

KRICT SEI 5.0 kV X500 10 µm W D 7.5 mm KRICT SEI 5.0 kV X500 10 µm W D 7.8 mm

KRICT SEI 5.0 kV X500 10 µm W D 7.8 mm KRICT SEI 5.0 kV X500 10 µm W D 7.6 mm

KRICT SEI 5.0 kV X500 10 µm W D 8.1 mm KRICT SEI 5.0 kV X500 10 µm W D 7.8 mm

(a) (b)

(c) (d)

(e) (f)

(g) (h)

(i) (j)

Page 4: *Department of Chemistry, Korea University, Seoul 136-701, Korea · 2005-03-29 · Plasticoder (internal mixer) and were vulcanized by a hot press. The morphology of the vulcanized

��� EPDM/��� �� ���� ��� ��� �� 169�

Polymer(Korea), Vol. 29, No. 2, 2005�

�� ����� ���� �� � �� ����. �� ��,

EPDM� 90 wt%� � ����� ��� �� ���� SR� �

�� � 4� 1 µm ��� ��� �� ����. �� �� �

��� ��� ���� ����� ����� MAH-g-EPDM�

EPDM� SR� �� ��� ��� ���� ������ ��

� ���.

3.3 ��� ��

Figure 4� EPDM/SR ���� ��� �� �� ��� ��

���. ����� ���� �� �� ����� ��� �

�� ��� ���� �� ��� ���� ���� ��� �

���, �� ��� ��� ��� EPDM�� �� ����.

��� � ��� ���� �� ��� ����. � ���

��� �� �� ���� ���� � �� ���� ��

� �����, �� � �� ���� ��� ��� ���

��� ��� ����. ��� ��� ���� ��� ��

� ���� ��� ���� ��.13 � ���� ��

� ���� ��� ��� �� �����, �� �� ���

����� �� ����� ����.

����� ��� � �� ��� ��� ��� ���� �

� ��� ���� ��� ��� ���. �� ��� 96�

�� � ��� ��� ��� 50%� �� ��� �� �

��� 50% ���� �� �� �����. �� ��� �

�� ���� �� EPDM� ��� ����� ���� ��

��� ����.

EPDM/SR ���� ����� �� � � �� �� ��

���� �� ��� Figure 5� 6� �����. ����� ��

�� �� � , ��� ��� ��� ���� �� �� ��

����� �����. �� ��� 24��� �� �� ��

�� ������, 48��� 96��� � �� �� �� ��

��. 24�� ��� � ���� �� � ���� ���

� EPDM/SR ���� � �� ���� ��� ����

� �� �� ���� ��� Kole ��7 ��� � ���� �

���. ���, �� ��� ����� � ��� �� �

� ��� ���� �����, �� � ��� �� ��

���� ����� � ����� ���� ��� ����

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Figure 4. Hardness of (a) EPDM/SR blends and (b) EPDM/SR blends with 5 phr of compatibilizer.�

Figure 5. Tensile strength of (a) EPDM/SR blends and (b) EPDM/SR blends with 5 phr of compatibilizer.�

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unaging 24 hr aging 48 hr aging 96 hr aging

Page 5: *Department of Chemistry, Korea University, Seoul 136-701, Korea · 2005-03-29 · Plasticoder (internal mixer) and were vulcanized by a hot press. The morphology of the vulcanized

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Figure 7. Contact angle of (a) EPDM/SR blends and (b) EPDM/SR blends with 5 phr of compatibilizer.�

unaging 24 hr aging 48 hr aging 96 hr aging

unaging 24 hr aging 48 hr aging 96 hr aging

unaging 24 hr aging 48 hr aging 96 hr aging

unaging 24 hr aging 48 hr aging 96 hr aging

Page 6: *Department of Chemistry, Korea University, Seoul 136-701, Korea · 2005-03-29 · Plasticoder (internal mixer) and were vulcanized by a hot press. The morphology of the vulcanized

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Polymer(Korea), Vol. 29, No. 2, 2005�

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