effect of abs grafting degree and compatibilization on the properties of pbt/abs blends

Effect of ABS Grafting Degree and Compatibilizationon the Properties of PBT/ABS Blends

Shulin Sun,1 Zhiyong Tan,1 Chao Zhou,1 Mingyao Zhang,1 Huixuan Zhang1,2

1School of Chemical Engineering, Changchun University of Technology, Changchun 130012,People’s Republic of China

2Changchun Institute of Applied Chemistry, Graduate School, Chinese Academy of Sciences,Changchun 130022, People’s Republic of China

Blends of PBT/ABS and PBT/ABS compatibilized withstyrene-acrylonitrile-glycidyl methacrylate (SAG) co-polymer were prepared by melt blending method.Grafting degree (GD) of ABS influences the morphologyand mechanical properties of PBT/ABS blends. ABScan disperse in PBT matrix uniformly and PBT/ABSblends fracture in ductile mode when ABS graftingdegree is more than 44.8%, otherwise, agglomerationtakes place and PBT/ABS blends fracture in brittle way.On the other hand, the grafting degree of ABS has noobvious influence on the morphology of PBT/ABSblends and PBT/ABS blends fracture in ductile modewhen SAG is incorporated since the compatibilizationeffect. However, PBT/SAG/ABS blends display muchlower impact strength values comparing with PBT/ABSwhen the blends fracture in ductile way. Side reactions inPBT/SAG/ABS blends were analyzed and which were themain reason for the decrease of impact strength of PBTblends. Tensile tests show that the tensile strength andtensile modulus of PBT blends decrease with the increaseof ABS grafting degree due to the higher effective volume.PBT/SAG/ABS blends display much higher tensile proper-ties than PBT/ABS blends since the compatibilizationeffect. POLYM. COMPOS., 28:484–492, 2007. ª 2007 Society ofPlastics Engineers

Keywords: PBT; ABS; SAG; compatibilization; grafting degree

INTRODUCTION

Blends of polybutylene terephthalate (PBT) and acrylo-

nitrile-butadiene-styrene (ABS) materials are of significant

commercial interest [1–3]. PBT is an important engineering

polymer because of its excellent tensile properties, abrasion

and chemical resistance, as well as its uses for electrical

insulation. The unnotched impact strength of PBT is high,

however, PBT is strongly notch sensitive and notched speci-

mens of PBT fail in a brittle manner [4–10]. ABS, which

consists of a butadiene rubber combedded within a matrix

of styrene/acrylonitrile copolymer (SAN), is generally noted

for its excellent toughness, aesthetics, and low cost [11–13].

Thus, there is interest in developing PBT/ABS blends with

goal being to retain the desirable properties of each of the

blend constituents.

The use of ABS for impact modification of PBT has

been reported by a number of investigators [14–20]. With

a proper choice of materials and process conditions blends

with excellent properties can be made without use of any

compatibilizers. Hage et al. [14] studied the effect of ABS

type, extrusion temperature, extrusion type, molding condi-

tion, and PBT type on the notched impact strength of PBT/

ABS blends in detail, and PBT/ABS blends with high

notched impact strength were obtained. However, the use-

ful processing window for these blends is very narrow.

Furthermore, these materials have unstable morphologies

since at low stress or quiescent conditions in the melt state

the ABS domains can grow by coalescence resulting a loss

of mechanical properties. By proper compatibilization one

can able to achieve better properties, a more stable mor-

phology, and a broader processing window.

A few studies on compatibilization of PBT/ABS blends

have been reported recently [15–20]. In PBT blends, epoxy

groups are proved to be more effective on compatibiliza-

tion than other functional groups [21–23]. As for the PBT/

ABS blends, compatibilizers were focused on the epoxy-

functionalized copolymers. Lee et al. [15] explored the use

of a reactive styrene-acrylonitrile-glycidyl methacrylate

(SAG) copolymer as a compatibilizer for PBT/ABS blends.

This SAG copolymer contains reactive epoxy groups that

are able to react with PBT end groups (–COOH or –OH)

under melt condition to form PBT-co-SAG copolymer.

However, no significant improvement of toughness was

achieved in their study may be due to the properties of

ABS they used. Hale et al. [16–20] used methyl methacry-

late-glycidyl methacrylate-ethyl acrylate (MGE) copoly-

Correspondence to: Huixuan Zhang; e-mail: [email protected]

DOI 10.1002/pc.20318

Published online in Wiley InterScience (www.interscience.wiley.com).

VVC 2007 Society of Plastics Engineers

POLYMER COMPOSITES—-2007

mer as compatibilizer for PBT/ABS blends. MGE has been

shown to be effective reactive compatibilizer for blends of

PBT with SAN or ABS as revealed by improvements in

SAN or ABS dispersion, morphological stability, and low

temperature toughness. In the previous paper, epoxy-func-

tionalized ABS was prepared in our lab and was used to

toughen PBT and PBT with super-tough properties was

obtained [24].

In this paper, ABS copolymers with different grafting

degree were prepared by emulsion polymerization method.

These ABS copolymers were used to toughen PBT and SAG

was used as compatibilizer. The effect of ABS grafting de-

gree and compatibilization on properties of PBT/ABS blends

was studied in detail. Since ABS itself is a two-phase mate-

rial, a portion of this work will focus on the simpler PBT/

SAG/SAN system for the compatibilization study.

EXPERIMENTAL

Materials

PBT was purchased from Engineering Plastics Plant of

YIHUA Group Corp. The hydroxyl and carboxyl end-

group concentrations are 44 and 20 meq/g, respectively.SAN resin was supplied by Jilin Chemical, China. Mn of

SAN is 32,000 and Mw is 74,000. The analysis was

calibrated with polystyrene standards. The acrylonitrile

(AN) content in SAN is 25 wt%. Copolymer of SAG was

synthesized by suspension polymerization method in our

lab with 5 wt% GMA and 25 wt% AN contents. ABS

copolymers were prepared by emulsion polymerization

method with changing chain transfer agent content. Tert-dodecyl mercaptan (TDDM) was used as chain transfer

agent and the properties of ABS copolymers were list in

Table 1.

Preparation of ABS Copolymers

In the preparation process a polybutadiene (PB) polymer

has to be synthesized first and then AN and St were poly-

merized on PB particles. PB latex used in this study was

supplied by JILIN Chemical Industry Group synthetic resin

factory. An oil-soluble initiator, cumene hydro-peroxide

(CHP), was used in combination with a redox system. The

redox initiator system, CHP, sodium pyrophosphate (SPP),

dextrose (DX), and iron (II) sulfate (FeSO4) was used with-

out further purification. The emulsion polymerization was

performed in a 2 L glass reactor under nitrogen at 638C.First, the water, PB, initiator and KOH were added to the

glass reactor and stirred 5 min under nitrogen, then the

mixture of St/AN and chain transfer agent, TDDM, were

added in a continuous feeding way to the glass reactor. The

polymers were isolated from the emulsion by coagulation

and dried in a vacuum oven at 608C for 24 h before being

used.

The grafting degree was determined by extracting the

ungrafted or free SAN resin by acetone (a solvent for SAN

but not for PB). After the acetone solutions of the dried

ABS impact modifiers were shaken for 8 h at room temper-

ature, the solutions were centrifuged at 15,000 rpm in a

GL-21M ultracentriguge for 30 min. The grafting degree

was calculated from the following equation:

Grafting degree ð%Þ ¼ 100� gel%� PB%

PB%

where gel% is the weight fraction of the acetone insoluble

part in the sample and PB% is the weight fraction of poly-

butadiene in the ABS sample.

Melt Blending and Molding Properties

The blends of PBT/SAG/SAN were carried out in a

Thermo-Haake mixer. The rotating speed was set at 50 rpm

and the temperature was set at 2408C. Then PBT blends

were compression-molded into plates of 1 mm thickness at

2408C for mechanical test.

Blends of PBT/ABS and PBT/SAG/ABS were carried

out in a twin-screw extruder, the temperature along the ex-

truder were 210, 220, 230, 230, 230, 230, 2308C and the

rotation speed was 60 rpm. The rods of blends were cooled

in a water bath and then pelletized. The PBT blends were

dried in a vaccum oven at 808C for 24 h then injection

molding was carried out to prepare Izod impact and tensile

specimens.

TABLE 1. Characteristics of ABS copolymers with different TDDM contents.

Designation

used here

Rubber content

(wt%)

Ratio of AN/St

(wt/wt)

CHP content

(ml)

TDDM content

(ml)

Grafting degree

(%)

ABS particle sizea

(mm)

ABS-T0 60 25/75 0.6 0 55.0 0.359

ABS-T0.2 60 25/75 0.6 0.2 51.1 0.344

ABS-T0.8 60 25/75 0.6 0.8 44.8 0.348

ABS-T1.2 60 25/75 0.6 1.2 41.5 0.365

ABS-T1.6 60 25/75 0.6 1.6 38.3 0.354

a Particle size was measured with a Brookhaven 90 Plus Laser Particle analyzer.

DOI 10.1002/pc POLYMER COMPOSITES—-2007 485

Rheological Properties

The rheological measurements were performed on a

Thermo-Haake mixer. The rotating speed was set at 50 rpm,

and the temperature was set at 230–2408C.

Morphological Properties

The disperse morphology of SAN and ABS in PBT ma-

trix was characterized by scanning electron microscopy

(SEM) (model Japan-5600). The sample surface was cut at

low temperature with a glass knife until a small and flat

surface was obtained. The samples were etched and coated

with a gold layer for SEM observation.

Mechanical Properties

Notched Izod impact tests of PBT blends were per-

formed at 23 6 28C according to ASTM D 256 on a XJU-

22 apparatus. The samples with dimensions 63.5 � 12.7 �6.35 mm3 were obtained from injection molded specimens.

The notch was milled in having a depth of 2.54 mm, an

FIG. 1. Morphology of PBT/SAG/SAN (80/x/20-x) blends with different SAG contents: (a) SAG ¼ 0%; (b)

SAG ¼ 1%; (c) SAG ¼ 3%; (d) SAG ¼ 5%; (e) SAG ¼ 10%; (f) SAG ¼ 20%.

486 POLYMER COMPOSITES—-2007 DOI 10.1002/pc

angle of 458 and a notch radius of 0.25 mm. The uniaxial

tensile tests were carried out at 23 6 28C on an AGS-H

tensile tester at a cross-head speed of 50 mm/min accord-

ing to the ASTM D 638. For both mechanical tests at least

five samples were tested and their results averaged.

RESULTS AND DISCUSSION

Effect of SAG on PBT/SAN Morphology

The effect of reactive compatibilization on the morphol-

ogy of PBT/SAN blends, a simplified model for the PBT/

ABS system, is described here. Figure 1 shows the change

in morphology within a series of blends (80 wt% PBT) as

the SAN/SAG ratio is varied. In these blends, the disperse

phase was etched out by acetone at room temperature for

5 h. As can be seen from Fig. 1, the large and spherical SAN

particles with different dimensions (0.5–2 mm) can be easily

identified from the non-compatibilized blend of Fig. 1a.

Compared with the non-compatibilized blend, the domain

size of SAN particles decreases with the increase of SAG

content in the PBT/SAG/SAN blends, and the interface

between PBT and SAN phase becomes obscure, especially

for the PBT/SAG blend (Fig. 1f). Figure 2 shows the number

average particle diameters for this blend series plotted as a

function of SAG content. The disperse phase particles size is

significantly reduced with the increase of SAG content.

Since the SAG copolymer used here are fully miscible with

the SAN phase, one may expect it reside in the SAN phase

while the epoxy groups form chemical linkages with the

PBT chain ends at the domain interfaces. This would be ex-

pected to reduce the SAN domain size to some degree by a

reduction of interfacial tension and to a greater degree by

steric stabilization of the SAN particles against coalescence.

Effect of SAG on PBT/SAN Rheological andMechanical Properties

Rheological measurements are often used to analyze the

occurrence of chemical reactions in reactive blending sys-

tem. A chemical reaction that takes place between the re-

active blend components will lead to an increase of the

blend torque compared to a mixture without any reactions.

Figure 3 illustrates the evolution of the torque and temper-

ature as a function of SAG content for PBT/SAG/SAN

blends having an overall dispersed phase concentration of

20 wt%. Increasing the SAG content results in continuous

increase of the torque and temperature values, which is

consistent with the chemical reactions between PBT and

SAG during melt blending. The increase of temperature is

partly due to viscous heating of highly viscous copolymers

and partly due to the exothermic heat of the reactions.

Figure 4 displays the effect of SAG content on tensile

strength and elongation at break of PBT/SAN blends (80

wt% PBT). The tensile strength and elongation at break

increase continuously with the increase of SAG content.

As we know, the tensile properties are sensitive to the

FIG. 2. Dispersed phase domain size of ternary PBT/SAG/SAN blends

as a function of SAG content.

FIG. 3. Effect of SAG content on torque and temperature of PBT/SAG/

SAN (80/x/20-x) blends prepared in Thermo-haake. Torque and tempera-

ture readings were taken after 10 min at 2408C and 50 r/min.

FIG. 4. Effect of SAG content on tensile strength and elongation at

break of PBT/SAG/SAN (80/x/20-x) blends prepared in Thermo-haake.


property of the interface, that is, interfacial adhesion. In this

study, the interface between PBT and SAN is modified by

reaction between PBT and SAG. The formation of PBT-co-SAN copolymer at the interface increases the interfacial ad-

hesion strength, so the PBT/SAG/SAN blends have higher

tensile strength and elongation at break than PBT/SAN

blends. The disperse phase morphology, rheological, and

mechanical properties of PBT/SAG/SAN blends testified

the compatibilization effect of SAG copolymer.

Morphology of PBT/ABS and PBT/SAG/ABS Blends

In this part, morphology of PBT/ABS and PBT/SAG/

ABS blends was studied by SEM observation. The differ-

ence between these ABS copolymers lies in their grafting

degree. Table 1 displays the influence of TDDM content on

the grafting degree of ABS. As the amount of TDDM in-

creases, the grafting degree of ABS copolymers decreases. The

increase of TDDM content in the reactive system improves

FIG. 5. Morphology of PBT/ABS and PBT/SAG/ABS blends with different ABS grafting degree: (a) PBT/

ABS (GD ¼ 55%); (b) PBT/SAG/ABS (GD ¼ 55%); (c) PBT/ABS (GD ¼ 44.8%); (d) PBT/SAG/ABS (GD ¼44.8%); (e) PBT/ABS (GD ¼ 41.5%); (f) PBT/SAG/ABS(GD ¼ 41.5).


the probability of chain propagation free radicals transfer-

ring to TDDM and increases the number of free SAN radi-

cals, which induces the decrease of ABS grafting degree. In

the previous study [25], it was pointed out that TDDM

could not change the number of grafting sites during emul-

sion polymerization process. So the decrease of grafting

degree will result in the decrease of molecular weight and

graft chain length of grafted SAN chains.

Figure 5 displays the effect of ABS grafting degree and

compatibilization of SAG on the morphology of PBT/ABS

blends. As for the PBT/ABS blends, ABS can disperse in

PBT matrix uniformly when ABS has higher grafting degree,

such as Fig. 5(a), however, with the decrease of grafting de-

gree, we can find agglomeration of ABS in PBT matrix takes

place, such as Fig. 5(c) and 5(e). Two reasons may induce

the formation of agglomeration structure of ABS phase. First,

for ABS with low grafting degree, the surface of the rubber

particles cannot be covered perfectly with grafted SAN

copolymers. Then agglomeration of the rubber particles

should be caused as the particles do not form a stable colloid;

second, the molecular weight of SAN chains on PB particles

decreases with the decrease of grafting degree, so ABS

copolymers with lower grafting degree have much shorter

grafting chain length. The shorter grafting chain length indu-

ces low entanglement density between the SAN chain and

PBT matrix then the interfacial adhesion strength between

PBT and ABS will become poor, which is not beneficial to

the dispersion of ABS in PBT matrix.

However, for PBT/SAG/ABS blends, the effect of ABS

grafting degree on morphology of PBT blends is not obvi-

ously. ABS can disperse in PBT matrix uniformly whatever

the ABS grafting degree, such as Fig. 5 (b), 5(d), and 5(f).

So we can conclude that the compatibilization effect of

SAG suppresses the influence of ABS grafting degree. The

compatibilization effect can reduce the interfacial tension

and suppress coalescence of the ABS particles by steric sta-

bilization to a greater degree.

Mechanical Properties of PBT/ABS andPBT/SAG/ABS Blends

The effect of ABS grafting degree and compatibilization

of SAG on the impact strength of PBT/ABS blends can be

seen from Fig. 6. PBT/ABS blends fracture in ductile mode

when ABS grafting degree is higher than 44.8%, otherwise,

PBT/ABS blends fracture in brittle mode. The impact prop-

erty of PBT/ABS blends is consistent with the morphologi-

cal properties. Different with PBT/ABS blends, PBT/SAG/

ABS blends fracture in ductile mode whatever the ABS

grafting degree, and grafting degree has no obvious effect

on impact strength. On the other hand, PBT/SAG/ABS blends

display much lower impact strength than PBT/ABS blends

in the ductile region. Side reactions in PBT/SAG/ABS

blends were analyzed in the following part and that were

FIG. 6. Effect of ABS grafting degree on Izod impact strength of PBT/

ABS and PBT/SAG/ABS blends.

FIG. 7. Effect of ABS grafting degree on tensile strength of PBT/ABS

and PBT/SAG/ABS blends.

FIG. 8. Effect of ABS grafting degree on tensile modulus of PBT/ABS

and PBT/SAG/ABS blends.


the main reasons for the decrease of impact strength of PBT

blends.

Figures 7 and 8 display the effect of ABS grafting

degree and compatibilization of SAG on tensile strength

and tensile modulus of PBT/ABS blends. The tensile

strength of PBT/ABS and PBT/SAG/ABS blends decreases

with the increase of ABS grafting degree. ABS copolymer

is a special core-shell copolymer. The shell is SAN copoly-

mer grafted onto the surface of the polybutadiene (PB) par-

ticles; this is called external grafting. Because of the swel-

ling of the monomer to the rubber particles, the grafting

polymerization can take place inside rubber particles, and

there exist some occlusions of SAN copolymers in the core

of PB; this is called internal grafting. In this paper, the

external and internal grafting of ABS will increase with

the increase of ABS grafting degree and which improves

the effective volume of the rubber particles. So according

to the Ishai-Cohen model [26], the tensile yield stress,

syt(F) of a composite containing a volume fraction, F, oflow modulus inclusions can be expressed as follows:

sytðFÞ ¼ sytð0Þð1� 1:21F2=3Þ

where syt (0) is the yield stress of the matrix. Applying this

model to PBT blends system, we can see that the increased

grafting degree increases the effective volume fraction of

PB particles and leads to the decrease of tensile yielding

strength of PBT/ABS and PBT/SAG/ABS blends. On the

other hand, PBT/SAG/ABS blends display much higher ten-

sile strength than PBT/ABS when ABS has the same graft-

ing degree due to the compatibilization effect of SAG.

Figure 8 displays the effect of ABS grafting degree and

compatibilization of SAG on tensile modulus of PBT/ABS

blends and similar change can be observed as Fig. 7.

SCHEME 1. Chemical reactions in PBT/SAG/ABS blends.


The tensile modulus decreases with the increase of grafting

degree due to the increase of effective volume of PB par-

ticles and PBT/SAG/ABS blends display much higher ten-

sile modulus than PBT/ABS blends.

Chemical Reactions in PBT/SAG/ABS Blends

In PBT/SAG/ABS blends, compatibilization reactions

and side reactions can take place simultaneously. The reac-

tive equations are listed in scheme 1. Reactions 1 and 2

belong to compatibilization reactions that involve epoxy

groups of SAG and carboxyl and hydroxyl end groups of

PBT. The reactions between epoxy groups and carboxyl

and hydroxyl groups have been used in many studies [27–

31]. Reaction 1and 2 postulate the formation of PBT-co-SAN copolymers at the blend interface. PBT-co-SAN co-

polymer, acting as compatibilizer, can increase interfacial

strengths and are believed to promote mixing in two ways.

First, disperse phase coalescence rate is reduced through

steric repulsion; second, disperse phase breakup rate is

increased since lower interfacial tension. These factors

result in a finer distribution of the disperse phase and

response for the better morphology and mechanical proper-

ties of PBT/SAG/ABS blends.

Reactions 3, 4 and 5 belong to side reactions that are

not beneficial to the improvement of PBT/SAG/ABS

blends properties. The reaction 3 involves the secondary

hydroxyl groups present on the copolymers of PBT-co-SAN (in reaction 1 and 2) formed at the interface. Reaction

4 is based on the bifunctionality of the PBT matrix, as each

PBT contains two functional groups that can react with the

epoxy groups. In contrast with reaction 3, this side reaction

occurs mainly at the interface. Similar reactions have been

proved in some papers [9, 24]. Reaction 5 takes place

between the epoxy groups of SAG and the hydroxyl groups

of ABS copolymer. The hydroxyl groups come from the

preparation progress of ABS. During the preparation of

ABS, the chemical reaction between iron (II) sulfate

(FeSO4) and cumene hydro-peroxide (CHP) takes place as

follows:

ROOHþ Fe2þ ! OH� þ RO� þ Fe3þ

The free radicals of hydroxyl can participate the chain ter-

mination progress so some hydroxyl groups will exist in

ABS copolymers and inducing the side reactions with SAG

in PBT/SAG/ABS blends. The relationship between the

torque value and time of ABS/SAG blends can be seen

from Fig. 9. SAG and ABS have the similar melt viscosity,

however, ABS/SAG blend displays much higher torque

value than the individual composites, which testifies the

chemical reactions between ABS and SAG. So in PBT/

SAG/ABS blends, compatibilization reactions are bene-

ficial to the improvement of blends properties, however,

the side reactions induce the decrease of PBT blends

toughness.

CONCLUSION

SAG copolymer is miscible with SAN and can react

with the carboxyl and/or hydroxyl groups of PBT. So SAG

can be used as compatibilizer of PBT/SAN or PBT/ABS

blends and the compatibilization effect has been testified

by morphology, rheological, and mechanical investigation.

The grafting degree of ABS influences the morphology of

PBT/ABS blends. ABS can disperse in PBT matrix uni-

formly when ABS grafting degree is higher than 44.8%,

otherwise, agglomeration takes place due to the lower graft-

ing degree. As for the compatibilized PBT/ABS blends, the

effect of ABS grafting degree on the dispersion of ABS is

suppressed with the addition of SAG and the ABS with dif-

ferent grafting degree can disperse in PBT matrix uniformly.

PBT/ABS blends have higher impact strength when ABS

grafting degree is higher than 44.8%, otherwise, PBT/ABS

blends display much lower impact toughness and fracture in

brittle mode. With the addition of SAG, PBT/ABS blends

fracture in ductile way whatever the ABS grafting degree.

However, compared to PBT/ABS blends, PBT/SAG/ABS

blends display much lower impact strength when all these

blends fracture in ductile mode since the side reactions in

PBT/SAG/ABS blends. Tensile tests show that the tensile

strength and tensile modulus of PBT blends decrease with

the increase of ABS grafting degree due to the higher effec-

tive volume. On the other hand, PBT/SAG/ABS blends dis-

play much higher tensile strength and tensile modulus than

PBT/ABS blends since the compatibilization effect.

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effect of abs grafting degree and compatibilization on the properties of pbt/abs blends

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