8
Polymer (Korea), Vol. 28, No. 5, pp 404-411 (2004) / , \28Ì \5x, 2004, pp 404-411 "Ý Ü0\Ô 0Ìp ¬ô q @ ÄÐ ì Ü0q À,, \¼ æÔ 0Ì @¼ <Ô |\ ìéXô È$. 1 ùÈ, ý A¸ ¸ Ü0\Ô @q, Ü0 è< qå< ì\ MjY_=ùñ&ÙõAmÕ -ñéÙÑq~$®mé ®:¯ñ}~ . ¯Ê> .. ¯½ .% 0x@# ظ<p`Q<U/# 0x@# 5</# \¼è# @8,0¬Ì# +5336#;#8¼# QX/#5337#<#<¼# ,# Thermal Properties and Microencapsulation of a Phosphate Flame Retardant with a Epoxy Resin Kyung-Hyun Baek, Jun-Young Lee*, Sang-Hyun Hong**, and Jung-Hyun Kim* % Graduate Program in Nano Science and Technology, Yonsei University, 134 shinchon-dong, seodaemun-ku, Seoul 120-749, Korea *Department of Chemical Engineering, Yonsei University, 134 shinchon-dong, seodaemun-ku, Seoul 120-749, Korea **Samsung Cheil Industries Chemical R&D Center, 332-2, Gocheon-dong, Uiwang-si, Gyeonggi-do 437-010, Korea e-mail : [email protected] (Received August 5, 2003;accepted September 9, 2004) 5¨¹¸ Ü0\¸ øìØ ,äØ´ø (TPP) 4A, pA q´ ðX dø¬ ¬°¼ Uq Ô ¸6½ U - X¼ ´é, ´¬áÐ @$. `éq ¸ Ü0\¸ TPPÔ ÄÐ Ü 5U @5 ÄÐ X\ p O iÜ ¸, Ü0\ Ð$< ÄÐ 5©ì Vq x \$ ¼pè$. ´¼ ´ðp D´ TPP¼ ´¬áÐ@$. É, 8 5U áÐ ,|¸ TPP ý |¸ ¸6½ U - H |©\ `\ ¨ XQ`U (O/W) -` ä \ `¡ ¸D Q©Õ| @X É@$. |©\ `\ Th< Ñ 8ì TPP ¨ p¸ $ É@|° ´¬áÐ Uq O 4A ùq ¸ D´ DSC TGA ´ Ä]@$. P áÐ ÅÐ UA p D´ SEM< TEM ´é, áÐ ¬p O è4 1 Ä]@$. |©\ `\ TL F127< ÌT °$ä` d,d´ø (SDBS)@ 1¹1 ¼ , 8ì `\ Å´ Ý@ X áÐ ÅÐ@ ¬U´° À ¼ ÅÐ U¼ 4@$. ,-897,.9¹The microcapsules containing triphenyl phosphate (TPP), a flame retardant, were prepared by phase- inversion emulsification technique using the epoxy resin (Novolac type) with excellent physical properties and network structure. This microencapsulation process was adopted for the protection of TPP evaporation and wetting of polymer composite during the polymer blend processing. The TPP, epoxy resin and mixed surfactants were emulsified to oil in water (O/W) by the phase inversion technology and then conducted on the crosslinking of epoxy resin by in-situ polymerization. The capsule size and size distribution of TPP capsules was controlled by mixed surfactant ratio, concentration and TPP contents. The formation and thermal property of TPP capsules were measured by differential scanning calorimetry and thermogravimetric analysis. The morphology and size of TPP capsules were also investigated by scanning and transmission electron microscopies. As the surfactant concentration increased, the TPP capsules were more spherical and mono-dispersed at the same weight ratio of mixed surfactants (F127 : SDBS). Keywords¹microcapsule, phosphate flame retardant, in-situ polymerization.

Thermal Properties and Microencapsulation of a … · 150 3000 4500 cps . propyl-ene oxide ethylene oxide Pluronic F127 (BASF, Germany) ... 12000 rpm 5 . 80 500 rpm 2 . (methyl al-

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Thermal Properties and Microencapsulation of a Phosphate Flame Retardant with a Epoxy Resin

Kyung-Hyun Baek, Jun-Young Lee*, Sang-Hyun Hong**, and Jung-Hyun Kim*� Graduate Program in Nano Science and Technology, Yonsei University,

134 shinchon-dong, seodaemun-ku, Seoul 120-749, Korea *Department of Chemical Engineering, Yonsei University, 134 shinchon-dong, seodaemun-ku, Seoul 120-749, Korea

**Samsung Cheil Industries Chemical R&D Center, 332-2, Gocheon-dong, Uiwang-si, Gyeonggi-do 437-010, Korea

†e-mail : [email protected]

(Received August 5, 2003;accepted September 9, 2004)

����� ���� ���� ���� (TPP)� ��, ��� �� ���� ��� ��� ���

� ��� �� ��� ��� ��� ������ ����. ��� �� ���� TPP� ��� �� �� �� � ��� ���� �� � ��� ��� ���� ��� ��� ���� ��� ���� �����. � ���� � TPP� ��������. �, � ��� ��� ���� TPP� �� ��� ��� �� ��� ��� ��� ���� �� ���� (O/W) ��� ����

�� ��� ���� ��� ����� ����� ����. ��� ���� ��� � ��� TPP ��� �� �� ����� ������ �� � �� ��� ��� � DSC� TGA� �� ����. �� �� ��� ���� ��� � SEM� TEM� ��� ��� �� � ���� �� ����. ��� ���� �� ��� F127� ��� ����� ��� (SDBS)� 1�1 ��, ��� ���� ��� ���� ��� ��� ��� � ��� �� ��� ��. ���������The microcapsules containing triphenyl phosphate (TPP), a flame retardant, were prepared by phase-inversion emulsification technique using the epoxy resin (Novolac type) with excellent physical properties and network structure. This microencapsulation process was adopted for the protection of TPP evaporation and wetting of polymer composite during the polymer blend processing. The TPP, epoxy resin and mixed surfactants were emulsified to oil in water (O/W) by the phase inversion technology and then conducted on the crosslinking of epoxy resin by in-situ polymerization. The capsule size and size distribution of TPP capsules was controlled by mixed surfactant ratio, concentration and TPP contents. The formation and thermal property of TPP capsules were measured by differential scanning calorimetry and thermogravimetric analysis. The morphology and size of TPP capsules were also investigated by scanning and transmission electron microscopies. As the surfactant concentration increased, the TPP capsules were more spherical and mono-dispersed at the same weight ratio of mixed surfactants (F127 : SDBS). Keywords�microcapsule, phosphate flame retardant, in-situ polymerization.

Polymer (Korea), Vol. 28, No. 5, 2004� Microencapsulation of a Phosphate Flame Retardant � �����

���, �28� �5�, 2004� �� ���� ������ � � ����

� ��� �� ��� � �� � ���� �

��� �� ���.2 ��� �� ���� ��� �

�� ���� � 200 � �� �� ��� ��� �

��� �� ��� ����� � �� ���� �

�� � ��� ���� ��� ��� ��� ���

���� ��. �� ��� ������ ����

�� ��� ���� � ���� ��� �� ��

� ����� �� ���� ���� ��� ����

�� ���� ������ ��� �� ��. �

� �� �� ���� �� �� ��� ��� �

��������� �� � ��� �, ����

��� ���� �� ������ �� � ��� �

�� ���� �� � ��� ��� �� ��� �

� ���� ���� ���� ��� ��� ��

� ����� ���� �� ����� ���� ��

� �� � ��.3-5

��� � ����� ��� ����� ����

�� ���� ���� ����� �� ��� ��

� � ��� ��� ��� ��� �� ���

�� ������ � � ����� ����� �

�. ������ ����� �� ���,6,7 ��

���,8 �����9-15 �� � ���, �� ���

������� ��� ��� ���� ��� �

�� ����� in-situ ����� �����.16-22

��� ���� ���� ��� ��� ���

�� � ���� ��� ��� ��� � � �

��.17,18 � ��� ��� ���� �� �� ��

� ���� ��� ���� ��� ���� �

��� ����. ��� ���� ��� �� ��

��� ��� ���� ����� ��� �� �

� surface activity, spreading, forming �� ����� �

� � ��.23-26 ��, in-situ ���� �� �� � �

��� ���� ���� ���� ���� ���

��� �� �� � �� ��� ��� ��.23,24

��� � ����� ���� in-situ �� ��

�� ���� ���� ��� ���� ��� �

��� ��� �� �� �� ��� ��� �� � �

���� �� � ��� ��� �� ��� ���

�. �� �� ���� ��� �� ��� ��� �

� � ��� �� � ����� ����.

�������

��� ������ �� ��� ���� ��� �

�� ��� 85�95 �� ��� ��� ��� YDCN-

500-90P (Kukdo Chem., Korea)�, ������ ���

47�49 �� �� ���� triphenyl phosphate (TPP)�

����(�)�� � ����. ��, YDCN-500-90 P

� ���� ��� ���� 150 ��� 3000�4500 cps

��� ��� ��. ���� ���� ��� propyl-

ene oxide � ethylene oxide� �� ���� ��� �

�� ���� Pluronic F127 (BASF, Germany)� ��

�� paste ��� ��� ���� sodium dodecyl-

benzene sulfonate (SDBS, Junsei co., Japan)� ���� �

���. ��� Pluronic F127� SDBS� HLB ��

�� 22� 40��� ��� �� ���� ����.

���� ��� ���� 2-piperazinoethylamine (AEP,

Sigma-Aldrich Co., U.S.A.)� �� � ����. ��

� ��� ��� ���� ����� � D.D.I. wa-

ter� ����.

������ ���� in-situ ���� �� �� �

��� ����� �� ��� ��� �. ���

�� (YDCN-500-90P), �� ��� (TPP), ��� (F127,

SDBS)� 1� �� 120 �� ���� �� �� �

��. �� ��� 70�80 �� �� � ��� AEP�

��� ���� 10 wt%� ���� �����. � �

���� ����� � 50 � �� D.D.I. water

� ��� �� 25%� ��� ��� � ����

(Omni, U.S.A)�� 12000 rpm� ���� 5� ��

�����. ��� ��� ��� ��� ��� �

�� ��� ��� � ���� 80 ��� 500 rpm�

���� 2� �� ���� ��� ��� ���

��. ��� �� ��� ��� ���� (methyl al-

cohol)� ��� 3�� �� ���� � 60 �� �

��� �� �����.

������ ���� ��� ��� Pluronic F127

� ��� ���� SDBS� ���� ����. �

�� ���� ���� ��� ��� (steric stabili-

zation)� ���� ��� ���� �� ���� �

�� (electrostatic stabilization)� ����.23,24 � ��

��� ���� ��� ���� ���� �����

�������� ����� ���� ����� �

���� �� ��� ��� � ��.25 ��� ��

� � ���� ���� �� ��� ���� ��

� �� ��� ���� � �� ��� ����

��� �� ����.

��, ���� �� ���� ��� ���� �

� ���� ��� �� ��� ��� ���� �

��� ��� ����. � �� ���� ����

�� ������ ��, ���� � ����� �

���� � �Baek et al. Polymer (Korea), Vol. 28, No. 5, 2004�

���� � ������� ���, �28� �5�, 2004��

� ����. Table 1� �� ��� (TPP)� ��

��� �� ��� � �� � ��� �����.

��� �� ��� ��� ���, ��� ��, ���

� �� �� ��� ���� �� 100 mL/min

�� ��� � ��� �� ��� �� ��� ��

�� ��� (DSC, TA Instrument 2920, U.S.A.)� ���

��� (TGA, TA Instrument 2050, U.S.A.)� ���

10 �/min� �� �� ���� �� ��� ��

�� ��� � ���� ��� (SEM, Hitachi s-4200,

Japan)� ���� ��� (TEM, JEOL JEM-2000 EXII,

Japan)� ���� ������ ���� � ��

�� ����. �� TEM ��� TPP �����

��� diglycidyl ether bisphenol A (DGEBA) ��� �

�� ��� �� � ���� � ����� ���

�� TPP ������ ��� ����.

������������

����������� ��� ��� ��� ��

� ��� � ��� ��� ������ �� ��

� ����� ����� � ��. � ����� �

� ���� ���� ������ �� � ��

�� �����, Figure 1� �� ��� (TPP)�

������� �� ���� ���� ��. Figure

1� ��� � ��� ���� ��, � �

� (phase-inversion point) �� �� ���� ���

� ��� �� ���� ��� �� ��� ��

� ���� ��� ���� � ��� ���� �

�. � � �� �� ��� ����� ��� �

� ���� �����,21 � ���� ���� ��

���� �� � ��� �� ����� ���

���� ��� ��� �� ����, ��� �

� ���� ����� ��� ���� ��. �

� ��� � ���� �� ���� ���� ��

��� ���� �� ���� �� �� ��� �

��� �� �� ��� ��� � ����

�� ���� �� � � ��.17 ���� ��� �

� ��� ��� ��� ��� �� ��� (TPP) ��

� ����� AEP� �� ��� �����, �� �

� in-situ ���� ���� �� ��� ��� �

�� ��� ���� �� �� ���� �� ��

� ���� ��� ���� ��� ���� ���

� �� ��. �� ��, ��� �� ��� �

��� ��� ��� ����� ����.

������������������� ��� ���

��� ���� in-situ ����� ��� TPP �

� ���� ������ DSC� TGA, ��� TEM�

�� �� ��� ��� ����. Figure 2(a)� �

�� ���� �� (F127�SDBS)� �� �� 1�1

� 12 wt%� �� ����� TPP ����� (��

B-2)� �� ��� �� ��� �� � �� ��

���� ��� ����� � � �� DSC �� �

��� ��. Figure 2(a)�� ��� ��� �����

���� � ���� TPP ������ � 50 �

���� ���� ���� ��. �� 47�49 ��

���� �� TPP� ��� ������� ��

� ���� ���� ��� TPP ������ �

�� ����� ����� ���� � � ��.

�� ��� ���� �� (F127�SDBS) 1�1�

20 wt% ���� ��� �� ����� �����

(�� B-4)� �� ��� �� ��� ����� ��

� TGA �� Figure 2(b)� �����. ��� TPP�

190�300 � ���� 100 wt% ����� ���

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

sam ple T P P

conten tsa (w t% ) F 127 : S D B S

m ixed surfactan t con ten tsa (w t% )

capsu le form ation

capsu le size (µm )

A -1 1 : 0 � - A -2 1 : 2 � - A -3 1 : 1 � 17�20 A -4 2 : 1 � - A -5

33

0 : 1

10

� - B -1 5 � - B -2 12 � 14�19 B -3 15 � 12�15 B -4

33 1 : 1

20 � 3�7 C -1 25 � - C -2 40

1 : 1 12 � 12�17

a based on the TPP+epoxy resin.

������� �� Schematic diagram of phosphate flame retardant microencapsulation via phase inversion and in-situ crosslinking reaction.�

Water

Epoxy resin + TPP+ Curing agent

Water added

Phase inversion

Water

Dispersed Epoxy mixtures

In-situ crosslinking

reaction Microcapsulatedparticles

Water

Epoxy resin + TPP+ Curing agent

Water added

Phase inversion

Water

Dispersed Epoxy mixtures

In-situ crosslinking

reaction Microcapsulatedparticles

Water

Epoxy resin + TPP+ Curing agent

Water added

Phase inversion

Water

Dispersed Epoxy mixtures

In-situ crosslinking

reaction Microcapsulatedparticles

Water

Epoxy resin + TPP+ Curing agent

Water added

Phase inversion

Water

Dispersed Epoxy mixtures

In-situ crosslinking

reaction Microcapsulatedparticles

Polymer (Korea), Vol. 28, No. 5, 2004� Microencapsulation of a Phosphate Flame Retardant � �����

���, �28� �5�, 2004� �� ���� ������ � � ����

�, ��� ��� ���� 330�470 � ��� 80

wt% �� ����� ����. � ���� TPP

����� (�� B-4)� ���� TPP� ���

320 � ���� 1��� ����� �����, ��

� ��� ��� ���� � 380 � ���� 2��

� ����� ���� � � ��. �� ��� TPP

� ���� �� (285 �)� ���� ������

� �� TPP� ���� ��� 285 ��� 324 ��

�� ����� � � ��. � � TPP ���

��� ��� ��� ��� �� ���� ����

�� ��� (TPP)� �� ������ ��� ��

� ��. �, �� � ��� ���� �� ��� TPP

� �� ��� ���� � � ��. ��� �� TPP

������ ��� ���� ����� 200 �

�� �� ��� � � �� ���� �� � ���

�� ���� �� � ����� ���� � ��

�� ����.

TPP ������ �� ��� � � ���� �

��� TEM� ���. �� ��� ����� �

� (B-2)� �� ��� DGEBA ��� �� ��� �

�� �� � ���� ���� ������ ��

TEM ��� ��� ����. Figure 3� ��� �

�� �� � TEM� �� ��� �� B-2� ���

���� ��. ������ ��� � 15 µm ��

� �� �� � �� ���� TPP� ����

��� ���� ��� �� � ��. � ���

��� �� ��� � in-situ ���� �� ��

��� ����� ����.

�������������� ��� ��� ��� TPP

�� ���� ������� ��� ���� �

�� ���� ���� ��� ��� (F127)� ��

�� ���� ���� ��� ��� (SDBS)� �

��� ����. ���� � �� �� TPP �

����� ��, �� � ����� ��� �� SEM

��� �� � � ���. Figure 4� ��� ����

�� �� (a�e, F127 : SDBS = 1:0, 1:2, 1:1, 2:1, 0:1)� �

� ��� TPP ����� ��� SEM ���. �

��� � ��� ��� (F127)� ��� ��

� (SDBS)� �� ��� �� ��� ����� �

� (Figure 4(c), A-3)� 17�20 µm ��� �� ���

���� � � ���. ��� ��� (F127)� ��

� ��� (SDBS)� �� ���� ��� �� (Figure

4(a), A-1)� (Figure 4(e), A-5)� ���, ���� �

�, ��� ���� �� (F127�SDBS) 1:2� ��

(Figure 4(b), A-2)� 2:1� (Figure 4(d), A-4)� �� ��

���� ��� �� ��� ��� �� ��� �

�� �� ����� �����. � ���

���� ��� ��� ���� ���� ���� ���

Temperature (�)

(a)

���

���

���

����

����

����

���

����

���

Hea

t flo

w (

W/g

)

� �� ���� ��� ���

Temperature (�)

(b)

����

���

��

��

���

��

����

���

Wei

ght (

%)

���

����

����

����

���

���

����

����

Der

ivat

ion

Wei

ght (

%/ �

)

������� �� Thermal properties of epoxy microcapsules inclu-ding phosphate flame retardant; (a) DSC curves and (b) TGA curves.�

������� �� TEM image of TPP microcapsule (B-2) with the multi-core structure containing 33 wt% of TPP contents based on the TPP + epoxy resin. �

���������������� ������������

���� � �Baek et al. Polymer (Korea), Vol. 28, No. 5, 2004�

���� � ������� ���, �28� �5�, 2004��

�� TPP �� ���� ���� ��� ��� �

��� �� ��� ���� ��� ���� ���

� ���� � ��� ���� �� �� ���

�����, �� ������ �� �� � ��

��� ��� ��� ��� ���� ��.

������������ TPP ������ ��� �

��� ���� �� �� �� ��� �� � ��

��� ����. � ���� �� ��

� ���� ��� ���� �� �� (F127 : SDBS

= 1�1)� ���� ����� ��� �� �� �

�� �� 5 wt%�� 20 wt%�� ����. Figure 5

� ��� ���� � (a�d, 5, 12, 15, 20 wt%)� ��

��� TPP ������ SEM ���, ����

��� 10 wt%� ��� ������ SEM ��

� Figure 4(c)�� �����. ���� � ���

���� ��� 5 wt%� �� ��� �� (Figure 5(a),

B-1)� ������ ���� �� ��� ���

���� 10 wt% (�� A-3) � ��� ��� �

����� ���� � � ��. �� � � �

�� ��� ���� ���� ���� �� TPP �

���� ��� ��� ���� � ���� �

�� ����� �� ��� � � ��. �, TPP ��

��� ������ �� � ���� ���� ��

���� ����� ���� ���� ��� �

� ��� �� �� ����� ����� � �

� ��. ����� �� �� � � 3�19 µm� �

� ��� �� ��� �� �� �� � � Table 1

� ���� ����.

��������������� ����� �� ��� �

��� 33 wt%� ���� ������ ����

� � ���� ������ �� ���� �� ��

TPP ����� ��� ��� �� ����

� � � � � � � � �

(a) (b) (c) �

� � � � � � � �

� (d)� (e)

��������� SEM images of TPP microcapsules prepared by varying ratio of mixed surfactants; F127 : SDBS = (a) 1 : 0 (A-1), (b) 1 : 2 (A-2), (c) 1 : 1 (A-3), (d) 2 : 1 (A-4), and (e) 0 : 1 (A-5).�

Polymer (Korea), Vol. 28, No. 5, 2004� Microencapsulation of a Phosphate Flame Retardant � �����

���, �28� �5�, 2004� �� ���� ������ � � ����

�� �� ����. ��� ���� ��� ��

�� ��� �� F127 : SDBS = 1�1� 12 wt%� ��

�� TPP ��� 25 wt% (Figure 6(a), C-1)�� 40 wt%

(Figure 6(b), C-2)� ���� ������ ���

�� SEM ��� �� �� ��� �� � ����

� ����. � TPP �� 33 wt%� �����

�� (Figure 5(b), B-2)� ������. ���� �

TPP ��� 25 wt% (Figure 6(a), C-1)� �����

��� ������ ���� ��. � ���

�� ��� ��� ����� ���� ��� ��

� � � � � � �

(a) (b)

� � � � � � � �

(c) (d) ��������� SEM images of TPP microcapsules prepared by varying mixed surfactant concentration based on the TPP + epoxy resin at a constant ratio of mixed surfactant (F127 : SDBS = 1 : 1); (a) 5 wt% (B-1), (b) 12 wt% (B-2), (c) 15 wt% (B-3), and (d) 20 wt% (B-4).�

� � � � � � �

(a) (b)

������� � SEM images of microcapsules prepared by varying TPP contents based on the TPP + epoxy resin; (a) 25 wt% (C-1) and (b) 40 wt% (C-2).�

��� � �Baek et al. Polymer (Korea), Vol. 28, No. 5, 2004�

��� � ������� ���, �28� �5�, 2004��

� � ��� � �� ���� ���� ��� �

�� ���� ��� �� �� ��� ��� �

�� ����� �����. ��� TPP �� 33 wt%

(�� B-4) �� 40 wt% (�� C-2)� ��� �� ��

� ����� ��� ����� � � ���. ��

TPP �� 33 wt%�� 40 wt%� ����� �� ��

��� ��� ���� �� ��� ��� � � �

�� (Table 1).

TPP ��� ��� �� ����� ����� (C-1,

B-2, C-2)� TGA �� ��� Figure 7� �����.

Figure 7(a)� �� ����� TPP� �� 25 wt%�

� 40 wt%� ����� ����� ���� � �

�� ���� ����� �� ���� �� 1��

� ���� �� ���� � � ��. ���� �

��� ���� ��� �� ���� �� 25 wt%

�� (�� C-1)� � 12 wt%, 33 wt% �� (�� B-2)

� � 24 wt%, ��� 40 wt% �� (�� C-2)� � 37

wt%� ����� ���� ����� �� ����

100% ������ �� ��� � � ��. �� �

� ���� ������ ��� �� 48%, 73%, �

�� 93%� �� ���� ��� 40 wt%� ��

�� �� �� TPP ��� 37 wt%�� �� �� �

�� ��� ���� � � � ��. �� Figure 7(b)

�� ��� ���� �� �� (derivation) �

��� �� � ��� �� �� � ��.

�������

���� �� ��� (TPP)� �� � ��� ���

��� ��� ��� �� ������� ��

� � in-situ ���� ��� ������ ���

�� ��� ����� ����. � ��� ��

�� ��� �� ��� ��� in-situ ���� �

�� ���� ��� ������ �� ���

�. �� ���� ���� ������ DSC� TGA

� ��� �� �� � �� ��� ����� �

� �� � ��� ��� ��� �� ���� TPP�

�� ��� ���� �� ��� ��� � �

���. �� ����� ��� ��� TEM ���

�� ���� ��� �� ������� ���

�. ��� ��� (F127)� ��� ��� (SDBS)

� �� �� 1�1� �, ��� ��� ���� �

���� ��� ������ ��� ���

���� ���� �� ��� ����� �

�� � � ���. �� �� ���� ��� 40

wt%� �� �� �� �� TPP ��� 37 wt%��

�� �� ��� �� (93 %)� �� � ���.

������� ��� ���������� ���

������ (MI-9911-00-0044)� ���������

2003�� ����21�� � (�)���� ��� ��

�� ��� �� ��� �� � �� ��� �

���.

������� ��

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Wei

ght (

%)

� �� ���� ��� ��� ����

Temperature (�)

(a)

���

���

��

��

Der

ivat

ion

Wei

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%/ �

)

� �� ���� ��� ��� ����

Temperature (�)

(b)

���

���

��

��

���

���

Polymer (Korea), Vol. 28, No. 5, 2004� Microencapsulation of a Phosphate Flame Retardant � ���

���, �28� �5�, 2004� �� ���� ������ � � ��

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