Us 6110982

7/21/2019 Us 6110982

http://slidepdf.com/reader/full/us-6110982 1/7

US006110982A

Ulllted

States Patent

[ 1 9 ] [ 1 1 ] P a t e n t N u m b e r : 6 , 1 1 0 , 9 8 2

R u s s i c k e t a l . [ 4 5 ] D a t e o f

P a t e n t : Aug.

2 9 , 2 0 0 0

[ 5 4 ]

EPOXY FOAMS USING

MULTIPLE RESINS 5 , 2 7 4 , 0 0 6

1 2 / 1 9 9 3 Kagoshima e t

a 1 . . . . . . . . . . . . . . . . . . .

5 2 1 / 1 3 5

ANDCURING AGENTS 5,457,165 10/1995 Hermansen

e t

a 1 . . . . . . . . . . . . . . . . 5 2 5 / 4 2 0 5

[ 7 5 ]

I n v e n t o r s :

Edward M.

R u s s i c k ,

R i o R a n c h o ;

OTHER

UBLICATIONS

get;

‘

R a n d ’

A l b u q u e r q u e ’ b ot h o f R u s s i c k ,

E .

M . ,

a n d R a n d , P . B . , “ D e v e l o p m e n t a n d C h a r a c

6 X ‘

t e r i Z a t i o n

of

a

NeW

Epoxy Foam

Encapsulant

a s

an

A bl e

_

foam Replacement,”

Sandia Nat i ona l Lab ora t o ri e s Report

[ 7 3 ] A s s l g n e e £ 2 1 5 1 2 ‘

C o r p o r a n o n ’

A l b u q u e r q u e ’ N ‘ S A N D 9 8 — 2 5 3 8 , A l b u q u e r q u e , NeW

e x i c o , 1 9 9 8 .

P r i m a r y

Examiner—Morton

F o e l a k

[ 2 1 ] A p p l ' N05 0 9 / 2 2 9 , 5 1 2 A t t o r n e y ,

A g e n t ,

o r Firm—Elmer A .

K l a v e t t e r

[ 2 2 ]

F i l e d : J a n . 1 3 , 1 9 9 9

[ 5 7 ]

ABSTRACT

7

[ 5 1 ]

I n t . C l . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . C08J 9 / 0 0 An poxy

foam

Comprising

a p l u r a l i t y

o f r e s i n s ,

a p l u r a l i t y

[ 5 2 ]

US .

C l . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

5 2 1 / 5 4 ; 5 2 1 / 9 1 ; 5 2 1 / 9 3 ;

o f

C u r i n g

a g e n t s , a t l e a s t one blowing a g e n t , a t l e a s t one

_

5 2 1 / 9 4 ; 5 2 1 / 9 5 ; 5 2 1 / 9 7 ; 5 2 1 / 9 9 ;

1 3 5 / 1 7 8

s u r f a c t a n t

a n d o p t i o n a l l y a t l e a s t o n e

? l l e r

a n d t h e p r o c e s s

Fleld

of

Search

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

f o r

[ m a k i n g ' Preferred

i s

an

ep ox y f o a m

comprising

two

5 2 1 / 8 9 ,

9 1 , 9 3 , 9 4 , 9 5 , 9 7 , 9 9 , 5 4 r e s i n s o f d i f f e r e n t

r e a c t i v i t i e s , t W o

c u r i n g

a g e n t s ,

a b l o w i n g

_

a g e n t ,

a s u r f a c t a n t , and a ? l l e r .

According

t o t h e p r e s e n t

[ 5 6 ]

R e f e r e n c e s

C l t e d i n v e n t i o n , a n epoxy foam i s

p r e p a r e d

W i t h t a i l o r a b l e

Us ATENT

DOCUMENTS

r e a c t i v i t y , e x o t h e r m , a n d p o r e

s i Z e b y

a p r o c e s s o f a d m i x i n g

a p l u r a l i t y

o f

r e s i n s

With a p l u r a l i t y

o f

c u r i n g

a g e n t s ,

a

2 , 9 5 9 , 5 0 8

1 1 / 1 9 6 0

Graham

e t

a 1 . . . . . . . . . . . . . . . . . . . . . . . .

5 2 1 / 1 3 5

S u r f a c t a n t and blowing a g e n t ,

whereby

a foamable mixture

3 7 3 1 6 7 1 8 7

4 / 1 9 6 7 G r o s n e r

e t

a 1 - ~ ~ ~ ~ ~ ~ 521/135

i s

f or med and

heating

s a i d foamable mixture a t a tempera

3 ’ 6 1 5 ’ 9 7 2

1 0 / 1 9 7 1 M i r k e h o u s e ?

J r ‘

2 2 1 / 1 3 2

t u r e g r e a t e r t h a n t h e b o i l i n g t e m p e r a t u r e o f t h e b l o W i n g

3 ’ 6 2 9 ’ 1 6 3 1 2 / 1 9 7 1 NO e n 2 1 / 1 3

agent W h ereby

s a i d

mixture i s f o a m e d

and c u r e d .

4 , 0 9 0 , 9 8 6

5/1978

Gormley e t

a l . . 2 6 0 / 2 . 5

4 , 7 98,848

1 /1989 D i e t h e i m

. . . . . . . .

. . 5 2 1 / 1 3 5

4 , 9 2 3 , 9 0 2 5 / 1 9 9 0 Wycech . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5 2 1 / 1 3 5 17 Claims,

N0

Drawings

7/21/2019 Us 6110982


6 , 1 1 0 , 9 8 2

1

EPOXYFOAMS USING MULTIPLE

RESINS

AND CURING GENTS

T h i s

i n v e n t i o n

W a s ma de W i t h Government s u p p o r t

u n d e r

C o n t r a c t N o . DE-AC04-94AL85000

a w a r d e d

by t h e

D e p a r t m e n t

o f E n e r g y .

T h e Go v e r n m e n t

h a s

c e r t a i n r i g h t s i n

t h e i n v e n t i o n .

BACKGROUND OF THE INVENTION

The i n v e n t i o n

r e l a t e s t o an epoxy f o a m

and

a process f o r

making

t h e

s a m e .

More

p a r t i c u l a r l y ,

t h i s i n v e n t i o n

r e l a t e s

t o

a t a i l o r a b l e epoxy foam e n c a p s u l a n t formed u s i n g a t l e a s t

tWo r e s i n s and

a t

l e a s t tWo c u r i n g a g e n t s .

I n t h e f a b r i ca t i o n o f e l e c t r o n i c d e v i c e s a n d

c i r c u i t s ,

t h e

e l e c t r o n i c d e v i c e s

a r e

p r o t e c t e d

from

t h e a d v e r s e e f f e c t s

o f

t h e e n v i r o n m e n t

by

? l l i n g t h e empty s p a c e s b e t W e e n com

p o n e n t s

on t h e d e v i c e

W i t h

a p o t t i n g

m a t e r i a l

t h a t encapsu

l a t e s t h e s e c o m p o n e n t s .

I f

t h e e l e c t r o n i c d e v i c e i s u s e d

o u t d o o r s ,

s u c h

a s

i n

a u t o m o t i v e ,

a i r c r a f t ,

m a r i n e ,

o r

b u i l d i n g

a p p l i c a t i o n s , t h e p o t t i n g o r e n c a p s u l a n t m a t e r i a l m u s t b e

s t a b l e enough t o p r o v i d e

p r o t e c t i o n

o v e r e x t r e m e o u t d o o r

t e m p e r a t u r e s

a n d h u m i d i t y c o n d i t i o n s , a s

W e l l

a s m e c h a n i c a l

s t r e s s e s .

A d d i t i o n a l l y ,

t h e

e n c a p s u l a n t

m a t e r i a l can s e r v e t o

i s o l a t e t h e p r o t e c t e d d e v i c e s

from

human i n t r u s i o n . I n some

a p p l i c a t i o n s , f u t u r e a c c e s s

t o

t h e

d e v i c e

i s d e s i r e d and s o t h e

e n c a p s u l a n t m u s t

b e c a p a b l e o f i s o l a t i n g t h e

d e v i c e f o r a

p e r i o d o f t i m e b u t

must

h a v e m e c h a n i c a l a n d s t r u c t u r a l

c h a r a c t e r i s t i c s

t o a l l o W

s u b s e q u e n t r e m o v a l

o f

t h e e n c a p s u

l a n t . C o n s e q u e n t l y , s u ch e n c a p s u l a n t s

m u s t

p o s s e s s s u i t a b l e

t h e r m a l ,

m e c h a n i c a l a n d

e l e c t r i c a l p r o p e r t i e s .

Epoxy compounds

h a v e

b e e n

W i d e l y u s e d a s a d h e s i v e s ,

e n c a p s u l a n t s

a n d

c o a t i n g s f o r a v a r i e t y

o f a p p l i c a t i o n s .

E p o x y co m p o u n d s

t y p i c a l l y

h a v e

g o o d

i n s u l a t i n g

p r o p e r t i e s

a n d

e x c e l l e n t a d h e s i o n ,

a n d

a r e

e a s y t o

p r o c e s s . HoWever,

? e x i b i l i Z e d e p o x i e s u s u a l l y h a v e p o o r t h e r m a l

s t a b i l i t y ,

h y d r o l y t i c s t a b i l i t y a n d m e c h a n i c a l

p r o p e r t i e s ;

a n d

c o n s e q u e n t l y ,

h a v e

n o t

b e e n

u s e d

f o r e l a s t o m e r i c a p p l i c a

t i o n s . R a t h e r , p o l y u r e t h a n e o r

s i l i c o n e

p o t t i n g

c o m p o s i t i o n s

h a v e

b e e n

u s e d f o r t h e s e

a p p l i c a t i o n s .

H o W e v e r ,

p o l y u r e

t h a n e s a r e

more

d i f f i cu l t t o p r o c e s s

due

t o

t h e i r

tendency t o

foam

W hen

i n c o n t a c t

W i t h m o i s t u r e - c o n t a i n i n g s u r f a c e s .

S i l i c o n e s

h a v e

t h e d i sa d v a n t a g e o f

b e i n g p o o r

a d h e s i v e s

a n d

a r e

a l s o

m e c h a n i c a l l y

W ea k

a n d

c o s t l y .

E p o x y

f o a m


h a v e a

g e n e r a l c o m p o s i t i o n t h a t

i n c l u d e s a

r e s i n ,

a c u r i n g a g e n t , a s u rf a c t a n t , a bloWing

a g e n t

a n d a ? l l e r

o r n u c l e a t i n g

a g e n t .

The

r e s i n ,

c u r in g a g e n t

a n d

s u r fa c t a n t , a s

W e l l

a s

t h e

c u r i n g

c o n d i t i o n s ,

a r e

chosen

t o

y i e l d

a

s p e c i ? c foam e n c a p s u l a n t

s t r u c t u r e .

The m i x t u r e i s

c a s t i n t o a m o l d and h e a t e d

t o

form and c u r e t h e

e n c a p s u l a n t .

Gormley e t a l . (US.

P a t . N o .

4 , 0 9 0 , 9 8 6 , i s s u e d o n M a y

2 3 ,

1 9 7 8 )

d e s c r i b e

a n

epoxy foam

c o m p o s i t i o n Which

u s e s

a

d e l t a - 1 - t e t r a h y d r o p h t h a l i c

a n h y d r i d e epoxy r e s i n W i t h a n

amine c u ri n g a g e n t

t o form

a t h e r m o s e t

epoxy

f o a m .

Her

mansen e t a l . (US. P a t . No. 5 , 4 5 7 , 1 6 5 , i s s u e d on O c t . 1 0 ,

1 9 9 5 ) n o t e t h a t t h e r e a r e v a r i o u s r e s i n s Which m a y

b e u s e d

i n f o r m i n g a n e n c a p s u l a n t ;

d i g l y c i d y l e t h e r s

a r e commonly

u s e d . Hermansen e t

a l . a l s o

d e s c r i b e

a n e n c a p s u l a n t

Which

u s e s

tWo r e s i n s

t o t a i l o r t h e

p r o p e r t y

o f t h e

formed encap

s u l a n t t o p r o v i d e b o t h d r y h e a t a n d

humid

h e a t

s t a b i l i t y .

The

i n v e n t i o n

a c c o r d i n g

t o

Hermansen

e t a l . d i f f e r s

from

o t h e r

formed


i n t h a t

t h e

i n v e n t i o n

u t i l i Z e s

more

t h a n

o n e

r e s i n

t o t a i l o r s p e c i ? c p r o p e r t i e s o f

t h e

e n c a p s u l a n t t o

a c h i e v e

d e s i r e d p r o p e r t i e s . R u s s i c k

a n d

Rand ( S a n d i a

N a t i o n a l L a b o r a t o r i e s T e c h n i c a l

R e p o r t

SAN 9 8 - 2 5 3 8 ,

A l b u q u e r q u e ,

N .

M e x . ,

D e c e m b e r ,

1 9 9 8 , i n c o r p o r a t e d b y

r e f e r e n c e

h e r e i n )

d e s c r i b e s

a neW epoxy foam

e n c a p s u l a n t

10

1 5

20

25

30

35

40

45

55

60

6 5

2

t h a t u t i l i Z e s

m u l t i p l e r e s i n s

a n d c u ri n g a g e n t s t o c o n t r o l t h e

r e a c t i v i t y , e x o t h e r m , a n d p o r e

s i Z e

a n d

t h e r e f o r e

t h e

m e c h a n i c a l ,

t h e r m a l , a n d

e l e c t r i c a l p r o p e r t i e s o f t h e f o r m e d

epoxy

foam e n c a p s u l a n t .

Such

c o n t r o l a l l o W s

f o r e p o x y

f o a m s o f l a r g e r v o l u m e s W i t h o u t e x c e s s i v e r e a c t i v i t y a n d

e x o t h e r m Which

c o u l d

l e a d

t o

l o W e r e d

p o t

l i f e ,

p r e m a t u r e

c u r i n g p r i o r t o ? l l i n g v o i d

v o l u m e ,

o r

b u r n o u t o f t h e

f o a m .

U s e f u l

Would

b e a

foam e n c a p s u l a n t

W i t h o u t

c a r c i n o g e n i c

c o n s t i t u e n t s t h a t h a s

t a i l o r a b l e m e c h a n i c a l ,

t h e r m a l , a n d

e l e c t r i c a l p r o p e r t i e s t h a t a l l o W e n c a p su l a t i o n o f a

component

such a s electromechanical

components o r

i n s t r u m e n t a t i o n

t h a t s u f ? c i e n t l y

i s o l a t e s

t h e

m a t e r i a l

f r o m

t h e o u t s i d e e n v i

r o n m e n t W i t h a d e q u a t e t h e r m a l / m e c h a n i c a l p r o p e r t i e s t o

a l l o W removal

s o

t h a t t h e e n c a p s u l a t e d

component

c a n be

a c c e s s e d .

SUMMARY OF

THE

INVENTION

A c c o r d i n g

t o

t h e

p r e s e n t i n v e n t i o n , a n epoxy

foam

i s

p r o v i d e d , c o m p r i s i n g a p l u r a l i t y o f r e s i n s , a p l u r a l i t y o f

c u r i n g a g e n t s , a t l e a s t one bloWing a g e n t , a t l e a s t o n e

s u r f a c t a n t ; and o p t i o n a l l y a t

l e a s t

one

? l l e r .

P r e f e r r e d i s

a n

e p o x y

foam c o m p r i s i n g t W o

r e s i n s

o f d i f f e r e n t

r e a c t i v i t i e s ,

tWo

c u r i n g a g e n t s ,

a

bloWing a g e n t ,

a s u r f a ct a n t , a n d a ? l l e r .

More p r e f e r r e d

i s an

epoxy foam

Wherein

t h e tWo r e s i n s a r e

Epon 8 3 0 a n d Epon

8 1 2 1 .

Also

a c c o r d i n g

t o t h e p r e s e n t i n v e n t i o n i s a

p r o c e s s o f

m a k i n g a n e p o x y foam W i t h

t a i l o r a b l e

p r o p e r t i e s ,

c o m p r i s

i n g a d m i x i n g a p l u r a l i t y o f r e s i n s

W i t h

a p l u r a l i t y o f c u r i n g

a g e n t s ,

a

s u r f a c t a n t a n d b l o W i n g a g e n t , Whereby

a

f o a m a b l e

m i x t u r e

i s formed and h e a t i n g s a i d

foamable m i x t u r e

a t a

t e m p e r a t u r e g r e a t e r

t h a n

t h e b o i l i n g

t e m p e r a t u r e o f

t h e

b l o W i n g a g e n t W h e r e b y

s a i d

m i x t u r e i s f o a m e d a n d

c u r e d .

The

epoxy

foam

a c c o r d i n g

t o

t h e

p r e s e n t i n v e n t i o n

c a n

b e

employed i n a k i t , W h e r e i n t h e

k i t

c o m p r i s e s a p r e m i x e d

c o m p o n e n t c o n s i s t i n g e s s e n t i a l l y

o f

t h e c u r i n g a g e n t s , a

p r e m i x e d c o m p o n e n t c o n s i s t i n g e s s e n t i a l l y o f

t h e e p o x y

r e s i n s , t h e

s u r f a c t a n t

a n d t h e n u c l e a t i n g a g e n t , a n d

a

c o m

p o n e n t c o n s i s t i n g e s s e n t i a l l y o f

t h e

b l o W i n g a g e n t .

DESCRIPTION

OF SPECIFIC EMBODIMENTS

Epoxy

f o a m s a r e f o r m e d b y c r o s s - l i n k i n g

r e a c t i o n s

betWeen epoxy r e s i n s a n d

c u r in g a g e n t s t h a t

c r e a t e

a

t h r e e

dimensional covalent bond netWork. There a r e numerous

c o m m e r c i a l l y a v a i l a b l e e p o x y r e s i n s a n d

c u ri n g a g e n t s

t h a t

a r e used

t o

a c h i e v e

epoxy foams W i t h d i f f e r e n t

t h e r m a l ,

m e c h a n i c a l , a n d e l e c t r i c a l p r o p e r t i e s .

A

y p e o f

e p o x y

r e s i n

t h a t

i s

commonly

u s e d

i s

d i g l y c i d y l

e t h e r

o f

b i s p h e n o l

A

(DGEBPA). E x a m p l e s o f t h e s e

a r e :

t h e

s o l i d Epon 1 0 0 1 ,

E p o n

1 0 0 2 ,

E p o n

1 0 0 4 ,

E p o n

1 0 0 7 a n d

E p o n

1 0 0 9 ; a n d t h e

l i q u i d , E p o n 8 2 6 , E p o n 8 2 8 a n d E p o n 8 3 0 , m a n u f a c t u r e d b y

S h e l l

C h e m i c a l

C o r p . A l s o , t h e f o l l o W i n g

e p o x y

r e s i n s

may

b e u s e d : t h e s o l i d

ERL-2002,

2003

a n d

3 0 0 1

a n d

t h e l i q u i d

ERL 7 7 2 , 2774 a n d 3794 m a n u f a c t u r e d

by B a k e l i t e

C o . o f

t h e Union C a r b i d e

P l a s t i c s

D i v i s i o n . Any epoxy r e s i n t h a t i s

c o m p a r a b l e t o t h e a b o v e l i s t e d epoxy r e s i n s ma y b e

u s e d

r e g a r d l e s s o f t h e m a n u f a c t u r e r .

The a d d i t i o n o f

a c u r i n g a g e n t t o

t h e epoxy r e s i n c a u s e s

t h e l i q u i d r e s i n

t o

c u r e

o r

harden i n t o a r i g i d c r o s s - l i n k e d

p o l y m e r .

W h e n

t h e

r e s i n i s i n t i m a t e l y mixed W i t h a s t o

i c h i o m e t r i c amount o f

a

c u r in g a g e n t c o n t a i n i n g l a b i l e

h y d r o g e n

a t o m s ,

t h e

e p o x y

r i n g

o p e n s

a n d

r e a c t s

W i t h

t h e

c u r a t i v e .

Most c u r e d

epoxy

foams

a r e

produced

u s i n g o n e o f

t h r e e

t y p e s

o f

c u r i n g a g e n t s W h i c h a r e a m i n e s , p o l y p h e n o l s ,

a n d

a n h y d r i d e s .

C u r e

i s

a c h i e v e d

b y

p o l y a d d i t i o n W i t h n o

b y - p r o d u c t

f o r m a t i o n , a n d

t h e

c u r e r e a c t i o n betWeen

epoxy

r e s i n s and c u r a t i v e s

i s exothermic Which,

i n

s o m e

c a s e s , can

7/21/2019 Us 6110982


6 , 1 1 0 , 9 8 2

3

e v o l v e

a

c o n s i d e r a b l e amount o f h e a t . C o n t r o l o f

evolved

h e a t

can

be

an important

c o n s i d e r a t i o n

i n an

epoxy

foam.

B e c a u s e a foamed epoxy i s a n i n s u l a t i n g m a t e r i a l ,

( i . e . ,

h a v i n g l o W

t h e r m a l

c o n d u c t i v i t y ) , h e a t

u n a b l e t o e s c a p e

f r o m

t h e

c e n t e r

o f

a s u f ? c i e n t l y

l a r g e

s a m p l e may a c t u a l l y

c h a r

o r

burn

t h e

i n t e r i o r

o f

t h e

foam.

A s i d e from a r e s i n a n d

c u r i n g

a g e n t , o t h e r c o n s t i t u e n t s

used t o m a k e a n epoxy foam

g e n e r a l l y i n c l u d e

a

bloWing

a g e n t ,

a s u r f a c t a n t , a n d a ? l l e r o r

n u c l e a t i n g

a g e n t

( h e r e a f t e r

r e f e r r e d t o a s a ? l l e r ) . Because e p o x i e s

n o r m a l l y

r e a c t W i t h

t h e c u r i n g

a g e n t

W i t h o u t e v o l v i n g v o l a t i l e s , t h e a d d i t i o n o f

a

b l o W i n g

a g e n t

i s

r e q u i r e d . The

b l o W i n g

a g e n t may b e a

c h e m i c a l

a g e n t ,

t h a t t h e r m a l l y

d e c o m p o s e s

a n d e v o l v e s g a s

due

t o

t h e

h e a t

o f

t h e

exothermic

epoxy r e a c t i o n ,

o r a

p h y s i c a l a g e n t , W h i c h s i m p l y

v a p o r i Z e s

a t i t s

b o i l i n g

t e m

p e r a t u r e t o

l i b e r a t e g a s . Chemical

a g e n t s i n c l u d e

ammoniu m

c a r b o n a t e , s o d i u m b i c a r b o n a t e ,

a n d

s u l f o n y l

h y d r a Z i d e .

P h y s i c a l a g e n t s i n c l u d e l i q u i d

s o l v e n t s s u c h

a s t o l u e n e ,

? u o r o c a r b o n s

( F C s ) , c h l o r o ? u o r o c a r b o n s ( C F C s ) , a n d

h y d r o c h l o r o ? u o r o c a r b o n s

( H C F C s ) .

S u r f a c t a n t s

a r e

u s e d i n epoxy foams t o promote foaming

a n d s t a b i l i Z a t i o n o f

t h e s u b s e q u e n t

c e l l u l a r

s t r u c t u r e .

A

s u r f a c t a n t g e n e r a l l y s e r v e s t o d e c r e a s e t h e s u rf a c e t e n s i o n o f

t h e

p r e - c u r e

c o m p o s i t i o n a n d t h e r e b y p r o m o t e

i n c r e a s e d

e x p a n s i o n , s m a l l e r c e l l s ,

a n d

more

u n i f o r m

c e l l

s i Z e a n d

t e x t u r e

o f

t h e e x p a n d e d f o r m e d p r o d u c t . The

s u r f a c t a n t s

u s e d i n p o l y u r e t h a n e foam s y s t e m s , s u c h a s s i l i c o n e - b a s e d

s u r f a c t a n t s ,

a r e

t h e

same ones g e n e r a l l y

used

i n

epoxy

f o a m s .

The

c e l l

s t r u c t u r e c a n b e g r e a t l y

a f f e c t e d

by

t h e

s u r f a c t a n t , Which i n t u r n i n ? u e n c e s t h e

p r o p e r t i e s

o f t h e

r e s u l t a n t

f o a m .

F i l l e r s a r e a dded t o

e po xy f o a m

formulations f o r

reasons

i n c l u d i n g

l o W e r i n g

c o s t ,

a d d i n g

c o l o r ,

r e d u c i n g e x o t h e r m s ,

a n d c o n t r o l l i n g s h r i n k a g e r a t e s . F i l l e r s i n t h e

f o r m

o f ? n e

p a r t i c l e s

( f o r e x a m p l e , ca r b o n

b l a c k o r f u m e d

s i l i c a )

may

a l s o s e r v e a s n u c l e a t i n g a g e n t s . S m a l l p a r t i c l e s p r o v i d e s i t e s

f o r h e t e r o g e n e o u s n u c l e a t i o n Which a l l o W f o r i n i t i a t i o n a n d

s u b s e q u e n t g r o W t h

o f f o a m c e l l s .

I n h e t e r o g e n e o u s

n u c l e a t i o n , g a s m o l e c u l e s d r i v e n b y

s u p e r s a t u r a t i o n

p r e f e r

e n t i a l l y form

n u c l e a t i o n s i t e s

on t h e s o l i d / ? u i d i n t e r f a c e s o f

t h e n u c l e a t i n g a g e n t . The u l t i m a t e c e l l s i Z e i s

d e t e r m i n e d

b y

o t h e r

f a c t o r s i n c l u d i n g t h e

e x o t h e r m ,

t h e

r a t e o f

c u r e , t h e

amount o f

b l o W i n g

a g e n t , a n d i n t e r a c t i o n s

b e t W e e n

t h e

epoxy

a n d

s u r f a c t a n t .

T h e r e

a r e s e v e r a l

i m p o r t a n t

p a r a m e t e r s

t h a t

must b e

c o n s i d e r e d

i n t h e development

o f a foam

W i t h

a d e s i r a b l e

c e l l u l a r

s t r u c t u r e .

F i r s t ,

t h e

r h e o l o g y

o f

t h e

epoxy

m i x t u r e

d u r i n g t h e r i s e o f

t h e

f o a m i s v i t a l l y

i m p o r t a n t . As t h e e p o x y

a n d c u r i n g a g e n t c r o s s - l i n k a n d c u r e , t h e l i q u i d

becomes

more v i s c o u s . The v i s c o s i t y i n c r e a s e i s n e c e s s a r y t o r e t a i n

t h e c e l l s t r u c t u r e c r e a t e d d u r i n g t h e r i s e o f t h e

f o a m .

An

epoxy t h a t d o e s n o t become

s u f ? c i e n t l y

v i s c o u s

t o m a i n t a i n

a c e l l u l a r s t r u c t u r e

d u r i n g

t h e r i s e o f t h e

foam

W i l l c o a l e s c e

a n d

c o l l a p s e . An e p o x y

t h a t becomes e x t r e m e l y v i s c o u s a n d

g e l s t o o e a r l y

may

p r e m a t u r e l y t e r m i n a t e t h e foam r i s e , n o t

a l l o W i n g f o r f u l l e x p a n s i o n .

A n o t h e r i m p o r t a n t p r o c e s s i n g

p a r a m e t e r

c l o s e l y r e l a t e d

t o

foam r h e o l o g y i s t h e epoxy c u r e r a t e , Which s d e p e n d e n t on

t h e

p r o c e s s i n g t e m p e r a t u r e , a s W e l l a s

t h e chosen r e s i n s o r

c u r i n g

a g e n t s .

A

e r y

f a s t

r e a c t i n g e p o x y - c u r a t i v e s y s t e m

With

a l a r g e

exotherm

may

e s u l t i n a

c u r e

r a t e

Which

does

n o t

a l l o W s u f ? c i e n t

p r o c e s si n g t i m e

f o r t h e foam t o r i s e .

F u r t h e r m o r e , a n

e x c e s s i v e amount

o f h e a t from a l a r g e

e x o t h e r m

c o u l d

r e s u l t i n b u r n

o u t

o f t h e i n t e r i o r

r e g i o n s

o f

t h e

f o a m . C o n v e r s e l y , a n e x t r e m e l y s l o W r e a c t i n g

e p o x y

m a y

n o t become v i s c o u s a n d g e l

W i t h i n a n

a p p r o p r i a t e

10

1 5

20

25

30

35

40

45

55

60

6 5

4

amount o f t i m e

t o

e s t a b l i s h a c e l l u l a r

s t r u c t u r e

d u r i n g t h e

foam r i s e , r e q u i r i n g a d d i t i o n o f e x t e r n a l h e a t o r a r e a c t i o n

a c c e l e r a t o r

t o i n c r e a s e t h e

c u r e

r a t e .

Other

p r o c e s s i n g

p a r a m e t e r s Which

a f f e c t

e p o x y

foam

q u a l i t y a n d

c e l l

s t r u c

t u r e a r e s u r f a c e t e n s i o n

and

c e l l

n u c l e a t i o n . S u r f a c t a n t i s

added

a t

a n

a p p r o p r i a t e

l e v e l

t o

c o n t r o l

t h e

s u r f a c e t e n s i o n

o f t h e ? u i d . As a l r e a d y

n o t e d ,

t h e s u r f a c t a n t c a n h a v e a

s i g n i ? c a n t

i n ? u e n c e

on

e l l

s i Z e a n d

foam

m o r p h o l o g y .

The

a d d i t i o n o f ?ne p a r t i c u l a t e s

such

a s

carbon

b l a c k o r fumed

s i l i c a can be

added

t o f a c i l i t a t e

t h e

n u c l e a t i o n o f

a

g r e a t

number o f s m a l l foam p o r e s . T h e r e f o r e ,

epoxy

foam e n c a p

s u l a n t s

o f d i f f e r e n t c e l l u l a r

s t r u c t u r e and t h e r e f o r e

d i f f e r e n t

m e c h a n i c a l , t h e r m a l

a n d

e l e c t r i c a l

p r o p e r t i e s ,

c a n

b e formed

b y

t a i l o r i n g

t h e c h o i c e

o f r e s i n s ,


a n d

p r o c e s s

i n g

c o n d i t i o n s .

A c c o r d i n g

t o

t h e p r e s e n t i n v e n t i o n , t h e e p o x y foam

c o m p r i s e s a p l u r a l i t y o f r e s i n s , a p l u r a l i t y o f c u r i n g a g e n t s ,

a

s u r f a c t a n t ,

a

bloWing a g e n t , a n d

a

? l l e r .

More


t h e

i n v e n t i o n

c o m p r i s e s t W o r e s i n s o f d i f f e r e n t r e a c t i v i t i e s ,

tWo

c u r i n g

a g e n t s

t h a t

c u r e

a t

d i f f e re n t r a t e s t h a t

f u n c t i o n

t o

p r o v i d e a d e s i r e d foam

s t r u c t u r e ,

a

s u r f a c t a n t t h a t f u n c t i o n s

t o l o W e r t h e

s u r f a c e

t e n s i o n

o f

t h e

epoxy m i x t u r e and

s t a b i l i Z e

t h e foam s t r u c t u r e e s t a b l i s h e d by t h e

b l o W i n g

a g e n t , a n d

a ? l l e r .

Dual r e s i n s a n d

d u a l

c u r i n g a g e n t s

o f

v a r y i n g

r e a c t i v i t i e s

p e r m i t t h e a d j u s t m e n t o f t h e r e s i n

r a t i o ,

c u ri n g a g e n t

r a t i o ,

o r

b o t h ,

t o a c h i e v e a d e s i r e d foam p o r e

s i Z e ,

d e n s i t y ,

o r

volume.

A ore r e a c t i v e

f o r m u l a t i o n

u t i

l i Z i n g

a

g r e a t e r r e l a t i v e amount o f t h e h i g h l y r e a c t i v e r e s i n

a n d / o r cu r in g a g e n t c o u l d

b e

u s e d

i n

a p p l i c a t i o n s

W h e r e

s m a l l e r foam

c e l l s

a r e

d e s i r e d and foam

volume

i s s m a l l .

Such a


c r e a t e s a f a s t e r c u r i n g epoxy

system

t h a t

r e s u l t s i n

e a r l y

t e r m i n a t i o n o f foam c e l l g r o W t h a n d e x p a n

s i o n . A e s s r e a c t i v e f o r m u l a t i o n employing

a l e s s e r

r e l a t i v e

a m o u n t

o f

t h e

h i g h l y

r e a c t i v e

r e s i n

a n d / o r c ur i n g a g e n t

may

b e u s e d

i n

a p p l i c a t i o n s

W h e r e l a r g e r foam c e l l s a r e

p e r m i s

s i b l e o r d e s i r e d a n d Where foam volume i s l a r g e . A

e s s

r e a c t i v e f o r m u l a t i o n c r e a t e s a s l o W e r c u r i n g

epoxy s y s t e m

t h a t r e s u l t s i n l a t e t e r m i n a t i o n

o f

foam c e l l g r o W t h a n d

e x p a n s i o n . C o n t r o l o f

p o r e

s i Z e

a n d d e n s i t y ,

c o m b i n e d

W i t h

c o n t r o l o f t h e p a r t i c u l a r c o n s t i t u e n t s c h o s e n

f o r

t h e

e p o x y

foam f o r m u l a t i o n a l s o

a l l o W

c o n t r o l o f m e c h a n i c a l , t h e r m a l ,

a n d e l e c t r i c a l p r o p e r t i e s o f t h e r e s u l t i n g

e p o x y

f o a m .

More


p r e f e r r e d i n t h e p r e s e n t i n v e n t i o n a r e

t h e

r e s i n s EPON

8 3 0

( m a n u f a c t u r e d

b y S h e l l C o r p o r a t i o n ) ,

a

d i g l y c i d y l e t h e r

o f b is p h e n o l

A

e s i n ,

Which

i s a h i g h

v i s c o s i t y

r e s i n W i t h

r e l a t i v e l y

l o W

r e a c t i v i t y W h i c h r a i s e s

t h e

i n i t i a l v i s c o s i t y

o f

t h e epoxy

foam m i x t u r e a n d

EPON

121


b y

S h e l l

C o r p o r a t i o n ) ,

a

b i s p h e n o l

r e s i n

W i t h

a c r y l a t e d p h e n o l s , t h a t i s h i g h l y

r e a c t i v e

c o m p a r e d W i t h

o t h e r

c o m m e r c i a l l y

a v a i l a b l e

r e s i n s a n d

Which c u r e s r a p i d l y

W i t h

e p o x y c u r i n g a g e n t s . A l s o

p r e f e r r e d

a r e t h e c u r i n g

a g e n t s

AN

MINE 0 4 9


b y A i r P r o d u c t s &

C h e m i c a l

C o r p o r a t i o n ) , a

c o m p o u n d c o n s i s t i n g

e s s e n t i a l l y

o f 3 - 3 ‘ - d i m e t h y l m e t h y l e n e d i ( c y c l o h e x y l a m i n e ) a n d E P I

CURE 270


by S h e l l C o r p o r a t i o n ) ,

a

com

p o u n d c o n s i s t i n g

e s s e n t i a l l y o f n - a m i n o e t h y l

p i p e r a Z i n e ,

d i e t h y l e n e t r i a m i n e ,

a n d n o n y l

p h e n o l . AN

AMINE

0 4 9 i s

a c y c l o a l i p h a t i c

amine

c u r i n g

a g e n t

Which

h a s a l o n g c u r e

t i m e ,

r e l a t i v e t o o t h e r

c o m m e r c i a l l y a v a i l a b l e

c u r i n g

a g e n t s ,

W i t h

epoxy r e s i n s and s e r v e s

t o

i n c r e a s e t h e g l a s s t r a n s i t i o n

t e m p e r a t u r e

o f

t h e

c u r e d

e p o x y , t h e r e b y i n c r e a s i n g m e c h a n i

c a l

s t a b i l i t y

a t

h i g h e r

t e m p e r a t u r e s .

EPI-CURE

3270

i s

a n

a l i p h a t i c a m i n e

c u r i n g a g e n t W h i c h

i s

more r e a c t i v e a n d

c u r e s

f a s t e r t h a t

t h e AN

AMINE 2 0 4 9 . The

p r e f e r r e d

b l o W i n g a g e n t i s F C - 7 2 E l e c t r o n i c

F l u i d


b y

3M o r p o r a t i o n ) ,

a

p e r ? u o r i n a t e d

s o l v e n t ( p r i m a r il y

com

p o u n d s

W i t h 6 c a r b o n s ) ,

a n d

h a v i n g a b o i l i n g p o i n t ( 5 6 ° ° C . )

7/21/2019 Us 6110982


7/21/2019 Us 6110982


6 , 1 1 0 , 9 8 2

7

3 6 . 3

g

o f

t h e epoxy


Were

Weighed

o u t i n a 4 “

I . D . > < 1 / z “ t h i c k aluminum mold p r e h e a t e d a t

6 5

° ° C . The

mold

W a s sealed

and

returned t o a 65°°C.

forced

convection oven

t o

c u r e

f o r 4 h o u r s .

The

r e s u l t i n g e p o x y foam

s a m p l e

h a d a d e n s i t y o f 0 . 3 4 7

g / c c

( 2 2

l b / f t 3 )

a n d h a d

a

n o m i n a l

c e l l

s i Z e

o f

a b o u t

200

m m .

EXAMPLE

The f o l l o w i n g i n g r e d i e n t s W e r e u s e d a t t h e

s p e c i ? e d

q u a n t i t i e s

t o

make

a n

epoxy foam s a m p l e :

Epon 830

epoxy

r e s i n : 1 0 . 0 3 g

Epon 8121

epoxy

r e s i n :

6 . 6 7

g

Ancamine 2 0 4 9

c u r i n g

a g e n t :

4 . 3 3 g

E p i - c u r e

3 2 7 0

c u r i n g

a g e n t :

4 . 5 0

g

DC-193 s u r f a c t a n t : 0 . 8 4 g

F C - 7 2

b l o W i n g a g e n t :

2 . 5 0

g

Cabot Monarch 280

c a r b o n b l a c k :

0 . 3 3

g

T h e E p o n

8 3 0

r e s i n ,

E p o n

8 1 2 1

r e s i n ,

DC-193

u r f a c t a n t ,

and

Monarch

280

carbon b l a c k Were

Weighed

o u t i n a

mixing c o n t a i n e r a t room t e m p e r a t u r e . The c o n t e n t s

o f

m i x i n g

c o n t a i n e r

W e r e

mixed t h o r o u g h l y W i t h a

s p a t u l a

f o r

a b o u t 2 m i n u t e s .

The FC-72

bloWing a g e n t

W a s

added

t o

c o n t e n t s o f m i x i n g

c o n t a i n e r ,

a n d

s t i r r e d

t o g e t h e r . T h e

FC-72 Was added

i n c r e m e n t a l l y

u n t i l t h e d e s i r e d

W e i g h t

Was

a c h i e v e d ( E C - 7 2 i s a d d e d

i n c r e m e n t a l l y s i n c e i t

i s a v o l a t i l e

s o l v e n t t h a t t e n d s t o

e v a p o r a t e

u n t i l

i t

i s

mixed

i n t o t h e

e p o x y r e s i n

m i x t u r e ) .

The Ancamine 2 0 4 9 c u r i n g a g e n t

Was

Weighed

o u t i n

t h e

m i x i n g c o n t a i n e r a t room t e m p e r a t u r e .

T h e E p i - c u r e 3 2 7 0

c u r i n g

a g e n t Was W e i g h e d o u t i n

m i x i n g

c o n t a i n e r a t room t e m p e r a t u r e . A l l

t h e

c o n t e n t s i n

t h e

mixing

c o n t a i n e r Were

mixed

t h o r o u g h l y W i t h a s p a t u l a f o r a b o u t 2

m i n u t e s . A f t e r m i x i n g , 1 8 . 2

g

o f

t h e

epoxy


Was

Weighed

o u t i n

a 4 “ I . D . > < 1 / z “ t h i c k aluminum mold p r e h e a t e d

a t 65°°C.

The

m o l d

W a s s e a l e d and r e t u r n e d t o

a 65°°C.

forced convection oven t o cure

f o r

4 h o u r s .

The r e s u l t i n g

e p o x y foam s a m p l e h a d a

d e n s i t y o f

0 . 1 7 4

g / c c ( 1 0 . 9

l b / f t 3 ) a n d h a d a n o m i n a l

c e l l

s i Z e o f a b o u t 4 0 0

mm

COMPARATIVE

EXAMPLE

The

f o l l o W i n g i n g r e d i e n t s W e r e u s e d a t t h e s p e c i ? e d

q u a n t i t i e s

t o

make a n

epoxy

foam

p a t c h

t o b e c o m p a t i b l e

With a n e x i s t i n g

epoxy

f oa m f o r m u l a t i o n , c a l l e d

A b l e f o a m ® , noW d i s c o n t i n u e d

b y

A b l e s t i c k C o r p o r a t i o n .

The epoxy

foam

p a t c h i s n o t made a c c o r d i n g t o t h e p r e s e n t

i n v e n t i o n

a s

o n l y

o n e

c u ri n g a g e n t

i s

u s e d

i n

t h i s

f o r m u l a

t i o n .

Epon 8 2 8 e p o x y

r e s i n : 85 o f

r e s i n

Epon 8 1 2 1 epoxy r e s i n : 15 o f r e s i n

E p i - c u r e 3 2 7 0 c u r i n g a g e n t : 2 1 . 4 p h r

DC-193 s u r f a c t a n t : 1 . 0 p h r

H C F C - 1 4 1 b

b l o W i n g a g e n t : 5 . 0

p h r ( m a n u f a c t u r e d

b y

A l l i e d S i g n a l C o r p . )

C a b o s i l M - 7 D : 2 . 0

p h r


b y C a b o t

C o r p . )

T h e s t e p W i s e p r o c e d u r e f o r p r e p a r a t i o n o f t h e

e p o x y f o a m

sample W a s a s f o l l o W s :

T h e

Epon

8 2 8 r e s i n , t h e

Epon

8 1 2 1

r e s i n ,

t h e

DC-193

s u r f a c t a n t , a n d t h e

C a b o s i l M-7D

Were Weighed

o u t i n

t h e

mixing

c o n t a i n e r

a t

room

t e m p e r a t u r e .

The

c o n t e n t s o f

m i x i n g

c o n t a i n e r

W e r e

mixed t h o r o u g h l y W i t h a s p a t u l a f o r

a b o u t 2 m i n u t e s .

The HCFC-141b b l o W i n g

a g e n t Was

a d d e d

t o c o n t e n t s

o f

m i x i n g c o n t a i n e r ,

a n d

s t i r r e d

t o g e t h e r .

The

b l o W i n g a g e n t

Was

a d d e d i n c r e m e n t a l l y u n t i l

t h e d e s i r e d

W e i g h t Was a c h i e v e d .

The

E p i - c u r e 3270 c u r i n g a g e n t Was

10

1 5

20

25

30

35

40

45

55

60

6 5

8

Weighed

o u t

i n

m i x i n g

c o n t a i n e r a t room t e m p e r a t u r e . A l l

t h e

c o n t e n t s i n t h e m i x i n g c o n t a i n e r Were mixed t h o r o u g h l y

W i t h a s p a t u l a f o r a b o u t 2 m i n u t e s . A f t e r

m i x i n g

t h e epoxy

formulation

W a s

used a s a patch

i n

an

e l e c t r o n i c

system t h a t

h a d p r e v i o u s l y b e e n

e n c a p s u l a t e d

W i t h t h e

Ablefoam® foam

and

f o r

Which

a

p a t c h

W a s

r e q u i r e d .

The

system

W a s

s e a l e d

and returned

t o

a 70°°C.

forced

convection oven t o c u r e .

T h e

r e s u l t i n g e p o x y f o a m p a t c h h a d p r o p e r t i e s c o n s i s t e n t

W i t h t h e Ablefoam® f o a m .

EXAMPLE

While t h e epoxy foam f o r m u l a t i o n

o f C o m p a r a t i v e

Example

1

Was s u f ? c i e n t

f o r s m a l l - v o l u m e

p a t c h i n g , t h e

f o r m u l a t i o n W a s n o t s u i t e d f o r more g e n e r a l

l a r g e

volume

a p p l i c a t i o n s b e c a u s e t h a t


had a

v e r y

s h o r t

p o t

l i f e

i . e . , p r o c e s s i n g

t i m e

p r i o r t o

c u r e ) .

F u r t h e r

e x p e r i m e n

t a t i o n

r e v e a l e d t h a t

epoxy

foam f o r m u l a t i o n s h a v i n g mul

t i p l e

e p o x y r e s i n s a n d m u l t i p l e

c u r i n g

a g e n t s c o u l d b e

t a i l o r e d

t o

h a v e t h e

d e s ir e d t h e r m a l ,

m e c h a n i c a l , a n d

e l e c

t r i c a l

p r o p e r t i e s

b y v a r y i n g

t h e

p r o p o r t i o n

o f

t h e

v a r y i n g

c o n s t i t u e n t s .

The f o l l o W i n g i n g r e d i e n t s W e r e

u s e d

a t

t h e

s p e c i ? e d

q u a n t i t i e s t o make a n e p o x y foam s a m p l e o f c y l i n d r i c a l

geometry

W i t h

a

d i a m e t e r

o f 3 i n c h e s and a l e n g t h o f 8

i n c h e s .

The

s t a n d a r d c u r a t i v e

r a t i o

W a s

modi?ed t o

cause t h e

f o r m u l a t i o n t o

be

l e s s r e a c t i v e

and

a l l o W f o r s u f f i c i e n t c u r e

t i m e s u c h t h a t

t h e

foam c o u l d r i s e s u f ? c i e n t l y t o

? l l

t h e

l a r g e r

v o l u m e m o l d :

Epon

8 3 0 e p o x y

r e s i n : 1 3 2 . 9

g

(60 o f r e s i n )

Epon 8 1 2 1 e p o x y

r e s i n :

8 8 . 7 g (40 o f r e s i n )

A n c a m i n e

2 0 4 9

c u r i n g a g e n t : 6 5 . 2 g ( 2 9 . 5 p h r )

E p i - c u r e

3 2 7 0

c u r i n g

a g e n t :

3 8 . 7 g ( 1 7 . 5 p h r )

DC-193

s u r f a c t a n t :

6 . 8 g ( 3 . 0 p h r )

F C - 7 2

b l o W i n g a g e n t : 1 3 . 3 g

( 6 . 0

p h r )

C a b o t Monarch

2 8 0

c a r b o n b l a c k : 4 . 4 g ( 2 . 0

p h r )

T h e s t e p W i s e

p r o c e d u r e

f o r

p r e p a r a t i o n o f

t h e e p o x y f o a m

sample W a s a s f o l l o W s :

T h e Epon 8 3 0

r e s i n ,

t h e

Epon 8 1 2 1

r e s i n ,

t h e

DC-193

s u r f a c t a n t , a n d

t h e

Monarch

280

c a r b o n b l a c k Were

Weighed

o u t

i n

t h e mixing c o n t a i n e r

a t

room t e m p e r a t u r e .

The

c o n t e n t s

o f

mixing c o n t a i n e r

Were

mixed

t h o r o u g h l y W i t h a

s p a t u l a

f o r a b o u t 2

m i n u t e s . The FC-72

b l o W i n g

a g e n t Was

a d d e d t o

c o n t e n t s

o f m i x i n g

c o n t a i n e r ,

a n d

s t i r r e d t o g e t h e r .

The FC-72 Was

a d d e d


u n t i l t h e

d e s i r e d

W e i g h t

Was a c h i e v e d

(EC-72

i s added i n c r e m e n t a l l y

s i n c e i t

i s

a

v o l a t i l e

s o l v e n t

t h a t

t e n d s

t o

e v a p o r a t e

u n t i l

i t

i s

mixed

i n t o

t h e e p o x y r e s i n m i x t u r e ) . T h e Ancamine 2 0 4 9

c u r i n g

a g e n t

W a s Weighed o u t i n

t h e

mixing c o n t a i n e r a t room

tempera

t u r e . The E p i - c u r e 3270 c u r in g a g e n t Was

Weighed

o u t

i n

mixing c o n t a i n e r a t room e m p e r a t u r e . A l l t h e c o n t e n t s

i n

t h e

m i x i n g

c o n t a i n e r

W e r e mixed t h o r o u g h l y

W i t h a s p a t u l a

f o r

a b o u t 2 m i n u t e s . A f t e r m i x i n g ,

300

g o f

t h e epoxy formu

l a t i o n Was

Weighed o u t i n a 3 “ I . D . > < 8 “

l o n g

c y l i n d r i c a l

aluminum mold

p r e h e a t e d

a t

6 5 °

C . The

mold

W a s s e a l e d

and r e t u r n e d t o a 65° C . forced convectio n oven t o cure f o r

4

h o u r s .

The r e s u l t i n g e p o x y foam

s a m p l e h a d

a d e n s i t y o f

2 0

l b / f t 3

and had

a

nominal

c e l l

s i Z e

o f a b o u t 250

mm.

EXAMPLE

2 0 l b / f t 3 D e n s i t y E p o x y Foam K i t

A r e m i x e d

epoxy

foam

k i t

h a s b e e n d e v e l o p e d f o r a n

epoxy

foam f o r m u l a t i o n f o r a foam d e n s i t y o f

a p p r o x i m a t e l y

20

l b / f t 3 . The

k i t

c o n s i s t s

o f

t h r e e

components

Which a r e

7/21/2019 Us 6110982


6 , 1 1 0 , 9 8 2

b l e n d e d t o g e t h e r

t o

form t h e epoxy foam

m i x t u r e .

The

e p o x y

foam k i t

makes

W e i g h i n g a n d m i x i n g

t h e m a t e r i a l s

more

c o n v e n i e n t

f o r

t h e

o p e r a t o r b e c a u s e

o n l y

t h r e e c o m

ponents

a r e involved r a t h e r t h a n t h e

seven

i n d i v i d u a l s t a r t

i n g m a t e r i a l s .

T h e k i t

c o n s i s t s

o f

Component A , W h i c h

i n c l u d e s

tWo

epoxy

r e s i n s , a s u r f a c t a n t ,

and

a

n u c l e a t i n g

a g e n t , Component B , W h i c h

i n c l u d e s

a

b l o W i n g

a g e n t , a n d

Component C

W h i c h

i n c l u d e s

t h e t W o

c u r i n g

a g e n t s .

T h e f o l l o W i n g i s t h e c o m p o s i t i o n o f C o m p o n e n t s A , B ,

a n d C t h a t make up t h e 20 l b / f t 3 d e n s i t y epoxy

foam

k i t s :

C o m p o n e n t A :

Epon

830 epoxy

r e s i n : 5 7 . 1

W t

Epon

8121

r e s i n : 3 8 . 1

W t

DC-193

s u r f a c t a n t : 2 . 9

W t

Monarch

280

c a r b o n b l a c k : 1 . 9 W t

C o m p o n e n t B :

FC-72

b l o W i n g

a g e n t :

1 0 0

Wt

C o m p o n e n t C :

Ancamine 2049

c u r i n g

a g e n t :

6 2 . 8 Wt

E p i - c u r e

3 2 7 0

c u r i n g

a g e n t : 3 7 . 2 W t

The f o l l o W i n g a r e t h e ? n a l a m o u n t s o f Components

,

B ,

and C o ma ke a n epoxy foam m i x t u r e f o r 20

l b / f t 3

foam

d e n s i t y :

Component

A :

6 6 . 5

Wt

Component B :

3 . 8

W t

Component C : 2 9 . 7 W t

T o

p r e p a r e

t h e e p o x y f o a m ,

Component

Ais W e i g h e d o u t i n

a mixing

c o n t a i n e r

a t room

t e m p e r a t u r e .

Component B s

a d d e d t o c o n t e n t s o f m i x i n g

c o n t a i n e r

a n d

s t i r r e d .

Compo

n e n t B

i s a d d e d


u n t i l t h e d e s i r e d W e i g h t i s

a c h i e v e d ( P C - 7 2 i s a d d e d i n c r e m e n t a l l y s i n c e i t i s

a v o l a t i l e

s o l v e n t t h a t t e n d s

t o

e v a p o r a t e

u n t i l

i t i s mixed

i n t o t h e

e p o x y

r e s i n

m i x t u r e ) .

Component

C i s W e i g h e d

o u t

i n t h e

mixing c o n t a i n e r a t room t e m p e r a t u r e .

A l l

t h e c o n t e n t s

i n

t h e

m i x i n g c o n t a i n e r a r e mixed t h o r o u g h l y W i t h a s p a t u l a f o r

a b o u t 2 m i n u t e s . A f t e r

m i x i n g ,

t h e epoxy f o r m u l a t i o n i s

Weighed o u t

i n a

mold p r e h e a t e d

a t

6 5 ° ° C .

The mold i s

s e a l e d

and

r e t u r n e d t o

a 65°°C.

forced convection oven t o

c u r e

f o r

4 h o u r s .

EXAMPLE

1 0

l b / f t 3

D e n s i t y E p o x y Foam K i t

A

r e m i x e d epoxy foam

k i t h a s

b e e n

d e v e l o p e d

f o r

a n

epoxy foam


f o r a

foam

d e n s i t y

o f


1 0

l b / f t 3 .

The k i t

c o n s i s t s

o f

t h r e e

components

Which

a r e

b l e n d e d t o g e t h e r t o form

t h e epoxy

foam m i x t u r e . The

e p o x y foam k i t makes W e i g h i n g

a n d

m i x i n g t h e m a t e r i a l s

more c o n v e n i e n t f o r t h e

o p e r a t o r

b e c a u s e o n l y

t h r e e c o m

ponents a r e involved r a t h e r t h a n t h e seven i n d i v i d u a l s t a r t

i n g m a t e r i a l s . T h e k i t c o n s i s t s o f Component A , W h i c h

i n c l u d e s

tWo

epoxy r e s i n s ,

a s u r f a c t a n t ,

and

a

n u c l e a t i n g

a g e n t , Component

B ,

W h i c h i n c l u d e s a b l o W i n g a g e n t , a n d

Component C W h i c h i n c l u d e s t h e t W o c u r i n g

a g e n t s .

T h e

f o l l o W i n g i s t h e

c o m p o s i t i o n

o f C o m p o n e n t s

A ,

B ,

a n d

C

f o r

t h e

1 0

l b / f t 3 d e n s i t y e p o x y

foam

k i t s :

C o m p o n e n t

A :

Epon

830

epoxy

r e s i n :

5 6 . 1 W t

Epon 8121

r e s i n :

3 7 . 4 W t

DC-193

s u r f a c t a n t :

4 . 7 W t

Monarch

280 c a r b o n b l a c k : 1 . 9 W t

C o m p o n e n t B :

FC-72

b l o W i n g

a g e n t :

1 0 0

Wt

10

1 5

20

25

30

35

40

45

55

60

6 5

1 0

C o m p o n e n t

C :

Ancamine 2049 c u r i n g a g e n t : 6 2 . 8 Wt

E p i - c u r e

3 2 7 0

c u r i n g

a g e n t : 3 7 . 2 W t

The f o l l o W i n g a r e t h e ? n a l a m o u n t s o f Components

A ,

B ,

a n d

C

t h a t a r e r e q u i r e d f o r making

t h e epoxy

foam m i x t u r e

f o r

1 0

l b / f t 3

f o a m

d e n s i t y :

Component A : 6 3 . 3 W t

Component B :

8 . 9 W t

Component

C : 2 7 . 8 W t

The p r o c e s s i n g

p r o c e d u r e i s

s i m i l a r t o t h a t

d e s c r i b e d

i n

Example

4

t o p r e p a r e

t h e 20

b / f t 3

epoxy

foam f o r m u l a t i o n .

The i n v e n t i o n

h a s

been

d e s c r i b e d

i n d e t a i l a b o v e and i n

t h e

s p e c i? c e x a m p l e s . F u r t h e r v a r i a t i o n s

W i l l

b e a p p a r e n t t o

t h o s e s k i l l e d i n

t h e

a r t . The t r u e s c o p e o f

t h e

i n v e n t i o n

i s t o

b e f o u n d

i n

t h e

a p p e n d e d

c l a i m s .

We l a i m :

1 .

An

epoxy

foam

W i t h a

d e n s i t y

betWeen a p p r o x i m a t e l y

1 0 l b / f t 3

a n d

a p p r o x i m a t e l y 2 2 l b / f t 3 ,

c o m p r i s i n g :

a t l e a s t tWo r e s i n s , one r e s i n b e i n g

more

r e a c t i v e

t h a n

t h e

o t h e r

r e s i n s ,

s a i d r e s i n s

b e i n g s e l e c t e d

f r o m t h e g r o u p

c o n s i s t i n g

o f

a d i g l y c i d y l e t h e r o f b i s p h e n o l A n d a

b i s p h e n o l

r e s i n W i t h a c r y l a t e d p h e n o l s ;

a t

l e a s t

t W o

c u r i n g

a g e n t s ,

o n e c u r in g a g e n t c u r in g f a s t e r

t h a n

t h e

o t h e r c u r i n g a g e n t s ;

a t

l e a s t o n e

bloWing

a g e n t ;

a t l e a s t

one s u r f a c t a n t ; and

o p t i o n a l l y a t

l e a s t o n e ? l l e r ; W h e r e i n t h e epoxy

foam

r e s u l t i n g f r o m

t h e

m i x t u r e o f

s a i d

r e s i n s ,

s a i d

c u r n g

a g e n t s ,

s a i d b l o W i n g a g e n t , s a i d s u r f a c t a n t a n d

o p t i o n

a l l y s a i d ? l l e r h a s

a

d e n s i t y b e t W e e n a p p r o x i m a t e l y 1 0

l b / f t 3 a n d a p p r o x i m a t e l y 2 2 l b / f t 3 .

2 . The

e p o x y

foam o f c l a i m 1 , W h e r e i n t h e a t l e a s t

t W o

r e s i n s

c o n s i s t s

e s s e n t i a l l y

o f

a

d i g l y c i d y l e t h e r

o f

b i s p h e n o l

A n d a b i s p h e n o l r e s i n W i t h

a c r y l a t e d

p h e n o l s .

3 .

The epoxy foam

o f

c l a i m

1 , W h e r e i n t h e a t

l e a s t

tWo

c u r i n g a g e n t s

a r e

s e l e c t e d

f r o m t h e g r o u p

c o n s i s t i n g

o f

a m i n e s , p o l y p h e n o l s ,

a n d

a n h y d r i d e s .

4 . The epoxy foam o f c l a i m 1 Wherein t h e a t l e a s t tWo


c o n s i s t s o f a

c y c l o a l i p h a t i c a m i n e c u ri n g a g e n t

a n d a

c u ri n g a g e n t c o m p r i s i n g

a n

n - a m i n o e t h y l p i p e r a Z i n e ,

d i e t h y l e n e

t r i a m i n e , a n d a

p h e n o l .

5 . The

epoxy

foam

o f

c l a i m 1 Wherein t h e

a t

l e a s t

one

b l o W i n g

a g e n t i s s e l e c t e d

f r o m

t h e g r o u p c o n s i s t i n g

o f a

p h y s i c a l b l o W i n g

a g e n t

a n d

a c h e m i c a l b l o W i n g a g e n t .

6 .

The

epoxy

foam

o f c l a i m

5 W h e r e i n t h e p h y s i c a l

b l o W i n g a g e n t i s s e l e c t e d f r o m t h e

g r o u p c o n s i s t i n g o f

t o l u e n e ,

? u o r o c a r b o n s , c h l o r o ? u o r o c a r b o n s

a n d

h y d r o c h l o

r o ? u o r o c a r b o n s .

7 . The

epoxy foam

o f c l a i m 5

Wherein t h e

c h e m i c a l

b l o W i n g a g e n t

i s s e l e c t e d f r o m

t h e g r o u p c o n s i s t i n g o f

ammonium c a r b o n a t e , s o d i u m b i c a r b o n a t e , a n d s u l f o n y l

h y d r a Z i d e .

8 . The epoxy foam o f c l a i m 1 Wherein t h e a t l e a s t one

s u r f a c t a n t i s

a n

e t h y l e n e o x i d e - p r o p y l e n e o x i d e s i l o x a n e

b l o c k

p o l y m e r .

9 . The epoxy foam o f c l a i m 1 Wherein t h e a t l e a s t one

? l l e r

i s

s e l e c t e d

f r o m

t h e g r o u p c o n s i s t i n g o f c a r b o n

b l a c k ,

fumed

s i l i c a ,

a n d

t i t a n i u m d i o x i d e .

1 0 . The epoxy foam o f c l a i m 1

Wherein

t h e a t l e a s t one

? l l e r i s a

n u c l e a t i n g

a g e n t .

1 1 .

The

epoxy

foam

o f

c l a i m

1

W h e r e i n

t h e

nominal

c e l l

s i Z e o f

t h e epoxy foam

i s betWeen a p p r o x i m a t e l y

200 mm

and a p p r o x i m a t e l y 400 m m .

1 2 .

A

r o c e s s

o f

making a n epoxy foam

W i t h a t a i l o r e d

d e n s i t y o f b e t W e e n


1 0 l b / f t 3 a n d a p p r o x i

m a t e l y

2 2

l b / f t 3 , c o m p r i s i n g :

7/21/2019 Us 6110982


6 , 1 1 0 , 9 8 2

1 1

admixing a t l e a s t

two

r e s i n s ,

one r e s i n

being more r e a c

t i v e t h a n

t h e o t h e r s

w i t h a a t l e a s t two c u r i n g a g e n t s ,

one

c u r i n g a g e n t

have a f a s t e r c u r e

r a t e t h a n

t h e o t h e r s ,

a s u r f a c t a n t a n d b l o w i n g a g e n t , whereby a f o a m a b l e

m i x t u r e

i s

f o r m e d ;

h e a t i n g s a i d

f o a m a b l e

m i x t u r e

a t

a

t e m p e r a t u r e

g r e a t e r

t h a n t h e b o i l i n g t e m p e r a t u r e o f

t h e b l o w i n g

a g e n t

whereby

s a i d

m i x t u r e i s foamed and c u r e d

t o

form a n

epoxy

foam

w i t h a t a i l o r e d

d e n s i t y o f

b e t w e e n a p p r o x i

m a t e l y 1 0 l b / f t 3 a n d a p p r o x i m a t e l y 2 2 l b / f t 3 .

1 3 . A r o c e s s a c c o r d i n g

t o

c l a i m 1 2 wherein a ? l l e r i s

added

t o s a i d

foamable m i x t u r e .

1 4 . A r o c e s s a c c o r d i n g

t o c l a i m 1 2 w h e r e i n

s a i d foam

a b l e

m i x t u r e i s

i n j e c t e d

i n t o a mold p r i o r t o h e a t i n g .

1O

1 2


6 6 . 5

w t o m p o n e n t A , c o n s i s t i n g

o f

a p p r o x i m a t e l y 5 7 wt d i g l y c i d y l

e t h e r

o f b is p h e n o l

A , a p p r o x i m a t e l y 3 8 wt f a b i s p h e n o l r e s i n w i t h

a c r y l a t e d p h e n o l s ,

a p p r o x i m a t e l y 3

w t

f a n

e t h y l e n e

o x i d e - p r o p y l e n e

o x i d e s i l o x a n e b l o c k p o l y m e r


a n d


2

w t

a r b o n

b l a c k ;


3 . 8 w t f c o m p o n e n t B , c o n s i s t i n g o f

a blowing a g e n t o f a p e r ? u o r i n a t e d

s o l v e n t

w i t h

a

b o i l i n g

p o i n t

o f a p p r o x i m a t e l y

5 6 C . ;

a n d a p p r o x i

m a t e l y 2 9 . 7 w t f c o m p o n e n t

C ,

c o n s i s t i n g o f


6 3 wt o f a c y c l o a l i p h a t i c amine

c u r i n g a g e n t a n d a p p r o x i m a t e l y

3 7

wt f a c u r i n g

a g e n t c o m p r i s i n g

a n n - a m i n o e t h yl p i p e r a Z i n e , d i e t h y l

e n e

t r i a m i n e ,

and a

p h e n o l .

1 7 . A r o c e s s o f

making

a n epoxy foam w i t h

a t a i l o r e d

d e n s i t y o f

a p p r o x i m a t e l y 1 0

l b / f t 3

a n d a p p r o x i m a t e l y

2 2

l b / f t 3 ,


a d m i x i n g

a d i g l y c i d y l

e t h e r

o f b i s p h e n o l

A ,

a b i s p h e n o l

1 5 .

An poxy foam

w i t h a

d e n s i t y o f a p p r o x i m a t e l y 1 0 1 5

l b / f t 3 , c o m p r i s i n g :

a p p r o x i m a t e l y 6 3 . 3 w t f

c o m p o n e n t A ,


a p p r o x i m a t e l y 5 6 wt d i g l y c i d y l

e t h e r

o f

b i s p h e n o l

A ,

a p p r o x i m a t e l y 37

wt f

a b i s p h e n o l r e s i n

w i t h

a c r yl a t e d p h e n o l s ,


5

w t

f

a n

e t h y l e n e

o x i d e - p r o p y l e n e

o x i d e s i l o x a n e b l o c k p o l y m e r

s u r f a c t a n t , a n d a p p r o x i m a t e l y 2

w t

a r b o n

b l a c k ;


8 . 9

w t f

c o m p o n e n t

B , c o n s i s t i n g o f

a blowing a g e n t o f a

p e r ? u o r i n a t e d s o l v e n t w i t h

a

b o i l i n g p o i n t o f a p p r o x i m a t e l y 5 6 C . ; a n d a p p r o x i

m a t e l y 2 7 . 8 w t f

c o m p o n e n t

C ,


a p p r o x i m a t e l y 6 3

wt

o f

a c y c l o a l i p h a t i c amine

c u r i n g a g e n t a n d a p p r o x i m a t e l y

3 7

wt f

a

c u r i n g



e n e

t r i a m i n e ,

and a

p h e n o l .

1 6 . An

epoxy

foam

w i t h

a d e n s i t y o f a p p r o x i m a t e l y

20

l b / f t 3 ,


20

25

r e s i n

w i t h

a c r y l a t e d

p h e n o l s , a n e t h y l e n e o x i d e

p r o p y l e n e o x i d e

s i l o x a n e

b l o c k

p o l y m e r


c a r b o n

b l a c k ,

a

b l o w i n g a g e n t

c o m p r i s i n g a p e r ? u o r i

n a t e d s o l v e n t w i t h

a

b o i l i n g

p o i n t o f a p p r o x i m a t e l y 5 6

C . , a

c y c l o a l i p h a t i c a m i n e c u r i n g a g e n t

a n d a

c u r i n g



e n e t r i a m i n e , and

a

phenol t o form

a

foamable

m i x t u r e ;

h e a t i n g s a i d f o a m a b l e m i x t u r e a t a t e m p e r a t u r e

g r e a t e r

t h a n

t h e

b o i l i n g t e m p e r a t u r e o f t h e

b l o w i n g

a g e n t

whereby s a i d m i x t u r e i s foamed and

c u r e d

t o form a n

epoxy foam w i t h a t a i l o r e d

d e n s i t y o f

b e t w e e n

a p p r o x i

m a t e l y 1 0 l b / f t 3 a n d a p p r o x i m a t e l y 2 2 l b / f t 3 .

* * * * *

Us 6110982

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