us3884964 - dispersante aa-ab-alcohol - continua

7/18/2019 US3884964 - Dispersante AA-AB-ALCOHOL - Continua

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U n i t e d S t a t e s

P a t e n t

[ 1 9 1

Otrhalek e t a l .

[ 1 1 1

3 , 8 8 4 , 9 6 4

[ 4 5 1 May

2 0 ,

1 9 7 5

[ 5 4 1

[ 7 5 ]

[ 7 3 1

[ 2 2 ]

[ 2 1 ]

[ 5 2 ]

[ 5 1 ]

[ 5 3 ]

[ 5 6 ]

2 , 7 6 5 , 2 2 9

PIGMENT DISPERSANT I N AQUEOUS

SLURRIES

I n v e n t o r s : J o s e p h V . O t r h a l e k , D e a r b o r n ,

M i c h . ; G u n t h e r H .

E l f e r s ,

M u t t e r s t a d t , G e r m a n y

BASF

W y a n d o t t e

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

W y a n d o t t e ,

M i c h .

F i l e d :

J a n .

3 1 ,

1974

A p p l . N o . : 4 3 8 , 3 3 6

A s s i g n e e :

US. Cl . . . . . . . . . . . . . 260/486 R; 106/309; 162/162;

2 6 0 / 4 2 . 2 l ; 2 6 0 / 4 2 . 5 2

Int. C l . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

C07c

69/54

Field of

S e a r c h . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

. .

260/486

R

R e f e r e n c e s C i t e d

UNITED

STATES PATENTS

l O / l 9 56 McLaughlin

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

92/21

2,9 9 9,038 9/ 1 96 1

Drannan

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

1 1 7/ 155

P r i m a r y E x a m i n er — l _ . o r r a i n e A . W e i n b e r g e r

A s s i s t a n t

Examiner—Paul J .

K i l l o s

A t t o r n e y ,

A g e n t, o r

Firm—Bernhard R . S w i c k ; J o s e p h

D . M i c h a e l s ;

R o b e r t

E . Dunn

[ 5 7 ]

ABSTRACT

A

e u t r a l i z e d

s o l u t i o n

o f p o l y m e r p r e p a r e d b y t h e f r e e

r a d i c a l p o l y m e r i z a t i o n o f a n

a l p h a ,

b e t a u n s a t u r a t e d

a c i d , e . g . , a c r y l i c a c i d w i t h

s m a l l amounts

o f

a n

a l k y l

e s t e r a n a l p h a , b e t a u n s a t u r a t e d

a c i d and

a l l y l a l c o h o l

w h e n add ed

t o

a n

aqueous pigment s l u r r y a t a r a t e of

l e s s

t h a n

o n e

p e r c e n t

p o l y m e r

s o l i d s

b y w e i g h t

o f p u l p

p r e s e n t

y i e l d s

i m p r o v e d p i g m e n t

d i s p e r s i o n h a v i n g

s i g

n i f i c a n t l y l o w e r v i s c o s i t y .

8

C l a i m s ,

No D r a w i n g s



3 , 8 8 4 , 9 6 4

1

PIGMENT DISPERSANT I N AQUEOUS SLURRIES

BACKGROUND OF THE INVENTION

1 .

F i e l d o f

t h e

I n v e n t i o n

T h i s

i n v e n t i o n r e l a t e s

t o t h e

c o n t r o l

o f

pigment

d i s

p e r s i o n s l u r r i e s which a r e mor e

pumpable

b y t h e

u s e

o f

a s o l u t i o n o f a n e u t r a l i z e d

copolymer

h a v i n g a h i g h a l

p h a ,

b e t a

u n s a t ur a t e d c a r b o n y l a c i d c o n t e n t .

2 .

D e s c r i p t i o n o f t h e Pr i o r

A r t

The

p r o b l e m

o f

p i g m e n t

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

p r e p a r a t i o n

o f

p a p e r ,

p a i n t s , i n k s a n d

t h e

l i k e

h a s p r e

v i o u s l y b e e n r e c o g n i z e d .

Am o n g t h e p r i o r a r t US a t . N o . 2 , 3 9 9 , 4 8 9 d i s

c l o s e s

t h e

u s e of sodium carbonate t o reduce

t h e

v i s

c o s i t y

o f c l a y

c o n t a i n i n g

p i g m e n t d i s p e r s i o n f o r

u s e

i n

p a p e r m a k i n g .

The p a t e n t

f u r t h e r

d i s c l o s e s

p o l y p h o s

p h a t e s s u c h a s

sodium

h e x a - m e t a - p h o s p h a t e h a v e

been

e m p l o y e d .

A a t e r

p a t e n t ,

US. P a t .

No. 3 , 0 2 1

, 2 5 7 ,

d i s c l o s e s

t h a t

t h e

amount

o f

p i g m e n t

d e p o s i t e d

on

p a p e r

d u r i n g t h e

papermaking

p r o c e s s

from

a g i v e n amount

o f pigment

d i s p e r s i o n

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

w i t h t h e p i g m e n t

o r

p o s t - t r e a t i n g

t h e p i g m e n t w i t h

w a t e r - s o l u b l e a n i o n i c

p o l y m e r ,

e . g . , a n

a c r y l a m i d e z a

c r y l i c a c i d copolymer w h e r e i n 8 0 t o 9 5 mole

p e r c e n t

o f t h e p o l y m e r

i s

a c r y l a m i d e .

US. P a t . N o . 3 , 2 3 4 ,0 7 6

d i s c l o s e s

t h e

u s e o f a c r y l a m i d e - d i a l l y l amine c o p o l y

mers

f o r

t h e

s am e

p u r p o s e . S t i l l another p a t e n t ,

US.

P a t , No.

3 , 5 0 9 , 0 2 1 ,

d i s c l o s e s

t h e

u s e o f m i x t u r e s o f

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

of 1 : 9

t o 9 : 1 t o achieve t h e s a m e

r e s u l t s .

I n accordance

w i t h

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

c o m p o s i t i o n

f o r

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

a n d

v i s c o s i t y

o f p i g m e n t s i n a n

a q u e o u s

s l u r r y

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

o f a n a l k a l i n e u t r a l i z e d t e r p o l y m e r p r o d u c e d

b y

t h e

f r e e r a d i c a l p o l y m e r i z a t i o n

o f

from about

60

t o about

8 8 p a r t s b y w e i g h t o f a t

l e a s t

one a l p h a , b e t a u n s a t u

r a t e d a c i d c o n t a i n i n g 3 t o

4

carbon

a t o m s ,

from

about

6 t o a b o u t

2 8

p a r t s

b y w e i g h t

o f a t l e a s t one a l k y l a t e

o f

a n

a l p h a ,

b e t a u n s a t u r a t e d a c i d c o n t a i n i n g 3 t o 4 c a r

bon a t o m s , s a i d a l k y l a t e c o n t a i n i n g from 1 t o

1 8

c a r

bon a t o m s , and from about 4 . 5 t o about 20 p a r t s by

w e i g h t o f a l l y l a l c o h o l , t h e t o t a l o f s a i d p a r t s b e i n g 1 0 0 .

A l s o

p r o v i d e d i s

a method f o r c o n t r o l l i n g t h e

v i s c o s i t y

o f s a i d

p i g m e n t i n

a n

a q u e o u s

s l u r r y c o m p r i s i n g a d d i n g

t o s a i d s l u r r y

a n

aqueous

s o l u t i o n

c o n t a i n i n g from

a b o u t t w e nt y t o a b o u t

? f t y

w e i g h t p e r c e n t

p o l y m e r

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

i n a n a m o u n t o f polymer

s o l i d s

o f

up

t o one p e r c e n t

by

w e i g h t o f

p i g m e n t i n t h e

s l u r r y .

DESCRIPTION OF THE

PREFERRED

EMBODIMENTS

The t e r p o l y m e r o f t h i s i n v e n t i o n i s an a l k a l i n e u t r a l

i z e d f r e e r a d i c a l p o l y m e r i z e d

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

a l p h a ,

b e t a

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

a l k y l a t e

o f a n a l p h a ,

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

More

p a r t i c u

l a r l y , t h e a c i d

i s

a l p h a , b e t a u n s a t u r a t e d and c o n t a i n s

3 t o 4 carbon a t o m s . Included

w i t h i n

t h i s group of

a c i d s

a r e

a c r y l i c a c i d ,

m e t h a c r y l i c

a c i d ,

c r o t o n i c

a c i d

a n d

i s o c r o t o n i c a c i d w i t h t h e ? r s t two a c i d s b e i n g t h e p r e

f e r r e d a c i d s . The

amoun t

o f

a c i d

employed i n p r e p a r

i n g t h e terpolymer

o f

t h i s

i n v e n t i o n

on a t o t a l

o f

100

p a r t s

b y

w e i g h t b a s i s w i l l b e

from

a b o u t

60 t o

a b o u t

88

p a r t s a n d ,

mor e p r e f e r a b l y ,

from about 75 t o about 88

p a r t s .

1 5

30

3 5

45

50

55

60

6 5

2

The a l k y l a t e s

c o n t a i n e d

i n

t h e

t e r p o l y m e r

o f t h i s

i n

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

o f

t h e

a c i d s employed h e r e i n a nd

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

a r e

a c r y l i c a n d


a c i d s . The

a l k y l p o r t i o n c o n t a in s from

t o 1 8

c a r b o n

atoms a n d ,

m o r e

p r e f e r a b l y ,

from

1 t o 1 0 carbon atoms

and i n c l u d e s

l i n e a r

o r

n o r m a l

a l k y l ,

b r a n c h e d a l k y l , h y

d r o x y a l k y l

a n d

c y c l o a k l y l .

I l l u s t r a t i v e

o f

t h e

a l k y l

g r o u p s

a r e

m e t h y l ,

h y d r o x y m e t h y l

e t h y l , h y d r o x y e t h y l ,

p r o p y l , i s o p r o p y l ,

b u t y l ,

2 - e t h y l h e x y l , c y c l o h e x y l ,

n o

n y l ,

o c t y l , d o d e c y l

a n d

s t e a r y l .

B a s e d o n

1 0 0

p a r t s t h e

a l k y l a t e d a c i d

i s p r e s e n t i n

t h e

t e r p o l y m e r i n a n amount

from

a b o u t

6

t o a b o u t 2 8 p a r t s

a n d ,

mor e

p r e f e r a b l y ,

from about 6

t o

about

1 5

p a r t s .

The t h i r d

component

o f t h e t e r p o l y m e r

i s

a l l y l a l c o

h o l which i s p r e s e n t , based on 100 p a r t s , i n a n a m o u n t

from

about

4 . 5

p a r t s

t o a b o u t 20 p a r t s and p r e f e r a b l y

from a b o u t 6

t o

a b o u t 1 5 p a r t s b y

w e i g h t .

The

t e r p o l y m e r

i s

p r e p a r e d b y

f r e e r a d i c a l p o l y m e r

i z a t i o n

i n

a n aqueous m e d i um

a t a temperature j u s t

above t h e f r e e z i n g temperature

up t o

t h e re?ux t e m

p e r a t u r e o f

t h e

aqueous

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

mor e

p r a c t i

c a l

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

i n

t h e r a n g e o f

about

50°C.

t o

about 1 0 0 ° C . , a

rang e

o f about 60°C. t o about

9 0 ° C . b e i n g

p a r t i c u l a r l y p r e f e r r e d .

P o l y m e r i z a t i o n

i n

accordance with t h i s

i n v e n t i o n

can be c a r r i e d out a t a t

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

The

p o l y m e r i z a

t i o n

i s

g e n e r a l l y conducted f o r

a

p e r i o d o f

2

t o 8 h o u r s

a nd

a

p e r i o d

o f

3 t o 5

h o u r s

i s

v e r y

s a t i s f a c t o r y . The

f o r e g o i n g

d e t a i l s ,

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

d e t a i l s a r e

w e l l

k n o w n t o t h o s e

s k i l l e d

i n t h e polymer

a r t s

a nd

f o r t h e

s a k e

o f b r e v i t y need n o t b e d i s c u s s e d

f u r t h e r .

I t h a s been

found

p r e f e r a b l e

t o

p r e p a r e an aqueous

s o l u t i o n

o f

a c i d , e s t e r

and

a l c o h o l

and

c h a r g e

t h e s o l u

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

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

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

i n

cremental a d d i t i o n s of an aqueous

s o l u t i o n

o f

t h e

c a t a

l y s t a t

such a

r a t e

s o

a s t o

evenly

maintain

t h e d e s i r e d

r e a c t i o n temperature. Th e

s o l i d s

content o f t h e r e a c

t i o n

system can range

from

about

20

t o about

50

per

c e n t

b y

w e i g h t . T h i r t y p e r c e n t h a s

b e e n

f o u n d

t o

b e

v e r y

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

v i e w o f

l o w enough

v i s c o s i t y

t o

p e r m i t

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

mer o l u t i o n .

Any

o f

t h e compounds k nown t o

g e n e r a t e

f r e e r a d i

c a l s a nd

which

a r e s o l u b l e

a t

e f f e c t i v e concentrations

i n t h e aqueous

p o l y m e r i z a t i o n

medium may b e u s e d a s

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

p r a c t i c i n g

t h i s

i n v e n t i o n .

E x a m p l e s

o f

u s e f u l


c a t a l y s t s

i n c l u d e t h e

a l k a l i m e t a l a n d a mmo n ium p e r s u l f a t e s ,

p e r b o r a t e s , o r

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

p e r o x i d e s

s u c h a s

b e n z o y l p e r o x i d e , cumene

h y d r o p e r o x i d e ,

t e r

t i a r y b u t y l p e r o x i d e , t e r t i a r y

b u t y l p e r b e n z o a t e , a c e t y l

b e n z o y l

p e r o x i d e ,

t e r t i a r y b u t y l p e r a c e t a t e a n d t e r t i a r y

b u t y l p e r o x y i s o b u t y r a t e .

Ammonium, p o t a s s i u m a n d

s o d i u m

p e r - s u l f a t e s

a r e p a r t i c u l a r l y p r e f e r r e d .

O r g a n i c

p e r o x i d e s ma y be u s e d

i n

combination

w i t h

t h e s e

i n o r

g a n i c p e r o x i d ic c a t a l y s t s . A z o n i t r i l e c o m p o u n d s s u c h

a s described i n US.

P a t . No. 2,471,959 can be

used

a l s o a s

a p o l y m e r i z a t i o n

c a t a l y s t

f o r t h e polymers o f

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

G e n e r a l l y ,

t h e

p r o p o r t i o n o f p o l y m e r i z a t i o n

c a t a l y s t

i s

i n

t h e range o f 0 . 1 percent t o 8 . 0 percent based on

t h e

w e i g h t

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

from

1

p e r c e n t

t o

3 p e r c e n t .

The c a t a l y s t

can

a l s o b e a

p e r o x i d i c

c a t a l y s t a c t i v a t e d

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

t o

p r o v i d e a

redox

s y s t e m .

Exa m

p l e s

o f

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

b i



. m z c r w

with .

“t

111C.

*

‘ L A d L t .

d d l a l i r

B C

1 3 , 5 8 ‘ ;

9 * 6 4

3

s u l ? t e s , s u c h a s

sodium

m e t a b i s u l ? t e , s u l ? t c s , hydro

s u l ? t e s

and

t h i o s u l f a t e s . The

redox s y s t e m ma y be f u r

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

e . g . , f e r r o u s i o n s

a t

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

o f t h e

o r d e r

o f

m a g

n i t u d e

o f

s e v e r a l p a r t s

p e r

m i l l i o n ,

o r w i t h

t e r t i a r y

amines

which

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

mixture.

The

p r o p o r t i o n o f

reducing

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

i n

t h e

po

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

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

t o 3 percent based on t h e weight

o f t h e

m o n o m e r s a n d

p r e f e r a b l y i s i n t h e r a n g e o f 0 . 0 2 p e r c e n t t o p e r c e n t

on

t h i s b a s i s . I n

t h e i n o r g a n i c r e d o x

s y s t e m

o f p e r s u l

f a t e

a nd b i s u l ? t e , t h e weight

r a t i o

can v a r y from 1 t o

1 0 p a r t s o f p e r s u l f a t e

p e r p a r t b y w e i g h t o f

b i s u l ? t e .

The


product

h a s

a n a c i d

pH

and can

be

n e u t r a l i z e d

w i t h

a l k a l i n e m a t e r i a l s

such a s a m m o n i a

o r ammonium h y d r o x i d e , mono- a nd d i a l k y l a m i n e s

c o n t a i n i n g t o

6

carbon atoms i n each a l k y l group and

a l k a l i m e t a l h y d r o x i d e s ,

e . g . ,

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

sodium h y d r o x i d e , t h a t

form

w a t e r - s o l u b l e

n e u t r a l i z a

t i o n

p r o d u c t s .

P r e f e r a b l y , t h e

n e u t r a l i z i n g a g e n t

w i l l

b e

a m m o n i a ,

ammonium

h y d r o x i d e ,

p o t a s s i u m h yd r o x i d e

o r sodium

h y d r o x i d e .

The

n e u t r a l i z i n g

a g e n t

i s added

t o t h e polymer s o l u t i o n u n t i l a f i n a l pH f about

7 . 5 t o

a b o u t 8 . 5 i s

o b t a i n e d .

Thus

n e u t r a l i z e d ,

t h e polymer

s o l u t i o n

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

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

s t o r a g e

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

m i n i m i z e d .

The

r e s u l t i n g polymer s o l u t i o n i s a d j u s t e d a s n e c e s

s a r y t o h a v e a polymer t o t a l s o l i d s content of between

a b o u t t w e n t y

a n d

a b o u t

f i f t y

w e i g h t p e r c e n t . The p o l y

m e r

s o l u t i o n

i s

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

i n comparison

t o

t h e

polymer s o l u t i o n s k n ow n

i n

t h e p r i o r a r t which a r e o n l y

e m u l s i o n s . I t i s b e l i e v e d t h a t t h e h i g h

a c i d

c o n t e n t o f

t h e

i n v e n t e d

p o l y m e r s

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

t o

t h i s

c o n d i t i o n .

The

p r o c e s s o f t h e p r e s e n t in v e n t i o n i s a p p l i c a b l e

t o

b o t h i n o r g a n i c pigments and ? l l e r s a s

t h e y a r e

k n ow n

i n i n d u s t r y . For convenience t h e s e

m a t e r i a l s w i l l b e

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

h e r e i n ,

i n c l u d e d but

a r e

not

l i m i t e d t o t i t a n i u m d i o x i d e ,

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

chrome

y e l l o w , z i n c o x i d e ,

t a l c ,

a g a l i t e , p e a r l f i l l e r , b l a n c ? x ,

b a r y t e s ,

c l a y

s u c h a s

c h i n a

c l a y , b a l l c l a y ,

k a o l i n i t e ,

m o n t m o r i l l o n i t e a n d t h e l i k e ,

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

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

i n c l u d e d

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

p i g m e n t s e x e m p l i ? e d b y b a r i u m

l i

t h o l r e d , b e n z i d i n e

orange

and s o

f o r t h .

Aqueous

s l u r r i e s o f pigments a r e used i n

t h e

m a n u

f a c t u r e

o f p a p e r ,

p a i n t ,

i n k

and

t h e

l i k e

t o

i m p a r t

c o l o r ,

body o r

f e e l ,

a n d t o

m o d i f y

t h e s p e c i ? c g r a v i t y o f t h e

p r o d u c t . I n o r d e r t o a v o i d

t h e problem

o f

d i s p e r s i n g t h e

p i g m e n t i n t h e ? n a l p r o d u c t a n d / o r p r o v i d e f o r a u t o

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

o f t h e end p r o d u c t ,

i t i s

o f t e n d e s i r »

a b l e

t o

use t h e

pigment

i n t h e

fo rm

of a n

aqueous

d i s

p e r s i o n . Moreover, i t has been found d e s i r a b l e t o a

h i g h pigment

c o n t e n t , i . e . ,

50 t o

7 5 o r

80

w e i g h t p e r »

c e n t ,

t o

a v o i d

d e a l i n g w i t h e x c e s s i v e am ou nts o f w a t e r .

However,

a t

t h e s e

h i g h

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

o f t e n

b e c o m e s

very

viscous

a n d d i f f i c u l t t o h a n d l e or

m ov e

b y

pumping and

t h e

l i k e .

To a v o i d t h e f o r e g o i n g p r o b l e m s , i t h a s b e e n found

advantageous

t o

add

t o t h e

v a r i o u s s l u r r i e s s m a l l

amounts

o f t h e p r e v i o u s l y d e s c r i b e d a q u e o u s polymer

s o l u t i o n

of


The

a m o u n t t o be added

w i l l

v a r y according t o t h e a m o u n t of pigment t o be d i s

p e r s e d . I t has been found t h a t e v e n

un de r

t h e most a d

v e r s e

c o n d i t i o n

a n

a m o u n t

by w e i g h t o f polymer s o l i d s

i n

t h e polymer

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

one

p e r c e n t o f

t h e p i g

25

30

35

40

50

55

60

65

m e n t p r e s e n t

i s

s u f f i c i e n t t o d i s p e r s e

t h e pigment p r e s

e n t .

Th e

a c t u a l a m o u n t

t o be added,

o f

c o u r s e , w i l l vary

depending on

t h e

source a n d t y p e of pigment a s w e l l a s

t h e amount o f

v i s c o s i t y

r e d u c t i o n

s o u g h t .

The f o l l o w i n g

examples

a r e i n c l u d e d

t o

i l l u s t r a t e

t h e

p r e p a r a t i o n

o f

t h e d i s p e r s a n t s

o f

t h e

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

and t h e

use

t h e r e o f bu t a r e n o t

t o

b e

co nside r e d l i m i t

i n g .

U n l e s s o t h e r w i s e

n o t e d , a l l

p a r t s a r e b y w e i g h t

and

a l l t e m p e r a t u r e s a r e i n d e g r e e s C e n t i g r a d e .

EXAMPLE

A - l i t e r , t h r e e - n e c k ? a s k e q u i p p e d w i t h s t i r r e r , t h e r

mometer, a d d i t i o n f u n n e l s , re?ux

condenser

and h e a t

exchange equipment

was

charged w i t h

236 g .

w a t e r .

A

m i x t u r e

o f

2 0 7 g , a c r y l i c a c i d ,

2 3 g .

b u t y l a c r y l a t e ,

and

1 1 . 5

g .

a l l y l a l c o h o l ( s o l u t i o n

1 )

and 1 1 5

g .

o f a 6

p e r

c e n t

a q u e o u s

p o t a s s i u m

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

1 1 ) were added concurrently t o t h e water a t

80°—85°C.

over

3 1 / 2 h o u r s .

Th e

r e a c t i o n product

was then

n e u t r a l

i z e d w i t h 1 7 5 g . 2 8 p e r c e n t aqueous ammonia. A l e a r

v i s c o u s

s o l u t i o n

was

o b t a i n e d

(Brook?eld

v i s c o s i t y :

1 , 8 0 0

c p s ) .

The p r o d u c t

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

d i s

p e r s a n t .

EXAMPLE

A - l i t e r , t h r e e - n e c k ? a s k

e q u i p p e d

w i t h

s t i r r e r ,

t h e r

mometer,

a d d i t i o n

f u n n e l s ,

re?ux

condenser an d

h e a t

exchange equipment

was

c h a r g e d

w i t h 1 , 2 3 0

g . w a t e r .

A i x t u r e o f 1 , 0 3 5 g . a c r y l i c

a c i d ,

1 1 5 g .

b u t y l

a c r y

l a t e , and 1 5 g . a l l y l a l c o h o l ( s o l u t i o n 1 ) an d 575 g . o f

a 6 p e r c e n t a q u e o u s p o t a s s i u m p e r s u l f a t e s o l u t i o n ( s o

l u t i o n 1 1 ) we r e a d d ed concurrently t o t h e water a t

80°—85°C.

over 3 h o u r s .

The

r e a c t i o n product was t h e n

n e u t r a l i z e d w i t h 1 , 1 5 0 g : 5 0 p e r c e n t a q u e o u s sodium

hydroxide s o l u t i o n .

A

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

a

t o t a l a c t i v e s o l i d s

o f

30

p e r c e n t was o b t a i n e d ,

which

e x h i b i t e d

a

p H o f

7 . 7 , B r o o k f i e l d v i s c o s i t y 3 , 0 4 0 c p s

( S p i n d l e N o . 4 ,

60 r . p . m . ) ,

and a

d e n s i t y

o f 1 . 2 5 . The

p r o d u c t i s

s a t i s f a c t o r y

a s

a

p i g m e n t d i s p e r s a n t .

EXAMPLE

F o l l o w i n g t h e p r o c e d u r e o f Example

a

d i s p e r s a n t

was

prepared b a s e d

on

8 2 p a r t s

o f

a c r y l i c a c i d , 9 p a r t s

o f m e t h y l m e t h a c r y l a t e and

9

p a r t s

o f

a l l y l

a l c o h o l .

The

t o t a l s o l i d s

o f t h e

polymer

s o l u t i o n

was 30

p e r c e n t

a nd

t h e s o l u t i o n was

n e u t r a l i z e d with

a

50 percent

sodium

h y d r o x i d e

s o l u t i o n .

The

s o l u t i o n h a s a v i s c o s i t y o f

2 , 5 6 0

c p s .

A

t a n d a r d

t e s t

p i g m e n t d i s p e r s i o n was

p r e p a r e d b y

m i x i n g i n a

m i x t u r e

o f

s p r a y - d r i e d

c a l c i u m

c a r b o n a t e

(trademark PURECAL 0

“SD”

) and water i n a

70:30

w e i g h t

r a t i o . With

n o

d i s p e r s a n t p r e s e n t t h e

m i x t u r e

wa s

s o s t i f f t h a t i t s v i s c o s i t y could not be determined.

The B r o o k ? e l o ‘ v i s c o s i t y o f a 70 p e r c e n t

b y

w e i g h t

d i s p e r s i o n o f

calcium

c a r b o n a t e

t o

which had

b e e n

added

0 . 7 5

p e r c e n t o f t h e t e r p o l y m e r o f t h i s example

was 2,450 c p s . The

d i s p e r s i o n

i s

s u i ta b l e f o r

p a i n t u s e .

S i m i l a r

r e s u l t s

w i l l

be

o b t a i n e d

wh e n k a o l i n i t e

i s t h e

p i g m e n t .

EXAMPLE

F o l l o w i n g

t h e

p r o c e d u r e

o f

Example

a

d i s p e r s a n t

was

p r e p a r e d

b a s e d

on 64

p a r t s o f a c r y l i c a c i d , 27 p a r t s

o f

h y d r o x y

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

a n d

9 p a r t s o f a l l y l

a l c o h o l .

The polymer s o l u t i o n s o l i d s a nd

n e u t r a l i z a t i o n

was t h e

s a m e

a s

i n Example

3 .

Th e s o l u t i o n v i s c o s i t y

was

2,648

c p s . The

Brook?eld

v i s c o s i t y o f

t h e

s t a n d a r d 70 p e r



3 , 8 8 4 , 9 6 4

5

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

c a r b o n a t e

d e s c r i b e d i n Ex

ample 3 t o which had bee n a dded 0 . 7 5

p e r c e n t

o f t h e

t e r p o l y m e r

d i s p e r s a n t

o f t h i s

e x a m p l e

w a s 2 , 9 5 0

c p s .

S i m i l a r

r e s u l t s

w i l l be o b t a i n e d w h e n t i t a n i u m d i o x

i d e i s

t h e p i g m e n t .

S t i l l o t h e r u s e f u l

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

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

p r e

p a r e d

a s

i n d i c a t e d

i n

Table

I

b e l o w .

5

6

a c i d

c o n t a i n i n g 3 t o 4 c a r b o n a t o m s , s a i d a l k y l a t e

c o n t a i n i n g

from

1 t o

1 8 carbon a t o m s , and

c .

f r o m

a b o u t 4 . 5

t o

a b o u t

2 0 p a r t s b y

w e i g h t o f

a l l y l

a l c o h o l .

t h e

t o t a l o f

s a i d p a r t s

b e i n g

1 0 0 .

2 .

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

o f

c l a i m 1 w h e r e i n t h e a c i d i s

a c r y l i c

a c i d

o r


a c i d .

Table

l

P a r t s

E x a m p l e

P a r t s

A l k y l a t e P a r t s

A l l y l

N e u t r a l i z i n g

N o . A c i d ( a ) A c i d Mon omer ( c ) A l k y l a t e

A l c o h o l

A g e n t

( b )

5 A 80

E

1 5 5 C

6 M 7 5 G 1 0

1 5

C

7 M

82

F 9 9 D

8 A

82

G l ( ) 8 C

( a )

A =

Acrylic

M cth acrylie

( h )

C =

Ammonium

hydroxide. 28 s o l u t i o n

D

= Sodium h y d r o x i d e . 5 0 7 1

. s n l u t i o n

( C ) E =

- e t h _ \ l h e x y l a c r y l a t e

F

uty l

ac

me

( i

=

l h y l

a c r y l a t e

The

f o r e g o i n g

e x a m p l e s and

methods

h a v e

b e e n d e ‘

s c r i b e d i n t h e

f o r e g o i n g s p e c i ? c a t i o n

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

i l l u s t r a t i o n

and

n o t

l i m i t a t i o n .

M a n y o t h e r modi?ca

t i o n s

and r a m i ? c a t i o n s w i l l n a t u r a l l y s u g g e s t them

s e l v e s

t o those

s k i l l e d i n t h e a r t based on t h i s d i s c l o

s u r e . Th e s e are in t e nded t o be c o m p r e h e n d e d a s within

t h e

s c o p e o f


The

e mb o dim e n t s of t h e i n v e n t i o n i n which

a n

e x c l u

s i v e

property

o r p r i v i l e g e i s claimed a r e d e ? n e d a s f o l

l o w s :

1 . A c o m p o s i t i o n f o r c o n t r o l l i n g

t h e

v i s c o s i t y

o f

p i g

ments

i n

a n

aqueous

s l u r r y

c o n s i s t i n g

e s s e n t i a l l y

o f

an

a l k a l i

n e u t r a l i z e d

t e r p o l y m e r

p r o d u c e d

b y

t h e

f r e e

r a d

i c a l p o l y m e r i z a t i o n i n

w a t e r

o f

a . from

about

60 t o

88

p a r t s

by weight

o f

a t

l e a s t one

a l p h a , b e t a

u n s a t u r a t e d c a r b o x y l i c

a c i d

c o n t a i n i n g

3 t o 4 carbon

atoms.

b . from about 6 t o 28 p a r t s by w e i g h t

o f

a t l e a s t one

a l k y l a t e

o f

a n a l p h a , b e t a

u n s a t u r a t e d c a r b o x y l i c

25

3 5

45

55

6 5

3 . The

composition o f

c l a i m

2

wherein t h e a c i d

i s

a c r y l i c a c i d .

4 . The c o m p o s i t i o n o f c l a i m 1 w h e r e i n

t h e a l k y l a t e

i s

a n

a l k y l a c r y l a t e o r

a n a l k y l

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

5 .

The

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

4 w h e r e i n t h e a l k y l a t e

i s m e t h y l

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

6 . The


o f c l a i m 5 w h e r e i n t h e a c i d i s

a c r y l i c a c i d .

7 .

The


o f

c l a i m

1

c o n t a i n i n g

f r o m a b o u t

75 t o

about

88

p a r t s of

a n

a l p h a ,

beta

unsaturated c a r

b o x y l i c

a c i d ,

from

a b o u t 6 t o a b o u t 1 5

p a r t s

o f a n

a l k y

l a t e

o f

an

a l p h a ,

b e t a un s a t u r a t e d

a c i d

and from about

6

t o about 1 5

p a r t s o f a l l y l a l c o h o l .

8 . The c o m p o s i t i o n o f c l a i m 7 c o n t a i n i ng

a b o u t 8 2

p a r t s

a c r y l i c a c i d , a b o u t 9

p a r t s m e t h y l -

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

a n d

a b o u t 9

p a r t s

a l l y l a l c o h o l .

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