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Патент USA US2411773

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“Patented Nov. 26, 1946 '
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UNITED‘ STATES PATENT OFFICE CURING NEOPRENE
Byron W. Bender, Cupsaw Lake, N. 1., assignor to
United States Rubber Company, New York,
N. _Y., a corporation of New Jersey
No Drawing. Application April 5, 1945,
Serial No. 586,817
,
2 Claims. (on, 260-92.?)
1
I
l
.
2
This invention relates to improvements in cur- Y
Tau I
ing neoprene (polychloroprene) .
I have found that the curing rate of neoprene
may be increased by incorporating with it, ‘prior
A
to cure, a small amount of a 3,3,3’,3'-tetraalkyl1,1'-spirobisindane-5,5’,6,6'-tetrol, as an accel-
5
a
,,
Ef?ii?t‘é’?fi'if..‘X‘Z?F..’_:i1:3:::::::::::::::::::::::: “f3 “f3
junction with a curing agent such as a metal
ggegggggggggggg-
oxide, known for the purpose, e. g., zinc oxide,
Wood rosin ....... -_
_
p
B
' -
H
erator of'the cure. It is used preferably in oon_
1
Mill mixed polychloroprene
.
--------- --
1°
1°
_
12
5
12
_
,
--
5
. magnesium
oxide, marge, etc.
10 {tear/‘stanzatafaeaammmeal
2
My accelerator avoids the disadvantages of ac‘
~
_
' ' '
"""" "
celerators such as catechol, resorcinol, and hydro-
. Y
,
Tests on presswured slabs
quinone, which are water-soluble and cause un-
'
desirable discoloration of the polychloroprene 15
stock.’
-
,
A
3
'
An accelerator ‘of the class above referred to
Minutes 0mm
.
may .be prepared by reacting 3 mols of acetone
Elongation
Tame
with 2 mols of catechol, and by a method such
'
“break
-
-
"""""""""" "
P" “51.5,,
P'1f'73b
’ t
“
The accelerator may be used for accelerating
‘ the cure of any form 01' polychloroprene, milled
>
’
2698
’
The faster rate of cure of compound B containing
25 si niii
g ‘ y n8
The
_
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hi
,
e
Eh I
m
odmus.
TAB!" n
Polychlomprene latex
K“) Wmmut ‘Zinc Oxide]
ucts (those derived directly from a dispersion 30
\
containing the neoprene) in which a quick cure »
desired,
e.
g.,
Q)
.
my accelerator is shown by its lower elongation,
accelerator 'is particularly useful in latex prodare
P" “M260
'
based on the weight of the neoprene, range from
modulus
“break
$3 -----------
The proportion of the accelerator may be var-
or reclaimed, in solution, or in dispersion.
Elongation
i
ied’; generally useful proportions, by weight
0.1% to2%.
-
Tepsue
V
as stated by Baker 8: McGowan, Journal Chemi- 20 7 a, '60, ____________ __ P
cal Society '(1938), pages 347-353.
and high
i
C
latex
'
The following examples illustrate the inven-
,,
,,
D
.
l‘o'rai solids ..... -; ..................... _i-.'-'_-.per c6155: "35' is
v tion, the parts being by weight:
Tests on ?lms
Modulus
'
Modulus
?gmlggu?e
Tensile El?n“?
on
300% 500%
60 at 160° F.
.
-
P. a. 5.
Tensile
'
300%
500%
Per cent
Elon
dog‘
at break
P. a. l.
Per cent
1i3,_...___-
90
160
850
1,160
90
170
1,341)
30 at 250° F--.
100
100
2, 100
1,140
90
150
2,100
1,080
' 60 ........... -- .
90
90
2,500
1,180
80
160
1,900
1,030
110
110
2, 600
1, 140
90
170
2, 200
1, 040
120.. ._ __ ..... __
1,130
2,411,773
_
3
.
E
,
1t ( T
Polychlmpme a 8K “ We
and my accelerator is indicated.
F
-
6,015 °,----' -------- --,-; -----------
‘tii’nitiiié‘f’i‘if‘fi‘it‘.ji’ffi‘i‘ff‘i‘fi‘i‘ff‘isfi‘i‘i23%;;
.
The test data show that the above tetrol is a
571'") 8°“d 5 -------------- -- m m
é’iii?t?éltt‘ttfff?..... -.::-__._.-__.-__:::::: ..... _.:-I
4
highest modulus stock, the use of both zinc omde
[(0) With zinc oxide]
5
wflery
effective eiclcelerator in both milled and latex
orms o polyc oroprene, Asa matter of fact, 11;
Inuit be useid win‘; precuring
caution inof milled
stocks
to
the stock
before
-
avo d scorch me an
114g
molding. In this respect, its action may be com
’
pared to that of the soecalled ultra accelerators
Tests on ?lms
Modulus
35:33:29
_
300% 500%
an a l60°-F.
plus._..__._
30at250°
Modulus
Tensile E3358
100
110
'
_
Tensile E?onga
at break 300% 500%
160
1230
P. 0.1.
1,400
2,300
Percent
1,140
1,030
210
280
300
380
at break
13.0. i.
1,900
2,600
Percent
030
730
so ___________ -_
250
330
2,500
820
380
400
2,500
640
1a) .......... __
300'
400
2,300
710
480
630
2,500
600
A"
Dimethylamine oleate was added as 10% solunon,
_
Sodium alginate was added as 2% solution.
The test ?lms were poured on glass plates and
in rubber. Because of this tendency to scorch
milled stocks; it will be of the greatest value in
25 polychloroprene latex, Just as the rubber “ultra”
» accelerators may be used more safely in latex
air-dried 16 hours at 70° F., then heated for one
than in milled stocks.
hour at 160° F., then further cured by heating for
various periods at 250°. F., as indicated.
Having thus described my invention, what I
claim and desire to protect by Letters Patent ls:
'
'
It may be seen from the above data for com- 30
1. A method of accelerating the cure of poly
pounds C and D that in the absence of zinc oxide ~ chloroprene which comprises incorporating
my accelerator has only a very slight e?ectlon
therein, priorto cure, a small amount of 3,3,3',3’
modulus-and breaking elongations and films from
tetramethyl-1,1'-spirobisindane-5,5’,6,6’-tetro1.
both of these compounds have low modulus and
2. A method of accelerating the cure of poly
high breaking elongation. However, in the pres- 35 chloroprene which comprises incorporating there
ence of zinc oxide, the data for compounds E and
in, prior to cure, a small amount of 3,3333’
-F Show that my amelemtor has a, marked ac- I
tetramethyl-1,1'-spirobisindane - 5,5',6,6' -tetrol,
celerating in?uence and causes appreciable rise
and Zinc Oxide_
in modulus and decrease in breaking elongation
‘
BYRON W.'BENDER.
for a given time of cure. Thus, to ‘obtain the 40
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