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Патент USA US2403734

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July 9, 1946.
‘ 2,403,734
‘Filed Oct. 23, 1945
'FIG. 1 .
HG. 2.
Patented July .9, 1946
Carl J. Malm and Gerard J. Clarke, Rochester,
N. Y., assignors to Eastman Kodak Company,
Rochester, N. Y., a corporation of New Jersey
Application October 23, 1943, Serial No. 507,353
3 Claims. ~ ( CL- 215_-—38)
The- present invention relates to bottle caps or .
closures for containers. More speci?cally, the in
vention relates to a bottle seal formed with inner
and outer shrunk coatings or caps.
mary importance, as will be apparent. An addi-v
tional feature is that in view of the fact that
the outer coating is of a gel type lacquer it is un
a?ected by water or high relative humidities and
will thuseifectively seal the bottle against leakage
of any of the contents which may find its way
The customary way of sealing bottles, and simi
lar containers, is by the use of a shrinkable cap
manufactured from viscose, or gelatin, as is well
known to those skilled in the art. Such caps,
contents against such contamination is of pri
' ‘7 past or through the inner coating.
however, have the disadvantage of being brittle:
The invention has, therefore, as its primary ob
at low relative humidities and low temperatures 10 ject, to provide a seal which not only e?ectively
so that they may crack and break, and thus fail
seals the bottle, but also protects the contents
to provide the desired seal ‘for the container.
thereof from contamination by any detrimental
Furthermore, such caps may be re-hydrated when‘
or undesirable solvent or solvents used in the seal.
subjected or exposedto water, and will swell so
as no longer to tightly grip the bottle to seal the
latter, as is well known.
A further object of the invention is the pro
vision of a bottle seal comprising an outer coat
> ing which is una?ected by water or high relative
humidities and which remains ?exible even at
One way of providing an e?ective seal is to dip
the vstoppered end of the bottle directly into a
bath of gel lacquer of the type which is a ?uid
' above 50° C. and sets; between 10 and, 50° C. to
provide a self-supporting gel. Suchgel type lac
quers‘ are_ described in the application to Fordyce
v8: Clarke No. 370,853, ?led December 19, 1940, now
U. S. Patent 2,350,742,’. issued June 6, 1944, to
which reference may be had for detailed descrip
tion thereof. Caps or coatings formed from these
gel lacquers are vunaffected by water or high rela
tive humidity, and remain ?exible even at low
low temperatures and low reiativehumidities, and
an inner coating which is impermeable to‘ the
20 solvent or solvents of the outer coating so as to
effectively protect the‘ contents of the bottle
against contamination by such solvents.
Another object of the invention is a seal of the
class described which is tough, durable, ?exible
25 and highly effective in use.
temperatures and low relative humidities, and
- To these and other ends, the invention resides
' in certain improvements and combination of
parts, all as will-be hereinafter more fully de
scribed, the novel features being pointed out in
-thus provide a seal which will not swell or crack 30 the claims at the end of the speci?cation.
after shrinking into position. One disadvantage,
In the drawing:
however, of a seal of this type is that whenever
the bottle is stoppered with a material which isv
susceptible to the solvent or solvents in the gel
Fig. 1 is a view of a portion of a bottle showing
- lacquer solution, there is danger of the solvent 35
or solvents of the lacquer getting throughthe
stopper and contaminating the contents of the
bottle, the disadvantage of which ‘will be readily
' obvious.
the inner or initial protective coating applied,
thereto, and
Fig. 2 is a view similar to Fig. 1 showing the
‘relation of the two coatings which seal the bottle
and effectively protect the contents vthereof
against contamination, the coatings being in sec
, It has been found thatthe danger of such con
tamination can ‘be e?ectively avoided by first ap- _
Similar reference numerals throughout
various views indicate the same part,
plying to the exposed part of the stopper,'a,n in
itial or inner coating which is unaffected by the
solvent or solvents of the lacquer. After the ap
ing a neck 12 and a closure member in the form
of a cork or rubber stopper 1 3. The inner sealing
The drawing shows a portion of a bottle I I hav
plication of the initial protective coating, the
stoppered end of the bottle may be then dipped
into a bath of the gel lacquer. Upon withdrawal
of the bottle from the bath, the lacquer sets to
portion of the neck II, as shown in the drawing.
After the initial coating has been applied, it will
a gel to provide ‘a second or outer coating-which
shrink, in a manner well known in the art, to
coating II is first‘ applied to the exposedpart of '
the stopper l3, and. ifde'sired, ‘to the adjacent
overlies the ?rst or inner; coating, and'which, 50 e'il'ectively seal the stopper and the top of the
upon shrinkage, provides a tough excellent seal,
bottle, as clearly ‘shown in Fig. 1.~ This-initial
‘ ,while the inner coating effectively prevents the
coating I! is of a'material which is una?ected by ~
solvent or solvents ‘of the gel-lacquer from pene-v _
the solvent or solvent vcombinations of the gel
trating the stopper and contaminating the con
lacquer coating to belatér described. Water so- -
tents of the bottle. This protection of thebottle' 55 lutions otpolyvinyl alcohol or gelatin or a water
tents of. the bottle. The material of the inner
coating M‘ is selected from the previously men
tioned group to provide a sub-layer which is un
affected by the solvents of the outer coating, and
alcohol solution of tar hydrolized cellulose ace
tate, such as one having an acetyl content of less
than 30% have been found to be admirably suited
for use for the inner or initial coating H. In
order that this inner coating l4 may withstand
will thus seal out or prevent the passage of such
solvents through the stopper and to the bottle
low temperatures without making the coating
contents. This inner coating thus protects the
stopper and the bottle contents against such con
brittle, it is advisable to plasticize the inner or
sub-coating with a water soluble plasticizer such
as glycerine or a glycol.
tamination. This feature is of primary and para
mount importance, as will be readily appreciated.
The outer coating IE will, on the other hand, re
' the stoppered end of the bottle is then dipped into
main ?exible, as mentioned above, and will not
a solution of a gel lacquer to provide an outer
crack or chip off and will thus e?ectively protect
protective coating l5. Such a gel lacquer com
the inner more brittle coating it. Of secondary
prises a cellulose mixed organic acid ester dis
solved in a suitable organic solvent or solvent 15 importance, the outer coating, due to the fact that
it is unaffected by water, will seal the bottle
combination, and may ‘be one of the lacquers de
against any leakage which might get past or
scribed in the above-mentioned applications and
through the inner coating H. The two coatings
shown in the following list. These gel lacquer so_
thus cooperate to provide a structure which both
lutions are ?uid above 50° C., but between 10 and
50° C. set to form a self-supporting gel contain 20 seals the bottle, and also protects the contents
After the inner coating 14 has been dried or set,
ins most, or at least a large part, of the original
solvent or solvents‘. As these solvents evaporate,
the gel shrinks so that the coating l5 formed
therefrom will tightly grip and seal theinner
coating 14, asclearly shown in Fig. 2. Coatings
thereof against contamination of the solvents or
the outer coating l5.
_While coatings l4 and I5 have been described as
being applied by dipping the stoppered end of the
bottle in an appropriate solution, it'is apparent
that these coatings may be formed of‘ separate
pre-shaped caps which are applied to the bottle,
and which, on drying‘, shrink to provide the de
sired seal. The method of forming caps from vis
made from such gel lacquers are una?ected by‘
water or high relative humidities and remain ?ex
ible even at low temperatures and low relative hu
midities and thus overcome the brittle feature of
prior caps or coatings. While any of the gel 30 cose~ or gelatine are well known to those in the
art. An improved type of separate pre-shaped
lacquer solutions listed below are suitable for the
cap composed of a gel lacquer to provide the
coating IS, an outstandingly satisfactory solu
outer coating. l5 may be formed in the manner
tion is that composed of cellulose acetate butyrate'
shown and described in applicant’s copending ap
containing about 37% butyryl and about 13% ace
tyl dissolved in a solvent composed of 20 to 30% 85 plication Number 507,352 filed October 23, 1943.
While certain embodiments of the invention
isopropyl alcohol and '70 to 80% _xylene.
Propionyl Butyryl
Ratio of
solvelriiés to
Perl cent
Per cent
Per cent
707 f 01 llFI'l?
I ' 26 ---- -_----- {323; iso‘propyl alcohol _____________________ .. }
__ n
13, 5’ __________ _.
n mine
iso~ ro
80% "than?!
1 alcohol _____________________ --
{33% is?epmpyl who, ________
__________ __
33 -------- -- $37; irso-propyl alcohol _____________________ -.
10% dioctyl Panama
11 I101‘!!!
n norm
---------- --
---------- --
---------- --
tert-amyl alcoh
' 5'1
iso—propy' alcohol
xy ene ___________ -.
85 o xylen ........... _.
--------------------- --
xy e
.-_. ...... -_
l..- - .
a iso-propy alcohol"
isol-propyl alcoho ..
3001101 mixture of 3-5 carbon atoms--_._
40,, butyl acetate-.__
. -_
c a iso-propyl alcohol
7oxylene .................... .i . _ . .
......... --
---------- --
95 , xylene ......... -.
ene ........................... ._
l5 ,, isol-propyl alcohoL
27‘ 6
---------- --
t l I]
()ziiate.r p enyl
5‘ 1
{15% iso‘propyl alcohoL-
20- 5 ---------- --
{90 ,, trichloroethylene. __
1 o ethylene dichloride-
---------- --
16' 5
D tert-butyl alcohol ........ __
{50 a tnchlorethylene._-_
1 Bolvesso #2 is a mixture of 90% xylenes and 10% other hydrocarbons.
The percentages of acetyl, 'propionyl and bu
tyryl in the above table are the percentages of
these substances in the esters. The heading
“ratio of solvents to solids” represents the ratio of
have been disclosed it is to be understood that the
inventive idea may be carried out in a number of
ways.. This application is, therefore, not to be
limited to the precise details described but is in
the solvents to the solids in the mixture.
70 tended to cover all variations and modi?cations
While such an’ outer vcoating l5 provides a
thereof falling within the scope of the appended
tough, ?exible protective cover for the inner coat
ins N, the solvents of the coating l5 are unable
We claim:
to penetrate the inner coating and work their way
1. A container closure cap or the type adapted
through the stopper It to contaminate, the con- .18 to shrink by loss or solvents comprising an inner
layer 0! polyvinyl alcohol. and an outer layer _’ to shrink'byloss oi’ "solvents comprising an inner
composed of cellulose lcetste butyrate.
2. A container closure cap ofthe type adapted "
layer or a polyvinyl aIcohoLzand- an outer layer
composed of cellulose acetate butymte‘ containing .
- to shrink by loss of solvents comprising an inner
' approximately 37% butyryl and approximately
layer of polyvinyl alcohol, and an outer layer I 13% acetyl dissolved in a solvent composed} or 20
composed of cellulose acetate butyrate dissolved
to 30% iso-propyi slcohol and 70 to 80% xylene.
in a solvent to form a solution which is adapted
s. A container closure cap or the ‘type adapted
amp a.
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