United States Patent (19) [11] 3,755,241

Brady (45) Aug. 28, 1973

54). POTTING COMPOUND AND METHOD OF Damusis, "Sealants,' Reinhold Pub., New York, 1967,
POTTING pages 164-165.
75 Inventor: Thomas G. Brady, Oneonta, N.Y. Meals & Lewis, "Silicones,' Reinhold, New York,
(73) Assignee: The Bendix Corporation, Sidney, 1959, pages 192-197
N.Y. Sinclair, "Product Data Bulletin No. 505, Poly B-D
Liquid Resins," 1965, pages cover and 1.
22 Filed: June 30, 1971
(21) Appl. No.: 158,606 Primary Examiner-Morris Liebman
Assistant Examiner-P. R. Michl
Related U.S. Application Data Attorney-Raymond J. Eixler and William S.
63 Continuation-in-part of Ser. No. 850,632, Aug. 15, Thompson
1969, abandoned.
57 ABSTRACT
52 U.S. C. 260/33.6 U3, 260/37 N, 260/859 R, A potting compound is used to embed delicate or coor
264/272, 260/4.5 R dinated instruments within a casing to protect them
5ll Int. Cl........................ C08g 51/14, C08g 51/28
58) Field of Search ..................... 260/859, 33.6 UB from shock or vibration which would destroy them or
derange them. The essential ingredients of the potting
56) References Cited compound are dihydroxypolybutadiene, an extender
UNITED STATES PATENTS oil, a microfine polypropylene powder, and an organic
diisocyanate. The resulting compound is presumed to
3,637,558 111972 Verdol.................................. 260/28 have an oil-modified polyurethane structure as a matrix
3,358,052 12/1967 Archer................................ 260/859 enclosing the polypropylene powder as an integrated,
3,427,366 2/1969 Verdol.................................... 260/5 dispersed phase. The compound has high adhesion to
3,283,036 1 1/1966 Larson................................ 260/897 practically everything used in potting, requires no in
OTHER PUBLICATIONS terlayer, is flexible at -65. F. and is heat resistant for
Ser. No. 465,161, p. 1-20, 25-31 (mentioned in U.S. short periods at 260° F.
Patent No. 3,637,558) 10 Claims, No Drawings
 3,755,241
2
POTTING COMPOUND AND METHOD OF ferred mode without detracting from the general use
POTTING fulness of mineral oils lighter than kerosene. The vis
This application is a continuation in part of Ser. No. cosity of one of the best of these oils at 100 F. is 180
850,632, filed Aug. 15, 1969 and now abandoned, and (sus), and at 210 F., 42. Its specific gravity 60/60 is
is entitled to its priority. .09024. It has a flash point COC of 340 and carbon
This invention relates to potting compounds. Potting analysis shows aromatic hydrocarbons 0%, naphthenic
compounds are shock-proof beds for delicate or coor hydrocarbons 57%, and paraffin hydrocarbons 43% by
dinated instruments. Their function is to furnish a pro weight. Other oils of these classes are numerous and
tective support for objects which may be destroyed, have been described in the literature. The polybutadi
dismantled, or deranged by vibration or shock. An ex 10 enes form a solution with this oil in which the polypro
ample of such is a blaster. A blaster is a capacitor dis pylene powder is easily and uniformly dispersed by stir
charge apparatus for generating blasting current. The ring. The more useful oil-polybutadiene solutions have
blaster shell contains electrical components such as ca a density reasonably approximating that of the polypro
pacitors; the potting is done by mounting the electrical pylene powder, but mixtures more remote in density
components in the shell and enclosing them by filling 15 are also useful provided the potting follows the mixing
the shell with a fluid potting compound, which is cured before substantial decantation occurs. All problems of
at room temperature or by heat, according to composi this type are averted by mixing the ingredients just be
tion, after the potting has been compositions of this in fore potting, as stratification of the polypropylene
vention, and a cure at room temperature for another. through the oil is slow in most cases and is practically
Our heat-cured potting compound will cure by itself at 20 nonexistent when the specific gravities of the solution
room temperature if left to stand long enough, but and the polypropylene are similar. (3) An organic di
cures faster at elevated temperature. Our new com isocyanate, preferably tolylene diisocyanate. (4) Poly
pounds will not revert to liquid, as some prior potting propylene powder filler in particle sizes about 30 to
compounds do. 100 microns. (5) Preferably but not necessarily an anti
Previous compounds required that the pot be coated 25 oxidant.
with an adhesive such as rubber, to make the potting The polybutadienes of the invention are homopoly
compound adhere to the shell or container but in our mers with hydroxyl end groups which fall within the
invention the shell can be made of any material of suffi formula
H
(, , , \ (
|W - JV) \ I).
cient strength, e.g., concrete, steel, or plastic and re in which n are repeating molecular units, n being 44 to
quires no adhesive coat, as the new potting compounds 75, those in which n is 65 to 75 having a viscosity at 30
adhere very well to all such materials. C. about 200 poises, and those in which n is 44 to 60
Among potting compounds there are several desider having a viscosity about 50 poises. For many uses the
ata, important among which are low density to make polymers of higher viscosity are preferred, but in some
them light, fineness to enable large quantities to be in 40 cases those of lower viscosity are highly satisfactory.
corporated, compatibility with the potted objects, high Among the extender oils useful in the process is a
elongation, flexibility at all working temperatures, par naphthenic process oil known in the trade as Tufflo
ticularly below zero, and resistance to disintegration at 6024, but its use, while satisfactory, does not minimize
elevated temperatures. There are large numbers of res 45 the satisfactory nature of other oils of the class de
inous compounds which might be tried in such compo scribed above.
sitions but only a few have been discovered which are Polypropylene powder can be purchased on the mar
reasonably satisfactory. ket in fine particle sizes, for instance in sizes from 75
The major object of the present invention is to pres to 100 microns, and gives satisfactory results. The ad
ent to industry a group of potting compounds which SO vantages which spring from its use are numerous: the
meet all these requirements and which have superior product made by using it is strong, resilient light, inter
qualities in some of them, particularly that certain of nally cohesive, externally adhesive, readily molded or
them can be cured rapidly and satisfactorily at room shaped, not rigid, not abrasive, of long life in mild and
temperature. heavy use, and easy to work with.
The objects are accomplished, generally speaking by 55 Tolylene diisocyanate is on the market in technical
a group of potting compounds having the composition: grades of satisfactory quality.
(l) hydroxy-terminated homopolymeric polybutadiene Various antioxidants are known for use in com
having two terminal hydroxy groups. This material is pounds of such resinous type, among them one which
not adequate in itself. (2) Extender oil. This material is unusually satisfactory and which is called 4-4" methy
is insufficient in itself but is essential to the invention. lene bis (2,6 ditert-butyl phenol).
The extender oils, herein so called, are true oils, for in 60 An antifoaming agent is often useful, those of silicone
stance paraffinic, cycloparaffinic, aliphatic, cycloali base being sometimes of superior effect, e.g. Dow Cor
phatic, aromatic oils which form solutions with the ning Antifoam A.
polybutadiene of our invention, and of which mineral The usual accelerators are useful for the cure system
oils lighter than kerosene fractions are generally indi 65 but dibutyl tin dilaurate has certain advantages.
cated, naphthenic and paraffinic oils being preferred. The ingredients are mixed by standard techniques,
Naphthenic type oils and paraffinic type oils, and com the isocyanate reacts with the hydroxy-terminated
bined naphthenic-paraffinic oils are given as a pre homopolymeric polybutadiene, producing something
 3,755,241
3 4.
structurally similar to the urethanes as a matrix within time and that different curing temperatures have an ef
which are the microfine particles of solid polypropyl fect not only on time but on product quality.
ene as a dispersed phase. Mixing is at room tempera The reaction is self-starting and proceeds with a ve
ture in most cases. locity related to the temperature of the ingredients. In
EXAMPLE 1. general, satisfactory results are attained when the hy
droxyl and isocyanate groups appear in proportions
A specific example of a low molecular weight, heat which are reactive, for instance mole for mole.
cured potting compound includes 100 parts by weight In many prior instances potting compounds have not
dihydroxy-polybutadiene; 50 parts by weight oil lighter been adherent, or have had only slight adherence, to
than kerosene, as above; 30 parts by weight microfine 10 some fillers and to some of the cases and containers
polypropylene powder (35 microns for example); 7 used in potting, which required that some mutually ad
parts by weight tolylene diisocyanate, 0.5 parts by herent interlayer be interposed, but in the present in
weight antioxidant. vention the compound has firm adhesion to practically
The ioscyanates useful in this reaction are organic di anything used in potting, eliminating the need for inter
isocyanates, listings of which will be found in published 15 COats.
works and patents relating to the preparation of poly The cured compound in the example above has low
urethanes. The literature, e.g., Hostettler U.S. Pat. No. density (about -- 0.9), which is quite important for uses
3,169,945, describes many such isocyanates and tech requiring strength and light weight; it has excellent ad
niques by which they may be transformed to suitable hesion; is flexible even at-65° F., which is most impor
urethanes. Tolylene diisocyanate is preferred but it is 20 tant in polar and high elevational work; and it exceeds
representative of a large class, not exclusive. In our all normal requirements in formal uses.
present example the ratio of -NCO to OH groups was EXAMPLE 2
about 1-1, the weight ratio of polybutadiene to tolylene
diisocyanate being about 93 parts by weight to 7 parts 100 parts by weight polybutadiene of the above for
by weight. 25 mula, in which n is in the range 65 to 75, 70 parts by
The polybutadiene has a viscosity from about 200 to weight extender oil as above, 7 parts by weight diisocy
about 50 at 30° C. In those viscosities it mixes and anate, 75 parts by weight polypropylene powder in
pours well. The diisocyanate in the above example was sizes of 75 to 100 microns, .5 parts by weight dibutyl
about 80%. 2-4 and 20% 2-6, but it can be pure, or a tin dilaurate, 1 part by weight 4,4'-methylene bis (2,6
mixture of such diisocyanates, changes in the ones 30 ditert-butylphenol), and 0.1 part by weight of silicone
chosen producing some variation in properties in the base antifoaming agent were mixed by dividing them
product. into two groups of which one contained the resin base
in forming the blaster any suitable container is used, and the other the catalyst. The polybutadiene, part of
steel, concrete, plastic or wood for example, and the 35 the polypropylene powder, antioxidant, antifoam, part
elements to be mounted are supported in their correct of the oil, went into the first stirred mixing pot, the sec
positions. The potting compound is then made by mix ond receiving the catalyst; the diisocyanate, the accel
ing the ingredients listed above at an appropriate tem erator, and the remainder of the oil. The partition pro
perature, for instance room temperature, or in the case vided an equal volume ratio of base to catalyst.
of more viscous oils enough higher to produce good flu 40 The polybutadiene, oil, antioxidant, and antifoam
idity, e.g., 30°–40°C. The preferred potting compound were mixed in a clean dry vessel and blended well be
pours well at room temperature, and others pour better fore adding the filler. Polypropylene powder was then
at temperatures up to 150° C., so that the temperature added and blended in. Evacuation was employed to re
will be selected according to good pouring viscosity. move entrained air. This constituted the base compo
In many instances the presence of bubbles in the set nent, which could be stored for days in sealed contain
potting compound is not objectionable, but in other 45 S.
cases where a dense body is desired the blaster may be The catalyst components were mixed in a dry, clean
kept under vacuum, for instance at a tank pressure of mixing vessel, oil diisocyanate, and accelerator first,
5 Torr abs., to assist in the extraction of bubbles. then with added polypropylene powder until a uniform
After the potting the potted apparatus will be cured mixture was produced. This component can also be
in the air at room temperature or at elevated tempera 50 stored for days in sealed containers without degrada
ture, e.g., in a circulating air oven. Curing time is re tion.
lated to temperature, being the shorter as the tempera In one commercial operation, the resin mixture con
ture is higher. A typical cure is 12-16 hours at tained 100 parts by weight polybutadiene of n 65 to 75,
200-225 F. Curing may be in stages, a first cure at low 10 parts by weight oil, 25 parts by weight polypropyl
temperature followed by a second at high temperature, 55 ene powder, 1 part by weight antioxidant, and 0.1 part
for instance up to 300 F. The cure will be stopped be antifoam agent. The catalyst component contained 60
fore degradation of the product sets in; degradation will parts by weight oil, 7 parts by weight tolylene diisocya
result from the use of a temperature that is too high or nate, 0.5 parts by weight dibutyl tin dilaurate, and 50
from a cure that is too long. The limiting factors will be 60 parts by weight polypropylene powser. The two blends
determined for each compound by test and observa were stored in separate sealed containers and used as
tion. For the mode described above, 200 to 225 F. for needed for potting blasters and capacitors.
12 to 16 hours is satisfactory. After cure, the potting In potting, the parts were mounted in correct position
compound will operate at 240° F. for extended periods in the shell, measured quantities of the two components
without degradation and will withstand 250' to 265 F. 65 were mixed and poured into the shell to cover the in
for shorter periods. Cooling may be in the air or forced struments, in general conformity to the directions
by refrigeration. It is to be understood that curing will found elsewhere herein. The base component in one
occur at room temperature over inordinate periods of commercial operation was mixed 100 parts by weight
 3,755,241
5 6
with 83 parts by weight of the catalyst component. 2. A composition according to claim 1 in which n is
From time of pouring into the shell to gelling was about from 44 to 60, the viscosity is not substantially over 100
10 minutes. The temperature employed for gelling was poises at 30° C., and the diisocyanate is from the class
86 F. of tolylene diisocyanates.
Inert ingredients such as pigments can also be used. 3. A composition according to claim 1 in which n is
The techniques of mixing and potting are known to from 65 to 75, the viscosity is substantially above 100
the art: Ordinary rotary mixers are satisfactory, the in poises and not substantially more than 200 poises at 30
gredients may be added in any order, air bubbles may C., and the diisocyanate is from the class of tolylene di
be eliminated under vacuum when their presente is un isocyanates.
desirable, the potting may take place under vacuum to 10 4. A composition according to claim 1 in which the
increase the speed of the potting and potting may be diisocyanate is from the class of tolylene diisocyanates,
assisted by vibration. the extender oil is from the class of mineral oils lighter
While the potting of blasters constitutes the specific than kerosene fractions, naphthenic oils, and paraffin
example of this specification the compounds may be oils.
used as sound and heat insulation, and may be molded 15 5. A composition according to claim 4 including an
and hardened to form protective nests for apparatus in antioxidant, a silicone base antifoam, and dibutyl tin
shipment. Many other uses will occur to those skilled dilaurate as the accelerator.
in the potting art. 6. A potting composition according to claim 1 in
The use of catalysts to speed the reaction of isocya which there are 100 parts by weight of the homopolym
nates with polyols is known but it is preferred not to use 20 eric butadiene, 50 to 70 parts by weight of the extender
catalysts in this invention because they reduce pot life. oil, and about 7 parts by weight of the diisocyanate and
The novel potting compounds have high elongation 30 to 75 parts by weight of polypropylene powder.
and are resistant to major shock, and to low and high 7. A potting composition according to claim 1 in
frequency vibration over extended periods of time. It is which there are 100 parts by weight of dihydrox
satisfactory for light instruments and for mounting mas 25 ypolybutadiene, 50 parts by weight of an extender oil
sive pieces. lighter than kerosene, about 7 parts by weight of tolyl
Another advantage of this invention is somewhat eso ene diisocyanate and 30 parts by weight of the polypro
teric and somewhat surprising. The microfine polypro pylene powder.
pylene particles do not interfere with the low intermo 8. A potting composition according to claim 1 in
lecular forces existing between the polybutadiene ure 30 which a solution of 100 parts by weight of homopolym
thane molecules, but appear to increase the bonding eric butadiene and 10 parts by weight of extender oil
force. having 25 parts by weight of polypropylene powder dis
As many apparently widely different embodiments of persed therein, is blended with a solution of 7 parts by
the present invention may be made without departing weight of tolylene diisocyanate in 60 parts of extender
from the spirit and scope thereof, it is to be understood 35 oil having 50 parts by weight of polypropylene powder
that the invention is not limited to the specific embodi dispersed therein to form the potting composition.
nents. 9. A pourable potting composition comprising a
What is claimed is: hydroxyl-terminated homopolymeric butadiene having
1. A pourable potting composition comprising a the formula
H. H.

\(, , - , J.W.
y_1, c)().
--" h ()
i).
hydroxyl-terminated homopolymeric butadiene having in which n is from 44 to 75 repeating molecular units,
the formula having a nominal viscosity of about 50 to about 200

no ( ) (,H. b ) ( . . ) on
in which n is from 44 to 75 repeating molecular units, poises, in solution in an extender oil which forms a so
having a nominal viscosity of about 50 to about 200 55 lution with said homopolymeric butadiene, an organic
poises, in solution in an extender oil which forms a so diisocyanate dissolved in said extender oil, microfine
lution with said homopolymeric butadiene, an organic polypropylene powder having a size from about 30 mi
diisocyanate dissolved in said extender oil, microfine crons to about 100 microns dispersed in said extender
polypropylene powder having a size from about 30 mi oil and being insoluble in said oil, and an accelerator,
crons to about 100 microns dispersed in said extender 60 the proportions of said homopolymeric butadiene, or
oil and being insoluble in said oil, and an accelerator, ganic diisocyanate and extender oil being such that
the proportions of said homopolymeric butadiene, or there are 100 parts by weight of homopolymeric buta
ganic diisocyanate and extender oil being such that the diene, 50 to 70 parts by weight extender oil, 7 parts by
mixture is pourable and self-curing to a solid state and weight diisocyanate, and 75 parts by weight polypro
the weight of the solid polypropylene being at least 30 65 pylene powder.
percent by weight of the homopolymeric butadiene and 10. A composition according to claim 9 in which in of
not substantially exceeding 75 percent of the weight of the polybutadiene is between 65 and 75.
the butadiene. k xk k sk x