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Патент USA US3085898

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United States Patent 0 F‘" Ce
1
3,085,890
Patented Apr. 16, 1963‘
2
lea?ng of lea?ng metallic pigments in admixture with
3,035,890
LEAFING ALUMENUM PAINT MANUFACTURE
Rolf Relies, New Kensington, lPa., assignor to Aluminum
tiompany of America, Pittsburgh, Pa, a corporation
such modi?ed vehicles. The particular vehicles contem
plated herein are those normally having acid numbers
_
Within the range 5 to 32, and the amines found to be
preferred are de?nable in terms of at least one of the
No Drawing. Filed Dec. 3, 1958, Ser. No. 777,843
26 Claims. (Cl. 105-241)
ethylene diamine and 1.3 \diamino propanol in that the
This invention relates generally to the manufacture
vehicles under consideration at temperatures as low as
of Pennsylvania
group consisting of tetraethylene pentamine, piperidine,
named amines are reactive with the organic acids in the
of paints and coating formulations and is more particu 10 25° C., or room temperature.
Typical examples of the organic acids common to the
ployed in the manufacture of readyamixed lea?ng alu~
vehicles regularly manufactured and marketed, and found
cminum paints and coating formulations.
to be destructive of the lea?ng properties of lea?ng grade
‘It is a recognized fact that many vehicles employed in
vmetallic ?akes, are the mono- and poly-basic acids,
the manufacture of ready-mixed paints, and similar coat 15 benzoic, abietic, phthalic, isophthalic, fumaric, maleic and
larly addressed to the treatment of acidic vehicles em
ing formulations, contain organic acids which prevent
their use in admixture with lea?ng grade metallic pig
ments, such as lea?ng aluminum ?akes, because ‘of the
sebacic.
.
No attempt is made to explain the exact chemistry in
volved in the chemical reaction which accounts for neu
leaf-destroying propensities of the acidic ‘components of
tralization of the organic acidic propensities or qualities
the vehicles. Probably the greatest offender in this re 20 of the vehicles destructive of leaf on admixture with leaf
spect is the widely growing class of synthetic alkyd resin
ing grade irnetallic pigments, but it has been established
vehicles, which, so far as metallic pigmentation is con
1n an extensive test program that the addition of one or
cerned, have only been capable of use in ready~mixed form.
more of the above-stated amines to such vehicles, prior
in admixture with non-lea?ng grade metallic pigments.
to the addition thereto of lea?ng grade metallic pigments,
The synthetic alkyd resin vehicles, however, are not alone 25 has opened an entirely new class of vehicles and ready
mixed lea?ng metallic paints, and similar coating formula
in this respect, oleoresinous varnish vehicles, esteri?ed
natural rosin and ‘oil-free varnishes being further exam
tions, which to date, in the case of lea?ng aluminum pig
ples of vehicles exhibiting varying degrees of the organic
mentation, have exhibited a shelf life of more than eight
acidity characteristic destructive of the leaf-producing
een months. In addition, the lea?ng type metallic coat
property of lea?ng grade metallic pigments.
ings formulated in accordance with the invention have
Lea?ng metallic pigments contemplated within the scope
exhibited increased durability, particularly when applied
of this invention are in regular commercial manufacture
to ferrous surfaces, when compared with unadjusted or
by dry hammer mill or wet ball mill processes, the pig
unmodi?ed lea?ng type metallic coatings, and have in
ments in either case consisting essentially of ?ake-like
many cases exhibited increased body or viscosity of the
paints or coating formulations thus produced.
particles having a lea?ng agent in the form of a fatty
acid, such as stearic or palmitic acid, or mixtures there
The actual amount of amine necessary to substantial
of, associated with the surfaces of the ?akes and imparting
thereto the property of “lea?ng” or “?oating,” which iden
ly neutralize the organic acids exhibited by a particular
vehicle will vary, ‘depending upon the acid number of the
ti?es the characteristic formation in a paint ?lm of a layer
vehicle and the particular amine or combination of
of metallic pigment immediately below and adjacent the 40 amines selected for addition thereto. In this regard, satis
exposed dried surface of the vehicle with which the pig
factory results have been realized when the above-named
ment has been initially thoroughly mixed.
amines, singly or in combination, are added to the organic
In respect of the organic acids which are destructive
of lea?ng, it has been discovered that the \dibasic acids
acid-containing vehicles in amounts .of 0.3 to 5 milli
grams per acid number per gram of non-volatile matter
are more destructive than the monobasic acids, and fur 45 in the organic acid-containing vehicle undergoing modi
ther, that the short chain acids are more destructive of
tication, and in no event should the total amount of added
{lea?ng than the long ‘chain acids, with leaf stability in
amine or amines exceed 5 milligrams per acid number per
creasing with increasing chain lengths and increasing
gram of the non-volatile matter in the vehicles.
equivalent weight of the organic acids.
It is among the objects of the present invention to pro
Signi?cant in the practice of the invention is the dis
covery that the above-named selected amines must be
vide vehicles characterized by inclusions of organic acids,
and treatment therefor, which permits their subsequent
admixture with lea?ng grades of metallic pigments, par
amines with the lea?ng metallic ?akes, in which latter
ticularly aluminum ?akes provided with a surface coat
cases the named amines have been found to be destruc
added to the organic acid-containing vehicles, as distin
guished from any initial contact or admixture of the
ing of a lea?ng agent, in the manufacture of ready-mixed 55 tive of the lea?ng agent on the surfaces of the individual
lea?ng metallic paints and similar coating formulations.
metallic ?akes. The organic acid-containing vehicles to
It is also an object of the invention to provide ready
which one or more of the amines of the invention have
mixed lea?ng type metallic paint and coating formula
‘been added have exhibited immediate improvement,
measured in terms of leaf retention of lea?ng metallic
coating formulations made therewith. However, in some
instances, depending on the composition ‘of the organic
tions incorporatinglea?ng grade metallic pigments in an
acidic vehicle modi?ed to neutralize the leaf-destroying
propensities of the vehicle.
These and other objects will be understood by those
skilled in the art to which this invention is addressed
on consideration of the following description.
acid-containing vehicle, and amine or amines added
thereto, optimum results in leaf retention have been ob
served when the treated or modi?ed vehicle has been al
The invention is basically predicated on the discovery 65 lowed to stand at room temperature for at least thirty
that vehicles exhibiting acidic leaf-destroying properties
minutes before dispersing a lea?ng metallic pigment
on admixture with lea?ng grade metallic pigments, and
therein. Organic acid-containing vehicles, modi?ed in
de?ned or evaluated in terms of containing leaf-destroying
accordance with the invention, and ready-mixed lea?ng
organic acids, can be modi?ed by additions thereto of
aluminum paints formulated therewith, have exhibited
one or more acid reactive amines selected for their ability 70 excellent stability on storage in sealed containers of the
to “tie-up” or otherwise neutralize the organic acids in
the vehicles when measured in terms of preventing de
same for periods of more than eighteen months at room
temperature in a test program evaluating therinvention.
8,085,890
4i
3
tional lea?ng determinations were also conducted at the
As used in the speci?cation and appended claims, the
end of one month, and one year.
term “acid number,” as applied to the organic acid-con
Table II records the results of the lea?ng determina
taining vehicles, is the number of milligrams of potassium
tions:
hydroxide required to neutralize one gram of the non
volatile matter or solids forming a component part of UK
the vehicle, as distinguished from the volatile content
thereof.
Examples selected from the test program conducted
to evaluate the modi?ed vehicles, and lea?ng aluminum
coating formulations made therefrom, are given herein as 10
follows:
Table II
Percent Leaflng
Aluminum Coating Formulation
Initial
73
82
One
Month
One
Year
EXAMPLE I
A synthesized organic acid-containing vehicle was formu
lated by mixing 50 grams of a 50 percent by weight non
volatile soya alkyd resin, exhibiting an acid number of
Modified Vehicle _____________________ _.
Unmodi?ed Vehicle __________________ _-
73
80
72
29
16 and containing 36 percent phthalic anhydride (by
weight of non-volatile matter), with 50 grams of volatile
values initially and at the end of one month, its lea?ng
value dropped considerably from a high of 82 to 29 per
hydrocarbon, such as mineral spirits, to provide a 25
cent at the end of one year, whereas the modi?ed vehicle
percent by weight non-volatile vehicle of suitable con
sistency for admixture with metallic ?ake pigments in the
coating formulation exhibited a lea?ng value of 72 at
the end of one year’s shelf storage.
EXAMPLE III
from which it will be observed that, although the unmodi
?ed vehicle coating formulation registered higher lea?ng
manufacture of commercially acceptable metallic coating
formulations, such as paints.
A third synthesized organic acid-containing alkyd ve
The vehicle so prepared was divided into two 50 gram
portions to one of which was added at room temperature
1 milligram per acid member per gram of non-volatile
hicle was prepared by mixing 50 grams of a 50 percent
non-volatile alkyd resin, exhibiting an acid number of
15 and containing 36 percent phthalic anhydride (by
matter in the synthesized vehicle, or 200 milligrams of
the amine tetraethylene pentamine, and in each portion
4 grams of lea?ng aluminum ?akes were thereafter dis
weight of non-volatile matter), with 50 grams of mineral
spirits, to provide a 25 percent by weight non-volatile
persed to provide an amine-modi?ed and an unmodi?ed 30 vehicle of suitable consistency for admixture with metallic
?ake pigments in the manufacture of metallic ready
metallic aluminum coating formulation.
mixed paints.
Initial lea?ng determinations were conducted on both
The vehicle so prepared was divided into two 50 gram
portions to one of which was added at room temperature
formulations before each was sealed in a separate con
tainer for shelf storage at room temperature. Additional
lea?ng determinations were also conducted at the end of
1.33 milligrams per acid number per gram of non-vola
tile matter in the synthesized vehicle, or 250 milligrams,
of the amine ethylene diamine, and in each portion of
the vehicle 4 grams of lea?ng aluminum ?akes were there—
one month, one year and nineteen months.
Table I records the results of the lea?ng determinations:
Table I
after dispersed to provide an amine-modi?ed and an un
modi?ed metallic ready-mixed paint.
Initial lea?ng determinations were conducted on both
ready~mixed paints before each was sealed in a separate
container for shelf storage at room temperature. Addi
tional lea?ng determinations were also conducted at the
end of one and three months’ shelf storage.
Table III records the results of the lea?ng determina
tions:
Table III
Percent lea?ng
Aluminum Coating Formulation
One
lnitial Month
Modi?ed Vehicle ________________ __
Unmodified Vehicle _____________ __
62
41
53
0
One
1 car
73
0
Nine
teen
Months
58
0
from which it will be observed that the aluminum coating
formulation made with the vehicle modi?ed to include 50
tetraethylene pentamine exhibited a lea?ng value of 58
percent at the end of nineteen months, whereas the coat
ing formulation made with the unmodi?ed vehicle reg
istered zero lea?ng value at the end of one month shelf
storage.
55
Percent Loa?ng
Aluminum Coating Formulation
Initial
Modi?ed Vehicle _____________________ -_
Unmodi?ed Vehicle __________________ ._
84
40
One
Mon th
47
0
Three
Months
82
0
EXAMPLE II
A synthesized S-gallon modi?ed phenolic resin linseed oil
varnish vehicle containing 50 percent non-volatile matter,
and exhibiting an ‘acid number of 14.3 was mixed with
50 grams of mineral spirits to provide a 25 percent by
weight non-volatile vehicle of suitable consistency for
admixture with metallic ?ake pigments in the manufac—
ture of commercially acceptable metallic coating formu
lations, such as paints.
The vehicle so prepared was divided into two 50 gram
portions to one of which was added at room temperature
1.12 milligrams per acid number per gram of non-volatile
matter in the synthesized vehicle or 200 milligrams, of
the amine piperidine, and in each portion of the vehicle
from which it will be observed that the ready-mixed
aluminum paint formulation made with the vehicle modi
?ed to include ethylene diamine exhibited a lea?ng value
of 32 percent at the end of three months, whereas the
unmodi?ed paint had completely lost its lea?ng property
at the end of one month.
EXAMPLE IV
Another synthesized organic acid-containing alkyd
vehicle was formulated by mixing 50 grams of a 50 per
cent by weight non-volatile alkyd resin exhibiting an acid
number of 15 and containing 36 percent phthalic anhy
dride (by weight of non-volatile matter), with 50 grams
4 grams of lea?ng aluminum ?akes were thereafter dis 70 of volatile hydrocarbon, such as mineral spirits, to pro
vide a 25 percent by weight non-volatile vehicle suitable
persed to provide an amine-modi?ed and an unmodi?ed
for admixture with varying amounts of metallic ?ake
aluminum coating formulation.
pigments in the manufacture of metallic coating formula
‘Initial lea?ng determinations were conducted on both
tions, such as ready-mixed metallically pigmented paints.
coating formulations before each was sealed in separate
The vehicle so synthesized was divided in two 50 gram
containers for shelf storage at room temperature. Addi
L
3,085,890
5
portions to one of which was added at room temper
ature 1.07 milligrams per acid number per gram of non
grams of a 50 percent non-volatile oil-free resin varnish
vehicle, exhibiting an acid number of 7.7, with 50 grams
of mineral spirits to provide a 25 percent by weight non
volatile vehicle suitable for admixture with metallic ?ake
volatile matter in the vehicle, or 200 milligrams, of 1.3
diamino propanol, and 4 grams of lea?ng aluminum ?akes
were thereafter dispersed in each portion of the synthe
pigments in the manufacture of ready-mixed paints.
sized vehicle to provide an amine-modi?ed and an un
The vehicle thus prepared was divided into two 50 gram
portions to one of which was added at room tempera
modi?ed metallic aluminum coating formulation.
Both coating formulations were sealed in separate con
tainers and stored at room temperature for more than
four months, lea?ng ‘determinations being conducted on
ture 2.12 milligrams per acid number per gram of non
volatile matter in the synthesized vehicle, or 200‘ milli
grams, of the amine piperidine, and in each portion of the
each of the formulations initially, and at the end of one
and three months.
vehicle 4 grams of lea?ng aluminum ?akes were there
after dispersed to provide an amine-modi?ed and an un~
Table IV records the results of the lea?ng determina
tions:
modi?ed metallic ready-mixed paint ‘formulation.
Table IV
Initial leafing determinations were conducted on both
15 ready-mixed ‘formulations before each was separately
sealed in containers for shelf storage at room tempera
Additional leafing ‘determinations were also con
ducted at the end of three and six month intervals of
sealed storage.
ture.
Percent Loafing
Aluminum Coating Formulation
Initial
One
Month
Three
Months
Table VI records the ‘results
20
of the lea?ng determina
tions:
Modi?ed Vehicle _____________________ _Unmodi?ed Vehicle ___________________ _.
48
40
46
0
29
0
Table VI
Percent Loa?ng
from which it will be observed that the coating formula 25
tion made with unmodi?ed vehicle lost its leaf at the end
of one month, as distinguished from a lea?ng value of
Aluminum Coating Formulation
Initial
Three
Months
29 percent at the end of three months’ storage at room
temperature for the coating formulation made with the
vehicle modi?ed with 1.3 diamino propanol.
30
EXAMPLE V
A synthesized S-gallon esteri?ed natural rosin vehicle
containing 50 percent non-volatile matter, and exhibiting
an acid number of 17.6, was mixed with 50 grams of
mineral spirits to provide a 25 percent by Weight non
volatile vehicle of suitable consistency for admixture with
Six
Months
Modi?ed Vehicle _____________________ __
95
95
95
Unmodi?ed Vehicle __________________ -i
0
0
0
from which it will be observed that the ready-mixed
aluminum paint formulations made with the vehicle modi
?ed to include piperidine exhibited a lea?ng of 95 percent
throughout its six months’ shelf storage at room ‘tem
perature, whereas the unmodi?ed paint formulation failed
to reveal a lea?ng property at any time.
In addition to the six examples described above, em
metallic flake pigments in the manufacture of commer
ploying synthesized organic acid-containing vehicles, three
commercial alkyd type organic acid-containing vehicles
cially acceptable metallic coating formulations, such as
paints.
The vehicle thus prepared was divided into two 50
gram portions to one of which was added ‘at room tem
were selected and modi?ed, in accordance with the prac
tice of the invention. The‘ three commercial vehicles
perature 0.9 milligram per acid number per gram of non
volatile matter in the synthesized vehicle, or 200 milli
positions and acid numbers, as follows:
were identi?ed by their manufacturer as having the com
grams, of the amine tetraethylene pentamine, and in each 45
portion of the vehicle 4 grams of lea?ng aluminum ?akes
were thereafter dispersed to provide an amine-modi?ed
and an unmodi?ed aluminum coating formulation.
Initial lea?ng determinations were conducted on both
‘
VEHICLE NO. 1
Acid No. 12.6
.
I
.
t
_
.
‘
Percent
Non-volatile alkyd resin ___________ __- ______ -Q--- 30
coating formulations before each was separately sealed 50
in containers for shelf storage at room temperature. Ad
ditional lea?ng determinations were also conducted at
the end of one month, one year and eighteen months.
Table V records the results of the lea?ng determina
tions:
Table V
Linseed oil __________________ __' _____ __j_ ______ .._ 56
Phthalic anhydride ___________________________ __ 33
Remainder volatile solvent.
~
VEHICLE NO. 2
~
'
VAcid No.
8.3
_
V
Non-volatile alkyd resin _______________________ __ 40
Soya oil
65
Phthalic anhydride___.. _______________________ __ 24
Percent Leaflng
Remainder volatile solvent.
Aluminum Coating Formulation
One ‘
One
Initial Month
Year
Eight
60
een
Months
Non-volatile alkyd resin ______________________ __ 30
Linseed oiL
Modi?ed Vehicle. ___
Unmodi?ed Vehicle__
77
88
75
75
S4
0
'
80
0
'
.VEHICLE NO. 3
Acid No. 15.2
__~_
52
Phthalic anhydride ___________________________ __ 35
Remainder volatile solvent.
. Tetraethylene pentamine was added to each of the
from which it will be observed that the ready-mixed
vehicles, Nos. 1, 2 and 3, at room temperature, in the
aluminum coating formulation made with the vehicle
amount of 0.7 milligram per acid number per gram of
modi?ed to include tetraethylene pentamine exhibited a
non-volatile matter in each vehicle, or 265, 230 and 320
lea?ng value of 80 percent at the end of eighteen months,
whereas the unmodi?ed paint had lost its lea?ng prop 70 milligrams of the amine tetraethylene pentamine were
added to 100 gram portions of vehicles Nos; 1, 2 and 3,
erty at the end of one‘year.
EXAMPLE VI
The vehicle of this example was a synthesized organic
respectively.
.
v
I 1 Ready mixed aluminum coating formulations or paints
were prepared by dispersing 10 grams of lea?ng aluminum
acid-containing oil-free varnish prepared by mixing 5O 75 ?akes in each 100 gram portion of the so modi?ed vehicles,
3,085,890
8
aluminum pigmentation in the manufacture of ready
mixed lea?ng aluminum coating formulations, the steps
as well as in equal portions of unmodi?ed vehicles Nos.
1, 2 and 3, and the six coating formulations thus pre
pared Were sealed in separate containers and shelf stored
at room temperature for more than six months, lea?ng
comprising, adding to the vehicles at room temperature
at least one organic acid-reactive amine selected from
determinations being conducted on each formulation Cit the group consisting of tetraethylene pentamine, piper-i
dine, ethylene diamine and 1.3 diamino propanol, the
initially, and at the end of one, three and six month in
said selected amines being destructive in themselves of
tervals.
lea?ng agent on the surfaces of individual ?akes of lea?ng
Table No. VII records the results of the lea?ng determi
aluminum pigmentation on direct contact therewith, and
nations:
10 allowing the so-treated vehicles to stand for a period of
Table Vll
at least thirty minutes.
3. A method of modifying vehicles containing organic
Percent Loa?ng
Aluminum Coating Formulation
Initial
‘Modi?ed Vehicle No. 1 ____________ ._
Unmodi?ed Vehicle No. 1___._
_
76
79
Modified Vehicle No. 2_ _.__.-
75
79
(i6
78
Unmodi?ed Vehicle No. ‘AModified Vehicle No. 3____
Unmodi?ed Vehicle No. 3--
-
Ono
Three
Six
Month Months Months 15
7G
72
72
58
61
0
75
68
45
37
65
42
0
55
0
0
55
0
acids destructive of lea?ng on admixture with lea?ng
aluminum pigmentation in the manufacture of ready
mixed lea?ng aluminum coating formulations character
ized by leaf retention following storage of the same,
comprising adding to the vehicles at room temperature at
least one of the amines selected from the group consisting
of tetraethylene pentamine, piperidine, ethylene diamine
20 and 1.3 diamino propanol, the said selected amines being
destructive in themselves of lea?ng agent on the surfaces
of
individual ?akes of lea?ng aluminum pigmentation on
from which it will be observed that the paint formula
direct contact therewith, and holding the so-treated ve
tions made with the modi?ed commercial vehicles all
hicles for a period of time su?icient to neutralize the
registered leaf retention at the end of six months’ shelf
organic acids present in the vehicle.
25
storage and absence of leaf ‘for the paints made with the
4. A method of modifying vehicles containing organic
same unmodi?ed commercial vehicles.
acids destructive of lea?ng on admixture with lea?ng
Lea?ng determinations in all instances Were conducted
aluminum pigmentation in the manufacture of leaf retain
in a manner similar to that described in A.S.T.M. speci
ing ready-mixed aluminum coating formulations, said ve
?cation D480-5l-4.
hicles having acid numbers within the range 5 to 32, com
The lea?ng aluminum ?ake content of the coating 30 prising
adding to the vehicles at room temperature at least
formulations prepared in accordance with the invention
one of the amines selected from the group consisting of
may be varied within conventional ready-mixed paint
tetraethylene pentamine, piperidine, ethylene diamine and
practice and requirements. Preferably, the lea?ng alumi
1.3 diamino propanol in amounts of 0.3 to 5 milligrams
num ?akes are dispersed in the previously modi?ed, or
per acid number per gram of non-volatile matter in the
ganic acid-containing vehicles in amounts falling within
vehicles, the said selected amines being destructive in
the range two ounces to three pounds of aluminum ?akes
themselves of lea?ng agent on the surfaces of individual
per gallon of modi?ed vehicle. Also, since the bulk of
?akes of lea?ng aluminum pigmentation on direct contact
aluminum pigments are presently manufactured and sold
therewith, the total amount of amines not exceeding 5
in the form of paste products, regularly produced com
milligrams per acid number per gram of the non-volatile
mercial lea?ng aluminum paste products comprising by
weight 60 to 78 percent aluminum ?akes, l to 5 percent
lea?ng agent, such as stearic or palmitic acids, or mix
tures thereof, and the remainder volatile hydrocarbon,
matter in the vehicles.
nates of zirconium, cobalt and manganese may be present
matter in the vehicles.
5. A method of modifying vehicles containing organic
acids destructive of lea?ng on admixture with lea?ng
aluminum pigmentation in the subsequent manufacture
lea?ng aluminum coating formulations made therewith
of leaf retaining ready-mixed aluminum coating formula
45
would preferably include one-eighth to four pounds of
tions and said vehicles having acid numbers Within the
the lea?ng paste per gallon of modi?ed, organic acid
range 5 to 32, the step of adding to the vehicles at room
containing vehicle.
temperature at least one of the amines selected from the
Whether the invention is practiced with commercially
group consisting of tetraethylene pentamine, piperidine,
available or synthesized organic acid-containing vehicles,
ethylene diamine and 1.3 diamino propanol in an amount
conventional hydrocarbon volatile solvent thinners, and
within the range of 0.3 to 5 milligrams per acid number
compatible mixtures thereof, may be substituted or added,
per gram of non-volatile matter in the vehicles, the said
as desired. Equivalent thinners in this respect are mineral
selected amines being destructive in themselves of lea?ng
spirits, xylol, toluol, high ?ash naphtha and varnish mak
agent on the surfaces of individual ?akes of lea?ng
er’s and painter’s naphtha, all of which :fall under the
aluminum pigmentation on direct contact therewith, the
general classi?cation of volatile hydrocarbons. Also, con
total amount of the added amines not exceeding 5 milli
ventional driers, such as napthenates, octates, and resi
grams per acid number per gram of the non-volatile
in the vehicles and coating formulations made therewith
6. A method of producing a ready-mixed lea?ng
without in any way detracting from the results of the
aluminum coating formulation in a synthetic alkyd resin
60
invention.
vehicle containing at least one leaf-destructive organic
What is claimed is:
acid, the steps comprising ?rst adding to the vehicle at
l. A method in the production of lea?ng aluminum
room temperature at least one of the amines selected
ready-mixed coating formulations in vehicles containing
from the group consisting of tetraethylene pentaminc,
organic acids destructive of the lea?ng property of lea?ng
piperidine,
ethylene diamine and 1.3 diamino propanol
aluminum pigment, the steps comprising, adding to the 65 in amounts of 0.3 to 5 milligrams per acid number per
vehicles at room temperature at least one organic acid
gram of non-volatile matter in the vehicle, the said
reactive amine selected from the group consisting of
selected amines being destructive in themselves of lea?ng
tetraethylene pentamine, piperidine, ethylene diamine and
agent on the surfaces of individual ?akes of lea?ng
1.3 diamino propanol, the said selected amines being
aluminum pigmentation on direct contact therewith allow
destructive in themselves of lea?ng agent on the surfaces 70
of individual ?akes of lea?ng aluminum pigmentation on
direct contact therewith, and thereafter dispersing lea?ng
aluminum ?akes in the so-treated vehicles.
ing the so-treated vehicle to stand at room temperature
for at least thirty minutes, and thereafter dispersing
lea?ng aluminum ?akes in amounts of two ounces to
three pounds per gallon in the so-treated vehicle.
7. A method of producing a ready-mixed lea?ng
acids destructive of lea?ng on admixture with lea?ng 75
2. A method of modifying vehicles containing organic
3,085,890
10
aluminum coating formulation in an oleoresinous varnish
vehicle containing at least one leaf-destructive organic
acid, the steps comprising ?rst adding to the vehicle at
room temperature at least one of the amines selected
gstructive in themselves of lea?ng agent on the surfaces of
individual ?akes of lea?ng aluminum pigmentation on
direct contact therewith, the total amount of said added
amines not exceeding 5 milligrams per acid number per
from the group consisting of tetraethylene pentamine,
piperidine, ethylene diamine and 1.3 diamino propanol
gram of non-voiatile content of the vehicle.
12. An oleoresinous varnish vehicle for admixture with
in amounts of 0.3 to 5 milligrams per acid number per
gram of non-volatile matter in the vehicle, the said selected
lea?ng aluminum ?akes in the manufacture of a lea?ng
aluminum ?akes in amounts of two ounces to three
panol in an amount of 0.3 to 5 milligrams per acid num
ber per gram of non-volatile content of the oleoresinous
aluminum ready-mixed coating formulation, said oleores
amines being destructive in themselves of lea?ng agent
inous varnish vehicle containing at least one organic
on the surfaces of individual ?akes of lea?ng aluminum 10 leaf-destructive acid within the acid number range 5 to
pigmentation on direct contact therewith, allowing the
32 and containing an addition of at least one amine
so~treated vehicle to stand at room temperature for at
selected from the group consisting of tetraethylene penta
least thirty minutes, and thereafter dispersing lea?ng
mine, piperidine, ethylene diamine and 1.3 diamino pro
pounds per gallon in the so-treated vehicle.
8. A method of producing a ready-mixed lea?ng
aluminum coating formulation in an esteri?ed natural
rosin vehicle containing at least one leaf-destructive or~
varnish vehicle, the said selected amines being destructive
in themselves of lea?ng agent on the surfaces of indi
vidual ‘flakes of lea?ng aluminum pigmentation on direct
ganic acid, the steps comprising ?rst adding to the vehicle
contact therewith the total amount of said added amines
at room temperature at least one of the amines selected
not exceeding 5 milligrams per acid number per gram of
non-volatile content of the vehicle.
13. A natural rosin vehicle for admixture with lea?ng
aluminum ?akes in the manufacture of a lea?ng aluminum
ready-mixed coating formulation, said natural rosin ve
25 hicle containing at least one organic leaf-destructive acid
from the group consisting of tetraethylene pentamine,
piperidine, ethylene diamine and 1.3 diamino propanol
in amounts of 0.3 to 5 milligrams per acid number per
gram of non-volatile matter in the vehicle, the said
selected amines being destructive in themselves of lea?ng
agent on the surfaces of individual ?akes of lea?ng
aluminum pigmentation on direct contact therewith, al
lowing the so-treated vehicle to stand at room tempera
ure for at least thirty minutes, and thereafter dispersing
lea?ng aluminum ?akes in amounts of two ounces to three
pounds per gallon in the so-treated vehicle.
9. A method of producing a ready-mixed lea?ng
aluminum coating formulation in an oil-free varnish
vehicle containing at least one leaf-destructive organic
acid, the steps comprising ?rst adding to the vehicle at
room temperature at least one of the amines selected
from the group consisting of tetraethylene pentamine,
piperidine, ethylene diamine and 1.3 diamino propanol in
within the acid number range 5 to 32 and containing an
addition of at least one amine selected from the group
consisting of tetraethylene pentamine, piperidine, ethylene
diamine and 1.3 diamino propanol in an amount of 0.3
to 5 milligrams per acid number per gram of non-volatile
content of the natural rosin vehicle, the said selected
amines being destructive in themselves of lea?ng agent
on the surfaces of individual ?akes of lea?ng aluminum
pigmentation on direct contact therewith, the total amount
of said added amines not exceeding 5 milligrams per acid
number per gram of non-volatile content of the vehicle.
14. An oil-free varnish vehicle for admixture with
lea?ng aluminum ?akes in the manufacture of a lea?ng
amounts of 0.3 to 5 milligrams per acid number per
aluminum ready-mixed coating formulation, said oil-free
gram of non-volatile matter in the vehicle, the said 40 varnish vehicle containing at least one free organic leaf
selected amines being destructive in themselves of lea?ng
destructive acid within the acid number range 5 to 32
agent on the surfaces of individual ?akes of lea?ng
and containing an addition of at least one amine selected
aluminum pigmentation on direct contact therewith, allow
ing the so-treated vehicle to stand at room temperatur
for at least thirty minutes, and thereafter dispersing lea?ng
aluminum ?akes in amounts of two ounces to three pounds
per gallon in the so-treated vehicle.
10. A vehicle for admixture with lea?ng aluminum
from the group consisting of tetraethylene pentamine,
piperidine, ethylene diamine and 1.3 diamino propanol
in an amount of 0.3 to 5 milligrams per acid number per
gram of non-volatile content of the oil-free varnish ve
hicle, the said selected amines being destructive in them
selves of lea?ng agent on the surfaces of individual flakes
?akes in the manufacture of a lea?ng aluminum ready~
of lea?ng aluminum pigmentation on direct contact there
mixed coating formulation, said vehicle having an acid 50 with, the total amount of said added amines not exceed
number within the range 5 to 32 and containing at least
ing 5 milligrams per acid number per gram of non
one organic leaf-destructive mono- and poly-basic acid
volatile content of the vehicle.
of the group benzoic, abietic, phthalic, isophthalic, fu
15. A lea?ng aluminum ready-mixed coating formula
maric, maleic and sebacic, and containing an addition of
tion consisting essentially of a pretreated vehicle contain
at least one amine selected from the group consisting of 55 ing at least one organic acid destructive of the lea?ng
tetraethylene pentamine, piperidine, ethylene diamine and
property of the aluminum pigment and at least one added
1.3 diamino propanol in an amount of 0.3 to 5 milli
amine selected from the group consisting of tetraethylene
grams per acid number per gram of non~volatile solid
pentamine, piperidine, ethylene diamine and 1.3 diamino
matter of the vehicle, the said selected amines being de
propanol in amounts within the range 0.3 to 5 milligrams
structive in themselves of lea?ng agent on the surfaces 60 per acid number per gram of non-volatile matter in the
of individual ?akes of lea?ng aluminum pigmentation on
vehicle, but not exceeding 5 milligrams per acid number
direct contact therewith, the total amount of said added
per gram of the non-volatile matter in the vehicle in total
amines not exceeding 5 milligrams per acid number per
amount, the said selected amines being destructive in
gram of non~volatile solid matter in the vehicle.
themselves of lea?ng agent on the surfaces of individual
65
11. A synethetic alkyd resin vehicle for admixture with
?akes of lea?ng aluminum pigmentation on direct con
lea?ng aluminum flakes in the manufacture of a lea?ng
tact therewith, in admixture with lea?ng aluminum ?akes
aluminum ready-mixed coating formulation, said syn
thetic alkyd resin vehicle containing at least one organic
leaf-destructive acid within the acid number range 5 to
in amounts Within the range tWo ounces to three pounds
per gallon of the pretreated vehicle.
16. A lea?ng aluminum ready-mixed coating formula
32 and containing an addition of at least one amine 70 tion consisting essentially of a pretreated vehicle con
selected from the group consisting of tetraethylene penta
mine, piperidine, ethylene diamine and 1.3 diamino pro
panol in an amount of 0.3 to 5 milligrams per acid num
taining at least one organic acid destructive of lea?ng
of aluminum pigmentation and having an acid number of
5 to 32 and containing at least one added amine selected
ber per gram of non-volatile content of the synthetic
alkyd resin vehicle, the said selected amines being de
from the group consisting of tetraethylene pentamine,
piperidine, ethylene diamine and 1.3 diamino propanol
8,085,890
l2
11
vehicle containing at least one organic acid destructive
in amounts within the range 0.3 to 5 milligrams per acid
of lea?ng of the aluminum pigmentation and having an
number per gram of non-volatile solids in the vehicle, but
acid number of 5 to 32 and containing at least one
not exceeding 5 milligrams per acid number per gram of
added amine selected from the group consisting of tetra
the non-volatile matter in the vehicle in total amount,
the said selected amines being destructive in themselves Gr ethylene pentamine, piperidine, ethylene diamine and 1.3
diamino propanol in amounts within the range 0.3 to 5
of lea?ng agent on the surfaces of individual ?akes of
milligrams per acid number per gram of non-volatile
lea?ng aluminum pigmentation on direct contact there
matter in the vehicle, but not exceeding 5 milligrams per
with, in admixture with lea?ng aluminum ?akes in
acid number per gram of the non-volatile matter in the
amounts within the range two ounces to three pounds per
10 vehicle in total amount, the said selected amines being
gallon of the pretreated vehicle.
destructive in themselves of lea?ng agent on the surfaces
17. A lea?ng aluminum ready-mixed coating formula
tion consisting essentially of a pretreated synthetic alkyd
of individual ?akes of lea?ng aluminum pigmentation
resin vehicle containing at least one organic acid destruc
tive of lea?ng of aluminum pigmentation and having an
aluminum ?akes in amounts Within the range two ounces
acid number of 5 to 32 and containing at least one added
amine selected from the group consisting of tetraethylene
pentamine, piperidine, ethylene diamine and 1.3 diamino
propanol in amounts within the range 0.3 to 5 milligrams
per acid number per gram of nonvolatile solids in the
vehicle, but not exceeding 5 milligrams per acid number
per gram of the non-volatile matter in the vehicle in
total amount, the said selected amines being destructive
in themselves of lea?ng agent on the surfaces of indi
vidual ?akes of lea?ng aluminum pigmentation on direct
contact therewith, in admixture with lea?ng aluminum
?akes in amounts within the range two ounces to three
pounds per gallon of the pretreated vehicle.
18. A lea?ng aluminum ready-mixed coating formu
lation consisting essentially of a pretreated oleoresinous
vehicle containing at least one organic acid destructive of
the lea?ng property of the aluminum pigmentation and
having an acid number of 5 to 32 and containing at least
one added amine selected from the group consisting of
tetraethylene pentamine, piperidine, ethylene diamine and
1.3 diamino propanol in amounts within the range 0.3 to
5 milligrams per acid number per gram of n0n~volatile
matter in the vehicle, but not exceeding 5 milligrams per
acid number per gram of the non-volatile matter in the
on direct contact therewith, in admixture with lea?ing
to three pounds per gallon of the pretreated vehicle.
20. A lea?ng aluminum ready-mixed coating formu
lation consisting essentially of a pretreated oil-free varnish
vehicle containing at least one organic acid destructive of
lea?ng of aluminum pigmentation and having an acid
number of 5 to 32 and containing at least one added
‘amine selected from the group consisting of tetraethylene
pentamine, piperidine, ethylene diamine and 1.3 diamino
propanol in amounts within the range 0.3 to 5 milligrams
per acid number per gram of non-volatile matter in the
vehicle, but not exceeding 5 milligrams per acid number
per gram of the non-volatile matter in the vehicle in total
amount, the said selected amines being destructive in
themselves of lea?ng agent on the surfaces of individual
?akes of lea?ng aluminum pigmentation on direct contact
therewith, in admixture with lea?ng aluminum ?akes in
amounts Within the range two ounces to three pounds
per gallon of the pretreated vehicle.
References Cited in the ?le of this patent
UNITED STATES PATENTS
2,178,181
2,234,164
McMahon ____________ __ Oct. 31, 1939
Harris ______________ __ Mar. 11, 1944
vehicle in total amount, the said selected amines being
2,522,538
Rethwisch et al. ______ __ Sept. 19, 1950
destructive in themselves of lea?ng agent on the surfaces 40
2,587,267
Wray et a1 -___-__ ____ __ Feb. 26, 1952
of individual ?akes of lea?ng aluminum pigmentation on
direct contact therewith, in admixture with lea?ng
2,904,525
Babcock et a1 _________ _-
ept. 15, 1959
FOREIGN PATENTS
aluminum ?akes in amounts within the range two ounces
to three pounds per gallon of the pretreated vehicle.
19. A lea?ng aluminum ready-mixed coating formu
lation consisting essentially of a pretreated natural rosin
483,814
Great Britain ________ __ Apr. 22, 1938
665,709
Great Britain ________ __ Jan. 30, 1952
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