Note: Descriptions are shown in the official language in which they were submitted.
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Surface Treatments For Pi~lnents Providing Improved Dispersibility
And Exhibiting Biocidal Activity
This invention relates to surfactant treated particulate titanium dioxide and
other pigments. More
particularly, this invention is concerned with surfactant treated titanium
dioxide and other
particulate materials readily employable in coating compositions, plastic
molding compositions,
reinforced plastic composite compositions, and paper making compositions.
Industrial pigment particles agglomerate or cake together into hard packed
clusters during the
drying operation near the end of the manufacturing process. Forces holding
pigment clusters
together are not large in many cases but are yet large enough that the pigment
user, those who
incorporate industrial pigments into their products such as paints and
plastics and the like, are
required to subject industrial pigments to a milling operation in which the
agglomerates are
sheared under stress into particles of suitable smallness and homogenized into
the matrix or
product which incorporates them. The process is dispersion.
Pigment dispersion is a bottleneck, a limiting requirement, and the most
expensive operation in
terms of energy and time in manufacturing processes which employ pigments.
This present
invention is concerned with the employment of surfactants for the surface
treatment of pigments
during the pigment manufacturing process in order to provide pigments of
improved
dispersibility in subsequent manufacturing processes and in some cases, to
provide
improvements in certain important aspects ofproducts incorporating these
surface treated pigments.
Titanium dioxide pigments present a special case. Uncoated titania pigments
are extremely
difficult to disperse. In addition, their employment in pigmented plastics,
coatings, papers, and
fiber compositions induces a photoactivity which results in oxidative
degradation which is
destructive of the materials of which they are a part. As a consequence, most
titanium dioxide
pigments are provided with some form of surface coating during manufacture to
promote
dispersibility and to reduce photoactivity. Two materials in widespread use at
present are silica
and alumina. These materials are coated onto the surfaces of pigment particles
in the range of
three to ten percent by weight of TiOz.
The surface treatment of pigments can provide the following beneficial primary
effects:
1. The total number of agglomerates is reduced.
2. Any agglomerates that are present are more easily broken up since their
mechanical strength
is reduced.
3. Pigment particle wettability is improved due to a lowering of the
interfacial tension between
the pigment surface and the application medium.
4. Wettability of the pigment particles is also improved due to the liberation
of the free energy
of solution of the coating agent on the pigment surface. (Surface Treatment of
Organic Pigments;
K. Merkle and H. Schafer; Pigment Handbook, page 158, Vol. III; John Wiley and
Sons, Inc.,
1973.)
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Pigments, their preparation and properties are described in volumes I, II and
III of the book
"Pigment Handbook" published by John Wiley & Sons, Inc. The uses, preparation
and
characterization of pigments is further described in the various units of "The
Federation Series
on Coating Technology" published by the Federation of Societies for Coating
Technology.
German Pat. Nos. 889,042 and 930, 998 teach the use of surface-active
substances as emulsifiers
together with oils in the manufacture of water-insoluble azo-dyestuffs having
a soft grain.
U.S. Pat. No. 3,120,508 discloses that water-insoluble azo-dyestuffs having a
particularly high
tinctorial strength can be prepared by adding during the coupling cationic
surface-active
compounds without simultaneously using oils.
U.S. Pat. No. 3,437,502 teaches improvement of opacity and dispersibility of
titanium dioxide
through surface treatment with silica and alumina. U.S. Pat. No. 3,658,566
teaches the
production of titanium dioxide of improved properties by treatment with oxides
of silicon and
aluminum. U.5. Pat. No. 4,599,114 discloses improvement ofpigmentary
properties for a variety
of pigments through surface treatment of pigment filter cakes.
Cationic surface-active compounds are described in the book "Surface-Active
Agents and
Detergents" by A. M. Schwartz, J. W. Perry and J. Berch, vol. II (1958), pages
103 to 119.
U.S. Pat. Nos. 4,599,114, 4,471,780, and 4,909,852 disclose compositions
having surfactants
consisting of the reaction product of a diamine, a carboxylic acid and a fatty
acid. U.S. Pat. No.
5,808,118 discloses a composition which is the reaction product of a diamine,
a sulfonic acid and
a fatty acid.
British Patent No. 1,080,115 discloses the use of primary long chain alkyl
amines for treating
pigments improving their dispersibility.
Suitable cationic surface-active substances are, for example, long-chained
aliphatic amino
compounds that contain about 10 to 18 carbon atoms, or the salts of such
nitrogen compounds
with carboxylic acids, such as for example, formic acid, acetic acid, oleic
acid, tallow fatty acid,
lactic acid or mineral acids, for example, hydrochloric acid. Fatty amines are
for example,
coconut oil amine, oleyl amine, stearyl amine, and tallow fat amine, as well
as the secondary and
tertiary amines or quaternary ammonium compounds derived therefrom that may
carry as
substituents aliphatic, aromatic or oxethylated radicals, for example,
alkyldimethyloxyethyl
ammonium chloride. Oxethylated fatty amines in their secondary, tertiary or
quaternary form are
also suitable. Also useful are the condensation products of long-chained, in
some cases also
unsaturated, carboxylic acids with amines, in particular alkylenediamines,
alkylenetriamines, or
alkylenepolyamines containing alkylene radicals of low molecular weight, for
example, ethylene
diamine, diethylene triamine, etc., as well as the secondary, tertiary or
quaternary amines formed
by alkylation of the condensation products, especially in the form of their
water-soluble salts
with the above-mentioned acids. Further, there may be used fatty acid amides
and esters of
long-chained carboxylic acids with alkylol amines, for example,
triethanolaminoleate, stearate,
and the like, further also cyclical, nitrogen-containing compounds, for
example, long-chained
derivatives of morpholine, imidazoline, piperidine, piperazine or pyridine.
The above-mentioned
amino compounds are used preferably in the form of their carboxylic or
hydrochloric salts.
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There is described herein the use of surfactants which have the capability of
increasing the
dispersibility of titanium dioxide and other pigments to which they are
applied.
Titanium dioxide is an established pigmentary material which can also be
employed as a
reinforcing filler, albeit an expensive one. It is commonly made by two
processes, the chloride
process and the sulfate process. The chloride process is dry process wherein
TiCl4 is oxidized
to Ti02 particles. In the sulfate process titanium sulfate, in solution, is
converted by a metathesis
reaction to insoluble and particulate titanium dioxide. In both processes,
particle formation can
be seeded by aluminum compounds. Thereafter, the processes are essentially the
same. The Ti02
particles in a water slurry are put through multiple hydroseparations to
separate out the large
particles and the further refined pigment in slurry form is passed to a
treating tank where the
particles may be treated with an aluminum compound and/or silicon compound,
such as
aluminum triethoxide, sodium aluminate, aluminum trichloride, aluminum
sulfate, ethyl silicate,
sodium silicate, silicon tetrachloride, trichlorosilane, and the like. By pH
adjustment, the pigment
is flocculated and precipitated with its coating of alumina and/or silica, or
without any coating.
It is then made into a filter cake by a vacuum drying and further dried in an
oven, generally of
a vibrating type. The optimum average particle size can range from about 0.05
to about 0.35
microns with a range of about 0.1 to about 0.25 more preferable.
One feature of the dispersion promoters of this invention is that they alter
the surface
characteristics of the titanium dioxide or other pigments so that it is more
readily and more
thoroughly dispersed within the resin or plastic in which it is incorporated,
and this serves to
enhance the appearance of the resulting composite and increase the overall
strength of the
composite when the particulate material employed is one which serves to
reinforce the plastic
or resin.
The amount of dispersion promoter provided upon the titanium dioxide
particles, as characterized
herein, is that amount which alters the surface characteristics of the
particles so that they are
more readily dispersed within the resin, plastic, paper making composition or
other medium in
which they are incorporated. Typically, the amount of the dispersion promoter
which is supplied
to the titanium dioxide may be from as little as about 0.25 weight percent to
about 5 weight
percent, based upon the weight of the titanium dioxide particles. As a rule,
about 0.5 to about 3
weight percent of the dispersion promoter and/or its derivatives is adequate
for the purposes of
appropriately alterating the surface characteristic of the particles.
Preferred is 2%. Most preferred
is 2 or less weight percent for titanium dioxide and inorganic color pigments,
1 or less weight
percent for inert pigments, and much higher amounts for the organic and carbon
black pigments
which have very high surface areas. For some pigment and mediums the amount of
dispersion
promoter may be from about 1.00 to about 15.0 percent or higher.
The amount of dispersion promoter provided when used with carbon black
particles, as
characterized herein, is that amount which alters the surface characteristics
of the particles so that
they are more readily dispersed within the resin, plastic, paper making
composition or other
medium in which they are incorporated. Typically, the amount of the dispersion
promoter which
is supplied to the carbon black may be from as little as about 1.00 weight
percent to about 15.0
weight percent, based upon the weight of the carbon black particles. As a
rule, about 4.0 to about
10.0 weight percent of the dispersion promoter and/or its derivatives is
adequate for the purposes
of appropriately alterating the surface characteristic of the particles. Most
preferred is about 8.0
percent.
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The amount of dispersion promoter provided when an organic pigment is used, as
characterized
herein, is that amount which alters the surface characteristics of the pigment
so that it is more
readily dispersed within the resin, plastic, paper making composition or other
medium in which
it is incorporate. Typically, the amount of the dispersion promoter which is
supplied to the
organic pigment may be from as little as about 1.00 weight percent to about
15.0 weight percent,
based upon the weight of the organic pigment. As a rule, about 4.0 to about
10.0 weight percent
of the dispersion promoter and/or its derivatives is adequate for the purposes
of appropriately
alterating the surface characteristic of the pigment. Most preferred is about
4.0 percent.
The amount of dispersion promoter provided when inert pigments are used, as
characterized
herein, is that amount which alters the surface characteristics of the pigment
so that it is more
readily dispersed within the resin, plastic, paper making composition or other
medium in which
it is incorporated. Typically, the amount of the dispersion promoter which is
supplied to the inert
pigment may be from as little as about 0.25 weight percent to about 3 weight
percent of the
dispersion promoter and/or its derivatives which is adequate for the purposes
of appropriately
alterating the surface characteristic of the pigment. Most preferred is 1 %.
The amount of dispersion promoter provided when inorganic color pigments are
used, as
characterized herein, is that amount which alters the surface characteristics
of the pigment so that
it is more readily dispersed within the resin, plastic, paper making
composition or other medium
in which it is incorporated. Typically, the amount of the dispersion promoter
which is supplied
to the inorganic color pigments may be from as little as about 0.25 weight
percent to about 5
weight percent of the dispersion promoter and/or its derivatives which is
adequate for the
purposes of appropriately alterating the surface characteristic of the
pigment. Most preferred is
2%.
The surfactants of this invention perform the role of dispersants when added
directly to
conventional paint formulations.
The dispersion promoter and/or its derivatives may be provided on the titanium
dioxide particles
by any of the known methods by which dispersion promoters are similarly
supplied to particulate
surfaces. Thus adding the dispersion promoter to the particles while tumbling,
mixing the
particles in a dilute liquid composition containing the dispersion promoter,
or forming a slurry
of the particles and dispersion promoter and drying, spray drying or the like
represent adequate
treating procedures.
The plastics and/or resin in which the titanium dioxide particles treated with
the dispersion
promoter and/or its derivatives include essentially any plastic andlor resin.
Included in the
definition of plastic are rubber compounds. The treated titanium dioxide
particles may be
supplied to the plastic and/or resin while the same is in any liquid or
compoundable form such
as a solution, suspension, latex, dispersion, and the like. It makes no
difference from the
standpoint of this invention whether the plastic contains solvent or
nonsolvent, or the solvent is
organic or inorganic except, of course, it would not be desirable for any
plastic or resin or any
of the treated titanium dioxide to employ a solvent or dispersing medium which
deleteriously
affects the components being blended.
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Suitable plastics and resins include, by way of example, thermoplastic and
thermosetting resins
and rubber compounds (including thermoplastic elastomers). The plastics and
resins containing
the treated particles of this invention may be employed, for example, for
molding (including
extrusion, injection, calendaring, casting, compression, lamination, and/or
transfer molding),
coating (including lacquers, film bonding coatings, powder coatings, coatings
containing only
pigment and resin, and painting,) inks, dyes, tints, impregnations, adhesives,
caulks, sealants,
rubber goods, and cellular products. Thus the choice and use of the plastics
and resins with the
treated particles of this invention is essentially limitless. For simple
illustration purposes, the
plastics and resins may be alkyd resins, oil modified alkyd resins,
unsaturated polyesters
employed in GRP applications, natural oils, (e.g., linseed, tung, soybean),
epoxides, nylons,
thermoplastic polyester (e.g., polyethyleneterephthalate,
polybutyleneterephthalate),
polycarbonates, polyethylenes, polybutylenes, polystyrenes, styrene butadiene
copolymers,
polypropylenes, ethylene propylene co- and terpolymers, silicone resins and
rubbers, EPDM
rubbers, SBR rubbers, nitrile rubbers, natural rubbers, acrylics (homopolymer
and copolymers
of acrylic acid, acrylates, methacrylates, acrylamides, their salts,
hydrohalides, etc.), phenolic
resins, polyoxymethylene (homopolymers and copolymers), polyurethanes,
polysulfones,
polysulfide rubbers, nitrocelluloses, vinyl butyrates, vinyls (vinyl chloride
and/or vinyl acetate
containing polymers) ethyl cellulose, the cellulose acetates and ethylene-
vinyl acetate
copolymers, ethylene-acrylic acid copolymers, ethylene-acrylate copolymers),
and the like.
Most pigments go through an aqueous phase in manufacture in which the pigment
particles are
present at maximum fineness. This phase offers an ideal opportunity to contact
the individual
particles with a surface treating agent or surfactant with resulting important
benefits to pigment
dispersibility.
The agents of the present invention are produced from a combination of the
following materials
described in the general formula:
an amine or an alkanolamine
a fatty amine or fatty diamine
a dibasic acid or polybasic acid
Advantageous amines which are used include 2-amino-2-methyl-1-propanol,
monoethanolamine,
diethanolamine, triethanolamine, n-butylamine, and ethylenediamine.
Advantageous fatty amines include coco amine, lauryl amine, soya amine,
stearyl amine, tallow
amine, ether amines, ether diamines, and ethoxylated amines.
Advantageous dibasic and polybasic acids include dimer and trimer C, 8 fatty
acids, glutaric acid,
succinic acid, and adipic acid.
Particularly good results were achieved through combining one equivalent of
monoethanolamine
and one equivalent of coco amine with two equivalents of polymerized C, 8
fatty acid containing
36 carbon atoms. (Formula X). Another surfactant which gave outstanding
pigmentary
properties was produced through combining one equivalent of 2-amino-2-ethyl-1-
propanol and
three equivalents of coco amine with four equivalents of C36 dimer acid
(Formula Y). Yet
another advantageous surfactant was produced by combining one equivalent of
ethylenediamine
and three equivalents of an ethoxylated coco amine with four equivalents of
C36 dimer acid
(Formula Z). Many other advantageous surfactants are possible. Selected
surfactants of this
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invention give excellent results when added to the grind step of conventional
pigment
dispersions. Selected surfactants of this invention are also useful in
enhanced oil recovery.
In some instances the advantages provided by the surface treating agents of
this invention are
enhanced if the pigment particles are first exposed to minute amounts of
materials of high charge
density which bind to pigment surfaces and then act to attract the surface
treating agents and bind
them more closely and with more complete coverage to the pigment particle
surfaces. Strong
acids and bases act in this manner. Aluminum chloride (28% in water) added at
the rate of one-
tenth of one percent of dry weight of pigment enhanced the performance of
Formula X when
added to the pigment slurry and mixed prior to adding Formula X. In some
instances, strong
bases such as 2-amino-2-methyl-1-propanol can be used advantageously.
Depending on the
pigment and surfactant being used, the surfactant may also be added alone
without any prior
treatment.
The agents of the present invention also exhibit biocidal activity when
employed solely as a
composition, when used as an additive, or when combined with a pigment to be
applied to a
surface.
The present invention is directed to an agent having the general formulas:
a halogenated carboxylic acid and an amine, or
a halogenated carboxylic acid and
a fatty acid, combined with
a polyamine.
The reaction may be carned out in the presence of a medium such as propylene
glycol or
isopropyl alcohol.
Advantageous halogenated carboxylic acids include chloroacetic acid,
chloropropionic acid,
trichloroacetic acid, chlorofluoroacetic acid, trifluoroacetic acid,
bromopropionic acid, and
iodobenzoic acid.
Advantageous fatty acids include,oleic acid, stearic acid, coconut fatty acid,
soya fatty acid, ether
acids or 3-(alkoxy-) propionic acids where the alkyl group is eight or more,
and polymerized C1g
acids.
Advantageous polyamines include coco, tallow, and oleyl diamines, 3-
diethylaminepropylamine,
and ether amines having the formula ROCHzCHzCH2NHCHzCH2CH2NHz where R is six
or
more.
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Many combinations of these components have been found to be useful.
Advantageous
compositions include one equivalent of 2-chloropropionic acid and one
equivalent of stearic acid
combined with two equivalents of tallow diamine (Formula A, Example I). One
equivalent of
2-chloropropionic acid and three equivalents of coconut fatty acid combined
with four
equivalents of tallow diamine (Formula B, Example II).
Some ofthe compositions ofthis invention may be used as direct-add dispersants
in conventional
paint dispersion. An example is one equivalent of 2-bromopropionic acid and
one equivalent Of
C,$ polymerized fatty acid combined with two equivalents of tallow diamine.
The reaction was
carned out in propylene glycol equal to 25% by weight of the
composition.(Formula C, Example
III). An effective direct-add dispersant can be produced by combining a
halogenated carboxylic
acid with an appropriate amine. An example is one equivalent of 2-
chloropropionic acid
combined with one equivalent of tallow diamine, the reaction carried out in
propylene glycol
equal to 25% of the weight of the composition Formula D, Example IV).
The compositions of this invention are also useful as biocides. In Formula E,
Example V, one
equivalent of 2-chloropropionic acid and one equivalent of oleic acid were
combined with two
equivalents of ether diamine. The composition functions as a mildewcide when
added to a
commercial paint formulation. In addition to paints, selected compositions may
be used as
antiseptic agents in toiletries and soaps and as disinfectants in cleansers.
Some compositions can
be used in food processing, such as Formulas F and G, Examples VI and VII,
were used as
antibacterial agents forpoultry processing rinses. Some compositions may be
used as surfactants
in enhanced oil recovery. Some compositions are useful as liquid crystals.
In some instances, it was found to be advantageous to add minute amounts of
materials of high
charge density to pigment slurries before adding the compositions of this
invention. Strong acids
and bases function in this way (Example II). Such acids and bases as aluminum
chloride (28%
in water), formic acid, and 2-amino 2-methyl-1-propanol have been used.
Example I
Titanium Dioxide Filter Cake (61 % Solids)
Two and one half percent based on dry weight of pigment) of Formula A were
added to titanium
dioxide slurry (ASTM 476-73, 1988. Type II, III, IV). The slurry was mixed for
optimal
pigment particle coverage and dried. The dry pigment was suitable for use in
waterborne and
solvent borne paint formulations.
Example II
Titanium Dioxide - Filter Cake (55% Solids)
One and one half percent (based on pigment solids) of Formula B was added to
titanium dioxide
slurry (Type II, III, and IV) previously treated with 0.1 percent (based on
dry weight of pigment)
of aluminum chloride (28% in water). The slurry was mixed well and dried. Dry
pigment was
suitable for dispersion in waterborne and solvent borne paints.
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Example III
Direct Add Dispersant - Titanium- Dioxide (Type II, III, IV)
400 ml plastic beaker - 2" blade - 2100 rpm
Grind portion:
40 grams medium oil alkyd
80 grams titanium dioxide
(95% Ti02 A1203 additive - Type II, III, IV)
2.0 grams Formula C
Grind is 7-8 Hegman in two minutes.
Let down:
88.6 grams grind portion
144.0 grams medium oil alkyd
21.0 grams mineral spirits
driers and antiskinning agent
Smooth, high gloss films.
Therefore the compositions of this invention perform as dispersants when used
in conventional
paint formulations.
Example IV
Direct Add Dispersant - Titanium Dioxide (Type II, III, IV)
400 ml plastic beaker - 2" blade - 2100 rpm
Grind portion:
40 grams medium oil alkyd
80 grams titanium dioxide
(95% TiOz _ A1203 additive Type II, III, IV)
2.0 grams Formula D
Grind is 7-8 Hegman in two minutes
Let down:
88.6 grams grind portion
144.0 grams medium oil alkyd
21.0 grams mineral spirits
driers and antiskinning agent
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Smooth, high gloss films.
Example V
Exterior Exposure - Mildewcide
Substrate: 3/8" x 4" x 20" Interior Masonite Panel.
Paint: Sears Interior Semi Gloss Wall & Trim #78114.
Panel A: Two brush coats paint with no addition.
Panel.B: Two brush coats of paint with five grams Formula E
added to one half pint.
Results: After seven weeks exterior, vertical South, the untreated panel is
covered
with incipient mildew. No mildew was found on painted area treated
with Formula E.
Example VI
Antibacterial Poultry Rinse
Formula F (twenty percent chlorine by weight), two equivalents of
trichloroacetic acid and one
equivalent of ether acid combined with three equivalents of ether diamine was
used at the rates
of 1%, 0.5%, and 0.25% in water as an antibacterial poultry rinse. Birds were
immersed for 15
seconds, allowed to drip, and immersed in slush ice for two hours. They were
removed, drained
and rinsed with a 400 ml sterile Butterfield Phosphate solution for one
minute. Rinsate was then
plated on Aerobic Count and E. coli count Petri Filin. Controls immersed in
plain water and
non-treated controls were included. Results were as follows:
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Antimicrobial Study: Whole Broilers treated with 1.0, 0.50 and 0.25 '%
Solutions ( 20%
Chlorine)
A = 1 % solution, B = .5% solution, C = .25% solution, D = Control, E = Non-
treated control
(CFU's/ml*)
Sample Treatment APC Ecoli
1 A 520 0
2 A 50 0
3 A 205 0
4 A 280 0
A 797 0
AVG. 370 0
Reduction 92 100
1 B 360 0
2 B 130 0
3 B 730 0
4 B 580 0
5 B 200 0
AVG. 400 0
Reduction 91 100
1 C 540 6
2 C 610 2
3 C 970 0
4 C 580 2
5 C 390 0
AVG. 618 2
Reduction 87 99
1 D 5,400 570
2 D 6,100 1,160
3 D 1,290 56
4 D 7,300 210
5 D 6,500 62
AVG. 5,318 412
Reduction -15 -57
1 E 1,390 45
2 E 5,800 190
3 E 2,900 150
4 E 7,400 360
5 E 5,700 570
AVG. 4,638 263
*based on a 400 ml one bird rinse
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Example VII
Antibacterial Poultry Rinse
Formula G (fifteen percent fluorine by weight), three equivalents of
trifluoroacetic acid and one
equivalent of ether acid combined with four equivalents of ether diamine was
used at the rates
of 1%, 0.25%, and 0.05% in water as in Example VI. Results were as follows:
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Antimicrobial Study: Whole Broilers treated with 15% Fluorine solution @ 1.0,
0.25 and 0.05%
A = 1% solution, B = .25% solution, C .0S% solution, D = Control, E Non-
treated control
(CFU's/ml*)
Sample# Treatment APC Ecoli
1 A 135 0
2 A 120 0
3 A 115 1
4 A 265 0
S A 105 0
AVG. 148 0
%Reduction 99 100
1 B 920 0
2 B 250 0
3 B 1,030 0
4 B 1,210 0
B 380 0
AV G. 75 8 0
Reduction 97 100
1 C 3,500 14
2 C 1,670 4
3 C 3,300 0
4 C 4,200 6
AVG. 3,168 6
Reduction 88 99
1 D 1,510 49
2 D 3,400 42
3 D 13,000 50
4 D 19,500 105
5 D 14,100 16
AVG. 10,302 52
%Reduction 61 91
1 E 15,300 34
2 E 18,100 470
3 E 27,000 94
4 E 7,400 60
S E 63,000 2,400
AVG. 26,160 612
*based on a 400 ml one bird rinse
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Example VIII
Aluminum Trihydroxide - Filter Cake (48% Solids)
Aluminum trihydroxide (median particle size 1.0 micron) was treated with 0.1
percent (based on
dry pigment weight) hydrochloric acid (37.4%). One percent (based on dry
pigment weight) of
Formula H (one equivalent of 2-chloropropionic acid and one equivalent of C 18
polymerized fatty
acid combined with two equivalents of tallow diamine) (the reaction being
carned out in 25%
by weight of propylene glycol based on the weight of the reactants) was added
to the slurry and
mixed for optimal particle coverage. The resulting aluminum trihydroxide
treated pigment was
suitable for employment in alkyd resin or EPDM rubber formulations.
Example IX
Phthalocycanine Blue - Filter Cake (45% Solids)
Four percent (based on dry weight of pigment) of Formula H (see Example VIII)
was slurried
with phthalocyanine blue filter cake. The resulting pigment was suitable for
incorporation into
waterborne and solvent borne inks.
Example X
Titanium Dioxide - Filter Cake (57% Solids)
One percent (based on dry weight of pigment) of Formula X (one equivalent of
monoethanolamine and one equivalent of coco amine combined with two
equivalents of C36
dimer acid) was added to titanium dioxide slurry (ASTM 476-73 1988. Type II,
III, IV)
previously treated with 0.1 percent aluminum chloride (28% in water) based on
dry weight of
pigment. The slurry was mixed for optimal particle coverage and dried to
recover the surface
treated pigment. The dried pigment was suitable for dispersion in waterborne
and solvent borne
paint formulations.
Example XI
Titanium Dioxide Slurry (28% Solids) - No Inorganic Surface Treatment
One percent (based on dry weight of pigment) of Formula Y (one equivalent of 2-
amino-2-
methyl-1-propanol and three equivalents of coco amine combined with four
equivalents of C36
dimer acid) was added directly to a 28% titanium dioxide slurry which had
received no previous
inorganic surface treatment. The slurry was agitated and the dry pigment
recovered. This
pigment was suitable for dispersion in waterborne and solvent borne paint
formulations.
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CA 02389040 2002-04-25
WO 01/30888 PCT/LTS00/41430
Example XII
Phthalocyanine Blue - Filter Cake (45% Solids)
Four percent (based on dry weight of pigment) of Formula Z (one equivalent of
ethylenediamine
and three equivalents of ethoxylated coco amine combined with four equivalents
of C36 dimer
acid) was slurned with phthalocyanine blue filter cake and dried. The
resulting surface treated
pigment was suitable for dispersion in both waterborne and solvent borne inks.
Example XIII
Aluminum Trihydroxide - Filter Cake (50% Solids)
One percent (based on dry pigment weight) of Formula Y (one equivalent of 2-
amino-2-methyl-
1-propanol and three equivalents of ethoxylated coco amine combined with four
equivalents of
C36 dimer acid) was added to aluminum trihydroxide filter cake (median
particle size 1.0 micron)
and slurned. The dried pigment was suitable for dispersion in alkyd resins and
EPDM rubber
formulations.
Example XIV
Dispersion Of Titanium Dioxide - Direct Addition Of Surfactant
400 ml plastic beaker - 2" blade - 2100 rpm
Grind portion:
40 grams medium oil alkyd
80 grams titanium dioxide
(95% TiOz - A1203 additive - Type II, III, IV)
2.0 grams Formula E (one equivalent n-butylamine and one
equivalent of coco amine combined with two equivalents
of C36 dimer acid)
Grind is 7 - 8H in two minutes.
Add: 26.54 grams medium oil alkyd
18.75 grams mineral spirits
driers and antiskinning agent
The surface treating agents of this invention perform as dispersants when used
in conventional
paint formulations.
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