CA1087775A - Titanium dioxide pigment slurries to impart high gloss to water-based paint systems - Google Patents
Titanium dioxide pigment slurries to impart high gloss to water-based paint systemsInfo
- Publication number
- CA1087775A CA1087775A CA293,437A CA293437A CA1087775A CA 1087775 A CA1087775 A CA 1087775A CA 293437 A CA293437 A CA 293437A CA 1087775 A CA1087775 A CA 1087775A
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- Prior art keywords
- titanium dioxide
- percent
- slurry
- weight
- water
- Prior art date
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/007—Metal oxide
- C09D17/008—Titanium dioxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/16—Nitrogen-containing compounds
- C08K5/17—Amines; Quaternary ammonium compounds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/36—Sulfur-, selenium-, or tellurium-containing compounds
- C08K5/41—Compounds containing sulfur bound to oxygen
- C08K5/42—Sulfonic acids; Derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Inorganic Chemistry (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Cosmetics (AREA)
Abstract
ABSTRACT
An aqueous slurry of from 60 to 80 percent titanium dioxide is prepared from titanium dioxide of uniform and small particle size. At least 80 percent by weight of pigment is incorporated into an aqueous system containing suitable dis-persant which slurry is then reduced to the final slurry con-centration with water.
An aqueous slurry of from 60 to 80 percent titanium dioxide is prepared from titanium dioxide of uniform and small particle size. At least 80 percent by weight of pigment is incorporated into an aqueous system containing suitable dis-persant which slurry is then reduced to the final slurry con-centration with water.
Description
BACRGROUND OF ~HE INVENT~ON
~ he present in~ention relates to the preparation and composition of titanium dioxide in an aqueous slurry suitable for incorporation in water-based acrylic paint æystems to impart high-glo~s characteristics to the dried paint film.
: In recent years substantial research has been undertaken to develop titanium dioxide slurries that were suitable for use in paper and water-based paint manufacture.
The economics and ease of use of such slurries has been a cubstantial incentive for the development of titanium dioxide slurries.
Hall and Looby dlsclose ln U. S. Patent 3J702,773 that a stabillzed tltanlum dloxide ~lurry o~ rrom 60 to 82 percent by welght Or tltanlum dlo~ide ror use ln paper manu-racturlng could be prepared. Roberts and Rowland dlsclose ln U. S. Patent 3,758,322 that a process ror produclng slurries Or ~rom 60 to 80 percent t~tanlum dlo~lde content can be prepared rrom a plgment slurry contalnlng 20 percent sollds, Daubenspeck and Jett dlsclose ln U. S. Patent 3,847,640 that a pigment slurry containing 60 to 65 percent titan~um dloxlde ls adapted to be used in latex ~la~ palnt formulations.
This invention provides another step rorward ln the development of titanlum dloxlde slurries. This lnventlon provldes a slurry o~ very hlgh sollds content that can be used to prepare high gloss water-based acrylic paint formulations.
SUMMARY OF THE INVENTION
~his invention provides an aqueous slurry of
~ he present in~ention relates to the preparation and composition of titanium dioxide in an aqueous slurry suitable for incorporation in water-based acrylic paint æystems to impart high-glo~s characteristics to the dried paint film.
: In recent years substantial research has been undertaken to develop titanium dioxide slurries that were suitable for use in paper and water-based paint manufacture.
The economics and ease of use of such slurries has been a cubstantial incentive for the development of titanium dioxide slurries.
Hall and Looby dlsclose ln U. S. Patent 3J702,773 that a stabillzed tltanlum dloxide ~lurry o~ rrom 60 to 82 percent by welght Or tltanlum dlo~ide ror use ln paper manu-racturlng could be prepared. Roberts and Rowland dlsclose ln U. S. Patent 3,758,322 that a process ror produclng slurries Or ~rom 60 to 80 percent t~tanlum dlo~lde content can be prepared rrom a plgment slurry contalnlng 20 percent sollds, Daubenspeck and Jett dlsclose ln U. S. Patent 3,847,640 that a pigment slurry containing 60 to 65 percent titan~um dloxlde ls adapted to be used in latex ~la~ palnt formulations.
This invention provides another step rorward ln the development of titanlum dloxlde slurries. This lnventlon provldes a slurry o~ very hlgh sollds content that can be used to prepare high gloss water-based acrylic paint formulations.
SUMMARY OF THE INVENTION
~his invention provides an aqueous slurry of
-2-1087'775 titanium dioxide which when dried from a water-based acrylic coating composition forms a high-gloss film, said aqueous ælurry contains from 60 to 80 percent titanium dioxide, from 0.2 to 1 percent based upon the weight of titanium dioxide of a compound of the formula -Rl R,2 l IR3 R4 I. H- L X I ~ c c 1~ S03M
where M is alkali metal, ~1 to R4 is hydrogen, methyl or ethyl, X is cyano or -COOR5, where R5 is H, or lower alkyl of 1 to 4 carbon atoms, Y is -COOH or -COONa, a and b are 10 to 100, and rrom 0.1 to 0.6 percent based on the weight o~ titanium dioxlde Or 2-amino-2-methyl-1-propanol.
Thls lnventlon also relates to a process for pro-duclng a hlgh sollds content tltanlum dioxlde aqueous slurry ~hlch comprlses preparlng a solutlon of 0.2 to 1 percent o~
a compound of formula I and 0.1 to 0.6 percent of 2-amino-2-methyl-1-propanol, based on the weight of the titanium dioxide in about 10 to 25 percent of water, adding 75 to 90 percent by weight of titanium dioxide, grinding with a disc mill until uniform and adding sufficient water to re-' duce the titanium dioxide content to from 60 to ~0 percent by weight of the finished slurry.
DESCRIPTION OF THE INVENTION
I This invention relates to a hish-solids, high-gloss - 30 aqueous composition of titanium dioxide which is commonly lo~ms referred to in the art as a slurry. The slurrie~ of this invention are high-æolids slurries, i.e., from 60 to 80, and preferably ~rom 70 to 80, percent by weight titanium dioxide. Most preferably, the solids content of the slurry will be from about 75 to 79 percent titanium dioxide. me compositions of this inventlon are also referred to as high-glo~s slurries. The term "h~gloss 81urry" means that when the ~lurry is incorporated into an acryllc palnt formu-lation and dried into a thin film the film is of high glo88.
The high-glosæ slurries of this invention can be prepared simply from a dry titanium dioxide which has not been sub-~ected to special surface treatments prior to incorporation into water. Outstanding gloss levels in acrylic water-based paint systems have been achieved when a chloride process titanium dloxide i8 æimultaneo w ly dr~ed and groud u~ing a fluid energy mill o~ the conf~ned vortex tM e such as is tau~ht in U, S. Patent 3,840,188, The titanium dioxide emp~oyed in the preparation of the ~lurry compositions of this invention will preferably be of uniformly small particle size with at leaæt 95 mass percent of the average particle size being one mlcron or les~ and with an average particle æize of lesæ than about o.6 microns.
The titanium dioxide will also be one which has no hydrous oxide after-treatment as the presence of hydrous oxide reduces the gloss of the fini~hed paint film. It is under~tood, howe~er, that the presence of rutili~ing agents such as co-oxidized aluminum and the like which are normally pre~ent in titanium dioxide produced by oxidation of titanium ~o~ms tetrachloride will not ob~iate the advantages of the slurries of this in~ention.
To achieve the outstanding properties of glo88 the slurry i8 prepared by adding dry titanium dioxide to about 13 to 20 percent by weight of water, preferably 13 to 15 percent by weight of water, ~hich contain~ about 0.2 to 1 percent, based on the weight of titanium dioxide, of a com-pound of formula I and from 0.1 to o.6 percent, based on the weight of tltanium dioxide, of 2-amino-2-met ffl l-l-propanol.
m e high-solids slurry is then ground until uni~orm using a disc mill such as a Hockmeyer* disperser manufactured by H, H. Hockmeyer, Inc. The grinding i8 continued until the slurry beco~es uniform and then sufficient water i8 added to reduce the solids content o~ the slurry to from about 60 to 80 percent by weight.
When preparing the slurries of this invention the titanium dioxide content of the initial slurry shouad be at least 80 percent by weight so that the disc mill can impart sufficient shear into the sy~tem to assure reduction in agglomerate size o~ the titanium dioxide within the limits of this invention. Ideally the particle size will be aæ
i fine as possible with the average particle size of less than ; about o.6 micronæ with not more than 5 mass per cent of the titanium d~oxide particles or agglomerates, as the case ma~
be, with a particle size greater than one micron. Therefore, depending on the pigment base being employed the gFinding time and pigment concentration will be adJu~ted to achieve the desired particle ~ize uniPormity and distrlbution. It has also been disco~ered that addition of about ~ive percent water to the system after the grinding step resultæ ~n * denotes trade mark ,~
10~7775 improved rheological propertiec of the slurry and handling and use of the finished slurry is markedly enhanced.
It ha~ al~o been dlscovered that the use Or a sult-able dlspersant system ~ nece~ary to achle~e a tltanlum dloxlde slurry whlch lmparts outstandlng glos~ to a palnt ~llm derived rrom a water-~a~ed system. The dlsper~ant ~ystem comprl~ed Or 0.2 to 1 percent o~ a compound Or ~ormula I and rrom 0.1 to 0.6 percent Or 2-amlno-2-methyl-1-propanol, based on the welght o~ titanium dloxlde present, will when comblned wlth the other processing conditlons descrlbed herein produce a tltanlum d~o~ide slurry wlth an unexpectedly high level Or gloss ln a drled palnt f~lm.
The rollowlng examples are lllustratlve Or the inventlon. All parts and percentages are by welght unless otherwlse noted.
Example 1 Titanium dloxlde produced by the oxidation o~
tltanlum tetrachlorlde and about 1.0 per cent aluminum oxide in aqueous slurry of about 55-75 per cent by weight solids ls ~ed to a ~luid energy mill as described ln the example Or U. S. Patent 3,840,188 and dried and ~round using a steam to pigment ratlo Or rrom 2.5 to 6 as described therein to ~ro-duce dry tltanlum dioxide o~ uniform and small particle size.
~ ple 2 To 5,300 ml of water in a five-gallon container is added 150 ml of a compound of formula I in which M is Na, Rl to R4 are hydrogen and X and Y are carboxyl groups, and 60 ml of 2-amino-2-methyl propanol. To the above solu-tion is added 30,000 g of titanium dioxide pigment obtained as described in Example 1. Then a Hockmeyer disperser ` ~W77~5 fitted with a four-inch blade rotating at 4,000 rpm i8 employed to grind the pigment. After grinding for 20 min-utes, 3,000 ml of water is added to reduce the solid~
concentration in the slurry to about 76.7 percent by weight.
m e particle size of the solids i8 determined u~ing a Micrometrics* 5000 Analyzer which shows a mass percent of particles finer than:
Mass % Size (~)**
84 o.6 0.47 16 0.325
where M is alkali metal, ~1 to R4 is hydrogen, methyl or ethyl, X is cyano or -COOR5, where R5 is H, or lower alkyl of 1 to 4 carbon atoms, Y is -COOH or -COONa, a and b are 10 to 100, and rrom 0.1 to 0.6 percent based on the weight o~ titanium dioxlde Or 2-amino-2-methyl-1-propanol.
Thls lnventlon also relates to a process for pro-duclng a hlgh sollds content tltanlum dioxlde aqueous slurry ~hlch comprlses preparlng a solutlon of 0.2 to 1 percent o~
a compound of formula I and 0.1 to 0.6 percent of 2-amino-2-methyl-1-propanol, based on the weight of the titanium dioxide in about 10 to 25 percent of water, adding 75 to 90 percent by weight of titanium dioxide, grinding with a disc mill until uniform and adding sufficient water to re-' duce the titanium dioxide content to from 60 to ~0 percent by weight of the finished slurry.
DESCRIPTION OF THE INVENTION
I This invention relates to a hish-solids, high-gloss - 30 aqueous composition of titanium dioxide which is commonly lo~ms referred to in the art as a slurry. The slurrie~ of this invention are high-æolids slurries, i.e., from 60 to 80, and preferably ~rom 70 to 80, percent by weight titanium dioxide. Most preferably, the solids content of the slurry will be from about 75 to 79 percent titanium dioxide. me compositions of this inventlon are also referred to as high-glo~s slurries. The term "h~gloss 81urry" means that when the ~lurry is incorporated into an acryllc palnt formu-lation and dried into a thin film the film is of high glo88.
The high-glosæ slurries of this invention can be prepared simply from a dry titanium dioxide which has not been sub-~ected to special surface treatments prior to incorporation into water. Outstanding gloss levels in acrylic water-based paint systems have been achieved when a chloride process titanium dloxide i8 æimultaneo w ly dr~ed and groud u~ing a fluid energy mill o~ the conf~ned vortex tM e such as is tau~ht in U, S. Patent 3,840,188, The titanium dioxide emp~oyed in the preparation of the ~lurry compositions of this invention will preferably be of uniformly small particle size with at leaæt 95 mass percent of the average particle size being one mlcron or les~ and with an average particle æize of lesæ than about o.6 microns.
The titanium dioxide will also be one which has no hydrous oxide after-treatment as the presence of hydrous oxide reduces the gloss of the fini~hed paint film. It is under~tood, howe~er, that the presence of rutili~ing agents such as co-oxidized aluminum and the like which are normally pre~ent in titanium dioxide produced by oxidation of titanium ~o~ms tetrachloride will not ob~iate the advantages of the slurries of this in~ention.
To achieve the outstanding properties of glo88 the slurry i8 prepared by adding dry titanium dioxide to about 13 to 20 percent by weight of water, preferably 13 to 15 percent by weight of water, ~hich contain~ about 0.2 to 1 percent, based on the weight of titanium dioxide, of a com-pound of formula I and from 0.1 to o.6 percent, based on the weight of tltanium dioxide, of 2-amino-2-met ffl l-l-propanol.
m e high-solids slurry is then ground until uni~orm using a disc mill such as a Hockmeyer* disperser manufactured by H, H. Hockmeyer, Inc. The grinding i8 continued until the slurry beco~es uniform and then sufficient water i8 added to reduce the solids content o~ the slurry to from about 60 to 80 percent by weight.
When preparing the slurries of this invention the titanium dioxide content of the initial slurry shouad be at least 80 percent by weight so that the disc mill can impart sufficient shear into the sy~tem to assure reduction in agglomerate size o~ the titanium dioxide within the limits of this invention. Ideally the particle size will be aæ
i fine as possible with the average particle size of less than ; about o.6 micronæ with not more than 5 mass per cent of the titanium d~oxide particles or agglomerates, as the case ma~
be, with a particle size greater than one micron. Therefore, depending on the pigment base being employed the gFinding time and pigment concentration will be adJu~ted to achieve the desired particle ~ize uniPormity and distrlbution. It has also been disco~ered that addition of about ~ive percent water to the system after the grinding step resultæ ~n * denotes trade mark ,~
10~7775 improved rheological propertiec of the slurry and handling and use of the finished slurry is markedly enhanced.
It ha~ al~o been dlscovered that the use Or a sult-able dlspersant system ~ nece~ary to achle~e a tltanlum dloxlde slurry whlch lmparts outstandlng glos~ to a palnt ~llm derived rrom a water-~a~ed system. The dlsper~ant ~ystem comprl~ed Or 0.2 to 1 percent o~ a compound Or ~ormula I and rrom 0.1 to 0.6 percent Or 2-amlno-2-methyl-1-propanol, based on the welght o~ titanium dloxlde present, will when comblned wlth the other processing conditlons descrlbed herein produce a tltanlum d~o~ide slurry wlth an unexpectedly high level Or gloss ln a drled palnt f~lm.
The rollowlng examples are lllustratlve Or the inventlon. All parts and percentages are by welght unless otherwlse noted.
Example 1 Titanium dloxlde produced by the oxidation o~
tltanlum tetrachlorlde and about 1.0 per cent aluminum oxide in aqueous slurry of about 55-75 per cent by weight solids ls ~ed to a ~luid energy mill as described ln the example Or U. S. Patent 3,840,188 and dried and ~round using a steam to pigment ratlo Or rrom 2.5 to 6 as described therein to ~ro-duce dry tltanlum dioxide o~ uniform and small particle size.
~ ple 2 To 5,300 ml of water in a five-gallon container is added 150 ml of a compound of formula I in which M is Na, Rl to R4 are hydrogen and X and Y are carboxyl groups, and 60 ml of 2-amino-2-methyl propanol. To the above solu-tion is added 30,000 g of titanium dioxide pigment obtained as described in Example 1. Then a Hockmeyer disperser ` ~W77~5 fitted with a four-inch blade rotating at 4,000 rpm i8 employed to grind the pigment. After grinding for 20 min-utes, 3,000 ml of water is added to reduce the solid~
concentration in the slurry to about 76.7 percent by weight.
m e particle size of the solids i8 determined u~ing a Micrometrics* 5000 Analyzer which shows a mass percent of particles finer than:
Mass % Size (~)**
84 o.6 0.47 16 0.325
3.5 >1 33 ~0.4 ~* 8~ indicateæ that 84~ of the particles are o.65~ or smaller.
The slurry prepared in Example 2 is compared with a commerc~ally available high-gloss titanium dioxide for gloss and hiding power as described below.
Air ~ry Emulsion Gloss An acrylic emulsion paint 20 i8 prepared containing a 22.8 pigment volume concentration.
me acrylic emulsion paint is drswn down to a film thickness of .008 inch and is allowed to dry for a mini~um of three days and the glo88 (60) of the paint f~lm is then determined.
Oven Dry Emulsion Gloæs An acrylic emulsion paint is prepared containing a 25 pigment volume concentration.
The acrylic emulsion paint is drawn down to a film thickness of .004 inch and i8 immediately placed ~nto a 110C. dra~t ~ree oven for thirty minutes and the gloss (60) of the paint ~ilm is then determined.
Hiding Power The above acrylic emulsion paint prep-arations are drawn down to a film thickness of .0025 inch on * denotes trade mark ~o~ms Morest 09 chart and drled ror 24 hours. Hldlng power o~ the palnt prepared rrom the slurrles Or this lnventlon ls com-pared ~lth that o~ the control. The relatl~e hldlng power (H.P.) o~ the slurrles Or this lnventlon are calculated as ~ollows:
H p ~ SX o~ Test Sam~le X 100 SX o~ Control Sample SX - Scatterlng power determined accordlng to the method Or D. B. Judd, "Optlcal Speclrlcatlons Or Llght Scatterlng Materials", Journal Or Research o~ the National Bureau Or Standards, Vol. 19, 1937, p. 287.
Emulslon Gloss Alr Dr~ Oven Dry H.P.
Slurry Or Example 2 62 75 102 Control 49 56 100 Example 3 2-Amino-2-methyl propanol l45 ml) and a com-pound of formula I in which M is Na, Rl to R4 are hydrogen and X and Y are carboxyl groups (114 ml) are added to 7,200 ml of water in a five-gallon container. To this mix-ture is added 22,700 g of the titanium dioxide pigment pre-pared in accordance with Example 1. The resultant slurry is then ground with a Hockmeyer disperser fitted with a four-inch ~lade for 20 minutes at 1,500 rpm. After this grinding the solids content of the slurry is reduced with 2,500 ml of water to give a final slurry with a solids con-centration of 68.2.
The emulslon gloss and hiding power o~ the slurry Or Example 3 ls compared with that o~ a commerclal gloss pigment wlth the followlng resultæ:
~08~7s Emulsion Gloss Air Dry H.P.
Slurry of Example 3 64 99 Control 56 100 Example 4 Sixty milliliters of 2-amino-2-methyl propanol - and 240 ml of a compound of formula I in which M i8 Na, Rl to R4 are hydrogen and X and Y are carboxyl groups are added to 5,300 ml of water in a five-gallon container. To the above mixture is added 30,000 g of a titanium dioxide pigment obtalned as described ln Example 1. Then a Hochmeyer disperser ~ltted with a rour-inch blade rotating at 2,000 rpm ls employed to grlnd the pigment. Arter grlnd-ing for 20 minutes 3,500 ml Or water is added to reduce the solids concentration ln the slurry to about 77 percent by weight.
The particle size Or the solids present in the slurry is determined using a Micrometrics 5000 Analyzer which shows a mass percent Or particles riner than:
Mass S Size (~) 84 0.51 .375 16 0.245 2.0 ~1 58 <0.4 The gloss and hlding power Or the slurry o~
Example 4 ls compared wlth that of a commerical ~loss pig-ment as described above with the rollowing results:
Emulsion Gloss Air Dry H.P.
Slurry Or Example 4 64 99 Control 49 100 _g_ ~os777s The rollowing examples are preQented to demon-strate that the high-sollds grlnd rollowed by dllutlon to a sollds concentratlon wlthln the range o~ 60 to 80 percent solids wlll produce a slurry whlch provldes lmproved gloss when compared to the same plgment which ls drled conven-tionally and lncorporated dlrectly lnto the palnt system.
; Example 5 Fifty-four milliliters of 2-amino-2-methyl pro-panol and 185 ml of a compound of formula I in which M is Na, Rl to R4 are hydrogen and X and Y are carboxyl groups a~e added to 2,930 ml of water. To the above mixture is added 18,000 g titanium dioxide pigment upon which has been precipitated 0.2 percent alumina. Then a Hochmeyer dis-perser fitted with a four-inch blade rotating at 2,000 rpm iæ employed to grind the pigment. After grinding for 20 minutes 1,800 ml of water is added to reduce the solids content of the slurry to 79 percent by weight.
The partlcle slze Or the sollds is determined using a Micrometrics 5000 Analyzer which shows a mass percent o~ particles ~iner than:
Mass S Slze (~) 84 0.54 0.35 16 0.245
The slurry prepared in Example 2 is compared with a commerc~ally available high-gloss titanium dioxide for gloss and hiding power as described below.
Air ~ry Emulsion Gloss An acrylic emulsion paint 20 i8 prepared containing a 22.8 pigment volume concentration.
me acrylic emulsion paint is drswn down to a film thickness of .008 inch and is allowed to dry for a mini~um of three days and the glo88 (60) of the paint f~lm is then determined.
Oven Dry Emulsion Gloæs An acrylic emulsion paint is prepared containing a 25 pigment volume concentration.
The acrylic emulsion paint is drawn down to a film thickness of .004 inch and i8 immediately placed ~nto a 110C. dra~t ~ree oven for thirty minutes and the gloss (60) of the paint ~ilm is then determined.
Hiding Power The above acrylic emulsion paint prep-arations are drawn down to a film thickness of .0025 inch on * denotes trade mark ~o~ms Morest 09 chart and drled ror 24 hours. Hldlng power o~ the palnt prepared rrom the slurrles Or this lnventlon ls com-pared ~lth that o~ the control. The relatl~e hldlng power (H.P.) o~ the slurrles Or this lnventlon are calculated as ~ollows:
H p ~ SX o~ Test Sam~le X 100 SX o~ Control Sample SX - Scatterlng power determined accordlng to the method Or D. B. Judd, "Optlcal Speclrlcatlons Or Llght Scatterlng Materials", Journal Or Research o~ the National Bureau Or Standards, Vol. 19, 1937, p. 287.
Emulslon Gloss Alr Dr~ Oven Dry H.P.
Slurry Or Example 2 62 75 102 Control 49 56 100 Example 3 2-Amino-2-methyl propanol l45 ml) and a com-pound of formula I in which M is Na, Rl to R4 are hydrogen and X and Y are carboxyl groups (114 ml) are added to 7,200 ml of water in a five-gallon container. To this mix-ture is added 22,700 g of the titanium dioxide pigment pre-pared in accordance with Example 1. The resultant slurry is then ground with a Hockmeyer disperser fitted with a four-inch ~lade for 20 minutes at 1,500 rpm. After this grinding the solids content of the slurry is reduced with 2,500 ml of water to give a final slurry with a solids con-centration of 68.2.
The emulslon gloss and hiding power o~ the slurry Or Example 3 ls compared with that o~ a commerclal gloss pigment wlth the followlng resultæ:
~08~7s Emulsion Gloss Air Dry H.P.
Slurry of Example 3 64 99 Control 56 100 Example 4 Sixty milliliters of 2-amino-2-methyl propanol - and 240 ml of a compound of formula I in which M i8 Na, Rl to R4 are hydrogen and X and Y are carboxyl groups are added to 5,300 ml of water in a five-gallon container. To the above mixture is added 30,000 g of a titanium dioxide pigment obtalned as described ln Example 1. Then a Hochmeyer disperser ~ltted with a rour-inch blade rotating at 2,000 rpm ls employed to grlnd the pigment. Arter grlnd-ing for 20 minutes 3,500 ml Or water is added to reduce the solids concentration ln the slurry to about 77 percent by weight.
The particle size Or the solids present in the slurry is determined using a Micrometrics 5000 Analyzer which shows a mass percent Or particles riner than:
Mass S Size (~) 84 0.51 .375 16 0.245 2.0 ~1 58 <0.4 The gloss and hlding power Or the slurry o~
Example 4 ls compared wlth that of a commerical ~loss pig-ment as described above with the rollowing results:
Emulsion Gloss Air Dry H.P.
Slurry Or Example 4 64 99 Control 49 100 _g_ ~os777s The rollowing examples are preQented to demon-strate that the high-sollds grlnd rollowed by dllutlon to a sollds concentratlon wlthln the range o~ 60 to 80 percent solids wlll produce a slurry whlch provldes lmproved gloss when compared to the same plgment which ls drled conven-tionally and lncorporated dlrectly lnto the palnt system.
; Example 5 Fifty-four milliliters of 2-amino-2-methyl pro-panol and 185 ml of a compound of formula I in which M is Na, Rl to R4 are hydrogen and X and Y are carboxyl groups a~e added to 2,930 ml of water. To the above mixture is added 18,000 g titanium dioxide pigment upon which has been precipitated 0.2 percent alumina. Then a Hochmeyer dis-perser fitted with a four-inch blade rotating at 2,000 rpm iæ employed to grind the pigment. After grinding for 20 minutes 1,800 ml of water is added to reduce the solids content of the slurry to 79 percent by weight.
The partlcle slze Or the sollds is determined using a Micrometrics 5000 Analyzer which shows a mass percent o~ particles ~iner than:
Mass S Slze (~) 84 0.54 0.35 16 0.245
4,0 >1 <0.4 The air dried gloss and hidin~ power of the slurrv ~f Example 5 is compared with that of a commercial ~loss pigment as described above with the following results:
~ulgion alo8~
_ Alr Dry ~.P.
Slurr~ Or ExaD~le 5 67~71~ 101 Control 60/49~ 100 repeat Or glo~ test ~xa~ple 6 Fl~ty-~our millillters Or 2-amlno-2-methrl propanol and 145 ml o~ a co~pound o~ ~or~ula I in ~hich M i~ Na, Rl to R4 are hJdrogon and X and ~ are earbo~l groups aro added to 3,200 ~1 Or ~ater. To the abo~e ~ixturo i~ addea 18,000 g Or t~tanium dtoxlde ~hich ha~ not been surrace troated. Then a -Hoekme~er dlsparser ritted wlth a four-in¢h blade rot~tlng at 2,0Q0 rpm i~ emplored to ~rind the pigmRnt. A~ter grinding ~or 20 minutes 1,800 ml o~ water 18 added to reduce the solid~ content to 78.5 percent b~ ~eight.
particle ~lze of the solld~ in the ~lurry ~eter~ined asln~ a Mlcro~etric~ 5000 Analyzer which ~ho~ a ma~ pereent o~ partleles riner than:
~a~ % Size (p) 84 .43 0.31 16 0.225 2.0 >1 80.0 ~o.4 The glo88~ e~ulslon glosJ and hidl4g po~er o~ tho ~lurry o~ k~mple 6 1~ comparod ~ith a co~merc~al glo~- pig-~ent as described aboY~ ~ith the rollo~ing result~:
~ulsion Glo~s Alr J~ O~n nr~ ~P.
Slurr~ o~ Exa~pl- 6 66~73~ 73 97 Control 60/64~ 56 lO0 ~ rey-at o~ glo~ tost
~ulgion alo8~
_ Alr Dry ~.P.
Slurr~ Or ExaD~le 5 67~71~ 101 Control 60/49~ 100 repeat Or glo~ test ~xa~ple 6 Fl~ty-~our millillters Or 2-amlno-2-methrl propanol and 145 ml o~ a co~pound o~ ~or~ula I in ~hich M i~ Na, Rl to R4 are hJdrogon and X and ~ are earbo~l groups aro added to 3,200 ~1 Or ~ater. To the abo~e ~ixturo i~ addea 18,000 g Or t~tanium dtoxlde ~hich ha~ not been surrace troated. Then a -Hoekme~er dlsparser ritted wlth a four-in¢h blade rot~tlng at 2,0Q0 rpm i~ emplored to ~rind the pigmRnt. A~ter grinding ~or 20 minutes 1,800 ml o~ water 18 added to reduce the solid~ content to 78.5 percent b~ ~eight.
particle ~lze of the solld~ in the ~lurry ~eter~ined asln~ a Mlcro~etric~ 5000 Analyzer which ~ho~ a ma~ pereent o~ partleles riner than:
~a~ % Size (p) 84 .43 0.31 16 0.225 2.0 >1 80.0 ~o.4 The glo88~ e~ulslon glosJ and hidl4g po~er o~ tho ~lurry o~ k~mple 6 1~ comparod ~ith a co~merc~al glo~- pig-~ent as described aboY~ ~ith the rollo~ing result~:
~ulsion Glo~s Alr J~ O~n nr~ ~P.
Slurr~ o~ Exa~pl- 6 66~73~ 73 97 Control 60/64~ 56 lO0 ~ rey-at o~ glo~ tost
Claims (5)
1. An aqueous slurry of titanium dioxide pigment to provide a high-gloss finish to paint films derived from acrylic water-based systems, said slurry containing from 60 to 80 percent titanium dioxide, from 0.2 to 1 percent of a compound selected from the formula where M is alkali metal, R1 to R4 is H, -CH3 or C2H5, X is -CN or -COOR5 where R5 is hydrogen or lower alkyl of 1-4 carbon atoms, Y is -COOH or -COONa, and a and b are 10 to 100, from 0.1 to 0.6 percent of 2-amino-2-methyl-1-propanol and the remainder water.
2. An aqueous slurry of Claim 1 which contains from 70 to 80 percent by weight of titanium dioxide.
3. An aqueous slurry of Claim 1 which contains from 75 to 79 percent by weight titanium dioxide.
4. A process for producing high solids content titanium dioxide aqueous slurry which comprises preparing solution of 0.2 to 1 percent of a compound of the formula where M is sodium, R1 to R4 is H, X is -COOH, Y is -COOH or -COONa, and a and b are 10 to 100, from 0.1 to 0.6 percent 2-amino-2-methyl-1-propanol in from 10 to 20 percent of water, the percentages being based upon the weight of the titanium dioxide present, adding from 80 to 90 percent by weight of dry titanium dioxide, grinding with a disc mill until the titanium dioxide is uniformly dispersed and then adding sufficient water to reduce the titanium dioxide content to from 60 to 80 percent by weight of the finished slurry.
5. A process for producing high solids content titanium dioxide aqueous slurry which comprises (a) drying and grinding titanium dioxide pigment prepared by the oxidation of titanium tetrachloride in a confined vortex fluid energy mill;
(b) preparing a solution of 0.2 to 1 percent, based on the weight of titanium dioxide, of a compound of the formula where M is alkali metal, R1 to R4 is H, -CH3 or C2H5, X is -CN or -COOR5 where R5 is H or alkyl of 1-4 carbon atoms, Y is -COOH or -COONa, and a and b are 10 to 100 and 0.1 to 0.6 percent, based on the weight of titanium dioxide, 2-amino-2-methyl-1-propanol in from 10 to 20 per-cent by weight of the slurry of water;
(c) adding from 80 to 90 percent by weight of the titanium dioxide of step (a) to form a slurry;
(d) grinding the slurry with a disc mill until the titanium dioxide is uniformly dispersed and is of an average particle size of less than about 0.6 micron with not more than five mass percent of the particles having an average particle size of greater than one micron;
(e) adding sufficient water to reduce the titanium dioxide content to from 75 to 79 percent by weight of the finished slurry; and (f) mixing the slurry until smooth and uniform.
(b) preparing a solution of 0.2 to 1 percent, based on the weight of titanium dioxide, of a compound of the formula where M is alkali metal, R1 to R4 is H, -CH3 or C2H5, X is -CN or -COOR5 where R5 is H or alkyl of 1-4 carbon atoms, Y is -COOH or -COONa, and a and b are 10 to 100 and 0.1 to 0.6 percent, based on the weight of titanium dioxide, 2-amino-2-methyl-1-propanol in from 10 to 20 per-cent by weight of the slurry of water;
(c) adding from 80 to 90 percent by weight of the titanium dioxide of step (a) to form a slurry;
(d) grinding the slurry with a disc mill until the titanium dioxide is uniformly dispersed and is of an average particle size of less than about 0.6 micron with not more than five mass percent of the particles having an average particle size of greater than one micron;
(e) adding sufficient water to reduce the titanium dioxide content to from 75 to 79 percent by weight of the finished slurry; and (f) mixing the slurry until smooth and uniform.
Applications Claiming Priority (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US75346076A | 1976-12-22 | 1976-12-22 | |
| US753,460 | 1976-12-22 | ||
| US85767677A | 1977-12-05 | 1977-12-05 | |
| US857,676 | 1977-12-05 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CA1087775A true CA1087775A (en) | 1980-10-14 |
Family
ID=27115747
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CA293,437A Expired CA1087775A (en) | 1976-12-22 | 1977-12-20 | Titanium dioxide pigment slurries to impart high gloss to water-based paint systems |
Country Status (10)
| Country | Link |
|---|---|
| JP (1) | JPS5388826A (en) |
| BR (1) | BR7708564A (en) |
| CA (1) | CA1087775A (en) |
| DE (1) | DE2757227A1 (en) |
| FR (1) | FR2375308B1 (en) |
| GB (1) | GB1596999A (en) |
| IE (1) | IE46124B1 (en) |
| IT (1) | IT1114193B (en) |
| MX (1) | MX148379A (en) |
| NL (1) | NL7714259A (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS59172559A (en) * | 1983-03-22 | 1984-09-29 | Onahama Sakai Kagaku Kk | Production of water paint |
| JPS59172560A (en) * | 1983-03-22 | 1984-09-29 | Onahama Sakai Kagaku Kk | Water paint composition |
| JPS601268A (en) * | 1983-05-26 | 1985-01-07 | Onahama Sakai Kagaku Kk | Water-soluble paint composition |
| GB8829402D0 (en) * | 1988-12-16 | 1989-02-01 | Tioxide Group Plc | Dispersion |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3758322A (en) * | 1971-07-21 | 1973-09-11 | American Cyanamid Co | Rutile tio2 slurries |
| DE2416720A1 (en) * | 1974-04-05 | 1975-10-23 | Bayer Ag | HIGH SOLID TITANIUM PIGMENT SUSPENSION |
-
1977
- 1977-12-20 CA CA293,437A patent/CA1087775A/en not_active Expired
- 1977-12-21 GB GB53164/77A patent/GB1596999A/en not_active Expired
- 1977-12-21 IE IE2600/77A patent/IE46124B1/en unknown
- 1977-12-22 FR FR7738798A patent/FR2375308B1/fr not_active Expired
- 1977-12-22 IT IT31148/77A patent/IT1114193B/en active
- 1977-12-22 NL NL7714259A patent/NL7714259A/en not_active Application Discontinuation
- 1977-12-22 JP JP15365077A patent/JPS5388826A/en active Pending
- 1977-12-22 BR BR7708564A patent/BR7708564A/en unknown
- 1977-12-22 DE DE19772757227 patent/DE2757227A1/en not_active Withdrawn
-
1978
- 1978-01-02 MX MX171883A patent/MX148379A/en unknown
Also Published As
| Publication number | Publication date |
|---|---|
| IT1114193B (en) | 1986-01-27 |
| BR7708564A (en) | 1978-08-22 |
| FR2375308B1 (en) | 1982-12-03 |
| GB1596999A (en) | 1981-09-03 |
| NL7714259A (en) | 1978-06-26 |
| DE2757227A1 (en) | 1978-07-06 |
| IE46124B1 (en) | 1983-02-23 |
| JPS5388826A (en) | 1978-08-04 |
| FR2375308A1 (en) | 1978-07-21 |
| MX148379A (en) | 1983-04-18 |
| IE46124L (en) | 1978-06-22 |
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