Pigment preparations in granule form

Details Pigment preparations in granule form Pigment preparations in granule form

1999-09-07

2001-09-04

Green, Anthony (Department: 1755)

Compositions: coating or plastic

Materials or ingredients

Pigment, filler, or aggregate compositions, e.g., stone,...

C106S412000, C106S433000, C106S447000, C106S494000, C106S495000, C106S496000, C106S497000, C106S498000, C106S499000

Reexamination Certificate

active

06284035

ABSTRACT:

The present invention relates to novel pigment preparations in granule form comprising as essential constituents
from 50 to 99.5% by weight of at least one inorganic pigment and
from 0.5 to 50% by weight of at least one organic pigment.
This invention further relates to the production of these pigment preparations and to their use for coloring polymeric materials.
As known from EP-A-816 440, combining bismuth vanadate with organic pigments gives pigments having high chroma values. Disclosed are pulverulent mixtures of these pigments, which are prepared by dry-milling the finished pigments.
Yet pulverulent pigment preparations have the disadvantage of leading to a pronounced dust nuisance in handling and of exhibiting unsatisfactory flowability in the case of container shipments.
It is an object of the present invention to remedy these defects and to provide pigment preparations having advantageous application properties.
We have found that this object is achieved by pigment preparations in granule form comprising as essential constituents
from 50 to 99.5% by weight of at least one inorganic pigment and
from 0.5 to 50% by weight of at least one organic pigment.
This invention further provides a process for producing pigment preparations which comprises conjointly wet-milling the as synthesized crude pigments and subsequently drying the pigment suspension millbase with agitation.
This invention also provides for the use of the pigment preparations for coloring polymeric systems.
The pigment preparations of the invention preferably comprise an inorganic pigment selected from a bismuth vanadate pigment, a lead chromate pigment, a cerium sulfide pigment, a rutile pigment or a spinel pigment or a mixture thereof; it will be appreciated that mixtures of pigments of the same class may also be present.
Particularly preferred inorganic pigments are bismuth vanadate pigments and rutile pigments.
Preferred organic pigments for the pigment preparations of the invention are anthraquinone pigments, anthrapyrimidine pigments, azo pigments, azomethine pigments, quinacridone pigments, quinophthalone pigments, diketopyrrolopyrrole pigments, indanthrone pigments, isoindoline pigments, isoindolinone pigments, metal complex pigments, perinone pigments, perylene pigments, phthalocyanine pigments, pyranthrone pigments, pyrazoloquinazolone pigments and thioindigo pigments and also mixtures thereof.
Particularly preferred organic pigments are isoindoline pigments and quinophthalone pigments.
The pigment preparations of the invention are of particular interest for yellow, orange, red and green hues, so that they generally comprise mixtures of multiple yellow pigments or mixtures of yellow pigments with orange pigments, red pigments, brown pigments and/or blue pigments.
The pigment preparations of the invention preferably comprise two or three different pigments. It will be appreciated that they may also comprise a greater number of pigments.
Specific examples of particularly suitable pigments are:
bismuth vanadate pigments:
C.I. Pigment Yellow 184;
lead chromate pigments:
C.I. Pigment Yellow 34; C.I. Pig-
ment Red 104;
cerium sulfide pigments:
C.I. Pigment Orange 75; C.I. Pig-
ment Red 265;
rutile pigments:
C.I. Pigment Yellow 53, 157, 158,
159, 160, 161, 162, 163, 164 and
189; C.I. Pigment Brown 24 and 33;
spinel pigments:
C.I. Pigment Yellow 119; C.I.
Pigment Brown 33, 34, 35, 37, 39
and 40; C.I. Pigment Blue 28, 36
and 72;
anthraquinone pigments:
C.I. Pigment Yellow 147 and 199;
anthrapyrimidine pigments:
C.I. Pigment Yellow 108;
azo pigments:
C.I. Pigment Yellow 3, 13, 62,
74, 151, 168 and 191:1; C.I.
Pigment Orange 5, 13, 34, 36, 64
and 67; C.I. Pigment Red 1, 2, 3,
4, 5, 23, 48:1, 48:2, 48:3, 48:4,
49, 49:1, 51:1, 52:1, 53:1,
57:1, 58:2, 58:4, 112, 144, 146,
148, 166, 170, 214, 220, 221
and 251;
azomethine pigments:
C.I. Pigment Yellow 129;
quinacridone pigments:
C.I. Pigment Orange 48 and 49;
C.I. Pigment Red 42, 122, 202
and 206;
quinophthalone pigments:
C.I. Pigment Yellow 138;
diketopyrrolopyrrole pigments:
C.I. Pigment Orange 71 and
73; C.I. Pigment Red 254,
255, 264, 270 and 272;
indanthrone pigments:
C.I. Pigment Blue 60 and 64;
isoindoline pigments:
C.I. Pigment Yellow 139 and 185;
C.I. Pigment Orange 61 and 69,
C.I. Pigment Red 260;
isoindolinone pigments:
C.I. Pigment Yellow 109, 110 and
173;
metal complex pigments:
C.I. Pigment Yellow 117, 153 and
177;
perinone pigments:
C.I. Pigment Orange 43; C.I.
Pigment Red 194;
perylene pigments:
C.I. Pigment Red 123, 149, 178,
179, 190 and 224;
phthalocyanine pigments:
C.I. Pigment Blue 15, 15:1, 15:2,
15:3, 15:4, 15:6 and 16;
pyranthrone pigments:
C.I. Pigment Orange 51; C.I.
Pigment Red 216;
pyrazoloquinazolone pigments:
C.I. Pigment Orange 67; C.I.
Pigment Red 251;
thioindigo pigments:
C.I. Pigment Red 88.
Examples of particularly preferred pigments are C.I. Pigment Yellow 184 and 53 and C.I. Pigment Brown 24 and also C.I. Pigment Yellow 138 and 139.
The pigment preparations of the invention are present in granular form, the individual particles generally comprising both inorganic and organic pigment. In general, the granules are predominantly spherical and have a median size within the range from about 5 to 3000 &mgr;m, preferably within the range from 10 to 500 &mgr;m. The granule size customarily has no effect on the tinctorial properties of the pigment preparations of the invention in use.
The pigment preparations of the invention may with advantage be prepared with the aid of the process of the invention by conjointly wet-milling the as-synthesized crude pigments and subsequently drying the pigment suspension millbase with agitation.
The first process step of the conjoint wet milling is performed on the as-synthesized crude pigments. The as-synthesized crude pigments may be, for example, in the form of moist filter cakes or in the form of pigment clinkers obtained after a concluding calcination. The pigments may, if desired, already be coated with, for example, stabilizing coatings, but their particle size and shape is not finalized.
The milling is preferably carried out in an aqueous medium. However, suitable media also include organic solvents, which may be protic or aprotic, and also mixtures of these solvents with each or one another and/or with water. It is favorable to use the liquid used in the final wash of at least one of the crude pigments.
Examples of suitable protic organic solvents are monohydric aliphatic alcohols, especially C
2
-C
12
alcohols, and also polyhydric alcohols, especially C
2
-C
3
alkylene glycols, and ether alcohols, especially C
2
-C
3
alkylene glycol C
1
-C
4
alkyl ethers. Specific examples are ethanol, propanol, diethylene glycol and ethylene glycol monobutyl ether.
Examples of suitable aprotic organic solvents are cyclic ethers such as tetrahydrofuran.
The pigments are customarily used in the milling in the form of from 10 to 60% strength by weight suspensions in the solvents mentioned.
It will be appreciated that it is also possible for the pigments used to be accompanied by customary dispersing assistants (non-ionic, anionic or cationic surfactants), whose presence may also be favorable for the subsequent granulation. However, their proportion is customarily not more than 2% by weight, based on the pigments.
The milling may with advantage be effected in an unstirred ball mill or in a stirred ball mill, preferably operated at from 100 to 2000 rpm. Examples of suitable grinding media are glass beads, zirconia beads or sand grains from about 0.4 to 30 mm in diameter.
Milling is customarily carried on until the median pigment particle size (d
50
value) is within the range from about 0.4 to 2 &mgr;m, preferably from 0.8 to 1.5 &mgr;m.
After the grinding media have been removed, the pigment suspension obtained is subjected to the agitated drying of the invention.
Examples of apparatus suitable for the large industrial scale therefore include tumble dryers, paddle dryers and force cleaned contact dryers, in each of which the drying is preferably effected under reduced pressure (a pressure within the range

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