WO2004009688A2

WO2004009688A2 - Use of solid pigment preparations for colouring plastics

Info

Publication number: WO2004009688A2
Application number: PCT/EP2003/007591
Authority: WO
Inventors: Andreas Stohr; Hansulrich Reisacher; Juan Antonio Gonzalez Gomez; Heinrich Schmeisser; Uemit Z. Hancer
Original assignee: Basf Aktiengesellschaft
Priority date: 2002-07-19
Filing date: 2003-07-14
Publication date: 2004-01-29
Also published as: AU2003250052A8; WO2004009688A3; DE10233081A1; AU2003250052A1

Abstract

The invention relates to the use of solid pigment preparations for colouring plastics, said preparations containing the following as essential constituents: (A) between 60 and 90 wt. % of at least one pigment; and (B) between 10 and 40 wt % of at least one surface-active additive from the group of non-ionic polyethers, their acidic phosphoric acid esters, phosphonic acid esters, sulphuric acid esters and/or sulphonic acid esters and their salts.

Description

Use of solid pigment preparations for coloring plastics

description

The present invention relates to the use of solid pigment preparations, which are essential components

(A) 60 to 90% by weight of at least one pigment and

(B) 10 to 40% by weight of at least one surface-active additive from the group of the nonionic polyethers and their acidic phosphoric, phosphonic, sulfuric and / or sulfonic esters and their salts

included, for coloring plastics.

The invention further relates to a method for coloring plastics.

Powder pigments are usually used to color plastics. The complete dispersion of the pigments in the plastic is a prerequisite for the development of maximum color strength and coloring effect. Such a dispersion requires appropriate know-how and a high input of shear energy and is therefore expensive. If the plastics processor does not have this know-how and the necessary complex and expensive dispersing devices, the colored plastics often have so-called pigment specks, i.e. pigment agglomerates that are not completely dispersed, on ,, are difficult to spin and / or have high pressure filter values.

Many plastics processors therefore use so-called masterbatches for coloring plastics. A masterbatch is a usually solid, concentrated pigment preparation in a meltable plastic matrix that is solid at room temperature, in which the powdered pigment is dispersed and thus finely distributed, i.e. the energy required to disperse the powder pigment was already used in the manufacture of the

Masterbatches applied. With the help of these masterbatches, the plastics processor can color the plastics without much energy consumption and at the same time obtain more consistent coloring results with regard to color strength and shade. From EP-A-1 081 195 granular pigment preparations for coloring plastics are known which contain nonionic polyethylene waxes as additives. These pigment preparations are produced by bringing the pigments into contact with the waxes during solvent finishing and spray drying. However, this manufacturing process is only applicable to organic pigments that are finished in organic solvents.

Furthermore, the older German patent applications 10204304.3 and 10204583.6, 10227657.9 and 10228199.8 describe the use of solid pigment preparations which contain nonionic surface-active additives based on polyethers or mixtures of these additives with anionic surface-active additives based on appropriately modified polyethers.

The object of the invention was to provide pigment preparations with which plastics of the most varied types can advantageously be colored.

Accordingly, the use of solid pigment preparations, which are essential components

(A) 60 to 90% by weight of at least one pigment and

(B) 10 to 40% by weight of at least one surface-active additive from the group of the nonionic polyethers and their acidic phosphoric, phosphonic, sulfuric and / or

Sulfonic acid esters and their salts

included, found for coloring plastics.

A process for coloring plastics was also found, which is characterized in that these pigment preparations are incorporated into the plastics by extrusion, rolling, kneading or grinding.

The pigment preparations to be used according to the invention contain at least one pigment as component (A) and at least one nonionic surface-active additive based on polyethers or at least one anionic surface-active agent based on the acidic phosphoric, phosphonic, sulfuric acid as component (B) - Or sulfonic acid esters of the polyethers or their salts (B) or a mixture of these non-ionic and anionic surface-active additives. Organic or inorganic pigments may be present as component (A) in the pigment preparations to be used according to the invention. The pigment preparations can of course also contain mixtures of different organic or different inorganic pigments or mixtures of organic and inorganic pigments.

The pigments are in finely divided form. Accordingly, the pigments usually have average particle sizes of 0.1 to 5 μm, in particular 0.1 to 3. μm and especially 0.1 to 1 μm. The organic pigments are usually organic colored and black pigments. Inorganic pigments can also be color pigments (colored, black and white pigments) as well as gloss pigments and the inorganic pigments usually used as fillers.

The following are examples of suitable organic color pigments:

- Monoazo pigments: C.I. Pigment brown 25;

C.I. Pigment Orange 5, 13, 36, 38, 64 and 67;

C.I. Pigment Red 1, 2, 3, 4, 5, 8, 9,

12, 17, 22, 23, 31, 48: 1, 48: 2, 48: 3,

48: 4, 49, 49: 1, 51: 1, 52: 1, 52: 2, 53,

53: 1, 53: 3, 57: 1, 58: 2, 58: 4, 63, 112,

146, 148, 170, 175, 184, 185, 187,

191: 1, 208, 210, 245, 247 and 251;

C.I. Pigment Yellow 1, 3, 62, 65, 73,

74, 97, 120, 151, 154, 168, 181, 183 and

191;

C.I. Pigment violet 32;

- Disazo pigments: C.I. Pigment Orange 16, 34, 44 and 72; C.I. Pigment Red 144, 166, 214, 220, 221 and 242;

C.I. Pigment Yellow 12, 13, 14, 16, 17, 81, 83, 106, 113, 126, 127, 155, 174, 176, 180 and 188;

Disazo condensation pigments: C.I. Pigment Yellow 93, 95 and 128;

CI Pigment Red 144, 166, 214, 220 ^' , 242 and 262;

CI Pigment Brown 23 and 41; - Anthanthrone pigments: CI Pigment Red 168;

- Anthraquinone pigments: C.I. Pigment Yellow 147, 177 and 199;

C.I. Pigment violet 31;

- Anthrapyrimidine pigments: C.I. Pigment yellow 108;

- Quinacridone pigments: C.I. Pigment Orange 48 and 49; C.I. Pigment Red 122, 202, 206 and 209;

C.I. Pigment violet 19;

- Quinophthalone pigments: C.I. Pigment yellow 138;

- Diketopyrrolopyrrole pigments: C.I. Pigment Orange 71, 73 and 81;

C.I. Pigment Red 254, 255, 264, 270 and

272;

- Dioxazine pigments: C.I. Pigment violet 23 and 37; C.I. Pigment blue 80;

- Flavanthrone pigments: C.I. Pigment yellow 24;

- Indanthrone pigments: C.I. Pigment Blue 60 and 64;

- Isoindoline pigments: C.I. Pigments Orange 61 and 69;

C.I. Pigment Red 260;

C.I. Pigment Yellow 139 and 185;

- Isoindolinone pigments: C.I. Pigment Yellow 109, 110 and 173;

- Isoviolanthrone Pigments: C.I. Pigment violet 31;

- Metal complex pigments: C.I. Pigment Red 257;

C.I. Pigment Yellow 117, 129, 150, 153 and 177;

C.I. Pigment green 8;

- Perinone pigments: C.I. Pigment orange 43; C.I. Pigment Red 194;

- Perylene pigments: C.I. Pigment black 31 and 32;

C.I. Pigment Red 123, 149, 178, 179, 190 and 224;

CI Pigment Violet 29; Phthalocyanine Pigments: CI Pigment Blue 15, 15: 1, 15: 2, 15: 3, 15: 4, 15: 6 and 16; CI Pigment Green 7 and 36;

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 and 181;

C.I. Pigment violet 38;

- Triarylcarbonium pigments: C.I. Pigment Blue 1, 61 and 62;

C.I. Pigment green 1;

C.I. Pigment Red 81, 81: 1 and 169;

C.I. Pigment violet 1, 2, 3 and 27;

- C.I. Pigment Black 1 (aniline black);

- C.I. Pigment Yellow 101 (Aldazine Yellow);

- C.I. Pigment Brown 22

Suitable inorganic color pigments are e.g.

- White pigments: titanium dioxide (C.I. Pigment White 6), zinc white, colored zinc oxide; Zinc sulfide, lithopone;

- black pigments: iron oxide black (C.I. Pigment Black 11),

Iron-manganese black, spinel black (C.I. Pigment Black 27); Carbon black (C.I. Pigment Black 7);

- Colored pigments: chromium oxide, chromium oxide hydrate green; Chrome green (C.I. Pigment Green 48); Cobalt green (C.I. Pigment Green 50); Ultramarine green;

Cobalt blue (CI. Pigment Blue 28 and 36; CI Pigment Blue 72); Ultramarine blue; Manganese blue; Ultramarine violet; Cobalt and manganese violet;

Iron oxide red (C.I. Pigment Red 101); Cadmium sulfoselenide (C.I. Pigment Red

108); Cerium sulfide (C.I. Pigment Red 265); Molybdate red (C.I. Pigment Red 104); ultramarine;

Iron oxide brown (C.I. Pigment Brown 6 and

7), mixed brown, spinel and corundum phases (C.I. Pigment Brown 29, 31, 33, 34, 35, 37, 39 and 40), chrome titanium yellow (C.I. Pigment Brown 24), chrome orange;

Cerium sulfide (C.I. Pigment Orange 75); Iron oxide yellow (C.I. Pigment Yellow 42); Nickel titanium yellow (C.I. Pigment Yellow 53; C.I. Pigment Yellow 157, 158, 159, 160, 161, 162, 163, 164 and 189); Chromium titanium yellow; Spinel phases (C.I. Pigment Yellow 119); Cadmium sulfide and cadmium zinc sulfide (C.I. Pigment Yellow 37 and 35); Chrome yellow (C.I. Pigment Yellow 34); Bismuth vanadate (C.I. Pigment Yellow 184).

Examples of inorganic pigments commonly used as fillers are transparent silicon dioxide, quartz powder, aluminum oxide, aluminum hydroxide, natural mica, natural and precipitated chalk and barium sulfate.

The luster pigments are single-phase or multi-phase platelet-shaped pigments whose play of colors is • characterized by the interplay of interference, reflection and absorption phenomena. Examples include aluminum flakes and aluminum, iron oxide and mica flakes coated one or more times, in particular coated with metal oxides.

The solid pigment preparations to be used according to the invention contain, as component (B), surface-active additives based on polyethers, which can be modified nonionically or anionically. Different nonionic and different anionic additives as well as mixtures of nonionic and anionic additives can be contained. Anionic surface-active additives are the acidic phosphoric acid, phosphonic acid, sulfuric acid and / or sulfonic acid esters of the polyethers and / or their salts.

The nonionic surface-active additives based on polyether are, in particular, polyalkylene oxides or reaction products of alkylene oxides with alcohols, amines, aliphatic carboxylic acids or aliphatic carboxylic acid amides. According to the invention, the term alkylene oxide should also be understood to mean aryl-substituted alkylene oxide, in particular phenyl-substituted ethylene oxide.

In addition to the unmixed polyalkylene oxides, preferably CC alkylene oxides and phenyl-substituted C ₂ -C alkylene oxides, such as polyethylene oxides, polypropylene oxides and poly (phenyl ethylene oxides), alkylene oxide block copolymers, but also random copolymers of these alkylene oxides, are particularly suitable as component (B).

Block copolymers which have polypropylene oxide and polyethylene oxide blocks or else poly (phenylethylene oxide) and polyethylene oxide blocks are very particularly suitable. Like the unmixed polyalkylene oxides, they can be obtained by polyaddition of the alkylene oxides to starter compounds, such as saturated or unsaturated aliphatic and aromatic alcohols, saturated or unsaturated aliphatic and aromatic amines, saturated or unsaturated aliphatic carboxylic acids and carboxamides. When using ethylene oxide and propylene oxide, these starter compounds can first be reacted with ethylene oxide and then with propylene oxide or preferably first with propylene oxide and then with ethylene oxide. Usually 1 to 300 ol, preferably 3 to 150 ol, of alkylene oxide are used per mol of starter molecule.

Suitable aliphatic alcohols generally contain 6 to 26 carbon atoms, preferably 8 to 18 carbon atoms, and can be unbranched, branched or cyclic. Examples include octanol, nonanol, decanol, isodecanol, undecanol, dodecanol, 2-butyloctanol, tridecanol, isotridecanol, tetra-decanol, pentadecanol, hexadecanol, 2-hexyl ecanol, heptadecanol, octadecanol, 2-heptylundecanol, 2-octyldecanol and 2-octyldecanol. Nonyltridecanol, 2-decyltetradecanol, oleyl alcohol and 9-octadecenol and also mixtures of these alcohols such as Cg / Cio- / C ₁₃ / C ₁₅ - and Ciβ / Ciβ-alcohols, and cyclopentanol and cyclohexanol. Of particular interest are the saturated and unsaturated fatty alcohols, which are obtained from natural raw materials through fat splitting and reduction, and the synthetic fatty alcohols from oxosynthesis. The alkylene oxide adducts with these alcohols usually have average molecular weights M _n of 200 to 5000, especially 400 to 2000.

5 Examples of the above-mentioned aromatic alcohols include, in addition to - and ß-naphthol and their C 1 -C 4 -alkyl derivatives, especially phenol and its Cχ-Ci ₂ alkyl derivatives, such as hexylphenol, heptylphenol, octylphenol, nonylphenol, isononylphenol, undecylphenol, dodecylphenol, Di- and tributylphenol and dinonylphenol 10 called.

Suitable aliphatic amines correspond to the aliphatic alcohols listed above. Here too, the saturated and unsaturated fatty amines, which preferably have 14 to 15 20 C atoms, are of particular importance. Aniline and benzidine and their derivatives may be mentioned as aromatic amines.

Suitable aliphatic carboxylic acids are, in particular, saturated and unsaturated fatty acids, which preferably contain 14 to 20 C atoms, and hydrogenated, partially hydrogenated and unhydrogenated resin acids and also polyvalent carboxylic acids, e.g. Dicarboxylic acids such as maleic acid.

Suitable carboxamides are derived from these carboxylic acids 25.

In addition to the alkylene oxide adducts with these monohydric amines and alcohols, the alkylene oxide adducts with at least bifunctional amines and alcohols are of particular interest.

30

Preferred at least bifunctional amines are di- to pentavalent amines, which in particular have the formula H ₂ N- (R-NR ¹ ) _n -H (R: C ₂ -C ₆ alkylene; R ¹ : hydrogen or Ci-C _δ - Alkyl; n: 1 to 5) correspond. Examples include: ethylenediamine,

35 diethylene triamine, triethylene tetramine, tetraethylene pentamine,

Propylenediamine-1,3, dipropylenetriamine, 3-amino-l-ethyleneaminopropane, hexamethylenediamine, dihexamethylenetriamine, 1,6-bis (3-aminopropylamino) hexane and N-methyldipropylenetriamine, with hexamethylenediamine and diethylenetriamine being particularly preferred and

40 ethylenediamine is very particularly preferred.

These amines are preferably first reacted with propylene oxide and then with ethylene oxide. The ethylene oxide content of the block copolymers is usually about 10 to 90 5% by weight. The block copolymers based on polyvalent amines generally have average molecular weights M _n of 1,000 to 40,000, preferably 1,500 to 30,000.

Dihydric to pentavalent alcohols are preferred as at least bifunctional alcohols. Examples include C ₂ -C ₆ alkylene glycols and the corresponding di- and polyalkylene glycols, such as ethylene glycol, propylene glycol-1, 2 and -1.3, butylene glycol-1, 2 and -1.4, hexylene glycol-1,6, Dipropylene glycol and polyethylene glycol, glycerol and pentaerythritol and bisphenol-A are mentioned, ethylene glycol and polyethylene glycol being particularly preferred and propylene glycol and dipropylene glycol being very particularly preferred.

Particularly preferred alkylene oxide adducts with at least bifunctional alcohols have a central polypropylene oxide block, that is to say they start from a propylene glycol or polypropylene glycol which is first reacted with further propylene oxide and then with ethylene oxide. The ethylene oxide content of the block copolymers is usually from 10 to 90% by weight.

The block copolymers based on polyhydric alcohols generally have average molecular weights M _n of 1000 to 20,000, preferably 1000 to 15,000.

Such alkylene oxide block copolymers are known and commercially available e.g. available under the names Tetronic and Pluronic (BASF).

The anionic surface-active additives (B) are the sulfonates, sulfates, phosphonates and phosphates of the polyethers.

The polyethers can be converted into the phosphoric acid monoesters or diesters and phosphonic acid esters or the sulfuric acid monoesters and sulfonic acid esters by reaction with phosphoric acid, phosphorus pentoxide and phosphonic acid or sulfuric acid and sulfonic acid. These acidic esters are preferably in the form of water-soluble salts, especially as alkali metal salts, especially sodium salts, and ammonium salts, but they can also be used in the form of the free acids.

Preferred phosphates and phosphonates are derived primarily from alkoxylated, in particular ethoxylated, fatty and oxo alcohols, alkylphenols, fatty amines, fatty acids and resin acids, preferred sulfates and sulfonates are based in particular on alkoxylated, especially ethoxylated, fatty alcohols, alkyl alcohols. phenols and amines, including polyvalent amines, such as hexamethylene diamine.

Such anionic surface active additives are known and commercially available for example under the name Nekal ^® (BASF), Tamol ^® (BASF), Cro dafos ^® (Croda), Rhodafac ^® (Rhodia), Maphoε ^® (BASF), Texapon ^® (co gnis), Empicol ^® (Albright & Wilson), Matexil ^® (ICI), Soprophor ^® (Rhodia) and Lutensit ^® (BASF).

The pigment preparations to be used according to the invention contain 60 to 90% by weight, preferably 70 to 85% by weight, of the component

(A) and 10 to 40% by weight, preferably 15 to 30% by weight, of component (B).

The pigment preparations to be used in accordance with the invention can advantageously be prepared by initially pigmenting (A) in aqueous, at least part of, the additive (s)

(B) containing suspension is subjected to wet comminution and the suspension is then dried, optionally after addition of the remaining amount of additive (B).

The pigment (A) can be used as a dry powder or in the form of a press cake.

The pigment (A) used is preferably a finished product, i.e. the primary grain size of the pigment is already set to the value desired for the application. This pigment finish is particularly recommended for organic pigments, since the raw material obtained during pigment synthesis is generally not suitable for the application. In the case of inorganic pigments, e.g. in the case of oxide and bismuth vanadate pigments, the primary grain size can also be set during pigment synthesis, so that the pigment suspensions obtained can be used directly for the preparation of the pigment preparations to be used according to the invention.

Since the finished pigment (A) usually reaglomerates again during drying or on the filter unit, it is used to adjust the above-mentioned average particle sizes in aqueous suspension of continuous or discontinuous wet comminution, for example a stirrer, dissolver or high-pressure homogenization or grinding, in particular in an agitator ball mill. At least one part of the additive (B) contained in the finished pigment preparation should be present during the wet comminution, preferably the entire amount of additive (B) is added before the wet comminution.

Depending on the method chosen for drying the aqueous pigment suspension - spray granulation and fluidized-bed drying, spray drying, drying in a paddle dryer, evaporation and subsequent comminution - the particle size of the pigment preparations according to the invention can be controlled in a targeted manner.

In the case of spray and fluidized bed granulation, coarse-particle granules with average grain sizes of 50 to 5000 m, in particular 100 to 1000 μm, can be obtained. Spray drying usually gives granules with average grain sizes <20 μm. Finely divided preparations can be obtained by drying in a paddle dryer and by evaporation with subsequent grinding. However, the pigment preparations used according to the invention are preferably in granule form, the coarse-particle granules being particularly preferred.

The spray granulation is preferably carried out in a spray tower with a one-off nozzle. The suspension is sprayed here in the form of larger drops, the water evaporating. Daε or the additives (B) melt at the drying temperatures and thus lead to the formation of largely spherical granules with a particularly smooth surface (BET values of generally <15 m ² / g, in particular <10 m ² / g), which is preferred according to the invention.

The gas inlet temperature in the spray tower is generally from 180 to 300 ° C., preferably from 150 to 300 ° C. The gas outlet temperature is generally 70 to 150 ° C., preferably 70 to 130 ° C.

The residual moisture of the pigment granules obtained is generally <2% by weight.

The pigment preparations can advantageously be used for coloring all kinds of plastics. The following plastic classes and types are mentioned as examples: modified natural substances:

Duroplaεte, e.g. Caεein-Kunstεtoffe; Thermoplastics, e.g. Cellulose nitrate, cellulose acetate, mixed cellulose esters and cellulose ether;

Synthetic plastics:

Polycondensates: Duroplaεte, for example, phenol resin, urea resin, thiourea, melamine resin, unsaturated polyester resin, allyl resin, silicone, Poly I ^'mid and polybenzimidazole; Thermoplastics, for example polyamide, polycarbonate, polyester, polyphenylene oxide, polysulfone and polyvinyl acetal;

Polymers: thermoplastics, e.g. Polyolefins, such as polyethylene, polypropylene, poly-1-butene and poly-4-methyl-1-pentene, ionomers, polyvinyl chloride, polyvinylidene chloride, polymethyl methacrylate, polyacrylonitrile, polystyrene, polyacetal ', fluoroplastics, polyvinyl alcohol, polyvinyl acetate and polyvinyl p-xylylene and copolymers, such as ethylene / vinyl acetate copolymers, styrene / acrylonitrile copolymers, acrylonitrile / butadiene / styrene copolymers, polyethylene glycol terephthalate and polybutylene glycol terephthalate;

Polyadducts: Duroplaεte, e.g. Epoxy resin and cross-linked polyurethane; Thermoplastics, e.g. linear polyurethanes and chlorinated polyethers.

When incorporated into plastics, the solid pigment preparations to be used according to the invention are notable for their particularly easy dispersibility. This also applies in particular to the pigment preparations in granular form which are preferably to be used according to the invention and which are distinguished by the following additional advantageous properties: excellent abrasion resistance, low tendency to compact or clump, uniform particle size distribution, good debris, free-flowing and metering capacity and freedom from dust in handling and application. The plastics can advantageously with little energy input, e.g. by extruding them together (preferably using a single or twin screw extruder), rolling, kneading or grinding, with the pigment preparations. They can exist as plastic masses or melts and can be processed into plastic moldings, foils and fibers.

In addition, the solid pigment preparations to be used according to the invention are distinguished by generally advantageous application properties, especially good color properties, in particular particularly high color strength and brilliance, and the good rheological properties of the plastics colored with them, in particular low pressure filter values (high filter service life) and good spinnability.

Of course, they can be used for direct coloring of plastics as well as for coloring masterbatches and compounds. In direct plastic coloring, they are generally used in quantities of 0.1 to 5% by weight, based on the plastic to be colored. When coloring masterbatches, up to 70% by weight pigment preparation, based on the plastic to be colored, can be used , are used.

Examples

Manufacture of pigment preparations in granular form and their use for coloring plastics

The pigment granules were produced by a

Suspension of 80 kg of finished pigment (A) and x kg of additive (B) in 150 kg of water was ground in a ball mill to a dso value of <1 μ and then in a spray tower with a single-component nozzle (gas inlet temperature 170 ° C., gas outlet temperature 80 ° C) was spray granulated. In the case of the additive (B4), the suspension was% sodium hydroxide solution ^■ ^■ wt set before the ^'grinding by the addition of 25 .- a pH = 7.

The following additives were used:

B1: block copolymer based on ethylenediamine / propylene oxide / ethylene oxide with an ethylene oxide content of 40% by weight and an average molecular weight M _n of 12,000.

B2: block copolymer based on ethylene oxide / propylene oxide / ethylene oxide with an ethylene oxide content of 50% by weight and an average molecular weight M _n of 6500.

B3: block copolymer based on ethylene oxide / propylene oxide / ethylene oxide with an ethylene oxide content of 10% by weight and an average molecular weight M _n of 3500.

B4: Acidic phosphoric acid ester based on alkoxylated C ₃ -C ₅ oxoxalcohol (6 mol PO and 12 mol EO / mol alcohol) The pigment granules obtained were incorporated into polyethylene (LDPE), soft PVC and polypropylene to assess their application properties. As a comparison, stains were obtained which were obtained 5 with the pigment not coated with additives.

^• The color properties were determined in white lightening in LDPE and soft PVC. For this purpose, 5% by weight LDPE or PVC colored with titanium dioxide and the respective pigment

10 preparation in the brightening ratio 1:10 (0.5% by weight of pure pigment + 5% by weight of titanium dioxide) mixed and on a machine mill at a roller temperature of 160 ° C. and 200 roller revolutions to form a roller skin of thickness 0, 4 mm processed. After halving the roller skin, half of the other 200 roller

Rolled 15 revolutions at a roll temperature of 130 ° C. The fur thickness was 0.3 mm. Each of the rolled skins was cut and pressed into sheets in a press with a distance frame (1 mm) at 180 ° C. The plates were then colorimetrically measured using the standard illuminant D65 according to the CIELAB formula (DIN

20 6174) were evaluated.

^■ The coloristic parameters color angle H and chroma C * and the color strength (details of the color equivalents FAE) were determined on the LDPE or PVC fur dispersed at 130 ° C. The coloration with the respective untreated pigment was assigned the FAE value 100 (standard). FAE values <100 mean a higher color strength than the standard, FAE values> 100 correspondingly a lower color strength.

30 To test the dispersibility of the pigment granules obtained, 2% by weight pigmented LDPE blown films were produced and visually examined for pigment specks. The rating in the form of the film grade (FN) was carried out on a scale from 1 (very good) to 5 (very bad).

35

The dispersion hardness was determined in white lightening in soft PVC. The PVC sheets investigated were produced as described above and measured colorimetrically. The calculation of the dispersion hardness (DH) was made from those obtained during the measurement

40 lightening ratios according to the following formula:

AVI

DH = - 1 x 100 • AV2

45 AVI: lightening ratio of the color produced at 130 ° C AV2: lightening ratio of the color produced at 160 ° C To determine the pressure filter values, the respective pigment granules were first dispersed in PE wax (40% by weight pigmentation). This preparation was then premixed with polypropylene (2.5% by weight pigmentation), melted in an extruder and conveyed through a defined filter package using a spinning pump.

The filter test was carried out as follows: after installing the filter cassette with the filter pack, there was a wait until the thermal equilibrium was reached. The filter package was used so that the fine sieve (number of warp threads in 3.5 mm: 42; number of weft threads in 3.5 mm: 17; number of stitches: 10870 / cm ² ; absolute filter fineness: 33-37 μm) of the material flow was reached. The system was then started up using unpig entiertem polypropylene, the developing before the filter ^'pressure (initial pressure Pl) was determined. Subsequently, the measurement was also conveyed through the filter package while measuring the pressure. The pressure upstream of the filter may increase due to any particles present. The. The highest pressure reached in this phase is the final pressure P2. Before each subsequent measurement, the extruder was cleaned with unpigmented polypropylene and the filter package was replaced. The pressure filter values (DFW) were calculated from the pressure values using the following formula (DFW values <2.0 bar / g are considered good):

DFW = P2 Pl [bar / g pigment]

Pl: initial pressure [bar], P2: final pressure [bar] G: amount of pigment [g]

The following table shows the composition of the pigment granules produced and the test results obtained in the plastics mentioned. The respective pigments not coated with the additive serve as a comparison and served as the standard for the specification of the coloristic parameters. H rH

Claims

claims

1. Use of solid pigment preparations which are essential components

(A) 60 to 90% by weight of at least one pig ent

included, for coloring plastics.

2. Use according to claim 1, characterized in that the pigment preparations as component (B) an additive from the group of alkylene oxide block copolymers, the reaction products of alkylene oxides with alcohols, amines, aliphatic carboxylic acids or carboxylic acid amides, the acidic phosphoric acid, , Phosphonic acid, sulfuric acid and sulfonic acid esters of these alkylene oxide compounds and the salts of these esters.

3. Use according to claim 1 or 2, characterized in that the pigment preparations are in the form of granules having an average grain size of 50 to 5000 microns and a BET surface area of <15 m ² / g.

4. Use according to claims 1 to 3, characterized in that the plastics are modified natural materials or synthetic synthetic materials.

5. Use according to claims 1 to 4, characterized in that the plastics are thermoplastics on the

Are based on polyolefins or polyvinyl compounds.

6. A process for coloring plastics, characterized in that solid pigment preparations according to claims 1 to 3 are incorporated into the plastics by extrusion, rolling, kneading or grinding.