UNIVERSAL PIGMENT PREPARATION

Abstract

A universal pigment preparation including a flocculation-stabilizing medium including (a1) reaction products of di- or polycarboxylic acids or hydroxycarboxylic acids with di- or polyols, and (a2) reaction products of alkylene oxides with alkoxylatable compounds, and at least one pigment. Paints, varnishes, printing inks, coating materials, floor coatings, potting compounds and filling compounds may be made using the universal pigment preparation.

Claims

1. A universal pigment preparation comprising a flocculation-stabilizing medium comprising (a1) reaction products of di- or polycarboxylic acids or hydroxycarboxylic acids with di- or polyols and (a2) reaction products of alkylene oxides with alkoxylatable compounds, and at least one pigment.

2. The universal pigment preparation according to claim 1, wherein the weight ratio of flocculation-stabilizing medium to pigment is 95:5 to 5:95.

3. The universal pigment preparation according to claim 1, wherein the weight ratio of reaction products (a1) to reaction products (a2) is 10:90 to 90:10.

4. The universal pigment preparation according to claim 1, wherein the di- or polycarboxylic acids are saturated and/or unsaturated and/or aromatic di- or polycarboxylic acids and the anhydrides or esters thereof.

5. The universal pigment preparation according to claim 4, wherein the di- or polycarboxylic acids are mixtures of saturated and α,β-unsaturated di- or polycarboxylic acids in a molar ratio of 1:99 to 99:1.

6. The universal pigment preparation according to claim 4, wherein the di- or polycarboxylic acids are citraconic, fumaric, itaconic, maleic and/or mesaconic acid, phthalic acid, isophthalic acid, terephthalic acid, cyclohexane-1,4-dicarboxylic acid, malonic acid, succinic acid, glutaric acid, methyltetra- and m ethyl hexahydrophthal i c acid, hexahydrophthalic acid, tetrahydrophthalic acid, dodecanedioic acid, pimelic acid, adipic acid, azelaic acid, suberic acid, sebacic acid, pyromellitic acid and/or trimellitic acid or the anhydrides or esters thereof or mixtures thereof.

7. The universal pigment preparation according to claim 1, wherein the di- or polyols are polyethylene glycols of the formula (I) ##STR00003## with x=1, 2, 3 or 4 to 10, with the proviso that: in the case that x=1 the R.sup.1 and R.sup.2 radicals are hydrogen, in the case that x=2, 3 or 4 to 10 the R.sup.1 radical is a linear or branched, saturated or mono- or polyunsaturated aliphatic, cycloaliphatic or aromatic hydrocarbyl radical having 2 to 50 carbon atoms, which may be interrupted by heteroatoms such as oxygen, nitrogen or sulphur, and R.sup.2 is a hydrogen, where the segments attached to R.sup.1 in a number of x may be of the same or different structure, m=0, 1, 2 or 3 to 100, n=0, 1, 2 or 3 to 100, and with the proviso that the product x*(m+n)=2, 3 or 4 to 100.

8. The universal pigment preparation according to claim 7, wherein the repeat units (—C.sub.2H.sub.4—O—).sub.m and (—C.sub.3H.sub.6—O—).sub.n are arranged in blocks, in random distribution or in a gradient distribution in the polymer chain.

9. The universal pigment preparation according to claim 7, wherein the polyalkylene glycols are polypropylene glycols or polypropylene-polyethylene glycols having a number-average molar mass of 100 to 2000 g/mol.

10. The universal pigment preparation according to claim 1, wherein the reaction products (a1) have an OH number between 1 and 450 mg KOH/g.

11. The universal pigment preparation according to claim 10, wherein the reaction products (a1) have a theoretical double bond content of 0 to 3 mmol/g.

12. The universal pigment preparation according to claim 1, wherein the reaction products (a2) are prepared by an alkoxylation ##STR00004## reaction of alkoxylatable compounds of the formula (II) where R.sup.3 is a linear or branched, saturated or mono- or polyunsaturated, aliphatic, cycloaliphatic or aromatic hydrocarbyl radical having 2 to 50 carbon atoms which may be interrupted by heteroatoms such as oxygen, nitrogen or sulphur, R.sup.4 is a linear or branched, saturated or mono- or polyunsaturated aliphatic, cycloaliphatic or aromatic hydrocarbyl radical which may be interrupted by heteroatoms such as oxygen, nitrogen or sulphur and may be substituted by OH groups, having 1 to 22 carbon atoms, a=1 to 8, b=0 to 7, with the proviso that the sum total of a and b=2 to 8, with alkylene oxides.

13. The universal pigment preparation according to claim 1, wherein the alkoxylatable compounds are diols, polyols, ethylene glycol, diethylene glycol, polyethylene glycol, propylene glycol, dipropylene glycol, polypropylene glycol, polyetherols, hexanediol, butanediol, neopentyl glycol, hexylene glycol, ricinoleic acid, hydroxystearic acid and polyhydroxystearic acid, glycerol, polyglycerol, pentaerythritol, trimethylolpropane, poly-OH-functional phenols such as novolaks or polyphenols, sorbitol, sorbitan, isosorbide, mannitol and sugars such as glucose, sucrose and esters thereof, and fatty acids such as oleic acid, lauric acid, or stearic acid.

14. The universal pigment preparation according to claim 1, wherein the alkylene oxides are ethylene oxide, propylene oxide, butylene oxide and/or styrene oxide.

15. The universal pigment preparation according to claim 1, wherein the reaction products (a2) have a weight-average molar mass of 300 to 15 000 g/mol.

16. The universal pigment preparation according to claim 1, wherein the pigments are organic or inorganic pigments or carbon black pigments.

17. The universal pigment preparation according to claim 1, comprising 0.5% to 85.5% by weight of reaction products (a1), 0.5% to 85.5% by weight of reaction products (a2) and 5% to 95% by weight of at least one pigment selected from the group of the organic, inorganic or carbon black pigments.

18. The universal pigment preparation according to claim 17, wherein dispersing additives and/or further auxiliary components are added.

19. The universal pigment preparation according to claim 18, wherein the volatile organic component is <20% by weight.

20. The universal pigment preparation according to claim 19, wherein it has a free-flowing consistency at room temperature.

21. The universal pigment preparation according to claim 20, wherein it has a viscosity at 25° C. and 100 1/s of <5000 mPas.

22. The universal pigment preparation according to claim 21, wherein it does not include any organic solvent having a boiling point below 250° C. or any water.

23. A flocculation-stabilizing medium comprising 10% to 90% by weight of (a1) and 90%.sub.to 10% by weight of (a2).

24. A pigment preparation comprising the flocculation-stabilizing medium according to claim 23.

25. (canceled)

26. The process for producing the universal pigment preparation according to claim 1, wherein the reaction products (a1) and the reaction products (a2) are first produced and then mixed, with no addition of volatile organic solvents and/or water, then the pigments are mixed in.

Description

[0122] The subject-matter of the invention will be described by way of example below, without the invention being restricted to these illustrative embodiments.

[0123] Test Methods:

[0124] Parameters or measurements are preferably determined using the methods described hereinbelow. In particular, these methods are used in the examples of the present intellectual property right.

[0125] GPC 1

[0126] The relative molar masses of the inventive reaction products (a1) are determined by size exclusion chromatography (GPC). For this purpose, three columns from Merck (PS 400, 250*7 mm, PS 40, 250*7 mm, and PS 1, 250*7 mm) with a particle size of 5μm are combined in series. After calibration, 20 μl of the condensation resin solution in tetrahydrofuran (c of condensation resin =20 mg/ml) are injected at 40° C. with a Rheodyne 7125 injector and analysed at a flow rate of 1 ml/min (Waters 510 HPLC pump) at 40° C. with degassed tetrahydrofuran as mobile phase and a differential refractometer at 40° C. (Waters model 410). Evaluation is made after calibration against polystyrene standards, which is carried out in the manner described above. Polystyrene standards (standard 1 Mp 377400, Mp 96000, Mp 20650, Mp 1300, Mp 162; standard 2 Mp 283300, Mp 50400, Mp 10850, Mp 2930, Mp 980; standard 3 Mp 218800, Mp 68900, Mp 10050, Mp 1940, Mp 580; Mp =molar mass at peak maximum) are commercially available, for example, from Merck or Polymer Laboratories.

[0127] GPC 2

[0128] GPC measurements for determining the polydispersity and the average molar masses Mw or Mn were conducted under the following measurement conditions: SDV 1000/10 000 Å column combination (length 65 cm), temperature 30° C., THF as mobile phase, flow rate 1 ml/min, sample concentration 10 g/l, RI detector, evaluation against polypropylene glycol standard.

[0129] Acid numbers were determined according to DIN EN ISO 2114.

[0130] The reported viscosities of the inventive reaction products (a1) were determined with an Anton Paar M102 rotary viscometer and with the CP50/2 measurement geometry at 23° C. and a shear rate of 100 1/s.

[0131] Glass transition temperatures were determined according to DIN 53765.

[0132] Determination of OH number

[0133] Hydroxyl numbers were determined according to the method DGF C-V 17 a (53) of the

[0134] Deutsche Gesellschaft fur Fettwissenschaft [German Society for Fat Science]. This involved acetylating the samples with acetic anhydride in the presence of pyridine and determining the consumption of acetic anhydride by titration with 0.5 N potassium hydroxide solution in ethanol using phenolphthalein.

[0135] 1. Preparation of inventive reaction products (a1)

[0136] Reaction products al-1:

[0137] Adipic acid and fumaric acid (molar ratio 1.95:1) were reacted in a molar ratio of the COOH groups to OH groups of 1:1.96 with polypropylene glycol 725 and methyldiethanolamine (molar ratio 12.17:1) at 180° C. to 190° C. under a nitrogen atmosphere until an acid number of 7 mg KOH/g and an OH number of 79 mg KOH/g had been attained.

[0138] Mn=2000 g/mol

[0139] Mw=3300 g/mol

[0140] Glass transition temperature −67° C.

[0141] Viscosity at 23° C.: 530 mPas

[0142] Reaction products al-2:

[0143] Adipic acid and fumaric acid (molar ratio 1.99:1) were reacted in a molar ratio of the COOH groups to OH groups of 1:2.55 with polypropylene glycol 725 at 240° C. under a nitrogen atmosphere until an acid number of 6 mg KOH/g and an OH number of 85 mg KOH/g had been attained.

[0144] Mn=1800 g/mol

[0145] Mw =2800 g/mol

[0146] Glass transition temperature −68° C.

[0147] Viscosity at 23° C.: 408 mPas

[0148] Polypropylene glycol 725 is available under trade names including ARCOL® PPG-725 from Covestro.

[0149] 2. Preparation of reaction products (a2):

[0150] Reaction Products a2-1:

[0151] Preparation of a polyoxyalkylene from glycerol with PO and EO

[0152] An initial charge of 380 g of glycerol and 23.2 g of potassium hydroxide in a 15 litre autoclave was heated to 115° C. while stirring. The reactor was evacuated down to an internal pressure of 30 mbar in order to remove any volatile ingredients present by distillation, and then nitrogen was injected to 3 bar. The internal pressure was then lowered again to <30 mbar. 7868 g of propylene oxide (PO) were metered into the inertized reactor while cooling at internal temperature 115° C. and an internal pressure of 3 to 4 bar (absolute) within 10 h. After further reaction at 115° C. for 1 h, 2729 g of ethylene oxide (EO) were metered into the reactor at internal temperature 115° C. and an internal pressure of 2 to 3 bar (absolute) within 3 h. Subsequently, volatile components were removed by distillation under reduced pressure at 115° C. After further reaction at 115° C. for 1 h, the reaction product was cooled down to 90° C., neutralized with phosphoric acid and discharged from the reactor via a filter. The product was almost colorless and of low viscosity at room temperature. The OH number was 63 mg KOH/g, and the acid number 0.1 mg KOH/g. According to GPC 2, the product has a weight-average molar mass M, of 2267 g/mol and a polydispersity M.sub.w/M.sub.n, of 1.04.

[0153] Reaction Products a2-2:

[0154] Preparation of Ethoxylated Sorbitan Monooleate

[0155] An initial charge of 1500 g of sorbitan monooleate and 2.6 g of potassium hydroxide solution (45%) in a 7 litre autoclave was heated to 120° C. while stirring. The reactor was evacuated down to an internal pressure of 30 mbar in order to remove water and any other volatile ingredients present by distillation, and then nitrogen was injected to 3 bar. The internal pressure was then lowered again to <30 mbar. 3050 g of ethylene oxide were metered into the inertized reactor while cooling at internal temperature 160° C. and an internal pressure of 3 to 4 bar (absolute) within 3 h. After further reaction at 160° C. for 1 h, the reaction product was cooled down to 120° C. and degassed at <30 mbar. This was followed by cooling to 90° C., neutralization with lactic acid and discharge from the reactor via a filter. The liquid product was pale yellowish. The OH number was 71 mg KOH/g, and the acid number 0.4 mg KOH/g. According to GPC 2, the product has a weight-average molar mass M, of 1704 g/mol and a polydispersity M.sub.w/M.sub.n of 1.18.

[0156] 3. Production of the Universal Pigment Preparations According to the Invention and Comparative Preparations for Testing the Viscosity

[0157] According to the formulations specified in Table 2, the inventive reaction products (a1) and (a2) were used to produce a universal pigment preparation (P1 to P9). For comparison, pigment preparations were made up with grinding resins that are standard on the market rather than the reaction products (a1) and the inventive reaction products (a2) (CM P1 to CM P6).

[0158] The reaction products (a1) and the comparative products were initially charged in PE cups, and then reaction products (a2) and further liquid components were metered in. The mixture was manually homogenized briefly with a metal spatula and then the pigment was weighed in. After manual rehomogenization, a defined amount of glass beads was weighed in (see Table 1). Dispersion was effected in a Hauschild Speedmixer at a speed of 2000 rpm and with the dispersing times specified in the table. The universal pigment preparations according to the invention thus obtained were screened through a 250 μm high-speed nylon screen.

TABLE-US-00001 TABLE 1 Dispersing parameters Glass beads (g) (d = 1.1 mm) Dispersion time Heliogen blue L7085 50 8 min Special black 4 50 8 min Bayferrox 130 M 30 4 min

[0159] Measurement of the Viscosities of the Preparations: The viscosities of the universal pigment preparations according to the invention and comparative examples were measured with a Haake RheoStress 1 rheometer. Measurement parameters:

[0160] cone/plate C35/2° , 23° C., multiple measurement points in the range of 1-1000 1/s. The viscosity was evaluated at 100 1/s. The results are listed in Table 2.

TABLE-US-00002 TABLE 2 Formulations for production of the inventive universal pigment preparations (P) and comparative examples comprising grinding resins that are customary on the market (CM P) CM CM CM CM CM CM P1 P2 P3 P4 P5 P6 P7 P8 P9 P1 P2 P3 P4 P5 P6 a1-2 17.2 17.5 11 17.2 17.5 11 a1-1 17.2 17.5 11 a2-2 25.6 26.2 16.4 25.6 26.2 16.4 25 25.5 10.5 25 25.5 10.5 a2-1 25.6 26.2 16.4 TEGO ® 16.7 17 15.8 VariPlus TC Laropal A81 16.7 17 15.8 TEGO ® 1.2 1.1 1.2 1.1 Dispers 656 TEGO ® 1.1 1.1 Dispers 650 Dimethyl- 0.2 0.3 0.1 0.2 0.3 0.1 0.2 0.3 0.1 0.2 0.3 0.1 0.2 0.3 0.1 amino- ethanol Heliogen 7 7 7 7 7 blue L7085 Special 6 6 6 6 6 black 4 Bayferrox ® 22.5 22.5 22.5 22.5 22.5 130 M Total 50 50 50 50 50 50 50 50 50 50 50 50 50 50 50 Producible? yes yes yes yes yes yes yes yes yes yes yes no yes yes no Viscosity at 1885 3214 1412 1940 2392 1146 2084 830 1179 4576 5035 6869 8283 100 1/s in mPas

[0161] All the inventive universal pigment preparations P1 -P9 were producible. The comparative preparations CM P1-CM P6 exhibited a much higher viscosity and hence limited flowability, or could not be produced at all.

[0162] 4. Verification of the Universal Usability of the Universal Pigment Preparations According to the Invention in Various Paint Systems

[0163] To verify the universal usability of the universal pigment preparations according to the invention and the comparative preparations, these are used for tinting of various conventional (solventborne) and aqueous paint systems. It is standard practice on the market to test usability on the basis of appearance, on the basis of color strength and finally on the basis of the “rub-up value” (ΔE). To determine the rub-up value, after the paint has been applied and shortly before it has dried through, a small area is rubbed with a finger. At this site, the pigments are stirred up again. Ideally, no difference arises between the rubbed and the unrubbed area. For this invention, color strength and rub-up value were considered relative to one another.

[0164] Four different white basecoats were used, each of which was mixed with the inventive universal pigment preparations P. The formulations are described below.

[0165] 4.1 Production of a Colored Basecoat 1 Based on an aqueous 2K PU acrylate System

[0166] 4.1.1 First of all, a clearcoat 1 according to Table 3 and a white paste 1 according to Table 4 are produced.

TABLE-US-00003 TABLE 3 Formulation for clearcoat 1 Amount (g) Bayhydrol A 145 58.3 Dimethylaminoethanol (20% in H.sub.2O) 1.4 Demineralized water 15.3

TABLE-US-00004 TABLE 4 Formulation for white paste 1 Amount (g) Demineralized water 18.4 TEGO Dispers 755 W 10 TEGO Foamex 830 1 Aerosil 200 0.5 Kronos 2310 70 Parmetol K40 0.1

[0167] For production of the basecoat 1, 65.2 parts of the clearcoat 1 are blended with 34.8 parts of the white paste 1 while stirring.

[0168] 4.1.2 Production of a colored basecoat 1

[0169] The white basecoat 1 is initially charged in a PE cup and the inventive universal pigment preparation P according to Table 6-8 is metered in. This is followed by homogenization in a Speedmixer at 2000 rpm for 1 min. The hardener 1 is added and the mixture is mixed at 2000 rpm for a further 1 min. The paints obtained are applied to glass plates with wet film thickness 150 μm with the aid of a bar applicator. After brief drying, the rub-up test is conducted by rubbing the applied paint with a finger. Subsequently, the paint drawdowns obtained are dried at room temperature for 24 h and then cured at 80° C. for another 2 h.

[0170] Curing is accomplished using an isocyanate hardener (hardener 1) according to the following formulation:

TABLE-US-00005 TABLE 5 Formulation for hardener 1 Amount (g) Bayhydur 3100 8 Methoxypropyl acetate 2

TABLE-US-00006 TABLE 6 Formulation for blue-colored basecoat 1 Amount (g) White basecoat 1 8.22 Hardener 1 1.78 Universal pigment preparation P1, P4 or P7 0.57

TABLE-US-00007 TABLE 7 Formulation for black-colored basecoat 1 Amount (g) White basecoat 1 8.22 Hardener 1 1.78 Universal pigment preparation P2, P5 or P8 0.67

TABLE-US-00008 TABLE 8 Formulation for red-colored basecoat 1 Amount (g) White basecoat 1 8.22 Hardener 1 1.78 Universal pigment preparation P3, P6 or P9 0.45

[0171] 4.2 Production of a Colored Basecoat 2 Based on an Aqueous 1K styrene acrylate

[0172] 4.2.1 First of all, a clearcoat 2 according to Table 9 and a white paste 2 according to Table 10 are produced.

TABLE-US-00009 TABLE 9 Formulation for clearcoat 2 Amount (g) Revacryl AE 6030 76.2 TEGO Foamex 855 (25% strength) 0.6 Butylglycol 5.5 Premix and adjust pH to 8.5 with ammonia Millicarb OG 8.7 Finntalc M 15 5.6 TEGO ViskoPlus 3060 1.5 TEGO Foamex 855 (25% strength) 0.6 Petroleum spirit 1.3 Adjust pH to 8.5 with ammonia

TABLE-US-00010 TABLE 10 Formulation for white paste 2 Amount (g) Demineralized water 18.4 TEGO Dispers 755 W 10 TEGO Foamex 830 1 Aerosil 200 0.5 Kronos 2310 70 Parmetol K40 0.1

[0173] For production of the basecoat 2, 71.4 parts of the clearcoat 2 are blended with 28.6 parts of the white paste 2 while stirring.

[0174] 4.2.2 Production of a colored basecoat 2

[0175] The white basecoat 2 is initially charged in a PE cup and the universal pigment preparation P according to Tables 11-13 is metered in. This is followed by homogenization in a Speedmixer at 2000 rpm for 1 min. The paints obtained are applied to glass plates with wet film thickness 150 μm with the aid of a bar applicator. After brief drying, the rub-up test is conducted by rubbing the applied paint with a finger. Subsequently, the paint drawdowns obtained are dried at room temperature for 24 hours and then cured at 80° C. for another 2 h.

TABLE-US-00011 TABLE 11 Formulation of blue-colored basecoat 2 Amount (g) White basecoat 2 10.00 Universal pigment preparation P1, P4 or P7 0.57

TABLE-US-00012 TABLE 12 Formulation of black-colored basecoat 2 Amount (g) White basecoat 2 10.00 g Universal pigment preparation P2, P5 or P8  0.67 g

TABLE-US-00013 TABLE 13 Formulation of red-colored basecoat 2 Amount (g) White basecoat 2 10.00 g Universal pigment preparation P3, P6 or P9  0.45 g

[0176] 4.3 Production of a Colored Basecoat 3

[0177] 4.3.1 The basecoat 3 is a commercial standard white alkyd resin paint “Impredur Hochglanzlack 840” from Brillux.

[0178] 4.3.2 Production of a colored basecoat 3

[0179] The white basecoat 3 is initially charged in a PE cup and the universal pigment preparation P according to Tables 14-16 is metered in. This is followed by homogenization in a Speedmixer at 2000 rpm for 1 min. The paints obtained are applied to glass plates with wet film thickness 150 μm with the aid of a bar applicator. After brief drying, the rub-up test is conducted by rubbing the applied paint with a finger. Subsequently, the paint drawdowns obtained are dried at room temperature for 24 hours and then cured at 80° C. for another 2 h.

TABLE-US-00014 TABLE 14 Formulation of blue-colored basecoat 3 Amount (g) White basecoat 3 10.00 Universal pigment preparation P1, P4 or P7 0.57

TABLE-US-00015 TABLE 15 Formulation of black-colored basecoat 3 Amount (g) White basecoat 3 10.00 Universal pigment preparation P2, P5 or P8 0.67

TABLE-US-00016 TABLE 16 Formulation of red-colored basecoat 3 Amount (g) White basecoat 3 10.00 Universal pigment preparation P3, P6 or P9 0.45

[0180] 4.4 Production of a Colored Basecoat 4 Based on a solventborne 2K PU polyester polyol System

[0181] 4.4.1 A white basecoat 4 according to Table 17 is produced.

TABLE-US-00017 TABLE 17 Formulation for white basecoat 4 Amount (g) Setal 1603 20 TEGO Airex 990 0.1 TEGO Dispers 628 1.8 Kronos 2310 30 Blanc Fixe Micro 29 Finntalk M 15 3 Butyl acetate 4.5 Dispersing in a Skandex for 1 h TEGO Glide 110 0.5 Solvent Naphtha 170 (Hydrosol A170) 0.5 TIB KAT 716 1% in BA 4 Butyldiglycol acetate 0.5 Setal 1603 6.1

[0182] Curing is accomplished using an isocyanate hardener (hardener 2) according to the following formulation:

TABLE-US-00018 TABLE 18 Formulation for hardener 2 Amount (g) Desmodur N3600 9 Butyl acetate 1

[0183] 4.4.2 Production of a colored basecoat 4

[0184] The white basecoat 4 is initially charged in a PE cup and the universal pigment preparation P according to Tables 19-21 is metered in. This is followed by homogenization in a Speedmixer at 2000 rpm for 1 min. The hardener is added and the mixture is mixed at 2000 rpm for a further 1 min. The paints obtained are applied to glass plates with wet film thickness 150 μm with the aid of a bar applicator. After brief drying, the rub-up test is conducted by rubbing the applied paint with a finger. Subsequently, the paint drawdowns obtained are dried at room temperature for 24 h and then cured at 80° C. for another 2 h.

TABLE-US-00019 TABLE 19 Formulation of blue-colored basecoat 4 Amount (g) White basecoat 4 8.60 Hardener 2 1.40 Universal pigment preparation P1, P4 or P7 0.75

TABLE-US-00020 TABLE 20 Formulation of black-colored basecoat 4 Amount (g) White basecoat 4 8.60 Hardener 2 1.40 Universal pigment preparation P2, P5 or P8 0.86

TABLE-US-00021 TABLE 21 Formulation of red-colored basecoat 4 Amount (g) White basecoat 4 8.60 Hardener 2 1.40 Universal pigment preparation P1, P4 or P7 0.58

[0185] 5. Production of Comparative Examples CM P7 to CM P12

[0186] The inventive basecoats 1-4 are compared with water-based pigment preparations that are standard on the market (CM P7, CM P9, CM P11) and solvent-based pigment preparations (CM P8, CM P10, CM P12) produced according to Table 22:

TABLE-US-00022 TABLE 22 Production of comparative examples CM P7 CM P8 CM P9 CM P10 CM P11 CM P12 Laropal A81 15.2 15 5 (60% in MPA) TEGO ® 20.8 13.8 9.5 VariPlus DS 50 TEGO ® 7.8 2 Dispers 670 TEGO ® 2.5 0.9 Dispers 656 TEGO ® 7.5 6.6 4 Dispers 750 W TEGO ® 0.5 0.5 0.5 Foamex 810 2-Amino-2- 0.2 0.1 methyl-1- propanol Heliogen 12.5 12.5 blue L7085 Special 11 12.5 black 4 Bayferrox 30 32.5 130 M Water 8.7 17.9 10.4 Methoxypropyl 19.8 14.7 5.1 acetate Total 50 50 50 50 50 50

[0187] All liquid components were initially charged and manually homogenized briefly with a metal spatula. Subsequently, the pigment was weighed in and the mixture was manually homogenized again. A defined amount of glass beads was added and, after the dispersion time specified in Table 1, dispersed in a Hauschild Speedmixer at a speed of 2000 rpm. The pigment preparations thus obtained were screened through a 250 μm high-speed nylon screen.

[0188] 6. Assessment of coloring capacity

[0189] The assessment of the coloring capacity of the colored basecoats 1-4 is effected on the basis of the measurement of color strength and the rub-up intensity (ΔE). This is done by using the X-Rite SP-62 colorimeter to analyse and compare the Lab* values of the rubbed area and the unrubbed area. The difference in hue AE in the rubbed area relative to the unrubbed area is calculated according to formula (III):

ΔE=√{square root over ((L.sub.RB.sup.*−L.sub.0.sup.*).sup.2+(a.sub.RB.sup.*−a.sub.0.sup.*).sup.2+(b.sub.RB.sup.*−b.sub.0.sup.*).sup.2)}  Formula (III)

[0190] The color strength F is calculated in accordance with Kubelka/Munk via the tristimulus value Y according to formula (IV) and (V):

[00001]$\begin{array}{cc}Y={\left(\frac{L_0^{*}+16}{116}\right)}^3.Math.100& \mathrm{Formula}.Math..Math.\left(\mathrm{IV}\right)\\ F=\frac{{\left(100-Y\right)}^2}{2.Math.Y}& \mathrm{Formula}.Math..Math.\left(V\right)\end{array}$

TABLE-US-00023 TABLE 23 Results for the coloring capacity of aqueous and solventborne basecoats with Heliogen blue L7085 P1 P4 P7 CM P1 CM P4 CM P7 CM P8 Basecoat 1 Color 47.82 48.10 48.60  17.57 20.69  38.04 — strength ΔE  1.68 0.6 1.24 20.4  17.42   4.87 — Visual compatible compatible compatible incompatible incompatible compatible immiscible compatibility Basecoat 2 Color 53.04 53.80 0.78 26.57 3.95 46.22 — strength ΔE  1.75 0.6 1.13 16.29 6.48  2.81 — Visual compatible compatible compatible incompatible incompatible compatible immiscible compatibility Basecoat 3 Color 50.37 51.43 59.16  37.63 2.99 — 48.13 strength ΔE  3.67 2.5 2.24 38.28 1.94 —  4.61 Visual compatible compatible compatible compatible compatible immiscible compatible compatibility Basecoat 4 Color 41.96 41.11 41.11  41.21 41.93  — 38.69 strength ΔE  1.65  1.01 1.41  0.96 0.97 —  1.97 Visual compatible compatible compatible compatible compatible immiscible compatible compatibility

TABLE-US-00024 TABLE 24 Results for the coloring capacity of various aqueous and solventborne basecoats with black pigment P2 P5 P8 CM P2 CM P5 CM P9 CM P10 Basecoat 1 Color strength 170.67 152.79 179.13 24.47 26.19 173.60 — ΔE  1.5  2.56  0.36 26.8  26.07  1.56 — Visual compatible compatible compatible incompatible incompatible compatible immiscible compatibility Basecoat 2 Color strength 187.38 177.28 188.58 96.06 71.77 190.46 — ΔE  1.3  1.27  0.10  2.35 14.9   0.31 — Visual compatible compatible compatible incompatible incompatible compatible immiscible compatibility Basecoat 3 Color strength 190.87 206.19 221.58 190.26 188.73 — 218.99 ΔE  1.73 1   0.10  0.87  1.88 —  1.32 Visual compatible compatible compatible compatible compatible immiscible compatible compatibility Basecoat 4 Color strength 133.19 122.82 128.05 130.24 137.20 — 102.59 ΔE  2.19  2.2  1.58  0.37  0.8 —  6.24 Visual compatible compatible compatible compatible compatible immiscible compatible compatibility

TABLE-US-00025 TABLE 25 Results for the coloring capacity of various aqueous and solventborne basecoats with Bayferrox 130 M P3 P6 P9 CM P11 CM P12 Basecoat 1 Color 46.63 44.45 51.15 49.12 — strength ΔE  1.82  1.48  0.46  2.75 — Visual compatible compatible compatible compatible immiscible compatibility Basecoat 2 Color 53.64 58.91 54.09 58.04 — strength ΔE  0.79  1.63  0.38  0.85 — Visual compatible compatible compatible compatible immiscible compatibility Basecoat 3 Color 52.48 49.06 59.16 — 54.98 strength ΔE  1.02  1.48  0.54 —  0.38 Visual compatible compatible compatible immiscible compatible compatibility Basecoat 4 Color 40.78 40.42 39.38 — 39.91 strength ΔE  1.83  0.53  0.84 —  1.57 Visual compatible compatible compatible immiscible compatible compatibility

[0191] It can clearly be seen from the results shown in Table 23 to Table 25 that the basecoats comprising the universal pigment preparations according to the invention have universal compatibility in all paint systems. For this purpose, the visual appearance is considered, and the color strength and the magnitude of the AE value are also compared relative to one another. The comparative examples based on the commercial standard resins (CM P1 to CM P6) show good compatibility in the solventborne systems, but fail in the aqueous range. The pigment preparations CM P7 to CM P12 that are standard on the market are not universally usable because of their solvent content and/or water content. When compared in the respective medium, it is found that the basecoats comprising the universal pigment preparations according to the invention give very similar or even better results.

TABLE-US-00026 TABLE 26 Materials used Materials Company Aerosil 200 Evonik Industries AG Filler Bayferrox ® 130 M Lanxess Pigment Bayhydrol A 145 Covestro Binder Bayhydur 3100 Covestro Hardener Blanc Fixe Micro Solvay Filler Desmodur N3600 Covestro Hardener Finntalk M 15 Mondominerals Filler Heliogen blue L7085 BASF Pigment Impredur High Gloss Enamel 840 Brillux Alkyd resin paint Kronos 2310 Kronos Pigment Laropal A81 BASF Binder Laropal A81 (60% in MPA) BASF Binder, self-diluted Millicarb OG ( ) Omya Filler Parmetol K40 Schülke Preservative Revacryl AE 6030 Synthomer Binder Setal 1603 ( ) Nuplex Binder Solvent Naphtha 170 (Hydrosol DHC Solvent Chemie Volatile organic solvent A170) Special black 4 Orion Engineered Carbons Pigment TEGO ® Airex 990 Evonik Industries AG Deaerating agent TEGO ® Dispers 628 Evonik Industries AG Dispersant TEGO ® Dispers 650 Evonik Industries AG Dispersant TEGO ® Dispers 656 Evonik Industries AG Dispersant TEGO ® Dispers 656 Evonik Industries AG Dispersant TEGO ® Dispers 670 Evonik Industries AG Dispersant TEGO ® Dispers 750 W) Evonik Industries AG Dispersant TEGO ® Dispers 755 W Evonik Industries AG Dispersant TEGO ® Foamex 810 Evonik Industries AG Defoamer TEGO ® Foamex 830 Evonik Industries AG Defoamer TEGO ® Foamex 855 (25%) Evonik Industries AG Defoamer TEGO ® Glide 110 Evonik Industries AG Surface additive TEGO ® VariPlus DS 50 Evonik Industries AG Binder TEGO ® ViskoPlus 3060 Evonik Industries AG Thickener TEGO ® VariPlus TC Evonik Industries AG Binder TIB KAT 716 1% in BA TIB Chemicals Curing catalyst

[0192] 7. Nonvolatile Content of the Universal Pigment Preparations According to the Invention

[0193] The nonvolatile content (NVC) of the inventive universal pigment preparations comprising Heliogen blue is determined by drying the sample. For this purpose, a sample of about 1 g is weighed accurately to 1 mg into an aluminium boat having a diameter of 6 cm, and the latter is dried in an oven at 130° C. for 2 h and then weighed again. The absolute loss is determined and this is used to calculate the nonvolatile content in per cent. The higher the percentage, the lower the level of volatile substances that are released into the indoor environment.

TABLE-US-00027 TABLE 27 Nonvolatile organic content of the universal pigment preparations according to the invention Pigment preparations NVC in % P1 97.0 P4 96.1 P7 97.1 CM P8 48.2

[0194] The nonvolatile content (NVC) of the universal pigment preparations according to the invention is well above 90%. They therefore contain just a very small content of volatile organic constituents.