PROCEDURE FOR THE PREPARATION OF EFFECT PIGMENT PASTES

Abstract

The present invention relates to a process for preparing an effect pigment paste comprising at least steps (1) and (2), namely, preparing a mixture containing at least one effect pigment (a) and at least one polymer (b) in a liquid medium (c) (step (1)), and dispersing the mixture obtained after step (1) to obtain the effect pigment paste (step (2)), wherein step (2) is performed with a vibrator and the effect pigment paste obtained after completion of step (2) is free of milling matter, an effect pigment paste that can be produced by said process containing an amount of effect pigment of at least 5% by weight based on the total weight of the effect pigment paste, and using a vibrator for dispersing effect pigments to produce an effect pigment paste.in which the effect pigment paste obtained after the completion of the dispersion is free of grinding media.

Description

PROCEDURE FOR THE PREPARATION OF EFFECT PIGMENT PASTES The present invention relates to a process for preparing an effect pigment paste comprising at least steps (1) and (2), namely, preparing a mixture containing at least one effect pigment (a) and at least one polymer (b) in a liquid medium (c) (step (1)), and dispersing the mixture obtained after step (1) to obtain the effect pigment paste (step (2)), wherein step (2) is carried out using a vibrator and the effect pigment paste obtained after completion of step (2) is free of milling matter, an effect pigment paste that can be produced by said process containing an amount of effect pigment of at least 5% by weight based on the total weight of said effect pigment paste, and the use of a vibrator for dispersing effect pigments to produce an effect pigment paste.in which the effect pigment paste obtained after the completion of the dispersion is free of grinding media. STATE OF THE ART Pigment pastes are a well-known product in the art. Their use in the paint industry significantly simplifies the technically complex process of pigment dispersion, ensuring, for example, optimal wetting and dispersion of the pigments, thus achieving better distribution in the resulting paint. This improves the application properties of both the coating and the resulting finish, resulting in, for example, a particularly homogeneous color or a more even color distribution. Pigment pastes containing effect pigments (effect pigment pastes) are also produced separately as an intermediate product before being incorporated into a coating for the same reasons, as the direct addition of these pigments to the coating would lead to the problems mentioned above. In the production of effect pigment pastes, dissolving devices or vibrators are often used to ensure sufficient homogenization of the effect pigments within the pastes. A disadvantage of these processes for producing effect pigment pastes, which are known in the prior art and typically involve such vibrators and / or solvents, is the frequent formation of dust, which is undesirable for the safety of the production workers. Furthermore, these processes often require a subsequent cleaning step, particularly due to the drying of pigment and / or binder agglomerates that accumulate on the edges of the containers used to produce the pastes when the aforementioned stirring and / or dissolving technique is employed.In addition, comparatively long processing times (stirring times) are often required, which is undesirable for economic reasons. > CC >> Grinding media are often used for homogenization: for example, the DE document - 2005 024722 A1 refers to pigment preparations for which the pigments are homogenized with suitable dispersing agents using zirconium oxide or corundum grinding media. The use of mixed zirconium oxide grinding media is also known from US 2004 / 0059050 A1. The use of glass or steel balls as grinding media for this purpose is known from WO 2012 / 002569 A1, WO 2009 / 068462 A1, and EP 1 080 810 A1. However, the disadvantage of these procedures is that the milling media used must be separated from the effect pigment pastes in a separate processing step after they have been produced, for example, by filtration. Furthermore, the use of milling media in the production of effect pigment pastes can cause undesirable damage to the effect pigments. Therefore, pigmented effect pastes are needed whose manufacturing process does not present the aforementioned drawbacks. Object It is therefore an object of the present invention to provide a process for the production of effect pigment pastes that has advantages over the known process of the prior art. In particular, it is an object of the present invention to provide such a process for the production of effect pigment pastes that eliminates a separation step of the milling media commonly used for the production of effect pigment pastes. Furthermore, the process must provide for the gentlest possible dispersion of the effect pigments to prevent damage to the pigments during the manufacturing process of the effect pigment paste.Furthermore, it was the task of the present invention to provide a process for the production of effect pigment pastes, which allows a reduction of emissions in the form of pigment powders and, if necessary, also of solvent vapors and the temporary reduction or complete avoidance, in particular, of the resulting cleaning work. Solution This task is accomplished with the objects claimed in the patent claims, as well as with the preferred embodiments of these objects described in the following description. A first object of the present invention is therefore a process for preparing an effect pigment paste comprising at least steps (1) and (2), namely (1) preparing a mixture comprising at least one effect pigment (a) and at least one polymer (b) in a liquid medium (c), and (2) dispersing the mixture obtained in step (1) to obtain the effect pigment paste, wherein step (2) is carried out using a vibrator and the effect pigment paste obtained after completion of step (2) is free of grinding media. > CC >> Another object of the present invention is the use of a vibrator for the dispersion of effect pigments to produce an effect pigment paste, wherein the effect pigment paste obtained after completion of the dispersion is free of grinding media. Another object of the present invention is an effect pigment paste, which can be prepared by the process according to the invention, namely, by the process comprising at least steps (1) and (2), namely (1) preparing a mixture comprising at least one effect pigment (a) and at least one polymer (b) in a liquid medium (c), and (2) dispersing the mixture obtained in step (1) to obtain the effect pigment paste, wherein step (2) is carried out using a vibrator and the effect pigment paste obtained after carrying out step (2) is free of grinding bodies, and wherein the effect pigment paste contains an amount of effect pigment (a) of at least 5% by weight, based on the total weight of the effect pigment paste. Effect pigment pastes with a minimum effect pigment content of at least 5% by weight cannot be successfully produced by the conventional procedure involving stirring instead of agitation, as shown by the experimental data presented below, especially when using an aluminum effect pigment as the effect pigment (a) (see experimental part: Comparative effect pigment paste VEP2 versus effect pigment paste EP3). Surprisingly, the process for producing an effect pigment paste was found to be characterized by a completely dust-free processing of the effect pigments during paste formulation. As a result, emissions of pigment dust that are typically produced are significantly reduced, and the associated cleanup work can be avoided or at least minimized, making the process advantageous from both a workplace safety and environmental perspective. Finally, the process according to the invention also ensures consistent quality in the effect pigment pastes produced. Furthermore, it was surprisingly found that the process according to the invention is characterized by the fact that mechanical removal of the grinding media is not required after the production of the effect pigment paste, and therefore a step of separating such grinding media, which is commonly used, can be dispensed with. In general, the process according to the invention is also advantageously characterized by time savings and, consequently, by an economic advantage, since the aforementioned separation step can be omitted. Furthermore, it was surprisingly found that the procedure according to the invention only allows for the gentle dispersion of the effect pigments by using a vibrator, thus avoiding damage to the pigments during the manufacturing process of the effect pigment paste, but nevertheless achieving at least as good a dispersion of the effect pigments as by > CC the agitation or dissolution commonly used. Furthermore, the procedure according to the invention allows surprisingly shorter processing times than the conventional procedure carried out using vibrators due to the use of a vibrator in step (2), which is advantageous for economic reasons. Furthermore, by using the vibrator, the procedure according to the invention allows for better standardization compared to conventional procedures such as the stirring process: when using vibrators, it is necessary to adjust, for example, the height and speed of the vibrator during the manufacturing process of the effect pigment pastes, whereas parameters such as frequency, time, can geometry, and degree of filling are much easier to adjust when using a vibrator in comparison. Finally, it was surprisingly found that the procedure according to the invention using a vibrator not only allows for a dispersion of the effect pigments at least as good as that achieved by the commonly used stirring or dissolving, but also requires no subsequent cleaning step, since, in contrast to the conventional procedure carried out using stirring and / or solvents, no drying of the pigment and / or binder agglomerates occurs during the manufacturing process. DETAILED DESCRIPTION The term "comprising" in the sense of the present invention, in relation to the effect pigment paste produced according to the invention and also in relation to the process according to the invention, preferably means "consisting of." In this context, with respect to the effect pigment paste produced according to the invention, in addition to components (a), (b), and (c), one or more of the additional components mentioned below may optionally be contained in the effect pigment paste produced according to the invention. All components may be present in their respective preferred embodiments mentioned below. With respect to the process according to the invention, in addition to steps (1) and (2), one or more additional steps mentioned below may also form part of the process.All steps can be used in their respective preferred embodiments mentioned below. The term dispersion in relation to pigments or effect pigments within the meaning of the present invention is known to those skilled in the art and is defined, for example, in the Römpp Chemie Lexikon, Lacke und Druckfarben, Thieme Verlag, 1998, page 148. Accordingly, with reference to DIN 55943 (November 1993), it should be understood as the breaking up of agglomerates present in a powdered pigment in a liquid medium, the dispersing medium, into smaller particles and their simultaneous wetting by the dispersing medium. The term pigment paste is also known to the expert in the field and is defined, by > CC >> For example, in the Römpp Lexikon, Lacke und Druckfarben, Thieme Verlag, 1998, page 452: “Pigment pastes” are preparations of pigment mixtures in carrier materials, such as polymers, in which the pigments are present at a concentration higher than that corresponding to the subsequent application. Consequently, an effect pigment paste represents a pigment paste that contains at least one effect pigment—specifically, at least one effect pigment (a) as a pigment. The subsequent application of pigment pastes is usually in the manufacture of coating compositions, such as base coats. Thus, an effect pigment paste is distinguished from a coating agent, such as a base coat, in that it is simply a preliminary step in the manufacture of such a coating agent. Therefore, a pigment paste as such cannot be used as a coating agent in itself.In pigment pastes, the relative weight proportion of pigments to polymers is usually higher than in the coating agents for which the paste is ultimately used. In addition to carrier materials, such as the polymer (b), also called paste binders, and the effect pigment (a), liquid diluents, such as water and / or organic solvents, are also present in the pigment paste, acting as a liquid medium (c). Various additives, such as wetting agents and / or thickeners, may also be used in a pigment paste. The terms effect pigment paste and effect pigment dispersion are interchangeable in this document. The expert is also familiar with the term vibrator. This refers to a device capable of vibrating, i.e., dispersing the mixture obtained after step (1) within step (2) of the procedures according to the invention for obtaining the effect pigment paste by means of vibration. The terms shake and stir are interchangeable herein and are clearly distinguished from the term agitate. In particular, when using a vibrator, no additional auxiliary means are required as with a stirrer, such as stirring rods or paddles. Procedure according to the invention The process according to the invention is a method for preparing an effect pigment paste. The effect pigment paste obtained after completing step (2) of the process according to the invention is free of grinding media. Grinding media, as understood here, are conventional grinding media known to a person skilled in the art, which are in a solid aggregate state, retain this aggregate state after the production of the respective pigment paste, and do not change their shape, particularly their plastic form, during the production of the pastes. Such conventional grinding media are, in particular, grinding media made of metals, semimetals, metal oxides, semimetal oxides, ceramics, and glass. Preferably, the process according to the invention is carried out entirely without the use of grinding media. Alternatively, grinding media may be added to the mixture. CC obtained after step (1) of the procedure according to the invention or during the performance of steps (1) and (2) can be carried out using these grinding media. In this case, however, the grinding media used are characterized by being in a solid state of aggregation at the beginning of the performance of step (2), but during the performance of step (2) they completely change to a liquid state and then become part of the liquid medium (c) or are themselves ground during the performance of step (2) and are then dispersed in the liquid medium (c), so that the effect pigment paste obtained after the performance of step (2) is free of grinding media. Preferably, the grinding media used in this case are selected from the group consisting of frozen water, frozen organic solvents, and grinding media of organic polymers and mixtures thereof. Preferably, the procedure according to the invention does not comprise an agitation step. The procedure according to the invention for the preparation of the effect pigment pastes has no other particular methodological feature, but can be carried out by mixing at least the essential ingredients (a), (b) and (c) described above and homogenizing the resulting mixture. Step (1) Step (1) of the procedure according to the invention provides for the preparation of a mixture comprising at least one effect pigment (a) and at least one polymer (b) in a liquid medium (c). The order of addition of the individual components is arbitrary, particularly if an aluminum effect pigment is used as the effect pigment (a). If a mica metal oxide pigment is used as the effect pigment (a), preferably all components are introduced except for the effect pigment (a), and the latter is added last to the resulting mixture. Step (2) Step (1) of the procedure according to the invention provides for the dispersion of the mixture obtained after performing step (1) to obtain the effect pigment paste, wherein step (2) is carried out using a vibrator and the effect pigment paste obtained after completing step (2) is free of grinding media. Commercially available vibrators are suitable for use in step (2) of the procedures according to the invention. Examples of such vibrators include devices from Fast & Fluid, such as the SK550 or the SK550 1.1 from the Skandex series. Collomix and Corob also offer suitable vibrators. Preferably, step (2) is performed in a container with a fill size in the range of 0.2 to 40 L. Preferably, step (2) is performed in a closed container. Preferably, the container used in step (2) is filled such that the fill level of the container is in the range of 15 to 95%. > DC Basically, containers of any type are suitable. Disposable or reusable containers can be used. Preferably, the mixture obtained according to step (1) of the procedure according to the invention is filled into a plastic bag, and the dispersion according to step (2) is carried out in the plastic bag. In this case, the degree of filling is preferably in the range of 15 to 80%. The plastic bag constitutes a reusable container and can be used several times, even without intermediate cleaning, especially when producing several successive batches of pigment pastes with identical composition. The duration of step (2) depends on the quantity of the effect pigment paste to be produced. In principle, however, the duration of step (2) of the procedure according to the invention is preferably a maximum of 20 minutes, particularly preferably a maximum of 18 minutes, and more preferably a maximum of 16 minutes. Preferably, step (2) is carried out for a duration of 1 to 15 minutes. Preferably, the temperature increase detected when performing step (2) of the procedure according to the invention is in the range of 0 to 40°C, preferably from 0.1 to 30°C. Preferably, step (2) of the procedure according to the invention is performed by shaking at a frequency in the range of 6 to 20 Hz, more preferably 8 to 18 Hz, more preferably 10 to 16 Hz. Preferably, step (2) of the procedure according to the invention is performed by vibration at an amplitude in the range of 1.0 to 8.0 cm, more preferably from 1.2 to 7.0 cm, more preferably from 1.4 to 6.5 cm. Preferably, step (2) of the procedures according to the invention is carried out by performing a vibration at an acceleration in a range of >1G to 26 G, particularly preferably from 2 to 23 G, especially from 4 to 19 G. Pigmented effect paste Preferably, the solids content of the effect pigment paste produced according to the invention is in the range of 15 to 65% by weight, particularly preferably 17.5 to 60% by weight, more preferably 20 to 55% by weight, in particular 22.5 to 50% by weight, and more preferably 25 to 45% by weight, in each case based on the total weight of the effect pigment paste. The determination of the solids content, i.e., the non-volatile content, is carried out according to the method described below. The weight percentage proportions of all components (a), (b) and (c) contained in the effect pigment paste according to the invention, as well as any other components that may be additionally present, add up to 100% by weight, based on the total weight of the effect pigment paste. Effect pigment paste - effect pigment (a) The effect pigment paste produced according to the invention contains at least one > CC >> effect pigment as component (a), preferably in an amount of at least 10% by weight, based on the total weight of the effect pigment paste. An expert in the field is familiar with the term "effect pigments." The corresponding definition can be found, for example, in the Römpp Lexikon, Lacke und Druckfarben (Paint and Paint Dictionary), Thieme Verlag, 1998, pages 176 and 471. A definition of pigments in general and further specifications for them are regulated in DIN 55943 (date: October 2001). Preferably, effect pigments are those pigments that have an optical effect or both color and optical effect, especially an optical effect. Therefore, the terms "optical and color effect pigment," "optical effect pigment," and "effect pigment" are preferably used interchangeably. Preferred effect pigments include, for example, platelet-shaped metallic effect pigments such as aluminum flake pigments, gilt bronzes, fire-tinted bronzes, and / or iron oxide aluminum pigments; pearlescent pigments such as fish silver, basic lead carbonate, bismuth oxychloride, and / or metal oxide mica pigments; and / or other effect pigments such as flaked graphite, flaked iron oxide, multi-layer PVD film effect pigments, and / or liquid crystal polymeric pigments. Flake effect pigments are particularly preferred, especially flaked aluminum pigments and metal oxide mica pigments contained in the pigment paste.Preferably, therefore, the effect pigment paste according to the invention contains as at least one effect pigment (a) at least one metallic effect pigment, such as at least one aluminum effect pigment preferably in platelet form and / or at least one mica metal oxide pigment. Preferably, the effect pigment (a) used is in powder form. The effect pigment paste produced according to the invention may optionally contain other pigments, in particular color pigments and / or fillers, other than at least one effect pigment (a). However, it is preferable that the effect pigment paste produced according to the invention does not contain any other color pigments or fillers. Preferably, the effect pigment paste produced according to the invention contains an effect pigment (a) content of at least 5% by weight, more preferably at least 7% by weight, more preferably at least 10% by weight, in particular at least 13% by weight, more preferably at least 15% by weight, in each case based on the total weight of the effect pigment paste. Preferably, the effect pigment paste produced according to the invention contains an effect pigment content (a) in the range of 5 to 85% by weight, more preferably 7 to 80% by weight, more preferably 10 to 75% by weight, more preferably 13 to 70% by weight, more preferably 15 to 65% by weight, or 15 to 60% by weight, in each case based on the total weight of the effect pigment paste. Pigmented effect paste - polymer (b) The polymer (b) present in the effect pigment paste produced according to the invention > CC is used as a binder for pigment pastes. For the purposes of the present invention, the term "binder," in accordance with DIN EN ISO 4618 (German version, date: March 2007), preferably means the non-volatile portions responsible for film formation in a composition such as the effect pigment paste produced according to the invention, excluding the pigments contained therein, such as the at least one effect pigment (a), and any other pigments and / or fillers that may be present. The non-volatile content can be determined according to the method described below. Accordingly, a binder component is a particular component that contributes to the binder content of a composition such as the effect pigment paste produced according to the invention. Preferably, the polymer (b) is used in the form of an aqueous dispersion or solvent for the preparation of the effect pigment paste. As polymer (b) so-called seed core polymers (SCS) may be used. Such polymers are known, for example, from WO 2016 / 116299 A1. Alternatively or additionally, at least one polymer selected from the group consisting of polyurethanes, polyureas, polyesters, poly(meth)acrylates and / or copolymers of such polymers, in particular polyurethane-poly(meth)acrylates and / or polyureas, may be used as a polymer (b). The preferred polyurethanes are described, for example, in German patent application DE 199 48 004 A1, page 4, line 19 to page 11, line 29 (polyurethane prepolymer B1), in European patent application EP 0 228 003 A1, page 3, line 24 to page 5, line 40, in European patent application EP 0 634 431 A1, page 3, line 38 to page 8, line 9, and in international patent application WO 92 / 15405, page 2, line 35 to page 10, line 32. The preferred polyesters are described, for example, in document DE 4009858 A1, column 6, line 53 to column 7, line 61 and column 10, line 24 to column 13, line 3 or WO 2014 / 033135 A2, page 2, line 24 to page 7, line 10 and page 28, line 13 to page 29, line 13. The preferred polyurethane-poly(me)acrylate ((me)acrylates) copolymers and their preparation are described, for example, in WO 91 / 15528 A1, page 3, line 21 to page 20, line 33 and in DE 4437535 A1, page 2, line 27 to page 6, line 22. The preferred polyurethane-polyurea copolymers are polyurethane-polyurea particles, wherein the polyurethane-polyurea particles each contain, in the reacted form, at least one polyurethane prepolymer containing an isocyanate group with anionic groups and / or groups that can be converted into anionic groups, and at least one polyamine containing two primary amino groups and one or two secondary amino groups. Preferably, these copolymers are used in the form of an aqueous dispersion. In principle, these polymers can be prepared by the polyaddition of, for example, polyisocyanates with polyols and polyamines, which is known per se. Polymers (b) may each have functional groups, in particular, selected from the > κ Ν CC > > group consisting of OH groups, COOH groups and amino groups, in particular OH groups. Particularly preferred are hydroxyfunctional polyurethane-poly(meth)acrylate copolymers and hydroxyfunctional polyurethane-polyurea polyesters and copolymers. Preferably, the effect pigment paste produced according to the invention contains a proportion of polymer (b) in the range of 1.0 to 25% by weight, particularly preferably 1.5 to 20% by weight, very preferably 2.0 to 17.5% by weight, in particular 2.5 to 15% by weight, and more preferably 4.0 to 12.5% ​​by weight, in each case based on the total weight of the effect pigment paste. The determination of the proportion of polymer (b) in the effect pigment paste can be made by determining the solid content (also called non-volatile content, solid content, or solids content) of a dispersion containing the polymer (b) used for the production of the effect pigment paste. Preferably, the relative weight ratio of the at least one effect pigment (a) to the polymer (b) in the effect pigment paste is at least 1:1, or at least 1.2:1, or at least 1.5:1 or higher in each case, particularly preferably at least 2.0:1 or higher, very particularly preferred at least 2.5:1 or higher, especially at least 3.0:1 or higher. Preferably, the relative weight ratio of the at least one effect pigment (a) to the polymer (b) in the effect pigment paste is in the range of 10:1 to 1:1 or 8:1 to 1:1, particularly preferably in the range of 10:1 to 1.2:1 or 10:1 to 1.5:1 or in the range of 8:1 to 1.2:1 or 8:1 to 1.5:1. Pigmented effect paste - component (c) Step (1) of the procedures according to the invention provides for the preparation of a mixture comprising at least one effect pigment (a) and at least one polymer (b) in a liquid medium (c). To provide a liquid medium (c) in step (1), at least one diluent is preferably provided, which consequently acts as component (c). The effect pigment paste produced according to the invention therefore preferably comprises at least one such diluent. The diluent can be water and / or at least an organic solvent. The effect pigment paste produced according to the invention may be aqueous. Preferably, it is a system comprising water as the main solvent component, preferably in an amount of at least 20% by weight, and organic solvents in a smaller proportion, preferably in an amount of <20% by weight, each based on the total weight of the effect pigment paste. Preferably, the effect pigment paste then contains a water content of at least 20% by weight, more preferably at least 25% by weight, more preferably at least 30% by weight, in particular at least 35% by weight, and more preferably at least 40% by weight, in each case based on the total weight of the effect pigment paste.Preferably, the effect pigment paste then contains a proportion of water that is in the range of 20 to 75% by weight, more preferably in the range of 25 to 70% by weight, more preferably in the range of 30 to 65% by weight or up to 60% by weight or up to 57.5 >. cc -X % by weight, in each case based on the total weight of the effect pigment paste. Preferably, the effect pigment paste in this case contains a proportion of organic solvents that is in the range of <20% by weight, particularly preferably in the range of 0 to <20% by weight, very particularly preferably in the range of 0.5 to 20% by weight or up to 17.5% by weight or up to 15% by weight, in each case based on the total weight of the effect pigment paste. Alternatively, the effect pigment paste produced according to the invention may be solvent-based. Preferably, it is a system containing, as the main constituent, organic solvents, preferably in an amount of at least 20% by weight, and water in a smaller proportion, preferably in an amount of <20% by weight, in each case based on the total weight of the effect pigment paste. Preferably, the effect pigment paste then contains an organic solvent content of at least 20% by weight, more preferably at least 25% by weight, more preferably at least 30% by weight, in particular at least 35% by weight, more preferably at least 40% by weight, in each case based on the total weight of the effect pigment paste.Preferably, the effect pigment paste then contains a proportion of organic solvents in the range of 20 to 75% by weight, more preferably in the range of 25 to 70% by weight, more preferably in the range of 30 to 65% by weight, or up to 60% by weight, or up to 57.5% by weight, in each case based on the total weight of the effect pigment paste. Preferably, in this case, the effect pigment paste contains a proportion of water in the range of <20% by weight, particularly preferably in the range of 0 to <20% by weight, very particularly preferably in the range of 0.5 to 20% by weight, or up to 17.5% by weight, or up to 15% by weight, in each case based on the total weight of the effect pigment paste. The addition of organic solvents is particularly suitable for effect pigment pastes containing aluminum effect pigments as the effect pigment (a). However, effect pigment pastes according to the invention can also be completely or almost completely free of organic solvents, in particular if metal oxide (mica) pigments are used as the effect pigment (a). The expert is familiar with the term organic solvent. This term is defined, for example, in Council Directive 1999 / 13 / EC of 11 March 1999 (Article §2, point 18) (referred to therein as solvent). Examples of such organic solvents are (hetero)cyclic, (hetero)aliphatic or (hetero)aromatic hydrocarbons, mono- or polyhydric alcohols, ethers, esters, ketones and amides, such as N-methylpyrrolidone, N-ethylpyrrolidone, dimethylformamide, toluene, xylene, butanol, ethyl and butyl glycol and their acetates, butyl diglycol, diethylene glycol dimethyl ether, cyclohexanone, methyl ethyl ketone, methyl isobutyl ketone, acetone, isophorone or mixtures thereof. Effect pigment paste - other optional components > CC >> The pigmented effect paste produced according to the invention may contain other optional ingredients or components: In addition to at least one effect pigment (a), the effect pigment paste may also contain other typical color pigments different from the effect pigment (a). A person skilled in the art is familiar with the term color pigments. The terms coloring pigment and color pigment are interchangeable. Inorganic and / or organic pigments may be used as coloring pigments. Preferably, the color pigment is an inorganic color pigment. White pigments, color pigments, and / or black pigments are particularly preferred as color pigments. Examples of white pigments include titanium dioxide, zinc white, zinc sulfide, and lithopone. Examples of black pigments include carbon black, iron-manganese black, and spinel black.Examples of colored pigments include chromium oxide, hydrated chromium oxide green, cobalt green, ultramarine green, cobalt blue, ultramarine blue, manganese blue, cobalt manganese violet, iron oxide red and cadmium sulfoselenide, molybdate red and ultramarine red, iron oxide brown, mixed brown, spinel and corundum phases and chromium orange, iron oxide yellow, nickel titanium yellow, chromium titanium yellow, cadmium sulfide, cadmium zinc sulfide, chromium yellow, and bismuth vanadate. The proportion of colored pigments is preferably in the range of 1.0 to 40.0% by weight, preferably 2.0 to 35.0% by weight, and particularly preferably 5.0 to 30.0% by weight, in each case based on the total weight of the effect pigment aqueous paste.However, it is preferable that the effect pigment paste produced according to the invention contains at least one effect pigment (a) as its sole pigment, i.e., preferably it does not contain any additional color pigments. Preferably, the effect pigment paste also does not contain fillers. The effect pigment paste may optionally comprise at least one thickener (also referred to as a thickener). Examples of such thickeners are inorganic thickeners, for example, metallic silicates such as coating silicates, and organic thickeners, for example, poly(meth)acrylic acid thickeners and / or (meth)acrylic acid copolymer thickeners, polyurethane thickeners, and polymer waxes. The metallic silicate is preferably selected from the smectite group. More preferably, the smectites are selected from the group consisting of montmorillonites and hectorites. In particular, the montmorillonites and hectorites are selected from the group consisting of aluminum-magnesium silicates and layered sodium-magnesium and sodium-magnesium-fluorine-lithium silicates. These layered inorganic silicates are marketed, for example, under the brand name Laponite®.Poly(meth)acrylic acid-based thickeners and (meth)acrylic acid-(meth)acrylate copolymer thickeners are optionally crosslinked and / or neutralized with a suitable base. Examples of such thickeners are Alkali Swellable Emulsions (ASEs) and their hydrophobically modified variants, Hydrophically Modified Alkali Swellable Emulsions (HASEs). Preferably, these thickeners are anionic. κ κ c C Corresponding products, such as Rheovis® AS 1130, are available on the market. Polyurethane-based thickeners (e.g., associative polyurethane thickeners) are optionally crosslinked and / or neutralized with a suitable base. Corresponding products, such as Rheovis® PU 1250, are commercially available. Suitable polymer waxes are, for example, optionally modified polymer waxes based on ethylene-vinyl acetate copolymers. A corresponding product is commercially available, for example, under the name Aquatix® 8421. Preferably, at least one thickener is present in the effect pigment paste produced according to the invention in an amount of at most 10% by weight, particularly preferably at most 7.5% by weight, very particularly preferred at most 5% by weight, in particular at most 3% by weight, more preferably at most 2% by weight, in each case based on the total weight of the effect pigment paste. The effect pigment paste produced according to the invention may contain one or more commonly used additives as additional component(s), depending on the desired application. For example, the effect pigment paste may contain a certain amount of at least one organic solvent, as previously mentioned. Furthermore, the effect pigment paste may contain at least one additive selected from the group consisting of reactive diluents, light stabilizers, antioxidants, deaerating agents, emulsifiers, slip additives, polymerization inhibitors, free radical polymerization initiators, adhesion promoters, flow agents, film-forming aids, sag control agents (SCA), flame retardants, corrosion inhibitors, driers, biocides, and mattifying agents. These may be used in known and customary proportions.Preferably, its content, based on the total weight of the effect pigment paste, is from 0.01 to 20.0% by weight, more preferably from 0.05 to 15.0% by weight, particularly preferably from 0.1 to 10.0% by weight, more preferably from 0.1 to 7.5% by weight, especially from 0.1 to 5.0% by weight and most preferably from 0.1 to 2.5% by weight. Pigmented effect paste according to the invention Using the procedures according to the present invention, an effect pigment paste can be produced. Another object of the present invention is an effect pigment paste that can be produced by the procedure according to the invention, wherein the effect pigment paste contains an amount of effect pigment (a) of at least 20% by weight, based on the total weight of the effect pigment paste, particularly when the at least one effect pigment is an aluminum effect pigment. Effect pigment pastes with a minimum content of at least 20% by weight of effect pigment are not those that can be successfully produced by the conventional procedure involving a stirring process, as shown by the experimental data presented below (see the experimental part: Comparison of effect pigment paste VEP2 versus effect pigment paste EP3). All preferred embodiments described above in relation to the procedure of > CC >> in accordance with the invention herein are also preferred embodiments with respect to the effect pigment paste according to the invention. Use in accordance with the invention The vibrator used in step (2) of the procedure according to the invention is suitable for dispersing effect pigments to produce an effect pigment paste. Another object of the present invention is, therefore, the use of a vibrator to disperse effect pigments to produce an effect pigment paste, wherein the effect pigment paste obtained after complete dispersion is free of milling media. Preferably, the effect pigment paste is that produced by the processes according to the invention. All preferred embodiments described above in relation to the effect pigment paste produced according to the invention and the process according to the invention are also preferred embodiments with respect to the use of the vibrator to disperse effect pigments to produce an effect pigment paste. METHODS OF DETERMINATION 1. Determination of the non-volatile fraction The determination of the non-volatile fraction (of the solid content) is carried out according to DIN EN ISO 3251 (date: June 2008). In this process, 1 g of sample is weighed onto a previously dried aluminum plate and dried for 60 minutes at 125 °C in an oven, cooled in a desiccator, and weighed again. The residue, relative to the total amount of sample used, corresponds to the non-volatile fraction. 2. Determination of the number and weight average molecular weight The number-average molecular weight (Mn) is determined by gel permeation chromatography (GPC). The method is based on DIN 55672-1 (August 2007). In addition to number-average molecular weight, weight-average molecular weight (Mw) and polydispersity (the ratio of weight-average molecular weight (Mw) to number-average molecular weight (Mn)) can also be determined using this method. Tetrahydrofuran is used as the eluent. The determination is performed relative to polystyrene standards. The column material consists of styrene-divinylbenzene copolymers. 3. Determination of the OH number The determination of the OH number is based on R.-P. Krüger, R. Gnauck, and R. Algeier, Plaste und Kautschuk, 20, 274 (1982) and is performed using acetic anhydride in the presence of 4-dimethylaminopyridine as a catalyst in a tetrahydrofuran (THF) / dimethylformamide (DMF) solution at room temperature (18 to 23°C). The remaining excess acetic anhydride is completely hydrolyzed after acetylation, and the acetic acid is back-titrated potentiometrically with an alcoholic potassium hydroxide solution. The acetylation time is 60 minutes and is sufficient > CC >> to ensure complete conversion. 4. Evaluation of the appearance of spots To assess the appearance of specks, effect pigment pastes are examined according to the following general rule: The respective paste is applied using a 100 µm box squeegee (if using aluminum effect pigments) or a 50 µm box squeegee (if using mica effect pigments) onto a 9 cm x 15 cm glass plate. After a drying time of 10 minutes at 80°C in a convection oven, the resulting film is visually assessed for the appearance of specks by holding it up to a light source to avoid mistaking air pockets for specks. A score from 1 to 5 is given (1 = no specks / 5 = many specks). Grade 1 corresponds to the iO (agree) rating. > κ C 16 κ c C > EXAMPLES AND COMPARATIVE EXAMPLES The following examples and comparative examples serve to explain the invention, but should not be interpreted restrictively. Unless otherwise stated, indications in parts are parts by weight and indications in percentages. 1. Characterization of the components used Polyester component: Polyester 1: produced according to DE 4009858 A1, example D (column 16, line 37 to column 6, line 60) Alu Stapa Hydrolux® 2154: Commercial aluminum effect pigment, available from Altana-Eckart, with a solids content of 65% by weight Mearlin® Exterior Super Red 439Z: Commercial-grade mica effect pigment, available from Merck. Mearlin® Exterior Fine Violet 539 V: Commercially available mica effect pigment from Merck. 2. Pigment pastes with an effect achieved through the use of aluminum effect pigments 2.1 Comparative effect pigment paste VEP1 A comparative effect pigment paste VEP1, composed of 33.33 parts by weight of polyester 1, 33.33 parts by weight of Alu Stapa Hydrolux® 2154 and 33.33 parts by weight of butyl glycol, is prepared as follows, using 4000 g of each of the aforementioned components: The butyl glycol is placed in a container, and Alu Stapa Hydrolux® 2154 is added in portions while stirring. The resulting mixture is stirred for 15 minutes. The stirring speed is adjusted so that the drum is clearly visible. The polyester component is then added while stirring, and the mixture is stirred for another 15 minutes. The total processing time is therefore 30 minutes. After the stirring process, cleaning was necessary due to dust formation and sedimentation of pigment and polyester residue on the side of the container. No speckling was observed. 2.2 EP1 effect pigment paste according to the invention A pigment paste with EP1 effect according to the invention, consisting of 33.33 parts by weight of polyester 1, 33.33 parts by weight of Alu Stapa Hydrolux® 2154 and 33.33 parts by weight of butyl glycol, is prepared as follows, 200 g of each of the aforementioned components having been used: The three components mentioned are added together in any order to a 1 L capacity container (disposable container) and agitated for 12 minutes without any further premixing. The Fast & Fluid SK550 device is used as the vibrator. The frequency during the > The CC vibration frequency is 12 Hz. Therefore, the total processing time is only 6 minutes. Cleaning was not required, as no dust formation or sedimentation of pigment and polyester residues was observed. No speckling (iO) was observed. 2.3 EP2 effect pigment paste according to the invention A pigment paste with EP2 effect according to the invention, consisting of 33.33 parts by weight of polyester 1, 33.33 parts by weight of Alu Stapa Hydrolux® 2154 and 33.33 parts by weight of butyl glycol, is prepared as follows, 50 g of each of the aforementioned components having been used: The three components mentioned are added together in any order to a 0.25 L capacity container (disposable container) and stirred for 3 minutes without any additional premixing. The Fast & Fluid SK550 device is used as a vibrator. The vibration frequency is 12 Hz. Therefore, the total processing time is only 3 minutes. Cleaning was not required, as no dust formation or sedimentation of pigment and polyester residue was observed. No speckling was observed. 2.4 EP3 effect pigment paste according to the invention A pigment paste with EP3 effect according to the invention, consisting of 50% by weight of polyester 1, 45% by weight of Alu Stapa Hydrolux® 2154 and 5% by weight of butyl glycol, is prepared as follows, wherein 600 g of butyl glycol, 6000 g of polyester 1 and 5400 g of Alu Stapa Hydrolux® 2154 have been used: The three components mentioned are added together in any order to a container with a filling capacity of 18 L (disposable container) and stirred for 12 minutes without any additional premixes. The Fast & Fluid SK550 device is used as a vibrator. The vibration frequency is 12 Hz. Therefore, the total processing time is only 12 minutes. Cleaning was not required, as no dust formation or sedimentation of pigment and polyester residue was observed. No speckling was observed. 2.5 Comparative effect pigment paste VEP2 An attempt was made to produce a comparative effect pigment paste VEP2 from 50 wt% Polyester 1, 45 wt% Alu Stapa Hydrolux® 2154, and 5 wt% butyl glycol, using 600 g of butyl glycol, 6000 g of Polyester 1, and 5400 g of Alu Stapa Hydrolux® 2154, and employing the production method described in section 2.1 in relation to VEP1. However, the resulting mixture had such a high viscosity that it was not possible to stir it, and therefore VEP2 could not be produced under these conditions. 2.6 EP4 effect pigment paste according to the invention An EP4 effect pigment paste according to the invention consisting of 33.33 parts by weight of polyester 1, 33.33 parts by weight of Alu Stapa Hydrolux® 2154 and 33.33 parts by weight of butyl glycol is prepared as follows, 4000 g of each component having been used > κ κ c C mentioned: ” The three components mentioned are added in any order to a plastic bag (e.g., a reusable container). The bag is sealed, and the mixture inside is vibrated without any further premixing for 12 minutes. The Fast & Fluid SK550 device is used as the vibrator. The frequency during agitation is 12 Hz. Therefore, the total processing time is only 12 minutes. Cleaning was not required, as no dust formation or sedimentation of pigment and polyester residue was observed. No speckling (iO) was observed. 3. Pigment pastes with a mica effect, using mica-effect pigments 3.1 Comparative Effect Pigment Paste EP3 Next, a comparative effect pigment paste VEP3 is prepared made with 75 parts by weight of a mixing varnish ML1 and 25 parts by weight of Mearlin® Exterior Super Red 439Z, in which 9000 g of ML1 and 3000 g of Mearlin® Exterior Super Red 439Z have been used: First, ML1 is prepared by mixing the following components: Rheovis® AS 1130 (commercially available polymer as a thickener), Dispex® Ultra FA 4437 (commercially available additive), 2,4,7,9-tetramethyl-5-decyndiol, 52% in butyl glycol (available from BASF SE) and deionized water and 10% dimethylethanolamine in water. The ML1 is placed in a container with a filling capacity of 18 L (disposable container), and the effect mica-pigment is slowly added using a dissolving device, taking care to avoid pigment clumping on the rim and in the dissolving device. This process takes approximately 20 minutes. After adding the pigment, the resulting mixture is dissolved for another 20 minutes. The total processing time is therefore 40 minutes. Cleaning was necessary due to observed dust formation and sedimentation of pigment and polyester residue. Mica and binder particles were found adhering to the stirrer and the walls of the container. 3.2 EP5 effect pigment paste according to the invention A pigmented paste with an EP3 effect is prepared from 75 parts by weight of a mixed varnish ML1 and 25 parts by weight of Mearlin® Exterior Super Red 439Z, using 9000 g of ML1 and 3000 g of Mearlin® Exterior Super Red 439Z: The ML1 is prepared as described in section 3.1. The two components mentioned are added together in any order to a container with a filling capacity of 18 L (disposable container) and stirred for 12 minutes without any additional premixing. The Fast & Fluid SK550 device is used as a vibrator. The vibration frequency is 12 Hz. Therefore, the total processing time is only 12 minutes. Cleaning was not required, as no dust formation or sedimentation of pigment and polyester residue was observed. No speckling was observed.

Claims

1. A process for preparing an effect pigment paste characterized in that it comprises at least steps (1) and (2), namely (1) preparing a mixture comprising at least one effect pigment (a) and at least one polymer (b) in a liquid medium (c), and (2) dispersing the mixture obtained according to step (1) to obtain the effect pigment paste, wherein step (2) is carried out using a vibrator and the effect pigment paste obtained after carrying out step (2) is free of grinding media.

2. The process according to claim 1, characterized in that a metallic effect pigment and / or a mica metal oxide pigment is used as at least one effect pigment (a).

3. The process according to claim 1 or 2, characterized in that an aluminum pigment is used as at least one effect pigment (a).

4. The procedure according to one of the preceding claims, characterized in that step (2) is performed in a closed container.

5. The procedure according to one of the preceding claims, characterized in that the mixture obtained according to step (1) is introduced into a plastic bag and the dispersion according to step (2) is carried out in the plastic bag.

6. The procedure according to one of the preceding claims, characterized in that step (2) is performed by shaking at a frequency in the range of 6 to 20 Hz.

7. The procedure according to one of the preceding claims, characterized in that step (2) is performed by shaking with an amplitude between 1.0 and 8.0 cm.

8. The process according to any of the preceding claims, characterized in that the effect pigment paste contains at least one effect pigment (a) in an amount of at least 5% by weight, each of them based on the total weight of the effect pigment paste.

9. The procedure according to one of the preceding claims, characterized in that step (2) is performed during a period of 1 to 15 minutes.

10. The process according to any one of the preceding claims, characterized in that the polymer (b) is selected from the group consisting of polyurethanes, polyureas, polyesters, poly(meth)acrylates, copolymers of said polymers, seed core polymers and mixtures thereof.

11. The process according to one of the preceding claims, characterized in that it is carried out without the use of grinding means.

12. The process according to any one of claims 1 to 10, characterized in that grinding media are added to the mixture obtained after step (1) and step (2) is carried out using said grinding media, wherein the grinding media are in a state of solid aggregation at the beginning of carrying out step (2), but during the carrying out of step (2) change completely to a liquid aggregate state and become part of the liquid medium (c) or during the carrying out of step (2) are crushed and are then present in a dispersed form in the liquid medium (c), so that the effect pigment paste obtained after carrying out step (2) is free of grinding media.

13. The process according to claim 12, characterized in that the grinding media are selected from the group consisting of frozen water, frozen organic solvents, and grinding media of organic polymers and mixtures thereof.

14. An effect pigment paste that can be produced by the process of 10 according to any one of claims 1 to 13, characterized in that said effect pigment paste contains an amount of effect pigment (a) of at least 5% by weight, based on the total weight of said effect pigment paste.

15. A use of a vibrator to disperse effect pigments to produce an effect pigment paste, characterized in that the effect pigment paste obtained after completing the dispersion is free of grinding media.