Classifications

• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D17/00—Pigment pastes, e.g. for mixing in paints
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
  • C01D17/00—Rubidium, caesium or francium compounds
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D17/00—Pigment pastes, e.g. for mixing in paints
  • C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
  • C09D17/006—Metal
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F31/00—Mixers with shaking, oscillating, or vibrating mechanisms
  • B01F31/60—Mixers with shaking, oscillating, or vibrating mechanisms with a vibrating receptacle
• • C—CHEMISTRY; METALLURGY
  • C01—INORGANIC CHEMISTRY
  • C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
  • C01D17/00—Rubidium, caesium or francium compounds
  • C01D17/003—Compounds of alkali metals
  • C01D17/006—Preparation of potassium compounds comprising precipitating potassium ions by an organic reagent or extracting them by a liquid organic phase
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
  • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
  • C09C1/62—Metallic pigments or fillers
  • C09C1/64—Aluminium
  • C09C1/644—Aluminium treated with organic compounds, e.g. polymers
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
  • C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
  • C09C1/62—Metallic pigments or fillers
  • C09C1/64—Aluminium
  • C09C1/644—Aluminium treated with organic compounds, e.g. polymers
  • C09C1/646—Aluminium treated with organic compounds, e.g. polymers concomitant with mechanical comminution, shaping or abrasion of the particles
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
  • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
  • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
  • C09C3/045—Agglomeration, granulation, pelleting
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK  ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
  • C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
  • C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
  • C09C3/046—Densifying, degassing, packaging
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
  • C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
  • C09D7/80—Processes for incorporating ingredients

Definitions

• the present invention relates to a method for producing an effect pigment paste comprising at least steps (1) and (2), namely production of a mixture containing at least one effect pigment (a) and at least one polymer (b) in a liquid medium (c) (step ( 1)), and
• step (2) Dispersion of the mixture obtained after step (1) to obtain the effect pigment paste (step (2)), step (2) being carried out using a vibrator and the effect pigment paste obtained after completion of carrying out step (2) being free of grinding media, a Effect pigment paste which can be produced by means of this process, wherein it contains an amount of effect pigment of at least 5% by weight, based on the total weight of the effect pigment paste, as well as a use of a vibrator for dispersing effect pigments for producing an effect pigment paste, the after completion the effect pigment paste obtained after the dispersion is free of grinding media.
• Pigment pastes are known in the prior art. The use of pigment pastes in the paint industry makes the technically complex process of
• Pigment dispersion is made much easier, since this ensures, for example, optimal wetting and dispersion of the pigments, so that an improved distribution state is also achieved in the resulting paint.
• effect pigment-containing pigment pastes effect pigment pastes
• An object of the present invention is therefore to provide a method for producing effect pigment pastes which have advantages over those from the Has prior art known method.
• the method should provide for the most gentle possible dispersion of the effect pigments in order to prevent damage to the pigments during the production process of the effect pigment paste.
• a first object of the present invention is therefore a method for producing an effect pigment paste comprising at least steps (1) and (2), namely
• step (2) Dispersion of the mixture obtained in step (1) to obtain the effect pigment paste, step (2) being carried out using a vibrator and the effect pigment paste obtained after completion of carrying out step (2) being free of grinding media.
• Another object of the present invention is the use of a vibrator for dispersing effect pigments for the production of an effect pigment paste, the effect pigment paste obtained after the end of the dispersion being free of grinding media.
• the present invention further provides an effect pigment paste which can be produced by means of the method according to the invention, ie by means of the method comprising at least steps (1) and (2), namely (1) production of a mixture comprising at least one effect pigment (a) and at least a polymer (b) in a liquid medium (c), and (2) dispersing the mixture obtained in step (1) to obtain the effect pigment paste, step (2) being carried out using a vibrator and the after completion of carrying out step (2) the effect pigment paste obtained is free of grinding media, 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 content of at least 5% by weight of effect pigment cannot be successfully produced by means of conventional processes that provide for stirring instead of shaking, as the following experimental data show, in particular when an aluminum effect pigment is used as effect pigment (a) (cf. Experimental part: Comparative effect pigment paste VEP2 vs. effect pigment paste EP3).
• the process for producing an effect pigment paste is characterized by a largely to completely dust-free processing of effect pigments during the formulation of the paste. This at least reduces emissions in the form of pigment dusts that usually occur and the associated cleaning work can also be carried out prevented or at least reduced, whereby the process is advantageous in terms of occupational safety and ecology.
• the method according to the invention also enables the produced effect pigment pastes to have a constant quality.
• the process according to the invention is distinguished by the fact that no mechanical removal of grinding media is necessary after production of the effect pigment paste and thus a separation step of such grinding media, which is usually used, can be dispensed with.
• the method according to the invention is thereby advantageously also distinguished by a saving of time and thus by an economic advantage, since the aforementioned separation step can be dispensed with.
• the method according to the invention enables the effect pigments to be dispersed only gently by using a vibrator, whereby damage to the pigments during the production process of the effect pigment paste can be prevented, but at least as good a dispersion of the effect pigments is achieved as by the usual stirring or dissolvers.
• step (2) the method according to the invention surprisingly enables shorter processing times than conventional methods which are carried out using stirrers, which is advantageous for economic reasons.
• the method according to the invention enables better standardization compared to conventional methods such as a stirring process: when using stirrers, it is necessary, for example, to adjust the stirrer height and speed during the manufacturing process of effect pigment pastes, whereas parameters such as frequency, time, Can geometry and degree of filling are much easier to adjust using a vibrator in comparison.
• the method according to the invention not only enables at least as good a dispersion of the effect pigments by using a vibrator as by commonly used stirring or dissolvers, but also that no subsequent cleaning step is required, since in contrast to conventional methods that use be carried out by stirring and / or dissolvers, no drying of pigment and / or binder agglomerates occurs during the manufacturing process.
• the term “comprising” in the sense of the present invention in connection with the effect pigment paste produced according to the invention and also in connection with the method according to the invention preferably has the meaning “consisting of”.
• the effect pigment paste produced according to the invention in addition to components (a), (b) and (c), one or more of the other components mentioned below may be contained in the effect pigment paste produced according to the invention. All components can each be present in their preferred embodiments mentioned below.
• the method according to the invention - in addition to steps (1) and (2) - one or more of the steps optionally mentioned below can also be part of the method. All steps can each be used in their preferred embodiments mentioned below.
• dispersing medium in connection with pigments or effect pigments within the meaning of the present invention is known to the person skilled in the art and is defined, for example, in Römpp Chemie Lexikon, Lacke und Druckmaschine, Thieme Verlag, 1998, page 148. Accordingly, reference is made to DIN 55943 (November 1993) the division of agglomerates present in a pigment powder in a liquid medium, the dispersing medium, in to understand smaller particles and their simultaneous wetting by the dispersing medium.
• pigment paste is also known to the person skilled in the art and is defined, for example, in Römpp Lexikon, Lacke und Druckmaschine, Thieme Verlag, 1998, page 452: Pigment pastes are preparations of pigment mixtures in carrier materials such as polymers in which the pigments are present in a higher concentration than the later application.
• An effect pigment paste accordingly represents a pigment paste which contains at least one effect pigment - namely at least one effect pigment (a) - as a pigment.
• the subsequent application of pigment pastes is usually in the production of coating materials such as basecoats.
• a pigment paste such as an effect pigment paste is thus to be distinguished from a coating agent such as a basecoat in that it merely represents a preliminary stage for the production of such a coating agent.
• a pigment paste as such cannot therefore itself be used as a coating agent.
• the relative weight ratio of pigments to polymers is usually greater than in the coating compositions, for the production of which the paste is ultimately used.
• the pigment paste also contains liquid diluents such as water and / or organic solvents that function as the liquid medium (c). Different additives such as wetting agents and / or thickeners can also be used in a pigment paste.
• effect pigment paste and “effect pigment dispersion” are interchangeable here.
• vibration This is understood to mean a device which is capable of “shaking”, that is, for dispersing the mixture obtained after step (1) within step (2) of the method according to the invention while obtaining the effect pigment paste by means of shaking.
• the terms “shaking” and “shaking” are interchangeable and are clearly differentiated from the term “stirring”.
• stirrer No other aids that are required when using a stirrer, such as stirring sticks, stirring sticks or stirring blades.
• the method according to the invention is a method for producing an effect pigment paste.
• the effect pigment paste obtained after carrying out step (2) of the process according to the invention is free from grinding media.
• Grinding media for the purposes of the present invention are conventional grinding media known to the person skilled in the art which have a solid aggregate state, still have this after production of the respective pigment paste and do not change their shape, in particular their plastic shape, 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.
• the process according to the invention is preferably carried out entirely without the use of grinding media.
• grinding media can be added to the mixture obtained after step (1) of the process according to the invention or while step (1) is being carried out and step (2) can be carried out using this grinding media.
• the grinding media used are characterized in that they are in a solid state of aggregation at the beginning of step (2), but completely change into a liquid state of aggregation in the course of step (2) and then become part of the liquid medium ( c) or are themselves comminuted in the course of performing step (2) and then dispersed in the liquid medium (c) so that the effect pigment paste obtained after performing step (2) is free of grinding media.
• the grinding media used in this case are preferably selected from the group consisting of frozen water, frozen organic solvents and grinding media made from organic polymers and mixtures thereof.
• the method according to the invention preferably does not include a step which includes stirring.
• the process according to the invention for producing the effect pigment pastes has otherwise no special features in terms of its method, but can be carried out by mixing at least the above-described essential constituents (a), (b) and (c) with one another and homogenizing the resulting mixture.
• Step (1) of the process according to the invention provides for the production of a mixture comprising at least one effect pigment (a) and at least one polymer (b) in a liquid medium (c).
• the order in which the individual components are added is arbitrary, in particular if an aluminum effect pigment is used as the effect pigment (a). If a metal oxide-mica pigment is used as the effect pigment (a), all components except for the effect pigment (a) are preferably initially introduced and this is then added last to the resulting mixture.
• Step (2) Step (1) of the process according to the invention provides for the mixture obtained after performing step (1) to be dispersed while maintaining the
• step (2) is carried out using a vibrator and the effect pigment paste obtained after the implementation of step (2) has been completed is free of grinding media.
• vibrators are suitable as vibrators which can be used in step (2) of the method according to the invention.
• Examples of such vibrators are, for example, devices from Fast & Fluid such as the SK550 device or the SK550 1.1 device from the Skandex series.
• the companies Collomix and Corob also offer suitable vibrators.
• Step (2) is preferably carried out in a container which has a filling size in a range from 0.2 to 40 liters.
• step (2) is in one closed container.
• the container preferably used in step (2) is preferably filled in such a way that the degree of filling of the container is in a range from 15 to 95%.
• vessels and / or packs of any kind are suitable as containers. Single-use packs or reusable packs can be used.
• the mixture obtained after step (1) of the process according to the invention is preferably filled into a plastic bag and the dispersion is carried out in the plastic bag in accordance with step (2).
• the degree of filling is preferably in a range from 15 to 80%.
• step (2) depends on the amount of effect pigment paste to be produced. In principle, however, the time taken to carry out step (2) of the method according to the invention is preferably a maximum of 20 minutes, particularly preferably a maximum of 18 minutes, most preferably a maximum of 16 minutes. Preferably step (2) is carried out over a period of 1 to 15 minutes.
• the temperature increase found when performing step (2) of the process according to the invention is preferably in a range from 0 to 40.degree. C., preferably from 0.1 to 30.degree.
• Step (2) of the method according to the invention is preferably carried out by shaking at a frequency in a range from 6 to 20 Hz, particularly preferably from 8 to 18 Hz, very particularly preferably from 10 to 16 Hz.
• Step (2) of the method according to the invention is preferably carried out by shaking at an amplitude in a range from 1.0 to 8.0 cm, particularly preferably from 1.2 to 7.0 cm, very particularly preferably from 1.4 to 6.5 cm carried out.
• Step (2) of the method according to the invention is preferably carried out by shaking at an acceleration in a range from> 1 G to 26 G, particularly preferably from 2 to 23 G, in particular from 4 to 19 G. Effect pigment paste
• the solids content of the effect pigment paste prepared according to the invention is preferably in a range from 15 to 65% by weight, particularly preferably from 17.5 to 60% by weight, very particularly preferably from 20 to 55% by weight, in particular from 22.5 to 50% by weight, most preferably from 25 to 45% by weight, based in each case on the total weight of the effect pigment paste.
• the solids content i.e. the non-volatile content, is determined according to the method described below.
• the proportions in% by weight of all components (a), (b) and (c) contained in the effect pigment paste according to the invention as well as further components which may be additionally present add up to 100% by weight, based on the total weight of the effect pigment paste - effect pigment ( a)
• the effect pigment paste produced according to the invention contains at least one 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.
• effect pigments are preferably those pigments which give an optical effect or give a color and an optical effect, in particular an optical effect.
• optical effect and Coloring pigment “ optical effect pigment ”and“ effect pigment ”are therefore preferably interchangeable.
• Preferred effect pigments are, for example, flake-form metallic effect pigments such as flake-form aluminum pigments, gold bronzes, fire-colored bronzes and / or iron oxide-aluminum pigments, pearlescent pigments such as fish silver, basic lead carbonate, bismuth oxychloride and / or metal oxide, flaky pigments, or other flaky metal oxide / mica pigments such as graphite and / or graphite flaky pigments (Mica) Iron oxide, multi-layer effect pigments from PVD films and / or liquid crystal polymer pigments.
• flake-form effect pigments, in particular flake-form aluminum pigments and metal oxide mica pigments are contained in the pigment paste.
• the effect pigment paste according to the invention therefore preferably contains, as at least one effect pigment (a), at least one metallic effect pigment such as at least one preferably flaky aluminum effect pigment and / or at least one metal oxide-mica pigment.
• the effect pigment (a) used is preferably in the form of a powder.
• the effect pigment paste produced according to the invention can optionally contain further pigments, in particular color pigments and / or fillers, which differ from the at least one effect pigment (a).
• the effect pigment paste produced according to the invention preferably does not contain any further pigment such as a colored pigment and also no filler.
• the effect pigment paste produced according to the invention preferably contains a proportion of effect pigment (a) of at least 5% by weight, particularly preferably at least 7% by weight, very particularly preferably at least 10% by weight, in particular at least 13% by weight , most preferably of at least 15% by weight, based in each case on the total weight of the effect pigment paste.
• the effect pigment paste produced according to the invention preferably contains a proportion of effect pigment (a) in a range from 5 to 85% by weight, particularly preferably from 7 to 80% by weight, very particularly preferably from 10 to 75% by weight, in particular from 13 to 70% by weight, most preferably from 15 to 65% by weight or from 15 to 60% by weight, based in each case on the total weight of the effect pigment paste.
• the polymer (b) present in the effect pigment paste prepared according to the invention is used as a pigment paste binder (paste binder).
• the term “binder” preferably refers to the non-volatile components of a composition responsible for film formation, such as the effect pigment paste or the effect pigment paste according to the invention with the exception of the pigments contained therein, such as the at least one effect pigment (a) and any other pigments and / or fillers present.
• the non-volatile content can be determined according to the method described below.
• a binder constituent is accordingly a specific component which contributes to the binder content of a composition such as the effect pigment paste produced according to the invention.
• the polymer (b) is preferably used in the form of an aqueous or solvent-containing dispersion for producing the effect pigment paste.
• SCS polymers So-called seed-core-shell polymers (SCS polymers) can be used as polymer (b). Such polymers are known, for example, from WO 2016/116299 A1.
• At least one polymer selected from the group consisting of polyurethanes, polyureas, polyesters, poly (meth) acrylates and / or copolymers of the polymers mentioned, in particular polyurethane-poly (meth) acrylates and / or polyurethane Polyureas are used.
• 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 the European patent application EP 0 634 431 A1, page 3, line 38 to page 8, line 9, and the international one
• Patent application WO 92/15405 page 2, line 35 to page 10, line 32.
• polyesters are described, for example, in DE 4009858 A1 in 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.
• Preferred polyurethane-poly (meth) acrylate copolymers ((meth) acrylated polyurethanes) and their production 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.
• Preferred polyurethane-polyurea copolymers are polyurethane-polyurea particles, the polyurethane-polyurea particles, in each case in converted form, at least one polyurethane prepolymer containing isocyanate groups and containing anionic groups and / or groups which can be converted into anionic groups and at least one polyamine containing two contain primary amino groups and one or two secondary amino groups.
• Such copolymers are preferably used in the form of an aqueous dispersion.
• Such polymers can in principle be produced by polyaddition, known per se, of, for example, polyisocyanates with polyols and polyamines.
• the polymers (b) can each have functional groups, in particular selected from the group consisting of OH groups, COOH groups and amino groups, in particular OH groups. Hydroxy-functional polyurethane-poly (meth) acrylate copolymers and hydroxy-functional polyesters and hydroxy-functional polyurethane-polyurea copolymers are particularly preferred.
• the effect pigment paste produced according to the invention preferably contains a proportion of polymer (b) in a range from 1.0 to 25% by weight, particularly preferably from 1.5 to 20% by weight, very particularly preferably from 2.0 to 17, 5% by weight, in particular from 2.5 to 15% by weight, most preferably from 4.0 to 12.5% by weight, in each case based on the total weight of the effect pigment paste.
• the determination or stipulation of the proportion of the polymer (b) in the effect pigment paste can be carried out by determining the solids content (also called non-volatile proportion, solids content or solids proportion) of a dispersion containing the polymer (b), which is used to make the effect pigment paste .
• the relative weight ratio of the at least one is
• Effect pigments (a) to the polymer (b) in the effect pigment paste at at least 1: 1 or at least 1.2: 1 or at least 1.5: 1 or in each case higher, particularly preferably at least 2.0: 1 or higher, very particularly preferably at least 2.5: 1 or higher, in particular at least 3.0: 1 or higher.
• the relative weight ratio of the at least one is
• Effect pigments (a) for the polymer (b) in the effect pigment paste in a range from 10: 1 to 1: 1 or from 8: 1 to 1: 1, particularly preferably in a range from 10: 1 to 1.2: 1 or from 10: 1 to 1.5: 1 or in a range from 8: 1 to 1.2: 1 or from 8: 1 to 1.5: 1.
• Step (1) of the process 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).
• a liquid medium (c) in step (1) at least one diluent is preferably provided, which consequently functions as component (c).
• the effect pigment paste produced according to the invention therefore preferably comprises at least one such diluent. Water and / or at least one organic solvent can be used as the diluent.
• the effect pigment paste produced according to the invention can be aqueous. It is preferably a system that contains water as the main component, preferably in an amount of at least 20% by weight, and organic solvents in smaller proportions, preferably in an amount of ⁇ 20% by weight, as the main component based on the total weight of the effect pigment paste.
• the effect pigment paste then preferably contains a proportion of water of at least 20% by weight, particularly preferably at least 25% by weight, very particularly preferably at least 30% by weight, in particular at least 35% by weight, most preferably of at least 40% by weight, based in each case on the total weight of the effect pigment paste.
• the effect pigment paste then preferably contains a proportion of water which is in a range from 20 to 75% by weight, particularly preferably in a range from 25 to 70% by weight, very particularly preferably in a range from 30 to 65% by weight. % or up to 60% by weight or up to 57.5% by weight, based in each case on the total weight of the effect pigment paste.
• the effect pigment paste preferably contains a proportion of organic solvents which is in a range of ⁇ 20% by weight, particularly preferably in a range from 0 to ⁇ 20% by weight, very particularly preferably in a range of 0.5 up to 20% by weight or up to 17.5% by weight or up to 15% by weight, based in each case on the total weight of the effect pigment paste.
• effect pigment paste produced according to the invention can be loose-based. It is preferably a system that contains organic solvents as the main component, preferably in an amount of at least 20% by weight, and water in smaller proportions, preferably in an amount of ⁇ 20% by weight, in each case based on the total weight of the effect pigment paste.
• the effect pigment paste then preferably contains a proportion of organic solvents of at least 20% by weight, particularly preferably at least 25% by weight, very particularly preferably at least 30% by weight, in particular at least 35% by weight, most of all preferably of at least 40% by weight, based in each case on the total weight of the effect pigment paste.
• the effect pigment paste then preferably contains a proportion of organic solvents which is in a range from 20 to 75% by weight, particularly preferably in a range from 25 to 70% by weight, very particularly preferably in a range from 30 to 65% by weight. -% or up to 60% by weight or up to 57.5% by weight, based in each case on the total weight of the effect pigment paste.
• the effect pigment paste preferably contains a proportion of water which is in a range from ⁇ 20% by weight, particularly preferably in a range from 0 to ⁇ 20% by weight, very particularly preferably in a range from 0.5 to 20% by weight or up to 17.5% by weight or up to 15% by weight, based in each case on the total weight of the effect pigment paste.
• effect pigment pastes which contain aluminum effect pigments as effect pigment (a).
• the effect pigment pastes according to the invention can, however, also be completely or almost completely free of organic solvents, in particular if metal oxide mica pigments (mica) are used as effect pigment (a).
• organic solvent is known to those skilled in the art. This term is defined, for example, in Council Directive 1999/13 / EC of March 11, 1999 (Article ⁇ 2, Item 18.) (referred to 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.
• the effect pigment paste produced according to the invention can contain further optional constituents or optional components:
• the effect pigment paste can additionally contain typical color pigments which are different from the effect pigment (a).
• color pigment A person skilled in the art is familiar with the concept of color pigments.
• the terms "coloring pigment” and "color pigment” are interchangeable.
• Inorganic and / or organic pigments can be used as color pigment.
• the color pigment is preferably an inorganic color pigment.
• White pigments, colored pigments and / or black pigments are used as particularly preferred color pigments. Examples of white pigments are titanium dioxide, zinc white, zinc sulfide and lithopone. Examples of black pigments are carbon black, iron-manganese black and spinel black.
• colored pigments are chromium oxide, chromium oxide hydrate green, cobalt green, ultramarine green, cobalt blue, ultramarine blue, manganese blue, ultramarine violet, cobalt and manganese violet, iron oxide red, cadmium sulfoselenide, molybdate red and ultramarine red, iron oxide brown, chrome brown, nickel yellow oxide yellow and corundum yellow Cadmium sulfide, cadmium zinc sulfide, chrome yellow and bismuth vanadate.
• the proportion of color pigments is preferably in the range from 1.0 to 40.0% by weight, preferably 2.0 to 35.0% by weight, particularly preferably 5.0 to 30.0% by weight, in each case based on on the total weight of the aqueous effect pigment paste.
• the effect pigment paste produced according to the invention preferably contains the at least one effect pigment (a) as the only pigment, ie it preferably contains no additional color pigments.
• the effect pigment paste preferably also does not contain any fillers.
• the effect pigment paste can optionally also contain at least one thickener (also referred to as a thickener).
• thickeners examples include inorganic thickeners, for example metal silicates such as sheet silicates, and organic thickeners, for example poly (meth) acrylic acid thickeners and / or (meth) acrylic acid- (meth) acrylate copolymer thickeners, polyurethane thickeners and polymeric waxes.
• the metal silicate is preferably selected from the group of smectites.
• the smectites are particularly preferably selected from the group of montmorillonites and flectorites.
• the montmorillonite and flectorite are from the group consisting of aluminum-magnesium-silicates as well Sodium-magnesium and sodium-magnesium-fluorine-lithium phyllosilicates.
• inorganic phyllosilicates are sold under the Laponite® brand, for example.
• Thickeners based on poly (meth) acrylic acid 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” (ASE), and hydrophobically modified variants of them, the “Hydrophically modified Alkali Swellable Emulsions” (HASE).
• these thickeners are anionic.
• Corresponding products such as Rheovis® AS 1130 are commercially available thickeners based on polyurethanes (e.g. polyurethane associative
• Thickeners are optionally crosslinked and / or neutralized with a suitable base.
• Corresponding products such as Rheovis® PU 1250 are commercially available.
• Polymeric waxes that are suitable, for example, are optionally modified polymeric waxes based on ethylene-vinyl acetate copolymers.
• a corresponding product is commercially available, for example, under the name Aquatix® 8421.
• the at least one thickener is preferably present in the effect pigment paste prepared according to the invention in an amount of at most 10% by weight, particularly preferably at most 7.5% by weight, very particularly preferably at most 5% by weight, in particular at most 3% by weight .-%, most preferably of at most 2 wt .-%, each based on the
• the effect pigment paste produced according to the invention can, depending on the desired application, contain one or more commonly used additives as further component (s).
• the effect pigment paste can contain a certain proportion of at least one organic solvent.
• the effect pigment paste can contain at least one additive selected from the group consisting of reactive diluents, light stabilizers, antioxidants, deaerating agents, emulsifiers, slip additives, polymerization inhibitors, initiators for radical polymerizations, adhesion promoters,
• Their content, based on the total weight of the effect pigment paste, is preferably 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 %, very particularly preferably 0.1 to 7.5% by weight, in particular 0.1 to 5.0% by weight and most preferably 0.1 to 2.5% by weight.
• An effect pigment paste can be produced by means of the method according to the invention.
• the present invention also provides an effect pigment paste which can be produced by means of the method according to the invention, the effect pigment paste containing an amount of effect pigment (a) of at least 20% by weight, based on the total weight of the effect pigment paste, in particular if 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 cannot be successfully produced using conventional processes that involve a stirring process, as the following experimental data show (see experimental part: Comparative effect pigment paste VEP2 vs. effect pigment paste EP3).
• the vibrator used in step (2) of the process according to the invention is suitable for dispersing effect pigments for producing an effect pigment paste.
• the present invention therefore also relates to the use of a vibrator for dispersing effect pigments for producing an effect pigment paste, the effect pigment paste obtained after the end of the dispersion being free of grinding media.
• the Effect pigment paste that which is produced by means of the method according to the invention.
• the non-volatile content (the solids content or solids content) is determined in accordance with DIN EN ISO 3251 (date: June 2008). 1 g sample is weighed into a previously dried aluminum dish and dried for 60 minutes at 125 ° C. in a drying cabinet, cooled in a desiccator and then reweighed. The residue based on the total amount of the sample used corresponds to the non-volatile content
• the number-average molecular weight (M n ) is determined by means of gel permeation chromatography (GPC). The determination method is based on DIN 55672-1 (date: August 2007). In addition to the number average molecular weight, this method can also be used to determine the weight average molecular weight (M w ) and the polydispersity (ratio of weight average molecular weight (M w ) to number average molecular weight (M n )). Tetrahydrofuran is used as the eluent. The determination is carried out against polystyrene standards. The column material consists of styrene-divinylbenzene copolymers.
• the OFI number is determined based on R.-P. Krüger, R. Gnauck and R. Algeier, Plaste und Kautschuk, 20, 274 (1982) and is using acetic anhydride in the presence of 4-dimethylaminopyridine as a catalyst in a tetrahydrofuran (TFIF) / dimethylformamide (DMF) solution at room temperature (18 to 23 ° C), whereby the remaining excess of acetic anhydride is completely hydrolyzed after acetylation and the acetic acid is back-titrated potentiometrically with an alcoholic potassium hydroxide solution. The acetylation time of 60 minutes is sufficient to guarantee complete conversion. 4. Assessment of the occurrence of specks
• the effect pigment pastes are examined in accordance with the following general rule:
• the respective paste is applied to a glass panel with dimensions 9 using a 100 ⁇ m box doctor blade (when using aluminum effect pigments) or a 50 ⁇ m box blade (when using mica effect pigments) cm x 15 cm applied.
• After a drying time of 10 minutes at 80 ° C. in a convection oven, the film formed in this way is visually assessed for the occurrence of specks by holding it against a light source in order not to misinterpret any air inclusions as specks.
• Grade 1 corresponds to the specification “OK” (OK).
• Polyester 1 produced according to DE 4009858 A1, example D (column 16, line 37 to column 6, line 60)
• Alu Stapa Hydrolux® 2154 Commercially available aluminum effect pigment, available from Altana-Eckart, with a solids content of 65% by weight
• Mearlin® Exterior Super Red 439Z Commercially available mica effect pigment, available from Merck
• Mearlin® Exterior Fine Violet 539 V Commercially available mica effect pigment, available from Merck
• Comparative effect pigment paste VEP1 A comparative effect pigment paste VEP1 made from 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 butylglycol is produced as follows, with 4000 g of each of the aforementioned components being used: Butylglycol is placed in a container submitted, Alu Stapa Hydrolux® 2154 added in portions with stirring and the resulting mixture stirred for a period of 15 minutes. The stirring speed is set so that a vortex is clearly visible. Then the polyester component is stirred with stirring added and the resulting mixture stirred for a period of 15 minutes. The processing time is therefore a total of 30 minutes. After the stirring process had been completed, the container had to be cleaned due to the formation of dust and deposits of pigment and polyester residues on the edge of the container. No specks could be observed (OK).
• An effect pigment paste EP1 according to the invention from 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 butylglycol is produced as follows, 200 g of each of the aforementioned components being used:
• the three aforementioned components are put together in any order in a container with a capacity of 1 L (disposable container) and shaken without further premixing for a period of 12 minutes.
• the device SK550 from Fast & Fluid is used as the vibrator.
• the frequency during shaking is 12 flz.
• the processing time is therefore only 6 minutes. Cleaning was not necessary because no dust formation and no settling of pigment and polyester residues could be observed. No specks could be observed (OK).
• An effect pigment paste EP2 according to the invention from 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 butylglycol is produced as follows, 50 g of each of the aforementioned components being used:
• the three aforementioned components are put together in any order in a container with a capacity of 0.25 L (disposable container) and shaken without further premixing for a period of 3 minutes.
• the device SK550 from Fast & Fluid is used as the vibrator.
• the frequency during shaking is 12 Hz.
• the processing time is therefore only 3 minutes in total. Cleaning was not necessary because there was no dust formation and no Settling of pigment and polyester residues could be observed. No specks could be observed (OK).
• Effect pigment paste EP3 An effect pigment paste EP3 according to the invention composed of 50% by weight of polyester 1, 45% by weight of Alu Stapa Hydrolux® 2154 and 5% by weight of butyl glycol is produced as follows, with 600 g of butyl glycol, 6000 g of polyester 1 and 5400 g Alu Stapa Hydrolux® 2154 have been used: The three above-mentioned components are combined in any order in a container with a capacity of 18 L (disposable container) and shaken without further premixing for a period of 12 minutes. The device SK550 from Fast & Fluid is used as the vibrator. The frequency during shaking is 12 Hz. The processing time is therefore only 12 minutes in total. Cleaning was not necessary because no dust formation and no settling of pigment and polyester residues could be observed. No specks could be observed (OK).
• Polyester 1 45% by weight of Alu Stapa Hydrolux® 2154 and 5% by weight of butyl glycol, with 600 g of butyl glycol, 6000 g of polyester 1 and 5400 g of Alu Stapa Hydrolux® 2154 being used, and the information under 2.1 in connection with VEP1 described manufacturing method has been used. However, the resulting mixture had such a high viscosity that stirring was not possible and therefore VEP2 could not be produced under these conditions.
• An effect pigment paste EP4 according to the invention composed of 33.33 parts by weight of polyester 1, 33.33 parts by weight of Alu Stapa Hydrolux® 2154 and 33.33
• butyl glycol Parts by weight of butyl glycol is prepared as follows, with 4000 g of each of the aforementioned components being used: The three aforementioned components are put together in any order in a plastic bag as an example of a reusable container, this is closed and the mixture in the bag is shaken without further premixing for a period of 12 minutes.
• the device SK550 from Fast & Fluid is used as the vibrator. The frequency during shaking is 12 flz. The processing time is therefore only 12 minutes. Cleaning was not necessary because no dust formation and no settling of pigment and polyester residues could be observed. No specks could be observed (OK).
• a comparative effect pigment paste VEP3 from 75 parts by weight of a mixed lacquer ML1 and 25 parts by weight of Mearlin® Exterior Super Red 439Z is produced as follows, with 9000 g of ML1 and 3000 g of Mearlin® Exterior Super Red 439Z being used:
• ML1 is produced by mixing the following components with one another: Rheovis® AS 1130 (commercially available polymer as thickener), Dispex® Ultra FA 4437 (commercially available additive), 2,4,7,9-tetramethyl-5-decynediol , 52% in butyl glycol (available from BASF SE) and deionized water as well as 10% dimethylethanolamine in water.
• ML1 is placed in a container with a capacity of 18 L (disposable container) and the mica effect pigment is slowly added using a dissolver, making sure that no pigment agglomerates form on the edge or on the dissolver. This process takes about 20 minutes. The resulting mixture is dissolverted for a further 20 minutes after the addition of pigment has ended. The processing time is therefore a total of 40 minutes. Cleaning was necessary as dust formation and the settling of pigment and polyester residues could be observed. Mica and binder particles adhered to the stirrer and to the walls of the vessel found.
• An effect pigment paste EP3 from 75 parts by weight of a mixed lacquer ML1 and 25 parts by weight of Mearlin® Exterior Super Red 439Z is produced as follows, with 9000 g of ML1 and 3000 g of Mearlin® Exterior Super Red 439Z being used:
• ML1 is produced as described under point 3.1.
• the two aforementioned components are put together in any order in a container with a capacity of 18 L (disposable container) and shaken without further premixing for a period of 12 minutes.
• the device SK550 from Fast & Fluid is used as the vibrator.
• the frequency during shaking is 12 flz.
• the processing time is therefore only 12 minutes. Cleaning was not necessary because no dust formation and no settling of pigment and polyester residues could be observed. No specks could be observed (OK).

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