Classifications

• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
  • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
  • C09B67/006—Preparation of organic pigments
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
  • B01F25/10—Mixing by creating a vortex flow, e.g. by tangential introduction of flow components
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J4/00—Feed or outlet devices; Feed or outlet control devices
  • B01J4/001—Feed or outlet devices as such, e.g. feeding tubes
  • B01J4/002—Nozzle-type elements
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F23/00—Mixing according to the phases to be mixed, e.g. dispersing or emulsifying
  • B01F23/50—Mixing liquids with solids
  • B01F23/51—Methods thereof
  • B01F23/511—Methods thereof characterised by the composition of the liquids or solids
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
  • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
  • B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
  • B01F25/23—Mixing by intersecting jets
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J14/00—Chemical processes in general for reacting liquids with liquids; Apparatus specially adapted therefor
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J19/24—Stationary reactors without moving elements inside
  • B01J19/2405—Stationary reactors without moving elements inside provoking a turbulent flow of the reactants, such as in cyclones, or having a high Reynolds-number
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
  • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
  • B01J19/26—Nozzle-type reactors, i.e. the distribution of the initial reactants within the reactor is effected by their introduction or injection through nozzles
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
  • C09B41/00—Special methods of performing the coupling reaction
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
  • C09B41/00—Special methods of performing the coupling reaction
  • C09B41/006—Special methods of performing the coupling reaction characterised by process features
  • C09B41/008—Special methods of performing the coupling reaction characterised by process features using mechanical or physical means, e.g. using ultra-sound, milling during coupling or microreactors
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
  • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
  • C09B67/0001—Post-treatment of organic pigments or dyes
  • C09B67/0017—Influencing the physical properties by treatment with an acid, H2SO4
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
  • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
  • C09B67/0071—Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
  • C09B67/0084—Dispersions of dyes
  • C09B67/0091—Process features in the making of dispersions, e.g. ultrasonics
• • C—CHEMISTRY; METALLURGY
  • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
  • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
  • C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
  • C09B67/0096—Purification; Precipitation; Filtration
• • 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
  • C09D11/00—Inks
  • C09D11/30—Inkjet printing inks
  • C09D11/32—Inkjet printing inks characterised by colouring agents
  • C09D11/322—Pigment inks

Definitions

• the present invention relates to a method for carrying out chemical and physical processes, in particular for the production of organic pigments, and to a swirl chamber reactor suitable therefor.
• Organic pigments have become of great industrial importance for coloring high molecular weight organic materials such as paints, plastics, printing inks or inks.
• quality requirements regarding coloristic and rheological properties such as color strength, color purity, transparency, dispersibility and viscosity are correspondingly high.
• special process conditions in pigment synthesis or subsequent conditioning such as grinding and finishing, are required to achieve a specific particle shape, size and distribution, which are known to the person skilled in the art.
• One goal of the pigment manufacturers is to make the process steps for pigment production as economical as possible, i.e. perform different process steps in the same equipment.
• One approach to achieving this goal was to use a microjet reactor for the production of azo colorants (EP-A-1 195411), for the fine distribution of organic pigments (EP-A-1 195413) and for the production of liquid pigment preparations (EP-A-1 195414).
• a gas phase is maintained in the reactor space and the educts are sprayed through a high-pressure nozzle onto a common collision point.
• Disadvantages of this method are the difficult adjustment of the educt jets to a common collision point, problems in carrying out the experiment when the pulse currents are unequal, and the product separation from the gas phase.
• medium A can pass into the nozzle of medium B, that is to say possibly a component in front of the corresponding nozzle fails and thus clogs it up and causes the microjet reactor to fail completely.
• the present invention was therefore based on the object of developing a universally applicable and technically reliable process for carrying out chemical and physical processes, in particular for the production of organic pigments, in which the products, in particular organic pigments, are produced in high quality.
• the invention relates to a method for carrying out chemical and physical processes, in particular for the production of organic pigments or pigment preparations, characterized in that two or more liquids or suspensions are passed through two or more nozzles which are not coaxially aligned with one another with a pressure between 1 and 1000 bar, preferably 2 to 500 bar, in particular 5 to 300 bar, and a volume flow between 5 and 500 l / h, preferably between 25 and 400 l / h and particularly preferably between 50 and 300 l / h, without using a carrier gas stream injected into a swirl chamber, thereby causing a turbulent mixing of the liquid phase with a change in substance and, after the change in substance, the liquid phase is continuously discharged from the swirl chamber through an outlet opening.
• the two or more, expediently 2 to 7, nozzles open into the swirl chamber and are distributed over its inner circumference in such a way that they are not aligned coaxially.
• the angle of entry of the axis of the nozzles can be between 90 ° (orthogonal injection) and 0 ° (tangential injection). It is also advantageous if the axes of the nozzles are at an angle between 0 ° and 90 °, based on the cross-sectional area of the swirl chamber against the outlet opening, which is expediently located at the head of the swirl chamber.
• the geometry of the swirl chamber can be of any type, but advantageous are shapes which allow little or no dead volume, such as a ball or cylinder, the bottom of which is flat or convexly curved outwards.
• the vortex chamber reactor can also be connected to a residence, e.g. a flow tube can be connected in order to maintain the mixture state generated in the vortex chamber reactor after the reaction mixture has left the vortex chamber for longer periods and to exclude back-mixing.
• the flow tube is preferably a double-walled one in order to be able to control endo- and exothermic chemical reactions or physical processes in a controlled manner.
• the reactor space of the apparatus according to the invention is virtually completely filled with the liquid phase during operation.
• the educts step into one Vortex chamber in which there are highly turbulent flow conditions.
• the invention also relates to a swirl chamber reactor (FIG. 1) for carrying out the processes described above, characterized in that two or more nozzles (3, 7), each with an associated pump and feed line (4, 6), for injecting a liquid medium each In a swirl chamber (2) enclosed by a housing (1) there are provided that the nozzles are not aligned coaxially with one another and that an outlet opening (5) is provided for removing the resulting products from the swirl chamber (2).
• a temperature measuring device (8) is brought up to the swirl chamber.
• Q 1 , Q 2 and Q 3 can be the same or different and N, NR 2 , CO, N-CO,
• R 1 and n are as defined above and R 20 is hydrogen, methyl or ethyl; and pyrazolones of the general formula (V),
• azo dyes 4- [5-hydroxy-3-methyl-pyrazol-1-yl] -benzenesulfonic acid, 2-amino-naphthalene-1,5-disulfonic acid, 5-methoxy-2-methyl-4 [3-oxo-butyrylamino] -benzenesulfonic acid, 2-methoxy-5-methyl-4- [3-oxo-butyrylamino] -benzenesulfonic acid, 4-acetylamino-2-amino-benzenesulfonic acid, 4- [4-chloro-6- ( 3-suIfo-phenylamino) - [1, 3,5] -triazin-2-yl-amino] -5-hydroxy-naphthalene-2,7-disulfonic acid, 4-acetylamino-5-hydroxy-naphthalene-2,7- disulfonic acid, 4-amino-5-hydroxy-naphthalene
• Suitable surfactants are anionic or anionic, cationic or cationic and nonionic substances or mixtures of these agents. Examples of surfactants, pigmentary and non-pigmentary dispersants which can be used for the process according to the invention are given in EP-A-1 195 411.
• the reactants can be injected as a mixture or separately.
• the azo colorant is preferably isolated directly after the reaction. However, it is also possible to carry out a post-treatment (finish) with water and / or an organic solvent, for example at temperatures from 20 to 250 ° C., if appropriate also with the addition of auxiliaries.
• the temperatures of the pigment solution supplied and the precipitation medium are expediently in the range from -50 to 250 ° C., preferably between 0 and 190 ° C., particularly between 0 to 170 ° C.
• the energy required for the heating can be supplied before it emerges from the nozzles of the pigment solution and / or the precipitation medium, for example in the supply lines, or via the thermostattable housing.
• Coarse-crystalline raw pigments include, for example, those from the group of the perylenes, perinones, quinacridones, for example unsubstituted quinacridone of the beta or gamma phase, or also crude quinacridone mixed crystal pigments, quinacridone quinones, anthraquinones, anthanthrones, benzimidazolones, disazo phthalocyanine pigments, and phthalates, such as indazo condensation pigments, such as indazo condensation pigments, such as indazo condensation pigments, and phthalone indigo phthalone pigments, such as disazo condensation pigments, phasone, dese phthalone digestion pigments such as indazo condensation pigments CuPc, unchlorinated CuPc of the alpha or beta phase, metal-free phthalocyanines or phthalocyanines with other metal atoms such as, for example, aluminum or cobalt, dioxazines, for example triphendioxazines,
• Suitable solvents are all liquids such as organic solvents, acids and alkalis, and mixtures thereof, optionally also with the addition of water, of which at most 40 times the amount by weight, preferably at most 25 times the amount by weight, in particular at most 15 times Amount of weight, based on the weight of the raw pigment to be dissolved, must be used in order to achieve a complete solution of the raw pigment. Solutions which have a pigment content of 2.5 to 40% by weight, preferably 5 to 20% by weight, based on the total weight of the solution, are therefore economically advantageous.
• glycerol such as polyethylene glycols or polypropylene glycols; Ethers such as methyl isobutyl ether, tetrahydrofuran or dimethoxyethane; Glycol ethers, such as monomethyl or monoethyl ether of ethylene or propylene glycol, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, butyl glycols or methoxybutanol; Ketones such as acetone, diethyl ketone, methyl isobutyl ketone, methyl ethyl ketone or cyclohexanone; aliphatic acid amides such as formamide, dimethylformamide, N-methylacetamide or N, N-dimethylacetamide; Urea derivatives such as tetramethyl urea; or cyclic carboxamides, such as N-methylpyrrolidone, valero or caprolactam; Esters,
• solvents are mixtures of organic, polar solvents, for example aliphatic acid amides, such as formamide, dimethylformamide or N, N-dimethylacetamide; Urea derivatives such as tetramethyl urea; cyclic carboxamides, such as N-methylpyrrolidone, valero- or caprolactam; Nitriles such as acetonitrile; aromatic solvents such as nitrobenzene, o-dichlorobenzene, benzoic acid or phenol; aromatic
• Heterocycles such as pyridine or quinoline; Hexamethylphosphoric acid triamide, 1, 3-dimethyl-2-imidazolidinone, dimethyl sulfoxide or sulfolane; or optionally mixtures of these solvents with alkalis, such as oxides or hydroxides of the alkali or alkaline earth metals, such as, for example, potassium hydroxide solution or sodium hydroxide solution.
• alkalis such as oxides or hydroxides of the alkali or alkaline earth metals, such as, for example, potassium hydroxide solution or sodium hydroxide solution.
• all liquids can be used as the precipitation medium which, when mixed with the pigment solution, reduce the solubility of the pigment to such an extent that precipitation is as quantitative as possible. Therefore water comes an aqueous-organic liquid or an organic liquid, with or without the addition of acids or bases.
• the precipitation medium is preferably water or an aqueous-organic liquid, if appropriate with the addition of acid, or a mixture of an organic liquid with an acid.
• organic liquids for the precipitation medium for example alcohols with 1 to 10 carbon atoms, such as methanol, ethanol, n-propanol, isopropanol, butanols, such as n-butanol, sec-butanol, tert-butanol, pentanols, such as n Pentanol, 2-methyl-2-butanol, hexanols, such as 2-methyl-2-pentanol, 3-methyl-3-pentanol, 2-methyl-2-hexanol, 3-ethyl-3-pentanol, octanols, such as 2 , 4,4-trimethyl-2-pentanol, cyclohexanol; or glycols, such as ethylene glycol, diethylene glycol, propylene glycol, dipropylene glycol, or glycerin; Polyglycols, such as polyethylene glycols or polypropylene glycols; Ether
• Urea derivatives such as tetramethyl urea; or cyclic carboxamides, such as N-methylpyrrolidone, valero- or caprolactam;
• Esters such as carboxylic acid -C 6 -alkyl esters, such as butyl formate, ethyl acetate or propyl propionate; or carboxylic acid CtC 6 glycol ester; or glycol ether acetates such as 1-methoxy-2-propyl acetate; or phthalic acid or benzoic acid C 1 -C 6 alkyl esters, such as ethyl benzoate; cyclic esters such as caprolactone; Nitriles such as acetonitrile or benzonitrile; aliphatic or aromatic hydrocarbons, such as cyclohexane or benzene; or by alkyl, alkoxy, nitro or halogen-substituted benzene, such as toluene, x
• customary auxiliaries such as, for example, surfactants, non-pigmentary and pigmentary dispersants, fillers, adjusting agents, resins, waxes, defoamers, anti-dust agents, extenders, colorants for shading, preservatives, drying retardants, additives for controlling the rheology, wetting agents, antioxidants, UV Absorbers, light stabilizers, or a combination thereof can be used.
• the total amount of auxiliaries added can be 0 to 40% by weight, preferably 1 to 30% by weight, in particular 2.5 to 25% by weight, based on the crude pigment.
• the pigment can be isolated directly after the precipitation, but it is also possible, if appropriate, to carry out an aftertreatment (finish) with water and / or an organic solvent, with or without intermediate insulation, for example at temperatures from 20 to 250 ° C., optionally with the addition of aids.
• Pigment preparations are dispersions of pigments in flocculation-stabilizing, liquid media.
• auxiliaries can also be present.
• the pigments are dispersed in the flocculation-stabilizing, liquid medium and completely enveloped by it.
• the flocculation-stabilizing, liquid media are similar or well compatible with the intended application medium.
• the pigments are contained in the pigment preparations in higher concentrations than in the later application medium.
• Pigment preparations serve as colorants for pigmenting high-molecular materials such as paints, emulsion paints, inks such as ink-jet inks, printing inks, plastics and printing inks for textile printing.
• Pigment preparations can usually be incorporated into the flocculation-stabilizing, liquid media with little distribution and mixing effort and without ecological problems and are characterized in many application media by excellent coloristic and rheological properties as well as by favorable flocculation and settling behavior.
• Fine pigment is normally used to make pigment preparations.
• the incorporation into the flocculation-stabilizing, liquid media takes place here by dispersion in roller mills, vibratory mills, Agitator ball mills with low and high energy density, mixers, roller mills or kneaders.
• the dispersing device used depends on the dispersibility of the pigment used, the flocculation-stabilizing liquid medium and the auxiliaries.
• Laboratory-scale products on a large industrial scale are often complex and can cause difficulties because, for example, the input of mechanical energy, the transfer of energy for effective grinding, the loss of energy due to the generation of heat and the necessary dissipation of heat from the apparatus geometries and sizes depend and thus also determine the economics of the process on an industrial scale.
• liquid pigment preparations with particularly advantageous rheological and coloristic properties can be produced with the aid of the swirl chamber reactor according to the invention.
• the procedure is such that a 10 to 80% by weight, preferably 20 to 60% by weight, in particular 30 to 50% by weight, suspension of a crude pigment, prepigment and / or pigment, based on the Total weight of the suspension, in a flocculation-stabilizing, liquid medium via 1, 2 or more nozzles is injected into the swirl chamber.
• the temperatures of the suspensions supplied are advantageously in the range from -50 to 250 ° C., preferably from 0 to 180 ° C., in particular between 0 and 100 ° C., in particular between 10 to 80 ° C. It is also possible to work under pressure above the boiling point of the flocculation-stabilizing liquid medium. If work is to be carried out at elevated temperature, the energy required for heating can be supplied to the suspension before it emerges from the nozzles, for example in the supply lines, or via the thermostattable housing.
• organic and inorganic pigments can be used for the process according to the invention, for example organic pigments such as perylene, perinone, quinacridone, quinacridonequinone, anthraquinone, anthanthrone, benzimidazolone, disazo condensation, azo, indanthrone, phthalocyanine , Triarylcarbonium, dioxazine.
• organic pigments such as perylene, perinone, quinacridone, quinacridonequinone, anthraquinone, anthanthrone, benzimidazolone, disazo condensation, azo, indanthrone, phthalocyanine , Triarylcarbonium, dioxazine.
• Coarse-crystalline raw pigments are understood to mean those raw pigments which are only suitable for pigmenting organic materials after the particles have been comminuted. In most cases, these are those with an average particle size D 50 of more than 1 ⁇ m. It is also possible to use finely divided, but strongly agglomerated and thus difficult to disperse prepigments or difficult to disperse pigments, or else mixtures of coarsely crystalline raw pigments, prepigments and pigments. Of course, it is also possible to convert easily dispersible pigments, prepigments or raw pigments into pigment preparations by the process according to the invention.
• the dispersing behavior of a pigment is its behavior when dispersing with regard to changing various criteria of the dispersion state (for example particle size, color strength, gloss) depending on various influencing variables (dispersing device, dispersing process, dispersing time, mill base composition).
• the color strength is mainly used to assess the dispersing behavior of pigments that are difficult to disperse. It increases with increasing quality of the dispersion state and with increasing particle fineness.
• the average particle diameter (D50) can therefore also be used to assess dispersibility.
• the test medium and the dispersion conditions are determined in advance depending on the area of application of the pigment.
• the dispersing effort (dispersing time) required to achieve a certain average particle size serves as a measure.
• the average particle size depends on the pigment used in each case.
• Prepigments that are difficult to disperse include, for example, dioxazine, phthalocyanine, anthanthrone, perylene and quinacridone prepigments.
• Azo, dioxazine, phthalocyanine, anthanthrone, perylene, quinacridone, diketopyrrolopyrrole, isoindolinone and isoindoline pigments are considered to be difficult to disperse pigments.
• a flocculation-stabilizing, liquid medium is understood to mean a medium which the reagglomeration of the dispersed pigment particles in the Prevents dispersion.
• the flocculation resistance is determined by the "rubout" test, in which the color strength difference or the color tone difference of the flocculated and deflocked sample is determined.
• a flocculation-stabilizing, liquid medium in the sense of the present invention brings about a color strength difference of less than 10%. The determination the color strength is in accordance with DIN 55986.
• Organic solvents of the flocculation-stabilizing, liquid medium for the purposes of the present invention are, if appropriate, water-miscible, alcohols, glycols and glycol ethers, such as ethanol, ethylene glycol, propylene glycol, butylene glycol, diethylene glycol, triethylene glycol, ethylene glycol dimethyl ether or glycerol; Polyglycols, such as polyethylene glycols or polypropylene glycols; polyols; polyether polyols; aromatic solvents such as white spirit; Ketones such as methyl ethyl ketone; or esters, such as butyl esters; into consideration.
• alcohols, glycols and glycol ethers such as ethanol, ethylene glycol, propylene glycol, butylene glycol, diethylene glycol, triethylene glycol, ethylene glycol dimethyl ether or glycerol
• Polyglycols such as polyethylene glycols or polypropylene glycols
• water as such monohydric alcohols, ketones or their mixtures with water without a carrier material are not flocculation-stabilizing, liquid media in the sense of the present invention.
• the moist raw or prepigments can be used. This eliminates the need for expensive drying. Because the same fine distribution device is used for all areas of application, there is no longer any need to maintain different types of fine distribution devices.
• urea and melamine-formaldehyde resins in particular urea and melamine-formaldehyde resins, alkyd resins, acrylic resins, phenoplasts, polycarbonates, polyolefins, such as polystyrene, polyvinyl chloride, polyethylene, polypropylene, polyacrylonitrile, polyacrylic acid esters, polyamides, polyurethanes or polyesters, rubber, casein, latices, silicones and silicone resins, individually or in mixtures.
• azo colorants, finely divided pigments and pigment preparations produced according to the invention are also suitable as colorants in electrophotographic toners and developers, such as e.g. One or
• Two-component powder toner also called one- or two-component developer
• magnetic toner
• liquid toner
• polymerization toner
• special toner
• Typical toner binders are polymerization, polyaddition and polycondensation resins, such as styrene, styrene-acrylate, styrene-butadiene, acrylate, polyester, phenol-epoxy resins, polysulfones, polyurethanes, individually or in combination, and polyethylene and polypropylene, which also contain other ingredients, such as charge control agents, waxes or flow aids, can contain or be modified afterwards with these additives.
• Typical hardener components are, for example, acid anhydrides, imidazoles and dicyandiamide and their derivatives, blocked isocyanates, bisacylurethanes, phenolic and melamine resins, triglycidyl isocyanurates, oxazolines and dicarboxylic acids.
• the azo colorants, finely divided pigments and pigment preparations produced according to the invention are suitable as colorants in ink-jet inks on an aqueous and non-aqueous basis and in those inks which work according to the hot-melt process.
• the azo colorants, finely divided pigments and pigment preparations produced according to the invention are also suitable as colorants for color filters, both for subtractive and for additive color generation.
• the pigment preparations mentioned according to the invention can of course also contain, as a pigment, an azo pigment which was prepared by the method described under A) above.
• a vortex chamber reactor which has either two or three nozzles, each with a diameter of 300 ⁇ m.
• the two or three nozzles enclose an angle of 144 ° in total and are set at an angle of 30 °, based on the cross-sectional area of the mixing chamber, against the outlet opening.
• the nozzles have an angular spacing of 72 °.
• the swirl chamber is a cylinder 5 mm in diameter and 11 mm in length.
• the pigment solution is metered into the vortex chamber reactor at a flow rate of 7 l / h (12.6 kg / h) through a nozzle, and water at a total flow rate of 23.8 l / h through two nozzles.
• the resulting pigment suspension (75 ° C) is collected in a storage vessel, suction filtered, washed neutral with water and worked up further.
• Example for an azo clutch clutch from C.I. Pigment Red 269:
• the diazonium salt solution and the naphthol solution are each metered into the vortex chamber reactor through a nozzle at a flow rate of 42.5 l / h and 42.0 l / h, respectively.
• Collection vessel collected, suction filtered, washed neutral with water and further processed.
• 3800 g of a commercially available pigment P.R.168, 400 g of a 5-core nonylphenol condensate composed of formaldehyde and nonylphenol and 600 g of an ethoxylated oleyl alcohol are stirred in 2500 g of ethylene glycol and 2700 g of water.
• This suspension is metered at a total flow rate of 42.5 l / h through two nozzles into the swirl chamber reactor.
• the resulting pigment preparation is collected in a storage container.

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• Chemical & Material Sciences (AREA)
• Chemical Kinetics & Catalysis (AREA)
• Organic Chemistry (AREA)
• Dispersion Chemistry (AREA)
• Life Sciences & Earth Sciences (AREA)
• Engineering & Computer Science (AREA)
• Materials Engineering (AREA)
• Wood Science & Technology (AREA)
• Inks, Pencil-Leads, Or Crayons (AREA)

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• 2002
  • 2002-10-25 DE DE10249747A patent/DE10249747A1/de not_active Withdrawn
• 2003
  • 2003-09-24 KR KR1020057006989A patent/KR20050056262A/ko not_active Application Discontinuation
  • 2003-09-24 US US10/532,565 patent/US20060042117A1/en not_active Abandoned
  • 2003-09-24 JP JP2004545781A patent/JP2006503940A/ja not_active Withdrawn
  • 2003-09-24 WO PCT/EP2003/010610 patent/WO2004037929A1/de active Application Filing
  • 2003-09-24 CN CNB038245442A patent/CN1298786C/zh not_active Expired - Fee Related
  • 2003-09-24 EP EP03748080A patent/EP1558682A1/de not_active Withdrawn

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