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EP1300513A2 - Utilisation de préparations solides d'azurant optiques pour l'azurage optique de papier - Google Patents

Utilisation de préparations solides d'azurant optiques pour l'azurage optique de papier Download PDF

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Publication number
EP1300513A2
EP1300513A2 EP02021335A EP02021335A EP1300513A2 EP 1300513 A2 EP1300513 A2 EP 1300513A2 EP 02021335 A EP02021335 A EP 02021335A EP 02021335 A EP02021335 A EP 02021335A EP 1300513 A2 EP1300513 A2 EP 1300513A2
Authority
EP
European Patent Office
Prior art keywords
brightener
solid
paper
weight
preparations
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP02021335A
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German (de)
English (en)
Other versions
EP1300513A3 (fr
Inventor
Dietrich Dr. Tegtmeyer
Rolf Dr. Brockmann
Bernhard Hunke
Thomas Hübbe
Erwin Dr. Bacher
Thomas Dr. Roick
Peter-Roger Nyssen
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Blankophor GmbH and Co KG
Original Assignee
Bayer AG
Kemira Oyj
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Bayer AG, Kemira Oyj filed Critical Bayer AG
Publication of EP1300513A2 publication Critical patent/EP1300513A2/fr
Publication of EP1300513A3 publication Critical patent/EP1300513A3/fr
Withdrawn legal-status Critical Current

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    • D—TEXTILES; PAPER
    • D21—PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21H—PULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H21/00—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties
    • D21H21/14—Non-fibrous material added to the pulp, characterised by its function, form or properties; Paper-impregnating or coating material, characterised by its function, form or properties characterised by function or properties in or on the paper
    • D21H21/30—Luminescent or fluorescent substances, e.g. for optical bleaching

Definitions

  • the invention relates to the use of solid, particulate brightener preparations for the optical brightening of paper.
  • the optical brightening of paper comes from the paper pulp, in the size press and in the paper line for use.
  • ecological aspects e.g. with the meaning of Avoidance of organic wastewater loads and economic aspects, e.g. in the In terms of cost-effective processes.
  • liquid brightener formulations be it in the form of solutions or of suspensions, also called slurries or slurries.
  • Stilbene brighteners substituted by sulfo groups are preferred, in particular Triazinylstilbene brighteners are used, which are often characterized by good substantivity on the one hand distinguish, but accordingly by a limited solubility in cold water on the other hand are marked. In purely aqueous solutions, they already tend to low concentrations to crystalline precipitates, in particular as a result of Hydration of the brightener compounds. Storage-stable aqueous solutions such as these e.g. are described in DE-A-2 928 053, therefore also contain considerable Amounts of fillers and organic solvents.
  • DE-A-2 715 864 therefore uses "slurries", ie suspensions, as a way out optical brightener described by mixing the water-moist brightener press cake with dispersants and optionally electrolytes, organic Extender agents (urea etc.) and gelling agents are produced.
  • slurries are longer Period not stable to sedimentation.
  • DE-A-2 715 864 also describes the advantages with regard to the dust behavior of Slurries over dry powders by drying and grinding of the water-moist press cake are obtained.
  • DE-A-3 523 207 describes low-dust solid brightener preparations for use described in textile dye baths, which are spray-dried by mixing optical brightener formulation with an aromatic carboxylic acid ester or Fatty acid polyol esters are obtained, and are characterized by good hot water solubility Mark (80 ° C).
  • solid, particulate brightener preparations which are preferably largely or completely free of crystalline brightener particles, especially their hydrate forms, are one in comparison to the above State of the art improved dissolution rate in water, especially in Cold water, preferably at 10 to 30 ° C, and therefore for continuous and discontinuous lightening of paper in the above-mentioned processes are suitable.
  • Especially for continuous application in the pulp (pulp) in papermaking also have more concentrated solutions above 5% sufficient stability against precipitation for the duration of the application.
  • solubility of> 0.1 g / l, preferably> 1 g / l, in particular> 5 g / l at 20 ° C understood.
  • R 1 , R 2 and R 3 independently of one another denote -NH 2 , -NH-CH 3 , -NH-C 2 H 5 , -N (CH 3 ) 2 , -N (C 2 H 5 ) 2 , -NH -CH 2 CH 2 OH, -NH-C 2 -C 4 -hydroxyalkyl, -N (C 2 -C 4 -hydroxyalkyl) 2 -NH-CH 2 CH 2 SO 3 H; -NH-CH 2 -CH 2 -O-CH 2 -CH 2 -OH, -OCH 3 , -OCH (CH 3 ) 2 , -O-CH 2 -CH 2 -O-CH 3 , -N (CH 2 -CH 2 -OH) 2 , -N (CH 2 -CHOH-CH 3 ) 2 , morpholino, -SCH 3 , -N (CH 2 -CH 2 -OH) CH 2 -CH 2 -CON
  • M is preferably H, Na, Li, K, Ca, Mg, ammonium or ammonium, which is mono-, di-, tri- or terasubstituted by C 1 -C 4 alkyl, C 2 -C 4 hydroxyalkyl or a mixture it.
  • Brighteners from the distilbene series can also be used are described for example in EP-A-0 385 374, and cationic brighteners.
  • Brighteners may also be used, which are obtained by cationizing anionic ones, in particular brighteners containing sulfo and / or carboxyl groups, for example by means of polymeric quaternary ammonium compounds can be obtained.
  • Such brighteners are e.g. in WO-A-9967317.
  • the solid preparations to be used according to the invention contain as a component b) water in the form of residual moisture.
  • the amount of water is under residual moisture understood as moisture, based on the solid preparation, comprehensively free Water, trapped water and adsorbed water, not crystal water (i.e. water stoichiometrically integrated in a crystal structure) or constitutional water [see Widmann, Riesen: “Thermoanalysis", Hüthigverlag, Heidelberg 1984].
  • the solid brightener preparations to be used according to the invention are preferred X-ray amorphous.
  • the solid brightener preparations can contain further auxiliaries, preferably in an amount of less than 10% by weight, based on the preparation, contain; as such e.g. to be mentioned: formulation aids such as fillers, blending agents, surfactants and / or defoamers, and organic thickeners or protective colloids, preservatives, dedusting agents and Electrolytes.
  • formulation aids such as fillers, blending agents, surfactants and / or defoamers, and organic thickeners or protective colloids, preservatives, dedusting agents and Electrolytes.
  • the solid Aulheller preparations preferably contain from ecological For this reason, only very small proportions of organic additives, auxiliary agents and / or impurities, in particular less than 5% by weight in total based on brightener of component a), very particularly less than 2% by weight.
  • electrolytes are sodium chloride, sodium sulfate, sodium carbonate, or one of the corresponding potassium salts or mixtures of the above Substances.
  • the amount of electrolyte can be less than or equal to 2% by weight, preferably 0.001 to 2 wt .-%, based on the total weight of the solid preparation, in particular 0.001 to 0.5 wt .-%.
  • sulfonated aromatics of Comp. A are also in the context of this application understood sulfomethylated aromatics.
  • Preferred sulfonated aromatics are: Naphthalenesulfonic acids, phenolsulfonic acids, dihydroxybenzenesulfonic acids, sulfonated Ditolyl ether, sulfomethylated 4,4'-dihydroxydiphenyl sulfone, sulfonated diphenylmethane, sulfonated biphenyl, sulfonated hydroxybiphenyl, especially 2-hydroxybiphenyl, sulfonated terphenyl or benzenesulfonic acids.
  • Aldehydes and / or ketones of component B) include, in particular, aliphatic, cycloaliphatic as well as aromatic in question.
  • Aliphatic are preferred Aldehydes, with particular preference formaldehyde and other aliphatic aldehydes with 3 to 5 carbon atoms.
  • Examples of unsulfonated aromatics of component C) are phenol, Cresol, 4,4'-dihydroxydiphenylsulfone or dihydroxydiphenylmethane in question.
  • urea derivatives for example, dimethylol urea, melamine or Guanidine can be called.
  • the condensation product preferably obtained in the condensation preferably has an average degree of condensation of 1 to 150, particularly preferred from 1 to 20, in particular from 1 to 5.
  • condensation products of component c) can be in the form of an aqueous solution or Suspension or as a solid, for example as a powder or granules, preferably as spray-dried powder or granules.
  • Preferred condensation products of component c) have an inorganic one Salinity below 10% by weight, preferably below 5% by weight, in particular below 1 wt .-%, based on the aqueous solution or suspension used Component or based on the solid of component c) used.
  • Low monomer means a residual monomer content of less than 30% by weight, preferably less than 20% by weight, based on the condensation product, particularly preferably ⁇ 10% by weight, preferably ⁇ 5% by weight. Under In this context, residual monomers are used to produce the condensation product understood reactants used.
  • Such low salt and low residual monomer condensation products are for example known from EP-A 816 406.
  • the condensation products of component c) can be produced in this way, for example that the sulfonated aromatics of component A) optionally in a mixture with unsulfonated aromatics of component C) by reacting the underlying aromatics with a sulfonating agent preferably sulfuric acid, especially concentrated sulfuric acid, chlorosulfonic acid, Amidosulfonic acid or oleum.
  • a sulfonating agent preferably sulfuric acid, especially concentrated sulfuric acid, chlorosulfonic acid, Amidosulfonic acid or oleum.
  • the condensation then takes place with aldehydes and / or ketones of the components B), preferably formaldehyde, optionally together with others Compounds of component C).
  • the condensation is preferably carried out in aqueous Solution at a pH of 0 to 9.
  • aqueous Solution at a pH of 0 to 9.
  • preferably per mol of sulfonated aromatics A) or per mole of a mixture of sulfonated aromatics of component A) and unsulfonated aromatics of component C) 0.4 to 1.5 mol, in particular 0.4 to 1.0 mol of component B) are used.
  • the separation of the inorganic acid or its salts and the reduction the residual monomer content can, for example, by means of membrane separation processes be performed.
  • the preferred membrane separation processes are Ultrafiltration, diffusion dialysis or electrodialysis in question.
  • membranes preferably in ultrafiltration
  • membranes have a molecular weight cut-off (MWCO) of 1,000 to 10,000 daltons.
  • the separation of the inorganic acid using a membrane separation process is preferably carried out by diafiltration with acid-stable ultra or Cross-flow filtration nanofiltration membranes.
  • suitable membranes include polyhydantoin membranes such as those found in EP-A 65 20 44 are known.
  • Preferred membranes for this purpose have a MWCO level of 2,000 to 10,000 daltons. If necessary, concentration is carried out simultaneously in this process step.
  • the solid brightener preparations to be used according to the invention contain a component d) from the group of inorganic solids, such as, for example, sheet silicates such as bentonite or montmorillonite, optionally hydrophobicized, highly disperse, amorphous pyrogenic silicic acids, highly disperse silica sols, very fine, optionally hydrophobicized kaolin or highly disperse aluminum oxide ;
  • component d) has a specific surface area [BET method] of 2 to 1,500, preferably 10 to 800 m 2 / g.
  • the brightener preparations can also contain organic thickeners contain.
  • Suitable thickeners are those from the group of anionic or non-ionic organic water-soluble polymers to name the following Can also be understood as protective colloids for solid brightener preparations can.
  • a compound is preferably used as the organic thickener, whose 4% aqueous solution has a viscosity of ⁇ 2 mPa.s at 20 ° C.
  • Starch derivatized starch and in particular are preferred as thickeners degraded starch in question.
  • Degraded starch is obtained, for example, by e.g. native potato, Wheat, corn, rice or tapioca starch an oxidative, thermal, enzymatic or hydrolytic degradation. Oxidative degradation is preferred here Starches, potato starch oxidatively degraded with hypochlorite is particularly preferred.
  • Dextrins and cyclodextrins are also particularly suitable.
  • dextrins are preferably white dextrins, yellow dextrins and maltodextrins with a Cold water solubility of greater than 50% by weight, preferably greater than 90%, measured at 10 g to 200 ml of water at 20 ° C understood.
  • Preferred cyclodextrins are those of the ⁇ -CD type with 6 glucopyranose units, ⁇ -CD with 7 glucopyranose units and ⁇ -CD with 8 glucopyranose units as well as branched AB, AC, AD-diclosyl-CD and mixtures of the dextrins mentioned.
  • Polysaccharides in particular, come as preferred anionic polyhydroxy compounds Xanthan and carboxymethyl cellulose in question.
  • cellulose derivatives methyl cellulose, Hydroxymethyl cellulose, hydroxyethyl and propyl cellulose can be used.
  • At least partially hydrolyzed come as thickeners Polymers and copolymers of vinyl acetate, which completely in water dispersible, preferably completely soluble, in question.
  • Partially hydrolyzed polyvinyl alcohols and polyvinyl alcohol are particularly preferred self.
  • Copolymers of vinyl acetate are used in particular as thickeners fully or partially hydrolyzed vinyl alcohol copolymers understood, in particular fully hydrolyzed Copolymers of alkyl vinyl ester and vinyl acetate with a proportion of alkyl vinyl ester of preferably 5 to 20 mol%, very particularly copolymers of alkyl vinyl acetate and vinyl acetate.
  • Homopolymers and copolymers of N-vinylpyrrolidone also come as thickeners in question that completely disperse in water.
  • the molecular weight of the homo- and copolymers of N-vinylpyrrolidone is preferably 2,000 to 1,200,000, preferably 10,000 to 150,000 g / mol.
  • Homopolymers of N-vinylpyrrolidone and copolymers are very particularly preferred with vinyl esters and Na methacrylate.
  • the brighteners of component a), in particular of the general formula (I), are either known or can be prepared by methods known per se and are usually as free acid or as its salts, preferably alkali metal salts used.
  • the solid brightener preparations are preferably produced by Drying a concentrated solution of the brighteners described, if necessary together with the auxiliary substances mentioned.
  • the process for producing the solid brightener preparations is, for example characterized in that the optical brighteners of component a) are preferred in solid form as finished or unfinished powder, granules or as water-moist Press cake, in an aqueous medium, optionally together with a part of components c) and / or d) and, if appropriate, further additives, completely dissolves and then dries.
  • An aqueous medium is preferably used which has a pH of 6.5 to 12, in particular from 7.5 to 12. Generally a temperature from 15 to 98 ° C, preferably from 40 to 98 ° C, in particular from 60 to 95 ° C for Achieved a complete solution. If necessary, clarification filtration the solution to separate unwanted by-products (e.g. triazines) to be required.
  • a pH of 6.5 to 12 in particular from 7.5 to 12.
  • a temperature from 15 to 98 ° C, preferably from 40 to 98 ° C, in particular from 60 to 95 ° C for Achieved a complete solution.
  • clarification filtration the solution to separate unwanted by-products (e.g. triazines) to be required.
  • the aqueous solution is preferably applied to a pH from 6.5 to 10, in particular 7.5 to 9.5, adjusted and dried in the transferred brightener preparation according to the invention.
  • a suitable method for the drying is in particular spray drying, preferably single-component spray drying using high pressure or swirl chamber nozzles or spray drying Atomizing disks, freeze drying with upstream or downstream granulation or dry processing, spray freeze drying, build-up granulation, for example after the plate or drum granulation process, if necessary with partial pre-dried product, fluid bed drying and granulation, mixer agglomeration and drying, if necessary in combination with fluidized bed or Fluid bed drying.
  • processes such as mixed agglomeration in suspension with subsequent fluidized bed or fluid bed drying, Granulation by means of paste shaping and subsequent drying and crushing or pelleting and steam jet agglomeration in question. Combinations of the methods mentioned are also possible.
  • Spray drying processes using high-pressure or swirl chamber nozzles spray drying with integrated and / or downstream Fluid bed agglomeration and / or drying, the build-up granulation using the plate process and fluid bed granulation and drying.
  • the solid brightener preparations to be used according to the invention a residual moisture content (component b)) of 0.1 to 15% by weight, in particular 0.5 up to 10% by weight and an average mass-related particle size of greater than or equal to 5 ⁇ m, especially 5 to 5000 ⁇ m, preferably 15 to 2000 ⁇ m and in particular from 40 to 1000 ⁇ m.
  • the solid brightener preparations to be used according to the invention are based in particular on a spherical or spherical one or particle structure derived therefrom. Agglomerates also come from Particles from the shapes mentioned in the range of the specified particle size in Question.
  • the solid brightener preparations can be powders, granules or so-called microgranules (e.g. from single-component nozzle spray drying).
  • the solid preparations can also be used known methods worked up, in particular dusted.
  • the dedusting can be used directly in connection with drying e.g. as injection dedusting or aerosol dedusting as well as following the drying, for example in a mixer or a fluidized bed.
  • Both water-soluble and water-insoluble or sparingly soluble compounds are suitable as dedusting agents.
  • dedusting agents Such means are known per se;
  • Examples of water-soluble dustproofing agents are polyglycols (PEG) and PEG block copolymers; White oils and aromatic or aliphatic alkyl esters boiling above 150 ° C. may be mentioned as poorly soluble dedusting agents.
  • Preferred dedusting agents are polyethylene glycol and glycerol mono (di / tri) acetic acid ester.
  • the use of the solid brightener preparations according to the invention relates to this Lightening paper pulps in papermaking ("bulk dyeing"), e.g. Cellulose, Wood pulp (chemical and mechanical pulp), the lightening of the paper industry commonly used coating slips, i.e. the lightening of unfilled, especially filled paper masses and pigmented coating slips, as well as lightening in the glue or film press.
  • bulk dyeing e.g. Cellulose, Wood pulp (chemical and mechanical pulp)
  • coating slips i.e. the lightening of unfilled, especially filled paper masses and pigmented coating slips, as well as lightening in the glue or film press.
  • the use according to the invention is preferably characterized in that the solid brightener preparation either yourself or, if necessary, after mixing with Water into an aqueous pulp mixture, paper coating slip or size press liquor is introduced.
  • Mixing with water means preferably dissolving.
  • the dissolving process can take place during or during the Are fed into the pulp mixture and / or in the pulp mixture itself, it is preferred that the dissolving process is complete before the paper sheet is formed is completed.
  • Use in bulk coloring or surface coating is particularly preferred, which is preferably characterized in that the solid brightener preparation continuously or discontinuously, preferably continuously, with a concentration of 0.01 to 40 wt .-%, based. on component a), in particular 1 to 25 wt .-% at a temperature of 10 to 75 ° C, in particular 15 to 55 ° C, and a pH of 6.0 to 12, in particular 6.5 to 11, very particularly 6.5 to 9.5, is dissolved in water and in an aqueous pulp mixture, paper coating slip or size press liquor is introduced.
  • an aqueous solution of the solid brightener preparation can preferably be used the pulp at each stage of the paper making process before Sheet formation can be added.
  • Continuous means that the brightener preparation in the Desired concentration, based on the mass of paper pulp, continuously the paper pulp is added; this advantageously takes place in the both the solid brightener preparation and water in a certain ratio for brightener preparation, for example in a stirrer tank, continuously be brought together, the optical brightener is released and the received, generally concentrated, solution to the material flow or the dilution water is metered into the paper machine in the desired ratio.
  • the invention further relates to the use in coating compositions for optical Lighten paper.
  • the preferred coating slips contain, for example, plastic dispersions as binders based on copolymers of butadiene-styrene, acrylonitrile-butadiene-styrene, Acrylic acid esters, ethylene vinyl chloride or ethylene vinyl acetate or based on homopolymers, such as polyvinyl chloride, polyvinylidene chloride, Polyethylene, polyvinyl acetate or polyurethanes.
  • a preferred binder consists of styrene-butyl acrylate or styrene-butadiene-acrylic acid copolymers. Further polymer latices are described, for example, in US Pat. No. 3,265,654.
  • Aluminum silicates, such as, are usually used to pigment the coating slips China clay and kaolin, also barium sulfate, satin white, titanium dioxide or natural or precipitated calcium carbonate.
  • the coating slips preferably contain 5 to 75% by weight of an at least white pigment.
  • the binder is preferably used in an amount sufficient that the dry content of polymeric compound 1 to 30 wt .-%, preferably Accounts for 5 to 25% by weight of the white pigment.
  • the amount of the invention The fixed brightener preparation to be used is preferably calculated in such a way that the brightener of component a) in amounts of 0.005 to 2 wt .-%, in particular 0.01 to 1.5 wt .-%, based on white pigment, is present.
  • the coating slip can be produced, for example, by the Components in any order at temperatures from 10 to 100 ° C, preferably 20 to 80 ° C, mixes.
  • the components here also include the usual ones Tools used to regulate rheological properties, such as viscosity or water retention that coating slips can be used.
  • Tools are e.g.
  • binders such as starch, casein, protein or Gelatin, cellulose ethers, such as carboxyalkyl cellulose or hydroxyalkyl cellulose, Alginic acid, alginates, polyethylene oxide or polyethylene oxide alkyl ethers, copolymers of ethylene oxide and propylene oxide, polyvinyl alcohol, polyvinyl pyrrolidone, water-soluble condensation products of formaldehyde with urea or melamine, Polyphosphates or polyacrylic acid salts.
  • cellulose ethers such as carboxyalkyl cellulose or hydroxyalkyl cellulose
  • Alginic acid alginates
  • polyethylene oxide or polyethylene oxide alkyl ethers copolymers of ethylene oxide and propylene oxide
  • polyvinyl alcohol polyvinyl pyrrolidone
  • water-soluble condensation products of formaldehyde with urea or melamine Polyphosphates or polyacrylic acid salts.
  • the solid brightener preparations to be used according to the invention are either into the finished coating slip or into one of the components of the coating slip incorporated.
  • the solid preparations can be added directly or likewise be added in the form of aqueous solutions. Aqueous solutions if necessary, produced continuously and in the process of the so-called intermediate step continuously introduced.
  • the coating slip can, in particular, be used to coat cellulose-based materials Paper, wood, foils, e.g. Cellulose, cellulose triacetate, cotton fabrics etc. can be used. Application to is particularly preferred Paper, cardboard and cardboard as well as photo paper.
  • the coating slip can be applied to the substrate by any conventional method be, for example with an air knife, a doctor knife, one Brush, roller, squeegee or rod, whereupon the coating e.g. with an infrared dryer, hot air dryer and / or contact dryer at temperatures the substrate surface in the range from 60 to 200 ° C., preferably from 90 up to 130 ° C, until a residual moisture of 3 to 6 wt .-% is dried.
  • any conventional method be, for example with an air knife, a doctor knife, one Brush, roller, squeegee or rod, whereupon the coating e.g. with an infrared dryer, hot air dryer and / or contact dryer at temperatures the substrate surface in the range from 60 to 200 ° C., preferably from 90 up to 130 ° C, until a residual moisture of 3 to 6 wt .-% is dried.
  • the brightener preparations to be used according to the invention continue to stand out by a number of advantages. As solid, concentrated, particulate preparations they are easy to pour, can be metered and, if necessary, they are low-dust or low-dust adjustable.
  • the solid brightener preparations can be used for the surface in the usual Glue and film press fleets are used, in portions or continuously in the form of solid preparations or concentrated preparations made therefrom Solutions are added.
  • the approximately 10% clear solution obtained had a pH of 8.5 and was above one Stable for more than 2 hours.
  • the approximately 10% clear solution obtained had a pH of 8.6 and was above one Stable for more than 2 hours.
  • the E1 / 1 value as a measure of the color strength determined by means of extinction was also 546th
  • a laboratory magnetic stirrer was placed in a beaker at room temperature 90 ml of deionized water are introduced and, with vigorous stirring, 10 g of a solid Brightener preparation as in Example 2, but following the spray drying in a mixer with 0.6% by weight based on the solid preparation triacetin (Glycerol triacetate) was dedusted, introduced and completely dissolved.
  • the approximately 10% clear solution obtained had a pH of 8.2 and was above one Stable for more than an hour.
  • Example 5 Use according to the invention in paper coating
  • the pH of the coating color was adjusted to 8-8.5 with dilute sodium hydroxide solution and the solids content of the coating color was adjusted to 60-65% by adding water.
  • the coating color was divided into 3 parts and in each part of the coating color were the solid brightener preparations described in Examples 1 to 3 in a quantity of 5 g based on 1 kg of coating color homogeneously introduced and over solved a period of 10 min.
  • the sheets coated in this way were dried in a drying cylinder at 95 ° C. for 1 min and then stored for 3 hours at 23 ° C and a humidity of 50%, before they were measured. In all 3 cases papers with a very high result high whiteness and good levelness.
  • the pH of the liquors was about 7.
  • the wet pickup was about 50-60%.
  • Example 7 Continuous process according to the invention for continuous dissolving and for use in pulp dyeing
  • the solid brightener preparation described in Example 1 was used over a period of time of 1 hour (stationary operation) continuously using a dosing screw a quantity of 120 kg / h (average over 10 min discharge time at fixed screw speed) using a hold-up disperser together with 880 l / h 45 ° C warm, partially demineralized water in a 500 l stirred tank with propeller stirrer from Initiated above and at the same time 1000 kg / h of the mixture obtained on the bottom removed by means of a rotor-stator pump.
  • the stirrer speed was set so that a high mixing effect was achieved, so that floating of particles of the solid brightener preparation was avoided.
  • the fixed Auheller preparations could also be made the compositions from Examples 2 and 3 with a comparably good result be resolved continuously.
  • the release stability with the fixed Brightener preparation from example 2 more than 6 hours and clear solutions were found up to a concentration of more than 22% by weight can be obtained.

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EP02021335A 2001-10-05 2002-09-23 Utilisation de préparations solides d'azurant optiques pour l'azurage optique de papier Withdrawn EP1300513A3 (fr)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE2001149314 DE10149314A1 (de) 2001-10-05 2001-10-05 Verwendung fester Aufhellerpräparationen zum Aufhellen von Papier
DE10149314 2001-10-05

Publications (2)

Publication Number Publication Date
EP1300513A2 true EP1300513A2 (fr) 2003-04-09
EP1300513A3 EP1300513A3 (fr) 2007-04-04

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EP02021335A Withdrawn EP1300513A3 (fr) 2001-10-05 2002-09-23 Utilisation de préparations solides d'azurant optiques pour l'azurage optique de papier

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160060814A1 (en) * 2013-04-29 2016-03-03 Blankophor Gmbh & Co., Kg Use of Micronized Cellulose and Fluorescent Whitening Agent for Surface Treatment of Cellulosic Materials
CN108472973A (zh) * 2015-11-24 2018-08-31 Omya国际股份公司 印刷水印
CN110512465A (zh) * 2019-08-28 2019-11-29 泰中特种纸有限公司 一种量子点辅助沉积制备彩色防伪水印纸的方法

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE2715864A1 (de) * 1976-04-14 1977-10-27 Ciba Geigy Ag Verfahren zum optischen aufhellen von papier
US4364845A (en) * 1978-07-17 1982-12-21 Ciba-Geigy Corporation Concentrated aqueous solutions of sulfo group-containing fluorescent brighteners which are stable on storage
BR9000850A (pt) * 1989-02-28 1991-02-05 Ciba Geigy Ag Formulacao aclaradora estavel a armazenagem,processo para sua preparacao e aplicacao
EP0835906B1 (fr) * 1996-10-10 2003-11-05 Ciba SC Holding AG Dispersions d'azurants optiques

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20160060814A1 (en) * 2013-04-29 2016-03-03 Blankophor Gmbh & Co., Kg Use of Micronized Cellulose and Fluorescent Whitening Agent for Surface Treatment of Cellulosic Materials
CN108472973A (zh) * 2015-11-24 2018-08-31 Omya国际股份公司 印刷水印
CN108472973B (zh) * 2015-11-24 2021-02-23 Omya国际股份公司 印刷水印
CN110512465A (zh) * 2019-08-28 2019-11-29 泰中特种纸有限公司 一种量子点辅助沉积制备彩色防伪水印纸的方法

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DE10149314A1 (de) 2003-04-17

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