Classifications

• • 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
  • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
  • D21H17/03—Non-macromolecular organic compounds
  • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
  • D21H17/07—Nitrogen-containing compounds
• • 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
  • D21H17/00—Non-fibrous material added to the pulp, characterised by its constitution; Paper-impregnating material characterised by its constitution
  • D21H17/03—Non-macromolecular organic compounds
  • D21H17/05—Non-macromolecular organic compounds containing elements other than carbon and hydrogen only
  • D21H17/14—Carboxylic acids; Derivatives thereof

Definitions

• the present invention relates to a process for the production of paper or cardboard which is sized in alkaline or neutral size and which consists in adding an anionic, hydrophobic sizing agent and a cationic retention agent to the pulp suspension having a pH of at least 6.5, wherein the sizing agent, etc. consists of an unsaturated aliphatic compound, e.g. an N-alkylamide group or alkyl ester group preferably having 6 to 22 carbon atoms and at least one acidic group, e.g. contains a carboxyl group.
• an unsaturated aliphatic compound e.g. an N-alkylamide group or alkyl ester group preferably having 6 to 22 carbon atoms and at least one acidic group, e.g. contains a carboxyl group.
• the pH of the fiber suspension is at least 6.5 in the absence of acids, e.g. Sulfuric or formic acid, or especially latent acidic sulfates such as e.g. Aluminum sulfate (alum) is discontinued.
• acids e.g. Sulfuric or formic acid
• latent acidic sulfates such as e.g. Aluminum sulfate (alum) is discontinued.
• paper with relatively little sizing agent is obtained which has an increased shelf life.
• the subject of the present invention thus relates to a process for the alkaline or neutral gluing of paper or cardboard, i.e. a process for the production of alkaline or neutral sized paper or cardboard, which is characterized in that aqueous, cellulose-containing, optionally filler-containing fiber suspensions, which in the absence of acids or latent acidic sulfates such as e.g.
• Aluminum sulfate has a pH of at least 6.5, preferably at least 7.0, at least (A) an anhydride group-free, aliphatic, unsaturated sizing agent, which has a single N-alkyl or N-alkenylamide group or alkyl or alkenyl ester group, each with at least 6 Carbon atoms in the alkyl or alkenyl radical as hydrophobic substituents and at least one anionic salt form or acidic, ie has a free group and (B) adds a polymeric, cationic retention agent in any order or simultaneously.
• A an anhydride group-free, aliphatic, unsaturated sizing agent, which has a single N-alkyl or N-alkenylamide group or alkyl or alkenyl ester group, each with at least 6 Carbon atoms in the alkyl or alkenyl radical as hydrophobic substituents and at least one anionic salt form or acidic, ie has a free group and
• the specified sizing agents (A) are new compounds which, together with the process for their preparation, also form further objects of the present invention.
• the sizing agents (A) used according to the invention generally have an anionic group, which is generally present as acidic carboxyl groups. Such groups are preferably present as salts, for example as amine, ammonium or sodium salts in aqueous medium at the pH values of at least 6.5, preferably at least 7.0, of the fiber suspensions and can optionally form anions during papermaking.
• the cationic retention agents (B) can also form cations.
• anion-active or cation-active retention agents The ability of the sizing agents and the retention aids to form anions or cations under the conditions of paper production can also be described as anion-active or cation-active.
• anionic sizing agents and the cationic retention agents can also be called anion-active sizing agents or cation-active retention agents.
• the sizing agents (A) have a single N-alkyl or N-alkenylamide group or alkyl or alkenyl ester group as hydrophobic substituents.
• the alkyl or alkenyl radicals in these N-alkyl or N-alkenyl groups or alkyl or alkenyl ester groups each independently have at least 6, especially 6 to 22, preferably 11 to 22, in particular 16 to 20 carbon atoms. Alkyl residues are preferred over alkenyl residues.
• the hydrophobic substituents are generally derived from unsaturated or, above all, saturated, primary fatty amines or fatty alcohols.
• the fatty amines and fatty alcohols are in turn derived from unsaturated or, above all, saturated C 6 -C 22 , preferably Cii-C22, in particular C 16 -C 20 fatty acids.
• C 6 -C 22 preferably Cii-C22, in particular C 16 -C 20 fatty acids.
• These are, for example, capronic, preferably caprylic, capric, lauric, myristic or myristoleic, palmitoleic, elaeostearic, clupanodonic acid, in particular oleic, elaidic, erucic, linoleic and linolenic acid.
• palmitic, stearic, oleic and behenic acids are of particular importance, with palmitic and especially stearic acids being of primary interest. Also easily accessible, technical mixtures of these Fatty acids come into consideration.
• Synthetic fatty acids and fatty alcohols that can be produced, for example, by oxo
• the preferred primary fatty amines from which the N-alkyl or N-alkenylamide groups of the sizing agents used according to the invention are derived are, for example Hexylamine, octylamine (also called caprylamine), especially dodecyl, hexadecyl and octadecenylamine (also called lauryl, palmityl and oleylamine) and its good accessibility because of in particular octadecylamine (also called stearylamine).
• fatty alcohols from which the alkyl or alkenyl ester groups of the sizing agents used according to the invention are derived e.g. Hexanol, n- and i-octanol, especially dodecanol, hexadecanol and octadecenol (also called lauryl, palmityl and oleyl alcohol) and its good accessibility because of especially octadecanol (also called stearyl alcohol) mentioned.
• Such half-esters or half-amides of the specified dicarboxylic acids preferably correspond to the formula wherein D 1 is straight-chain or branched alkenylene having 2 to 6 carbon atoms and 1 or 2 double bonds or ethynylene, R 1 is alkyl or alkenyl having 6 to 22, preferably 11 to 22, in particular 16 to 20 carbon atoms and X is -NH- or -0- , and especially the formula wherein D 2 is straight-chain or branched alkenylene with 2 or 3 carbon atoms, R 2 is alkyl or alkenyl with 16 to 20 carbon atoms and X has the meanings given.
• alkenyl radicals having 3 carbon atoms are preferably branched. Accordingly, the focus of interest is sizing agents, the compounds of the formula which may be in salt form represent, wherein D 3 is an alkenylene radical of the formula or means and R 2 and X have the meanings given.
• sizing agents of the formula (3) are, for example, compounds of the formulas which are optionally present in salt form called.
• the compounds of the formulas (6), (7), (8) and (9) are mixtures of isomers.
• the sizing agents Before they are used as component (A) in the paper sizing process according to the invention, the sizing agents generally do not need Recrystallization to be cleaned, but can usually as such, as they arise in their manufacture, i.e. can be used without further processing.
• the sizing agent (A) and the retention agent (B) are added separately (in any order) to the fiber suspension in the process according to the invention for sizing paper or cardboard, it is expedient to use the sizing agent at least partially in salt form.
• such salts can be obtained by adding the sizing agents (A) Manufactured by adding, inter alia, an alkylamine or alkanolamine with a total of at most 6 carbon atoms, for example trimethylamine, triethylamine, monoethanolamine, diethanolamine, especially by adding ammonia or an alkali metal hydroxide, for example potassium or especially sodium hydroxide, generally in an aqueous medium at room temperature (about 15 to about 25 ° C) completely or partially converted into the corresponding salts.
• alkali metal hydroxide for example potassium or especially sodium hydroxide or in particular ammonia
• An alkali metal hydroxide is expediently generally used in the form of its dilute, about 1 to 10 percent by weight, aqueous solutions.
• a maximum of 3 mol, especially 0.1 to 1.5, in particular 0.9 to 1.1 mol, of ammonia or alkali metal hydroxide is expediently used per acidic group of the sizing agent present.
• the sizing agents present as salts thus have, for example, acidic carboxyl groups which are at least partially converted into the groups -COO ⁇ M ⁇ , where M denotes the corresponding amine, ammonium or alkali metal cations.
• Preferred sizing agents (A) of the type mentioned have molecular weights of about 200 to about 500, preferably about 300 to about 400 and, owing to their content of at least one acidic group of the type mentioned, an acid number (mg KOH / g substance) of about 100 to about 300 , preferably about 130 to about 180.
• the sizing agents used as component (A) in the paper sizing process according to the invention are compounds which are known per se and those which are new per se, which are prepared by methods known per se.
• the compounds which may be present in salt form are new per se, including those of the formula or correspond in which R 1 is alkyl or alkenyl having 6 to 22, preferably 11 to 22, in particular 16 to 20 carbon atoms, the process for their preparation being characterized in that an amine of the formula wherein R 1 has the meaning given, with citraconic anhydride or the alcohol of the formula wherein Ri has the meanings given, is reacted with itaconic anhydride as a rule in approximately equimolar amounts.
• a polymeric, cationic retention agent (B) which generally has a molecular weight of at least about 1000, is always used in the paper sizing process according to the invention. preferably has about 2000 to about 2,000,000. Retention agents with molecular weights in the range of 10,000 to 100,000 are particularly preferred. In principle, any commercially available retention agent can be used in the process according to the invention.
• Examples of conventional retention agents (B) which are particularly suitable for use together with the sizing agent (A) in the paper sizing process according to the invention are polyalkyleneimines; Epihalohydrin adducts of reaction products of polyalkylene polyamines and aliphatic dicarboxylic acids; Epihalohydrin adducts of reaction products of polyalkylene polyamines, dicyandiamide and optionally unesterified or esterified with alkanols, organic dicarboxylic acids; Reaction products of dicyandiamide, formaldehyde, ammonium salts of strong inorganic acids and alkylene diamines or polyalkylene polyamines; cationically modified starches or carbohydrates from locust bean or guar gum; Copolymers based on polyamide amines and reaction products of epihalohydrins and polymerized diallylamines mentioned.
• epichlorohydrin adducts of reaction products from polyalkylene polyamines and aliphatic dicarboxylic acids are described, for example, in British patent specification 865 727, epichlorohydrin adducts from reaction products consisting of dicyandiamide and diethylenetriamine or triethylene tetramine, for example in German Offenlegungsschrift 2,710,061 and 486, Epin.
• Preferred cationically modified starches or carbohydrates from locust bean or guar gum are, for example, alkylene oxide adducts of these starches or carbohydrates, the alkylene oxide used having 2 or 3 carbon atoms in the alkylene radical and quaternary ammonium groups has or in particular represents, for example, a trimethylglycidylammmonium halide.
• Copolymers based on polyamide amines have molecular weights of 10 3 to 10 5 , preferably 10 3 to 10 '* and are made, for example, of aliphatic, saturated dicarboxylic acids having 2 to 10, preferably 3 to 6 carbon atoms, in particular adipic acid, and polyalkylene polyamines, for example Polypropylene and polyethylene polyamines, especially dimethylaminohydroxypropyldiethylenetriamine, are available. They are described, for example, in the CTFA Cosmetic Ingredient Dictionary, 3rd edition 1982, of the Cosmetic Toiletry and Fragrance Association. Reaction products from epihalohydrins and polymerized diallylamines preferably have molecular weights from 1000 to 2000 and are described, for example, in US Pat. Nos. 3,700,623 and 4,279,794.
• retention agents (B) which are in the foreground of interest for use together with the sizing agents (A) in the paper sizing process according to the invention, is a corn or potato starch modified with a quaternary ammonium group-containing propylene oxide, the 25% suspension of which in distilled water at 20 ° C has a pH of 4.2 to 4.6, a polyethyleneimine which has a molecular weight of 10,000 to 100,000, an epichlorohydrin adduct of a reaction product of triethylene tetramine and dicyandiamide, an epichlorohydrin adduct of a reaction product of diethylene triamine , Dicyandiamide and dimethyl adipate, a reaction product of dicyandiamide, formaldehyde, ammonium chloride and ethylenediamine, an epichlorohydrin adduct of a poly-N-methyldiallylamine and a copolymer of adipic acid and dimethylaminohydroxypropyl-
• the mass sizing of paper or cardboard is generally 0.02 to 3, preferably 0.05 to 3, in particular 0.1 to 0.8 percent by weight of the sizing agent (A) and 0.02 to 3, preferably 0.05 to 3, in particular 0.1 to 0.4 percent by weight of the retention agent (B), based in each case on dry matter at (A) and (B) and on the solids content of the fiber suspension.
• 0.02 to about 0.05 weight percent of the sizing agent means (A) and the retention aid (B) are only sufficient for the so-called “size press control", which cannot be determined with conventional sizing tests (see, for example, article “Control and Understanding of Size Press Pickup” by DR Dill in the magazine TAPPI ( Proceedings of the Technical Association of the Pulp and Paper Industry, Volume 57, No.
• the pulp suspension, to which the sizing agents (A) and the retention agents (B) are added, is shown in US Pat Usually a solids content of 0.1 to 5, preferably 0.3 to 3, in particular 0.3 to 1 percent by weight and a Schopper-Riegler freeness of about 10 ° to about 60 °, especially 20 to 60 °, preferably 20 to 45 °, in particular 25 to 35 °, It generally contains cellulose, in particular those made from softwood, for example pinewood, or made of hardwood, ie hardwood, for example beech wood, which, according to conventional processes, for example the sulfite or, above all, the sulfate process The fiber also contains toffsuspension, if necessary, sanded wood.
• Waste paper can also be contained in the fiber suspension.
• pulp suspensions made according to the so-called CMP or CTMP process Chemimechanical and chemithermomechanical pulping processes, see for example article “Developments in Refiner Mechanical Pulping” by SA Collicutt and co-workers in TAPPI, Volume 64, No. 6 from June 1981, pages 57 to 61) manufactured, come into consideration.
• the fiber suspension can also contain organic or mineral fillers.
• Organic fillers include synthetic pigments, e.g. Polycondensation products made of urea or melamine and forasldehyde with large specific surfaces, which are in highly dispersed form and e.g. in British Patent 043 937 and 1 318 244 are described as mineral fillers, among others, titanium dioxide, calcium sulfate and especially talc and / or chalk (calcium carbonate).
• the fiber suspension contains 0 to 40, preferably 5 to 25, in particular 15 to 20 percent by weight, based on the solids content of the fiber suspension, of dry matter of the fillers of the type specified.
• Fibrous suspensions containing no filler can be used in a wide pH range, e.g. 6.5 to 10.0, especially 7 to 10 are present. Fiber suspensions are preferred which, if appropriate by adding talc, especially calcium carbonate, especially chalk, have a pH of about 7 to about 9.
• the fibrous suspension can also contain additives such as e.g. Starch or its degradation products that increase fiber / fiber or fiber / filler bonding.
• High molecular weight polymers of the acrylic acid series e.g. Polyacrylamides with molecular weights of more than 1,000,000 can be added to the fiber suspension as an aid to retain the finest pulp fiber particles, with minimal amounts of about 0.005 to 0.02 percent by weight, based on the dry matter of the polymer and the solids content of the fiber suspensions, being sufficient.
• the fibrous suspension is processed further in a manner known per se on sheet formers or, preferably, continuously on paper machines of conventional design to give paper or cardboard. After drying at about 100 to 140 ° C. for about 0.5 to 10 minutes, papers with a variable basis weight of, for example, 50 to 200 g / m 2 are obtained.
• the aqueous composition for carrying out the paper sizing process according to the invention contains, in addition to optional customary additives, the sizing agent (A), provided that the sizing agent and the retention agent (B) are added separately to the fiber suspension.
• the preparation generally contains the sizing agent in whole or in part in the form of its salts (obtained using, for example, ammonia, an alkyl or alkanolamine or an alkali metal hydroxide of the type specified in the ratios given above).
• such compositions contain 5 to 30, preferably 5 to 20 percent by weight of dry matter of the sizing agent, which is at least partially in salt form, based on the weight of the aqueous composition.
• the aqueous compositions of the type mentioned may contain surface-active compounds as usual additives, e.g. Dispersants or further emulsifiers and / or water-soluble organic solvents.
• dispersants and emulsifiers are e.g. Conventional lignin sulfonates, lignin carboxylates, carboxymethyl cellulose, ethylene oxide adducts of alkylphenols, fatty amines, fatty alcohols or fatty acids, fatty acid esters of polyhydric alcohols, substituted benzimidazoles or condensation products from formaldehyde and aromatic sulfonic acids, especially naphthalenesulfonic acids.
• Further surface-active compounds are preferably the anionic surfactants, especially sulfate surfactants, e.g. Diethanolamine lauryl sulfate, sodium lauryl sulfate or ethoxylated lauryl sulfates.
• sulfate surfactants e.g. Diethanolamine lauryl sulfate, sodium lauryl sulfate or ethoxylated lauryl sulfates.
• Possible water-soluble organic solvents are aliphatic ethers with 1 to 10 carbon atoms, e.g. Dioxane, ethylene glycol n-butyl ether or diethylene glycol monobutyl ether or alcohols with 1 to 4 carbon atoms, e.g. Isopropanol, ethanol or methanol.
• the quantitative ratio (component (A)): (additives) in the composition is 1: 0.02 to 1: 0.3, preferably 1: 0.05 to 1: 0.1, based on the dry matter of the sizing agents and additives.
• compositions are prepared in a conventional manner by combining the sizing agent (A) together with the retention agent (B) or the sizing agent (A) usually partly in the form of its salt alone either in the molten state or preferably in the solid state, in particular in powdered form, usually in the presence of glass beads and, if necessary, emulsifiers (in the case of sizing agents in the molten state) or dispersants (in the case of sizing agents in powder form) at a maximum of 90 ° C, preferably about 50 to 85 ° C for emulsions, in particular about 15 up to about 25 ° C.
• dispersions with storage-stable, homogeneous, further dilutable emulsions or preferably dispersions being obtained.
• the sizing agents together with the retention aids or the sizing agents which are present entirely or at least partially as salts are generally self-dispersing or self-emulsifying, the use of dispersants or emulsifiers is generally not absolutely necessary. This also applies to the optional addition of solvents and / or surfactants, which are only used if the dispersions or emulsions have insufficient storage stability.
• a process for producing paper with a glued surface in which a glue liquor which contains the components (A) and (B) for example by spraying, preferably by padding, generally applied to the paper at room temperature (15-25 ° C.) and then the impregnated paper at 60 to 140 ° C., preferably 90 to 110 ° C. for 0.1 to 10, preferably Is dried for 2 to 6 minutes. After drying, a paper is obtained which has a surface application of sizing and retention agent from 50 to 150, preferably 60 to 120 mg / m 2 .
• the paper to be glued is any type of paper with any basis weight, for example paper and cardboard boxes made from bleached or unbleached sulfite or sulfate cellulose.
• the glue liquor required for this is prepared by diluting with water the emulsions or dispersions specified above which contain both the sizing agent (A) and the retention agent (B).
• the emulsions or dispersions are diluted so that a glue liquor is formed which (A) 0.02 to 0.4, preferably 0.05 to 3, in particular 0.05 to 1 percent by weight of sizing agent (calculated as dry matter), based on the total weight the aqueous glue liquor, the sizing agent optionally being in salt form, and (B) 0.01 to 0.2, preferably 0.05 to 0.1, in particular 0.3 to 0.8 percent by weight retention agent (calculated as dry substance) on the total weight of the aqueous glue liquor.
• pulp suspensions of the most varied types can be easily processed into paper in mass sizing with relatively particularly small amounts of sizing and retention agent, which has good sizing properties (alkali drop test, ink floating time and, above all, water absorption according to Cobb ) having.
• This also applies to surface sizing, where the good sizing effects can be achieved with only small amounts of sizing and retention agent.
• the low area applications enable a quick working process, so that good surface sizes can be achieved within 20 to 40 seconds at the drying temperature of 90 to 110 ° C, for example.
• the paper sized according to the process has good mechanical properties, ie good strengths, in particular good tear strength.
• wood pulp can be used for mass sizing Containing fibrous suspensions or those containing waste paper are processed.
• the compatibility of the sizing agent used according to the invention with various fillers such as chalk and also various additives of the type specified above is also advantageous.
• the sizing and retention agents used according to the invention have good compatibility with the customary auxiliaries, pigments, binders used in the paper industry, in particular optical brighteners and other additives.
• the sizing and retention agents used are easily accessible, inexpensive and do not tend to form undesirable foams.
• the degree of whiteness of the sized paper is not significantly influenced by the size and can even be improved in both the mass and the surface size under certain circumstances. Above all, the generally surprisingly high storage stability of the size dispersions of the type indicated is of great advantage.
• EXAMPLE 1 The procedure is as described in instruction A, but 11.2 parts of citraconic anhydride (0.1 mol) are used (instead of 9.6 parts of maleic anhydride). 34.6 parts of the compound of the formula (8) are obtained as white powder.
• EXAMPLE 2 The procedure is as described in instruction A, but 11.2 parts of itaconic anhydride (0.1 mol) and 27.0 parts of stearyl alcohol (0.1 mol) (instead of 9.8 parts of maleic anhydride and
• Examples 3 to 8 A pulp suspension of bleached birch sulfate pulp and pine sulfate pulp in a weight ratio of 1: 1 in water of 10 ° dH (German degrees of hardness), which has a Schopper-Riegler freeness of 35 ° and a solids content of 0.5%, is included 20% chalk as a filler and then with 0.01% PERCOL e 292 (cationic, high molecular weight (MW> 1 ⁇ 10 7 ) polyacrylamide) as an aid to retain the finest cellulose fiber particles, the pH value given in Table I below changing the Fibrous suspension sets.
• the percentages relate to dry matter of auxiliaries and fillers, based on the solids content of the fiber suspension.
• Formulations of the sizing agent are prepared by in each case 7% of the stated sizing agents in powder form, as are obtained in the production, with 3.5% each of POLYMIN @ P (polyethyleneimine with a molecular weight of 10,000 to 100,000) as the retention agent in the presence of deionized water and glass beads with a diameter of 2 mm at room temperature (15 to 25 ° C).
• POLYMIN @ P polyethyleneimine with a molecular weight of 10,000 to 100,000
• the dispersions obtained are pourable, homogeneous and stable in storage. The percentages indicate the dry matter content of sizing or retention agent, based on the total weight of the formulation.
• the aqueous formulation of the sizing agent and the retention agent is now added to the fiber suspension in such a way that the amount used is also given in Table I below Dry substance of the sizing agent, based on the solids content of the fiber suspension, arises.
• the fiber suspension is then processed in a laboratory sheet former "Formette Dynamique" from Allimand, Grenoble, France, to paper sheets which, after drying at 130 ° C. for 3 minutes, have a basis weight of 80 g / m 2 .
• Both surfaces of the paper sheets obtained ie the surface obtained on the screen side of the sheet former and the opposite or top side, are tested for their sizing properties.
• the water absorption according to Cobb is measured after 30 seconds of exposure (WA Cobb 30 ) according to DIN 53 132.
• the results of the WA Cobb 30 measurements in g / m 2 of the sieve side (SS) and top side (OS) after drying at 130 ° C and after storage for one day at 23 ° C and a relative humidity of 50% are in given in Table I below.
• WA Cobb 30 values over 100 correspond to a completely unsatisfactory sizing of the paper.
• POSAMYL e E7 (cationically modified starch with a nitrogen content of 0.4%), a native potato starch cationically modified with trimethylglycidylammonium chloride, the nitrogen content of which is 1.3%, a condensation product of dicyandiamide and triethylene tetramine, the further reacted with epichlorohydrin and produced, for example, according to Example 2 of German Offenlegungsschrift 2,710,061, an epichlorohydran adduct of a reaction product of diethylenediamine and adipic acid, which is produced, for example, according to Example 1 of British Patent 865 727, a reaction product of dicyandiamide, formaldehyde, ammonium chloride and ethylenediamine , for example according to Beis 1 of US Pat.
• Examples 9 to 15 The procedure is as given in Examples 5 to 8, but the sizing agent and the retention agent are added separately to the fiber suspension, the stated amount (in%) of sizing agent in powder form at room temperature (15 to 25 ° C.) in the presence of water and glass beads with an aqueous, 5% ammonia solution to a self-emulsifying, also pourable, homogeneous and storage-stable emulsion and the formulations of the sizing agent given in Table II below are formed.
• the Val% indicated mean the number of equivalents of ammonia for 100 equivalents, based on the number of acidic groups present in the sizes used.
• the fiber suspension is mixed with the specified amount of dry substance of the sizing agent, the amount of sizing and retention agent being based on the solids content of the fiber suspension.
• the sizing results are also shown in Table II. When using 10 to 300 val% ammonia or sodium hydroxide (as a 5% aqueous solution) for the formulation of the sizing agent, similarly good sizing results are obtained as those given in Table II.

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• 1985
  • 1985-09-09 EP EP85810409A patent/EP0176479A1/de not_active Withdrawn
  • 1985-09-11 FI FI853476A patent/FI853476L/fi not_active IP Right Cessation
  • 1985-09-12 ZA ZA856982A patent/ZA856982B/xx unknown
  • 1985-09-12 NO NO853576A patent/NO853576L/no unknown
  • 1985-09-12 DK DK415085A patent/DK415085A/da not_active Application Discontinuation
  • 1985-09-12 ES ES546899A patent/ES8801953A1/es not_active Expired
  • 1985-09-12 AU AU47394/85A patent/AU4739485A/en not_active Abandoned
  • 1985-09-12 BR BR8504416A patent/BR8504416A/pt not_active IP Right Cessation
  • 1985-09-13 JP JP60203243A patent/JPS6170096A/ja active Pending

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