Classifications

• • C—CHEMISTRY; METALLURGY
  • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
  • C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
  • C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
  • C11D3/02—Inorganic compounds ; Elemental compounds
  • C11D3/12—Water-insoluble compounds
  • C11D3/124—Silicon containing, e.g. silica, silex, quartz or glass beads
  • C11D3/1246—Silicates, e.g. diatomaceous earth
  • C11D3/1253—Layer silicates, e.g. talcum, kaolin, clay, bentonite, smectite, montmorillonite, hectorite or attapulgite
  • C11D3/1273—Crystalline layered silicates of type NaMeSixO2x+1YH2O

Definitions

• the invention relates to improved builder compositions Solvent residue behavior, obtainable by contacting crystalline layered sodium disilicate and water as well as subsequent Heat treating the builder compositions thus obtained.
• the object of the present invention was to provide a builder composition to provide improved release residue behavior.
• EP 0 650 926 describes the roll compaction of crystalline layered Sodium disilicate by roll compaction with the addition of hardening agents such as Water, silica sol, silica gel, surfactants, water glass, maleic acid-acrylic acid polymers and other copolymers.
• hardening agents such as Water, silica sol, silica gel, surfactants, water glass, maleic acid-acrylic acid polymers and other copolymers.
• the goal is to produce a counter mechanical abrasion resistant granules.
• the granulation itself takes place at 15 up to 130 ° C.
• the compacted material is not preheated because the temperature alone due to the mechanical friction between the compacted material and the compacting rollers is achieved.
• the dwell time of the compacted material in the roller compactor, the Formation of the flakes and the comminution to the granulate moves overall in the range of fractions of a second to a few seconds.
• builder compositions are based on Based on crystalline layered sodium silicate, which are obtainable by that you can crystalline layered sodium silicate with water or aqueous Solutions of detergent ingredients in a certain relationship with each other in contact and subsequently the Bullder compositions thus obtained heat treated, show an improved release residue behavior.
• the sodium silicates a) are preferably those with x values of 2, 3 or 4. Sodium disilicate Na 2 Si 2 O 5 * yH 2 O with x equal to 2 are particularly preferred.
• the sodium silicates a) can also be are mixtures.
• Crystalline layered sodium disilicate a) is composed of changing percentages of the polymorphic phases alpha, beta, delta and epsilon. Commercial products can also contain amorphous components. With the latter, x can also be non-even in commercial products. 1.9 x x 2,2 2.2 is preferred.
• Preferred crystalline layered sodium silicates a) contain 0 to 40% by weight of alpha sodium disilicate, 0 to 40% by weight of beta sodium disilicate, 40 to 100% by weight of delta sodium disilicate and 0 to 40% by weight of amorphous fractions.
• Particularly preferred crystalline layered sodium silicates a) contain 7 to 21% by weight alpha-sodium disilicate, 0 to 12% by weight beta-sodium disilicate, 65 to 95% by weight of delta sodium disilicate and 0 to 20% by weight of amorphous parts. Crystalline layered sodium silicates a) with a Content of 80 to 100 wt .-% delta sodium disilicate.
• crystalline ones can also be used layered sodium silicates a) with a content of 70 to 100 wt .-% beta-sodium disilicate be used.
• alpha-sodium dislicicate corresponds to the Na-SKS-5 described in EP-B-0 164 514, characterized by the X-ray diffraction data shown there, which are assigned to the alpha-Na 2 Si 2 O 5 , the X-ray diffraction diagrams of the Joint Committee of Powder Diffraction standards are registered under numbers 18-1241, 22-1397, 22-1397A, 19-1233, 19-1234 and 19-1237.
• the above-mentioned beta-sodium disilicate corresponds to Na-SKS-7 described in EP-B-0 164 514, characterized by the X-ray diffraction data shown there, which are assigned to beta-Na 2 Si 2 O 5 , the X-ray diffraction diagrams of the Joint Committee of Powder Diffraction standards are registered under numbers 24-1123 and 29-1261.
• the aforementioned delta sodium disilicate corresponds to the Na-SKS-6 described in EP-B-0 164 514, characterized by the X-ray diffraction data shown there, which are assigned to the delta-Na 2 Si 2 O 5 , the X-ray diffraction diagrams of the Joint Committee of Powder Diffraction standards are registered under number 22-1396.
• the crystalline layered sodium silicates a) additionally contain cationic and / or anionic constituents.
• the cationic constituents are preferably alkali metal ions and / or alkaline earth metal cations and / or Fe, W, Mo, Ta, Pb, Al, Zn, Ti, V, Cr, Mn, Co and / or Ni.
• the anionic constituents are preferably aluminates, sulfates,
• Fluorides chlorides, bromides, iodides, carbonates, hydrogen carbonates, nitrates, Oxide hydrates, phosphates and / or borates.
• the crystalline layered sodium silicates a based on the total SiO 2 content, contain up to 10 mol% boron.
• the crystalline layered sodium silicates a based on the total content of SiO 2 , contain up to 20 mol% of phosphorus.
• the crystalline layered sodium silicate a) is preferred as a powder with a average particle size of 0.1 to 4000 ⁇ m, particularly preferably 10 to 500 ⁇ m, particularly preferably 20 to 200 microns, used.
• Suitable water for component b) are, for example Tap water, Condensed water (condensate), water vapor, demineralized water, Process water (if not too heavily contaminated) etc.
• the water can also be in the form of aqueous solutions or dispersions of Detergent ingredients are used. Suitable as detergent ingredients all common detergent ingredients and mixtures thereof.
• Suitable as detergent ingredients all common detergent ingredients and mixtures thereof.
• by using such solutions or Dispersions achieve secondary advantages. So in the case of aqueous solutions of alkali silicates, polyethylene glycols and long-chain alkyl ethoxylates hardening of the granules can be achieved; in the case of dyes one Coloring of the granules.
• Suitable detergent ingredients c) are preferably the substances described later in connection with the detergents and cleaning agents containing the builder composition.
• Alkali silicates, nonionic surfactants, anionic surfactants, cationic surfactants, polycarboxylate polymers, polycarboxylate copolymers, polyethylene glycols, bentonites, hectorites, saponites and / or dyes are particularly preferred as detergent ingredients c).
• the nonionic surfactants are preferably alkyl alkoxylates, Gluconamides, alkyl polyglycosides and / or amine oxides. Particularly preferred nonionic surfactants are those in connection with the washing and Detergents containing the builder composition described later.
• Preferred anionic surfactants are carboxylates, sulfonates and sulfates, particularly preferably (C 9 -C 13 ) alkylbenzenesulfonates, alpha-olefin sulfonates, alkanesulfonates, esters of sulfofatty acids, disalts of alpha-sulfofatty acids, sulfuric acid monoesters of (C 12 -C 18 ) fatty alcohols and Soap.
• Particularly preferred anionic surfactants are those described later in connection with the washing and cleaning agents containing the builder composition.
• Preferred polycarboxylate polymers and copolymers are copolymers of acrylic acid and maleic anhydride or their alkali metal salts, preferably the sodium and potassium salts.
• the molecular weight of the homopolymers is preferably in the range from 1,000 to 100,000 g / mol.
• the molecular weight of the copolymers is preferably in the range from 2,000 to 200,000 g / mol, particularly preferably 50,000 to 120,000 g / mol.
• Acrylic acid / maleic acid copolymers with a molecular weight of 50,000 to 100,000 g / mol are particularly preferred.
• Copolymers of acrylic acid or methacrylic acid with vinyl ethers such as, for example, vinyl methyl ether, vinyl esters, ethylene, propylene and styrene, are also preferred.
• Commercial products are, for example, ®Sokalan CP 5 and PA 30 from BASF, ®Alcosperse 175 or 177 from Alco and LMW 45 N and SPO2 N from Norsohaas.
• Preferred cationic surfactants are quaternary (C 6 -C 16 ) -N-, preferably (C 6 -C 10 ) -N, alkyl and alkenyl ammonium compounds, in which the remaining N positions are methyl, hydroxyethyl and / or Hydroxypropyl groups are substituted.
• Particularly preferred cationic surfactants are those described later in connection with the detergents and cleaning agents containing the builder composition.
• Preferred polyethylene glycols are those with a molecular weight of 1000 to 10000 g / mol, particularly preferably 2000 to 8000 g / mol.
• Preferred bentonites, hectorites and saponites are montmorillonites with the formula Na x [Al 4-x Mg x (OH) Si 4 O 10 ] * nH 2 O with 0.1 x x 0,4 0.4 and 0 n n 20 20, preferably x approx. 0.33 and n approx.
• Preferred dyes are oxidation-stable dyes and / or pigments, particularly preferably the ®Sandolan types (S. Blau E-HRL 180, S. NBG 125 (brilliant red), S. MFBL (green)) or also ®Vitasin types (V. ponceau 4RC82 (red), V. quinoline yellow 70 (yellow) and ®Telon types (Telon Blau AFN, DyStar textile dyes), also pigments such as ®Patentblau (DyStar), ®Unisperse types or ®Terasil-T- Types (both from Ciba) can be used, and the dyes can be used as solutions or dispersions.
• ®Sandolan types S. Blau E-HRL 180, S. NBG 125 (brilliant red), S. MFBL (green)
• ®Vitasin types V. ponceau 4RC82 (red
• V. quinoline yellow 70 yellow
• the concentration of the respective detergent ingredients in the aqueous solutions or dispersions also depends on the manageability (pumpability, flowability, storage stability, etc.) of the respective solution or dispersion. Any concentration is possible within the limits of the ratio c) according to the invention of the crystalline layered sodium silicate a) to the water from component b).
• the weight ratio of the crystalline layered sodium silicate a) to the detergent ingredients is preferably 5: 1 to 1000: 1, particularly preferably 7: 1 to 200: 1, particularly preferably 10: 1 to 100: 1.
• the molar ratio c) of the crystalline layered sodium silicate a) to the water from component b) is preferably 1: 1 to 20: 1, particularly preferably 1: 1 to 10: 1 and particularly preferably 1.2: 1 to 5: 1.
• the contacting of components a) and b) can be done by all methods take place, which ensure sufficient contact of the components.
• Mixing, spraying and spraying techniques are preferred, particularly preferred Mixing techniques.
• Preferred mixers are paddle, ring layer or Ploughshare mixer e.g. from Lödige, free fall mixers, e.g. from Telschig, Eirich mixers, Schugi mixers, fluidized bed mixers and drum mixers.
• the mixing times are preferably 0.5 s to 60 min, particularly preferably 2 s to 15 min.
• Component b) can also be brought into contact with the crystalline layered sodium silicate a) in the gas, vapor or aerosol state.
• Components a) and b) can be brought into contact at ambient temperature, but also at elevated temperature. Temperatures of 0 to 300 ° C. are preferred, particularly preferably 10 to 200 ° C. The heat can be brought in by external heating. If necessary, all components or only a few can be preheated.
• the heat treatment is preferably carried out at temperatures between 40 and 300 ° C. particularly preferably 60 to 200 ° C, particularly preferably 70 to 150 ° C.
• the duration of the heat treatment is preferably 2 to 1000 minutes, especially preferably 2 to 120 min, particularly preferably 10 to 120 min.
• the water vapor partial pressure during the heat treatment is preferred 10 mbar to 10 bar, particularly preferably 250 mbar to 3 bar.
• Preferred apparatus for the heat treatment are fluidized beds, belt and Tunnel kilns, flight promotions and storage containers.
• Preferred apparatus for this are paddle, ring bed or ploughshare mixers, e.g. from Lödige, free fall mixers, e.g. from Telschig, Eyrich-Mixer, Nauta-Mixer and drum mixer.
• the contacting takes place and separately heat treating the builder composition Apparatuses. This can be batchwise batchwise or preferably continuously respectively. In another embodiment, the contacting and the Heat treatment carried out in one apparatus, also continuously can be worked.
• the builder composition obtained after bringing components a) and b) into contact is further mechanically treated.
• Preferred mechanical further treatments are compacting, granulating, grinding, crushing and / or grain fractionation.
• the mechanical further treatment as a whole or in partial steps can take place before and after the heat treatment. Multiple heat treatments at different process stages are also within the meaning of the invention.
• components a) and b) are first brought into contact, then heat-treated and finally mechanically treated.
• the components are particularly preferably brought into contact first, then heat-treated, then compacted, then ground / crushed and finally fractionated by grains.
• the components are also particularly preferably brought into contact first, then heat-treated, then ground and finally fractionated by means of grains.
• components a) and b) are first brought into contact, then mechanically treated and finally heat-treated.
• the components are particularly preferably brought into contact first, then compacted, then ground, then fractionated and finally heat-treated.
• the compacting serves to enlarge the grain (grain build-up). It differs from agglomeration in two ways.
• a binder does not necessarily have to be used for compacting, which is essential for agglomeration.
• the powder to be compacted is not only pressed together by the acting pressure and the grains hooked into one another, but rather powder grains are also crushed against one another.
• the compacting is preferably press granulation, such as roll compacting or briquetting, particularly preferably roll compacting.
• the temperature of the material during the compacting is preferably between 10 and 200 ° C., the desired temperature being able to be controlled by external heating / cooling or by the frictional heat being released by itself.
• the dwell time under pressure is only a few fractions of a second until the resulting scraps are crushed with mills of the relevant type and, if necessary, grain fractionated.
• the duration of the heating is thus much shorter than in the targeted heat treatment according to the invention and is therefore too short for an improvement in the dissolving residue behavior.
• the scraps formed in the roll compacting are immediately comminuted with mills of the relevant type and, if necessary, grain fractionated.
• the good grain is discharged from the grain fractionation and undersize and oversize are returned to the compactor or the mills in the sense of circulating currents.
• the duration of the heating is much shorter than in the case of the targeted heat treatment.
• Roll compacting is preferably carried out with a line pressing force of 2 to 200 kN / cm roll width, particularly preferably 10 to 160 kN / cm roll width, and at a temperature of 20 to 200 ° C.
• a line pressing force of 2 to 200 kN / cm roll width, particularly preferably 10 to 160 kN / cm roll width, and at a temperature of 20 to 200 ° C.
• Suitable roll compactors are, for example, those from the companies Hosokawa-Bepex and Alexanderwerk.
• the grinding serves to reduce the grain size of powders and pressed granules and the shredding of flakes.
• the grain fractionation classifies the regrind into oversize, undersize, undersize, preferably by screening and / or screening. Screening is particularly preferred. Suitable sieves are e.g. those of the companies Rhewum, Locker or Allgeier.
• the builder composition according to the invention is preferably around a powder with an average particle size of 0.1 to 4000 ⁇ m, especially preferably 10 to 500 ⁇ m, particularly preferably 20 to 200 ⁇ m.
• the Builder composition according to the invention ⁇ m granules with a medium Particle size of 200 to 2000 microns, preferably 400 to 900 microns.
• the builder composition according to the invention is likewise preferably a ground granulate with an average particle size from 0.1 to 300 ⁇ m, preferably 10 to 200 ⁇ m.
• the builder compositions according to the invention are therefore preferred characterized in that the dissolving residue of an aqueous 0.25 wt .-% solution, at 20 ° C and after stirring for 20 minutes, less than or equal to 50%, preferably less than or is equal to 30%.
• the invention also relates to detergents and cleaning agents containing at least one builder composition according to the invention.
• the detergents are preferably heavy-duty detergents, compact heavy-duty detergents, compact color detergents, heavy-duty detergents with low bulk density, special detergents, such as stain salts, bleach boosters, curtain detergents, wool detergents, modular detergents and commercial detergents.
• the cleaning agents are preferably machine dishwashing detergents and machine dishwashing detergents. Silicates are particularly in demand here because of their good dirt dispersion, their high alkalinity and because of their protective effect on the glass. Glass damage means both the formation of layered deposits on glasses and the erosion of the glass surface - both of which lead to the known undesirable clouding of glasses.
• Special detergents and cleaning agents contain 1 to 50% by weight of the builder composition according to the invention, for example heavy duty detergents, color detergents, water softeners and stain salts, or 60 to 100% by weight of the same, for example modular detergent systems.
• Other special detergents and cleaning agents for example machine dishwashing detergents, contain 0.5 to 30% by weight of the builder composition according to the invention.
• the cobuilders are preferably crystalline aluminosilicates, mono-, oligo- or polymeric or copolymeric carboxylic acids, alkali ortho-, alkali-pyro- and Alkali polyphosphates, crystalline layered silicates, crystalline alkali silicates without Layer structure and / or X-ray amorphous alkali silicates.
• the bleaching systems are preferably active chlorine carriers and / or organic or inorganic active oxygen carriers (e.g. perborates, percarbonates, Percarboxylic acids, etc.), bleach activators (e.g. TAED), bleach catalysts (e.g. according to DE 199 13 995, WO 98/23531, WO 00/36061), enzymes for removing Discoloration, etc.
• active chlorine carriers e.g. perborates, percarbonates, Percarboxylic acids, etc.
• bleach activators e.g. TAED
• bleach catalysts e.g. according to DE 199 13 995, WO 98/23531, WO 00/36061
• enzymes for removing Discoloration etc.
• the surface-active substances are preferably anionic, cationic, non-ionic and / or zwitterionic surfactants.
• Alkyl alkoxylates, alkyl ester alkoxylates and gluconamides are nonionic surfactants and / or alkyl polyglycosides are particularly preferred.
• alkyl alkoxylates preference is given to using ethoxylated alcohols, preferably primary alcohols, preferably having 8 to 22 carbon atoms and preferably 1 to 80 EO units per mole of alcohol, the alcohol radical being linearly or preferably 2-methyl-branched or linear and methyl-branched Contains residues in the mixture, as is usually the case in oxo alcohol residues.
• ethoxylated alcohols preferably primary alcohols, preferably having 8 to 22 carbon atoms and preferably 1 to 80 EO units per mole of alcohol, the alcohol radical being linearly or preferably 2-methyl-branched or linear and methyl-branched Contains residues in the mixture, as is usually the case in oxo alcohol residues.
• the preferred ethoxylated alcohols include, for example, C 11 alcohols with 3, 5, 7, 8 and 11 EO units, (C 12 -C 15 ) alcohols with 3, 6, 7, 8, 10 and 13 EO units, (C 14 -C 15 ) alcohols with 4, 7 and 8 EO units, (C 16 -C 18 ) alcohols with 8, 11, 15, 20, 25, 50 and 80 EO units and mixtures thereof.
• the degrees of ethoxylation given represent statistical averages, which can be an integer or a fraction for a specific product.
• fatty alcohol EO / PO adducts can also be used, such as the ®Genapol types 3970, 2909 and 2822 from Clariant GmbH.
• R 2 CO-N (R 3 ) -Z polyhydroxy fatty acid amides of the formula R 2 CO-N (R 3 ) -Z, in which R 2 CO for an aliphatic acyl radical having 6 to 22 carbon atoms, R 3 for hydrogen, an alkyl or hydroxyalkyl radical with 1 to 4 carbon atoms and Z represents a linear or branched polyhydroxyalkyl radical having 3 to 10 carbon atoms and 3 to 10 hydroxyl groups.
• Alkyl glycosides of the general formula RO (G) x are preferably used, where R is a primary straight-chain or methyl-branched, in particular methyl-branched, aliphatic radical having 8 to 22, preferably 12 to 18 carbon atoms and G is a glycose unit with 5 or 6 carbon atoms, preferably for glucose.
• the degree of oligomerization x which indicates the distribution of monoglycosides and oligoglycosides, is preferably a number between 1 and 10, particularly preferably x is between 1.2 and 1.4.
• Preferred anionic surfactants of the sulfonate type are the known (C 9 -C 13 ) alkylbenzenesulfonates, alpha-olefin sulfonates and alkanesulfonates. Esters of sulfo fatty acids or the disalts of alpha sulfo fatty acids are also suitable.
• Suitable anionic surfactants are sulfonated fatty acid glycerol esters, which are mono-, di- and triesters and their mixtures, such as those produced by esterification by 1 mol of monoglycerol with 1 to 3 mol of fatty acid or in the transesterification of triglycerides with 0.3 to 2 Moles of glycerol can be obtained.
• alkyl sulfates are the sulfuric acid monoesters of the (C 12 -C 18 ) fatty alcohols, such as lauryl, myristyl, cetyl or stearyl alcohol and the fatty alcohol mixtures obtained from coconut oil, palm and palm kernel oil, which also contain fractions of unsaturated alcohols, for example oleyl alcohol, can contain. Soaps are particularly suitable as further anionic surfactants. Saturated fatty acid soaps are suitable, such as the salts of lauric acid, myristic acid, palmitic acid, stearic acid, hydrogenated erucic acid and behenic acid, and in particular those soap mixtures derived from natural fatty acids, such as coconut, palm kernel or tallow fatty acids.
• the anionic surfactants can be in the form of their sodium, potassium or ammonium salts, and also as soluble salts of organic bases, such as mono-, di- or triethanolamine.
• the anionic surfactants are preferably in the form of their sodium or potassium salts, in particular in the form of the sodium salts.
• the pH regulators are preferably soda, trona, potash, citric acid, sodium citrate and / or bicarbonate.
• detergents and cleaning agents can optionally also contain enzymes, such as. Protease, amylase, lipase and cellulase.
• the invention also relates to components for modular detergent systems, which preferably 60 to 100 wt .-% of the builder composition according to the invention contain.
• Components a), b), c) and d) are preferably those listed above Connections used.
• the builder composition according to the invention can also expressly be used as Component for the production of compounds for detergents and cleaning agents, Water softener and modular detergent systems can be used.
• Compounds can achieve special effects.
• liquid Components in powder or tablet detergents and cleaning agents be incorporated.
• coloring or sprinkling of washing and cleaning agents possible. It can also be used for special Disintegration effects, better dispersion of difficult to disperse Achieve components or the porosity of tablets.
• the surfactants b) listed above are preferred as surfactants Connections used.
• Preferred polycarboxylate copolymers b) are those listed above Connections used.
• Preferred pH regulators b) are those listed above Connections used.
• the compounds are preferred as powders with an average particle size of 0.1 to 4000 ⁇ m, particularly preferably 10 to 500 ⁇ m, particularly preferably 20 up to 200 ⁇ m.
• the compounds are as Granules with an average particle size of 200 to 2000 microns, preferably 400 to 900 ⁇ m.
• the compounds are preferred either by agglomeration, grinding, Grain fractionation etc. or by compacting, grinding, grain fractionation etc. manufactured.
• the detergents, cleaning agents, water softeners and modular components can e.g. in powder, granule, gel, liquid or tablet form be used.
• the respective composition is pressed into the corresponding shape by means of a tablet press, the shape being able to take many forms (for example cylindrical, cuboid, elliptical, annular, etc.).
• the ratio of radius to height can be between 0.2 to 5.
• the pressure can be between 12 and 0.3 kN / cm 2 .
• the compression pressure is essentially independent of the geometric shape of the tablet.
• pressures of 0.7 to 14.2 kN / cm 2 are preferred, pressures of 2.8 to 10 kN / cm 2 are particularly preferred.
• Multistage pressing into more complex shapes is also preferred.
• the division into different compartments serves a certain separation of otherwise incompatible ingredients.
• any proportions of the formulation are pressed onto one another in several steps, so that several layers result.
• a layer thickness ratio of the two layers of 1:10 to 10: 1 is particularly preferred.
• Other forms of application are, for example, tablets with inserted spherical compartments.
• the different layers and compartments of the tablets can also be colored differently.
• the builder composition itself can also mixes with other builders, e.g. non-layered silicates, Zeolites, phosphates, etc. act.
• a ground solid sample was measured in a Philips PW1710 X-ray powder diffractometer (CuK alpha 2 radiation, wavelength 1.54439 Angstroms, acceleration voltage 35kV, heating current 28 mA, monochromator, Scanning speed 3 degrees 2 theta per minute).
• the measured intensities were evaluated as follows: substance characteristic peak (d-value in angstroms) Alpha phase 3.29 +/- 0.07, typically 3.31 Beta phase 2.97 +/- 0.06 Delta phase 3.97 +/- 0.08
• the crystalline proportions in percent by weight were calculated from the intensities I a , I b and I d - measured in pulses - of the alpha, beta and delta phase using the following formulas:
• Alpha content: A [%] 100 * I a / (I a + I b + I d )
• Beta-content: B [%] 1.41 * 100 * I b / (I a + I d )
• Delta content: D [%] 100 - A - D
• AM [%] (I at the -70) * 100/450
• the inserts with the desired screens were inserted into a Retsch screening machine.
• the mesh size of the sieves decreased from top to bottom.
• 50 g of the powder to be examined were placed on the widest sieve.
• the powder material was conveyed through the various sieves by the oscillating movement of the sieving machine.
• the residues on the sieves were balanced and calculated based on the weight of the material.
• the d 50 value could be calculated from the values.
• the optical brighteners were melted in a quarter of the amount Stirred alkyl ethoxylates and in a household multimixer (Braun) with the Half of the soda or bicarbonate or phosphate amount mixed.
• Ploughshare mixers from Lödige were the remaining soda and the total quantities on builder composition according to the invention, phosphate, zeolite, bicarbonate, Citric acid or polymer mixed for 15 minutes at 300 rpm. After that the Half of the remaining alkyl ethoxylate sprayed on in 5 minutes.
• alkanesulfonate, polyvinylpyrrolidone, alkylbenzenesulfonate, soap, antifoam, Phosphonate or compound with optical brightener added and Mixed for 10 minutes at 300 rpm.
• the mixture was in the tumble mixer from the Lödige mixer under low shear stress with percarbonate, perborate, TAED or enzymes added and mixed for 5 minutes.
• the detergent formulations were mixed and pressed into the appropriate shape using a Matra tablet press.
• the pressure was between 12 and 0.3 kN / cm 2 .
• the compacts had a height of approx. 18 mm and a diameter of 41 mm.
• the powder mixture from Example 2 was in a roll compactor at a Line pressing force of 90 kN / cm roll length processed. There were about 3 kg of good grain obtained from which the dissolving residue was determined (see Table 1).
• the heat-treated material from Example 5 was used in a roll compactor a line pressure of 90 kN / cm roll length processed. There were about 3 kg Good grain was obtained, from which the dissolving residue was determined (see Table 1).
• Example 7 8 kg of powder mixture were prepared in a drying cabinet Heat treated at 80 ° C for 30 min and in a roller compactor at one Line pressing force of 90 kN / cm roll length processed. There were about 3 kg of good grain obtained from which the dissolving residue was determined (see Table 1).
• Example 5 4 kg of the material from Example 5 were mixed with a ball mill for about 60 minutes U 280A0 from Welte, which is metal-lined on the inside and whose drum moves with it rotates approx. 50 rpm, ground. 44 kg of porcelain balls were used as grinding media used. The material had an average particle diameter of 63 microns and gave a residue of approx. 50%.
• Example 8 4 kg of the material from Example 8 were mixed with a ball mill for about 60 minutes U 280A0 from Welte, which is metal-lined on the inside and whose drum moves with it rotates approx. 50 rpm, ground. 44 kg of porcelain balls were used as grinding media used. The material had an average particle diameter of 55 microns and gave a solution residue of 7%.
• the Lödige was 5.6 kg in a ploughshare mixer Builder composition according to the invention from Example 7 with 2.4 kg Citric acid mixed to 8 kg powder mixture.
• the mixture was made in one Roll compactor processed at a pressure of 90 kN / cm roller width.
• a water softener formulation was used in the Lödige ploughshare mixer prepared according to Table 2 a, the solid components at 15 minutes 300 rpm were mixed. The alkyl ethoxylate was melted and under Mix sprayed on.
• Test detergent with the compositions given in Table 2 b manufactured.
• a stain salt formulation was used prepared according to Table 2 b, the solid components at 15 minutes 300 rpm were mixed. The alkanesulfonate was melted and under Mix sprayed on.
• Machine dishwashing detergent with the compositions according to Table 3 manufactured.
• a machine dishwashing gel with the one shown in Table 4 Composition was made in a dispersant (Ultraturrax, from Hanke and Kunkel) water glass, phosphate, soda, sodium hydroxide, Phosphonate, polymer, alkanesulfonate, phosphoric acid ester mixed together.
• a dispersant Ultraturrax, from Hanke and Kunkel
• phosphate soda
• sodium hydroxide sodium hydroxide
• Phosphonate polymer
• alkanesulfonate polymer
• phosphoric acid ester phosphoric acid ester

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• 2001
  • 2001-04-28 DE DE10121051A patent/DE10121051A1/de not_active Withdrawn
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