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
  • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
• • 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
  • C11D11/00—Special methods for preparing compositions containing mixtures of detergents
  • C11D11/02—Preparation in the form of powder by spray drying
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/66—Non-ionic compounds
  • C11D1/83—Mixtures of non-ionic with anionic compounds
• • 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
  • C11D17/00—Detergent materials or soaps characterised by their shape or physical properties
  • C11D17/06—Powder; Flakes; Free-flowing mixtures; Sheets
  • C11D17/065—High-density particulate detergent compositions
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/04—Carboxylic acids or salts thereof
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/02—Anionic compounds
  • C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
  • C11D1/22—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aromatic compounds
• • 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
  • C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
  • C11D1/66—Non-ionic compounds
  • C11D1/72—Ethers of polyoxyalkylene glycols

Definitions

• Spray-dried detergents of conventional compositions generally have bulk densities of 250 to 450 g / l (grams per liter) and, depending on the composition and method of operation, and only in exceptional cases of 480 g / l.
• powders with higher bulk densities for example from 550 to 750 g / l, have been of increasing interest since they require less packaging material and thus enable raw material to be saved and waste to be reduced.
• DE-A-25 48 639 teaches a process for increasing the bulk density of granulated or spray-dried detergents in a device which is known in the art under the name "Marumerizer” and is normally used to round off extruded particles of irregular shape.
• This device consists of a vertical cylinder with smooth side walls and a surface roughened turntable that rotates in the lower area of the cylinder.
• the device is primarily intended for intermittent operation.
• the largest available systems of this type with a diameter of the turntable of approx. 1 m can only take a batch of a maximum of 45 to 50 kg of tower powder.
• the compositions contain 4 to 20, preferably 5 to 15% by weight of at least one anionic surfactant from the class of soaps, sulfonates and sulfates.
• Suitable soaps are derived from natural or synthetic, saturated or monounsaturated fatty acids with 12 to 22 carbon atoms. Are particularly suitable from natural fatty acids such. B. coconut, palm kernel or tallow fatty acid derived soap mixtures. Preferred are those which are composed of 50 to 100% of saturated C12-18 fatty acid soaps and 0 to 50% of oleic acid soap. Their proportion is preferably 8 to 15% by weight, based on the composition.
• Usable surfactants of the sulfonate type are linear alkylbenzenesulfonates (C9 ⁇ 13-alkyl) and olefin sulfonates, ie mixtures of alkene and hydroxylalkanesulfonates as well as disulfonates, as can be obtained, for example, from C12 ⁇ 1inen monoolefins with a terminal or internal double bond by sulfonating with gaseous sulfur trioxide and subsequent receives alkaline hydrolysis of the sulfonation products.
• alkanesulfonates which can be obtained from C12 ⁇ 18 alkanes by sulfochlorination or sulfoxidation and subsequent hydrolysis or neutralization, and also alpha sulfonated hydrogenated coconut, palm kernel or tallow fatty acids and their methyl or ethyl esters and mixtures thereof.
• Suitable sulfate-type surfactants are the sulfuric acid monoesters from primary alcohols of natural and synthetic origin, i.e. from fatty alcohols, e.g. Coconut fatty alcohols, tallow fatty alcohols, oleyl alcohol, lauryl, myristyl, palmityl or stearyl alcohol, or the C10 ⁇ 18 oxo alcohols and the sulfuric acid esters of secondary alcohols of this chain length.
• the sulfuric acid monoesters of the primary alcohols or alkylphenols ethoxylated with 1 to 3 mol of ethylene oxide are also suitable.
• Sulfated fatty acid alkanolamides and sulfated fatty acid monoglycerides are also suitable.
• Surfactants containing sulfonate groups are preferred, and among these in turn the alkylbenzenesulfonates, alpha-sulfofatty acid ester salts and the alpha-sulfofatty acid ester disalts.
• the anionic surfactants are usually in the form of their sodium salts. Their proportion, based on the composition, is preferably 5 to 15% by weight.
• nonionic surfactants additive products of 2 to 20, preferably 3 to 15 moles of ethylene oxide (EO) with 1 mole of a compound having essentially 10 to 20, in particular 12 to 18, carbon atoms from the group of alcohols can be used as nonionic surfactants (component B).
• Suitable nonionic surfactants are derived from primary alcohols, for example coconut oil or tallow fatty alcohol, oleyl alcohol, oxo alcohol, or from secondary alcohols having 8 to 18, preferably 12 to 18, carbon atoms.
• Combinations of water-soluble nonionic surfactants (component B1) and water-insoluble or water-dispersible nonionic surfactants (component B2) are preferred used.
• Component B1 includes those with 6 to 15 EO and an HLB value of more than 11, component B2 those with 2 to 6 EO and an HLB value of 11 or less. It has proven to be advantageous to mix component B2 completely into the already spray-dried powder in the mixer. Component B1 can be sprayed in whole or in part, or can be added in whole or in part in the mixer.
• the nonionic surfactants can also have propylene glycol ether groups (PO). These can be arranged at the end or distributed statistically with the EO groups.
• Preferred compounds of this class are those of the type R- (PO) x - (EO) y , in which R is the hydrophobic radical, x are numbers from 0.5 to 3 and y numbers from 3 to 20.
• nonionic surfactants are ethoxylates of alkylphenols, 1,2-diols, fatty acids and fatty acid amides, and block polymers of polypropylene glycol and polyethylene glycol or alkoxylated alkylenediamines (Pluronics and Tetronics type). Furthermore, the above-described nonionic surfactants of the EO type can be partially replaced by alkyl polyglycosides. Suitable alkyl polyglycosides have, for example, a C8 ⁇ 16 alkyl radical and an oligomeric glycoside radical with 1.5 to 6 glucose groups. Alkyl glycoside type surfactants are preferably incorporated in the spray dried powder.
• the content of the agents in nonionic surfactants or nonionic surfactant mixtures is 2 to 15% by weight, preferably 3 to 12% by weight and in particular 4 to 10% by weight.
• Component (C) consists of finely crystalline, synthetic, water-containing zeolites of the NaA type, which have a calcium binding capacity in the range from 100 to 200 mg CaO / g (according to the information in DE 22 24 837). Their particle size is usually in the range from 1 to 10 ⁇ m.
• the content of these zeolites in the compositions is 10 to 40, preferably 15 to 35,% by weight. Most or all of the zeolite can be incorporated and sprayed into the spray mixture. It is more advantageous if part of it is added in powder form during the mixing process. This proportion can be up to 5% by weight, based on the composition. It is preferably 1 to 4% by weight. This procedure leads to a further increase in bulk density and at the same time improves the flow behavior of the agent.
• the zeolite is preferably used together with polyanionic co-builders. These include compounds from the class of polyphosphonic acids and homo- or copolymeric polycarboxylic acids, derived from acrylic acid, methacrylic acid, maleic acid and olefinic unsaturated, copolymerizable compounds.
• the preferred phosphonic acids or phosphonic acid salts are 1-hydroxyethane-1,1-diphosphonate, ethylenediaminetetramethylenephosphonate (EDTMP) and diethylenetriamine-pentamethylenephosphonate, mostly in the form of their sodium salts and their mixtures.
• the amounts used, calculated as free acid, are usually up to 1.5% by weight, based on the composition, preferably 0.1 to 0.8% by weight.
• aminopolycarboxylic acids in particular nitrilotriacetic acid, furthermore ethylenediaminetetraacetic acid, diethylenetriaminepentaacetic acid and their higher homologues. They are generally in the form of sodium salts. Their proportion can be up to 2% by weight, in the case of nitrilotriacetic acid up to 10% by weight.
• co-builders are homopolymers of acrylic acid and methacrylic acid, copolymers of acrylic acid with methacrylic acid and copolymers of acrylic acid, methacrylic acid or maleic acid with vinyl ethers, such as vinyl methyl ether or vinyl ethyl ether, furthermore with vinyl esters, such as vinyl acetate or vinyl propionate, acrylamide, methacrylamide and with ethylene, Propylene or styrene.
• vinyl ethers such as vinyl methyl ether or vinyl ethyl ether
• vinyl esters such as vinyl acetate or vinyl propionate
• acrylamide, methacrylamide and with ethylene, Propylene or styrene are particularly useful co-builders.
• the proportion thereof in the interest of sufficient water solubility is not more than 70 mole percent, preferably less than 60 mole percent.
• Copolymers of acrylic acid or methacrylic acid with maleic acid as are characterized, for example, in EP 25 551-B 1, have proven to be particularly suitable. These are copolymers which contain 50 to 90 percent by weight of acrylic acid. Copolymers in which 60 to 85 percent by weight acrylic acid and 40 to 15 percent by weight maleic acid are present and which have a molecular weight between 30,000 and 120,000 are particularly preferred.
• polyacetal carboxylic acids as described, for example, in US Pat. Nos. 4,144,226 and 4,146,495, which are obtained by polymerizing esters of glycolic acid, introducing stable terminal end groups, and saponifying to give the sodium or potassium salts.
• polymeric acids which are obtained by polymerizing acrolein and disproportionating the polymer according to Canizzaro using strong alkalis. You are essentially out Acrylic acid units and vinyl alcohol units or acrolein units built.
• the proportion of the (co) polymeric carboxylic acids or their salts, based on acid can be up to 8% by weight, preferably 1 to 6% by weight.
• the co-builders mentioned prevent the formation of fiber incrustations due to their complexing and retarding properties (so-called threshold effect) and improve the dirt-dissolving and dirt-dispersing properties of the agents.
• the agents are preferably phosphate-free.
• part of the zeolite and part of the co-builders can also be replaced by polyphosphates, in particular sodium tripolyphosphate (Na-TPP).
• Na-TPP sodium tripolyphosphate
• the content of Na-TPP should not be more than 25% by weight, preferably less than 20% by weight and in particular 0 to at most 5% by weight.
• the Na-TPP can also be sprayed via the spray mixture, partial hydrolysis to pyrophosphate and orthophosphate generally occurring. It may therefore be advantageous to add it in powder form to the mixer together with the sprayed powder and to process it together with it.
• the sodium silicate improves grain stability and Grain structure of the powdery or granular agents and has a favorable effect on the induction and dissolving behavior of the agents when entering washing machines. It also has an anti-corrosive effect and improves washability.
• Sodium carbonate the proportion of which is up to 15% by weight, preferably 2 to 12% by weight and in particular 5 to 10% by weight, is also suitable as further washing alkalis (component D).
• the total amount of sodium silicate and sodium carbonate is 4 to 20% by weight, preferably 5 to 10% by weight and in particular 7 to 12% by weight.
• the other constituents (component E), the proportion of which is 0 to 30% by weight, preferably 1 to 25% by weight, include graying inhibitors (dirt carriers), textile-softening substances, colorants and fragrances, and neutral salts, such as sodium sulfate and water.
• the agents can contain graying inhibitors which keep the dirt detached from the fibers suspended in the liquor and thus prevent graying.
• Cellulose ethers such as carboxymethyl cellulose, methyl cellulose, hydroxyalkyl celluloses and mixed ethers such as methyl hydroxyethyl cellulose are suitable. Methyl hydroxypropyl cellulose and methyl carboxymethyl cellulose. Mixtures of different cellulose ethers are also suitable, in particular mixtures of carboxymethyl cellulose and methyl cellulose or methyl hydroxyethyl cellulose. Their proportion is preferably 0.3 to 3% by weight.
• Suitable optical brighteners are alkali metal salts of 4,4-bis- (2 ⁇ -anilino-4 ⁇ -morpholino-1,3,4-triazinyl-6 ⁇ amino) -stilbene-2,2′-disulfonic acid or compounds of the same structure which wear a diethanolamino group instead of the morpholino group.
• Brighteners of the substituted diphenylstyryl type may also be used, e.g.
• synthetic layered silicates which, after suspension in water (16 ° dH, room temperature), have a swelling capacity - determined as the quotient of the sediment volume (V s ) / total volume (V) after previous treatment with excess soda solution, careful washing and 20 hours after slurrying in 9 parts by weight of water / one part by weight of layered silicate - of V s / V less than 0.6, in particular less than 0.4, as well as synthetic layered silicates, which are mixed crystalline and have structure-determining saponite and / or hectorite-like crystal phases, which are interspersed in an irregular arrangement with crystalline alkali polysilicate.
• Layered silicates of this type are characterized in more detail in DE 35 26 405.
• the layered silicate content can be, for example, 5 to 20% by weight.
• softening additives are long-chain fatty acid alkanolamides or dialkanolamides and reaction products of fatty acids or fatty acid diglycerides with 2-hydroxyethyl-ethylenediamine and quaternary ammonium salts, the 1 to 2 alkyl chains with 12-18 C atoms and 2 short-chain alkyl radicals or hydroxyalkyl radicals, preferably methyl radicals , contain.
• These softening additives are preferably added to the powder together with the nonionic surfactants in the mixer, for example in proportions of up to 10% by weight, preferably 0.5 to 5% by weight, based on the composition.
• the spray drying of the powders to be processed is carried out in a manner known per se by spraying a slurry under high pressure by means of nozzles and counter-sliding hot combustion gases in a drying tower.
• the spray-dried powder leaving the drying tower should have an initial density (liter weight) of at least 350 g / l in the interest of a desired high final density.
• the density of the is preferably Tower powder at least 400 g / l.
• Specifically light tower powders for example those containing zeolite, can be more densely compressed than those which already have a higher initial density, but overall they have a lower final weight than relatively heavy tower powders.
• the process can be used to process powders with a broad and narrow grain spectrum. It is also not necessary to previously screen out coarse fractions from the tower powder, as is the case with conventional powders. Rather, the process means that coarse parts are crushed, loose, voluminous components are compacted, irregularly shaped parts are rounded off and very fine parts are compacted. Overall, the process reduces the average grain size.
• the powders leaving the tower can be processed immediately in the manner according to the invention.
• the temperature of the powder is not critical per se, especially when it has dried thoroughly, ie when its water content corresponds to or is below the theoretical water-binding capacity.
• plastic in particular water-rich powders, however, it should not exceed 50 ° C., preferably 40 ° C., as is generally the case when the powder is conveyed pneumatically.
• the powder can also be stored for any length of time, but this generally only plays a role in the event of production interruptions.
• a continuous flow of material is always advantageous, for which the method according to the invention is particularly suitable due to the continuous mode of operation.
• the powder should be free-flowing and not sticky.
• Suitable salts are e.g. Sodium sulfate, soda or phosphates or polyphosphates, which can be mixed in proportions of up to 20% by weight, preferably up to 10% by weight.
• Suitable adsorbents are zeolite and finely divided silica. Preference is given to finely divided, i.e. zeolite NaA having a particle size of at most 10 ⁇ m is added in proportions of up to 4% by weight, preferably 0.5 to 3% by weight.
• the mixing device used to carry out the method consists of an elongated mixing drum of essentially cylindrical shape, which is mounted horizontally or moderately descending against the horizontal and is equipped with at least one filler neck or funnel and a discharge opening. Inside, there is a central, rotatable shaft that carries several radially aligned striking tools. When rotating, these should be at a certain distance from the smooth inner wall of the drum. The length of the striking tools should be 80% to 98%, preferably 85% to 95% of the inner radius of the mixing drum.
• the shape of the striking tools can be of any type, ie they can be straight or angled, of uniform cross-section or pointed, rounded or widened at their ends. Their cross-section can be circular or angular with rounded edges. Different shaped tools can also be combined. Those with a drop to wedge-shaped cross-section have proven successful, with a flat or rounded surface in the Direction of rotation points, since with such tools the compaction effect outweighs the crushing effect.
• the tools can be attached diametrically in pairs or in a star shape to the shaft to avoid imbalances. A spiral arrangement has proven to be advantageous. The number of tools is not critical, but it is advisable to arrange them at a distance of 5 to 25 cm in the interest of high efficiency.
• the conveying of the mixed material in the mixer can also be accomplished or accelerated by means of additional conveyor blades.
• These conveyor blades can be arranged individually or in pairs between the mixing tools.
• the degree of delivery can be regulated by the angle of attack of the blades.
• the inner radius of the mixer is, depending on the desired throughput, advantageously 10 to 60, preferably 15 to 50 cm, its inner length 70 to 400 cm, preferably 80 to 300 cm and the ratio of inner length to inner radius 4: 1 to 15: 1, preferably 5: 1 to 10: 1.
• the number of striking tools is usually 10 to 100, usually 20 to 80.
• the inner wall of the cylinder should be bare in order to avoid undesired sticking of the powder.
• the rotational speed of the shaft is lower than that Consideration of the Froude number above 800 rpm (revolutions per minute), usually between 1,000 and 3,000 rpm. With larger mixers it can be reduced accordingly.
• the residence time of the powder in the mixer depends on the performance of the system and the size of the desired effect. It should not be less than 10 seconds and not more than 60 seconds. It is preferably 20 to 50 seconds. It can be influenced by the inclination of the mixer, by the shape and arrangement of the striking and conveying tools and, to a certain extent, also by the amount of the powder supplied and removed. By reducing the initial cross-section, a certain back pressure and thus an increase in the residence time in the mixer can be achieved.
• the mixer should be operated in such a way that a constant powder throughput takes place after the start-up time, i.e. that the amount of powder fed in and taken out is the same and constant at all times.
• the Froude number should be 50 to 1,200, preferably 100 to 800 and in particular 250 to 500.
• the powder may heat up slightly as a result of mechanical processing. However, additional cooling is generally unnecessary or is only required if the supplied Powder tends to stick at elevated temperature. However, this problem can advantageously be solved by cooling the tower powder sufficiently beforehand, for example in the case of pneumatic conveying.
• the nonionic surfactant is fed into the mixer in the area in which intensive mechanical processing of the powder takes place. It has proven to be advantageous to arrange the feeds in the mixer wall.
• the otherwise generally customary arrangement of short spray nozzles in the hollow rotating shaft makes it necessary to use spray nozzles at low rotational speeds which work with excess pressure or are operated according to the principle of the perfume atomizer with compressed air. This method of operation also requires expenditure for pressure pumps or dust extraction systems for the compressed air discharged from the mixer.
• the arrangement in the mixer wall does not require comparable investments.
• the supplied nonionic surfactant can spread on the inner wall and is constantly absorbed, distributed and adsorbed by the powder hitting the wall.
• the outlet nozzles arranged on the hollow shaft are advantageously extended to such an extent that they protrude into the powder stream. Due to the increased centrifugal forces, this enables compressed air-free conveying and atomization of the nonionic surfactant, which is then distributed and absorbed by the powder stream.
• the number of feeds is expediently from 1 to 10, with an arrangement in the cylinder wall preferably being arranged laterally in the region of the rising powder stream. If there are several feeders arranged one behind the other, the last one should be installed so far in front of the outlet opening that the emerging nonionic surfactant is still homogeneously distributed.
• the nonionic surfactant is supplied in liquid form. High-melting compounds are melted beforehand and fed in at temperatures above the melting point.
• the moving powder also expediently has a minimum temperature which is in the range of the melting point of the nonionic surfactant or above. This temperature range can be easily adjusted by a suitable product guide after the spray drying.
• the nonionic surfactant can be introduced into the powder in this way. It is also possible to add a part of it to the spray batch and only enter the rest via the mixer. Basically, however, surfactants with a low degree of ethoxylation (low HLB value corresponding to component B2) should only be incorporated via the mixer.
• the proportion which is introduced via the tower spray powder should not exceed 50% by weight, based on nonionic surfactant.
• 0.5 to 6% by weight, in particular 1 to 5% by weight, of the nonionic surfactant contained in the agent is introduced via the mixer.
• the powder entered is taken away by the rotating striking tools and hits the inner wall of the mixer without sticking to it, even if it is in the meantime a thin film of nonionic surfactants is covered. This film is constantly removed by the lively powder and adsorbed on it. At most, a thin powder coating is formed, which is constantly renewed and the bare inner surface of the mixer can be seen again and again.
• the powder particles thus describe a spiral movement from the mixer inlet to the mixer outlet. If the powder adheres to the inner wall for a long time, so that a layer of powder forms that has to be scraped off by the rotating tools, the powder is too moist or too sticky or too warm or the locally metered amount of nonionic surfactant is too high. This non-stationary condition causes the mix to heat up excessively and the mixer to settle. One can counteract the formation of such deposits by the described addition of adsorbents.
• the products obtained have a bulk density increased by 50 to 200 g / l compared to the tower powder used, are extremely free-flowing and do not require any aftertreatment, in particular no post-drying and no sieving of enlarged or lumpy agglomerates. You can therefore immediately after leaving the mixer, if necessary after adding other powder components such as bleach (e.g. sodium perborate as monohydrate or tetrahydrate), bleach activators (e.g. granulated tetraacetylethylene diamine), enzyme granules, defoamers (e.g. silicone or paraffin defoamers applied to carrier material), be filled directly into the shipping container.
• bleach e.g. sodium perborate as monohydrate or tetrahydrate
• bleach activators e.g. granulated tetraacetylethylene diamine
• enzyme granules e.g. silicone or paraffin defoamers applied to carrier material
• a horizontally arranged mixer was used, the cylindrical interior of which had a radius of 15 cm and an inner length of 125 cm.
• inlet area length 30 cm
• several conveyor blades were arranged spirally on the inner shaft.
• 5 tapered, angled at their ends and then 25 additional mixing tools were spirally attached to the inner shaft, the latter having a wedge-shaped cross-section with rounded corners.
• the distance between the tools and the inside wall of the cylinder was 0.5 cm, which resulted in a ratio of tool length from the central axis to the inside wall of the mixer of 96.7% of the inside radius.
• inclined conveying blades total number 10 were installed in a spiral arrangement between the mixing tools.
• a total of 4 feeds (diameter approx. 10 mm) were arranged at a mutual distance of 10 cm in the first third of the mixing section laterally in the area of the rising powder stream, via which the nonionic component (b) was fed into the mixer.
• the size of the outflow opening at the outlet end of the mixer could be regulated by means of a flap. In the following Examples 1 to 4, this flap was set so that a slight back pressure and thus a uniform filling state formed in the mixer during continuous operation.
• the rotational speed was approximately 1,500 rpm and the average residence time was 20 to 60 seconds, on average 30 to 40 seconds spray-dried powder, which was transported via a pneumatic conveyor system after leaving the tower discharge and had a temperature of approx. 30 ° C or after an intermediate storage of 20 to 25 ° C.
• composition of the powder, the Froude number and the throughput in tons per hour (t / h) as well as the liter weight before and after the treatment can be found in Table I.
• Example 1 the components a and d - m as well as the water and the main part of the sodium sulfate (component n) were used for the tower spray powder.
• the nonionic surfactant (component b) heated to 45 ° C., was introduced into the mixer by means of the side feeds.
• a mixture of component b and the main amount (2% by weight) of component c was fed in in the same way.
• the rest of component c (0.3% by weight) was contained in the tower powder.
• the remainder of the sodium sulfate and the minor constituents served as a granulation base and as coating substances for the constituents listed under p to r. These were subsequently mixed with the perborate (which had been sprayed with the perfume) into the treated powder.
• the bulk density of the finished mixture A obtained in this way is also given (in each case in g / liter).
• Example 4 43 parts by weight of tower powder, comprising components a, c, d, g, h, i, k and l, as well as 52% of component e and 74% of component f with 2 parts by weight of component b im Mixer processed according to the manner given in Examples 1-3.
• the remaining parts of components e and f and parts of component m sodium sulfate, water) were in the form of spray-dried granules which had been impregnated with the rest of component b.
• This granulate 29 parts by weight
• the result was a powder mixture with excellent pourability, which did not require any post-treatment (powdering) with finely divided zeolite.
• the powders proved to be easy to pour, non-dusting and dissolved quickly when sprinkled in household washing machines, without lumps and without residue.
• the powder components did not separate.

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• 1988
  • 1988-04-15 DE DE3812530A patent/DE3812530A1/de not_active Withdrawn
• 1989
  • 1989-04-08 EP EP89106222A patent/EP0337330B1/fr not_active Expired - Lifetime
  • 1989-04-08 AT AT89106222T patent/ATE138096T1/de active
  • 1989-04-08 ES ES89106222T patent/ES2086308T3/es not_active Expired - Lifetime
  • 1989-04-08 DE DE58909678T patent/DE58909678D1/de not_active Expired - Fee Related
  • 1989-04-14 JP JP1096206A patent/JPH01311200A/ja active Pending
  • 1989-04-14 DK DK182389A patent/DK182389A/da not_active Application Discontinuation
  • 1989-04-15 KR KR1019890005006A patent/KR890016160A/ko not_active Abandoned
• 1991
  • 1991-01-18 US US07/644,469 patent/US5149455A/en not_active Expired - Fee Related

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