EP0603207B1 - Verfahren zur herstellung von tensidgranulaten - Google Patents
Verfahren zur herstellung von tensidgranulaten Download PDFInfo
- Publication number
- EP0603207B1 EP0603207B1 EP92917099A EP92917099A EP0603207B1 EP 0603207 B1 EP0603207 B1 EP 0603207B1 EP 92917099 A EP92917099 A EP 92917099A EP 92917099 A EP92917099 A EP 92917099A EP 0603207 B1 EP0603207 B1 EP 0603207B1
- Authority
- EP
- European Patent Office
- Prior art keywords
- surfactant
- surfactants
- weight
- granules
- liquid component
- 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.)
- Revoked
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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
- 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
- C11D1/831—Mixtures of non-ionic with anionic compounds of sulfonates with ethers of polyoxyalkylenes without phosphates
-
- 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
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
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- 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
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/14—Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
-
- 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
- C11D1/02—Anionic compounds
- C11D1/12—Sulfonic acids or sulfuric acid esters; Salts thereof
- C11D1/28—Sulfonation products derived from fatty acids or their derivatives, e.g. esters, amides
-
- 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
- the invention relates to a process for the production of detergent granules which are active in washing and cleaning, and to a surfactant granulate produced by the process according to claim 17.
- the storage-stable and dust-free granules have an increased bulk density.
- anionic oleochemical surfactant compounds are the known sulfofatty acid methyl esters (fatty acid methyl ester sulfonates, MES), which by ⁇ -sulfonation of the methyl esters of fatty acids of plant or animal origin with predominantly 10 to 20 carbon atoms in the fatty acid molecule and subsequent neutralization to form water-soluble mono salts, in particular the corresponding alkali salts.
- MES fatty acid methyl ester sulfonates
- ester cleavage gives them the corresponding sulfofatty acids or their di-salts, which, like mixtures of di-salts and sulfofatty acid methyl ester mono-salts, have important washing and cleaning properties.
- comparable problems also occur in other surfactant classes when trying to display the corresponding surfactant raw materials in dry form.
- a final bleaching for example with aqueous hydrogen peroxide, is generally required in their synthesis, so that here too, today's technology leads to the aqueous paste form.
- APG pastes Such aqueous alkyl glycoside pastes (APG pastes) are more at risk from hydrolysis or microbial contamination, for example, than corresponding dry products.
- simple drying according to the technologies customary hitherto presents considerable difficulties.
- drying an aqueous paste of the alkali salts of detergent soaps and / or ABS pastes can also cause considerable problems.
- Granulation is an alternative to spray drying of surfactant pastes.
- European patent application EP 403 148 describes a process for producing FAS granules which are dispersible in cold water.
- a highly concentrated aqueous FAS paste is used which contains less than 14% by weight of water and less than 20% by weight of further additives contains, mechanically processed at temperatures between 10 and 45 ° C until granules are formed.
- FAS granules are obtained which are already dispersed at washing temperatures between 4 and 30 ° C; however, the process temperature to be observed and the relatively low maximum water content of the surfactant paste are critical process parameters.
- a method for producing FAS and / or ABS granules is known from European patent application EP 402 112, the neutralization of the anionic surfactants in acid form to give a paste with a maximum of 12% by weight of water with the addition of auxiliaries such as polyethylene glycols and ethoxylated alcohols or alkylphenols, which have a melting point above 48 ° C., and the granulation is carried out in a high-speed mixer. Again, the amount of water to be maintained is a critical process parameter. In addition, it is not disclosed what bulk densities the surfactant granules obtained by this process have.
- the object of the invention was to provide a method for producing heavy, free-flowing surfactant granules, in which the content of a non-surfactant liquid component is not a critical process parameter.
- the invention accordingly relates to a process for the production of detergent-active granules with a bulk density above 500 g / l by granulation of a surfactant preparation which has a non-surfactant liquid component, a surfactant preparation form which is used under normal pressure at temperatures between 20 and 40 ° C in liquid to pasty form, if desired granulated with the addition of an inorganic or organic solid and dried at the same time.
- the process according to the invention has the advantage that it is not limited to the production of granules of only a few surfactants, but that free-flowing granules of anionic, nonionic, amphoteric, cationic surfactants and mixtures of these can be prepared by this process, the composition of the granules can be predetermined.
- the production of anionic surfactants or nonionic surfactants or mixtures of anionic surfactants and nonionic surfactants is preferred.
- the process according to the invention has advantages over the spray drying process, since the process according to the invention can also be used to produce granules which contain nonionic surfactants which, owing to their known pluming behavior, are not accessible by spray drying. In addition, due to the preferably lower process temperatures and gentle drying, there is no browning of the granules.
- the surfactant preparation form used according to the invention which is in liquid to pasty form under normal pressure at temperatures between 20 and 40 ° C., contains a mixture of one or more surfactants and a non-surfactant liquid component, the constituents of organic and / or contains inorganic nature.
- the surfactant preparation form consists of at least two separate parts, the first of which is a mixture of one or more surfactants and a non-surfactant liquid component which contains constituents of organic and / or inorganic nature, and the second or the following Share either one or more surfactants present under normal pressure and at temperatures between 20 and 40 ° C in liquid to pasty form, which surfactants are at least partially from the Surfactants of the first part are different, or a further mixture of one or more surfactants, which are at least partially different from the surfactants of the first part, and a non-surfactant liquid component which contains constituents of organic and / or inorganic nature.
- Another embodiment of the invention provides that at least one component of the non-surfactant liquid component is not incorporated into the surfactant-containing parts of the surfactant preparation form mentioned, but is added separately.
- the individual surfactant-containing parts of the surfactant preparation form as well as constituents of the non-surfactant liquid component, which are separate and not, are included in the surfactant preparation form be added in a homogeneous mixture with surfactants.
- the non-surfactant liquid component which can contain one or more constituents, has a boiling point or boiling range under normal pressure, preferably below 250 ° C. and in particular below 200 ° C.
- the non-surfactant liquid component particularly advantageously contains constituents which boil between 60 and 180 ° C. at normal pressure.
- Mono- and / or polyfunctional alcohols for example methanol, ethanol, propanol, isopropanol, butanol, secondary and tertiary butanol, pentanol, ethylene glycol, 1,2-propanediol, glycerol or, are preferably used as the optional organic constituent of the non-surfactant liquid component Mixtures of these are used.
- the proportion of the mono- and / or polyfunctional alcohols used as the non-surfactant liquid component is preferably 0.5 to 10% by weight, based on the surfactant preparation form.
- water as the inorganic component of the non-surfactant liquid component, optionally together with organic components such as ethanol, 1,2-propanediol or glycerol.
- the proportion of water is preferably 25 to 80% by weight, based on the surfactant preparation form.
- the total proportion of the non-surfactant liquid component is preferably 30 to 70 % By weight and in particular 45 to 60% by weight, in each case based on the surfactant preparation form.
- Anionic surfactants used are, for example, those of the sulfonate and sulfate type.
- Preferred surfactants of the sulfonate type are C9-C13 alkylbenzenesulfonates, olefin sulfonates, i.e. Mixtures of alkene and hydroxyalkanesulfonates and disulfonates, such as those obtained, for example, from C12-C18 monoolefins with terminal and internal double bonds by sulfonation with gaseous sulfur trioxide and subsequent alkaline or acidic hydrolysis of the sulfonation products, are considered.
- esters of ⁇ -sulfofatty acids which, by ⁇ -sulfonation of the methyl esters of fatty acids of plant and / or animal origin with 10 to 20 C atoms in the fatty acid molecule and subsequent neutralization, are converted into water-soluble mono-salts, for example, by the process according to the invention the ⁇ -sulfonated methyl esters of hydrogenated coconut, palm kernel or tallow fatty acids, and the ⁇ -sulfofatty acids or their di-salts obtainable by ester cleavage.
- Suitable surfactants of the sulfate type are the sulfuric acid monoesters from primary alcohols of natural and synthetic origin, in particular from fatty alcohols, for example from coconut oil alcohols, tallow fatty alcohols, oleyl alcohol, lauryl, myristyl, palmityl or stearyl alcohol, or the C10-C20 oxo alcohols, and those and this chain length.
- the sulfuric acid monoesters of alcohols ethoxylated with 1 to 6 moles of ethylene oxide, such as 2-methyl-branched C9-C11 alcohols with an average of 3.5 moles of ethylene oxide, are suitable.
- Sulfated fatty acid monoglycerides are also suitable.
- surfactant granules containing C12-C18 alkyl sulfates (FAS) or C16-C18 alkyl sulfates (TAS) alone or together with other surfactants is preferred.
- Natural fatty acids e.g. Soap mixtures derived from coconut, palm kernel or tallow fatty acids. Preferred are those which are composed of 50 to 100% of saturated C12-C18 fatty acid soaps and 0 to 50% of oleic acid soaps.
- the process according to the invention produces granules which contain soap mixed with other surfactants.
- the anionic surfactants can be used in the form of their sodium, potassium, calcium and ammonium salts and as water-soluble salts of organic bases, such as mono-, di- or triethanolamine. They are preferably used in the form of aqueous preparations, in particular in the form of about 30 to 60% by weight aqueous preparations in which the anionic surfactants are obtained during their preparation by neutralizing the corresponding acids.
- Granules produced by the process according to the invention preferably contain nonionic surfactants, in particular together with anionic surfactants, for example alkylbenzenesulfonate and / or fatty alkyl sulfate.
- the nonionic surfactants are preferably derived from liquid ethoxylated, in particular primary alcohols with preferably 9 to 18 carbon atoms and an average of 1 to 12 moles of ethylene oxide per mole of alcohol, in which the alcohol radical can be linear or methyl-branched in the 2-position, or linear and may contain methyl-branched radicals in the mixture, as are usually present in oxo alcohol radicals.
- linear residues of alcohols of native origin with 12 to 18 carbon atoms such as, for example, coconut oil, tallow oil or oleyl alcohol, are particularly preferred.
- the degrees of ethoxylation given represent statistical averages, which can be an integer or a fraction for a specific product.
- Preferred alcohol ethoxylates have a restricted homolog distribution (narrow range ethoxylates, nre).
- alcohol ethoxylates are preferred which have an average of 2 to 8 ethylene oxide groups.
- the preferred ethoxylated alcohols include, for example, C9-C11 oxo alcohol with 7 EO, C13-C15 oxo alcohol with 3 EO, 5 EO or 7 EO and in particular C12-C14 alcohol with 3 EO or 4 EO, C12-C18 alcohols with 3 EO, 5 EO or 7 EO and mixtures of these , such as mixtures of C12-C14 alcohol with 3 EO and C12-C18 alcohol with 5 EO.
- the granules produced by the process according to the invention can be used as nonionic surfactants, alkyl glycosides of the general formula RO- (G) x , in which R is a primary straight-chain or aliphatic radical with 8 to 22, preferably 12 to 18, carbon atoms in the 2-position , G is a symbol which stands for a glycose unit with 5 or 6 carbon atoms, and the degree of oligomerization x is between 1 and 10, preferably between 1 and 2 and in particular is significantly less than 1.4.
- R is a primary straight-chain or aliphatic radical with 8 to 22, preferably 12 to 18, carbon atoms in the 2-position
- G is a symbol which stands for a glycose unit with 5 or 6 carbon atoms
- the degree of oligomerization x is between 1 and 10, preferably between 1 and 2 and in particular is significantly less than 1.4.
- the proportion of the surfactants is preferably 20 to 75% by weight and in particular 35 to 70% by weight, in each case based on the surfactant preparation form.
- the surfactant preparation form preferably contains, as further constituents, additives which are ingredients of detergents and cleaning agents.
- additives which are ingredients of detergents and cleaning agents.
- surfactant preparations which contain additives in amounts of 0.001 to 15% by weight, based on the surfactant preparation form, are used in the process according to the invention.
- Particularly preferred additives are dyes, foam inhibitors, bleaches and / or constituents which improve solubility.
- Suitable dyes are temperature-stable dyes, preferably pigment dyes, which are advantageously used in amounts of 0.001 to 0.5% by weight, based on the surfactant preparation form.
- Suitable foam inhibitors are, for example, soaps of natural and synthetic origin, which have a high proportion of C18-C24 fatty acids.
- Suitable non-surfactant-like foam inhibitors are organopolysiloxanes and their mixtures with microfine, optionally silanized silica, paraffins, waxes, microcrystalline waxes and their mixtures with silanized silica.
- Bisacylamides derived from C12-C20 alkylamines and C2-C6 dicarboxylic acids are also useful. Be an advantage too Mixtures of various foam inhibitors are used, for example those made from silicone and paraffins or waxes.
- the foam inhibitors are preferably bound to a granular, water-soluble or dispersible carrier substance.
- the foam inhibitor content of the surfactant preparation form is preferably 0.01 to 0.5% by weight.
- bleaching agents which supply H2O2 in water
- sodium perborate tetrahydrate and sodium perborate monohydrate are of particular importance.
- Other useful bleaching agents are, for example, peroxy carbonate, peroxypyrophosphate, citrate perhydrate, peroxaphthalate, diperazelaic acid or diperdodecanedioic acid.
- hydrogen peroxide as a bleaching agent in surfactant preparation forms which are used according to the invention.
- the content of bleach in the surfactant preparation form is preferably 0.5 to 15% by weight, in particular the content of hydrogen peroxide is 0.5 to 5% by weight.
- the constituents which improve the solubility include liquid, pasty and solid compounds which are soluble or dispersible in the other constituents of the surfactant preparation form.
- Polyethylene glycols with a relative molecular weight between 200 and 20,000 and highly ethoxylated fatty alcohols with 14 to 80 ethylene oxide groups per mole of alcohol, in particular C12-C18 fatty alcohols with 20 to 60 ethylene oxide groups, for example tallow fatty alcohol with 30 EO or 40 EO, are preferably used as constituents which improve solubility .
- the use of polyethylene glycols with a relative molecular weight between 200 and 600 is particularly preferred. These polyethylene glycols are advantageously used as a separate component of the non-surfactant liquid component.
- the content of the surfactant preparation form in these constituents which improve the solubility of the finished granules is preferably 1 to 15% by weight and in particular 2 to 10% by weight.
- the surfactant preparation form is granulated and dried at the same time. "Drying” is understood to mean the partial or complete removal of the non-surfactant liquid component. If desired, residual values of free, ie unbound water and / or mono- and / or polyfunctional alcohols are present as long as the finished granules are free-flowing and non-sticky. However, a free water content of 10% by weight and in particular 0.1 to 2% by weight, based in each case on the finished granules, is preferably not exceeded.
- the surfactant granules can be produced in all devices in which granulation can be carried out with simultaneous drying. Examples of this are heatable mixers and granulators, in particular granulators of the Turbo dryer (R) type (device from Vomm, Italy).
- the invention provides that the combination of these two process steps is carried out in a batch or continuous fluidized bed. It is particularly preferred to carry out the process continuously in the fluidized bed.
- the surfactant preparation form or the individual parts of the surfactant preparation form can be introduced into the fluidized bed simultaneously or in succession via one, for example via a nozzle with several openings, or via several nozzles.
- Fluidized bed apparatuses which are preferably used have base plates with dimensions of at least 0.4 m.
- fluidized bed apparatuses are preferred which have a base plate with a diameter between 0.4 and 5 m, for example 1.2 m or 2.5 m.
- fluidized bed apparatuses are also suitable which have a base plate with a diameter greater than 5 m.
- a perforated base plate or a Conidur plate (commercial product from Hein & Lehmann, Federal Republic of Germany) is preferably used as the base plate.
- the process according to the invention is preferably carried out at fluidizing air speeds between 1 and 8 m / s and in particular between 1.5 and 5.5 m / s.
- the granules are discharged from the fluidized bed advantageously by means of a size classification of the granules. This classification can take place, for example, by means of a sieving device or by means of an opposed air flow (classifier air) which is regulated in such a way that only particles of a certain particle size out the fluidized bed is removed and smaller particles are retained in the fluidized bed.
- the inflowing air is composed of the heated or unheated classifier air and the heated soil air.
- the soil air temperature is preferably between 80 and 400 ° C, in particular between 90 and 350 ° C.
- the vortex air cools down due to heat losses and the heat of vaporization of the components of the non-surfactant liquid component.
- the temperature of the vortex air is approximately 5 cm above the base plate 60 to 120 ° C., preferably 65 to 90 ° C. and in particular 70 to 85 ° C.
- the air outlet temperature is preferably between 60 and 120 ° C, in particular below 100 ° C and particularly advantageously between 70 and 85 ° C.
- a starting mass In the process which is preferably carried out in the fluidized bed, it is necessary for a starting mass to be present at the beginning of the process and which serves as an initial carrier for the sprayed-in surfactant preparation form.
- Ingredients of detergents and cleaning agents are particularly suitable as starting mass, in particular those which can also be used as solids in the process according to the invention and which have a particle size distribution which corresponds approximately to the particle size distribution of the finished granules.
- surfactant granules it is preferred to use surfactant granules as starting mass which have already been obtained in a previous process.
- the components of the non-surfactant liquid component evaporate partially or completely in the fluidized bed. Dried to dried germs are formed, which are coated with further quantities of the surfactant preparation form, granulated and in turn dried at the same time.
- the surfactant preparation form is granulated with the addition of an inorganic or organic solid and dried at the same time, it being possible for the solid to be dusted pneumatically via blow lines.
- This solid which serves as a carrier for the surfactant preparation form, preferably consists of ingredients from washing and cleaning agents.
- Suitable solids are, for example, surfactants or surfactant mixtures which were produced by granulation, by spray drying or by the process according to the invention and are recycled to increase the surfactant concentration in the finished granulate.
- the use of spray-dried and / or surfactant granules obtained by the process according to the invention is preferred.
- Highly ethoxylated fatty alcohols with, for example, 20 to 80 EO, preferably 20 to 60 EO and in particular tallow fatty alcohol with 30 or 40 EO can also advantageously be used as solids - as an alternative to incorporation into the surfactant preparation form.
- non-surfactant ingredients of detergents and cleaning agents preferably one or more constituents from the group of the alkali carbonates, alkali sulfates, crystalline and amorphous alkali silicates and layered silicates and zeolite, in particular zeolite NaA in detergent quality, salts of citric acid, are used as solids, solid peroxy bleaching agents and optionally bleach activators and solid polyethylene glycols with a relative molecular weight greater than or equal to 2,000, in particular between 4,000 and 20,000, are used.
- Solids Preference is given to using finely divided materials as solids, which can either be produced directly in this state, are commercially available, or are converted into this finely divided state by conventional comminution methods, for example by grinding with conventional mills.
- Preferred solids have, for example, no more than 5% by weight of particles with a diameter above 2 mm and preferably no more than 5% by weight of particles with a diameter above 1.6 mm.
- solids are preferred which consist of at least 90% by weight of particles with a diameter below 1.0 mm. Examples of these are alkali carbonates with more than 90% by weight of particles with a diameter of less than or equal to 0.5 mm and zeolite NaA powder in detergent quality which contains at least 90% by weight of particles with a diameter below 0.03 mm .
- the added solids are used with particular advantage in amounts of 10 to 50% by weight and in particular 20 to 45% by weight, based in each case on the sum of the surfactant preparation form and the solid.
- the surfactant granules which can be produced by the process according to the invention are claimed.
- Preferred surfactant granules have a surfactant content of 10 to 100% by weight, in particular 30 to 80% by weight and with particular advantage between 40 and 70% by weight, in each case based on the finished granules.
- Pure surfactant granules are obtained when the non-surfactant liquid component is completely evaporated and the granules are thus completely dried and the solid that may be added consists of a pure surfactant material.
- surfactant granules which have been prepared by the process according to the invention and now serve as a solid in the process according to the invention are preferably comminuted to the desired particle size distribution and recycled.
- the content of surfactants in the granules can be set to any of the desired values.
- the surfactant granules obtained by the process according to the invention preferably have a bulk density between 550 and 1000 g / l, in particular between 550 and 850 g / l, and are dust-free, that is to say in particular they contain no particles with a particle size below 50 ⁇ m. Otherwise, the particle size distribution of the surfactant granules corresponds to the usual particle size distribution of a heavy detergent of the prior art.
- the surfactant granules have a particle size distribution in which a maximum of 5% by weight, preferably a maximum of 3% by weight of the particles have a diameter above 2.5 mm and a maximum of 5% by weight, with particular advantage a maximum of 3% by weight of the Particles have a diameter below 0.1 mm.
- the surfactant granules are characterized by their light color and their free-flowing properties. A further measure to prevent the surfactant granules produced according to the invention from sticking together is not necessary.
- the surfactant granules being powdered in a known manner with finely divided materials, for example with zeolite NaA, soda, in order to further increase the bulk density.
- This powdering can be carried out, for example, during a rounding step.
- preferred surfactant granules already have such a regular, in particular approximately spherical, structure that a Rounding step is usually not necessary and is therefore not preferred.
- Examples 1 to 10 a surfactant preparation form, which could consist of one or more separate parts, was granulated through a nozzle into a granulation drying system (AGT) from Glatt, Federal Republic of Germany, together with a solid and simultaneously dried.
- a surfactant granulate which had been obtained in a previous batch (under the same process conditions) and had approximately the same composition as the finished granules of Examples 1 to 10 was used as the starting mass.
- the process conditions can be found in Table 1.
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Detergent Compositions (AREA)
- Emulsifying, Dispersing, Foam-Producing Or Wetting Agents (AREA)
- Compounds Of Unknown Constitution (AREA)
- Glanulating (AREA)
- Materials For Medical Uses (AREA)
- Medicinal Preparation (AREA)
- Cleaning Or Drying Semiconductors (AREA)
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE4127323 | 1991-08-20 | ||
| DE4127323A DE4127323A1 (de) | 1991-08-20 | 1991-08-20 | Verfahren zur herstellung von tensidgranulaten |
| PCT/EP1992/001831 WO1993004162A1 (de) | 1991-08-20 | 1992-08-11 | Verfahren zur herstellung von tensidgranulaten |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| EP0603207A1 EP0603207A1 (de) | 1994-06-29 |
| EP0603207B1 true EP0603207B1 (de) | 1995-05-10 |
Family
ID=6438571
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| EP92917099A Revoked EP0603207B1 (de) | 1991-08-20 | 1992-08-11 | Verfahren zur herstellung von tensidgranulaten |
Country Status (10)
| Country | Link |
|---|---|
| US (1) | US5516447A (da) |
| EP (1) | EP0603207B1 (da) |
| JP (1) | JPH06510070A (da) |
| KR (1) | KR100204549B1 (da) |
| AT (1) | ATE122387T1 (da) |
| CA (1) | CA2116104A1 (da) |
| DE (2) | DE4127323A1 (da) |
| DK (1) | DK0603207T3 (da) |
| ES (1) | ES2071513T3 (da) |
| WO (1) | WO1993004162A1 (da) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7064100B2 (en) | 2001-12-04 | 2006-06-20 | Henkel Komanditgesellschaft Auf Aktien (Henkel Kgaa) | Method for producing bleach activator granules |
Families Citing this family (60)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4304062A1 (de) * | 1993-02-11 | 1994-08-18 | Henkel Kgaa | Verfahren zur Herstellung von Tensidgranulaten |
| US5739097A (en) * | 1993-02-11 | 1998-04-14 | Henkel Kommanditgesellschaft Auf Aktien | Process for the production of surfactant granules |
| DE4304015A1 (de) * | 1993-02-11 | 1994-08-18 | Henkel Kgaa | Verfahren zur Herstellung von Granulaten |
| DE4403323A1 (de) * | 1993-09-23 | 1995-08-10 | Henkel Kgaa | Extrudierte Wasch- oder Reinigungsmittel mit verbesserten Löseeigenschaften |
| DE4335955A1 (de) * | 1993-10-21 | 1995-04-27 | Henkel Kgaa | Verfahren zur Herstellung wasch- oder reinigungsaktiver Extrudate mit verbessertem Redispergiervermögen |
| DE4404279A1 (de) * | 1994-02-10 | 1995-08-17 | Henkel Kgaa | Tablette mit Buildersubstanzen |
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| DE19851454B4 (de) * | 1998-11-09 | 2010-11-04 | Henkel Ag & Co. Kgaa | Tensid-Granulate durch Wirbelschichtgranulation |
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| US6730652B1 (en) * | 1999-04-19 | 2004-05-04 | The Procter & Gamble Company | Process for making non-staining colored particles for improving aesthetics of a liquid automatic dishwashing detergent product, the particles, and a composition |
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| WO2001038473A1 (de) * | 1999-11-23 | 2001-05-31 | Cognis Deutschland Gmbh | Verfahren zur herstellung von entschäumergranulaten |
| EP1126017B1 (de) * | 2000-02-18 | 2005-10-26 | Glatt Ingenieurtechnik GmbH | Verfahren zur Herstellung von Vollwaschmitteln und Vollwaschmittelkomponenten |
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| DE10159388A1 (de) * | 2001-12-04 | 2003-06-12 | Henkel Kgaa | Verfahren zur Herstellung von umhüllten Bleichaktivatorgranulaten |
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| WO2005032736A1 (ja) * | 2003-10-03 | 2005-04-14 | Mitsubishi Gas Chemical Company, Inc. | 固体粒子の洗浄方法 |
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| EP3743494B1 (en) | 2018-01-26 | 2025-08-06 | Ecolab Usa Inc. | Solidifying liquid amine oxide surfactant with urea binder and optional carrier |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE140987C (da) * | 1903-05-16 | |||
| DE1903743A1 (de) * | 1969-01-25 | 1970-08-13 | Westfalia Dinnendahl Groeppel | Umluftsichter |
| US3769222A (en) * | 1971-02-09 | 1973-10-30 | Colgate Palmolive Co | Free flowing nonionic surfactants |
| US3703772A (en) * | 1971-07-27 | 1972-11-28 | Colgate Palmolive Co | Drying of detergents |
| US4487710A (en) * | 1982-03-01 | 1984-12-11 | The Procter & Gamble Company | Granular detergents containing anionic surfactant and ethoxylated surfactant solubility aid |
| DE3504628A1 (de) * | 1985-02-11 | 1986-08-14 | Henkel KGaA, 4000 Düsseldorf | Verfahren zur herstellung eines rieselfaehigen granulats |
| FR2581323B1 (fr) * | 1985-05-06 | 1987-05-29 | Rhone Poulenc Spec Chim | Nouvelle composition tensio-active, son procede d'obtention et ses applications |
| US4828721A (en) * | 1988-04-28 | 1989-05-09 | Colgate-Palmolive Co. | Particulate detergent compositions and manufacturing processes |
| DE3835918A1 (de) * | 1988-10-21 | 1990-04-26 | Henkel Kgaa | Verfahren zur herstellung von tensidhaltigen granulaten |
| US5045238A (en) * | 1989-06-09 | 1991-09-03 | The Procter & Gamble Company | High active detergent particles which are dispersible in cold water |
| CA2017921C (en) * | 1989-06-09 | 1995-05-16 | John Michael Jolicoeur | Formation of detergent granules by deagglomeration of detergent dough |
| CA2017922C (en) * | 1989-06-09 | 1995-07-11 | Frank Joseph Mueller | Formation of discrete, high active detergent granules using a continuous neutralization system |
| DK161743C (da) * | 1989-07-03 | 1992-02-17 | Niro Atomizer As | Fremgangsmaade og apparat til agglomerering af et pulverformigt materiale |
| KR0170424B1 (ko) * | 1990-07-05 | 1999-01-15 | 호르스트 헤를레,요한 글라슬 | 세제 및 청정제용 표면 활성제 과립의 제조방법 |
| IT1252682B (it) * | 1991-11-13 | 1995-06-23 | Vomm Impianti & Processi Srl | Prodotto in granuli di elevato peso specifico, particolarmente quale additivo di detersivi in polvere e metodo per il suo ottenimento |
-
1991
- 1991-08-20 DE DE4127323A patent/DE4127323A1/de not_active Ceased
-
1992
- 1992-08-11 WO PCT/EP1992/001831 patent/WO1993004162A1/de not_active Ceased
- 1992-08-11 DK DK92917099.1T patent/DK0603207T3/da active
- 1992-08-11 AT AT92917099T patent/ATE122387T1/de active
- 1992-08-11 EP EP92917099A patent/EP0603207B1/de not_active Revoked
- 1992-08-11 US US08/196,141 patent/US5516447A/en not_active Expired - Lifetime
- 1992-08-11 KR KR1019940700499A patent/KR100204549B1/ko not_active Expired - Fee Related
- 1992-08-11 DE DE59202174T patent/DE59202174D1/de not_active Revoked
- 1992-08-11 CA CA002116104A patent/CA2116104A1/en not_active Abandoned
- 1992-08-11 ES ES92917099T patent/ES2071513T3/es not_active Expired - Lifetime
- 1992-08-11 JP JP5504079A patent/JPH06510070A/ja active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7064100B2 (en) | 2001-12-04 | 2006-06-20 | Henkel Komanditgesellschaft Auf Aktien (Henkel Kgaa) | Method for producing bleach activator granules |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH06510070A (ja) | 1994-11-10 |
| ATE122387T1 (de) | 1995-05-15 |
| DE4127323A1 (de) | 1993-02-25 |
| DE59202174D1 (de) | 1995-06-14 |
| EP0603207A1 (de) | 1994-06-29 |
| WO1993004162A1 (de) | 1993-03-04 |
| ES2071513T3 (es) | 1995-06-16 |
| DK0603207T3 (da) | 1995-07-24 |
| US5516447A (en) | 1996-05-14 |
| CA2116104A1 (en) | 1993-03-04 |
| KR100204549B1 (ko) | 1999-06-15 |
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