EP1131400B1 - Procede de production de granules tensioactifs - Google Patents

Procede de production de granules tensioactifs Download PDF

Info

Publication number
EP1131400B1
EP1131400B1 EP99963299A EP99963299A EP1131400B1 EP 1131400 B1 EP1131400 B1 EP 1131400B1 EP 99963299 A EP99963299 A EP 99963299A EP 99963299 A EP99963299 A EP 99963299A EP 1131400 B1 EP1131400 B1 EP 1131400B1
Authority
EP
European Patent Office
Prior art keywords
aqueous
surfactant
fluidized bed
granules
anionic surfactants
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.)
Expired - Lifetime
Application number
EP99963299A
Other languages
German (de)
English (en)
Other versions
EP1131400A1 (fr
Inventor
Karl-Heinz Schmid
Christoph Breucker
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Cognis IP Management GmbH
Original Assignee
Cognis IP Management GmbH
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Cognis IP Management GmbH filed Critical Cognis IP Management GmbH
Publication of EP1131400A1 publication Critical patent/EP1131400A1/fr
Application granted granted Critical
Publication of EP1131400B1 publication Critical patent/EP1131400B1/fr
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D3/00Other compounding ingredients of detergent compositions covered in group C11D1/00
    • C11D3/02Inorganic compounds ; Elemental compounds
    • C11D3/04Water-soluble compounds
    • C11D3/044Hydroxides or bases
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D1/00Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
    • C11D1/02Anionic compounds
    • C11D1/12Sulfonic acids or sulfuric acid esters; Salts thereof
    • C11D1/14Sulfonic acids or sulfuric acid esters; Salts thereof derived from aliphatic hydrocarbons or mono-alcohols
    • C11D1/146Sulfuric acid esters
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11DDETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
    • C11D11/00Special methods for preparing compositions containing mixtures of detergents
    • C11D11/0082Special 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

Definitions

  • the invention relates to a process for the preparation of surfactant granules containing anionic surfactants by granulation and simultaneous drying in the fluidized bed, which is carried out in the presence of volatile bases, and their use for the preparation of particular pH-neutral detergents, dishwashing detergents and cleaning agents and oral hygiene products.
  • Anionic surfactants such as alkyl sulfates and alkyl ether sulfates are common surfactants, which find a wide application in cleaning processes of all kinds due to their high washing power. Due to their manufacturing process, these are usually obtained in salt form as aqueous solutions or pastes, which are converted into their powder or granules, for example, by conventional drying technology, especially in the spray tower or in granulating. At the drying temperatures prevailing there, however, pH-neutral solutions or pastes of the alkyl (ether) sulfate would decompose autocatalytically into the corresponding olefinic base and the corresponding salts of hydrogen sulfate, which themselves act as acid in aqueous solution.
  • such pastes according to the prior art are provided with a so-called alkali reserve, ie such pastes are mixed with an excess of free hydroxides, in particular of sodium hydroxide.
  • the sodium hydroxide is then able to trap the possibly formed by autocatalysis acid and so stop the decomposition process.
  • the alkali reserve is added in excess, usually in such amounts that, for example, a fatty alcohol sulfate paste has a pH above 10, small residual amounts of unused sodium hydroxide always remain in the aqueous solution or paste of the alkyl (ether) sulfates.
  • the residual amounts of the alkali reserve are present as minor constituents of the anionic surfactants.
  • these residual alkali components in the anionic surfactants cause problems in a number of applications, as they may cause odors and color shifts, for example due to undesirable interactions with perfume raw materials or dyes.
  • there are a number of application fields for example in cosmetics or in the field of so-called pH-neutral detergents, dishwashing detergents and cleaners for which pH-neutral anionic surfactants are desired.
  • From the DE 197 07 649 C1 discloses a process for producing detergent raw materials by simultaneous drying and granulation of aqueous pastes in a thin film evaporator.
  • the drying of these pastes is carried out at a temperature in the range of 120-130 ° C in the presence of a Alkalicarbonatzusatzes to paste and / or an alkaline gas stream.
  • the autocatalytic decomposition of the anionic surfactants during their drying should continue to be effectively prevented.
  • no disturbing residual amounts of alkaline substances should be present in the resulting surfactant granules.
  • it was within the scope of the invention desired to produce anionic surfactants as granules with a high bulk density, which have only slightly dusty shares.
  • the object has been achieved by adding to the aqueous, anionic surfactant (in salt form) containing surfactant pastes before and / or during the granulation and simultaneous drying in the fluidized bed with volatile bases.
  • the invention includes the finding that anionic surfactant granules which have no or lower residual amounts of alkaline substances are obtainable with the method according to the invention, so that they do not cause any undesired interactions with perfume or dyes. Furthermore, the invention includes the knowledge that by the ubiquitous presence of the volatile bases in the fluidized bed are effectively reduced even at the most remote locations of the apparatus, for example in the filter, decomposition of already formed dried anionic surfactants under thermal stress and Wandandbackept the decomposed product can be reduced.
  • An object of the present invention therefore relates to a process for the preparation of surfactant granules, wherein after dissolving the surfactant granules in water, the aqueous solution has a pH value between 7 and 9.5, by granulation and simultaneous drying of an aqueous, anionic surfactant in salt form containing surfactant the fluidized bed, characterized in that prior to or during the granulation and simultaneous drying volatile bases in amounts of 0.05 to 5 wt .-% - based on the active substance of the anionic surfactants in aqueous surfactant preparation in the form
  • aqueous surfactant preparations containing anionic surfactants are used for the process.
  • these are aqueous surfactant preparations which contain exclusively anionic surfactants.
  • These are preferably used in the form of aqueous pastes, in particular with an active substance content of from 25 to 90% by weight, based on aqueous anionic surfactant paste.
  • anionic surfactants are fatty alcohol sulfates, fatty alcohol ether sulfates, glycerol ether sulfates, hydroxy mixed ether sulfates, monoglyceride (ether) sulfates, fatty acid amide (ether) sulfates and alkyl oligoglucoside sulfates. If the anionic surfactants contain polyglycol ether chains, they may have a conventional, but preferably a narrow homolog distribution.
  • fatty alcohol sulfates and / or fatty alcohol ether sulfates as anionic surfactants.
  • Particularly suitable are those which follow the formula (I) , R 1 O- (CH 2 CH 2 O) m SO 3 X (I) in which R 1 is a linear or branched alkyl and / or alkenyl radical having 6 to 22 carbon atoms, m is 0 or numbers from 1 to 10 and X is an alkali and / or alkaline earth metal, ammonium, alkylammonium, alkanolammonium or glucammonium.
  • sulfates based on technical C 12/14 - or C 12/18 alcohol fractions , based on natural oils and fats such as coconut oil, palm kernel oil, palstearin or tallow or even based on Ziegleralkoholen bwz. also of oxo alcohols in the range of C8 to C15 (or mixtures thereof of the abovementioned linear alcohols of natural oils and fats or Ziegleralkoholen with oxo alcohols) in the form of their sodium, potassium and / or magnesium salts.
  • Typical examples of ether sulfates of alcohols ethoxylated with on average 1 to 10 and in particular 2 to 5 moles of ethylene oxide are selected from the group caproic alcohol, capryl alcohol, 2-ethylhexyl alcohol, capric alcohol, lauryl alcohol, isotridecyl alcohol, myristyl alcohol, cetyl alcohol, palmoleyl alcohol, stearyl alcohol, isostearyl alcohol, oleyl alcohol, Elaidyl alcohol, petroselinyl alcohol, arachyl alcohol, gadoleyl alcohol, behenyl alcohol, erucyl alcohol and brassidyl alcohol and their technical mixtures, in the form of their sodium and / or magnesium salts.
  • the ether sulfates may have both a conventional and a narrow homolog distribution.
  • aqueous surfactant preparations to be used for the purposes of the invention may contain, in addition to the anionic surfactants necessarily contained, optionally further surfactants or also additives which are preferably ingredients of detergents and cleaners.
  • Nonionic surfactants are preferably present in the aqueous surfactant preparations as further surfactants.
  • Suitable nonionic surfactants are liquid alkoxylated, advantageously ethoxylated, in particular primary alcohols having preferably 9 to 18 carbon atoms and an average of 1 to 12 moles of ethylene oxide (EO) per mole of alcohol, wherein the underlying alcohols may be methyl-branched linearly or in the 2-position, or linear and methyl-branched radicals in the mixture, as they are usually present in Oxoalkoholresten.
  • the nonionic surfactants of the type described are derived from linear alcohols of natural origin having 12 to 18 C atoms, such as coconut oil, tallow fatty acid or oleyl alcohol.
  • the degrees of ethoxylation given represent statistical means which, for a particular product, may be an integer or a fractional number.
  • Preferred alcohol ethoxylates have a narrow homolog distribution (narrow range ethoxylates, nre).
  • alcohol ethoxylates are preferred which have on average 2 to 8 ethylene oxide groups.
  • the preferred ethoxylated alcohols include, for example, C 9 -C 11 -oxoalcohol with 7 EO, C 13 -C 15 -oxoalcohol with 3 EO, 5 EO or 7 EO and in particular C 12 -C 14 -alcohol with 3 EO or 4 EO, C 12 -C 18 -alcohols with 3 EO, 5 EO or 7 EO and mixtures of these, such as mixtures of C 12 -C 14 -alcohol with 3 EO and C 12 -C 18 -alcohol with 5 EO.
  • alkyl glycosides of the general formula RO- (G) X in which R is a primary straight-chain or methyl-branched in the 2-position aliphatic radical having 8 to 22, preferably 12 to 18 carbon atoms, G is a symbol which represents a glycose unit having 5 or 6 carbon atoms, and the degree of oligomerization x is between 1 and 10, preferably between 1 and 2, and in particular less than 1.4, to be contained in the aqueous Tensidzurungsformen.
  • nonionic surfactants are present in the aqueous surfactant preparations with the anionic surfactants, their amount used can vary within wide ranges. As a rule, the nonionic surfactants are present in amounts of up to 50% by weight, calculated as the active substance and based on the active substance of the surfactants, in the aqueous surfactant preparations.
  • the aqueous surfactant preparation may contain additives, which are preferably ingredients of detergents and cleaners, preferably in amounts of from 0.001 to 80% by weight, based on the active substance of the aqueous surfactant preparation.
  • additives are inorganic builders such as zeolites, SKS6, sodium carbonate, sodium sulfate, Aerosil and / or organic builders such as starch, cellulose, cellulose ethers, microcrystalline cellulose and the like.
  • aqueous pastes are preferred as aqueous surfactant preparations containing as surfactants exclusively anionic surfactants, in particular fatty alcohol sulfates and / or fatty alcohol ether sulfates in the form of their sodium, potassium and / or magnesium salts.
  • Such pastes are commercially available and currently have an addition of aqueous hydroxides as alkali reserve.
  • the aqueous hydroxides are added according to the prior art, usually in amounts such that crizspielswesie Fettalkoholsulfatpasten (measured as 1 wt.% Aqueous solution) a pH above 10 have.
  • the addition of the aqueous hydroxides takes place during the preparation of the fatty alcohol sulfates by means of continuous neutralization.
  • the anionic surfactant pastes have such an amount of alkali reserves that the pH is between 7 and 9.5.
  • Such pH values of the anionic surfactant pastes can already be set in the neutralization step after sulfation of the alcohols by addition of the calculated amount of hydroxides, in particular sodium hydroxide, during the preparation of the sulfates. This is recommended in particular for highly viscous anionic surfactant pastes, in particular those which have active substance contents of 60 to 90% by weight. In the case of low-viscosity anionic surfactant pastes with active substance contents below 30% by weight, the same procedure can be followed.
  • low-viscosity anionic surfactant pastes with high alkali reserves can also be added subsequently, preferably first with customary inorganic and / or organic acids, for example citric acid, phosphoric acid, lactic acid, glycolic acid. Gluconic acid or sulfuric acid, especially citric acid, neutralize, preferably to a pH between 7 and 9.5. If desired, the acids can also be used to set a lower pH below 7, for example in the case of low-viscosity fatty alcohol ether sulfate pastes. In the context of the invention, it is of course also possible to use neutral aqueous pastes of anionic surfactants, which have not additionally been stabilized by the addition of hydroxides with an alkali reserve. For the purposes of the present invention, all anionic surfactants (pastes) having a pH of between 7 and 9.5 are considered to be pH-neutral anionic surfactants (pastes).
  • bases are preferably to be understood as meaning those compounds which, in the sense of the Broenstedt base definition, are capable of taking up protons. These are compounds which are already bases in themselves, such as ammonia or amines, as well as compounds which release by decomposition first bases, such as ammonium carbonate.
  • volatile such bases are referred to in the context of the invention, if they are preferably in the fluidized bed plants prevailing temperatures, especially at 60 ° C and below, are gaseous.
  • Particularly suitable volatile bases are those which are volatile even at room temperature (about 20 ° C.), such as ammonia and / or mono-, di- and trialkylamines having 1 and / or 2 carbon atoms in the alkyl radical. Particularly suitable is ammonia. Ammonia can be used as gas or in the form of its aqueous solutions such as concentrated ammonia.
  • the volatile bases are added preferably in amounts of from 0.05 to 5, in particular 0.1 to 1,% by weight, calculated as the active substance content of base and based on the active substance content of anionic surfactants in the aqueous surfactant preparation.
  • the volatile bases may be added to an embodiment of the present invention corresponding to the anionic surfactant-containing surfactant pastes just prior to their granulation and simultaneous drying.
  • the volatile bases in particular ammonia, in the form of their aqueous solutions, in particular concentrated ammonia, are added to the aqueous anionic surfactant preparations, which may have previously been pH neutral, before they are injected into the fluidized bed apparatus and subjected to granulation and simultaneous drying.
  • the surfactant preparations containing aqueous anionic surfactants may be pre-adjusted to pH neutral, and irrespective of this, to inject an aqueous base solution into the fluidized-bed apparatus.
  • the aqueous surfactant preparations with the anionic surfactants as usual via a nozzle into the fluidized bed apparatus and to inject the aqueous base solutions, in particular concentrated ammonia, preferably above the sieve bottom of the fluidized bed apparatus. Since there is negative pressure above the sieve bottom, the aqueous base solution is simply sucked into the fluidized bed.
  • the volatile bases are added to the fluidizing air supplied for granulation and drying in the fluidized bed apparatus.
  • the aqueous, optionally pH neutral adjusted anionic surfactant preparations are injected here in the fluidized bed apparatus and are only there in the presence of the fluidized air supplied with the volatile bases, preferably ammonia as a gas, granulated and dried.
  • the volatile bases preferably ammonia as a gas
  • aqueous surfactant preparations containing anionic surfactants can be granulated alone or mixed with solid support materials in the fluidized bed and dried at the same time.
  • the water evaporates from the preparation (paste), resulting in dried to dried germs, which are coated with the optionally admixed carrier materials, granulated and dried again at the same time.
  • carrier materials are to be mixed, they are mixed simultaneously with the aqueous surfactant preparations (pastes), but separately from these, preferably via an automatically controlled solids dosage.
  • carrier materials are mixed in the context of the invention, these are preferably inorganic carrier materials and in particular alkali metal carbonates, alkali metal sulphates, crystalline or amorphous alkali metal silicates, crystalline or amorphous sheet silicates and / or zeolites.
  • the proportion of carrier materials to surfactant is not critical and may be in the weight ratio of 0: 100 to 50: 50, preferably 80:20.
  • Preferably used fluidized bed apparatuses have bottom plates (sieve bottom) with a diameter between 0.4 and 5 m, for example 1.2 m or 2.5 m.
  • a bottom plate perforated bottom plates a Contidurplatte (commercial product of the company Hein & Lehmann, Federal Republic of Germany) or perforated bottom plates can be used, the holes (openings) are covered by a mesh with meshes less than 600 microns.
  • the grid can be arranged within or above the passage openings. However, the grid is preferably located directly below the openings of the inflow base.
  • a metal gauze is sintered with the appropriate mesh size.
  • the metal gauze consists of the same material as the distributor plate, in particular of stainless steel.
  • the mesh size of said grid is between 200 and 400 microns.
  • the process is preferably carried out at fluidized air velocities of between 1 and 8 m / s and in particular between 1.5 and 5.5 m / s.
  • the discharge of the granules is advantageously carried out by size classification of the granules. This classification is preferably carried out by means of an opposing air flow (classifier air), which is regulated so that only particles from a certain particle size removed from the fluidized bed and smaller particles are retained in the fluidized bed.
  • the incoming air is composed of the heated or unheated classifier air and the heated floor air.
  • the soil air temperature is preferably between 80 and 400 ° C.
  • the fluidizing air is cooled by heat losses and by the heat of vaporization and is preferably about 5 cm above the bottom plate 60 to 120 ° C, preferably 65 to 90 ° C and especially 70 to 85 ° C.
  • the air outlet temperature is preferably between 60 and 120 ° C, in particular below 80 ° C.
  • a starting material which serves as an initial carrier for the sprayed surfactant paste.
  • Suitable starting compounds are the surfactant granules optionally containing carrier materials themselves, which have already been obtained in a preceding process sequence, or the carrier materials can be used as starting material.
  • surfactant granules obtained with a particle size in the range between 0.1 and 1.6 mm are already used as starting material from one of the preceding process sequences.
  • the granules obtained from the fluidized bed are then preferably cooled in a separate fluidized bed and classified by means of a sieve into granules with particle sizes between 0.1 and 1.6 mm as a good grain fraction and in granules above 1.6 mm as an oversize fraction, while particles below 0, 1 mm already in the fluidized bed in an exhaust filter during drying, separated there from the exhaust air and then fed as seed material back into the fluidized bed.
  • the oversize fraction is ground and also returned to the fluidized bed.
  • the surfactant granules are considered to be dried, provided that the content of free water is preferably below 10% by weight, in particular from 0.1 to 2% by weight, based in each case on the finished granules.
  • surfactant granules are obtained with high bulk density, preferably above 500 g / l and in particular between 550 and 1000 g / l.
  • the active substance content varies depending on the addition of carrier materials used and in particular is more than 50% by weight, preferably between 85 and 98% by weight.
  • the surfactant granules obtained by the process of the invention are pH neutral, i. after dissolution of the surfactant granules in water, the aqueous solution has a pH between 7 and 9.5. Furthermore, the surfactant granules are dust-free and pourable and not or barely tacky, so that they are easy to handle in big bags and siliertransport.
  • the granules according to the invention may be present in customary amounts, preferably in the range from 0.1 to 50% by weight, based on average.
  • the surfactant granules produced according to the invention are preferably suitable for the preparation of pH-neutral detergents, dishwashing detergents and cleaners, such as pH-neutral powder cleaners and pH-neutral soaps, and also detergents, such as toilet stones, mixed with dyes.
  • the pH-neutral washing, rinsing and cleaning agents may be in powdery, granulated or particulate form.
  • a 1% aqueous solution of the granules showed a pH of 8.8 at 25 ° C.
  • 500 g of this sodium lauryl sulfate granules were stored at 80 ° C. for 72 hours in a porcelain dish in a drying oven. After this time, no gray specks could be detected in the product.
  • Example 1 10,000 kg of a 65 wt .-% sodium lauryl sulfate (52% C12 / 21% C 14/10% C 16/17% C 18) containing aqueous paste with a free alkali content of 0.1 wt .-% sodium hydroxide continuously injected with 2000 kg per hour at a temperature of 70 ° C in the fluidized bed plant (SKET plant), wherein the drying air had on entering the fluidized bed at a temperature of 180 ° C, at the outlet of 90 ° C.
  • the fluidized bed had a temperature of 70 ° C. 24 kg of a 25% aq.
  • Ammonia solution was mixed by means of a forced-controlled Multi-piston metering pump fed continuously together with the aqueous surfactant paste in the fluidized bed of the SKET system.
  • a 1% aqueous solution of the granules showed a pH of 9.5 at 25 ° C.
  • 500 g of this sodium lauryl sulfate granules were stored at 80 ° C. for 72 hours in a porcelain dish in a drying oven. After this time, no gray specks could be detected in the product.
  • Example 1 10,000 kg of a 65 wt .-% sodium lauryl sulfate (52% C12 / 21% C 14/10% C 16/17% C 18) containing aqueous paste with a free alkali content of 0.1 wt .-% sodium hydroxide continuously injected with 2,000 kg per hour at a temperature of 70 ° C in the fluidized bed plant (SKET plant), wherein the drying air had on entering the fluidized bed at a temperature of 160 ° C, at the outlet of 90 ° C.
  • the fluidized bed had a temperature of 60 ° C.
  • a 1% aqueous solution of the granules showed a pH of 9.2 at 25 ° C.
  • 500 g of this sodium lauryl sulfate granules were stored at 80 ° C. for 72 hours in a porcelain dish in a drying oven. After this time, gray specks appeared isolated in the product, which were isolated and had an acidic pH.

Landscapes

  • Chemical & Material Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Cosmetics (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Medicinal Preparation (AREA)
  • Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)

Claims (7)

  1. Procédé pour la préparation de granulats d'agents tensioactifs, la solution aqueuse après la dissolution dans de l'eau présentant un pH entre 7 et 9,5, par granulation et séchage simultané d'une composition d'agents tensioactifs aqueuse, contenant des agents tensioactifs anioniques sous forme de sel dans une couche tourbillonnante, caractérisé en ce qu'on ajoute, avant ou pendant la granulation et le séchage simultané, des bases volatiles, sous forme des solutions aqueuses, en des quantités de 0,05 à 5% en poids - par rapport à la substance active des agents tensioactifs anioniques dans la composition aqueuse d'agents tensioactifs.
  2. Procédé selon la revendication 1, caractérisé en ce qu'on utilise comme compositions aqueuses d'agents tensioactifs des pâtes aqueuses d'agents tensioactifs anioniques présentant une teneur en agents tensioactifs de 25 à 90% en poids - par rapport à la pâte.
  3. Procédé selon l'une quelconque des revendications 1 ou 2, caractérisé en ce qu'on utilise comme agents tensioactifs anioniques des sulfates d'alcools gras comprenant 6 à 22 atomes de carbone sous forme de leurs sels.
  4. Procédé selon l'une quelconque des revendications 1 ou 2, caractérisé en ce qu'on utilise comme agents tensioactifs anioniques des sulfates d'oxoalcools comprenant 6 à 15 atomes de carbone sous forme de leurs sels.
  5. Procédé selon l'une quelconque des revendications 1 à 4, caractérisé en ce qu'on utilise comme base volatile de l'ammoniaque aqueuse.
  6. Procédé selon l'une quelconque des revendications 1 à 5, caractérisé en ce que la granulation et le séchage simultané sont réalisés en mélangeant un ou plusieurs solides inorganiques et/ou organiques.
  7. Procédé selon l'une quelconque des revendications 1 à 6, caractérisé en ce que la granulation et le séchage simultané sont réalisés dans une couche tourbillonnante continue (procédé SKET), où l'évacuation des granulats de la couche tourbillonnante est réalisée via une classification des grosseurs.
EP99963299A 1998-11-23 1999-11-13 Procede de production de granules tensioactifs Expired - Lifetime EP1131400B1 (fr)

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
DE19853893 1998-11-23
DE19853893A DE19853893A1 (de) 1998-11-23 1998-11-23 Verfahren zur Herstellung von Tensidgranulaten
PCT/EP1999/008763 WO2000031230A1 (fr) 1998-11-23 1999-11-13 Procede de production de granules tensioactifs

Publications (2)

Publication Number Publication Date
EP1131400A1 EP1131400A1 (fr) 2001-09-12
EP1131400B1 true EP1131400B1 (fr) 2010-12-22

Family

ID=7888656

Family Applications (1)

Application Number Title Priority Date Filing Date
EP99963299A Expired - Lifetime EP1131400B1 (fr) 1998-11-23 1999-11-13 Procede de production de granules tensioactifs

Country Status (5)

Country Link
EP (1) EP1131400B1 (fr)
AT (1) ATE492626T1 (fr)
DE (2) DE19853893A1 (fr)
ES (1) ES2357380T3 (fr)
WO (1) WO2000031230A1 (fr)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022238210A1 (fr) 2021-05-10 2022-11-17 Basf Se Sulfates d'éther à base de mélanges d'alcools tridécyliques isomères

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
EP2801606A1 (fr) * 2013-05-07 2014-11-12 The Procter and Gamble Company Particule séchée par pulvérisation comprenant du sulfate

Family Cites Families (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE4216629A1 (de) * 1992-05-20 1993-11-25 Henkel Kgaa Verfahren zur Herstellung aniontensidhaltiger Wasch- und Reinigungsmittel
DE4304062A1 (de) * 1993-02-11 1994-08-18 Henkel Kgaa Verfahren zur Herstellung von Tensidgranulaten
DE19707649C1 (de) * 1997-02-26 1998-10-22 Henkel Kgaa Verfahren zur Herstellung von Waschmittelrohstoffen
DE19710152C2 (de) * 1997-03-12 1999-04-22 Henkel Kgaa Verfahren zur Herstellung von Aniontensidgranulaten

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022238210A1 (fr) 2021-05-10 2022-11-17 Basf Se Sulfates d'éther à base de mélanges d'alcools tridécyliques isomères

Also Published As

Publication number Publication date
ATE492626T1 (de) 2011-01-15
DE19853893A1 (de) 2000-05-25
ES2357380T3 (es) 2011-04-25
DE59915230D1 (de) 2011-02-03
WO2000031230A1 (fr) 2000-06-02
EP1131400A1 (fr) 2001-09-12

Similar Documents

Publication Publication Date Title
EP0474915B2 (fr) Détergent
EP0603207B1 (fr) Procede de fabrication de granulats tensioactifs
EP0725813B1 (fr) Utilisation de melanges detergents pour la fabrication de blocs desodorisants pour toilettes
EP0541608B1 (fr) Procede de production de granules actifs de lavage et de nettoyage
EP0632826B1 (fr) Procede de fabrication de produits de lavage et de detergents coulants se presentant sous forme de granules et/ou de granules partiels
WO1993015180A1 (fr) Procede pour fabriquer des produits solides de lavage et de nettoyage de densite apparente elevee et presentant une vitesse de dissolution amelioree
EP0966515B1 (fr) Procede de preparation de matieres premieres detergentes
DE19524464C2 (de) Verfahren zur Herstellung von Zuckertensidgranulaten
EP0796318B1 (fr) Preparations solides coulantes
WO1992013938A1 (fr) Melange pulverulent d'agents tensio-actifs
EP1131400B1 (fr) Procede de production de granules tensioactifs
EP1078029B1 (fr) Granules de sulfate d'alkyle
EP0457965B1 (fr) Détergents pour machine à laver qui forment peu de mousse
EP0859048A2 (fr) Procédé pour la fabrication de granules tensioactifs
DE19806495C1 (de) Verfahren zur Herstellung wasser- und staubfreier Aniontensidgranulate
EP0876454B1 (fr) Produits de depart liquides pour agents de lavage, de rin age et de nettoyage
WO2001046375A1 (fr) Procede de production de granules de tensioactifs de sucre
WO1999010470A1 (fr) Utilisation de sulfates d'ester de polyglycol d'acide gras
DE19817509C2 (de) Verwendung von Fettsäurepolyglycolestersulfaten
EP0929647B1 (fr) Procede de production de granules de tensioactifs anioniques anhydres et sans poussiere
WO1999036495A1 (fr) Granules tensioactifs homogenes pour la production de detergents et de nettoyants en morceaux
DE19520105A1 (de) Verfahren zur Herstellung wasserfreier, rieselfähiger Tensidpulver
WO1996020271A1 (fr) Procede de preparation d'agents tensioactifs exempts d'eau
WO1999010459A1 (fr) Procede de production de granules d'agents de surface anioniques exempts d'eau et de poussiere

Legal Events

Date Code Title Description
PUAI Public reference made under article 153(3) epc to a published international application that has entered the european phase

Free format text: ORIGINAL CODE: 0009012

17P Request for examination filed

Effective date: 20010512

AK Designated contracting states

Kind code of ref document: A1

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: COGNIS DEUTSCHLAND GMBH & CO. KG

RAP1 Party data changed (applicant data changed or rights of an application transferred)

Owner name: COGNIS IP MANAGEMENT GMBH

17Q First examination report despatched

Effective date: 20060628

GRAJ Information related to disapproval of communication of intention to grant by the applicant or resumption of examination proceedings by the epo deleted

Free format text: ORIGINAL CODE: EPIDOSDIGR1

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

RIC1 Information provided on ipc code assigned before grant

Ipc: C11D 1/29 20060101ALN20100504BHEP

Ipc: C11D 1/28 20060101ALN20100504BHEP

Ipc: C11D 1/14 20060101ALN20100504BHEP

Ipc: C11D 11/04 20060101ALI20100504BHEP

Ipc: C11D 17/06 20060101ALI20100504BHEP

Ipc: C11D 11/00 20060101AFI20100504BHEP

GRAP Despatch of communication of intention to grant a patent

Free format text: ORIGINAL CODE: EPIDOSNIGR1

RIC1 Information provided on ipc code assigned before grant

Ipc: C11D 11/04 20060101ALI20100713BHEP

Ipc: C11D 17/06 20060101ALI20100713BHEP

Ipc: C11D 11/00 20060101AFI20100713BHEP

GRAS Grant fee paid

Free format text: ORIGINAL CODE: EPIDOSNIGR3

GRAA (expected) grant

Free format text: ORIGINAL CODE: 0009210

AK Designated contracting states

Kind code of ref document: B1

Designated state(s): AT BE CH CY DE DK ES FI FR GB GR IE IT LI LU MC NL PT SE

REG Reference to a national code

Ref country code: GB

Ref legal event code: FG4D

Free format text: NOT ENGLISH

REG Reference to a national code

Ref country code: CH

Ref legal event code: EP

REG Reference to a national code

Ref country code: IE

Ref legal event code: FG4D

REF Corresponds to:

Ref document number: 59915230

Country of ref document: DE

Date of ref document: 20110203

Kind code of ref document: P

REG Reference to a national code

Ref country code: DE

Ref legal event code: R096

Ref document number: 59915230

Country of ref document: DE

Effective date: 20110203

REG Reference to a national code

Ref country code: NL

Ref legal event code: VDEP

Effective date: 20101222

REG Reference to a national code

Ref country code: ES

Ref legal event code: FG2A

Ref document number: 2357380

Country of ref document: ES

Kind code of ref document: T3

Effective date: 20110425

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CY

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20101222

Ref country code: FI

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20101222

Ref country code: SE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20101222

REG Reference to a national code

Ref country code: IE

Ref legal event code: FD4D

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: PT

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20110422

Ref country code: GR

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20110323

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: NL

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20101222

PLBE No opposition filed within time limit

Free format text: ORIGINAL CODE: 0009261

STAA Information on the status of an ep patent application or granted ep patent

Free format text: STATUS: NO OPPOSITION FILED WITHIN TIME LIMIT

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: IE

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20101222

Ref country code: DK

Free format text: LAPSE BECAUSE OF FAILURE TO SUBMIT A TRANSLATION OF THE DESCRIPTION OR TO PAY THE FEE WITHIN THE PRESCRIBED TIME-LIMIT

Effective date: 20101222

26N No opposition filed

Effective date: 20110923

REG Reference to a national code

Ref country code: DE

Ref legal event code: R097

Ref document number: 59915230

Country of ref document: DE

Effective date: 20110923

BERE Be: lapsed

Owner name: COGNIS IP MANAGEMENT G.M.B.H.

Effective date: 20111130

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: MC

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20111130

REG Reference to a national code

Ref country code: CH

Ref legal event code: PL

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: CH

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20111130

Ref country code: LI

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20111130

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: BE

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20111130

REG Reference to a national code

Ref country code: AT

Ref legal event code: MM01

Ref document number: 492626

Country of ref document: AT

Kind code of ref document: T

Effective date: 20111113

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: AT

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20111113

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: LU

Free format text: LAPSE BECAUSE OF NON-PAYMENT OF DUE FEES

Effective date: 20111113

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 17

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 18

REG Reference to a national code

Ref country code: FR

Ref legal event code: PLFP

Year of fee payment: 19

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: ES

Payment date: 20181218

Year of fee payment: 20

Ref country code: FR

Payment date: 20181127

Year of fee payment: 20

Ref country code: GB

Payment date: 20181130

Year of fee payment: 20

Ref country code: IT

Payment date: 20181122

Year of fee payment: 20

PGFP Annual fee paid to national office [announced via postgrant information from national office to epo]

Ref country code: DE

Payment date: 20190131

Year of fee payment: 20

REG Reference to a national code

Ref country code: DE

Ref legal event code: R071

Ref document number: 59915230

Country of ref document: DE

REG Reference to a national code

Ref country code: GB

Ref legal event code: PE20

Expiry date: 20191112

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: GB

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20191112

REG Reference to a national code

Ref country code: ES

Ref legal event code: FD2A

Effective date: 20200806

PG25 Lapsed in a contracting state [announced via postgrant information from national office to epo]

Ref country code: ES

Free format text: LAPSE BECAUSE OF EXPIRATION OF PROTECTION

Effective date: 20191114