NO850289L - POWDER DETERGENTS AND PROCEDURES FOR PREPARING THIS - Google Patents

POWDER DETERGENTS AND PROCEDURES FOR PREPARING THIS

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Publication number
NO850289L
NO850289L NO850289A NO850289A NO850289L NO 850289 L NO850289 L NO 850289L NO 850289 A NO850289 A NO 850289A NO 850289 A NO850289 A NO 850289A NO 850289 L NO850289 L NO 850289L
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carbon atoms
weight
atoms
fabric softener
component
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NO850289A
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Norwegian (no)
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Helmut Hein
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Rewo Chemische Werke Gmbh
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    • 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
    • C11D3/0005Other compounding ingredients characterised by their effect
    • C11D3/001Softening compositions
    • 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
    • C11D1/38Cationic compounds
    • C11D1/62Quaternary ammonium compounds
    • 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
    • C11D3/12Water-insoluble compounds
    • C11D3/124Silicon containing, e.g. silica, silex, quartz or glass beads

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Detergent Compositions (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

1. A detergent based on anionic and non-ionic surfactants that has fabric-softening properties, characterized in that it contains, as fabric softener, from 5 to 25 % by weight of a powdered fabric-softening agent consisting of A) from 60 to 80 % by weight of a fabric softener based on one or more nitrogenous cationic surface-active substances having at least one hydrocarbon group that is attached to the nitrogen atom and has at least 8 carbon atoms, which softener optionally contains conventional additives, wherein the surface-active substances consist of at least one of the following compounds : a) a quaternary ammonium compound of the formula see diagramm : EP0151936,P6,F1 wherein R**1 and R**2 are alkyl radicals having from 8 to 24 C-atoms, R**3 and R**4 are alkyl radicals having from 1 to 4 C-atoms, and A- is an anion, b) an alkylimidazolinium compound of the general formula see diagramm : EP0151936,P7,F2 wherein R**5 is an alkyl radical having from 1 to 4 C-atoms, R**6 is an alkyl radical having from 8 to 25 C-atoms, R**7 is an alkyl radical having from 1 to 4 C-atoms or is hydrogen, and R**8 is an alkyl radical having from 8 to 25 C-atoms, and A- is an anion, c) a quaternary ammonium compound of the general formula see diagramm : EP0151936,P7,F3 wherein R**9 and R**10 are alkyl radicals having from 8 to 24 C-atoms or are fatty acid amidoalkyl radicals, R**11 is an alkyl radical having from 1 to 4 C-atoms, R**12 is hydrogen or methyl, x is an interger from 1 to 5, and A- is an anion, and B) from 20 to 40 % by weight of a highly adsorbent silicic acid having a surface area of from approximately 250 to approximately 600 m**2/g, wherein component A) has been adsorbent onto component B).

Description

Trommelvaskemaskiner, som hovedsakelig er vanligeDrum washing machines, which are mainly ordinary

i europeiske husholdinger, vasker som regel i to arbeids-operasjoner. I hovedvaskeoperasjonen blir vasken først renset ved hjelp av et vaskepulver. Derpå følger flere spyleoperasjoner. I det siste spylebad tilsettes et vaskemykningsmiddel ved efterbehandlingen. Dette skal gi vasken et mykt, flosset grep og behagelige bæreegenskaper, også når vasken må tørres under ugunstige betingelser. in European households, as a rule, washes in two working operations. In the main washing operation, the sink is first cleaned using a washing powder. This is followed by several flushing operations. In the last rinse bath, a fabric softener is added during the finishing process. This should give the wash a soft, frayed grip and comfortable carrying properties, even when the wash has to be dried under unfavorable conditions.

Forsøk på å forene vaskebehandlingene i en enkelt vaskeoperasjon, dvs. tilsette mykneren allerede til vaskepulveret, er allerede foretatt i mange tilfelle. Attempts to combine the washing treatments in a single washing operation, i.e. adding the softener already to the washing powder, have already been carried out in many cases.

De tidligere løsningsforsøk har overveiende den ulempe at den myknende virkning går tapt. Dette skyldes at det kationiske mykningsmiddel med det i overskudd tilstedeværende anioniske tensid i vaskemidlet danner tungtoppløselige salter og forblir uvirksomt i vaskevæsken. Derved er efter den avsluttende spyling neppe noen kationisk mykner påvisbar på tekstilet ennå. Slike produkter viser da også en meget utilfredsstillende mykgjørende virkning. The previous solution attempts mainly have the disadvantage that the softening effect is lost. This is because the cationic softener with the anionic surfactant present in excess in the detergent forms poorly soluble salts and remains inactive in the washing liquid. Thereby, after the final rinse, hardly any cationic softener is still detectable on the textile. Such products then also show a very unsatisfactory softening effect.

Allerede fremstillingen av slike vaskemidler inneholdende vaskemykningsmidler er problematisk. Ved fremstillingen av vaskepulver blir som reget et flytende forkonsentrat fremstilt (slurry) som derpå underkastes sprøytetørring. Already the production of such detergents containing fabric softeners is problematic. In the production of washing powder, as usual, a liquid pre-concentrate is produced (slurry) which is then subjected to spray drying.

Hvis mykningsmidlet allerede tilsettes dette forkonsentrat, danner det seg straks ved vaskemiddelfremstillingen et salt med de anioniske tensider. If the softener is already added to this pre-concentrate, a salt with the anionic surfactants is immediately formed during the preparation of the detergent.

Den ønskede forsinkede virksomhet er altså bare opp-nåelig når det kationiske mykningsmiddel foreligger i pulver-form og vaskepulveret deretter tilblandes. Da det kationiske mykningsmiddel imidlertid har en lavere krystallisa-sjonstilbøyelighet, er fremgangsmåten ved sprøytetørring ikke anvendbar. Også fremgangsmåten ved valsetørring gir på grunn av den langsomme krystallisasjon og konsolidering av produktet betraktelige vanskeligheter. Dessuten blir derved betraktelig krystallisasjonsvarme frigjort, hvilket fører til at det ferdig fremstilte pulver igjen sammenbakes. The desired delayed operation is therefore only achievable when the cationic softener is in powder form and the washing powder is then mixed in. However, since the cationic plasticizer has a lower crystallisation tendency, the method of spray drying is not applicable. Due to the slow crystallization and consolidation of the product, the method of roller drying also presents considerable difficulties. In addition, considerable heat of crystallization is thereby released, which causes the finished powder to be baked together again.

Det er derfor et behov for et pulverformig vaskemykningsmiddel som kan fremstilles problemfritt og kan til blandes til vanlige vaskemiddelpulvere og ved hvilket de ønskede mykningsegenskaper ikke går tapt i vaskeoperasjonen. There is therefore a need for a powdered detergent softener which can be produced without problems and can be mixed into ordinary detergent powders and in which the desired softening properties are not lost during the washing operation.

Et slikt pulverformig vaskemykningsmiddel fremstilles ifølge oppfinnelsen. Det består ifølge oppfinnelsen av: A) 60 til 80 vekt% av et vaskemykningsmiddel på basis av ett eller flere nitrogenholdige kationiske overflateaktive stoffer med i det minste en til nitrogenatomet bundet hydrocarbongruppe med minst 8 carbonatomer som eventuelt inneholder vanlige hjelpestoffer med stabiliserende eller gjenfuktende virkning og/eller tilsetningsstoffer, B) 20 til 40 vekt% høysugedyktig kiselsyre, idet komponenten A) er adsorbert på komponenten B). Such a powdered fabric softener is produced according to the invention. According to the invention, it consists of: A) 60 to 80% by weight of a fabric softener based on one or more nitrogen-containing cationic surface-active substances with at least one hydrocarbon group with at least 8 carbon atoms bound to the nitrogen atom, which possibly contains common auxiliary substances with a stabilizing or re-moistening effect and /or additives, B) 20 to 40% by weight highly absorbent silicic acid, the component A) being adsorbed on the component B).

Som kationiske overflateaktive stoffer kan man anvende de som vaskemyknere kjente lipofile grupper inneholdende kvartære ammoniumforbindelser og alkylimidazoliniumforbindelser med overflateaktive egenskaper. Slike forbindelser er f.eks. beskrevet i Chemistry and Industry, 1969, s. 893 - 894. As cationic surfactants, the lipophilic groups known as detergent softeners containing quaternary ammonium compounds and alkylimidazolinium compounds with surface-active properties can be used. Such compounds are e.g. described in Chemistry and Industry, 1969, pp. 893-894.

Fortrinnsvis består de pulverformige overflateaktive stoffer i komponent A) av minst én av de følgende forbindelser : Preferably, the powdered surfactants in component A) consist of at least one of the following compounds:

a) kvartære ammoniumforbindelser med formel:a) quaternary ammonium compounds of formula:

hvor R 1 og R 2er alkylgrupper med 8-24 carbonatomer, og where R 1 and R 2 are alkyl groups with 8-24 carbon atoms, and

R 3 og R<4>er alkylgrupper med 1-4 carbonatomer, og A- er et anion. b) Alkylimidazoliniumforbindelser med den generelle formel: R 3 and R<4> are alkyl groups with 1-4 carbon atoms, and A- is an anion. b) Alkylimidazolinium compounds with the general formula:

hvor R 5 er en alkylgruppe med 1-4 carbonatomer, R<6>er en alkylgruppe med 8-25 carbonatomer, R<7>er en alkylgruppe med 1-4 carbonatomer eller hydrogen, og R ger en alkylgruppe med 8-25 carbonatomer, og A- er et anion, eksempelvis methosulfat, ethosulfat eller et halogen. c) Kvartære ammoniumforbindelser med den generelle formel: where R 5 is an alkyl group with 1-4 carbon atoms, R<6>is an alkyl group with 8-25 carbon atoms, R<7>is an alkyl group with 1-4 carbon atoms or hydrogen, and R gives an alkyl group with 8-25 carbon atoms , and A- is an anion, for example methosulfate, ethosulfate or a halogen. c) Quaternary ammonium compounds with the general formula:

9 10 9 10

hvor R og R er alkylgrupper med 8 og 24 carbonatomer inneholdende fettsyreamidoalkylgrupper, R"^ er en alkylgruppe med 1-4 carbonatomer, R " er hydrogen eller methyl, x er et tall fra 1 - 5, og A- er et anion. where R and R are alkyl groups with 8 and 24 carbon atoms containing fatty acid amidoalkyl groups, R"^ is an alkyl group with 1-4 carbon atoms, R " is hydrogen or methyl, x is a number from 1 - 5, and A- is an anion.

Særlig foretrukket er herunder l-methyl-2-alkyl-3-fettsyreamidoethylimidazoliniummethosulfat. Among them, 1-methyl-2-alkyl-3-fatty acid amidoethylimidazolium methosulphate is particularly preferred.

Som grupper R"*", R", R^, R^, R^ og R anvendes vanligvis fettsyrealkylgrupper, fortrinnsvis med en C-kjedelengde på C 16 til C 18. As groups R"*", R", R^, R^, R^ and R, fatty acid alkyl groups are usually used, preferably with a C chain length of C 16 to C 18.

En rekke andre forbindelser som kommer på tale, er nevnt i EU - A - 406 og DE - A - 30 25 369. Særlig nevnes: methyl-bis-(talgamidoethyl)-2-hydroxypropylammoniummetholsul-fat, N,N-dimethyl-bis-(isopropanol-oljesyreester)-ammonium-metholsulfat, N-talg-pentamethylpropylendiammoniumklorid. A number of other compounds that come into question are mentioned in EU - A - 406 and DE - A - 30 25 369. Particular mention is made of: methyl-bis-(talgamidoethyl)-2-hydroxypropylammonium metholsulphate, N,N-dimethyl-bis -(isopropanol-oleic acid ester)-ammonium-methol sulfate, N-tallow-pentamethylpropylenediammonium chloride.

Som egnede hjelpestoffer kommer særlig ikke-ionogene tensider -i betraktning, som de f.eks. er beskrevet i DE - A - 30 25 369, særlig reaksjonsprodukter av fettsyre-ethanolamid eller fettsyreaminer med ethylenoxyd og/eller propylenoxyd som virker som dispergerings- eller emulgerings-midler, og eventuelt oppviser en ytterligere mykgjørende virkning. Non-ionic surfactants in particular come into consideration as suitable excipients, such as those e.g. is described in DE - A - 30 25 369, in particular reaction products of fatty acid ethanolamide or fatty acid amines with ethylene oxide and/or propylene oxide which act as dispersing or emulsifying agents, and possibly exhibit a further softening effect.

Andre ikke-ionogene emulgatorer er slike på basis av oxyalkylater, f.eks. reaksjonsprodukter av ethylenoxyd med alkylfenoler eller fettalkoholer. Som eksempel på slike hjelpestoffer kan nevnes: oleylalkoholpolyglycolether, nonylfenolpolyglycolether eller stearinsyremonoglycerid-polyglycolether. Other non-ionic emulsifiers are those based on oxyalkylates, e.g. reaction products of ethylene oxide with alkylphenols or fatty alcohols. Examples of such auxiliary substances can be mentioned: oleyl alcohol polyglycol ether, nonylphenol polyglycol ether or stearic acid monoglyceride polyglycol ether.

Vanlige tilsetningsstoffer er særlig duftstoffer, farvestoffer og optiske lysnere. Common additives are in particular fragrances, dyes and optical brighteners.

Som komponent B) anvendes en høysugedyktig kiselsyre særlig en med 250 til 600 m 2 /g, fortrinnsvis 350 til 500 m 2/g As component B) a highly absorbent silicic acid is used, particularly one with 250 to 600 m 2 /g, preferably 350 to 500 m 2 /g

(BET) .(BET) .

Egnede findelte, høysugedyktige bærer-kiselsyrer med størst mulig spesifikk overflate, fremstilles ved felning og sprøytetørring og kan erholdes i handelen. Suitable finely divided, highly absorbent carrier silicic acids with the largest possible specific surface are produced by felting and spray drying and can be obtained commercially.

En fremgangsmåte ifølge oppfinnelsen til fremstilling av pulverformige vaskemykningsmidler, erkarakterisert vedat man påfører 60 - 80 vektdeler av et vaskemykningsmiddel på basis av ett eller flere nitrogenholdige kationiske overflateaktive stoffer med minst én til nitrogenatomet bundet hydrocarbongruppe med minst 8 carbonatomer som eventuelt inneholder vanlige hjelpestoffer med stabiliserende eller gjenfuktende virkning og/eller tilsetningsstoffer, i en pulverblander, eventuelt sammen med hjelpe- og/eller duftstoffer på 20 - 40 vektdeler høysugedyktig kiselsyre. A method according to the invention for the production of powdery fabric softeners is characterized by applying 60 - 80 parts by weight of a fabric softener based on one or more nitrogen-containing cationic surface-active substances with at least one hydrocarbon group bound to the nitrogen atom with at least 8 carbon atoms, which possibly contain common auxiliary substances with stabilizing or moisturizing effect and/or additives, in a powder mixer, possibly together with auxiliaries and/or fragrances of 20 - 40 parts by weight highly absorbent silicic acid.

En egnet blander er eksempelvis den i handelen værende "Pflugschar-blander". A suitable mixer is, for example, the commercially available "Pflugschar mixer".

Kiselsyren tilblandes den kationiske mykner, idet hver av de ovenfor nevnte kvartære imidazolinium- og ammoniumforbindelser kan medanvendes, likegyldig hvilken struktur den enkelte har. Videre påvirkes ikke egenskapene av mykneren ved typen av anionet. Det er herved også likegyldig om mykneren foreligger i flytende form eller først må smeltes for å tilsettes kiselsyren som smelte. De i handelen til-gjengelige kvartære myknere inneholder videre ofte oppløs-ningsmidler, særlig lavere alkoholer og glycoler, som f.eks. isopropanol, 1,2-propylenglycol eller hexylenglycol. Disse oppløsningsmidler forstyrrer i alminnelighet ikke, dvs. The silicic acid is mixed with the cationic plasticizer, as each of the quaternary imidazolinium and ammonium compounds mentioned above can be used together, regardless of the structure of the individual. Furthermore, the properties of the plasticizer are not affected by the type of anion. It is also irrelevant whether the plasticizer is in liquid form or must first be melted in order to add the silicic acid as a melt. The commercially available quaternary plasticizers also often contain solvents, especially lower alcohols and glycols, such as e.g. isopropanol, 1,2-propylene glycol or hexylene glycol. These solvents generally do not interfere, i.e.

en mykner med inntil 25% isopropanol kan blandes med f.eks. kiselsyre til et fint pulver. a plasticizer with up to 25% isopropanol can be mixed with e.g. silicic acid to a fine powder.

Herved er det i alminnelighet ved viderebearbeidelsen av pulveret nødvendig å treffe sikkerhetsforholdsregler på grunn av de dannede oppløsningsmiddeldamper. In this way, it is generally necessary to take safety precautions during the further processing of the powder due to the solvent vapors formed.

Likeledes kan vaskemykningsmidler som bringes i handelen i de ovennevnte ikke-ionogene tensider, påføres på slike oppløsninger på kiselsyren. De sammen med den kationiske vaskemykner påførte ikke-ioniske tensider, forstyrrer selvsagt ikke ved vaskebehandlingen. Likewise, detergent softeners that are sold in the above-mentioned non-ionic surfactants can be applied to such solutions on the silicic acid. The non-ionic surfactants applied together with the cationic fabric softener obviously do not interfere with the washing process.

Oppfinnelsen angår videre et vaskemiddel med mykgjør-ende egenskaper som erkarakterisert vedat det som vaskemykningsmiddel inneholder 5 til 2 5 vekt% av et pulverformig vaskemykningsmiddel som består av A) 60 til 80 vekt% av et vaskemykningsmiddel på basis av ett eller flere nitrogenholdige, kationiske, overflateaktive stoffer med minst én til nitrogenatomet bundet hydrocarbongruppe med minst 8 carbonatomer, som eventuelt inneholder vanlige hjelpestoffer med stabiliserende eller gjenværende virkning og/eller tilsetningsstoffer, The invention further relates to a detergent with softening properties which is characterized in that it contains, as detergent softener, 5 to 25% by weight of a powdered detergent softener consisting of A) 60 to 80% by weight of a detergent softener based on one or more nitrogen-containing, cationic, surface-active substances with at least one hydrocarbon group with at least 8 carbon atoms bound to the nitrogen atom, which possibly contain common auxiliary substances with a stabilizing or residual effect and/or additives,

og and

B) 20 til 40 vekt% høysugedyktig kiselsyre, idet komponenten A) er adsorbert på komponenten B). B) 20 to 40% by weight highly absorbent silicic acid, the component A) being adsorbed on the component B).

Det pulverformige vaskemykningsmiddel kan ifølge oppfinnelsen problemfritt blandes til de vanlige husholdnings-vaskemidler for fullvask eller 60°-vask. According to the invention, the powdered fabric softener can easily be mixed with the usual household detergents for full washing or 60° washing.

Herved skal det passes på at kornstørrelsen av vaskepulver og vaskemykningspulver ifølge oppfinnelsen ikke er for forskjellig slik at en adskillelse unngåes. Vaskepulver ligger for det meste i et størrelsesområde fra 450 til 500^u. Et typisk- mykningspulver ifølge eksempel 2 oppviser en korn-størrelsesfordeling ifølge følgende siktanalyse: 100 - 200 u : 10,9 % Hereby, care must be taken that the grain size of washing powder and washing softening powder according to the invention is not too different so that a separation is avoided. Washing powder is mostly in a size range from 450 to 500 ^u. A typical softening powder according to example 2 exhibits a grain size distribution according to the following sieve analysis: 100 - 200 u : 10.9%

200 - 300 n : 47,2 % 200 - 300 n : 47.2%

300 - 400 n : 29,1 % 300 - 400 n : 29.1%

400 - 500 n : 12,8 % 400 - 500 n : 12.8%

Denne fordeling er som regel egnet. For bedre til-pasning til kornstørrelsen av vaskemidlet kan myknings-pulveret ved en passende føring av hastighet og temperatur av plogskjærblanderen pågranuleres. Derved økes kornstørr-elsen til det to- til tredobbelte. This distribution is usually suitable. For a better adaptation to the grain size of the detergent, the softening powder can be granulated by suitable control of speed and temperature of the ploughshare mixer. Thereby, the grain size is increased two to threefold.

Egnede typiske vaskemiddelformuleringer med tilsvarende rammereseptur er eksempelvis beskrevet i Tensid-Taschenbuch, 2. oppi., Carl Hanser Verlag, Miinchen/Wien og i "Wasch-mittelchemie", Hiithig-Verlag, Heidelberg (1976). Suitable typical detergent formulations with corresponding framework recipes are described, for example, in Tensid-Taschenbuch, 2nd oppi., Carl Hanser Verlag, Munich/Vienna and in "Wasch-mittelchemie", Hiithig-Verlag, Heidelberg (1976).

Slike vaskemidler er vanligvis basert på anioniske og ikke-ioniske tensider såvel som eventuelt skuminhibitorer, og inneholder vanligvis kompleksdanner, ioneutbytter, bleke-midler, blekeaktivatorer, stabilisatorer, forgrånings-inhibitorer, enzymer, optiske lysningsmidler, korrosjons-inhibitorer, duftsstoffer, farvestoffer, elektrolytter. Such detergents are usually based on anionic and non-ionic surfactants as well as possibly foam inhibitors, and usually contain complex formers, ion exchangers, bleaching agents, bleaching activators, stabilizers, graying inhibitors, enzymes, optical brighteners, corrosion inhibitors, fragrances, dyes, electrolytes .

Overraskende oppviser vaskemykningsmidlene ifølge oppfinnelsen ikke de ovennevnte ulemper ved vaskemykningsmidler tilsatt til kjente vaskemidler. Surprisingly, the fabric softeners according to the invention do not exhibit the above-mentioned disadvantages of fabric softeners added to known detergents.

Vaskemykningsmidlene ifølge oppfinnelsen kan fremstilles problemfritt og som pulver tilblandes vanlige vaskemiddelpulvere. Kompleksdannelsen med de kationiske bestanddeler av vaskemykningsmidlet ifølge oppfinnelsen med anioniske tensider opptrer ikke. I stedet danner den krystallinske struktur av vaskemykningsmidlet ifølge oppfinnelsen en sikker forsinket oppløsning av den kationiske vaskemiddelmykner-komponent slik at under vaskeoperasjoner blir ved det lett oppløselige anioniske tensid smusset løst fra trådene og opp-løst i vaskevannet, hvorved anion-tensidet forbrukes tilsvarende. Det forsinket oppløsende kationiske mykningsmiddel kan herunder uhindret tiltrekkes på fibrene. Den i vaskemyk ningsmidlet inneholdte bærerkiselsyre forblir i vaskevannet og er ikke lenger påvisbar på det ferdigvaskede tekstil. Negativ innvirkning på vaskeoperasjonen, vasketøyet eller vaskemaskinen har ikke kunnet påvises. The detergent softeners according to the invention can be produced without any problems and ordinary detergent powders are mixed as a powder. Complex formation with the cationic components of the fabric softener according to the invention with anionic surfactants does not occur. Instead, the crystalline structure of the detergent softener according to the invention forms a safe delayed dissolution of the cationic detergent softener component so that during washing operations the dirt is loosened from the threads and dissolved in the wash water by the easily soluble anionic surfactant, whereby the anionic surfactant is consumed accordingly. The delayed-dissolving cationic softener can therefore be attracted to the fibers unimpeded. The carrier silicic acid contained in the fabric softener remains in the wash water and is no longer detectable on the finished textile. A negative impact on the washing operation, the laundry or the washing machine has not been demonstrated.

De følgende eksempler viser fremstillingen av vaskemykningsmidlet ifølge oppfinnelsen. The following examples show the production of the fabric softener according to the invention.

Som vaskepulver anvendes et i handelen værende fullvaskemiddel med følgende sammensetning: As washing powder, a commercially available full detergent with the following composition is used:

Eksempel 1 Example 1

30 vektdeler kiselsyre med en overflate på 500 m 2/g (Sipernat 50 S, Degussa) anbringes i en 'Loedige" blander. Under stadig omrøring tilsettes langsomt en smelte av 70 deler dimethyldistearylammoniumklorid. Blandingen blir slik innstilt på optimal skjæring. Man rører fortsatt i ca. 30 parts by weight of silicic acid with a surface area of 500 m 2 /g (Sipernat 50 S, Degussa) is placed in a 'Loedige' mixer. With constant stirring, a melt of 70 parts dimethyldistearylammonium chloride is slowly added. The mixture is thus set to optimal cutting. Stirring is continued for approx.

30 minutter og får et frittflytende pulver.30 minutes and get a free-flowing powder.

Eksempel 2Example 2

28 vektdeler kiselsyre med en overflate på 450 m 2/g ("Sipernat" 50, Degussa) anbringes under langsom omrøring i en "Loedige" blander under langsom omrøring, og 7 2 vektdeler av en oppløsning av 75% l-methyl-2-talgalkyl-3-talgamido-ethylimidazoniniummethosulfat i 25% isopropanol blir under løpende blander påsprøytet ved hjelp av en egnet dyse med et trykk på 3 bar. Blanderen innstilles på optimal skjæring. 28 parts by weight of silicic acid with a surface area of 450 m 2 /g ("Sipernat" 50, Degussa) are placed under slow stirring in a "Loedige" mixer under slow stirring, and 7 2 parts by weight of a solution of 75% l-methyl-2- tallow alkyl-3-tallow gamido-ethylimidazoninium methosulphate in 25% isopropanol is sprayed on while stirring using a suitable nozzle at a pressure of 3 bar. The mixer is set to optimal cutting.

Man blander i ytterligere 20 minutter inntil et jevnt, flytende pulver fritt for klumper erholdes. Mix for a further 20 minutes until a smooth, liquid powder free of lumps is obtained.

Eksempel 3Example 3

I en plogskjæremaskin (Loedige) anbringes 24 vektdeler bærerkiselsyre, og under stadig blanding med en hastighet på 120 o/min innsprøytes så 68 vektdeler l-methyl-2-oleyl-alkyl-3-amidoethyl-imidazoliniummethosulfat ufortynnet. In a ploughshare machine (Loedige) 24 parts by weight of carrier silicic acid are placed, and under constant mixing at a speed of 120 rpm, 68 parts by weight of undiluted 1-methyl-2-oleyl-alkyl-3-amidoethyl-imidazolium methosulphate are injected.

Derpå påsprøytes på samme måte 8 vektdeler nonylfenolpolyglycolether. Blanderen innstilles så på optimal skjæring og kjøres under skjæring i 30 minutter inntil pulverets korn-størrelse har stabilisert seg. Pulveret er da ferdig til av-fylling. Then 8 parts by weight of nonylphenol polyglycol ether are sprayed on in the same way. The mixer is then set to optimum cutting and run during cutting for 30 minutes until the powder's grain size has stabilised. The powder is then ready for filling.

Eksempel 4Example 4

For fremstilling av et mykningsgjørende vaskepulver anbringes i en plogskjærblander (Loedige) først 4,5 vektdeler bærerkiselsyre, og derpå blir under stadig blanding 10,5 vektdeler at en smeltet blanding av 75% N,N-bis-talgamidoethyl-N-(2-hydroxyethyl)-N-methylammoniummethosulfat og 25% 1,2-propylenglycol påsprøytet på kiselsyren. Blandingsoperasjonen fortsettes deretter i 30 minutter under optimal skjæring inntil kornstørrelsen er avpasset til det vaskepulver som ska,l anvendes. For the production of a softening washing powder, first 4.5 parts by weight of carrier silicic acid are placed in a plowshare mixer (Loedige), and then, with constant mixing, 10.5 parts by weight become a molten mixture of 75% N,N-bis-talgamidoethyl-N-(2- hydroxyethyl)-N-methylammonium methosulfate and 25% 1,2-propylene glycol sprayed onto the silicic acid. The mixing operation is then continued for 30 minutes under optimal cutting until the grain size is adapted to the washing powder to be used.

Deretter blir uten skjæring under stadig blanding ved ca, 100 o/min 85 vektdeler av et i handelen vanlig, ved sprøytetørring fremstilt vaskepulver tilsatt, og blandingen ble fortsatt (ca. 20 min) inntil det ble dannet et homogent pulver, Then, without cutting, while constantly mixing at approx. 100 rpm, 85 parts by weight of a commercially available, spray-dried washing powder is added, and the mix was continued (approx. 20 min) until a homogeneous powder was formed,

Eksempel 5Example 5

De i tabellen angitte mykningsmiddelformuleringer ble fremstilt på samme måte som beskrevet i eksempel 3. The plasticizer formulations indicated in the table were prepared in the same way as described in example 3.

Virkningsraåten av vaskemidlet inneholdende vaskemykningsmidlet ifølge oppfinnelsen, blir påvist ved følgende vaskeforsøk. Som vaskemiddel ble anvendt et i handelen vanlig produkt med den ovenfor angitte sammensetning. Som mykningsmiddel ble de følgende i handelen vanlige kvartære ammoniumforbindelser anvendt: The effectiveness of the detergent containing the fabric softener according to the invention is demonstrated by the following washing test. A commercially available product with the above-mentioned composition was used as detergent. The following commercially common quaternary ammonium compounds were used as softeners:

1. dimethyldistearylammoniumklorid1. dimethyldistearylammonium chloride

2. l-methyl-2-talgalkyl-3-talgamidoethylimidazolinium-methosulfat 2. 1-methyl-2-tallow alkyl-3-tallow gamidoethylimidazolinium methosulfate

Begge mykningsmidler inneholder ca. 25% isopropanol. Hver gang ble 70 vektdeler av mykneren adsorbert på 30 vektdeler felt bærerkiselsyre med en spesiell overflate på Both softeners contain approx. 25% isopropanol. Each time, 70 parts by weight of the plasticizer were adsorbed on 30 parts by weight of field silica support with a special surface of

450 m 2/g (etter BET) i en plogskjærblander.450 m 2 /g (after BET) in a ploughshare mixer.

Vaskingen ble gjort med standardvalkefrottévev i enThe washing was done with standard valke terry cloth in one

i handelen vanlig husholdnings-fullvaskemaskin. Vasketempera-turen utgjorde fortrinnsvis 60°C. Bedømmelsen av den myk-gjørende virkning skjedde ved parvis statistiske sammenlign-inger med 25 forsøkspersoner. I denne test betyr 50 punkter = meget myk og 0 punkter = ubehandlet råvev. Resultatene kan taes ut av følgende tabell: in the trade ordinary household full washing machine. The washing temperature was preferably 60°C. The assessment of the softening effect took place by pairwise statistical comparisons with 25 subjects. In this test, 50 points = very soft and 0 points = untreated raw tissue. The results can be taken from the following table:

På samme måte ble vaskemiddel som inneholder myknings-middelformuleringene i tabellen, prøvet med hensyn på deres mykningsgjørende virkning (tilsatt ble igjen et i handelen vanlig fullvaskemiddel med den ovenfor angitte sammensetning). Resultatene er angitt i tabell 3: In the same way, detergents containing the softening agent formulations in the table were tested with regard to their softening effect (a commercially available full detergent with the above-mentioned composition was again added). The results are shown in table 3:

Claims (7)

Pulverformig vaskemykningsmiddel, karakterisert ved at det består av A) 60 til 80 vekt% av et vaskemykningsmiddel på basis av ett eller flere nitrogenholdige kationiske overflateaktive stoffer som eventuelt inneholder vanlige hjelpestoffer med stabiliserende eller igjenfuktende virkning og/eller tilsetningsstoffer, B) 20 til 40 vekt% høysugedyktig kiselsyre, idet bestanddel A) er adsorbert på bestanddel B). Powdered fabric softener, characterized in that it consists of A) 60 to 80% by weight of a fabric softener based on one or more nitrogen-containing cationic surface-active substances which possibly contain common auxiliary substances with a stabilizing or re-wetting effect and/or additives, B) 20 to 40% by weight highly absorbent silicic acid, since component A) is adsorbed on component B). 2. Pulverformig vaskemykningsmiddel ifølge krav 1, karakterisert ved at de overflateaktive stoffer i bestanddel A) består av minst én av de følgende forbindelser:a) kvartære ammoniumforbindelser med formel: 2. Powdery fabric softener according to claim 1, characterized in that the surfactants in component A) consist of at least one of the following compounds: a) quaternary ammonium compounds with formula: • 1 2 hvor R og R er alkylgrupper med 8-24 carbonatomer, og R 3 og R 4er alkylgrupper med 1-4 carbonatomer, og A- er et anion,b) alkylimidazoliniumforbindelser med den generelle formel: • 1 2 where R and R are alkyl groups with 8-24 carbon atoms, and R 3 and R 4 are alkyl groups with 1-4 carbon atoms, and A- is a anion,b) alkylimidazolinium compounds with the general formula: hvor R er en alkylgruppe med 1 til 4 carbonatomer, R 6 er en-alkylgruppe med 8-25 carbonatomer, R 7 er en alkylgruppe med 1-4 carbonatomer eller hydrogen, og R ger en alkylgruppe med 8-25 carbonatomer, og A- er et anion,c) kvartære ammoniumforbindelser med den generelle formel: where R is an alkyl group of 1 to 4 carbon atoms, R 6 is an alkyl group of 8-25 carbon atoms, R 7 is an alkyl group of 1-4 carbon atoms or hydrogen, and R gives an alkyl group of 8-25 carbon atoms, and A- is an anion, c) quaternary ammonium compounds with the general formula: hvor R 9 og R 10 er alkylgrupper med 8 og 24 carbonatomholdige fettsyreamidoalkylgrupper, R"^ er en alkylgruppe med 12 1-4 carbonatomer, R er hydrogen eller methyl, x er tall fra 1 til 5, og A- er et anion. where R 9 and R 10 are alkyl groups with 8 and 24 carbon atom-containing fatty acid amidoalkyl groups, R"^ is an alkyl group with 12 1-4 carbon atoms, R is hydrogen or methyl, x is a number from 1 to 5, and A- is an anion. 3. Pulverformig vaskemykningsmiddel ifølge krav 1 eller 2, karakterisert ved at det overflateaktive stoff er l-methyl-2-alkyl-3-fettsyreamidoethylimidazolinium-methosulfat. 3. Powdery fabric softener according to claim 1 or 2, characterized in that the surfactant is 1-methyl-2-alkyl-3-fatty acid amidoethylimidazolinium methosulfate. 4. Pulverformig vaskemykningsmiddel ifølge ett eller flere av kravene 1 til 4, karakterisert ved at komponenten 1 A) som hjelpestoffer inneholder ikke-ionogene emulgatorer. 4. Powdery fabric softener according to one or more of claims 1 to 4, characterized in that component 1 A) contains non-ionic emulsifiers as excipients. 5. Pulverformig vaskemykningsmiddel ifølge ett eller flere av kravene 1 til 4, karakterisert ved at den høysugedyktige kiselsyre har en overflate fra ca. 250 til 600 m <2> /g. 5. Powdery detergent softener according to one or more of claims 1 to 4, characterized in that the highly absorbent silicic acid has a surface from approx. 250 to 600 m <2> /g. 6. Fremgangsmåte ved fremstilling av pulverformige vaskemykningsmidler, karakterisert ved at man påfører 60 - 80 vektdeler av et vaskemykningspreparat på basis av ett eller flere nitrogenholdige kationiske overflate aktive stoffer med minst én til nitrogenatomet bundet hydrocarbongruppe med minst 8 carbonatomer som eventuelt inneholder vanlige hjelpestoffer med stabiliserende eller tilbake-fuktende virkning og/eller tilsetningsstoffer, i en pulverblander, eventuelt sammen med hjelpe- og/eller duftstoffer på 20 - 40 vektdeler høysugedyktig kiselsyre. 6. Process for the production of powdery fabric softeners, characterized by applying 60 - 80 parts by weight of a fabric softener preparation based on one or more nitrogen-containing cationic surfactants with at least one hydrocarbon group bound to the nitrogen atom with at least 8 carbon atoms, which possibly contain common adjuvants with stabilizing or re-moistening effect and/or additives, in a powder mixer, possibly together with auxiliaries and/or fragrances of 20 - 40 parts by weight highly absorbent silicic acid. 7. Vaskemiddel med mykgjøringsegenskaper, karakterisert ved at det som vaskemykningsmiddel inneholder 5 til 25 vekt% av et pulverformig vaskemykningsmiddel bestående av A) 60 til 80 vekt% av et vaskemykningsmiddel på basis av ett eller flere nitrogenholdige kationiske overflateaktive stoffer med minst én til nitrogenatomet bundet hydrocarbongruppe med minst 8 carbonatomer som eventuelt inneholder vanlige hjelpestoffer med stabiliserende eller gjenfuktende virkning og/eller tilsetningsstoffer, og B) 20 til 40 vekt% høysugedyktig kiselsyre, idet komponenten A) er adsorbert på komponenten B).7. Detergent with softening properties, characterized in that it contains 5 to 25% by weight of a powdered fabric softener consisting of A) 60 to 80% by weight of a fabric softener based on one or more nitrogen-containing cationic surface-active substances with at least one hydrocarbon group bound to the nitrogen atom with at least 8 carbon atoms, possibly containing common auxiliary substances with a stabilizing or re-moistening effect and/or additives, and B) 20 to 40% by weight highly absorbent silicic acid, the component A) being adsorbed on the component B).
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