DK165336B - CONCENTRATED SUBSTANCES AND THEIR PROCEDURES FOR THEIR PREPARATION - Google Patents
CONCENTRATED SUBSTANCES AND THEIR PROCEDURES FOR THEIR PREPARATION Download PDFInfo
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- DK165336B DK165336B DK281583A DK281583A DK165336B DK 165336 B DK165336 B DK 165336B DK 281583 A DK281583 A DK 281583A DK 281583 A DK281583 A DK 281583A DK 165336 B DK165336 B DK 165336B
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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
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/001—Softening compositions
- C11D3/0015—Softening compositions liquid
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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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/38—Cationic compounds
- C11D1/62—Quaternary ammonium compounds
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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
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/835—Mixtures of non-ionic with cationic compounds
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
iin
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Den foreliggende opfindelse angår koncentrerede stofblødgø-rende midler, der er egnede til brug i skyl lekredsløbet i en vaskeproces, og som er stabile ved både lave og høje omgivelsers temperatur, dvs. at disse midler ikke danner en gel, og 5 som let dispergeres i vand, når de bruges.The present invention relates to concentrated fabric softening agents suitable for use in the flushing cycle of a washing process and which are stable at both low and high ambient temperatures, i.e. that these agents do not form a gel and 5 which are readily dispersed in water when used.
Midler indeholdende kvaternære ammoniumsalte, der har mindst én langkædet hydrocarbylgruppe er almindeligt anvendt til at give stofblødgørende virkninger ved skylning af vasketøj, 10 se f.eks. US-patentskrift nr. 3.349.033, 3.644.203, 3.946.115, 3.997.453, 4.073.735 og 4.119.545.Agents containing quaternary ammonium salts having at least one long chain hydrocarbyl group are commonly used to provide fabric softening effects when washing laundry, see e.g. U.S. Patent Nos. 3,349,033, 3,644,203, 3,946,115, 3,997,453, 4,073,735, and 4,119,545.
Til de fleste vandige blødgørende midler indeholdende katio-niske kvaternære ammoniumforbindelser som aktive bestanddele 15 har koncentrationen af disse kationiske stoffer i almindelighed været begrænset til intervallet fra ca. 3-6 vægt% (se US-patentskrift nr. 3.904.535 og 3.920.565). En sådan lav koncentration nødvendiggøres i almindelighed af, at de kationiske stoffer danner geler i vandige systemer i koncentrationer over 20 ca. 8%, og selvom brugen af elektrolytter til at nedsætte viskositeten af sådanne midler er kendt (se især US-patentskrift nr. 4.119.545), er disse elektrolytter langt fra tilfredsstillende. Ud fra et funktionelt synspunkt virker elektrolytterne ofte ikke som krævet, især i koncentrationer af de kationiske 25 stoffer i nærheden af 12-15%. Selvom virkningen af elektrolytterne kan mildne nogle af geleringsproblemerne, er deres anvendelse endvidere langt fra tilfredsstillende til at give et højkoncentreret vandigt system af kationiske stoffer, som ikke gelerer eller ændres alvorligt i viskositet inden for det sæd-30 vanlige temperaturinterval, der forekommer ved håndtering deraf, f.eks. ca. -18eC op til ca. 60°C. I US-patentskrift nr. 3.681.241 er beskrevet en koncentreret stofblødgørende emulsion, der består i det væsentlige af 3,5 til 6,5 vægtdele af en forbindelse repræsenteret f.eks. ved distearyldimethylammo-35 niumchlorid, fra 3,5 til 6,5 vægtdele af et alkylamidoimidazo-1 iniumalkylsulfat og fra 0-3 vægtdele af et andet, men lignende fedtaminoimidazoliniumalkylsulfat, hvor sidstnævnteFor most aqueous softening agents containing cationic quaternary ammonium compounds as active ingredients, the concentration of these cationic substances has generally been limited to the range of from 3-6% by weight (see U.S. Patent Nos. 3,904,535 and 3,920,565). Such a low concentration is generally required by the fact that the cationic substances form gels in aqueous systems at concentrations above about 20%. 8%, and although the use of electrolytes to reduce the viscosity of such agents is known (see, in particular, U.S. Patent No. 4,119,545), these electrolytes are far from satisfactory. From a functional point of view, the electrolytes often do not work as required, especially at concentrations of the cationic 25 in the vicinity of 12-15%. Furthermore, although the effect of the electrolytes may mitigate some of the gelling problems, their use is far from satisfactory to provide a highly concentrated aqueous system of cationic substances which do not gell or seriously alter viscosity within the usual temperature range encountered in handling them. , eg. ca. -18 ° C up to approx. 60 ° C. U.S. Patent No. 3,681,241 discloses a concentrated fabric softening emulsion consisting essentially of 3.5 to 6.5 parts by weight of a compound represented e.g. by distearyl dimethylammonium chloride, from 3.5 to 6.5 parts by weight of an alkylamidoimidazo-1 aluminum alkyl sulfate and from 0-3 parts by weight of another but similar fatty aminoimidazolinium alkyl sulfate, the latter being
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2 hævdes at give stabilitet af midlet ved lav temperatur. Den samlede mængde aktive stoffer ligger fra ca. 8-13%.2 is claimed to provide stability of the agent at low temperature. The total amount of active substances ranges from approx. 8-13%.
I GB-patentansøgning nr. 2.053.249A, offentliggjort den 4. fe-5 bruar 1981, er beskrevet kationiske stofblødgørende midler indeholdende 15-60 vægt% kationisk blødgørende stof, 25-75 vægt% af et vandigt medium og 0,5-40 vægt% af en nærmere angivet vandopløselig polymer.GB Patent Application No. 2,053,249A, published February 4, 1981, discloses cationic fabric softeners containing 15-60% by weight cationic softener, 25-75% by weight of an aqueous medium and 0.5-40 % by weight of a specified water-soluble polymer.
10 I US-patentskrift nr. 3.974.076 er beskrevet et kvaternært ammoniumholdigt blødgørende middel med sædvanlige kationiske koncentrationer, dvs. ca. 3% til ca. 6%. Disse midler er ejendommelige ved den meget lille partikelstørrelse af den i hovedsagen vanduopløselige kvaternære blødgørende ammoniumfor-15 bindelse, dvs. 90 vægt% af de kvaternære ammoniumforbindelser eksisterer som partikler, der vil gå gennem et 1,2 mikron filter. Midlerne beskrives som en kombination af det kationiske, blødgørende middel, en C8-C20 alkylal kohol, med fra ca. 0,1% til ca. 2,0% af et ikke-ionisk overfladeaktivt middel, 20 som har en HLB fra ca. 8 til ca. 15 og fortrinsvis fra ca. 10 til ca. 14. De foretrukne ikke-ioniske stoffer har en lipofil hydrocarbylmolekyldel ækvivalent med 9-15 carbonatomer med 7-13 hydrofile ethylenoxidmolekyldele. Dette patent angår ikke problemet med stabilitet af koncentrerede vandige, kationiske 25 blødgørende midler, men forbedring af niveauet og ensartethed af blødgøring under anvendelse af sædvanlige koncentrationer.U.S. Patent No. 3,974,076 discloses a quaternary ammonium-containing plasticizer having the usual cationic concentrations, i.e. ca. 3% to approx. 6%. These agents are characterized by the very small particle size of the substantially water-insoluble quaternary softening ammonium compound, i.e. 90% by weight of the quaternary ammonium compounds exist as particles that will pass through a 1.2 micron filter. The agents are described as a combination of the cationic plasticizer, a C8-C20 alkylalcohol, with from about 0.1% to approx. 2.0% of a nonionic surfactant having an HLB of approx. 8 to approx. 15 and preferably from ca. 10 to approx. 14. The preferred nonionic substances have a lipophilic hydrocarbyl moiety equivalent to 9-15 carbon atoms with 7-13 hydrophilic ethylene oxide moieties. This patent does not address the problem of stability of concentrated aqueous cationic plasticizers, but improvement of the level and uniformity of softening using usual concentrations.
BE-patentskrift nr. 888.535 omhandler tekstilblødgøringsmidler omfattende 10 til 30 vægt% af an kationisk, blødgørende for-30 bindelse, som bl.a. kan være en kvaternær ammoniumforbindelse, 0,2-3 vægt% af et ikke-ionisk tensidaktivt middel, som bl.a. kan være C3-10 alkylphenol kondenseret med 6 til 12 mol ethy-len- eller propylenoxid samt 3-7 vægt% af en viskositetsmodificerende bestanddel opnået ved konjugation af et opløsnings-35 middel med en elektrolyt (jf. krav 1 i skriftet).BE Patent Specification No. 888,535 discloses textile softeners comprising 10 to 30% by weight of an cationic softening compound, such as e.g. may be a quaternary ammonium compound, 0.2-3% by weight of a non-ionic surfactant active agent, e.g. may be C3-10 alkylphenol condensed with 6 to 12 moles of ethylene or propylene oxide as well as 3-7% by weight of a viscosity-modifying component obtained by conjugation of a solvent with an electrolyte (see claim 1 in the specification).
Det anvendte opløsningsmiddel, er en alkohol, fortrinsvis ethylen-, propylen- eller hexylenglycol (jf. krav 11 og 12 iThe solvent used is an alcohol, preferably ethylene, propylene or hexylene glycol (cf. claims 11 and 12 of
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3 skr i ftet).3 feet in feet).
På side 10, linie 20-24 i skriftet anføres det, at det af eksemplerne fremgår, at det ikke er tilstrækkeligt blot at an-5 vende elektrolytter, men at det er nødvendigt også at anvende opløsningsmidler.On page 10, lines 20-24 of the script, it is stated that the examples show that it is not enough merely to use electrolytes, but that it is also necessary to use solvents.
I de i skriftet angivne eksempler anvendes elektrolytterne i mængder på fra 0,05 til 0,25 vægt%.In the examples set forth in the specification, the electrolytes are used in amounts of 0.05 to 0.25% by weight.
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Den foreliggende opfindelse angår ved lav og høj temperatur stabile, koncentrerede, vandige blødgørende midler baseret på blødgørende kvaternære ammoniumforbindelser og en mindre mængde af både et ikke-ionisk overfladeaktivt stof og en elektro-15 lyt. Opfindelsen angår også en fremgangsmåde til fremstilling af højt koncentrerede stofblødgørende midler.The present invention relates to low and high temperature stable, concentrated aqueous softening agents based on softening quaternary ammonium compounds and a minor amount of both a nonionic surfactant and an electrolyte. The invention also relates to a process for preparing highly concentrated fabric softeners.
Midlerne ifølge opfindelsen er stabile vandige midler, der indeholder en høj koncentration af det kationiske stofblødgø-20 rende middel, som er en vanddispergerbar, kvaternær ammoniumforbindelse som beskrevet i det følgende, ikke-ionisk overfladeaktivt middel og elektrolyt.The agents of the invention are stable aqueous agents containing a high concentration of the cationic fabric softening agent which is a water dispersible, quaternary ammonium compound as described below, nonionic surfactant and electrolyte.
Den foreliggende opfindelse angår således et stabilt, vandigt, 25 koncentreret stofblødgørende middel omfattende et kationisk blødgørende stof i form af en vanddispergerbar, kvaternær ammoniumforbindelse, et ikke-ionisk, overfladeaktivt stof samt en elektrolyt, hvilket middel er ejendommeligt ved, at det omfatter (A) 12 til 20 vægt% af et kationisk blødgørende stof 30 med formlen 35Thus, the present invention relates to a stable aqueous concentrated fabric softener comprising a cationic softening agent in the form of a water dispersible, quaternary ammonium compound, a nonionic surfactant and an electrolyte which is characterized in that it comprises (A 12 to 20% by weight of a cationic plasticizer 30 of formula 35
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4 I " 5 i Rl\ /r3 + x“ _ R2 R4 j 10 hvori R^, R2, R3 og R4 er alifatiske carbonhydridgrupper med cl“c30' hvoraf to er alkyl med C14-C30, og X er en vandopløse-liggørende anion, (B) 1-5 vægt% ikke-ionisk, overfladeaktivt stof valgt blandt ethylenoxidkondensater af Cj2-C20 alifatiske 15 alkoholer og alkylphenoler med HLB-værdi på 16,5 ± 1,0 og (C) ca. 0,5 til ca. 1,5 vægt% elektrolyt.4 I "5 in R 1 / R 3 + x" - R 2 R 4 j 10 wherein R 1, R 2, R 3 and R 4 are aliphatic hydrocarbon groups having C 1 -C 30, two of which are alkyl with C 14 -C 30, and X is a water-soluble anion, (B) 1-5 wt.% nonionic surfactant selected from ethylene oxide condensates of C 2 -C 20 aliphatic alcohols and alkyl phenols with HLB value of 16.5 ± 1.0 and (C) about 0.5 to about 1.5 wt% electrolyte.
X er en vandopløseliggørende anion, såsom chlorid, bromid, io-did, fluorid, sulfat, metosulfat, nitrit, nitrat, phosphat og 20 carboxylat (dvs. acetat, adipat, propionat, phthalat, benzoat, oleat osv.).X is a water-solubilizing anion such as chloride, bromide, iodide, fluoride, sulfate, methosulfate, nitrite, nitrate, phosphate and carboxylate (i.e., acetate, adipate, propionate, phthalate, benzoate, oleate, etc.).
Typiske kationiske stoffer af formlen I indbefatter følgende: 25 disteary1 di methyl ammon i umchlori d ditalgdimethylammoniumchlorid di hexadecyldimethyl ammon i umchlorid distearyIdimethyl ammon i umbromid di(hydrogeneret talg) dimethylammoniumbromid 30 distearyl, di (isopropyl) ammoniumchlorid distearyIdimethylammoniummethosulfat.Typical cationic compounds of formula I include the following: 25 distearyl di methyl ammon in umchloride d ditalgdimethylammonium chloride di hexadecyldimethyl ammon in um chloride distearyl dimethyl ammon in umbromide di (hydrogenated tallow) dimethylammonium bromide distearyl, di (isopropylmethyl) ammonium ammonium ammonium ammonium ammonium ammonium ammonium
Den ikke-ioniske komponent af de foreliggende midler omfatter fra ca. 1 til ca. 5 vægt% af midlet og kan i almindelighed va-35 riere med det kationiske blødgørende middel i et vægtforhold mellem kationisk stof og ikke-ionisk stof fra ca. 20:1 til ca. 3:1 og fortrinsvis fra ca. 10:1 til ca. 5:1. De ikke-ioniskeThe nonionic component of the present compositions comprises from ca. 1 to approx. 5% by weight of the agent and can generally vary with the cationic plasticizer in a weight ratio of cationic substance to nonionic substance from about 5%. 20: 1 to approx. 3: 1 and preferably from ca. 10: 1 to approx. 5: 1. The non-ionic ones
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5 forbindelser er ethylenoxidkondensater af Ci2-C20 alifatiske alkoholer og alkylphenoler karakteristiske ved en HLB (hydro-fi 1 -1 ipofil balance) på 16,5 ± 1,0. En fuldstændig diskussion af HLB-systemet kan findes i "The HLB System" (1976 udgave 16 5 sider) udgivet af ICI United States, Inc.. I almindelighed er . de ikke-ioniske stoffer, der anvendes i midlet ifølge opfin delsen, hydrofile af karakter med en stor og stærk hydrofil gruppe. I den foreliggende opfindelse er denne gruppe en oxy-ethylkæde med i almindelighed mindst ca. 15 terminale oxy-10 ethylgrupper (dvs. oxyethylgrupperne hænger sammen og ender i en hydroxylgruppe).Five compounds are ethylene oxide condensates of C12-C20 aliphatic alcohols and alkylphenols, characterized by a HLB (hydrophilic 1 -1 ipophilic balance) of 16.5 ± 1.0. A full discussion of the HLB system can be found in "The HLB System" (1976 edition 16 5 pages) published by ICI United States, Inc .. Generally, the. the nonionic substances used in the composition of the invention are hydrophilic in character with a large and strong hydrophilic group. In the present invention, this group is an oxyethyl chain having generally at least approx. 15 terminal oxy-10 ethyl groups (i.e., the oxyethyl groups are interconnected and end up in a hydroxyl group).
Særligt egnede ikke-ioniske overfladeaktive stoffer indbefatter en Cj3_j5 alifatisk alkohol indeholdende 20 mol kondense-15 ret ethylenoxid, som fås som Synperonic® A20, en ethoxyleret octylphenol med 16 mol ethylenoxid, der fås som Triton® X-165, og en ethoxyleret nonylphenol med 30 mol ethylenoxid, der fås som Dowfax® NP30.Particularly suitable nonionic surfactants include a C Cj_j aliphatic alcohol containing 20 moles of condensed ethylene oxide available as Synperonic® A20 30 moles of ethylene oxide available as Dowfax® NP30.
20 Den tredje bestanddel er en elektrolyt (ionisk materiale) i en mængde fra ca. 0,1 til ca. 1,5 vægt%. Brugen af en elektrolyt virker ikke blot til at regulere viskositeten, men understøtter også stabiliseringen af systemet mod gelering og faseomvending ved højere temperaturer, f.eks. over ca. 40eC. Særligt 25 egnede elektrolytter indbefatter natriumchlorid og calcium-chlorid. Andre nyttige elektrolytter indbefatter natriumfor-miat, natriumnitrit, natriumnitrat, natriumacetat samt vandopløselige salte af andre kationer, såsom kalium, lithium, magnium, ammonium og lignende.The third component is an electrolyte (ionic material) in an amount of from approx. 0.1 to approx. 1.5% by weight. The use of an electrolyte not only acts to regulate the viscosity, but also supports the stabilization of the system against gelation and phase reversal at higher temperatures, e.g. over approx. 40eC. Particularly suitable electrolytes include sodium chloride and calcium chloride. Other useful electrolytes include sodium formate, sodium nitrite, sodium nitrate, sodium acetate, and water-soluble salts of other cations such as potassium, lithium, magnium, ammonium and the like.
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Mindre mængder lavere alkanoler kan anvendes, især hvor man ønsker yderligere at modificere viskositeten. I almindelighed er alkoholer tilbøjelige til at nedsætte viskositeten ved omgivelsernes temperatur, men moderate mængder kan bevirke en 35 nedsættelse af faseomvendingstemperaturen. De foretrukne midler ifølge opfindelsen udviser faseomvendingstemperaturer over ca. 80eC og fortrinsvis over ca. 90eC med alkoholmængder i in-Smaller amounts of lower alkanols can be used, especially where further modification of the viscosity is desired. In general, alcohols tend to decrease the viscosity at ambient temperature, but moderate amounts can cause a reduction in the phase reversal temperature. The preferred agents of the invention exhibit phase reversal temperatures above ca. 80 ° C and preferably above approx. 90 ° C with alcohol amounts in
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6 tervallet fra ca. 1 til ca. 10 vægt%. Særligt egnede alkoholer er ethyl- og isopropylalkohol.6 ranges from approx. 1 to approx. 10% by weight. Particularly suitable alcohols are ethyl and isopropyl alcohol.
Foruden de i det foregående nævnte komponenter af de blødgø-5 rende midler ifølge opfindelsen kan der også inkluderes flere, sædvanlige supplerende og eventuelle bestanddele, som ikke skadeligt påvirker stabiliteten og/eller funktionelle egenskaber af de foreliggende midler. Der kan f.eks. findes parfumer, farvestoffer, pigmenter, uklarhedsskabende midler, ger-10 micider, optiske klaringsmidler, antikorrosionsmidler (f.eks. natriumsilikat), vandopløselige polymere, antistatiske midler og lignende. Hvor disse anvendes, kan hver især omfatte fra 0,01% til ca. 5 vægt% af midlet.In addition to the aforementioned components of the softening agents of the invention, there may also be included several, usual supplementary and optional ingredients which do not adversely affect the stability and / or functional properties of the present agents. For example, There are perfumes, dyes, pigments, cloud-forming agents, gericides, optical brighteners, anti-corrosion agents (eg sodium silicate), water-soluble polymers, antistatic agents and the like. Where used, each may comprise from 0.01% to ca. 5% by weight of the agent.
15 Som eksempel på vandopløselige polymere kan der nævnes poly-ethylenglycol (molekylvægt 400). Blandt andre nyttige polymere kan henvises til offentliggjort GB-patentansøgning nr. 2.053.249A, der er nævnt ovenfor. Midlerne ifølge opfindelsen kan indeholde enhver og alle disse polymere og andre vandoplø-20 selige polymere. I midlerne ifølge opfindelsen kan man anvende fra 0,1 til 20 vægt% beregnet på det samlede middel af disse materialer.As an example of water-soluble polymers there may be mentioned polyethylene glycol (molecular weight 400). Among other useful polymers, reference is made to published GB Patent Application No. 2,053,249A mentioned above. The agents of the invention may contain any and all of these polymers and other water-soluble polymers. In the compositions of the invention, from 0.1 to 20% by weight based on the total composition of these materials can be used.
Den langkædede alkylsubstituent (R) i de kationiske stoffer 25 anvendt ifølge opfindelsen kan ikke blot være af en enkelt kædelængde, men består mere sandsynligt af en blanding af alkyler med forskellige kædelængder. I denne henseende kan et særligt nyttigt kvaternært blødgørende stof, hvori alkylgrup-perne er afledt af talg, indeholde ca. 35% °9 6°¾ c18 °9 30 mindre mængder C^4 og andre. På lignende måde kan det alifatiske alkoholforstadium, som kan indgå i de ikke-ioniske stoffer, der anvendes i midlet ifølge opfindelsen, være af en enkelt kædelængde, men mere sandsynligt vil det være og kan det være en blanding med vilkårlige mængdeforhold mellem de 35 virksomme kædelængder.The long chain alkyl substituent (R) of the cationic substances 25 used in the invention may not only be of a single chain length, but more likely consists of a mixture of alkyls of different chain lengths. In this regard, a particularly useful quaternary plasticizer, wherein the alkyl groups are derived from sebum, may contain approx. 35% ° 9 6 ° ¾ c18 ° 9 30 smaller amounts of C ^ 4 and others. Similarly, the aliphatic alcohol precursor which may be included in the non-ionic substances used in the composition of the invention may be of a single chain length, but more likely it will be and may be a mixture of any proportional proportions of the active substances. chain lengths.
De stofblødgørende midler ifølge opfindelsen må foruden viskositet og fasestabilitet have en passende viskositet (dvs. tilIn addition to viscosity and phase stability, the fabric softening agents of the invention must have an appropriate viscosity (i.e.
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7 hældelighed) og vanddispergerbarhed i skyl lekredsløbet (eller enhver anden form for fortynding før brugen), som forbrugeren er blevet vant til og kræver på baggrund af deres brug af de mindre koncentrerede produkter. Produkterne ifølge opfindelsen 5 kan således have viskositeter, der ligger fra ca. 30 cps. til ca. 250 cps. og fortrinsvis fra ca. 40 cps. til ca. 120 cps.7 pourability) and water dispersibility in the rinse play circuit (or any other dilution prior to use) to which the consumer has become accustomed and require based on their use of the less concentrated products. Thus, the products of the invention 5 may have viscosities ranging from ca. 30 cps. to approx. 250 cps. and preferably from ca. 40 cps. to approx. 120 cps.
Opfindelsen angår endvidere en fremgangsmåde til fremstilling af midlerne ifølge opfindelsen, hvilken fremgangsmåde er ejen-10 dommelig ved, at der først fremstilles en vandig opløsning af det ikke-ioniske, overfladeaktive stof i varmt vand ved en temperatur op til ca. 80°C, fortrinsvis på ca. 70°C, hvorefter, kationisk blødgørende stof tilsættes i smeltet form til dannelse af en gel, hvorpå gelen afkøles til under 40°C, for-15 trinsvis til lige under 40°C, og elektrolytten derefter tilsættes for at bryde gelen, hvorpå blandingen afkøles til stuetemperatur under omrøring.The invention further relates to a process for the preparation of the compositions according to the invention, characterized in that an aqueous solution of the non-ionic surfactant in hot water is first prepared at a temperature up to approx. 80 ° C, preferably at approx. 70 ° C, after which cationic softening agent is added in molten form to form a gel whereby the gel is cooled to below 40 ° C, preferably to just below 40 ° C, and then the electrolyte is added to break the gel whereupon the mixture cool to room temperature with stirring.
Ved denne fremgangsmåde (A) tilsættes således ikke-ioniske ma-20 terialer og farvende stof til præparatets vægtmængde vand, som har en temperatur på fortrinsvis ca. 70°C. Til denne opløsning sættes langsomt det kationiske blødgørende stof i smeltet form. I reglen vil der dannes en gel. Blandingen afkøles til ca. 40°C, hvorpå elektrolytten tilsættes for at bryde gelen.Thus, in this process (A), nonionic materials and coloring matter are added to the weight of water of the composition having a temperature of preferably about 70 ° C. To this solution is slowly added the cationic plasticizer in molten form. As a rule, a gel will form. The mixture is cooled to ca. 40 ° C, then the electrolyte is added to break the gel.
25 Midlet afkøles så til stuetemperatur under omrøring.The agent is then cooled to room temperature with stirring.
En modifikation af fremgangsmåde (A) indebærer, at der først fremstilles en vandig opløsning af det ikke-ioniske, overfladeaktive stof i varmt vand ved en temperatur op til ca. 80eC, 30 hvorpå pH-værdien indstilles med alkalisk materiale til over ca. 10, fortrinsvis til ca. 12, før tilsætning af det kationiske, blødgørende stof i smeltet for-m. I dette tilfælde dannes ingen gel. Efter afkøling til ca. 40°C genindstilles pH-værdien til under 7, fortrinsvis til 5-6, og der afkøles under 35 omrøring til stuetemperatur, hvorpå elektrolytten tilsættes til indstilling af viskositeten (fremgangsmåde B).A modification of process (A) involves first preparing an aqueous solution of the nonionic surfactant in hot water at a temperature up to about 30 ° C. 80 ° C, whereupon the pH is adjusted with alkaline material to above approx. 10, preferably to ca. 12 before adding the cationic softening agent in molten form. In this case, no gel is formed. After cooling to approx. At 40 ° C, the pH is reset to below 7, preferably 5-6, and cooled to room temperature with stirring, then the electrolyte is added to adjust the viscosity (Method B).
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Endnu en fremgangsmåde (C) indebærer tilsætning af de ikke-ioniske stoffer til mindst 80% varmt vand ved en temperatur op til ca. 40°C, hvorefter elektrolytten tilsættes efterfulgt af det kationiske, blødgørende stof i smeltet form. Den eventu-5 elle rest af vand tilsættes så, og midlet afkøles under omrøring til stuetemperatur.Yet another method (C) involves adding the nonionic substances to at least 80% hot water at a temperature up to approx. 40 ° C, after which the electrolyte is added followed by the cationic plasticizer in molten form. The optional residue of water is then added and the agent is cooled with stirring to room temperature.
De følgende eksempler tjener til at illustrere den foreliggende opfindelse. Delene er efter vægt, med mindre ande.t er 10 anført.The following examples serve to illustrate the present invention. The parts are by weight, with smaller parts. 10 are listed.
Eksempel 1Example 1
Ved at følge den ovenfor beskrevne fremgangsmåde (A) bliver to 15 dele af en ethoxyleret nonylphenol (indeholdende 16 mol ethy-lenoxid) opløst i ca. 75 dele vand ved en temperatur på ca. 70eC. Til denne opløsning sættes langsomt 20 dele distearyldi-methylammoniumchlorid (75% aktiv og indeholdende ca. 10% iso-propanol og resten vand) i smeltet form (temperatur = 55°C) 20 under omrøring. Der dannes en gel. Gelen afkøles til ca. 40°C, og derefter tilsættes 0,5 dele calciumchloriddehydrat. Blandingen afkøles til stuetemperatur (ca. 20°C) under omrøring. Der fremkommer et stabilt produkt, som ikke skiller i flere faser, med en viskositet på ca. 100 cps.Following the procedure described above (A), two 15 parts of an ethoxylated nonylphenol (containing 16 moles of ethylene oxide) are dissolved in ca. 75 parts of water at a temperature of approx. 70eC. To this solution is slowly added 20 parts distearyl dimethyl ammonium chloride (75% active and containing about 10% isopropanol and the residual water) in molten form (temperature = 55 ° C) 20 with stirring. A gel is formed. The gel is cooled to ca. 40 ° C and then 0.5 parts of calcium chloride dehydrate is added. The mixture is cooled to room temperature (about 20 ° C) with stirring. A stable product which does not separate in several phases, with a viscosity of approx. 100 cps.
2525
Eksempel 2Example 2
Fremgangsmåden i eksempel 1 gentages under anvendelse af følgende dele af (A) kationisk stof (aktivt), (B) overfladeaktivt 30 stof og (C) elektrolyt.The procedure of Example 1 is repeated using the following portions of (A) cationic (active), (B) surfactant and (C) electrolyte.
(a) A = 12; B = 1,0; C = 0,5 (b) A = 14; B = 1,5; C = 0,5 (c) A = 16; B = 1,8; C = 0,7 35 (d) A = 18; B = 2,5; C = 1,0.(a) A = 12; B = 1.0; C = 0.5 (b) A = 14; B = 1.5; C = 0.5 (c) A = 16; B = 1.8; C = 0.7 (d) A = 18; B = 2.5; C = 1.0.
Der fremkommer også her stabile produkter uden tendens til faseseparation.Stable products also appear here without a tendency for phase separation.
DK 165336 BDK 165336 B
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Eksempel 3Example 3
Yderligere fasestabile midler kan fremstilles ved gentagelse af eksempel 1 og 2 under anvendelse i stedet for distearyldi-5 methylammoniumchlorid af følgende: (a) di talgdi methylammon i umchlorid (b) distearyldimethylammoniummethosulfat (c) di(hydrogeneret talg) dimethylammoniumbromid 10 (d) dihexadecyldimethylammoniumchlorid (e) distearyldiethylammoniumchlorid.Additional phase-stable agents can be prepared by repeating Examples 1 and 2 using in place of distearyl dimethyl ammonium chloride of the following: (a) di tallow di methylammon in um chloride (b) distearyldimethylammonium methosulfate (e) distearyl diethylammonium chloride.
Eksempel 4 15 Yderligere fasestabile midler kan fremstilles ved gentagelse af eksempel 1, 2 og 3, idet der i alle tilfælde tilsættes 1 del polyethylenglycol (molekylvægt 400) sammen med det ikke-ioniske stof i det første trin i fremstillingsmåden.Example 4 Additional phase-stable agents can be prepared by repeating Examples 1, 2 and 3, in each case adding 1 part of polyethylene glycol (molecular weight 400) with the nonionic substance in the first step of the process.
20 Polyethylenglycol (molekylvægt 400) illustrerer lavmolekylære vandopløselige polymere, der kan anvendes, hvis det ønskes, i blødgøringsmidlerne ifølge opfindelsen.Polyethylene glycol (molecular weight 400) illustrates low molecular weight water-soluble polymers which can be used, if desired, in the plasticizers of the invention.
Eksempel 5 25Example 5 25
Hver af de foregående eksempler 1-4 gentages under anvendelse som elektrolyt af følgende: (a) natriumchlorid 30 (b) natriumnitrat (c) natriumformiat (d) ammoniumbromid (e) kaliumchlorid (f) ca1ciumnitrat 35 (g) 1 i thiumacetat (h) magniumchlorid.Each of the foregoing Examples 1-4 is repeated using as electrolyte the following: (a) sodium chloride (b) sodium nitrate (c) sodium formate (d) ammonium bromide (e) potassium chloride (f) calcium nitrate 35 (g) 1 in thium acetate (h) ) magnesium chloride.
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DK 165336BDK 165336B
Eksempel 6Example 6
Hvert af eksemplerne 1-5 gentages, for såvidt angår sammen-5 sætningen, men der følges fremgangsmåde (B) til fremstillingen. Ved denne fremgangsmåde indebærer ændringen i forarbejdningen, der er beskrevet i eksempel l, indstilling af pH-værdien til 12 med natriumhydroxid efter opløsning af det ikke-ioniske stof (og polyethylenglycol, hvor dette anvendes) 10 og genindstilling af pH-værdien til 5-6 med saltsyre efter tilsætningen af det kationiske stof. På dette punkt dannes ingen gel som i fremgangsmåde (A). Elektrolytten tilsættes, efter at blandingen er kølet til stuetemperatur.Each of Examples 1-5 is repeated as far as the composition is concerned, but method (B) is followed for the preparation. In this process, the change in processing described in Example 1 involves adjusting the pH to 12 with sodium hydroxide after dissolution of the nonionic substance (and polyethylene glycol, where used) 10 and resetting the pH to 5- 6 with hydrochloric acid after the addition of the cationic substance. At this point, no gel is formed as in process (A). The electrolyte is added after the mixture is cooled to room temperature.
15 Eksempel 7Example 7
Hver af eksemplerne 1-5 gentages igen for såvidt angår sammensætningen, men ved at følge fremgangsmåde (C) til fremstillingen. Ved denne fremgangsmåde opløses det ikke-ioniske stof (og 20 den vandopløselige polyethylenglycol, hvor denne anvendes) i 80% af præparatets vægtmængde af vand ved en temperatur på 35-40°C. Elektrolytten tilsættes så efterfulgt af det smeltede kationiske stof. Præparatets resterende vægtmængde vand tilsættes så, og derefter afkøles blandingen til stuetemperatur 25 under omrøring.Each of Examples 1-5 is repeated again as far as the composition is concerned, but following Method (C) for the preparation. In this process, the nonionic substance (and the water-soluble polyethylene glycol, where used) is dissolved in 80% of the weight of the composition of water at a temperature of 35-40 ° C. The electrolyte is then added, followed by the molten cationic substance. The remaining amount of water of the preparation is then added and then the mixture is cooled to room temperature 25 with stirring.
De vandige blødgørende midler ifølge opfindelsen er generelt anvendelige som andre sådanne midler og er især nyttige i skyl lekredsløbet i automatiske tøjvaskemaskiner. Ved sådanne 30 operationer og ved andre ønskede metoder til behandling af tøj benyttes midlerne i reglen således, at de giver en koncentration af aktive stoffer fra ca. 0,005% til 0,3% beregnet på vægten af tøjet, der behandles, fortrinsvis 0,007% til ca. 0,2% og bedst fra ca. 0,01% til ca. 0,15%.The aqueous softeners of the invention are generally useful as other such agents and are particularly useful in flushing the circuit in automatic laundry machines. In such operations and in other desired methods of treatment of clothing, the agents are generally used so as to provide a concentration of active substances of approx. 0.005% to 0.3% based on the weight of the garment being treated, preferably 0.007% to approx. 0.2% and best from approx. 0.01% to approx. 0.15%.
3535
Claims (9)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US39041182A | 1982-06-22 | 1982-06-22 | |
| US39041182 | 1982-06-22 |
Publications (4)
| Publication Number | Publication Date |
|---|---|
| DK281583D0 DK281583D0 (en) | 1983-06-17 |
| DK281583A DK281583A (en) | 1983-12-23 |
| DK165336B true DK165336B (en) | 1992-11-09 |
| DK165336C DK165336C (en) | 1993-03-29 |
Family
ID=23542374
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DK281583A DK165336C (en) | 1982-06-22 | 1983-06-17 | CONCENTRATED SUBSTANCES AND THEIR PROCEDURES FOR THEIR PREPARATION |
Country Status (18)
| Country | Link |
|---|---|
| AU (1) | AU558320B2 (en) |
| BE (1) | BE893887A (en) |
| BR (1) | BR8303280A (en) |
| CA (1) | CA1208854A (en) |
| CH (1) | CH655332A5 (en) |
| DE (1) | DE3225687A1 (en) |
| DK (1) | DK165336C (en) |
| ES (2) | ES523460A0 (en) |
| FR (1) | FR2528864B1 (en) |
| GB (1) | GB2122662B (en) |
| GR (1) | GR77513B (en) |
| IT (1) | IT1172269B (en) |
| MX (1) | MX158906A (en) |
| NL (1) | NL8302227A (en) |
| NO (1) | NO163629C (en) |
| NZ (1) | NZ204517A (en) |
| SE (1) | SE462050B (en) |
| ZA (1) | ZA834209B (en) |
Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4497716A (en) * | 1982-12-23 | 1985-02-05 | Lever Brothers Company | Fabric softening composition |
| NZ207932A (en) * | 1983-05-11 | 1986-03-14 | Colgate Palmolive Co | Fabric softener compositions containing quaternary ammonium compounds |
| GB8410322D0 (en) * | 1984-04-19 | 1984-05-31 | Unilever Plc | Aqueous concentrated fabric softening composition |
| GB8410320D0 (en) * | 1984-04-19 | 1984-05-31 | Unilever Plc | Aqueous fabric softening composition |
| GB8719083D0 (en) * | 1987-08-12 | 1987-09-16 | Albright & Wilson | Fabric conditioners |
| EP0309052B1 (en) * | 1987-09-23 | 1992-11-25 | The Procter & Gamble Company | Stable biodegradable fabric softening compositions containing linear alkoxylated alcohols |
| GB8818593D0 (en) * | 1988-08-04 | 1988-09-07 | Albright & Wilson | Fabric conditioners |
| US5066414A (en) * | 1989-03-06 | 1991-11-19 | The Procter & Gamble Co. | Stable biodegradable fabric softening compositions containing linear alkoxylated alcohols |
| EP2159276A1 (en) * | 2008-08-30 | 2010-03-03 | Clariant (Brazil) S.A. | Solid or gel surfactant composition |
Family Cites Families (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3660286A (en) * | 1969-01-03 | 1972-05-02 | Lever Brothers Ltd | Liquid wash cycle softener |
| US3920565A (en) * | 1973-02-23 | 1975-11-18 | Procter & Gamble | Fabric softener composition and method |
| US3974076A (en) * | 1974-01-11 | 1976-08-10 | The Procter & Gamble Company | Fabric softener |
| LU71307A1 (en) * | 1974-11-18 | 1976-09-06 | ||
| JPS52134030A (en) * | 1976-04-30 | 1977-11-09 | Kao Corp | Softening composition for fabrics and hairs |
| US4119545A (en) * | 1977-03-28 | 1978-10-10 | Colgate Palmolive Company | Concentrated fabric softening composition |
| DE3025369A1 (en) * | 1980-07-04 | 1982-01-28 | Hoechst Ag, 6000 Frankfurt | SOFT SOFT CONDENSER CONCENTRATE |
| BE888535A (en) * | 1981-04-23 | 1981-08-17 | Lesieur Cotelle | LIQUID SOFTENING COMPOSITIONS FOR TEXTILES, |
-
1982
- 1982-06-15 ZA ZA834209A patent/ZA834209B/en unknown
- 1982-07-09 DE DE19823225687 patent/DE3225687A1/en active Granted
- 1982-07-15 FR FR8212357A patent/FR2528864B1/en not_active Expired
- 1982-07-20 BE BE0/208632A patent/BE893887A/en unknown
-
1983
- 1983-06-09 NZ NZ204517A patent/NZ204517A/en unknown
- 1983-06-15 GR GR71691A patent/GR77513B/el unknown
- 1983-06-17 IT IT48525/83A patent/IT1172269B/en active
- 1983-06-17 DK DK281583A patent/DK165336C/en not_active IP Right Cessation
- 1983-06-20 SE SE8303507A patent/SE462050B/en not_active IP Right Cessation
- 1983-06-20 AU AU15961/83A patent/AU558320B2/en not_active Ceased
- 1983-06-21 BR BR8303280A patent/BR8303280A/en unknown
- 1983-06-21 GB GB08316857A patent/GB2122662B/en not_active Expired
- 1983-06-21 MX MX197751A patent/MX158906A/en unknown
- 1983-06-21 CA CA000430819A patent/CA1208854A/en not_active Expired
- 1983-06-21 ES ES523460A patent/ES523460A0/en active Granted
- 1983-06-21 NO NO832245A patent/NO163629C/en unknown
- 1983-06-22 NL NL8302227A patent/NL8302227A/en not_active Application Discontinuation
- 1983-06-22 CH CH3420/83A patent/CH655332A5/en not_active IP Right Cessation
-
1984
- 1984-03-07 ES ES530347A patent/ES8505402A1/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| ES530347A0 (en) | 1985-05-16 |
| SE8303507D0 (en) | 1983-06-20 |
| AU1596183A (en) | 1984-01-05 |
| SE462050B (en) | 1990-04-30 |
| NO163629C (en) | 1990-06-27 |
| NL8302227A (en) | 1984-01-16 |
| GB2122662B (en) | 1986-01-22 |
| ZA834209B (en) | 1985-01-30 |
| NO832245L (en) | 1983-12-23 |
| GB2122662A (en) | 1984-01-18 |
| ES8505402A1 (en) | 1985-05-16 |
| DE3225687C2 (en) | 1991-11-21 |
| AU558320B2 (en) | 1987-01-29 |
| CA1208854A (en) | 1986-08-05 |
| MX158906A (en) | 1989-03-29 |
| IT8348525A0 (en) | 1983-06-17 |
| BE893887A (en) | 1983-01-20 |
| CH655332A5 (en) | 1986-04-15 |
| FR2528864A1 (en) | 1983-12-23 |
| NZ204517A (en) | 1986-09-10 |
| DE3225687A1 (en) | 1983-12-22 |
| SE8303507L (en) | 1983-12-23 |
| DK281583D0 (en) | 1983-06-17 |
| DK165336C (en) | 1993-03-29 |
| NO163629B (en) | 1990-03-19 |
| ES8501434A1 (en) | 1984-11-16 |
| IT1172269B (en) | 1987-06-18 |
| GR77513B (en) | 1984-09-24 |
| ES523460A0 (en) | 1984-11-16 |
| GB8316857D0 (en) | 1983-07-27 |
| BR8303280A (en) | 1984-02-07 |
| FR2528864B1 (en) | 1987-05-07 |
| DK281583A (en) | 1983-12-23 |
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