DK142241B - Process for the preparation of free-flowing nonionic urea-ethoxamer inclusion compounds. - Google Patents
Process for the preparation of free-flowing nonionic urea-ethoxamer inclusion compounds. Download PDFInfo
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- DK142241B DK142241B DK50572AA DK50572A DK142241B DK 142241 B DK142241 B DK 142241B DK 50572A A DK50572A A DK 50572AA DK 50572 A DK50572 A DK 50572A DK 142241 B DK142241 B DK 142241B
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- Prior art keywords
- slurry
- approx
- urea
- mixture
- ethoxamer
- Prior art date
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- 238000000034 method Methods 0.000 title claims description 25
- 150000001875 compounds Chemical class 0.000 title description 7
- 238000002360 preparation method Methods 0.000 title description 4
- 239000002002 slurry Substances 0.000 claims description 29
- 239000000203 mixture Substances 0.000 claims description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 18
- 239000004202 carbamide Substances 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 11
- 150000001298 alcohols Chemical class 0.000 claims description 10
- 125000000217 alkyl group Chemical group 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 8
- 238000001704 evaporation Methods 0.000 claims description 7
- 125000004432 carbon atom Chemical group C* 0.000 claims description 6
- 230000008020 evaporation Effects 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 2
- 239000005977 Ethylene Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000003599 detergent Substances 0.000 description 17
- 239000002736 nonionic surfactant Substances 0.000 description 15
- 239000000047 product Substances 0.000 description 14
- 239000000843 powder Substances 0.000 description 12
- 239000002904 solvent Substances 0.000 description 10
- 239000004094 surface-active agent Substances 0.000 description 9
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 6
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- 239000000126 substance Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 4
- RZVAJINKPMORJF-UHFFFAOYSA-N Acetaminophen Chemical compound CC(=O)NC1=CC=C(O)C=C1 RZVAJINKPMORJF-UHFFFAOYSA-N 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 238000007711 solidification Methods 0.000 description 3
- 230000008023 solidification Effects 0.000 description 3
- 150000001449 anionic compounds Chemical class 0.000 description 2
- 239000003945 anionic surfactant Substances 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000012851 eutrophication Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 150000003013 phosphoric acid derivatives Chemical class 0.000 description 2
- 239000007921 spray Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 150000001721 carbon Chemical group 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 235000014113 dietary fatty acids Nutrition 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 239000000194 fatty acid Substances 0.000 description 1
- 229930195729 fatty acid Natural products 0.000 description 1
- 150000004665 fatty acids Chemical class 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- YEYZNBKNDWPFSQ-UHFFFAOYSA-N methanol;urea Chemical compound OC.NC(N)=O YEYZNBKNDWPFSQ-UHFFFAOYSA-N 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000008239 natural water Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000002000 scavenging effect Effects 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 239000000271 synthetic detergent Substances 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 210000002700 urine Anatomy 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D11/00—Special methods for preparing compositions containing mixtures of detergents
- C11D11/0082—Special methods for preparing compositions containing mixtures of detergents one or more of the detergent ingredients being in a liquefied state, e.g. slurry, paste or melt, and the process resulting in solid detergent particles such as granules, powders or beads
-
- 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
-
- 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
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/12—Water-insoluble compounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/32—Amides; Substituted amides
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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)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Description
i 142241in 142241
Opfindelsen angår en fremgangsmåde til fremstilling af en fritstrømmende partikelformet blanding af urinstof og en flydende ethoxyleret langkædet alkohol med en alkylkæde med fra ca. 12 til ca. 18 carbonatomer og gennemsnitlig fra ca.The invention relates to a process for the preparation of a free flowing particulate mixture of urea and a liquid ethoxylated long chain alcohol having an alkyl chain having from approx. 12 to approx. 18 carbon atoms and average from approx.
5 10 til ca. 19 ethylenoxidenheder.10 to approx. 19 ethylene oxide units.
De mest almindeligt anvendte overfladeaktive midler i kraftigt virkende detergentprodukter er anioniske forbindelser med rensende egenskaber. Typiske eksempler på disse anioniske forbindelser er de højere alkyl-enkernede-aromatiske sul-10 fonater, såsom de højere alkylbenzensulfonater. Disse syn tetiske detergenter medvirker effektivt til fjernelse af snavs fra tekstilstoffer, når de anvendes i forbindelse med phosphatbuildere, hvis funktion er at "blødgøre" vandet, der anvendes, og at tilvejebringe rensende virkning. Imidlertid 15 er der i dag stor diskussion med hensyn til nytten af at anvende phosphatforbindelser i detergentprodukter, på grund af deres påståede forårsagelse af eutrophicationsprocessen i søer, floder og strømme. Selv om eutrophicationsprocessen, hvori en overdreven vækst af vandplanteliv promulgeres i na-20 turlige vandmasser, forstås det ikke fuldstændigt, og det hævdes, at phosphatforbindelserne, der findes i detergent-holdigt spildvand, er en vigtig faktor i forbindelse med fremmeisen af dette fænomen.The most commonly used surfactants in powerful detergent products are anionic compounds with scavenging properties. Typical examples of these anionic compounds are the higher alkyl monomeric aromatic sulphonates such as the higher alkylbenzene sulphonates. These synthetic detergents effectively assist in removing dirt from textile fabrics when used in conjunction with phosphate builders whose function is to "soften" the water used and to provide a purifying effect. However, 15 there is much debate today regarding the utility of using phosphate compounds in detergent products, due to their alleged cause of the eutrophication process in lakes, rivers and streams. Although the process of eutrophication, in which excessive growth of aquatic life is promoted in natural water masses, is not completely understood and it is claimed that the phosphate compounds found in detergent-containing wastewater are an important factor in promoting this phenomenon.
Selv om ikke-ionogene overfladeaktive midler ikke er så 25 virksomme som anioniske overfladeaktive midler i nærværelsen af store mængder phosphatbuildere, har det vist sig, at når phosphatindholdet i et detergentprodukt reduceres væsentligt, tilvejebringer de ikke-ionogene overfladeaktive midler rensende virkninger, som er bedre end anioniske stoffers, i 30 produktet med det samme reducerede phosphatindhold. Rensningsvirkningen af ikke-ionogene overfladeaktive midler påvirkes tilsyneladende langt mindre af vandets hårdhed end rensningsvirkningen af de almindeligt anvendte anioniske overfladeaktive midler påvirkes. I det tilfælde at phosphatbuilderne 35 helt eller delvis fjernes fra detergenterne, kan inkorpore- 142241 2 ringen af voksende større mængder ikke-ionogene overfladeaktive midler i detergentprodukterne blive meget ønskelig.Although nonionic surfactants are not as effective as anionic surfactants in the presence of large amounts of phosphate builders, it has been found that when the phosphate content of a detergent product is substantially reduced, the nonionic surfactants provide purifying effects which are better than the anionic substances in the product with the same reduced phosphate content. The purification effect of nonionic surfactants is apparently much less affected by the water hardness than the purification effect of the commonly used anionic surfactants. In the event that the phosphate builders 35 are completely or partially removed from the detergents, the incorporation of growing larger amounts of nonionic surfactants into the detergent products may be highly desirable.
For tiden tilsættes små mængder ikke-ionogene overfladeaktive midler til detergentprodukter, først og fremmest for at 5 reducere den under vaskningen dannede skummængde. De mest almindeligt anvendte ikke-ionogene overfladeaktive midler er ethoxylerede langkædede alkoholer. Den ikke-ionogene ethoxamer, der anvendes, har typisk en 12-18 carbonatomhol-dig alkylkæde, og gennemsnitlig 10-19 ethylenoxidenheder.Presently, small amounts of nonionic surfactants are added to detergent products, primarily to reduce the amount of foam formed during the wash. The most commonly used nonionic surfactants are ethoxylated long chain alcohols. The nonionic ethoxamer used typically has a 12-18 carbon atom-containing alkyl chain, and an average of 10-19 ethylene oxide units.
10 Omfanget af ethylenoxidindhold, som giver den største rensningsvirkning i disse overfladeaktive midler, resulterer sædvanligvis i et ikke-ionogent materiale, som er en viskos væske ved stuetemperatur og derfor uegnet til direkte tilsætning til det tørre detergentpulver. Det har imidlertid 15 vist sig, at når en væsentlig mængde, typisk over 5 vægt%, ikke-ionogent overfladeaktivt middel inkorporeres i deter-gentopslæmningen før sprøjtetørring, opstår der et signifikant luftforureningsproblem. Dette problem, der i industrien kendes som "pluming", viser sig som en tæt sort røg, der ud-20 sendes fra sprøjtetårnet.The amount of ethylene oxide content which gives the greatest purification effect in these surfactants usually results in a nonionic material which is a viscous liquid at room temperature and therefore unsuitable for direct addition to the dry detergent powder. However, it has been found that when a significant amount, typically above 5% by weight, of nonionic surfactant is incorporated into the detergent slurry prior to spray drying, a significant air pollution problem occurs. This problem, known in the industry as "pluming," appears as a dense black smoke emitted from the spray tower.
Formålet med den foreliggende opfindelse er at tilvejebringe en fremgangsmåde til omdannelse af flydende ikke-ionogene overfladeaktive midler til tør fritstrømmende form, således at de let kan eftertilsættes til sprøjtetørrede detergent-25 produkter, for derved i væsentlig grad at forøge indholdet af ikke-ionogent overfladeaktivt middel i det færdige detergentprodukt. At gøre indholdet af ikke-ionogent overfladeaktivt middel i det fritstrømmende pulver, der kan tilsættes senere, så stort som muligt, og at vælge specielt egnede 30 bærere til de flydende ikke-ionogene materialer, er vigtige yderligere formål med opfindelsen.The object of the present invention is to provide a process for converting liquid nonionic surfactants into dry free flowing form so that they can be readily added to spray dried detergent products, thereby substantially increasing the content of nonionic surfactants. agent in the finished detergent product. Making the content of nonionic surfactant in the free-flowing powder which can be added later as large as possible and selecting particularly suitable carriers for the liquid nonionic materials are important further objects of the invention.
Fremgangsmåden ifølge opfindelsen til fremstilling af en fremgangsmåde til fremstilling af en fritstrømmende partikelformet blanding af urinstof og en flydende ethoxyleret lang- 142241 3 kædet alkohol med en alkylkæde med fra ca. 12 til ca. 18 carbonatomer og gennemsnitlig fra ca. 10 til ca. 19 ethylen= oxidenheder er ejendommelig ved, at a) der fremstilles en opslæmning af partikelformet urinstof 5 med en partikelstørrelse på under 0,074 mm og methanol,· b) opslæmningen indeholder fra ca. 80 til ca. 90 vægt% urinstof og fra ca. 10 til ca. 20 vægti methanol, c) opslæmningen blandes med den flydende ethoxylerede alka-hol i et vægtforhold alkohol:urinstof på mindst 3:2, 10 d) afdampning af i alt væsentlig alt methanol fra blandingen af opslæmningen og den ethoxylerede alkohol, og e) mikrofindelte silicapartikler sættes til blandingen af opslæmningen og ethoxyleret alkohol før afdampningen.The process of the invention for preparing a process for producing a free flowing particulate mixture of urea and a liquid ethoxylated long chain alcohol having an alkyl chain having from about 12 to approx. 18 carbon atoms and average from approx. 10 to approx. 19 ethylene = oxide units are characterized in that a) a slurry of particulate urea 5 having a particle size of less than 0.074 mm and methanol is prepared; b) the slurry contains from ca. 80 to approx. 90% by weight of urea and from approx. 10 to approx. C) the slurry is mixed with the liquid ethoxylated alcohol in a weight ratio of alcohol: urea of at least 3: 2, 10 d) evaporation of substantially all methanol from the mixture of the slurry and the ethoxylated alcohol, and e) microfine fraction silica particles are added to the mixture of the slurry and ethoxylated alcohol before evaporation.
Som det fremgår heraf, angår opfindelsen en hidtil ukendt 15 fremgangsmåde til fremstilling af urlnstof-ethoxamer-adduk= ter, som er fritstrømmende og indeholder mindst tre dele tensid pr. to dele urinstof, dvs. væsentligt mere end 50% tensid og således mere end den højeste mængde, som er angivet i den kendte teknik. Den hidtil ukendte fremgangsmåde 20 ifølge den foreliggende opfindelse, der omfatter de nye trin først at fremstille en opslæmning af urinstof og opløsningsmiddel, derpå forene opslæmningen med tensidkomponenten, tilsætte mikrofindelte silicapartikler og derpå afdampe opløsningsmidlet, giver overraskende og fordelagtigt et ad-25 dukt med det definerede tensidindhold.As can be seen, the invention relates to a novel process for the preparation of urea-ethoxamer adducts which are free-flowing and contain at least three parts of surfactant per day. two parts of urea, viz. substantially more than 50% surfactant and thus more than the highest amount indicated in the prior art. The novel process 20 of the present invention, comprising the new steps of first preparing a slurry of urea and solvent, then combining the slurry with the surfactant component, adding microfine silica particles and then evaporating the solvent, provides a surprising and advantageous product with the defined surfactant content.
I teknikken kendes fremgangsmåder til fremstilling af urin= stof-tensid-addukter og produkter med indtil 50% tensid.In the art, processes for the preparation of urine substance surfactant adducts and products with up to 50% surfactant are known.
Man har ikke tidligere kendt en fremgangsmåde som den i nærværende patentansøgning definerede til fremstilling af et 142241 4 fritstrømmende produkt med et tensidkomponentindhold på 60% eller mere.It is not known in the past for a method as defined in the present patent application to produce a free-flowing product having a surfactant component content of 60% or more.
Urinstof-ethoxamer-inklusionsforbindelserne fremstillet ved hjælp af den hidtil ukendte fremgangsmåde med indtil ca.The urea-ethoxamer inclusion compounds prepared by the novel process with up to about
5 62,5 vægt% ethoxamerindhold kan karakteriseres som fritstrøm mende pulvere. Som sådan kan de let tørblandes med partikelformede kraftigt virkende detergentpulvere, efter at de er sprøjtetørret. Det høje ethoxamerindhold i de hidtil ukendte inklusionsforbindelser tillader en væsentlig forøgelse af 10 indholdet af ikke-ionogent overfladeaktivt middel i pulverformede detergenter ved eftertilsætning, hvorved man undgår behandlingspluming og klæbrighedsproblemerne, som er karakteristiske for de tidligere kendte metoder.5 62.5% by weight ethoxamer content can be characterized as free flowing powders. As such, they can be readily dry blended with particulate strong-acting detergent powders after spray-dried. The high ethoxamer content of the novel inclusion compounds allows a substantial increase in the content of nonionic surfactant in powdered detergents upon addition, thereby avoiding treatment plummeting and the stickiness problems characteristic of the prior art methods.
Fritstrømmende urinstof-ethoxamer-inklusionsforbindelser, frem- 15 stillet i overensstemmelse med den hidtil ukendte metode og under anvendelse af methanol som opslæmningsmiddel, er blevet opnået med et ethoxamerindhold så højt som ca. 62,5 vægt%. Opløsningsmidlet i urinstof-opløsningsmiddelopslæmningen er fortrinsvis den minimale mængde, som resulterer i en viskos 20 masse. Denne minimumsmængde er typisk mellem ca. 10 og 20 vægt% af opslæmningsblandingen.Free-flowing urea-ethoxamer inclusion compounds prepared in accordance with the novel method and using methanol as a slurry have been obtained with an ethoxamer content as high as ca. 62.5% by weight. Preferably, the solvent in the urea-solvent slurry is the minimum amount which results in a viscous mass. This minimum amount is typically between approx. 10 and 20% by weight of the slurry mixture.
Partikelstørrelsen af urinstoffet anvendt til dannelse af opslæmningen har vist sig at være en betydningsfuld faktor til bestemmelse af det endelige ethoxamerindhold i inklu-25 sionsforbindelsen. Det har vist sig, at jo finere partiklet urinstof, der anvendes, jo større er det endelige ethoxamer= indhold i inklusionsforbindelsen. Yderligere blev der konstateret kortere tørrings- eller hærdningstider, når der blev anvendt urinstof med finest partikelstørrelse.The particle size of the urea used to form the slurry has been found to be a significant factor in determining the final ethoxamer content of the inclusion compound. It has been found that the finer particle urea used, the greater the final ethoxamer = content of the inclusion compound. Further, shorter drying or curing times were found when using the finest particle size urea.
5 14224 15 14224 1
Ved fremgangsmåden ifølge opfindelsen kan der anvendes urinstofpartikler, der kan passere gennem en U.S.sigte nr. 200 (0,074 ram) (i det følgende forkortet som en partikelstørrelse på -200 si) til dannelse af urinstof-opløsningsmiddelopslæm-5 ning.In the process of the invention, urea particles which can pass through a U.S. sieve No. 200 (0.074 ram) (hereinafter abbreviated as a particle size of -200 s) can be used to form urea-solvent slurry.
Ifølge opfindelsen kan tørringstiden, dvs. det tidsrum ved stuetemperatur, som er nødvendig for, at blandingen af opslæmningen og ethoxamer størkner til et fast fritstrømmende pulver, reduceres væsentligt ved at tilsætte mikrofindelte 10 silicapartikler, sædvanligvis i mængder på mindre end ca.According to the invention, the drying time, i.e. the time at room temperature required for the mixture of the slurry and ethoxamer to solidify into a solid free-flowing powder is substantially reduced by adding microfine 10 silica particles, usually in amounts of less than about 10%.
5 vægt%, til blandingen. De følgende stoffer har vist sig at være virksomme i forskellig grad til at reducere tørringstiden for blandingen af opslæmning og ethoxamer: Submik.ro- skopiske pyrogene siliciumdioxidpartikler ("Cab-O-Sil", frem-15 stillet af Cabot Corporation), svampelignende silicagel ("Sy- loid", fra Davison Chemical Div. af W.R. Grace Company}*5% by weight, to the mixture. The following substances have been found to be variously effective in reducing the drying time of the slurry and ethoxamer mixture: Submicroscopic pyrogenic silica particles ("Cab-O-Sil", manufactured by Cabot Corporation) ("Syloid", from Davison Chemical Div. By WR Grace Company} *
Ifølge en særlig udførelsesform for de hidtil ukendte fremgangsmåder har det vist sig, at det tidspunkt i løbet af processen, hvor størkningshjælpemidlet tilsættes til urinstof-20 ethoxameropslæmningen, er signifikant. I denne henseende har det vist sig, at tørringstiden kan reduceres væsentligt ved at tilsætte silicapartiklerne til opslæmning-ethoxamer-blan-dingen, efter at en væsentlig del af methanolet har fået lov til at fordampe ved stuetemperatur. Dette indebærer sæd-25 vanligvis, at opslæmning-ethoxamer-blandingen får lov til at henstå ved stuetemperatur i ca. 1 time før størkningshjælpemidlet blandes i blandingen. Der anvendes ethoxamere med en alkylkæde med fra 12 til 18 carbonatoraer og gennemsnitlig fra ca.10 til ca,19 ethylenoxidenheder. Foretrukne ethoxa= 142241 6 mere er tilgængelige under handelsnavnet "Neodol 45-11” og "AlfonicS'1618-78”. "Neodol 45-11" er en ethoxyleret alkohol med en alkylkæde på 14-15 carbonatomer og gennemsnitlig 11 ethylenoxidenheder, fremstillet af Shell Chemical Corpora-5 tion. Ligeledes er "Alfonic^ 1618-78" en ethoxyleret fedtal= kohol med en alkylkæde på 16-18 carbonatomer og gennemsnitlig 19 ethylenoxidenheder, fremstillet af Continental Oil Company.According to a particular embodiment of the novel processes, it has been found that the time during the process when the solidification aid is added to the urethane ethoxamer slurry is significant. In this regard, it has been found that the drying time can be substantially reduced by adding the silica particles to the slurry-ethoxamer mixture after a substantial portion of the methanol has been allowed to evaporate at room temperature. This usually implies that the slurry-ethoxamer mixture is allowed to stand at room temperature for approx. 1 hour before the solidification aid is mixed into the mixture. Ethoxamers having an alkyl chain having from 12 to 18 carbon atoms and on average from about 10 to about 19 ethylene oxide units are used. Preferred ethoxa = 142241 6 more are available under the trade names "Neodol 45-11" and "AlfonicS'1618-78". "Neodol 45-11" is an ethoxylated alcohol having an alkyl chain of 14-15 carbon atoms and an average of 11 ethylene oxide units, made by Shell Chemical Corporation. Likewise, "Alfonic ^ 1618-78" is an ethoxylated fatty acid = carbon having an alkyl chain of 16-18 carbon atoms and an average of 19 ethylene oxide units, manufactured by Continental Oil Company.
Ved udøvelsen af den hidtil ukendte fremgangsmåde fremstil-10 les en opslæmning med ca. 10-20 vægt% opløsningsmiddel og 80-90 vægt% urinstof i partikelform. Opslæmningen blandes derpå med en ethoxamermængde, som er tilstrækkelig til at give et vægtforhold fra ca. 3/2 til ca. 3,5/2 med det i opslæmningen tilstedeværende urinstof. Blandingen af opslæm-15 ningen og ethoxamerblandingen gennemføres fortrinsvis ved anvendelse af forskydningskræfter og tryk, som med en labo= ratoriemorter og støder. Opslæmning-ethoxamerblandingen får derpå lov til at henstå ved stuetemperatur i ca. 1 time. I løbet af dette tidsrum fordamper en væsentlig del af opløs-20 ningsmidlet, og blandingen, som dog- stadig er våd, bliver hårdere og tørrere end da den oprindelig blev blandet. Et størkningshjælpemiddel kan derpå tilsættes til opslæmning-ethoxamer-blandingen. Størkningshjælpemidlet blandes omhyg-, geligt i blandingen i små mængder, indtil der opnås et fint, 25 tørt pulver. Der opnås typisk et fint, tørt pulver, når størkningshjælpemidlet indgår i en mængde på mindre end ca. 5 vægt% af slutblandingen og efter fordampning af mindst 99% f·;:· 7 142241 af opløsningsmidlet. Det resulterende fritstrømmende pulver indeholder en begrænset mængde opløsningsmiddel, typisk mindre end ca. 1 vægt% af inklusionsforbindelsen.In the practice of the novel method, a slurry of approx. 10-20 wt% solvent and 80-90 wt% urea in particulate form. The slurry is then mixed with an amount of ethoxamer sufficient to give a weight ratio of approx. 3/2 to approx. 3.5 / 2 with the urea present in the slurry. The mixture of the slurry and the ethoxamer mixture is preferably carried out using shear forces and pressures, as with a laboratory mortar and impactor. The slurry-ethoxamer mixture is then allowed to stand at room temperature for approx. 1 hour. During this time, a substantial portion of the solvent evaporates and the mixture, however still wet, becomes harder and drier than when it was initially mixed. A solidification aid can then be added to the slurry-ethoxamer mixture. The solidifying aid is mixed gently in the mixture in small quantities until a fine, dry powder is obtained. Typically, a fine, dry powder is obtained when the solidifying agent is present in an amount of less than about 100%. 5% by weight of the final mixture and after evaporation of at least 99% of the solvent. The resultant free-flowing powder contains a limited amount of solvent, typically less than about 10%. 1% by weight of the inclusion compound.
Eksempel.Example.
5 Ifølge den foregående fremgangsmåde blev 2 ml methanol blan det med 5 g urinstofpartikler med en diameter på højst 0,074 mm, idet de kan passere en U.S. sigte nr. 200, til dannelse af en opslæmning. Ca. 5-9,3 g "Neodol 45-11" ethoxamer blev lidt efter lidt og omhyggeligt blandet med urinstof-methanol= 10 opslæmningen. En væsentlig del af methanolopløsningsmidlet blev derpå fordampet fra blandingen, ved at denne henstod ved stuetemperatur i ca. 1 time. Efter denne times henstand var blandingen stadig våd, selv om den var væsentlig hårdere og tørrere end da den oprindelig blev blandet. På dette 15 tidspunkt blev ca. 0,5 g silicastof, typisk "Cab-O-Sil" eller "Syloid", tilsat til og blandet med den stadig våde ορέ læmning-ethoxamer-blanding i små mængder, indtil der blev opnået et fint tørt pulver. Det fritstrømmende pulver, der blev fremstillet i overensstemmelse med den foregående me-20 tode, og indeholdende fra ca. 50 til ca. 62,5 vægt% af et rensende ikke-ionogent overfladeaktivt middel, er et meget velegnet post additiv til sprøjtetørrede detergentpulvere.According to the foregoing procedure, 2 ml of methanol was blended with 5 g of urea particles with a diameter not exceeding 0.074 mm, capable of passing a U.S. screen No. 200, to form a slurry. Ca. 5-9.3 g of "Neodol 45-11" ethoxamer was gradually and carefully mixed with urea-methanol = the slurry. A substantial portion of the methanol solvent was then evaporated from the mixture, leaving it at room temperature for approx. 1 hour. After this hour's stand, the mixture was still wet, although substantially harder and drier than when it was originally mixed. At this time, approx. 0.5 g of silica, typically "Cab-O-Sil" or "Syloid", added to and mixed with the still wet ορέ curing ethoxamer mixture in small amounts until a fine dry powder is obtained. The free-flowing powder prepared in accordance with the foregoing method, containing from ca. 50 to approx. 62.5% by weight of a cleansing nonionic surfactant is a very suitable item additive for spray-dried detergent powders.
Den hidtil ukendte fremgangsmåde løser problemerne med hensyn til crutcher gelering, pluming og håndtering, som opstår, 25 når man gør forsøg på i væsentlig grad at forøge indholdet af ikke-ionogent overfladeaktivt middel i sprøjtetørrede detergentprodukter over ca. 5 vægt%. Det ved hjælp af den hidtil ukendte fremgangsmåde fremstillede fritstrømmende pulver kan eftertilsættes til sprøjtetørrede detergentprodukter til 30 væsentlig forøgelse af indholdet af ikke-ionogent overfladeaktivt middel. For eksempel med faciliteter til eftertilsæt-ning af 20 vægt% af et pulverformet detergentprodukt kan indholdet af ikke-ionogent overfladeaktivt middel i slutproduktet forøges fra de typiske 2-5 vægt% til ca. 15-20 vægt%.The novel method solves the problems of crutcher gelling, pluming and handling that occur when attempting to substantially increase the content of nonionic surfactant in spray-dried detergent products over approx. 5% by weight. The free-flowing powder prepared by the novel process can be added to spray-dried detergent products to substantially increase the content of nonionic surfactant. For example, with facilities for the addition of 20% by weight of a powdered detergent product, the content of nonionic surfactant in the final product can be increased from the typical 2-5% by weight to approx. 15-20% by weight.
Claims (4)
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US11467571A | 1971-02-11 | 1971-02-11 | |
| US11467571 | 1971-02-11 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| DK142241B true DK142241B (en) | 1980-09-29 |
| DK142241C DK142241C (en) | 1981-02-23 |
Family
ID=22356736
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| DK50572AA DK142241B (en) | 1971-02-11 | 1972-02-04 | Process for the preparation of free-flowing nonionic urea-ethoxamer inclusion compounds. |
Country Status (6)
| Country | Link |
|---|---|
| BE (1) | BE779138A (en) |
| DK (1) | DK142241B (en) |
| ES (1) | ES399670A1 (en) |
| IT (1) | IT949705B (en) |
| SE (1) | SE411460B (en) |
| ZA (1) | ZA72343B (en) |
-
1972
- 1972-01-18 ZA ZA720343A patent/ZA72343B/en unknown
- 1972-02-03 IT IT48121/72A patent/IT949705B/en active
- 1972-02-04 DK DK50572AA patent/DK142241B/en unknown
- 1972-02-09 BE BE779138A patent/BE779138A/en unknown
- 1972-02-10 SE SE7201569A patent/SE411460B/en unknown
- 1972-02-11 ES ES399670A patent/ES399670A1/en not_active Expired
Also Published As
| Publication number | Publication date |
|---|---|
| DK142241C (en) | 1981-02-23 |
| BE779138A (en) | 1972-05-30 |
| ZA72343B (en) | 1973-08-29 |
| ES399670A1 (en) | 1974-12-01 |
| SE411460B (en) | 1979-12-27 |
| IT949705B (en) | 1973-06-11 |
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