DK159812B - QUICK-DRY, STABLE, SLIM POWDER SUSPENSION, ITS APPLICATION AND PROCEDURE FOR ITS PREPARATION - Google Patents

QUICK-DRY, STABLE, SLIM POWDER SUSPENSION, ITS APPLICATION AND PROCEDURE FOR ITS PREPARATION Download PDF

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DK159812B
DK159812B DK578881A DK578881A DK159812B DK 159812 B DK159812 B DK 159812B DK 578881 A DK578881 A DK 578881A DK 578881 A DK578881 A DK 578881A DK 159812 B DK159812 B DK 159812B
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suspension
hydroxyethyl cellulose
alcohol
water
aqueous
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DK578881A
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DK159812C (en
DK578881A (en
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Frank William Marschner
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Colgate Palmolive Co
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    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q15/00Anti-perspirants or body deodorants
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/06Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite
    • A61K47/08Organic compounds, e.g. natural or synthetic hydrocarbons, polyolefins, mineral oil, petrolatum or ozokerite containing oxygen, e.g. ethers, acetals, ketones, quinones, aldehydes, peroxides
    • A61K47/10Alcohols; Phenols; Salts thereof, e.g. glycerol; Polyethylene glycols [PEG]; Poloxamers; PEG/POE alkyl ethers
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K47/00Medicinal preparations characterised by the non-active ingredients used, e.g. carriers or inert additives; Targeting or modifying agents chemically bound to the active ingredient
    • A61K47/30Macromolecular organic or inorganic compounds, e.g. inorganic polyphosphates
    • A61K47/36Polysaccharides; Derivatives thereof, e.g. gums, starch, alginate, dextrin, hyaluronic acid, chitosan, inulin, agar or pectin
    • A61K47/38Cellulose; Derivatives thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/27Zinc; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
    • A61K8/731Cellulose; Quaternized cellulose derivatives
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00Medicinal preparations characterised by special physical form
    • A61K9/0012Galenical forms characterised by the site of application
    • A61K9/0014Skin, i.e. galenical aspects of topical compositions

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Epidemiology (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Inorganic Chemistry (AREA)
  • Medicinal Chemistry (AREA)
  • Birds (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Dermatology (AREA)
  • Cosmetics (AREA)
  • Medicinal Preparation (AREA)

Description

iin

DK 159812 BDK 159812 B

Den foreliggende opfindelse angår en hurtigttørrende, stabil, si i magt i g suspension af findelte faste partikler, suspensio-, nens anvendelse og en fremgangsmåde til fremstilling af suspensionen, der er ensartet suspenderet i en bærer omfattende 5 et højt alkoholindhold af en lavere alifatisk monovalent alkohol og et lavt vandindhold, og hydroxyethylcel 1ulose som suspenderingsmiddel, og som især har anvendelighed i medicinske lotioner og produkter til den personlige hygiejne, såsom rollons, dansesko, lotioner og på forskellige substrater, såsom 10 deodorantpuder.The present invention relates to a quick-drying, stable, powerful suspension of finely divided solid particles, the use of the suspension, and a method of preparing the suspension uniformly suspended in a carrier comprising a high alcohol content of a lower aliphatic monovalent alcohol. and a low water content, and hydroxyethyl cellulose as a suspending agent, and having particular utility in medical lotions and personal hygiene products such as rollons, dance shoes, lotions and on various substrates such as 10 deodorant pads.

Produkter på basis af alkohol foretrækkes i reglen på grund af deres hurtigttørrende og udmærkede opløseliggørende egenska ber. Uorganiske salte er dog i almindelighed uopløselige i al-15 kohol, hvorfor præparater heraf kræver højere forhold mellem vand og alkohol, hvilket giver vådere produkter, som tørrer langsommere. Saltkoncentrationer er også begrænsede af deres opløselighed i sådanne systemer. På den anden side afhænger opløseligheden af organiske forbindelser (f.eks. parfumer) af 20 et højt alkoholindhold, med mindre de er emulgerede, og derfor kræves i reglen kompromier. Visse salte, såsom natriumbi-carbonat, dekomponerer i vand eller vand/alkoholopløsninger og omdannes til natriumcarbonat, og derfor må der anvendes en pulversuspension.Alcohol-based products are generally preferred because of their quick-drying and excellent solubilizing properties. However, inorganic salts are generally insoluble in alcohol, so preparations thereof require higher water-alcohol ratios, resulting in wetter products which dry more slowly. Salt concentrations are also limited by their solubility in such systems. On the other hand, the solubility of organic compounds (e.g., perfumes) depends on a high alcohol content, unless they are emulsified, and therefore compromises are usually required. Certain salts, such as sodium bicarbonate, decompose in water or water / alcohol solutions and are converted to sodium carbonate and therefore a powder suspension must be used.

2525

De foreliggende hidtil ukendte vandige alkoholiske suspensioner indeholdende hydroxyethylceu1lulose som det væsentlige suspenderingsmiddel gør det muligt at anvende alkoholopløselige og uopløselige bestanddele i hurtigttørrende produkter in-30 deholdende et højt alkoholindhold.The present novel aqueous alcoholic suspensions containing hydroxyethyl cellulose as the major suspending agent make it possible to use alcohol soluble and insoluble ingredients in fast drying products containing a high alcohol content.

Den kendte teknik er fuld af præparater indeholdende hydroxy-ethylcellulose, som fortykkelsesmiddel som sådan eller i kombination med andre fortykkelsesmidler, som beskrevet i ameri-35 kansk patent nr. 4.002.881, som angår et tandplejemiddel, og i amerikansk patent nr. 4.145.413, som angår et middel til at gøre huden mørk. Hydroxyethylcellulosen danner en vandig gel i de nævnte præparater, og bevirker derved en fortykkelse.The prior art is full of compositions containing hydroxyethyl cellulose, as a thickener as such or in combination with other thickeners, as disclosed in U.S. Patent No. 4,002,881, which relates to a dentifrice, and in U.S. Patent No. 4,145. 413, which relates to a means of darkening the skin. The hydroxyethyl cellulose forms an aqueous gel in said compositions, thereby causing a thickening.

22

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En anden gruppe præparater, der anvender hydroxyethylcellulo-se som et middel til at regulere lægemiddelfrigørelse af en medicintablet, er terapeutiske præparater til vedligeholdt frigørelse, som beskrevet i de amerikanske patenter nr. 3.136.Another group of compositions utilizing hydroxyethyl cellulose as a means of regulating drug release of a drug tablet are sustained release therapeutic compositions, as described in U.S. Patents No. 3,136.

5 695, 4.235.870 og 4.167.558.5,695, 4,235,870 and 4,167,558.

Hydroxyethylcellulose har også været anvendt som stabiliseringsmiddel til et præparat indeholdende prostaglandin E gruppen, som vist i amerikansk patent nr. 4.036.954, og som et 10 filmdannende bærestof for et lægemiddel, som vist i amerikansk patent nr. 4.136.162.Hydroxyethyl cellulose has also been used as a stabilizer for a composition containing the prostaglandin E group, as shown in U.S. Patent No. 4,036,954, and as a film-forming carrier for a drug, as disclosed in U.S. Patent No. 4,136,162.

Stabile vandige dispersioner eller suspensioner af faste stoffer eller vanduopløselige forbindelser indeholdende hydroxy-15 ethylcellulose som det ene af en stabiliserende eller en suspenderende kombination er beskrevet i amerikansk patent nr. 3.258.326, som angår et fast pesticidt middel i vandige medier, og i amerikansk patent nr. 3.927.205, der beskriver en vandig suspension af et vanduopløseligt eller sparsomt opløse-20 ligt farmaceutisk stof. Amerikansk patent nr. 3.387.222 beskriver en vandig opløsning eller suspension af et terapeutisk middel indeholdende hydroxyethylcellulose som fortykkelsesmiddel, og som er nyttigt som imprægneringsmiddel til en syntetisk medicinsk forbinding.Stable aqueous dispersions or suspensions of solids or water-insoluble compounds containing hydroxyethyl cellulose as one of a stabilizing or suspending combination are described in U.S. Patent No. 3,258,326, which relates to a solid pesticidal agent in aqueous media, and in U.S. Pat. No. 3,927,205, which discloses an aqueous suspension of a water-insoluble or sparingly soluble pharmaceutical. U.S. Patent No. 3,387,222 discloses an aqueous solution or suspension of a therapeutic agent containing hydroxyethyl cellulose as a thickening agent and useful as an impregnating agent for a synthetic medical compound.

2525

Amerikansk patent nr. 3.290.218 beskriver endvidere, at en vandig eller ikke-vandig suspension af vanduopløselig ethylcellulose giver en stabil suspension af et farmaceutisk eller kosmetisk aktivt fast stof. Oet er væsentligt, at ethylcellu-3Q losen er i hovedsagen uopløselig i de vandige eller ikke-van-dige bærevæsker.U.S. Patent No. 3,290,218 further discloses that an aqueous or non-aqueous suspension of water-insoluble ethyl cellulose provides a stable suspension of a pharmaceutical or cosmetically active solid. It is essential that the ethyl cellulose-3Q solution be substantially insoluble in the aqueous or non-aqueous carrier liquids.

Vandige ethanolopløsninger af natrium eller kaliumbicarbonat som deodorantprodukter er beskrevet i britisk patent nr.Aqueous ethanol solutions of sodium or potassium bicarbonate as deodorant products are described in British patent no.

35 1.553.739. Selv om disse bicarbonatopløsninger er effektive deodoranter, er der iagttaget armhuleirritation ved en mængde kaliumbicarbonat på ca. 10%. Det har også vist sig, at vandige35, 1,553,739. Although these bicarbonate solutions are effective deodorants, armpit irritation has been observed at an amount of potassium bicarbonate of approx. 10%. It has also been found to be watery

DK 159812 BDK 159812 B

3 eller vandig/alkoholiske natriumbicarbonatopløsninger er pH ustabi1e.3 or aqueous / alcoholic sodium bicarbonate solutions are pH stable.

Ældningsundersøgelser har vist, at bicarbonatet i opløsning 5 nedbrydes og frigør CO2 og gradvis omdannes til natriumcarbo-nat (et kendt hudirritationsmiddel). Bicarbonatopløsninger har også opløsel ighedsbegrænsninger. Der kræves forholdsvis store mængder vand til højere bicarbonatmængder. Som følge heraf tillades mindre alkohol, hvilket resulterer i vådere og lang-10 sommere tørrende produkter. Fremstilling af natriumbicarbonat-opløsninger over 6,9% er endvidere umulig på grund af dets begrænsede vandopløselighed.Aging studies have shown that the bicarbonate in solution 5 decomposes and releases CO 2 and gradually converts to sodium carbonate (a known skin irritant). Bicarbonate solutions also have dissolution constraints. Relatively large amounts of water are required for higher amounts of bicarbonate. As a result, less alcohol is allowed, resulting in wetter and longer-summer drying products. Furthermore, preparation of sodium bicarbonate solutions above 6.9% is impossible due to its limited water solubility.

Den kendte teknik beskriver også aerosol suspens i oner, som dis-15 penseres via en beholder under tryk, og som indeholder natriumbi ncarbonat opslæmmet med drivmidler i en 50:50 blanding i amerikansk patent nr. 2.959.225, og alkalimetalbicarbonat i en 0,3 til 15% drivmiddelopløselig bærer såsom ethanol med ca.The prior art also discloses aerosol suspension in ones dispensed via a pressurized container containing sodium bicarbonate suspended with propellants in a 50:50 mixture of U.S. Patent No. 2,959,225, and alkali metal bicarbonate in a 0. 3 to 15% propellant soluble carrier such as ethanol with approx.

90% drivmiddel i britisk patent nr. 1.476.117. Vanskeligheder-20 ne og ulemperne med aerosolsuspensioner af natrium eller kali-umbicarbonat, der er diskuteret i førnævnte patenter, indbefatter udfældning og/eller agglomerering af de tørre partikler, tilstopning af dispenseringsdysen, uensartet udsprøjt-° ning af deodorantmateriale, manglende, vedhæftning af bicarbo-25 natdeodoranten på det sprøjtede område, på grund af tilbagespringningen af det tørre pulver og/eller en for våd sprøjtevæske, der resulterer i en for lang tørretid, foruden at den er skadelig for omgivelserne.90% propellant in British Patent No. 1,476,117. The difficulties and disadvantages of sodium or potassium bicarbonate aerosol suspensions discussed in the aforementioned patents include precipitation and / or agglomeration of the dry particles, clogging of the dispensing nozzle, non-uniform spraying of deodorant material, lack of deodorant material, -25 night deodorant on the sprayed area, due to the return of the dry powder and / or too wet spray liquid resulting in too long a drying time, besides being detrimental to the environment.

30 Der findes imidlertid ingen beskrivelse af en stabil suspension af findelte faste stoffer i et vandigt alkoholisk medium, såsom ethanol, indeholdende et højt alkoholindhold og et minimalt vandindhold, ved anvendelse af hydroxethylcellulose, som det væsentlige suspenderingsmiddel.30 However, there is no description of a stable suspension of finely divided solids in an aqueous alcoholic medium, such as ethanol, containing a high alcohol content and a minimal water content, using hydroxethyl cellulose as the major suspending agent.

Formålet med den foreliggende opfindelse er at angive en stabil, hurtigttørende slimagtig pulversuspension i et alkoholisk 35 4The object of the present invention is to provide a stable, fast-drying mucous powder suspension in an alcoholic

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medium indeholdende en minimal mængde vand, og en kritisk mængde hydroxyethylcellulose som suspenderingsmiddel i mængder over dens normale opløse! ighed i det alkoholiske medium, hvilken suspension kræver ingen eller ringe rystning før brugen, 5 specielt en suspension, hvori pulveret er alkalimetalbicarbo-nat.medium containing a minimal amount of water, and a critical amount of hydroxyethyl cellulose as suspending agent in amounts above its normal solution! in the alcoholic medium, which suspension requires no or little shaking before use, especially a suspension in which the powder is alkali metal bicarbonate.

Pulversuspensionen ifølge opfindelsen er ejendommelig ved, at mængden af hydroxyethylcellulose overstiger opløseligheden for 10 den vandopløselige hydroxyethylcellulose i alkoholen, og vandindholdet er tilstrækkeligt til at forhindre udfældning af suspenderingsmidlet og mindst 5 vægt%.The powder suspension according to the invention is characterized in that the amount of hydroxyethyl cellulose exceeds the solubility of the water-soluble hydroxyethyl cellulose in the alcohol, and the water content is sufficient to prevent precipitation of the suspending agent and at least 5% by weight.

Mere specielt angår den foreliggende opfindelse en suspension, 15 hvori det suspenderede pulver består af alkalimetalbicarbonat-partikler og udgør 1-20 vægt/vægt%. Det alkoholiske medium kan være en lavere monovalent alkohol valgt blandt gruppen bestående af methanol, ethanol, isopropanol og blandinger deraf. Brugen af polyvalente alkoholer, såsom propylenglycol, buty-20 lenglycol og polyoler deraf, og glycerin nedsætter den kritiske mængde vand, som kræves i det hydroxyethylcelluloseholdige alkoholiske medium. Tilsætning af alkoholopløselige forbindelser, såsom olier, parfumer, osv. har ingen skadelig virk-ing på egenskaberne af de foreliggende vandige alkoholiske 25 pulversuspensioner. Tilstedeværelse af medsuspenderingsmidler, såsom si 1iciumdioxid, bentonit og lignende har heller ingen skadelig virkning på de vandige alkoholiske pul versuspensioner ifølge opfindelsen.More particularly, the present invention relates to a suspension in which the suspended powder consists of alkali metal bicarbonate particles and is 1-20 w / w%. The alcoholic medium may be a lower monovalent alcohol selected from the group consisting of methanol, ethanol, isopropanol and mixtures thereof. The use of polyhydric alcohols, such as propylene glycol, butylene glycol and polyols thereof, and glycerine reduce the critical amount of water required in the hydroxyethyl cellulose-containing alcoholic medium. Addition of alcohol-soluble compounds such as oils, perfumes, etc. has no detrimental effect on the properties of the present aqueous alcoholic powder suspensions. Also, the presence of co-suspending agents such as silica, bentonite and the like has no detrimental effect on the aqueous alcoholic pulse versus suspensions of the invention.

30 Det har overraskende vist sig, at pulvere kan suspenderes i alkoholiske/vandige medier indeholdende et højt alkoholindhold og et lavt vandindhold ved at anvende den vandopløselige hy-droxyethylcellulose i mængder over dens alkoholopløselighed, som kan øges af specielle polyvalente alkoholer. Denne polymer 35 er enestående ved sin evne til at danne stabile suspensioner.30 Surprisingly, it has been found that powders can be suspended in alcoholic / aqueous media containing a high alcohol content and a low water content by using the water-soluble hydroxyethyl cellulose in amounts above its alcohol solubility which can be increased by special polyhydric alcohols. This polymer 35 is unique in its ability to form stable suspensions.

Selv om hydroxyethylcellulose normalt betragtes som et fortykkelsesmiddel til systemer af den vandige type, har den vistAlthough hydroxyethyl cellulose is usually considered a thickener for aqueous type systems, it has shown

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5 at have usædvanlige suspenderingsegenskaber i vandige alkoholiske systemer med højt alkoholindhold. Sådanne suspensioner er seje og slimagtige og giver udmærkede suspenderingsegenskaber. Dette suspenderingsmiddel giver exceptionel stabile slim-5 agtige suspensioner uden nogen pulverudski11e1 se efter 13 uger ved -18eC, 4°C, omgivelsernes temperatur, 35°C, 43°C og 49°C, og kræver ingen rystning før brugen. Denne uventede egenskab, at danne en stabil slimagtig pulversuspension i et medium med højt alkoholindhold og lavt vandindhold, haves ikke af andre 10 cellulosederivater, såsom hydroxypropylcellulose, natriumcar-boxymethylcellulose, hydroxypropylmethylcellulose (methocel) og andre vandopløselige polymere. Under anvendelse af 10% mikropulveriseret natriumbicarbonat som det partikel formede materiale, der skal suspenderes, i et alkoholisk/vandigt me-15 dium indeholdende 25% vand, blev suspenderingsegenskaberne af andre vandopløselige cel 1uloseagtige gummier afprøvet ved tilsætning af 0,4% hydroxypropylmethylcellulose, 0,4% hydroxy-propylcellulose, eller 0,8% natriumcarboxymethylcellulose. Det viste sig, at alle de ovennævnte prøver skilte ad med et klart 20 vandlag for oven, idet adskillelsen skete i løbet af minutter. Det fysiske udseende af den ønskede suspension er dannelsen af en slimagtig væske, der synes sej, når den hældes. De foreliggende hidtil ukendte alkoholiske/vandige hydroxyethylcellulo-seholdige medier giver fremragende suspenderingsegenskaber for 25 pulvere med udmærket stabilitet inden for et bredt temperaturinterval .5 having unusual suspending properties in high alcoholic aqueous alcoholic systems. Such suspensions are cool and slimy and provide excellent suspending properties. This suspending agent provides exceptionally stable mucus-like suspensions without any powder excretion after 13 weeks at -18 ° C, 4 ° C, ambient temperature, 35 ° C, 43 ° C and 49 ° C, and requires no shaking prior to use. This unexpected property of forming a stable mucosal powder suspension in a high alcohol and low water content medium is not borne by other cellulose derivatives such as hydroxypropyl cellulose, sodium carboxymethyl cellulose, hydroxypropyl methyl cellulose (methocel) and other water-soluble polymers. Using 10% micropulvered sodium bicarbonate as the particulate material to be suspended in an alcoholic / aqueous medium containing 25% water, the suspending properties of other water-soluble cellulose-like gums were tested by the addition of 0.4% hydroxypropylmethylcellulose, , 4% hydroxypropyl cellulose, or 0.8% sodium carboxymethyl cellulose. It was found that all of the above samples separated a clear 20 water layer from above, the separation occurring within minutes. The physical appearance of the desired suspension is the formation of a slimy liquid that appears cool when poured. The present novel alcoholic / aqueous hydroxyethyl cellulose-containing media provide excellent suspending properties for 25 powders of excellent stability over a wide temperature range.

Produkterne afgives godt fra roll-on og pumpedispensere. Sejheden af hydroxyethylsuspensionssystemet antages at være grun-30 den til dets bedre suspenderingsegenskaber.The products are delivered well from roll-on and pump dispensers. The toughness of the hydroxyethyl suspension system is believed to be due to its better suspending properties.

Foruden hydroxyethylcel1ulosen, som er det væsentlige suspenderingsmiddel, er det valgfrit at anvende medsuspenderingsmidler, såsom findelt si 1iciumdioxid (Cab-O-sil) eller betonit i 35 kombination med hydroxyethylcellulose. Hydroxyethylcellulosen som sådan udgør ca. 0,1 til 1%, og det findelte siliciumdio-xid eller bentonit udgør ca. 0,1 til 1%, og den samlede mængde er fortrinsvis ca. 0,9 til 2 vægt% af det samlede præparat.In addition to the hydroxyethyl cellulose, which is the major suspending agent, it is optional to use co-suspending agents such as finely divided silica (Cab-O-sil) or concreteite in combination with hydroxyethyl cellulose. The hydroxyethyl cellulose as such constitutes approx. 0.1 to 1%, and the finely divided silica or bentonite constitutes approx. 0.1 to 1%, and the total amount is preferably about 0.9 to 2% by weight of the total composition.

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66

Det partikelformede materiale suspenderet i den alkoholiske/ vandige bærer kan være ethvert uorganisk eller organisk salt, der er uopløseligt i alkohol, såsom natrium eller kaliumbicar-bonat, zinkundecylenat, pigmenter, visse aluminium eller zir-5 konforbindelser og lignende. Specielt kan det suspenderede pulver, som er uopløseligt i alkohol, vælges af gruppen bestående af et uorganisk eller organisk metalsalt, pigment, mineral, polymer eller salt deraf, eller pulvere afledt af korn.The particulate material suspended in the alcoholic / aqueous carrier may be any inorganic or organic salt which is insoluble in alcohol, such as sodium or potassium bicarbonate, zinc decylene, pigments, certain aluminum or zirconium compounds and the like. In particular, the suspended powder which is insoluble in alcohol may be selected by the group consisting of an inorganic or organic metal salt, pigment, mineral, polymer or salt thereof, or powders derived from grains.

Det har vist sig at høje mængder af saltet eller andet pulve- 10 riseret materiale kan suspenderes i de foreliggende alkoholi- ske/vandige medier indeholdende hydroxyethylcel1ulose, som suspenderingsmiddel. Herved kan store mængder partikelformet materiale inkorporeres i stabile alkoholiske/vandige medier.It has been found that high amounts of the salt or other powdered material can be suspended in the present alcoholic / aqueous media containing hydroxyethyl cellulose as the suspending agent. Hereby large quantities of particulate material can be incorporated into stable alcoholic / aqueous media.

Det foretrækkes at anvende mikropulveriseret pulver, med en 15 partikelstørrelse på ca. 5 til 100 mikron og fortrinsvis 10 til 25 mikron. Jo mindre partiklerne er, des lettere er det at suspendere dem i bæreren, og det fremkomne produkt giver en ikke-kornet glat fornemmelse ved påføring og udtørring på huden .It is preferred to use microp powdered powder, having a particle size of approx. 5 to 100 microns and preferably 10 to 25 microns. The smaller the particles, the easier it is to suspend them in the carrier, and the resulting product gives a non-grainy smooth feel when applied and dried on the skin.

2020

Selv om pulversuspensioner i det væsentlige ikke har nogen koncentrationsgrænser og kan anvendes med enhver ønsket effektiv mængde, kan mængder op til ca. 50% og så lave som 1% suspenderes .Although powder suspensions have essentially no concentration limits and can be used with any desired effective amount, amounts up to approx. 50% and as low as 1% are suspended.

25 Bæreren, hvori det parti kel formede materiale suspenderes, omfatter et alkoholisk vandigt medium, hvor alkoholen er en monovalent alkohol, som er en lavere alkanol, såsom ethanol, isopropylalkohol eller methanol. Polyvalente alkoholer kan an-30 vendes delvis i stedet for den monovalente alkohol, men overstiger ikke indholdet af monovalent alkohol. Egnede polyvalente alkoholer indbefatter glycerin, propylenglycol, butylengly-col og polyglycoler deraf. Indholdet af hydroxyethylcellulose må overstige opløseligheden af den vandopløselige hydroxyeth-35 ylcellulose i det alkoholiske medium. Opløseligheden af denne vandopløselige polymer i ethanol, er 70 vægt%. Under dette niveau fås en ensartet viskøs væske, der kan hældes jævnt.The carrier in which the particulate material is suspended comprises an alcoholic aqueous medium, the alcohol being a monovalent alcohol which is a lower alkanol such as ethanol, isopropyl alcohol or methanol. Polyhydric alcohols may be used in part instead of the monovalent alcohol but do not exceed the content of monovalent alcohol. Suitable polyhydric alcohols include glycerine, propylene glycol, butylene glycol and polyglycols thereof. The content of hydroxyethyl cellulose must exceed the solubility of the water-soluble hydroxyethyl cellulose in the alcoholic medium. The solubility of this water-soluble polymer in ethanol is 70% by weight. Below this level is obtained a uniform viscous liquid that can be poured evenly.

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Selv om den har et æstetisk tiltalende udseende kan den ikke bære suspenderet pulver, og der vil ske udskillelse. I koncentrationer over opløseligheden danner hydroxyethy1 cel 1ulosen den ønskede slimagtige væsketype. Et 70:30 forhold mellem 5 ethanol og vand er derfor optimalt. Det viste sig imidlertid at dette problem kan elimineres ved tilstrækkelig tilsætning af en polyvalent alkohol, såsom glycerin, propylenglycol, bu-tylenglycol og polyglycoler deraf. Det har derfor vist sig, at den monovalente alkohol udgør ca. 55 til 85%, og vandindholdet 10 kan være så lavt som 5%, hvis der er mindst 10% polyvalent alkohol til stede i suspensionen. Det kombinerede indhold af vand og polyvalent alkohol er mindst ca. 15% og kan være op til ca. 30%, hvorimod vandindholdet som sådan kan være op til ca. 25%. Det er således klart, at mængderne af monovalent 15 alkohol, vand og polyvalent alkohol er indbyrdes afhængig af hinanden.Although it has an aesthetically pleasing appearance, it cannot carry suspended powder and excretion will occur. At concentrations above the solubility, the hydroxyethyl cellulose forms the desired mucous liquid type. A 70:30 ratio of 5 ethanol to water is therefore optimal. However, it was found that this problem can be eliminated by sufficient addition of a polyhydric alcohol such as glycerine, propylene glycol, butylene glycol and polyglycols thereof. It has therefore been found that the monovalent alcohol constitutes approx. 55 to 85% and the water content 10 may be as low as 5% if at least 10% polyhydric alcohol is present in the suspension. The combined content of water and polyhydric alcohol is at least approx. 15% and can be up to approx. 30%, while the water content as such can be up to approx. 25%. Thus, it is clear that the amounts of monovalent alcohol, water and polyhydric alcohol are interdependent.

De slimagtige vandige alkoholiske suspensioner ifølge opfindelsen kan anvendes til fremstilling af faste eller halvfaste 20 produkter på basis af alkohol såsom stifter eller cremer. De har vist sig særlig nyttige til fremstilling af roll-on deodoranter, deodorantstifter, medicinske lotioner, medicinske indgnidningspræparater og andre hurtigttørrende kosmetiske præparater.The mucous aqueous alcoholic suspensions of the invention may be used to prepare solid or semi-solid alcohol-based products such as sticks or creams. They have proven particularly useful in the manufacture of roll-on deodorants, deodorant sticks, medical lotions, medical rubbing preparations and other quick-drying cosmetic preparations.

2525

De har vist særlig anvendelse til fremstilling af hurtigttørrende stabile bicarbonatholdige deodorantprodukter, som kræver ingen eller ringe rystning før brugen. Disse deodorantpræparater under anvendelse af suspensioner af natrium eller kalium-30 bicarbonat har vist sig at være mindre irriterende for huden end bicarbonatopløsninger.They have shown particular use in the preparation of fast-drying stable bicarbonate-containing deodorant products which require no or little shaking before use. These deodorant preparations using suspensions of sodium or potassium bicarbonate have been found to be less irritating to the skin than bicarbonate solutions.

Deodorantproduktet kan også sammensættes som en deodorantstift ved tilsætning af et fedtsyresalt, såsom natriumstearat, som 35 geleringsmiddel. Et natriumsalt af en mættet højere fedtsyre indeholdende 14 til 22 carbonatomer, såsom myristin, palmitin, stearin, osv. har vist sig effektivt som geleringsmiddel vedThe deodorant product may also be formulated as a deodorant pin by the addition of a fatty acid salt such as sodium stearate as a gelling agent. A sodium salt of a saturated higher fatty acid containing 14 to 22 carbon atoms, such as myristin, palmitin, stearin, etc. has been shown to be effective as a gelling agent in

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8 dannelse af en fast stift, hvorimod de lavere fedtsyresalte og de umættede fedtsyresalte ikke virker som geleringsmidler der-i. Den fremkomne stift er en fast slimagtig suspension af deodorant aktive bestanddel i et alkoholisk/vandigt medium.8 to form a solid pin, whereas the lower fatty acid salts and the unsaturated fatty acid salts do not act as gelling agents therein. The resultant pin is a solid mucous suspension of deodorant active ingredient in an alcoholic / aqueous medium.

55

Denne anvendelse som mellemprodukt af den slimagtige suspension forhindrer udskillelse efter varm udhældning i beholdere og muliggør en længere afkølingsperiode til størkning. Dette er særligt fordelagtigt, for ved den sædvanlige størkning af 10 varmesuspensionspræparater er hurtig afkøling, som normalt er ca. 1 til 5 minutter, nødvendig for at undgå udskillelse af suspenderede partikler. Med de foreliggende slimagtige suspensioner udskilles eller udfælder de suspenderede partikler ikke, og der haves længere tid til afkøling, hvilket er at forelå trække, når man skal danne en fast stift.This use as an intermediate of the mucous suspension prevents secretion after hot pouring into containers and allows a longer cooling period to solidify. This is particularly advantageous, because in the usual solidification of 10 heat suspension preparations, rapid cooling, which is usually approx. 1 to 5 minutes, necessary to avoid suspension of suspended particles. With the present slime-like suspensions, the suspended particles are not separated or precipitated and there is longer time for cooling, which is to be done when forming a solid pin.

Suspensionsdeodorantprodukterne kan også indeholde ikke-flyg-tige polære eller ikke-polære bestanddele, for at bevirke aflejring af en tør ikke klæbrig usynlig film på huden ved for-20 dampning, og ikke en hvid bicarbonatrest. Disse ikke-flygtige midler indbefatter polyvalente alkoholer, såsom glycering, propylenglycol, butylenglycol og polyglycoler deraf, og blødgørende olier, såsom hvedekimolie, og eventuelle andre alkoholopløselige olier, herunder isopropylmyristat, isopropyl-25 palmitat, andre fede estere, fede aminer, fede alkoholer, fede ethere, såsom stearylether, ethoxylerede fedtalkoholer og syrer. Den tilstedeværende mængde blødgøringsmiddel er mindre ca. 1 til 5%. Det har også vist sig at tilstedeværelse af mindre mængder lipofile midler, såsom olier, silicon, lecithin og 30 voksarter og/eller vanduopløselige harpikser og polymere i dette deodorantsuspensionsprodukt vil regulere bicarbonatfri-gørelse i armhulen. Det er blevet iagttaget, at en bicarbonat roll-on deodorantsuspension indeholdende hvedekimolier og ste-aryletherolier danner en vandresistent film, når den er tør, 35 hvilket kan forklare den gradvise frigørelse af bicarbonat i armhulen og nedsætte risikoen for hudirritation. Forsøgsresultater har vist at det meste af bicarbonatet frigøres i lø- 9The suspension deodorant products may also contain non-volatile polar or non-polar constituents to effect deposition of a dry non-sticky invisible film on the skin upon evaporation and not a white bicarbonate residue. These non-volatile agents include polyhydric alcohols such as glycation, propylene glycol, butylene glycol and polyglycols thereof, and emollient oils such as wheat germ oil and any other alcohol soluble oils including isopropyl myristate, isopropyl palmitate, other fatty esters, fatty esters, fatty ethers such as stearyl ether, ethoxylated fatty alcohols and acids. The amount of plasticizer present is less approx. 1 to 5%. It has also been found that the presence of smaller amounts of lipophilic agents such as oils, silicone, lecithin and 30 waxes and / or water-insoluble resins and polymers in this deodorant suspension product will regulate bicarbonate release in the armpit. It has been observed that a bicarbonate roll-on deodorant suspension containing wheat germ oils and steryl aryl oils forms a water resistant film when dry, which may explain the gradual release of bicarbonate into the armpit and reduce the risk of skin irritation. Experimental results have shown that most of the bicarbonate is released in solution 9

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bet af 15 minutten med stigende mængder gennem perioder på 1 time og 6% time, hvilket viser en tidsbestemt frigørelsesegenskab af den tørre film. Andre deodorantmidler kan anvendes i stedet for den aktive bicarbonatbestanddel.bet of 15 minutes with increasing volumes through periods of 1 hour and 6% hour, showing a timed release property of the dry film. Other deodorant agents may be used in place of the active bicarbonate component.

55

Foruden de væsentlige komponenter af det foreliggende middel kan man også inkludere mindre mængder af sådanne komponenter som parfumer, farvende midler, midler, der absorberer ultraviolet lys for at fremme farven og lignende, for at forbedre 10 den æstetiske værdi og forbrugernes accept af produktet. Salte- eller pH-stødpudemidl er kan opløses eller suspenderes i det foreliggende alkoholiske/vandige suspensionsprodukt, hvis det ønskes. Mindre mængder af andre bestanddele, der ikke har nogen skadelig virkning på de gavnlige egenskaber af de fore-15 liggende midler, kan også inkluderes.In addition to the essential components of the present agent, minor amounts of such components as perfumes, colorants, ultraviolet light absorbing agents, and the like may be included to enhance the aesthetic value and consumer acceptance of the product. Salts or pH buffers can be dissolved or suspended in the present alcoholic / aqueous suspension product if desired. Smaller amounts of other ingredients which have no detrimental effect on the beneficial properties of the present agents may also be included.

Kendte bakteriostater kan også tilsættes. En bicarbonatsus-pension er dog effektiv som deodorant uden anvendelse af tilsatte bakteriostater.Known bacteriostats may also be added. However, a bicarbonate suspension is effective as a deodorant without the use of added bacteriostats.

2020

Suspensionerne ifølge opfindelsen har fundet anvendelighed i deodorantprodukter til personlig hygiejne, såsom roll-on, dansesko, på substrater, såsom deodorantpuder, fodlotioner og legemslotioner.The suspensions of the invention have found utility in personal hygiene deodorant products such as roll-on, dance shoes, on substrates such as deodorant pads, foot lotions and body lotions.

2525

En anden anvendelse af de foreliggende slimagtige vandige alkoholiske medier er til fremstilling af hurtigttørrende stabile medicinlotioner indeholdende en partikel formet aktiv bestanddel, såsom zinkundecylenat og andet antifungalt/antibak-30 terielt middel, der kan dispenseres via en pumpe eller ved simpel udspredning med fingrene. De samme additiver kan inkluderes i medicinlotionerne som i deodorantprodukterne.Another use of the present mucous aqueous alcoholic media is to prepare fast-drying stable drug lotions containing a particulate active ingredient such as zinc aundecylenate and other antifungal / antibacterial agent which can be dispensed via a pump or by simple spreading of the fingers. The same additives can be included in the drug lotions as in the deodorant products.

Fremgangsmåden til fremstilling af de stabile slimagtige pul-35 versuspensioner ifølge opfindelsen omfatter i almindelighed kombinering af en opvarmet vandig eller vandig/monovalent eller polyvalent alkoholisk blanding indeholdende hydroxyeth-The process for preparing the stable mucous pulse counter-suspensions of the invention generally comprises combining a heated aqueous or aqueous / monovalent or polyhydric alcoholic mixture containing hydroxyethane.

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10 ylcellulose som suspenderingsmiddel med en monovalent alkoholisk dispersion af et partikelformet materiale, såsom et alka-1 imetalbicarbonat eller, zinkundecylenat eller lignende, der kan indeholde et andet suspenderingsmiddel, og blanding ind-5 til der dannes en tyk stabil slimagtig, sej suspension. Specielt fremstilles en klar del 1 bestående af en viskøs opløsning af hydroxyethylcellulose ved opvarmning og blanding med vand, eller en vandholdig blanding af monovalent eller polyvalent alkohol til en temperatur på ca. 54 til 60°C. En del 2, 10 fortrinsvis homogeniseret dispersioh af part i kel formet materiale i en monovalent alkohol med eller uden et suspenderingsmiddel tilsættes under blanding til del 1 til dannelse af en tyk ensartet slimagtig sej suspension, hvori de faste partikler er ensartet suspenderet og forbliver i suspension. Parfu-15 men, de farvende stoffer, blødgøringsmidlerne og andre valgfrie bestanddele kan sættes til den alkoholiske partikelformede dispersion, før den sættes til den vandige/alkoholiske viskøse hydroxyethylcelluloseopløsning eller bagefter. Den endelige suspension homogeniseres fortrinsvis for at bevirke 20 et homogent endeligt tykt slimagtigt suspensionprodukt. Hvis der ønskes en stift, bliver et egnet geleringsmiddel, såsom et natriumsalt af en mættet C14-C22 fedtsyre (f.eks. myristinsy-re, palmi tinsyre, stearinsyre osv.), opløst i del 1, og den endelige slimagtige suspension hældes i stiftbeholdere og får 25 lov at tørre ved stuetemperatur. Slutproduktet er en fast slimatig suspension af pulver i et alkoholisk/vandigt medium indeholdende hydroxyethylcellul ose.10 yl cellulose as a suspending agent with a monovalent alcoholic dispersion of a particulate material such as an alkali-1-metal bicarbonate or, zinc -undecylenate or the like, which may contain another suspending agent, and mixing until a thick stable mucous, tough suspension is formed. Specifically, a clear portion 1 consisting of a viscous solution of hydroxyethyl cellulose is prepared by heating and mixing with water, or an aqueous mixture of monovalent or polyhydric alcohol to a temperature of ca. 54 to 60 ° C. Part 2, 10, preferably homogenized dispersion of part in curd shaped material in a monovalent alcohol with or without a suspending agent is added under mixing to part 1 to form a thick uniform mucosal tough suspension wherein the solid particles are uniformly suspended and remain in suspension. . The perfume, coloring agents, plasticizers and other optional ingredients may be added to the alcoholic particulate dispersion before being added to the aqueous / alcoholic viscous hydroxyethyl cellulose solution or afterwards. The final suspension is preferably homogenized to produce a homogeneously finely thick mucus suspension product. If a pin is desired, a suitable gelling agent, such as a sodium salt of a saturated C14-C22 fatty acid (e.g., myristic acid, palmitic acid, stearic acid, etc.), is dissolved in part 1 and the final mucous suspension is poured into pin containers and allowed to dry at room temperature. The final product is a solid, slimy suspension of powder in an alcoholic / aqueous medium containing hydroxyethyl cellulose.

En anden metode til fremstilling af stabile slimagtige parti-30 kelformede suspensioner består i tilsætning i rækkefølge af bestanddelene til en opvarmet opløsning (ca. 60°C) af vand og alkohol, under omrøring og/eller homogenisering. Mere specielt sættes hydroxyethylcellulosen til den varme vandige/alkoholi-ske opløsning, efterfulgt af den monovalente alkohol og efter-35 fulgt af et andet suspenderingsmiddel, hvis det ønskes, og derpå efterfulgt af det partikel formede materiale, og efterfulgt af parfumen, farven eller andre valgfrie bestanddele.Another method of preparing stable mucosal particulate suspensions consists in adding, in succession, the ingredients to a heated solution (about 60 ° C) of water and alcohol, with stirring and / or homogenization. More particularly, the hydroxyethyl cellulose is added to the hot aqueous / alcoholic solution, followed by the monovalent alcohol and followed by another suspending agent, if desired, and then the particulate material, followed by the perfume, the color or other optional ingredients.

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1111

Denne metode giver en tyndere suspension end når man anvender den førnævnte metode med 2 dele. Begge metoder kræver imidlertid først fremstilling af en viskøs vandig hydroxyethylcel1u-loseopløsning før tilsætning af endelige mængder monovalent 5 alkohol. Rækkefølgen af tilsætningen og fremstillingsmetoderne er derfor vigtige for at opnå den ønskede slimagtige suspension .This method gives a thinner suspension than when using the aforementioned two-part method. However, both methods first require the preparation of a viscous aqueous hydroxyethyl cellulose solution before adding final amounts of monovalent alcohol. The order of addition and preparation methods are therefore important to obtain the desired mucous suspension.

De følgende konkrete eksempler illustrerer nærmere opfindel-10 sen. Alle mængde af forskellige bestanddele er efter vægt, med mindre andet er anført.The following concrete examples further illustrate the invention. All amounts of various components are by weight, unless otherwise stated.

EKSEMPEL 1-4 15EXAMPLES 1-4

Del 1 12 2 åPart 1 12 2 å

Afioniseret vand 15,00 15,00 5,00 15,00Deionized water 15.00 15.00 5.00 15.00

Propylenglycol - 10,00 10,00 SD 40 Ethanol 10,00 - - 15,00 20 Natrosol 250 HR(1) 0,40 0,40 0,40 0,40Propylene Glycol - 10.00 10.00 SD 40 Ethanol 10.00 - 15.00 Natrosol 250 HR (1) 0.40 0.40 0.40 0.40

Del 2 12 3 4 SD 40 Ethanol 63,15 60,65 70,65 56,10Part 2 12 3 4 SD 40 Ethanol 63.15 60.65 70.65 56.10

Cab-O-Sil(2) 0,50 0,50 0,50 0,50 25 Natriuiribicarbonat 10,00 10,00 10,00 5,00 (Mikropulveriseret)Cab-O-Sil (2) 0.50 0.50 0.50 0.50 Sodium Ribicarbonate 10.00 10.00 10.00 5.00 (Micropulverized)

Zinkrincinoleat ~ " 5,00Zinc rincinoleate ~ "5.00

Del 3 1 2 2 2 30 „ ΛPart 3 1 2 2 2 30 "Λ

Parfume 0,50 0,50 0,50 0,50 FD & C Green No. 3 0,30 0,30 0,30 (0,1%) 35Perfume 0.50 0.50 0.50 0.50 FD&C Green No. 0.30 0.30 (0.1%) 35

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Del 3 (fortsat) .1 2^ 3 4 D & C Green No. 8 0/10 0,15 0,15 (2,75%)Part 3 (continued) .1 2 ^ 3 4 D&C Green No. 0.15 0.15 (2.75%)

Arlamol El 1 - 1,50 1,50 1,50 (4)Arlamol E1 - 1.50 1.50 1.50 (4)

Wickenol 535v - 1,00 1,00 1,00 100,00 100,00 100,00 5 pH 1% vandig opløsning 8,45 -Wickenol 535v - 1.00 1.00 1.00 100.00 100.00 100.00 5 pH 1% aqueous solution 8.45 -

Udseende Tyk, Tyk, Tyk, Lotion viskos viskos viskos konsistens •slimagtig slimagtig slimagtig slimagtig suspension suspension suspension suspensionAppearance Thick, Thick, Thick, Lotion viscous viscous viscous consistency • slimy slimy slimy slimy suspension suspension suspension suspension

Eksempel 1 tørrer hurtigt til et jævnt tørt ikke-klæbrigt hvidt pulver på huden.Example 1 quickly dries to an even dry non-sticky white powder on the skin.

Eksempel 2, 3 og 4 tørrer til en jævn tør ikke-klæbrig 10 usynlig film på huden.Examples 2, 3 and 4 dry to an even dry non-sticky 10 invisible film on the skin.

Ingen eksempler viser nogen udskillelse af bicarbonat eller væske ved henstand, og ingen kræver rystning før brugen, og ingen er irriterende for huden.No examples show any excretion of bicarbonate or liquid upon standing, and no one requires shaking before use and none is irritating to the skin.

Ældningsforsøg gennem en periode på 2 uger ved stuetemperatur, 15 4°C og 43°C vister ingen udskillelse af bicarbonat.Aging experiments over a period of 2 weeks at room temperature, 15 4 ° C and 43 ° C show no excretion of bicarbonate.

Fremstilling af eksempler.Preparation of Examples.

Trin 1.Step 1.

Del 1 (alle eksempler): disperger natrosol i enten ethanol eller propylenglycol. Tilsæt vand under konstant blanding 20 og opvarm til 54-60°C indtil der dannes en ensartet klar viskøs opløsning.Part 1 (all examples): disperses natrosol in either ethanol or propylene glycol. Add water under constant mixture 20 and heat to 54-60 ° C until a uniform clear viscous solution is formed.

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Trin 2.Step 2.

Del 2 (eksempel 1-3): disperger Cab-O-Sil i alkohol og tilsæt natriumbicarbonat gradvis under hurtig blanding.Part 2 (Examples 1-3): Disperse Cab-O-Sil in alcohol and gradually add sodium bicarbonate with rapid mixing.

Homogeniser til ensartethed.Homogenize to uniformity.

5 (Eksempel 4) opløs zinkricinoleat i varm ethanol. Tilsæt natriumbicarbonat og Cab-O-Sil og bland. Homogeniser til ensartethed.5 (Example 4) dissolve zinc castinoleate in hot ethanol. Add sodium bicarbonate and Cab-O-Sil and mix. Homogenize to uniformity.

Trin 3.Step 3.

Tilsæt del 2 til del 1 under blanding (der dannes en tyk 10 slimagtig ' sej suspension) .Add part 2 to part 1 while mixing (forming a thick 10 slimy 'tough suspension').

Trin 4.Step 4.

Del 3· bland alle bestanddele med del 1 og 2. Homogeniser blandingen til en tyk ensartet slimagtig suspension.Part 3 · Mix all ingredients with Parts 1 and 2. Homogenize the mixture to a thick uniform mucous suspension.

^ Natrosol 250 HR: Hercules Inc., Hydroxyethylcellulose.^ Natrosol 250 HR: Hercules Inc., Hydroxyethyl Cellulose.

(2) 15 Cab-O-Sil: Cabot Corporation, findelt siliciumdioxid.(2) Cab-O-Sil: Cabot Corporation, finely divided silica.

(3)(3)

Arlamol E: I.C.I. American Inc., Polyoxypropylenstearyl= ether.Arlamol E: I.C.I. American Inc., Polyoxypropylene Stearyl = Ether.

(4)(4)

Wickenol 535: Wickhen Products Inc., Hvedekimglycerider. EKSEMPEL 5 20 Bestanddel %Wickenol 535: Wickhen Products Inc., Wheat germ glycerides. EXAMPLE 5 Component%

Propylenglycol 10,0Propylene glycol 10.0

Bentone LT (1) 0,5Bentone LT (1) 0.5

Afioniseret vand 15,0Deionized water 15.0

Natriumbicarbonat Mikropulveriseret 10,0 25 SD 40 Ethanol 64,5 100,0 14Sodium bicarbonate Microp powder 10.0 25 SD 40 Ethanol 64.5 100.0 14

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Dette eksempel danner også en god ensartet slimagtig suspension, idet bentone LT er en kombination af hydroxyethyl= cellulose og bentonitler. Dette eksempel viser specificiteten af dette særlige suspenderingsmiddel til dannelse af en 5 stabil slimagtig viskos suspension i overensstemmelse med den foreliggende opfindelse.This example also forms a good uniform mucus suspension, with bentone LT being a combination of hydroxyethyl cellulose and bentonite clays. This example shows the specificity of this particular suspending agent to form a stable mucous viscous suspension in accordance with the present invention.

Fremstilling af eksempel 5 1. Disperger bentone LT i propylenglycol.Preparation of Example 5 1. Disperses bentone LT in propylene glycol.

2. Tilsæt vand og opvarm til 54-60°C, indtil blandingen 10 er ensartet viskos.2. Add water and heat to 54-60 ° C until mixture 10 is uniformly viscous.

3. Tilsæt natriumbicarbonat, og bland kontinuerligt.3. Add sodium bicarbonate and mix continuously.

4. Tilsæt alkohol, bland fuldstændigt indtil ensartethed og homogeniser.4. Add alcohol, mix completely until uniform and homogenize.

^Bentone LT: NL Industries Gellant er et organoler ma- 15 teriale beregnet til lavmolekylære systemer af polært opløsningsmiddel/vand, og 100% vandsystemer. Det er en kombination af hydroxyethylcellulose og bentonitler.^ Bentone LT: NL Industries Gellant is an organols material designed for low molecular weight systems of polar solvent / water, and 100% water systems. It is a combination of hydroxyethyl cellulose and bentonite clay.

EKSEMPEL 6EXAMPLE 6

Eksempel 2 gentages med undtagelse af at stearyletheren og 20 hvedekimglyceriderne udelades og ethanolindholdet forøges til 63,15%. Dette produkt giver en stabil ensartet slimagtig suspension med høj viskositet, hvoraf bicarbonatpartiklerne ikke udskiller sig ved henstand men forbliver i suspension. Når dette produkt anvendes i en roll-on beholder med en 25 kugle på 2,5 cm, giver det god udlevering og hurtig tørring til dannelse af en usynlig film på huden.Example 2 is repeated except that the stearyl ether and wheat germ glycerides are omitted and the ethanol content is increased to 63.15%. This product provides a stable uniform mucus suspension with high viscosity, of which the bicarbonate particles do not secrete upon standing but remain in suspension. When used in a 2.5 cm roll-on container, this product provides good dispensing and quick drying to form an invisible film on the skin.

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15 EKSEMPEL 7 og 8.EXAMPLES 7 and 8.

7 878

Roll-on deodorant Medicinsk indgnidn±ngs~— præparatRoll-on deodorant Medical rub ± ngs ~ - preparation

Del_1 --Part 1 --

Vand 15,00 17,0 5 Propylenglycol 10,00 10,0Water 15.00 17.0 5 Propylene Glycol 10.00 10.0

Natrosol 250 HR (1) 0,40 0,4Natrosol 250 HR (1) 0.40 0.4

Del 2 SD 40 Ethanol 60,40 64,3Part 2 SD 40 Ethanol 60.40 64.3

Cab-O-Sil (2) 0,50 0,5 3_0 Natriumbicarbonat 10,00 (Mikropulveriseret)Cab-O-Sil (2) 0.50 0.5 3_0 Sodium Bicarbonate 10.00 (Microp Powdered)

Zinkundecylenat - 5,0Zincundecylenate - 5.0

Del 3Part 3

Hvedekimglycerider 1,00 1,0 15 Arlamol E (3) 1,50 1,5Wheat germ glycerides 1.00 1.0 15 Arlamol E (3) 1.50 1.5

Parfume 0,50 0,3Perfume 0.50 0.3

Farveopløsning 0,65Color solution 0.65

Uvinul D-50 (5) 0,05 100,00 100,00 (5)Uvinul D-50 (5) 0.05 100.00 100.00 (5)

Absorptionsmiddel for ultraviolet lys, 2,4-dehydroxybenzo= 20 phenon: GAF Corporation.Absorbent for ultraviolet light, 2,4-dehydroxybenzo = phenone: GAF Corporation.

Fremgangsmåde.Course of action.

Del_1Part 1

Kombiner vand og propylenglycol og tilsæt natrosol gradvis under blanding. Opvarm til 60°C, til dannelse af en 25 ensartet viskes blanding.Combine water and propylene glycol and gradually add natrosol while mixing. Heat to 60 ° C to form a uniformly wiped mixture.

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Del 2Part 2

Homogeniser Cab-O-Sil og derefter bicarbonat eller zink= undecylenat i ethanol. Tilsæt del 2 gradvis til dell under blanding.Homogenize Cab-O-Sil and then bicarbonate or zinc = undecylenate in ethanol. Gradually add part 2 to dell while mixing.

5 Del 35 Part 3

Tilsæt under blanding del 3 bestanddelene til del 1 og 2, og homogeniser derefter hele blandingen.While mixing, add part 3 ingredients to parts 1 and 2, then homogenize the entire mixture.

Resultater.Results.

Begge produkter danner en sej slimagtig hvid uigennemsigtig 10 væske med udmærkede suspenderingsegenskaber. Der iagttages ingen kendelig udskillelse af natriumbicarbonat i eksempel 7 efter 13 ugers lagring indenfor et bredt temperaturinter- val.Both products form a cool slimy white opaque 10 liquid with excellent suspending properties. No appreciable excretion of sodium bicarbonate in Example 7 is observed after 13 weeks of storage within a wide temperature range.

EKSEMPEL_7 15 Stabilitet ved forskellige temperaturer (urystet)EXAMPLE_7 Stability at various temperatures (unshaken)

Temperaturbetingelser -18°C 4°C Stuetemp. 35°C 43°C 49°CTemperature conditions -18 ° C 4 ° C Room temperature. 35 ° C 43 ° C 49 ° C

% NaHC03 10,6 10,5 10,6 10,6 10,3 10,1% NaHCO3 10.6 10.5 10.6 10.6 10.3 10.1

Analyseret (øverste 0,6 cm af vasken) 20 Rystet kontrol ved stuetemperatur = 10,7.Analyzed (upper 0.6 cm of the sink) 20 Shaken control at room temperature = 10.7.

De følgende eksempler illustrerer virkningen af vandmængderne på dannelsen og stabiliteten af de ønskede suspensioner og fordelen ved, at tilsætte en polyvalent alkohol til præparater med lav fugtighed.The following examples illustrate the effect of the amounts of water on the formation and stability of the desired suspensions and the advantage of adding a polyhydric alcohol to low moisture preparations.

1717

DK 159812 BDK 159812 B

EKSEMPEL 9-14EXAMPLES 9-14

Eksempel 9 1£ 11 12 13 14Example 9 1 £ 11 12 13 14

Del 1. % % % % % %Part 1. % % % % % %

Vand 37,7 25,0 15,0 15,0 5,0 15,0Water 37.7 25.0 15.0 15.0 5.0 15.0

Propylengly- col 10,0 - - 10,0 20,0Propylene glycol 10.0 - - 10.0 20.0

Glycerin - - - - - 10,0Glycerin - - - - - 10.0

Natrosol 0,4 0,4 0,4 0,4 0,4 0,4Natrosol 0.4 0.4 0.4 0.4 0.4 0.4 0.4

Del 2.Part 2.

SD 40 Ethanol 37,7 64,4 74,6 64,6 60,4 64,6SD 40 Ethanol 37.7 64.4 74.6 64.6 60.4 64.6

Cab-O-Sil 0,5- - - 0,5Cab-O-Sil 0.5- - - 0.5

Natriumbi- carbonat 10,0 10,0 10,0 10,0 10,0 10,0 (Mikropulveriseret)Sodium bicarbonate 10.0 10.0 10.0 10.0 10.0 10.0 (Microp Powdered)

Del 3.Part 3.

Består af olier, parfume 3,7- - - 3,7-Consists of oils, perfume 3.7- - - 3.7-

Farve, UVColor, UV

absorptions- - 0,2- middel _ _ _ _ _ _ 100,0 100,0 100,0 100,0 100,0 100,0absorbent 0.2 agent _ _ _ _ _ _ 100.0 100.0 100.0 100.0 100.0 100.0

Eksempel i) 1£ 1]. 12_ 1_3 14Example i) 1 £ 1]. 12_ 1_3 14

Udseende: ens- siim- ikke- slim- slim- ' slim- artet agtig homo- agtig agtig agtig viskes genAppearance: single-non-slimy-slimy-slimy-like gay-like

Stabilitet: sepa- stabil sepa- stabil stabil stabil rerede ration ved henstandStability: sepa- stable sepa- stable stable stabilized ration at standstill

DK 159812 BDK 159812 B

1.8 'i 10 U 12 13 141.8 'i 10 U 12 13 14

Bemærkninger: over- vand- util- tilfreds- Tilfreds- tilfredsskud af maaigde stra&- stillende stillende stillende vand omtrent keligt propylen- propylen- propylen- rigtig vand glyoolkam- glycolkcm-glycolkom- til lidt pensation pensation pensation.Notes: over-water-unsatisfied Satisfied satisfaction of high-stressed-posing pos- sible still water approxi- mately propylene-propylene- propylene-rich water glyoolcamoglycolccm-glycolcom- to a little retirement pension retirement.

overskudsurplus

Fremgangsmåde:Course of action:

Lignende fremgangsmåder, som anvendt i eksempel 7 og 8, undtagen for sammensætning 13. Halvdelen af mængden af pro= 5 pylenglycol kombineres med vand, der tilsættes natrosol, og blandingen opvarmes til 60°C und blandning, indtil den er ensartet tyk. Resten af propylenglycolen tilsættes og blandes før tilsætning af del 2.Similar procedures, as used in Examples 7 and 8, except for composition 13. Half of the amount of propylene glycol is combined with water added to natrosol, and the mixture is heated to 60 ° C and mixed until uniformly thick. The rest of the propylene glycol is added and mixed before adding part 2.

Stabilitet efter 5 uger (stuetemperatur, urystet).Stability after 5 weeks (room temperature, unshaken).

10 Eksempel 10 12 13 14 %NaHC03 10,3 10,6 10,5 10,1Example 10 12 13 14% NaHCO 3 10.3 10.6 10.5 10.1

Analyseret (øverste 0,6 cm af væske) EKSEMPEL 15 15 Medicinsk lotion til indgnidning.Analyzed (upper 0.6 cm of fluid) Example 15 15 Medical lotion for rubbing.

Del 1 %Part 1 %

Afioniseret vand 24,0Deionized water 24.0

Hydroxyethylcellulose 0,4Hydroxyethyl cellulose 0.4

Isopropanol 15,0 20 Del 2Isopropanol 15.0 Part 2

Isopropanol 53,1Isopropanol 53.1

Cab-O-Sil 0,5 19Cab-O-Sil 0.5 19

DK 159812 BDK 159812 B

Del 2 (fortsat) Z inkundecylenat 5,0Part 2 (continued) Z incundecylenate 5.0

Parfume 0,5Perfume 0.5

Zinkstearat 1,5Zinc stearate 1.5

Fremgangsmåde; 5 Del li Disperger hydroxyethylcellulosen i alkohol, tilsæt vand og opvarm blandingen under omrøring til 60°C.Course of action; Part I Dispersate the hydroxyethyl cellulose in alcohol, add water and heat the mixture with stirring to 60 ° C.

Del 2: Sæt Cab-O-Sil til alkohol og bland godt. Tilsæt zinkundecylenat og bland dispersionen godt. Tilsæt zinkstearat og parfume og bland. Bland del 1 og 2.Part 2: Add Cab-O-Sil to alcohol and mix well. Add zinc cecylenate and mix the dispersion well. Add zinc stearate and perfume and mix. Mix parts 1 and 2.

10 Der dannes en tyk slimagtig gel af cremekonsistens.10 A thick, slimy gel of cream texture is formed.

Efter påføring på huden udviser den en meget glat fornemmelse og er rimeligt vandskydende under vand.After application to the skin, it has a very smooth feel and is reasonably water-resistant under water.

EKSEMPEL 16EXAMPLE 16

Eksempel 8 gentages med undtagelse af, at vandindholdet 15 nedsættet til 14% og ethanolindholdet forøges til 67,3%.Example 8 is repeated except that the water content is reduced to 14% and the ethanol content is increased to 67.3%.

Det fremkomne produkt er en god suspension med en sej konsistens .The resulting product is a good suspension with a cool consistency.

EKSEMPEL 17EXAMPLE 17

Deodorantstift.Deodorant diocese.

20 —L·. i20 — L ·. in

Afioniseret vand 5,0Deionized water 5.0

Propylenglycol (del 1) 10,0Propylene Glycol (Part 1) 10.0

Hydroxyethylcellulose 0,4Hydroxyethyl cellulose 0.4

Propylenglycol (del 2) 15,0 25 Natriumstearat 6,0 20Propylene Glycol (Part 2) 15.0 Sodium Stearate 6.0 20

DK 159812 BDK 159812 B

Del 2. %Part 2. %

Vandfri ethanol 53,1Anhydrous ethanol 53.1

Cab-O-Sil 0,5Cab-O-Sil 0.5

Mikropulveriseret NaHCO^ 10,0 5 Del 1: Bland vandet og del 1 propylenglycol og tilsæt hydroxyethylcellulose. Opvarm blandingen til 60-66°C indtil der er dannet en viskøs gel. Del 2 propylenglycol tilsættes og blandes godt til dannelse af en homogen tyk gelopløsning. Natrium-10 stearat tilsættes og blandingen opvarmes til 66- 71°C indtil natriumstearatet er fuldstændigt opløst.Micropulverized NaHCO® 10.0 5 Part 1: Mix the water and part 1 propylene glycol and add hydroxyethyl cellulose. Heat the mixture to 60-66 ° C until a viscous gel is formed. Part 2 propylene glycol is added and mixed well to form a homogeneous thick gel solution. Sodium 10 stearate is added and the mixture is heated to 66-71 ° C until the sodium stearate is completely dissolved.

Del 2: Cab-O-Sil dispergeres i ethanol og natriumbicar= bonat tilsættes og blandes indtil det er ensartet dispergeret og suspenderet. Blandingen opvarmes 15 til ca. 57°C.Part 2: Cab-O-Sil is dispersed in ethanol and sodium bicarbonate is added and mixed until uniformly dispersed and suspended. The mixture is heated to 15 to approx. 57 ° C.

Del 2 sættes til del 1 under blanding til dannelse af en viskos slimagtig suspension, som hældes i stiftbeholdere og får lov at afkøle til stuetemperatur. Der sker ingen synlig adskillelse. Der 2q fås en udmærket suspension i stiftform, som er glat ved påføring og ikke klæbrig.Part 2 is added to part 1 under mixing to form a viscous mucous suspension which is poured into pin containers and allowed to cool to room temperature. There is no visible separation. An excellent suspension in pin 2q is obtained which is smooth on application and non-sticky.

Andre polyvalente alkoholer kan anvendes i stedet for pro= pylenglycol eller glycerin helt eller delvist i ovenstående eksempler, såsom butylenglycol, polypropylenglycol, osv.Other polyhydric alcohols may be used in place of propylene glycol or glycerine in whole or in part in the above examples, such as butylene glycol, polypropylene glycol, etc.

25 På lignende måde kan ethanol og isopropanol erstattes med methanol. Ligeledes kan andet partikelformet materiale anvendes i stedt for natriumbicarbonat og zinkundecylenat, såsom kaliumbicarbonat, uorganiske eller organiske salte eller andre alkohol-uopløselige pulvere.Similarly, ethanol and isopropanol can be replaced with methanol. Likewise, other particulate material may be used in place of sodium bicarbonate and zinc ounceylate, such as potassium bicarbonate, inorganic or organic salts or other alcohol-insoluble powders.

Claims (9)

1. Hurt igttørrende, stabil slimagtig pulversuspension af findelte faste partikler, der er ensartet suspenderet i en bærer omfattende et højt alkoholindhold af en lavere alifatisk mo- 10 novalent alkohol og et lavt vandindhold, og hydroxyethylcel1u- lose som suspenderingsmiddel, kendetegnet ved, at mængden af hydroxyethylcellulose overstiger opløseligheden for den vandopløselige hydroxyethylcellulose i alkoholen, og vandindholdet er tilstrækkeligt til at forhindre udfældning af suspenderingsmidlet og mindst 5 vægt%A rapidly drying, stable mucous powder suspension of finely divided solid particles uniformly suspended in a carrier comprising a high alcohol content of a lower aliphatic monovalent alcohol and a low water content, and hydroxyethyl cellulose as the suspending agent, characterized in that the amount of hydroxyethyl cellulose exceeds the solubility of the water-soluble hydroxyethyl cellulose in the alcohol and the water content is sufficient to prevent precipitation of the suspending agent and at least 5% by weight 2. Suspension ifølge krav 1, kendetegnet ved, at det suspenderede pulver består af alkalimetalbicarbonatpartik-ler og udgør 0,1-20 vægt/vægt%.Suspension according to claim 1, characterized in that the suspended powder consists of alkali metal bicarbonate particles and is 0.1-20 w / w%. 3. Suspension ifølge krav 1, kendetegnet ved, at 2q det suspenderede pulver består af zinundecylat.Suspension according to claim 1, characterized in that 2q of the suspended powder consists of zinundecylate. 4. Suspension ifølge krav 1, kendetegnet ved, at den indeholder en polyvalent alkohol i en mængde, der ikke overstiger indholdet af monovalent alkohol og er tilstrækkelig til at forhindre udfældning af suspenderingsmidlet.Suspension according to claim 1, characterized in that it contains a polyhydric alcohol in an amount which does not exceed the content of monovalent alcohol and is sufficient to prevent precipitation of the suspending agent. 5. Anvendelse af suspensionen ifølge krav 1 til fremstilling af en fast suspension. DK 159812BUse of the suspension according to claim 1 for the preparation of a solid suspension. DK 159812B 6. Anvendelse ifølge krav 5, kendetegnet ved, at et natriumsalt af en mættet C14-C22 fedtsyre som geleringsmiddel opløses i den opvarmede hydroxyethylcelluloseopløsning før 5 blanding med den alkoholiske dispersion af det pulveriserede materiale, og den slimagtige suspension hældes i stiftbeholdere og får lov at afkøle til stuetemperatur.Use according to claim 5, characterized in that a sodium salt of a saturated C14-C22 fatty acid as a gelling agent is dissolved in the heated hydroxyethyl cellulose solution before mixing with the alcoholic dispersion of the powdered material and the slime-like suspension is poured into pin containers and allowed to cool to room temperature. 7. Anvendelse af suspensionen ifølge krav 1 til fremstilling 10 af en viskøs lotion.Use of the suspension according to claim 1 for the preparation of a viscous lotion. 8. Fremgangsmåde til fremstilling af suspensionen ifølge krav 1, kendetegnet ved, at der først fremstilles en viskøs vandholdig hydroxyethylcelluloseopløsning før tilsætnin- 15 gen af den monovalente alkohol og det pulveriserede materiale.Process for preparing the suspension according to claim 1, characterized in that a viscous aqueous hydroxyethyl cellulose solution is first prepared before the addition of the monovalent alcohol and the powdered material. 9. Fremgangsmåde til fremstilling af den slimagtige suspension ifølge krav 1, kendetegnet ved, at der fremstilles en klar viskøs vandig eller vandig alkoholisk opløsning af hy- 20 droxyethylcellulose opvarmet til en temperatur på ca. 54-60°C, og denne opvarmede viskøse opløsning blandes med en monovalent alkoholdispersion af det pulveriserede materiale, indtil der dannes en viskøs slimagtig suspension med de pulveriserede partikler ensartet suspenderet deri. 25 30 35Process for the preparation of the mucous suspension according to claim 1, characterized in that a clear viscous aqueous or aqueous alcoholic solution of hydroxyethyl cellulose heated to a temperature of approx. 54-60 ° C, and this heated viscous solution is mixed with a monovalent alcohol dispersion of the powdered material until a viscous mucous suspension is formed with the powdered particles uniformly suspended therein. 25 30 35
DK578881A 1980-12-29 1981-12-28 QUICK-DRY, STABLE, SLIM POWDER SUSPENSION, ITS APPLICATION AND PROCEDURE FOR ITS PREPARATION DK159812C (en)

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ZA829387B (en) * 1981-12-30 1984-08-29 Colgate Palmolive Co Liquid deodorant
DE3376957D1 (en) * 1982-06-24 1988-07-14 Robert Alan Smith Pharmaceutical gel composition
IT1231410B (en) * 1987-09-22 1991-12-04 Cooperativa Farmaceutica ANTI-INFLAMMATORY PHARMACEUTICAL COMPOSITION WITH PROLONGED EFFECT FOR TOPICAL USE
GB2233227A (en) * 1989-06-09 1991-01-09 Paul Eldred Buckenham Zinc compositions for treatment of foot odour
GB9122674D0 (en) * 1991-10-25 1991-12-11 Boots Co Plc Toiletries composition
GB9406554D0 (en) * 1994-03-31 1994-05-25 Unilever Plc Deodorant compositions
JP4115670B2 (en) * 1999-03-02 2008-07-09 クエスト インターナショナル サービスズ ベーフェー Fragrance composition containing odor neutralizer
WO2000051560A1 (en) 1999-03-02 2000-09-08 Shaw Mudge & Company Fragrance and flavor compositions containing odor neutralizing agents
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