CA1272641A - Pad fragrance sampling device - Google Patents

Pad fragrance sampling device

Info

Publication number
CA1272641A
CA1272641A CA000495734A CA495734A CA1272641A CA 1272641 A CA1272641 A CA 1272641A CA 000495734 A CA000495734 A CA 000495734A CA 495734 A CA495734 A CA 495734A CA 1272641 A CA1272641 A CA 1272641A
Authority
CA
Canada
Prior art keywords
sheets
microcapsules
adhesive composition
adhesive
liquid
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
CA000495734A
Other languages
French (fr)
Inventor
Jack W. Charbonneau
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
3M Co
Original Assignee
Minnesota Mining and Manufacturing Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Minnesota Mining and Manufacturing Co filed Critical Minnesota Mining and Manufacturing Co
Application granted granted Critical
Publication of CA1272641A publication Critical patent/CA1272641A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

Links

Classifications

    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61QSPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q13/00Formulations or additives for perfume preparations
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B32LAYERED PRODUCTS
    • B32BLAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B5/00Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts
    • B32B5/16Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by features of a layer formed of particles, e.g. chips, powder or granules
    • AHUMAN NECESSITIES
    • A45HAND OR TRAVELLING ARTICLES
    • A45DHAIRDRESSING OR SHAVING EQUIPMENT; EQUIPMENT FOR COSMETICS OR COSMETIC TREATMENTS, e.g. FOR MANICURING OR PEDICURING
    • A45D40/00Casings or accessories specially adapted for storing or handling solid or pasty toiletry or cosmetic substances, e.g. shaving soaps or lipsticks
    • A45D40/0087Casings or accessories specially adapted for storing or handling solid or pasty toiletry or cosmetic substances, e.g. shaving soaps or lipsticks for samples
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/0208Tissues; Wipes; Patches
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/02Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/11Encapsulated compositions
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61LMETHODS OR APPARATUS FOR STERILISING MATERIALS OR OBJECTS IN GENERAL; DISINFECTION, STERILISATION OR DEODORISATION OF AIR; CHEMICAL ASPECTS OF BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES; MATERIALS FOR BANDAGES, DRESSINGS, ABSORBENT PADS OR SURGICAL ARTICLES
    • A61L9/00Disinfection, sterilisation or deodorisation of air
    • A61L9/015Disinfection, sterilisation or deodorisation of air using gaseous or vaporous substances, e.g. ozone
    • A61L9/04Disinfection, sterilisation or deodorisation of air using gaseous or vaporous substances, e.g. ozone using substances evaporated in the air without heating
    • A61L9/12Apparatus, e.g. holders, therefor
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61MDEVICES FOR INTRODUCING MEDIA INTO, OR ONTO, THE BODY; DEVICES FOR TRANSDUCING BODY MEDIA OR FOR TAKING MEDIA FROM THE BODY; DEVICES FOR PRODUCING OR ENDING SLEEP OR STUPOR
    • A61M35/00Devices for applying media, e.g. remedies, on the human body
    • A61M35/003Portable hand-held applicators having means for dispensing or spreading integral media
    • A61M35/006Portable hand-held applicators having means for dispensing or spreading integral media using sponges, foams, absorbent pads or swabs as spreading means
    • AHUMAN NECESSITIES
    • A45HAND OR TRAVELLING ARTICLES
    • A45DHAIRDRESSING OR SHAVING EQUIPMENT; EQUIPMENT FOR COSMETICS OR COSMETIC TREATMENTS, e.g. FOR MANICURING OR PEDICURING
    • A45D2200/00Details not otherwise provided for in A45D
    • A45D2200/10Details of applicators
    • A45D2200/1009Applicators comprising a pad, tissue, sponge, or the like
    • A45D2200/1018Applicators comprising a pad, tissue, sponge, or the like comprising a pad, i.e. a cushion-like mass of soft material, with or without gripping means
    • AHUMAN NECESSITIES
    • A45HAND OR TRAVELLING ARTICLES
    • A45DHAIRDRESSING OR SHAVING EQUIPMENT; EQUIPMENT FOR COSMETICS OR COSMETIC TREATMENTS, e.g. FOR MANICURING OR PEDICURING
    • A45D2200/00Details not otherwise provided for in A45D
    • A45D2200/10Details of applicators
    • A45D2200/1009Applicators comprising a pad, tissue, sponge, or the like
    • A45D2200/1036Applicators comprising a pad, tissue, sponge, or the like containing a cosmetic substance, e.g. impregnated with liquid or containing a soluble solid substance
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/41Particular ingredients further characterized by their size
    • A61K2800/412Microsized, i.e. having sizes between 0.1 and 100 microns
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10STECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S428/00Stock material or miscellaneous articles
    • Y10S428/905Odor releasing material
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/15Sheet, web, or layer weakened to permit separation through thickness
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/249921Web or sheet containing structurally defined element or component
    • Y10T428/249994Composite having a component wherein a constituent is liquid or is contained within preformed walls [e.g., impregnant-filled, previously void containing component, etc.]
    • Y10T428/249995Constituent is in liquid form
    • Y10T428/249997Encapsulated liquid
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/25Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/25Web or sheet containing structurally defined element or component and including a second component containing structurally defined particles
    • Y10T428/254Polymeric or resinous material
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2984Microcapsule with fluid core [includes liposome]
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2984Microcapsule with fluid core [includes liposome]
    • Y10T428/2985Solid-walled microcapsule from synthetic polymer
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2984Microcapsule with fluid core [includes liposome]
    • Y10T428/2985Solid-walled microcapsule from synthetic polymer
    • Y10T428/2987Addition polymer from unsaturated monomers only
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10TTECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION
    • Y10T428/00Stock material or miscellaneous articles
    • Y10T428/29Coated or structually defined flake, particle, cell, strand, strand portion, rod, filament, macroscopic fiber or mass thereof
    • Y10T428/2982Particulate matter [e.g., sphere, flake, etc.]
    • Y10T428/2989Microcapsule with solid core [includes liposome]

Abstract

Abstract of the Disclosure Microencapsulated materials are released by removing individual elements from a pad of sheets bonded by adhesive layers containing capsules.

Description

1~7~i4~

P~l) L~ AN(I SAMPLING DF.VICE

Fielcl of the Invention This invention relates to microencapsulated materials, art;cles contairlin~ microencapsulated materials and the method o~ l)re~aring snch articles. In particular, the present invention rel.ate.s to multi-element pad samples of microencap.sulate(i materials adhe.sively secured in a stacked array o- temporarily adllered element.s .such that upon breaking o[ the a(llle.siorl of the element.s an(3 separation of said element.s, the capsule.s rupture, releasing or making available for application the material contained tllerein.

Background of the Invention ~.ncap.sulated materials have been used for many years in a wide variety of commercial applications. Early uses of encapsulated materials included paper coated with capsules bearing coloring material therein which could be used as a recording medium. I).S. Patent No. 3,016,303 discloses one of the early efforts using encapsulated material as the ima(3e source on recording paper. U.S.
Patent Nos. 4,05~,~3~ and 4,~01,404 show other methods of application of encap.sulated coloring materials on paper substrates to be used as imaging media and the like. U.S.
Patent No. 3,503,7~3 shows microcapsules having coloring material therein which are ruptureable by the application of heat, pre~sure anc3/or radiation because of a metal coating on tlle .surface of the capsule. These ruptureable microcapsules, in one embodiment, may be secured between a substrate and a photocon(3uctive top coat to enable photosensitive i.maging of the system.
A wide variety of processes exist by WlliCh micro-capsules can be manufacture(3. These varied processes provide different techni~ues for producing capsules of varying sizes, alternative materials for the composition of the capsule shell and various differellt functional 1'~7i~

materials within til~ shell. Some of these various processe~s are shown in l).S Pltent Nos. 3,516,~46; 3,516,941; and British Patent Specificatioll Nos. 1,15~,725; 2,041,319 and
2,048,206. ~ wide variety of differerlt materials may also be used in makirly til~ ca~)sule shells. ~ popular material for shell form~tion is the polymeri7ation reaction product between urea an(l forma~dellyde or melamine and Lormaldehyde, or the polycorldensatiorl products of monomeric or low rnolecular weight polymers of dimethylolurea or rnethylolated urea with aldellydes. ~ variety of capsule forming materials are disclo.sed, for example, in U.S. Patent Nos. 3,516,846 and 4,087,37~, and l].K. Patent Specification Nos. 2,006,709 and 2,062,570.
As showrl in these references, the principal utility of microencapsulated materials is in the formation of a surface coated with the rnicrocapsules in a binder. The microcapsules are ruptured by various means to release the material contained therein. In addition to release of physically observable materials such as ink in order to form a visi~le image, other types of active in~redients such as odor releasirlg materials, bacteriostatic materials, chemically active materials and the like have been provided in this manner.
U.S. Patent 4,186,743 discloses a perfuming self-adhering sanitary napkin having a pressure-sensitive adhesive layer bonded to a strippable cover sheet having a binder layer with microcapsules on the surface thereof in contact with the pressure-sensitive adhesive layer. Upon stripping of the cover sheet, capsules are broken, the pressure sensitive adhesive is exposed and the napkin may adhere to undergarments to keep them properly positioned.
U.S. Patent 4,487,801 discloses a fragrance releasing pull-apart sheet comprising a non-pressure-sensitive binder layer contailling microcapsules adhered between two sheets. IJpon separation of the sheets, the adhesive and caE~sules rupture, releasing the material within the capsules.

-~ 7~
-3- 60557-2978 Summary of the Invention The present invention provides a stacked, coherent array of elements for providing access to an encapsulated liquid or spreadable material, said array comprising 1) at least three sheets, each pair of adjacent sheets in adjacent elements bound by an adhesive composition layer, 2) said adhesive composition layer containing micro-capsules with an encapsulated material comprising a liquid or spreadable material within the shell of the microcapsules, and 10 3) said microcapsules having an average diameter between 4 and 100 micrometers, the cohesive strength of the adheslve composition layer being less than the strength of the bond between said adhesive composition and the faces of said sheets, the tensile rupture strength of said microcapsules being such that the cohesive failure of the adhesive results in breakage of the microcapsules, and the tensile rupture strength between said two sheets being at least l.Og/cm and less than 90g/cm at 20C and 50~ relative humidity.
The microcapsules are ruptured by pulling apart the sheets leaving behind the remainder of the stacked array from which additional individual sheets can be removed. The removal of indivi-dual sheets causes the capsules in the adhesive layer joining that sheet to the remainder of the stacked array to rupture and release the ingredients contained therein. The exposed or released ingredi-ent may be applied to another surface, such as skin, by rubbing the surface of the individual sheet with ruptured capsules against another surface.
The invention will further be described, by way of example .~

,, , -3a- 60557~2978 only, with reference to the accompanying drawings, wherein:-Figure 1 shows a side view of the stacked array ofelements according to a preferred embodiment of the present inven-tion.
Figure 2 shows a side view of an alternative construction of a stacked array according to the present invention.
Figure 1 shows the stacked array 2 of the present inven-tion with a top sheet 4 adhesively secured to bottom sheet 8 by an adhesive layer 6 having ruptureable microcapsules 18 therein. The surface of the bottom sheet 8 which is away from the top sheet 4 has an adhesive layer 10 thereon securing it to the next sheet 12.
That sheet 12 is further secured by adhesive layer 14 to another sheet 16. These layers will cumulatively form a pad or stacked array 2.
Figure 2 shows an alternative construction for a stacked array or pad 20 of the present invention. The top sheet 22 has a polymeric binder with microcapsules 42 therein which ~orms a coating layer 24 on the backside of the top sheet ~ Th~t coating layer 24 is secured by adhesive layer ?6 to the next top sheet 2~. Similarly, top sheets 2~3 and 34 ar-? coate(i on their backsi-3es with micro-capsules contain;ng l)in~ler layers 30 and 36 and .secured to the next top layers ~)y adheisve layers 32 and 3~.

I)etailed l)escription of the Invention Existing fr.1grance releasing elements such as those disclosed in IJ..S. Patent 4,~7,~301 are designed to provide a one-tilne rele1se of material contained therein.
After its fir~t II.Se, ti~e article is e.ssentially valueless, although solne ad(3itiorlal, unhrokell capsules in the exposed adl1esive may be rupture-3 by abrasion. The elements are also primarily desigl1e(1 for insertion in maga~.ines or mailers to provide a single occurrence of fragrance.
The present invention provides a pad or stacked array of indivi-lual elements. ~ach individual element, when separated from the pad provides access to the material encapsulated in one of the layers. Each individual element may thereupon be used to provide reasonably accurate and consistant amounts of fragrance to the air or materials for application to other surfaces such as medication, perfumes, lipstick, skin creams, repellant or the like. The pad may be conveniently carried in a pocket or purse with no possibility of spillage of the carried materials. ~1l1ere the ruptured adhesive layers with microcapsules therein is a hypoallergenic pressllre-sensitive adhesive, topical or even transcutaneous me(1ications may be applied by adherence of that layer to the skin.
The present invention relates to an article comprising at least three elements or sheets (and preferably a multiplicity, e.g., 50, lO0 or more) each pair of two adjacent elernents or sheets being temporarily secured by means o~ an a(~hesive layer having microcapsules dispersed tl1ereirl. The sheet materials or elements of the present inver1tior1 comE)rise any sheet or film forming material, or multi~)le adhered layers of such materials, particularly 1~aE)er and most preferahly coated paper.
Generally flexible sl1eets of paper are preferred although polymeric films Inay ~,e use(1. Coate(l paper is a conventional an(1 st~r1d;1r(1 item in cornmerce used for printiny o~ (lur1]ity images the1-eor1. It is generally a fibrous sheet haviny a pigment-bearing resinous coating on one or both sur-Eaces. 1Isually tl1e pigment provides a white, bone or ivory coloration to the sheet. Most generally pigme11t.s pr~oducing a white coloration are used.
The binder used in the resinous coating is generally colorless and/or trar1sE)arer1t~ The binder is generally a synthetic or natura1 oryanic polymeric material. Typical pigments for producing wl1ite coated paper are fine white pigment such as clay, calcium carbonate, titania, silica, zinc oxide, etc. Typical binders include latices (e.g., styrene-butadiene, butadiene-acrylonitrile, etc.), film-formir1g polymers (e.g., polymethylrnethacrylate), and natural resins (e.g., casein, amnnonium caseinate, starch, etc.3. The c->atings usually cornprise hetween 65-90% by weight of pigment, preferably 70-~30% by weight of pigment, and 10-35% by weight of binder, preferably 20-30% by weight of binder.
The adhesive material for the capsules must form a bond to the surfaces of the sheets which is stronger than the cohesive strength of the adhesive with the capsules dispersed therein. A]though it is generally desirable to have an adhesive, the absolute cohesive strengtll of which is less than its adhesive strength to the coated surface of the coated ~aper cover sheets, this is not essential. When capsules are included within the adhesive composition, the effective cohesive strength of the adhesive tends to be reduced. Adheslves, which by themselves would cause the slleets to be darnaged during separation, can be used in cornbination Witl1 capsules in the practice of the present invention because of lowered effective cohesive strength.

i4~

The capsules in the present invention may comprise any ruptureable capsule containing an active ingredient therein. The tensi]e rupture strength of the capsules must be such tha~ the cohesive failure of the adhesive results in capsule i,reakage. It has also been found that the size of the capsnles play.s a role in the usefulness of capsules witllin rupt~reable ~heets according to the practice of the present inventiorl. Generally the capsules should have an average diameter between 6 and 50 microns and preferably between 12 and 30 microns when the capsule payload is between 80 arlcl 90~ hy weight of the total capsule weight.
It is highly ~>referrell that the capsules have an average diameter betweerl l4 and 26 microns and it is most preferred that the capsules have a diameter between 15 and 25 rnicrons. These dimensions play a surprisingly important role in the a~ility to control the percentage of rupture of capsules in the practice of the present invention. With lower payloads (e.g., 70-80~), the capsules should be larger to provicle the necessary rupture strength. The broadest range of capsule size unde~ any conditions would be about 4 to 100 microns, with smaller than 8 micron capsules used with a 90-95% by weight payload. Eight to thirty micron capsules are generally preferred.
A basic relationship exists amongst the factors of peel force adhesive coating weight and the median capsule diameter. This relationship can be expressed as P=k (CW/d2)~ wherein P equals the peel force, Cw equals the adhesive line coating weight, d equals the median diameter of the capsu]es and k equals a co-efficient relating to binder and substrate properties. The peel force should be in the range of 1.5 to 12 ounces per lineal inch, preferably 1.5 to 8.0 ounces per lineal inch. The coating weight of adhesive and microcapsules should be at a coating weight of approx;mately one pound for 300 to 800 square feet. Preferably the coating weight should be between approximately one pound for each 400 to 650 square feet.
At higher coating wei~hts, the surface of the cover sheets 1~7~i4~

tend to tear, while at lower coating weights, the ~sheets tend to pull a~art an(l the adhesive to paper bond tends to rupture in a-lvance of the capsules included therein. The capsules shoul(~ ~orm ~)etween ~0 and 90 percent by volume of the total adhesive conll-osition, and preferahly between 50 and ~5 percent o~ the total composition volume. If certain microcapsule shell rnaterials are used, such as gelatin, the capsule may cornpri~se ag much as lOO~ of the adhesive compositions .
Any class of pressure-sensitive aAhesive may be used in the exterior surface of one of said sheets where pressure-sensitive adhesives are usedO Typically, acrylate and polyurethane pressure-sensitive adllesives are used to bond the article to another ~surface.
There are nurnerous advantages to the practice of the present invention and techniques for improving products using the present invention. The pads may be easily carried in a pocket or purse or suitcase without any fear of spillage. Relatively precise dosages and amounts may be provided without measurelllent. Samples may be provided without opening sealed containers. Application may be made to surfaces without lirect contact by the hands of the person applying the material.
The present invention enables the manufacture of a device for exposing a liquid or spreadable material (e.g., to the atmospllere), said device comprising:
1) at least three elements or sheets bound by at least two adhesive composition layers, 2) said adhesive composition layers containing microcapsules with said liquid within the shell of said microcapsules, and 3) said microcapsules having an average diameter hetween 4 and lOO rnicrometers, the cohesive strength of the adhesive composition layer being less than the strength of the bond between said adhesive composition and a face of said elements or sheets, the tensile rupture strength of said microcapsules being -r-less than the cohe.sive strength of the adhesive composition, and the rupture force of said adhesive composition layer containing microcapsules at 50% relative humidity bein-J between at least 1 ounce per linear five-arld-one-ilalf inclle3 arld less tilan 45 ounces ~er linear five-and-one-llalf inclles (greater than 2.0g/cm and less than 90y/cm), at least one portion of an interior surface of said sheets having a zone along an edge thereof which is not adhered to an adjacent sheet. It is preferred that the rupture strengtll between the sheets excedes 8.0g/cm and is less than ~Og/cm and most: preferahly excedes 16g/cm and is less than 75~/cm. ~rhe rninimum strengt11 at this ambient condition (i.e., 20C and 5()% R.H.) i.5 necessary to keep the sheets from falling apart from forces incurred during handling. This problem has frequently occurrecd in magazine inserts wllere coated paper was used. The maximum limit on the rupture strength is necessary to keep the paper from tearing (termed fiber pull or fiber rupture) before the adhesive and capsules rupture. This would prevent release of the liquid from the capsules. A "liquid" according to the present invention includes liquids with materials dissolved or dispersed therein (e.g., pigments) and gels which are capable of flowing under moderate pressure. A
"spreadable material" means any material which can be spread at room temperature by moderate hand pressure. Soft waxy materials such as lipsticks, rouge and the like are intended by the description. Solid powders, which do not flatten and sprea-3 out to form a film-like coating, are not included in the term spreadable. Such materials which are not liquid at room temperature may be cold ground to form particles and then encapsulated. The particles would tend to be rougll and irregular in shape, but useful.
It is also desirable to have the construction resist the effects of variable ambient conditions. It is therefore desirable that rupture strength excede 4.0g/cm after storage at 120C an-3 less than 1% R.~l. for seventy-two hours. This test would be performecl by storage -!3-in an oveo, removal to a neutral environment (e.g., sealed bag or jar) until the article is at room temperature, and then measuring tile rupture strer-gtll. It is preferred that the rupture strenytl~ is at least ~.Og/cm and most preferred S that the ruptllrr st:rengtil i..5 at least 16g/cm under those conditions. The article must still display a rupture strengtll ~etweetl 2 an(l 90g/cm at 20C and 50% R.H.
~ number of methods have been found which enable these conditions to be met according to the present invention. The use o~ viscosity increasing agents in the binder provides a more even coating and one that ruptures before fiber plJ]l be(3ins. The use of additional coatinys over the coate-l paper which contain polymers different from the binder of the adhesive layer and which do not form a solution or chemically bond to tlle binder of the adhesive layer provides a useful article according to the present invention. The use of larger size capsules tends to weaken the cohesive strenyth of the adhesive composite and prevent fiber pull. The use of capsules which are not moisture sensitive in combination with tllese large capsules (i.e., greater than 30 rnicrons and up to 95 rnicrons) provides a useful adhesive layer. Higher capsule-to-binder ratios reduce the collesive strength of the adhesive, as does the addition of non-visco~ity enhancinc3 particulate fillers.
According to the preferred practice of the present invention, if the stacked array uses coated paper surfaces, the binder between the sheets preferably contains viscosity increaser.s (viscofiers) in addition to the rnicrocapsules. The use of viscofiers reduced the criticality of proportions of materials and provided increased coating and manufacturing latitude. Viscosity enhancers or visco~sity increasing agents are well known in the art. Any material which when pre.sent in the coating solution in an amount not greater than 10% by weight increases the viscosity by at least 5% is a viscofier according to the present invention. Preferably viscosity is increased by at least 20%. They are either inorganic l~t~4l --1 ()--particulate materials (e.g., silica, amorphous ~ilica, bentonite clay, montmorillonite clay, etc.) or organic particu]ate or soluble materials (e.c3., water softenable acrylic particles, water swellable poly(methylmetl~crylate), water soluble or organic solvent soluble polylners, etc:.). The inorganic particles tend to be preferre(~. ~rhe visco~iers enhancers have been found to be necessary ir~ c]ry weight proportions of the adhesive mix in amounts oE ~rom 0.~5 to 12% by weight, preferably from 5 to 12~ by weight. In general, the weight proportions of materials in the (lried adhesive layers according to the present invention are generally as follows:
Microcapsllles 21 - 80%
Adllesive 19.75 - 70 Viscosity Enllancer~s 0.25 - 12%

Other optional ingre~ients such as surfactants, coating aids and the like may he present. Preferred proportions of these ingredients are:
Microcapsules 44.5 - ~0%
~dhesive 19.5 - 55%
Viscosity Enhancers 0.5 - 10%

The nature and composition of the adhesive binder is not critical to the practice of the invention as long as the required adhesive and cohesive properties are met. The adhesive may be pressure sensitive, water or solvent soluble or thermally activatable. ~ single layer of a non-pressure~sensitive adhesive is preferred. There is no need for rejoining the sheets after rupturing of the capsules and so the pressure sensitive function is not essential to practice of the invention although it is highly desirable in some uses as previously described.
The adhesive (with Inicrocapsules) may be applied between two separate .sheets in either a continuous or discontinuous pattern.s. It i8 usually desirable to leave at least some portion of at least one outer edge of the ~7;~

sheets unbonded so as to provid~ arl area where separation can be easily started.
It i3 ;)referred that t:he capsule-bearing adhesive coated inside portion between the sheets constitute from 60 to 95% of the ~I]rface area of the ~heets. lO to 95 percent adhesive covera~3~ ca~ e used to leave an e~ye or corner that can be rea(]iLy graspe-l to pull one sheet fron another.
Some uses may allow for only a single corner to be uncoated so as to provide a starting point for the separation of the sheets, bnt the 6(~ to gr~ range is preferred with 70 to 90%
more preferred. rrhe adhesive free zones may he on the same edge of the sheet or may be on varying or alternative edges of the ~sheet (e.-~., left side, then right side, then left again).
Any class of adhesives including but not limited to polyurethanes, polyacrylates, polyvinyl resins (e.g., polyvinyl alcohol, polyvinyl chloride), polyamides, polyesters, polyolefins, starches, gum arabic, gelatin and the like may be readily used in the practice of the present invention. ~ashirlg of the capsules before mixing them with the adhesive often tends to provide more consistency in their properties by removing low molecular weight, unreacted materials.
In effect, to best practice the present invention it is desirable that certain properties within the article have relative values for each of the materials used. The cohesive strength oE the sheet material should exceed the adhesive strength i>etween the binder and the sheet. The adhesive stren(3th of the binder to the sheet should exceed the cohesive strength oE the binder and capsules therein.
The cohesive strength of the hinder should exceed the tensile rupture limits of the capsules. As previously noted, the size of the capsules has an important effect upon the practice of the present invention. With capsules less than 8 rnicrorls, there tends to be less rupturing of the capsules during separation of the sheets which prevents the useful and e~ficient release of materials. ~bove 30 1~7~,~i41 -1?--microns, the particles are so large that they are morereadily burst (.sometimes too readily) by handling of the sheets and manufacturing procedures. Furthermore, with the large size particles ;t i.s extremely difficult to control bursting upon sei)aralion of the sheets because of increased effects upon aclhesive clnd collesive properties of materials in contact with the cal)sules. The preferred ranges of 8 to 30 and 15 to 25 microns is important to the practice of the present inventiorl witl, a high quality product. ~ithin these limits, rupture in excess of 50 percent of the capsules can be easily obtained. r~upture in excess of 80 percent of the capsules can ofterl he accomplislled in the practice of the present invetltion withirl those limits.
The capsules may contain a wide variety of active materials therein. The least useful of materials to be included therein would be coloring agents since separation of the sheets would generally produce uniform coloration rather than a clistinct image. The most preferred types of ingredients would he fragrant materials (such as essences and perfumes) or materials WhiCll provide chemically active vapors or liquids (e.g., bacteriostats, insect repellants or deodorants) to be wiped on or transferred to another surface. These may or may not also be colored. For example, a testing kit for the presence of chemical vapors could be produced ~y providing material within the capsules which would react in the vapor phase with the material for which a leak is heing investigated. By separating the sheet, rupturing the capsules and exposing the vapor test material, a color forming reaction in the air or on the sheet could be readily observable.
These ancl other aspects of the present invention will be shown in the following examples.

Example 1 A 70 lh stock of one side coated paper was used as the top sheet 2 of the label 14. A slurry was prepared from rose fragrance in urea-aldehyde microcapsules ~;~7;~i41 manufactured according to the p~ocess of Example 10 of U.S.
Patent 3,516,941. The slurry contained 64% dry weight of capsules, 2~.50~ dry weight of poly(vinyl alcohol) (Gelvatol~ ~0-1()), 10.50% poly(vinyl alcohol) (Gelvatol~2()-~), an(l 1~ glycerin in water. The slurry was applied to ~35~ ~f the s~rface of the uncoated face of a continuous web o~ pressure sensitive label stock at a coating wei~3ht Or 3.5 pourlds per 1300 ft2. After the slurry was applied, the uncoate(l face of the top sheet was mated to the wet slurry coated face of the label stock and dried. The lamir~ate was then die-cut into appropriate sizes (e.g., 3 x ~ cm~ . The cut labels were then removed and affixed by the pre~qsure sensitive-adhesive to one another in a stacke-3 array o~ fifty individual elements.
The edge of the top sheet which was over the uncoated surface of the label stock was ea.sily raised and grasped by one hand. Upon pulling the top sheet, fragrance was released and the hottom sheet remained firmly adhered to the rernaining elements of the pad.
Mechanical handling of the pad did not produce any significant level of capsule breakage.

~xample 2 The slurry of Example 1 was coated onto 85~ of the surface of the coated face of one-side coated paper stock at a coating weight of 3.5 po~nds per 1300 ft2.
Before drying, another sheet of paper stock was laid coated side up on the slurry coated surface. The application of slurry and paper stock was repeated until fifty sheets were arrayed. The pad was oven dried at moderate temperatures (about 110F, 42C) ~or twelve hours, then die-cut into pads that were 3 x ~ crn. Individual elements could be stripped from the pal.s. The adhesive bearing surface of the element was rubbed ayainst the skin, transferring the fragrance.

Claims (20)

The embodiments of the invention in which an exclusive property or privilege is claimed are defined as follows:
1. A stacked, coherent array of elements for providing access to an encapsulated liquid or spreadable material, said array comprising 1) at least three sheets, each pair of adjacent sheets in adjacent elements bound by an adhesive composition layer, 2) said adhesive composition layer containing microcapsules with an encapsulated material comprising a liquid or spreadable material within the shell of the microcapsules, and 3) said microcapsules having an average diameter between 4 and 100 micrometers, the cohesive strength of the adhesive composition layer being less than the strength of the bond between said adhesive composition and the faces of said sheets, the tensile rupture strength of said microcapsules being such that the cohesive failure of the adhesive results in breakage of the microcapsules, and the tensile rupture strength between said two sheets being at least 1.0g/cm and less than 90g/cm at 20°C and 50% relative humidity.
2. The device of claim 1 wherein said adhesive composition comprises said microcapsules and a polymeric binder, and there are at least twenty adjacent pairs of sheets.
3. The device of claim 2 wherein said surfaces are on flexible sheets of paper and said polymeric binder is a pressure-sensitive adhesive.
4. The device of claim 2 wherein said sheets are flexible paper and said binder is a non-pressure-sensitive polymeric binder.
5. The device of claim 1 wherein said micro-capsules have an average diameter between 8 and 30 micrometers,
6. The device of claim 1 wherein said individual elements comprise two sheets, a top sheet and a bottom sheet, having said adhesive composition layer between said two sheets and also having a pressure-sensitive adhesive layer on the surface of said bottom sheet which is not in contact with said adhesive composition layer.
7. The device of claim 4 wherein said individual elements comprise two sheets, a top sheet and a bottom sheet, having said adhesive composition layer between said two sheets and also having a pressure-sensitive adhesive layer on the surface of said bottom sheet which is not in contact with said adhesive composition layer.
8. The device of claim 2 wherein said microcapsules comprise gelatin and are between 21 and 100%
by weight of said adhesive composition and said binder comprises between 0 and 78.75% by weight.
9. The device of claim 4 wherein said microcapsules comprise between 50 and 85% by volume of said adhesive composition and are formed of a urea-aldehyde polymer.
10. The device of claim 2 wherein said microcapsules comprise between 50 and 85% by volume of adhesive composition and comprise a polymeric shell material.
11. The device of claim 1 wherein said top sheet has perforated lines thereon to enable removal of individual portions of said top sheet.
12. The device of claim 2 wherein said encapsulated material is a liquid which comprises a perfume and the shell of said microcapsules comprises a urea-formaldehyde resin.
13. The device of claim 6 wherein said encapsulated material is a liquid which comprises a perfume.
14. The device of claim 7 wherein said encapsulated material is a liquid which comprises a perfume.
15. The device of claim 1 wherein the encapsulated material is a liquid which contains a medically active ingredient.
16. The device of claim 2 wherein said encapsulated material is a liquid which contains a medically active ingredient.
17. The device of claim 7 wherein said encapsulated material is a liquid which comprises a medically active material.
18. The device of claim 1 wherein said encapsulated material is a spreadable material selected from the group consisting of lipstick, rouge, and medically active ingredients.
19. The device of claim 2 wherein said encapsulated material is a spreadable material selected from the group consisting of lipstick, rouge, and medically active ingredients.
20. The device of claim 7 wherein said encapsulated material is a spreadable material selected from the group consisting of lipstick, rouge, and medically active ingredients.
CA000495734A 1985-01-24 1985-11-20 Pad fragrance sampling device Expired - Lifetime CA1272641A (en)

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
US06/695,045 US4661388A (en) 1985-01-24 1985-01-24 Pad fragrance sampling device
US695,045 1985-01-24

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US (1) US4661388A (en)
EP (1) EP0188883A3 (en)
JP (1) JPS61169237A (en)
KR (1) KR940000621B1 (en)
AU (1) AU573404B2 (en)
BR (1) BR8506569A (en)
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AU573404B2 (en) 1988-06-09
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EP0188883A2 (en) 1986-07-30
KR940000621B1 (en) 1994-01-26
US4661388A (en) 1987-04-28
JPS61169237A (en) 1986-07-30
EP0188883A3 (en) 1988-06-01
AU5036185A (en) 1986-07-31

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