throbber
United States Patent [191
`Ehrlich
`
`[54] AQUEOUS BUBBLE BLOWING
`COMPOSITION
`[75] Inventor: Joseph R. Ehrlich, New York, NY.
`[73] Assignee: Jack S. Wachtel, Larchmont, N .Y. ; a
`part interest
`[21] Appl. No.: 200,424
`[22] Filed:
`Oct. 24, 1980
`
`[63]
`
`Related US. Application Data
`Continuation-impart of Ser. No. 26,527, Apr. 3, 1979,
`abandoned.
`
`[51] Int. Cl.3 .................... .. CllD 1/20; B01J 13/00
`[52] US. Cl. .................................. .. 252/542; 252/ 307;
`252/545; 252/ 548; 252/550; 252/DIG. 14
`[58] Field of Search ................. .. 252/3, 153, 542, 545,
`252/548, 550, 307, DIG. 14; 46/6, 7
`References Cited
`U.S. PATENT DOCUMENTS
`
`[56]
`
`Raspert .............................. .. 252/307
`2,433,625 12/ 1947
`2,469,045
`5/ 1949 La Vietes .
`252/ 307
`2,959,887 11/1960 Remeika ..
`........ .. 46/6
`3,328,307
`6/1967 Schmitz
`. 252/ 106
`3,561,154
`2/1971
`Skinner
`........ .. 46/6
`3,630,951 12/1971
`Netherly ................... .. 252/307
`
`[11]
`[45]
`
`4,284,534
`Aug. 18, 1981
`
`3,862,823
`
`1/ 1975 Green et a1. ........................... .. 8/137
`
`FOREIGN PATENT DOCUMENTS
`
`51-11805 1/1976 Japan .
`51-21588 2/1976 Japan .
`
`OTHER PUBLICATIONS
`C.A. 45160g: vol. 83, 1975, p. 100.
`Primary Examiner-P. E. Willis, Jr.
`Attorney, Agent, or Firm—Jacobs & Jacobs
`[57]
`ABSTRACI‘
`A non-toxic, non-eye-irritating bubble composition,
`consisting essentially of an aqueous solution of from
`about 1.5 to about 6% by weight of lauric diethanol
`amide, from about 0.75 to about 3% by weight of an
`alkanolamido half ester of a sulfosuccinic acid salt as
`surfactant, from about 0.05 to about 6% of a water-solu
`ble ?lm-forming agent selected from the group consist
`ing of polyvinylpyrrolidone, polyethylenoxide, polyvi
`nylalcohol, cellulose and gelatin, the weight ratio of
`said lauric diethanolamide to said surfactant on a dry
`basis being from about 1.74:1 to about 2.4:1, from 0 to
`about 10% by weight of glycerin, and the balance wa
`ter.
`
`11 Claims, No Drawings
`
`TEVA EXHIBIT 1045
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC
`
`

`
`1
`
`4,284,534
`2
`alkanolamine is ethoxylated. The general formula for
`these surfactants is
`
`AQUEOUS BUBBLE BLOWING COMPOSITION
`
`5
`
`40
`
`45
`
`The present application is a continuation-in-part of
`my copending application, Ser. No. 026,527 ?led Apr.
`3, 1979, now abandoned, which discloses bubble com
`positions. The copending application of Jack Wachtel,
`Ser. No. 026,528 ?led Apr. 3, 1979 discloses apparatus
`for blowing bubbles. Both of these applications are
`incorporated herein by reference thereto.
`wherein
`,
`The present invention relates to aqueous bubble com<
`R1 is alkanoyl or alkenoyl, e.g. R| is alkanoyl or al
`positions and to a method for making bubbles there
`kanoyl of 10 to 20 carbon atoms;
`'
`from.
`R2 is lower alkylene, i.e. of l to 6 carbon atoms e.g.
`The present invention provides an improved bubble
`ethylene or isopropylene;
`composition for making “snow storm bubbles.” These
`.
`n is 0. to 5 or higher; and
`bubbles, with only a single blast of air, ?ow out of the
`M is a monovalent metal, such as an alkali metal.
`blowing tube in a sustained stream of bubbles, looking
`In the present invention, preferred surfactants are those
`almost like a ?owing liquid. Over one-hundred bubbles
`formed from the amide obtained by reacting lauric acid
`per puff or blast of air can be produced, a phenomenon
`with monoethanolamine (MEA) ethoxylated with three
`20
`quite unlike anything in the prior art. The present inven
`. ethoxy groups or from the amide formed by reacting
`tion provides for bubble solutions of unusually great
`oleic acid with monoisopropanolamine (MIPA).
`capacity. From any given volume of the liquid one can
`The surfactant is present on a dry basis in an amount
`produce many times more bubbles than from an equal
`of from about 1.0 to about 3%, preferably from about 1
`volume of commercial bubble solution. This is accom
`to about 2.5% by weight of the composition. It is essen
`plished without using ingredients that are toxic when
`tial that the ratio of amide to surfactant, on a dry basis
`ingested or are irritating to the eye or skin.
`be from about 1.7:] to about 2.4:1, preferably from
`In particular, the present invention provides a non
`about 1.9:1 to about 2.121, and most preferably 2.021.
`toxic, non-eye irritating bubble composition, consisting
`The third essential component of the invention is
`polyoxyethylene, polyvinylpyrrolidone, polyvinylalco
`essentially of an aqueous solution of from about 2.0 to
`about 6% by weight of lauric diethanolamide, from :
`hol, gelatin or a cellulose, such as methyl cellulose,
`about 1.0 to about 3% by weight of an alkanolamido
`hydroxypropyl cellulose, etc., which are all water-solu
`half ester of a sulfosuccinic acid salt as‘ surfactant, from
`ble ?lm-forming agents. These materials are employed
`about 0.05 to about 6% of a water-soluble ?lm-forming
`in an amount of from about 0.05 to about 6%, preferably
`agent selected from the group consisting of polyvinyl
`from about 0.10 to about 5%, by weight, based on the
`pyrrolidone, polyethyleneoxide,polyvinylalcohol, cel
`weight of the composition.
`lulose derivatives and gelatin, the weight ratio of said
`Surprisingly, the results of the present invention are
`lauric diethanolamide to said surfactant on a dry basis
`obtained only when all of the following are observed:
`being from about 1.711 to about 2.4:1, from'about 0 to
`1. The acid moiety of the alkanolamide must be lauric
`about 10% by weight of glycerin, and the balance wa
`acid;
`2. the alkanolamine moiety of the alkanolamide must
`be diethanolamine;
`3. the ratio of alkanolamide to surfactant must be
`from about 1.74:1 to about 2.4:1, preferably essen
`tially 2:1, and
`4. the speci?ed ?lm-former must be used in an amount
`of from about 0.05 to about 6%.
`When the ingredients and proportions speci?ed
`above are employed, the resulting bubble solution is
`capable of forming vast numbers of bubbles per puff of
`air, a feat unheard of in the prior art. In any case, the
`bubbles are made by forming a layer of the bubble com
`position on a surface by placing a small amount, e.g. a
`few drops, of the composition on the surface, touching
`the layer with the tip of a narrow tube, withdrawing the
`tip with a thin liquid ?lm of the bubble composition
`across the opening at said tip, and holding the tube
`against the lips of the user with said tip pointed up
`wardly and withthe tube at an acute angle with respect
`to the vertical, and then expelling the air gently through
`the tube to form bubbles from the thin liquid ?lm across
`the tip. This procedure is described in detail in my co
`pending application, Ser. No. 026,527, mentioned
`above. While a simple straw can be used to produce
`these bubbles, the bubble pipe of the above-mentioned
`Wachtell application, Ser. No. 026,528 is preferred.
`Pipes having multiple tubes other than the Wachtel
`bubble pipe can also be used.
`
`The lauric diethanolamide used in the invention is
`commercially available. Thus, Witco Chemical Corp.,
`Organics Div., 277 Park Ave., New York, NY. 10017,
`sells this product under the tradename Witcamid 5195.
`A 10% water solution of this product will start crystal
`lizing after about 10 hours. Crystallization starts at the
`top of the liquid, with long, needle-like crystals growing
`down to the bottom. At that point, the entire mass ap
`pears to be solid with no loss in weight. With a 7%
`solution, crystallization takes several days; with a 5.5%
`solution crystallization takes 6-8 weeks; with a 4.9%
`solution, 14-15 weeks. Other commercially available
`lauric diethanolarnides include Schercomid SL-EX and
`Clindrol 100L.
`55
`The lauric diethanolamide is used in an amount of
`from about 2.0 to about 6%, preferably from about 2 to
`about 5%, by weight, based on the weight of the com
`position.
`The surfactant employed in the bubble compositions
`of the present invention cooperates with the lauric di
`ethanolamide to provide ?lm-forming properties as well
`as proper viscosity. The alkanolamido half esters of
`sulfosuccinic acid salts used as surfactant in the inven
`tion are commercially available and are formed by re
`acting maleic anhydride with the amide of a higher fatty
`acid with a lower alkanolamine, followed byvreacting
`the product with sodium bisulfate. In some cases, the
`
`ter.
`
`-
`
`65
`
`TEVA EXHIBIT 1045
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC
`
`

`
`5
`
`TRADENAME
`Polyox WSR-N-IO
`Polyox WSR-N-750
`Polyox WSR-N-3000
`Polyox WSR-ZOS
`Elvanol 71-30 ‘
`PVP K-30
`PVP K-90
`Duponol C
`
`4
`-continued
`CHEMICAL IDENTITY
`
`Polyethylene Oxide M.W. 100,000
`Polyethylene Oxide M.W. 300,000
`Polyethylene Oxide M.W. 400,000
`Polyethylene Oxide M.W. 600,000
`Polyvinyl alcohol, 99% hydrolized,
`Polyvinylpyrrolidone M.W. ' 40,000
`Polyvinylpyrrolidone M.W. 360,000
`USP grade Sodium Lauryl Sulfate
`
`In the following Examples and in this speci?cation
`and appended claims, all parts, percentages and propor
`tions 'are by weight, unless otherwise stated.
`
`EXAMPLE 1
`A bubble solution was formed from the following:
`
`4,284,534
`3
`When polyoxethylene is used as the ?lm-forming
`agent, the bubbles can break with a crackling noise.
`Depending on the amount of polyoxyethylene, the bub
`bles may also form ?akes, which gently fall to the
`ground like snow. In general, the higher the molecular
`weight of the polyoxyethylene, the smaller the amount
`that is used. Thus, Polyox WSR-N-IO (MW 100,000) is
`generally used at 4% or more, while Polyox WSR-N
`750 (MW 300,000) can be used at about 2% and Polyox
`WSR-N-3000 (MW 400,000) can be used at 0.1%. Po
`lyox WSR-205 (MW 600,000) does not precisely ?t this
`rule, as amounts as high as 2% may have to be used.
`(compare Examples 8 and 12 hereinafter).
`High molecular weight polyvinylpyrrolidone also
`gives crackling and ?aking, but only‘at high concentra
`tions.
`Other additives can be used, but are not essential. For
`example, sodium lauryl sulfate increases the viscosity of
`the solution, and most of all helps keep the bubble solu
`tions clear and uniform. Depending on the type of ?lm
`forming material, some solutions have a tendency to
`become ‘hazy or even turbid or to separate into clear
`layers. Sodium lauryl sulfate often acts as a hydrotrope
`in such cases, and can be used in an amount of 0.3 to
`1.5%; higher percentages might have an adverse affect
`on viscosity.
`Another useful additive is sodium chloride in small
`quantities. Depending on the speci?c composition of
`the solution, a useful quantity is‘ from 0.05% to 0.5%,
`usually 0.16-0.2%. The sodium chloride may cause a
`tremendous viscosity increase and must be used spar
`ingly. In some cases, the addition of sodium chloride
`increases the viscosity, number of bubbles and their
`?oating time very impressively.
`The addition of glycerine, e.g. up to 10%, increases
`the ?oating time of the bubbles. The use of glycerin
`almost invariably eliminates the effect of crackling and
`?aking. In certain formulations, the addition of bacteri
`ocides can be helpful.
`The following Examples illustrate preferred embodi
`ments of the invention. In these Examples, trade names
`are used to identify the ingredients to aid the public in
`reproducing the Examples. The operation of the inven
`tion does not depend on the use of the speci?c trade
`45
`named material; the same chemicals made by other
`companies can be used. For example, Standopol SH-lOO
`and SH-135 are the trade names of Henkel, Inc. for a
`30% and 35% aqueous solution, respectively, of diso
`dium monoleamido PEG-2 sulfosuccinate, a surfactant
`50
`of the~formula set forth above. Monomate OPA-100
`manufactured by Mona Industries, Inc., Patterson, NJ.
`and EMCOL 41612 manufactured by Witco Chemical
`Corp., Houston, Tex., are also suitable surfactants.
`The following is a key to the materials used in the
`Examples.
`
`20
`
`25
`
`30
`
`35
`
`55
`
`Parts
`
`3.50
`4.50
`
`0.75
`0.16
`4.00
`87.09
`
`Diethanolamide (Witcamid 5195)
`Alkanolamide half ester of sulfo
`succinic acid sodium salt (Schercopol
`. LMPS)
`Sodium lauryl sulfate (Duponol C)
`Sodium chloride
`Polyoxethylene (polyox WSRN-IO)
`Water
`
`‘ The diethanolamide, alkanolamido half ester of sulfo
`succinic acid sodium salt and polyoxyethylene were
`mixed together under heating to no more than 50° C.,‘
`after which the sodium chloride and part of the water
`was added, followed by addition of the remainder of the
`water and the sodium lauryl sulfate. Heating was con
`tinued until all of the ingredients were well dissolved,
`after which the solution was left to cool. The solids
`content was 10.16%.
`Using simple straws of 4 to 6 mm in diameter, a large
`number of bubbles per puff of air are obtained from the
`resulting bubble solution. The bubbles sink down as
`?akes.
`The solution can be diluted with water to a solids
`content of 7.5% while retaining its ability to form ?ak
`ing bubbles.
`The procedure of Example 1 was followed in the
`following Examples.
`
`EXAMPLE 2
`
`Parts
`
`2.80
`3.60
`4.00
`89.60
`
`Schercomid SL-EX
`Schercopol LMPS
`Polyox N-l0
`Water
`
`TRADENAME
`
`CHEMICAL IDENTITY
`
`Schercomid SL-EX
`
`Witcamid 5195
`Clindrol 100L
`Schercopol LMPS
`
`Schercopol OMS-Na 3s
`
`Schercopol OMIS-Na 40
`
`} lauric diethanolamide
`
`-
`
`39% aqueous solution of diso
`dium monolauramido
`MEA sulfosuccinate
`35% aqueous solution of
`disodium monooleamido
`MEA sulfosuccinate
`40% aqueous solution of
`disodium monooleamido MIPA
`sulfosuccinate
`
`60
`
`65
`
`A bubble solution of 8.2% solids was obtained. This
`solution gave 40-70 multiple bubbles that crackle
`lightly on bursting and come down slowly as thin ?akes.
`The addition of 0.5 parts sodium lauryl sulfate makes
`the solution translucent/transparent, less stringy and
`gives 70-80 individual bubbles with mild crackling and
`thin ?akes. Further addition of 3.5 parts of glycerin
`makes the bubbles ?oat for several minutes with no
`crackling noise, but still a few ?akes.
`
`TEVA EXHIBIT 1045
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC
`
`

`
`5
`
`4,284,534
`
`6
`
`EXAMPLE 3
`
`-.
`
`'
`
`,
`
`.
`
`EXAMPLE 8
`
`5
`
`a
`
`.
`
`‘
`
`Parts
`
`3.50
`4-50
`0.25
`91.75
`
`Witcamid 5195
`Schercopol LMPS
`POlYOX WSR 205
`Water
`
`Parts
`
`4.40 ~
`5.50
`4.(X)
`2.76
`1.10
`82.24
`
`Witcamid 5195
`Schercopol LMPS
`Glycerin
`PVP K_9()
`Duponol C
`Water
`
`g
`The solution was clear and contained 10.39% solids
`and gave 80-90 long-?oating bubbles-
`
`EXAMPLE 4
`
`'
`
`7
`
`Parts
`
`3.50
`4,50 _
`.16
`‘ 4.59
`87.25
`
`.
`
`Witcamid 5195
`Schercopol LMPS
`Sodium Chloride
`Polyox WSR N-10
`Water
`
`.
`
`I
`
`.
`
`The solution contained 10.0% solids and produced
`-
`bl
`' h
`kl'
`d ? k .
`80 9o bub > es wit ‘some crac mg an
`a CS
`EXAMPLE 5
`
`_
`
`P
`
`3115
`
`3.50
`‘432
`1'50
`9034
`
`Witcamid 519s
`ZZEF'COPZ: Laws
`polylz'rsvsanliw
`water
`
`10
`
`The solution contained 4.3% solids and formed up to
`50 slightly crackling, weakly ?aking, heavy bubbles.
`Many multiple bubbles were formed_ Using 2 parts
`Polyox WSR 205 in place of 0.25 parts gave no different
`15 result.
`
`'
`EXAMPLE 9
`
`20
`
`25
`
`Pam
`3.50
`4.50
`.76
`.13
`2.00
`
`89.11
`
`_
`
`'
`
`Schercomid SL-EX
`Schercopol LMPS
`Duponol C
`Sodium Chloride
`Elvanol 71-30
`
`Water
`
`The solution contained 8.14% solids and formed
`70-80 fast disappearing bubbles with no crackling and
`no ?akes. The solution separates on standing and re
`30 quires shaking before use.
`
`.
`
`EXAMPLE 10
`Example 9 is repeated but the Elvanol is replaced by
`35 Polyox WSR-N-3000. This yields a clear, uniform, vis
`cous solution which provides 70-80 crackling bubbles.
`
`The solution contained 6.91% solids and gave 80-90
`bubbles with loud crackles.
`
`40
`
`EXAMPLE 6
`
`Parts
`5.52
`4.52
`.15
`~46
`'75
`50
`
`90.10 -
`
`Witcamid 5195
`Schercopol LMPS
`Sodium Chloride
`Gelatin (30° mmmgmm)
`Duponol C
`Bacterium“
`
`Water ~
`
`-
`
`45
`
`50
`
`The solution contained 6.64% solids and formed 80
`quickly bursting bubbles. When 2.5 parts glycerin was
`added, ?oating bubbles were obtained.
`55
`
`EXAMPLE 7
`.
`
`.
`
`.
`
`Parts‘
`3.50
`4.50
`.16
`98-22
`
`.
`
`Witcamid 5195
`Schercopol LMPS
`Sodium chloride
`1:51)“ WSR N40
`
`ater
`
`I
`.
`The solution contained 6.41% solids and formed
`80-100 crackling bubbles with no ?akes.
`
`60
`
`EXAMPLE 11
`
`Parts
`4.4
`5.5
`.8
`.2
`'1
`89")
`
`Schercomid SL-EX
`Schercopol LMPS
`Duponol C
`Sodium Chloride
`p°ly°x WSR'N‘3OOO
`water
`
`The clear viscous solution contained 7.64% solids
`and formed 70 bubbles with thin ?akes and crackling.
`ThlS solution was d1luted to 6.79% solids and still
`formed 60-70 crackling bubbles and thin ?akes.
`
`.
`
`.
`
`.
`
`.
`
`.
`
`EXAMPLE l2
`
`Pam
`
`3.50
`4.50
`.75
`.16
`2'27
`88'82
`
`Schercomid SL-EX
`Schercopol LMPS
`Duponol C‘
`Sodium Chloride
`P°'y°" WSR'PJSO
`water
`
`I
`
`The hazy viscous solution had 8.43% solids and gave a
`65 100 and more slightly crackling bubbles and thin flakes,
`including multiples and clusters. When 3.2 parts glyc
`erin were added, 100-120 long ?oating bubbles were
`obtained.
`
`TEVA EXHIBIT 1045
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC
`
`

`
`'7
`
`EXAMPLE 13
`
`4,284,534
`
`8
`?aking bubbles were formed. When diluted with water
`to 6.27% solids, 40-50 bubbles were formed (no ?akes).
`
`Parts
`
`3.50
`4.50
`.75
`.16
`'45
`90.64
`
`Schercomid SL-EX
`Schercopol LMPS
`Duponol C
`Sodium Chloride
`polyox WSR_N_3()()Q
`Water
`
`The solution had a solids content of 6.61% and was
`very slightly hazy and had very low viscosity. 80 bub
`bles with some ?akes, some multiples, were formed.
`EXAMPLE 14
`
`5
`
`10
`
`parts
`
`3-50
`4.50
`.75
`.15
`1.82
`89.28
`
`EXAMPLE 18
`
`SCherwmid'SL-EX
`Schercopol LMPS
`Duponol C
`Sodium Chloride
`Polyox WSR-N-3000
`Water
`
`A hazy viscous solution of 7.46% solids was obtained
`15 from which 60-80 crackling, ?aking, pulverizing bub
`bles were formed. The solution can be diluted 20—25%
`with water with good results.
`
`2O
`
`EXAMPLE 19
`
`This solution had 8.42% solids and formed up to 90 25
`crackling, ?aking bubbles. The solution can be diluted
`20% to 7.02 solids with good results.
`
`.
`
`Parts
`
`2.96
`3.80
`.60
`lag
`91:24
`
`.
`Schercomid SL-EX
`Schercopol LMPS
`Duponol C
`52113532131123?“
`water
`
`Parts
`350
`4.40
`.75
`.15
`2.27
`8893
`
`Schercomid SL-EX
`Schercopol LMPS
`Duponol C
`Sodium Chloride
`Polyox WRS-N-3000
`Wm"
`
`EXAMPLE 15
`
`Parts
`
`2.60
`3.30
`.40
`.16
`91.62
`1.92
`
`Witcamid 5159
`Schercomid LMPS
`Duponol C
`Sodium Chloride
`Water
`Polyox WSR-N-3000
`
`A slightly hazy solution of 6.44% solids was obtained
`30 from which 60-90 crackling bubbles were formed, with
`multiples, bubbles breaking in a cloud of dust, droplets
`and ?akes.
`
`35
`
`EXAMPLE 2O
`
`P
`am
`1.95
`1.95
`
`4.82
`>65
`.90
`.27
`39-46
`
`Witcamid 5195
`Schercomid SL-EX
`
`Schercopol LMPS
`PVP K-90
`Duponol C
`Sodium Chloride
`Wat"
`
`45 A clear solution of 7.60% solids was obtained, from
`which 80 bubbles were formed.
`
`EXAMPLE 21
`
`50
`
`55
`
`Fans
`
`3.50
`
`4.40
`
`1:10
`90.75
`
`Schercomid SL-EX
`
`Schercopol LMPS
`5x11: 538
`Duponol C
`Water
`
`A solution was obtained with 6.81% solids and very
`low viscosity. 50-60 sinking bubbles were formed. The
`60 addition of 0.24 parts sodium chloride increased the
`.
`.
`viscosity and 60-80 bubbles were formed.
`
`EXAMPLE 22
`
`_
`
`_
`
`_
`
`The solution contained 6.32% solids and formed 70
`bubbles, with multiples, clusters thick ?akes, and some 40
`crackling
`
`EXAMPLE 16
`
`Parts
`
`2.40
`3.00
`1.90
`2.70
`90.00
`
`‘
`
`_
`_
`W|tcam1d 5195
`Schercopol LMPS
`Polyox WSR-N-3000
`Glycerin
`Water
`
`_
`
`_
`
`I
`
`The solution contained 5.47% SOlldS and was hazy
`and viscous. It formed 50-70 bubbles with no ?akes and
`no crackling.
`
`EXAMPLE 17
`
`I!
`.2:
`
`Parts
`
`3'50
`4.50
`_75
`.15
`4.55
`86.55
`
`I
`scherwm‘d SL‘EX
`Schercopol LMPS
`Duponol c
`Sodium Chloride
`Polyox WSR-N-75O
`Water
`
`_
`
`'
`
`_
`
`I
`
`I
`
`65
`
`Parts
`
`ThlS solution contained 10.70% solids and was turbid
`and very viscous. It formed 50-60 bubbles with heavy
`?akes. When diluted with water to 8.57% solids, 60
`
`L6
`3,3
`.4
`
`wimamid 5195
`schercopol LMPS
`Duponol C
`
`TEVA EXHIBIT 1045
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC
`
`

`
`9
`-continued
`
`4,284,534
`
`10
`EXAMPLE 26
`
`Parts
`
`1.0
`
`1'6
`.l
`2-9
`.5
`87.7
`
`Sodium lauryl ether sulfate,
`30% aqueous solution
`pvp ](_90
`Gelatin 300 bloomgram
`Glycerin 95%
`Bacteriocide
`Water
`
`5
`
`10
`
`Parts
`3.80
`4.90
`
`0.40
`0.40
`89.80
`
`Schercomid SL-EX
`Schercopol LMPS
`sDétggglolciloride
`Polyox WSR~N-3000
`Hydroxypropyl Cellulose
`Water
`
`A thin clear solution of 6.78% solids was obtained,
`h. h
`60:70 n t.
`b bbl
`ff
`W ‘C gave
`03 mg u es per pu ‘
`EXAMPLE 23
`
`l
`
`Pans
`
`44
`5~5
`0-3
`01
`0'1
`0'6
`88'4
`
`_
`Schercomld SL'EX
`s°h?°°P°1 [MP5
`D“R°“°' C _
`S°d“"" Chkmde
`p°ly°x WSR‘N‘3OOO
`P°IY°X WSR'N 1°
`water
`
`clear viscous Solution,“ 73% Solids was formed’
`WhlCh gave 80-100 vamshmg bubbles.
`The solutions of Examples 1-26 are non-toxic. They
`are non-irritating to the eye, as determined by the
`Dralze eye-irritation test. The compositions are no
`more than minimal irritants as determined by the Pri
`mary Dermal Irritants test.
`What is claimed:
`l. A non-toxic, non-eye-irritating bubble composi
`20 tion, consisting essentially of an aqueous solution of
`from about 2.0 to about 6% by weight of lauric diethan
`olamide, from about 1.0 to about 3% by .weight of an
`alkanolamido half ester of a sulfosuccinic acid salt as
`surfactant, from about 0.05 to about 6% of a water-solu
`25 ble ?lm-formin a ent selected from the rou consist
`.
`. g g .
`g . P
`.
`lng of polyvmylpyrrolldone, polyethylenoxlde, polyvi
`A slightly hazy, viscous solution was obtained which
`nylallcolwl, a_ cgnulose {1nd gelatm, th‘} Weight 1'3"‘) of
`contained 7.94% solids and which gave 100 crackling
`salq Zulu: célet anglamliieTtlo Saul‘) Sm gcifalmfon aodry
`aki
`. hin bubbles when 3 a 11S of
`basis emg rom a out .
`. to a out .
`.
`, rom to
`(but “Pt ? ng) yams g _
`'
`'
`_
`p
`30 about 10% by weight of glycerln, and the balance wa
`glycerm are added, the result is 120 vanishing bubbles
`ten
`that ?oat for a long time. This is a snowstorm that can
`2. The composition according to claim 1, wherein
`be used indoors. The bubbles are completely dry to the
`531d Surfactant 15 0f the formula
`touch.
`
`PL
`EXAM E 24
`
`Parts
`
`4.4
`5'5
`'6
`'16
`1'00
`87;:
`'
`
`Witcamid 5195
`schem°p°l LMPS
`D“R°“°1 C v
`S°d'“m chbnde
`my” WSR'N'3OOO
`3;’ Terge A590 F
`at“
`
`35
`
`40
`
`||
`HC|I—C—(OC2H4),,—-O—R2-NH—R|
`MSO3—C—-C—OM
`"
`
`45
`
`wherein R1 is alkanoyl or alkenoyl, R2 is lower alkylene,
`n is 0 to 5, and M is a monovalent metal.
`3. The composition according to claim 2, wherein R1
`is alkanoyl or alkenoyl of 10 to 20 carbon atoms.
`4. The composition according to claim 2, wherein R1
`is lauroyl, R2 is ethylene, n is 3 and M is sodium.
`5. The composition according to claim 2, wherein R]
`‘5 oleoyl, R2 15 ISPPTOPYICIIQ‘H 15 Zero fmd M 15 5001"!!!’
`A slightly hazy viscous solution of 8.30% solids was
`6'.Th‘? c°mp°sltl9n a.°°°’dmg ‘P clam‘ 1' Wham“ ‘he
`obtained which formed 80-100 ?oating bubbles with
`launc diethanolamide 1s present in an amount of from
`.
`.
`.
`slight crackling and thin ?akes. These bubbles ?oat 50 about 2 to about 5% by weight
`though they (19 not contain glycerin and Still crackle
`7. The composition according to claim 1, wherein the
`and ?ake. Bio Terge AS-90F is sodium alpha ole?n
`ratio of lauric diethanolamide to surfactant is from
`sulfonate made by Stepan Chemical Co., North?eld, Ill.
`about 13:1 to about 2.111.
`_
`_
`8. The composition according to claim 1, wherein the
`55 ratio of lauric diethanolamide to surfactant is essentially
`2:1.
`
`EXAMPLE 25
`'
`
`Parts
`3.60
`5J0
`m
`.10
`_5o
`2_]()
`3300
`
`Schercomid SL-EX
`schmopol OMIsNa 35
`Dupono] c
`Sodium chlo?de
`pow‘,X wsR_N_3o00
`Gym-in
`water
`
`60
`
`9. The composition according to claim 1, wherein the
`surfactant is present in an amount of from about '1 to
`about 25% by weight‘
`_
`_
`,
`10. The composition according to clalm 1, wherein
`the ?lm-forming material 18 present in an amount of
`from about 0.10 to about 5% by weight. _
`1l.‘The composition according to claim 1, further
`containing at least one of sodium lauryl sulfate in an
`amount of from about 0.3 to about 1.5% by weight, and
`65 sodium chloride in an amount of from about 0.05% to
`about 0.5% by weight and glycerine in an amount of up
`to about 10% by weight.
`# it
`
`Ill
`
`0!
`
`it
`
`A viscous, slightly hazy solution of 5.98% solids was
`formed which gave 70-80 ?oating bubbles.
`
`TEVA EXHIBIT 1045
`TEVA PHARMACEUTICALS USA, INC. V. MONOSOL RX, LLC

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