Shelf stable spray dried particles
US-2015374018-A1 · Dec 31, 2015 · US
US2016108340A1 · US · A1
| Field | Value |
|---|---|
| Publication number | US-2016108340-A1 |
| Application number | US-201514884694-A |
| Country | US |
| Kind code | A1 |
| Filing date | Oct 15, 2015 |
| Priority date | Oct 16, 2014 |
| Publication date | Apr 21, 2016 |
| Grant date | — |
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A method of forming microcapsules having improved physical properties and release control as well as the microcapsules formed by the process wherein the capsule wall is formed by the concurrent polymerization of monomers, oligomer and/or prepolymers on the inside of the capsule wall and different monomers, oligomers and/or prepolymers on the exterior of the capsule wall as it forms.
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We claim: 1 . Microcapsules formed in an oil-in-water or water-in-oil microencapsulation process wherein the shell wall is formed from an oil phase (meth)acrylate polymer wall forming composition and from an aqueous phase (meth)acrylate polymer wall forming composition wherein said oil phase (meth)acrylate wall forming composition comprises the combination of either (A) (a) at least one oil soluble or dispersible amine (meth)acrylate, (b) at least one oil soluble or dispersible acidic (meth)acrylate or at least one oil soluble or dispersible simple acid or both, and (c) at least one oil soluble or dispersible multifunctional (meth)acrylate monomer or oligomer or (B) (a) at least one oil soluble or dispersible acidic (meth)acrylate, (b) at least one oil soluble or dispersible simple base, and (c) at least one oil soluble or dispersible multifunctional (meth)acrylate monomer or oligomer, or (C) one or more oil soluble or dispersible mono-, di- or multi-functional (meth)acrylate monomers or oligomers and said aqueous phase (meth)acrylate polymer wall forming composition comprises at least one water soluble or dispersible (meth)acrylate monomer and/or oligomer wherein the shell wall is as a result of the concurrent or sequential polymerization of the wall forming compositions at the interface of the oil and aqueous phases. 2 . The microcapsules of claim 1 wherein the oil phase wall forming composition comprises (A) (a) at least one oil soluble or dispersible amine (meth)acrylate, (b) at least one oil soluble or dispersible acidic (meth)acrylate or at least one oil soluble or dispersible simple acid or both, and (c) at least one oil soluble or dispersible multifunctional (meth)acrylate monomer or oligomer. 3 . The microcapsules of claim 2 wherein the oil phase wall forming composition comprises of (A) (a) at least one oil soluble or dispersible amine (meth)acrylate, (b) at least one oil soluble or dispersible acidic (meth)acrylate, and (c) at least one oil soluble or dispersible multifunctional (meth)acrylate monomer or oligomer 4 . The microcapsules of claim 2 wherein the oil phase wall forming composition comprises (A) (a) at least one oil soluble or dispersible amine (meth)acrylate, (b) at least one oil soluble or dispersible simple acid, and (c) at least one oil soluble or dispersible multifunctional (meth)acrylate monomer or oligomer. 5 . The microcapsules of claim 1 wherein the oil phase wall forming composition comprises (A) (a) at least one oil soluble or dispersible amine (meth)acrylate, (b) the combination of at least one oil soluble or dispersible acidic (meth)acrylate and at least one oil soluble or dispersible simple acid, and (c) at least one oil soluble or dispersible multifunctional (meth)acrylate monomer or oligomer. 6 . The microcapsules of claim 1 wherein the oil phase wall forming composition comprises (B) (a) at least one oil soluble or dispersible acidic (meth)acrylate, (b) at least one oil soluble or dispersible simple base, and (c) at least one oil soluble or dispersible multifunctional (meth)acrylate monomer or oligomer. 7 . The microcapsules of claim 1 wherein the oil phase wall forming composition comprises (C) one or more oil soluble or dispersible mono-, di- or multi-functional (meth)acrylate monomers or oligomers 8 . The microcapsules of claim 1 wherein the shell wall of the microcapsule further comprises a polymeric emulsifier originating from the aqueous phase which polymeric emulsifier is entrapped or encased in the shell wall material. 9 . The microcapsule of claim 1 wherein the oil phase wall forming composition comprises one or more oligomers/prepolymers of any two or more of the components of (A), (B) or (C). 10 . The microcapsule of claim 1 wherein the aqueous phase wall forming composition comprises one or more polyethylene glycol di(meth)acrylates, ethoxylated mono- or multi-functional (meth)acrylates, and (meth)acrylate monomers and/or oligomers. 11 . The microcapsule of claim 1 wherein the shell wall comprises two discrete layers, a (meth)acrylate polymer derived from the oil phase composition and a (meth)acrylate polymer derived from the aqueous phase composition said shell wall having been formed by sequentially polymerizing the two (meth)acrylate polymers wherein initiation of polymerization of the second of the two (meth)acrylate wall forming compositions is delayed until the first has formed a shell wall that completely isolates the two phases from one another. 12 . The microcapsule of claim 10 wherein the interface between the two discrete layers comprises a copolymer of (meth)acrylate monomers, oligomers and/or prepolymers of the two phases and/or physically distinct but intertwined and/or are embedded polymer chains of one (meth)acrylate polymer in the other. 13 . The microcapsule of claim 1 wherein a cross-sectional make-up of the shell wall transitions from a (meth)acrylate polymer derived solely form the oil phase composition to a (meth)acrylate polyer derived solely from the aqueous phase composition with in its composition with an intermediary section which transitions from a substantially wholly oil phase based (meth)acrylate polymer based to a substantially wholly aqueous phase based (meth)acrylate polymer based with midsection region comprising an interpenetrating network and/or copolymer of the wall forming materials from each phase said capsule wall having been formed by concurrently forming the capsule wall from both the aqueous phase and the oil phase, with or without a brief stagger, provided said stagger is not delayed to a point where the capsule wall of the first initiated wall forming material is fully intact whereby the one phase is fully isolated from the other phase. 14 . A method of making microcapsules whose shell wall comprises on one surface a first (meth)acrylate polymer and on its other surface a second (meth)acrylate polymer, said first (meth)acrylate polymer derived from an aqueous phase (meth)acrylate polymer wall forming composition and said second (meth)acrylic polymer derived from an oil phase first (meth)acrylate polymer wall forming composition, and an intermediate region comprising an interpenetrating network and/or copolymer of the two wall forming compositions, said method comprising: (i) forming an oil-in-water or a water-in-oil emulsion of the two (meth)acrylate polymer wall forming compositions, (ii) subjecting the emulsion to conditions for concurrently, at last in part, polymerizing the wall forming materials of each of the oil phase and water phase, and (iii) allowing the reaction to continue until the microcapsules of desired wall thickness are attained. 15 . The method of claim 14 wherein oil phase (meth)acrylate polymer wall forming composition comprises either (A) a combination of (a) at least one oil soluble or dispersible amine (meth)acrylate, (b) at least one oil soluble or dispersible acidic (meth)acrylate or at least one oil soluble or dispersible simple acid or both, and (c) at least one oil soluble or dispersible multifunctional (meth)acrylate monomer or oligomer, (B) a combination of (a) at least one oil soluble or dispersible acidic (meth)acrylate, (b) at least one oil soluble or dispersible simple base, and (c) at least one oil soluble or dispersible multifunctional (meth)acrylate monomer or oligomer, or (C) one or more oil soluble or dispersible mono-, di- or multi-functional (meth)acrylate monomers or oligomers. 16 . The method of claim 15 wherein the method further comprises the step of oligomerizing and/or prepolymerizing some or all of the (meth)acrylate polymer wall fo
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