Unagglomerated core/shell nanocomposite particles
First Claim
1. A method of preparing unagglomerated, dispersed core/shell nanocomposite particles in suspension, comprising:
- preparing a reverse micelle microemulsion by forming a mixture comprised of a surfactant, a solvent and an aqueous core precursor at room temperature;
adding a shell precursor material;
treating the reverse micelle microemulsion with a dispersing agent;
breaking the microemulsion to form a suspension of nanocomposite particles by adding a breaking agent to the microemulsion; and
washing and dispersing the suspension of nanocomposite particles simultaneously to produce said unagglomerated, dispersed core/shell nanoparticles in suspension.
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Abstract
The present invention provides a method for the synthesis of unagglomerated, highly dispersed, stable core/shell nanocomposite particles comprised of preparing a reverse micelle microemulsion that contains nanocomposite particles, treating the microemulsion with a silane coupling agent, breaking the microemulsion to form a suspension of the nanocomposite particles by adding an acid/alcohol solution to the microemulsion that maintains the suspension of nanocomposite particles at a pH of between about 6 and 7, and simultaneously washing and dispersing the suspension of nanocomposite particles, preferably with a size exclusion HPLC system modified to ensure unagglomeration of the nanocomposite particles. The primary particle size of the nanocomposite particles can range in diameter from between about 1 to 100 nm, preferably from between about 10 to 50 nm, more preferably about 10 to 20 nm, and most preferably about 20 nm.
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Citations
42 Claims
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1. A method of preparing unagglomerated, dispersed core/shell nanocomposite particles in suspension, comprising:
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preparing a reverse micelle microemulsion by forming a mixture comprised of a surfactant, a solvent and an aqueous core precursor at room temperature;
adding a shell precursor material;treating the reverse micelle microemulsion with a dispersing agent; breaking the microemulsion to form a suspension of nanocomposite particles by adding a breaking agent to the microemulsion; and washing and dispersing the suspension of nanocomposite particles simultaneously to produce said unagglomerated, dispersed core/shell nanoparticles in suspension. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 32, 33, 34, 35, 36, 37, 38, 40, 41, 42)
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17. The method oftlaim 1, wherein the core of the nanocomposite particle contains hydrogel materials selected from the group consisting of polyvinyl alcohol, polymethyl methacrylate and 2-hydroxylethyl methacrylate.
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31. A method of synthesizing unagglomerated, dispersed core/shell nanocomposite particles, comprising:
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preparing a reverse micelle microemulsion, comprising; (i) forming a mixture comprised of poly(oxyetheylene)-nonylphenyl ether, cyclohexane and an aqueous active-medical-agent precursor at room temperature; (ii) stimng the mixture for about 30 minutes; (iii) adding NH4OH to form a suspension; (iv) stirring the suspension for about 15 minutes; (v) adding a shell precursor; and (vi) maturing the microemulsion for about 24 hours; treating the reverse micelle microemulsion with 3-aminopropyltrimethoxysilane; breaking the microemulsion to form a suspension of the nanocomposite particles by adding to the micro emulsion an acetic acidethanol solution which maintains the suspension at a pH of between about 6 and 7; and washing and dispersing the suspension of nanocomposite particles using a size-exclusion HPLC system comprising; (i) packing a HPLC column with spherical silica beads of about 20 μ
m in diameter;(ii) pumping ethanol through the HPLC column; (iii) pumping the nanoparticle suspension into the HPLC column through a stationary phase at a flow rate of about 1 ml/min; (iv) measuring changes in UV absorbance or fluorescence with detectors connected to an out-flow of the HPLC packed column in order to determine when the column is fully saturated with nanoparticles; and (v) eluting and redispersing the nanoparticles with an ethanol/water solution of up to about 70 v/o water.
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39. A method of synthesizing unagglomerated, dispersed corelshell nanocomposite particles, comprising:
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preparing a reverse micelle microemulsion, comprising; (i) forming a first mixture comprised of poly(oxyetheylene)-nonylphenyl ether, cyclohexane, a drug agent precursor and Ca++ at room temperature; (ii) forming a second mixture comprised of poly(oxyetheylene)-nonylphenyl ether, cyclohexane, a drug agent precursor and PO4−
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with optional SO2−
; and(iii) mixing and maturing the first and second mixtures for about two minutes; treating the reverse micelle microemulsion with 3-aminopropyltrimethoxysilane; breaking the micro emulsion to form a suspension of the nanocomposite particles by adding to the microemulsion an acetic acid/ethanol solution which maintains the suspension at a pH of between about 6 and 7; and washing and dispersing the suspension of nanocomposite particles using a size-exclusion HPLC system comprising; (i) packing a HPLC column with spherical silica beads of about 20 μ
m in diameter;(ii) pumping ethanol through the HPLC column; (iii) pumping the nanoparticle suspension into the HPLC column through a stationary phase at a flow rate of about 1 ml/min; (iv) measuring changes in UV absorbance or fluorescence with detectors connected to an out-flow of the HPLC packed column in order to determine when the column is fully saturated with nanoparticles; and (v) eluting and redispersing the nanoparticles with an ethanovwater solution of up to about 70 v/o water.
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Specification