# US 5,705,222 A · Process for preparing nanocomposite particles > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 5,705,222 A - Document ID: US5705222A - Status: Granted - Kind: A - Application number: 08/562,972 - Filed: 1995-11-27 - Granted: 1998-01-06 - Earliest claimed: 1995-11-27 - Assignees: The Trustees of Columbia University in the City of New York - Inventors: Ponisseril Somasundaran; Tsung-Yuan Chen - Web page: https://patentgrep.com/patent/US5705222A ## CPC - B01J 13/02: Making microcapsules or microballoons {(for medical preparations A61K9/50)} - B01J: CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS ## Abstract This invention relates generally to a process for preparing composite particles. More specifically, this invention relates to a process for preparing polymer-coated composite particle dispersions wherein excess polymer is removed by a controlled washing step. This invention further relates to a process for preparing composite particles wherein the particles have an inner core particle coated with at least one polymer coating and at least one shell particle coating. ## Claims ### Claim 1 A process for preparing composite particle dispersions consisting essentially of: dispersing a plurality of core particles in a first solution wherein the core particles do not irreversibly self-flocculate, adding an amount of a polymer to the dispersion of core particles wherein the polymer has an affinity for the dispersed core particles, and removing the excess polymer by a solid/liquid separation process. ### Claim 2 (depends on 1) A process for preparing composite particle dispersions according to claim 1 consisting essentially of: dispersing a plurality of core particles in a first aqueous solution having a pH sufficiently different from the isoelectric point such that the core particle zeta potential is at least +/-20 millivolts, adding an amount of a polymer to the dispersion of core particles, the polymer having a potential opposite that of the dispersed core particles, and removing excess polymer by a) centrifuging the solution, thereby forming a supernatant solution which comprises non-adsorbed excess polymer and a residual solution containing polymer-coated core particles, b) removing the supernatant solution, c) re-dispersing the residual solution in a pure aqueous solution, and d) repeating steps a) through c) as necessary until the excess polymer in the supernatant solution is substantially eliminated. ### Claim 3 (depends on 2) A process for preparing composite particle dispersions according to claim 2, wherein the core particles have an average diameter between 0.1 and 1.0 .mu.m. ### Claim 4 (depends on 3) A process for preparing composite particle dispersions according to claim 3, wherein steps a) through c) are repeated as necessary until the excess polymer concentration in the supernatant solution is less than 1 ppm. ### Claim 5 (depends on 4) A process for preparing composite particle dispersions according to claim 4, wherein the core particle zeta potential is at least +/-40 millivolts. ### Claim 6 (depends on 5) A process for preparing composite particle dispersions according to claim 5, wherein the amount of polymer added is the minimum necessary amount to produce polymer-coated core particles having the maximum polymer adsorption density. ### Claim 7 A process for preparing composite particle dispersions comprising: dispersing a plurality of core particles in a first aqueous solution wherein the core particles do not irreversibly self-flocculate, the first solution having a pH sufficiently different from the isoelectric point such that the core particle zeta potential is at least +/-20 millivolts, adding an amount of polymer to the dispersion of core particles, wherein the polymer has an affinity for the dispersed core particles, the polymer having a potential opposite that of the dispersed core particles, removing the excess polymer by a) centrifuging the solution, thereby forming a supernatant solution which comprises non-adsorbed excess polymer and a residual solution containing polymer-coated core particles, b) removing the supernatant solution, c) re-dispersing the residual solution in a pure aqueous solution, and d) repeating steps a) through c) as necessary until the excess polymer in the supernatant solution is substantially eliminated, and a suspension of shell particles having a size between 1 and 100 nm dispersed in a second aqueous solution is added to the solution of polymer-coated core particles, and excess shell particles are subsequently removed by a) centrifuging the solution, thereby forming a supernatant solution which comprises non-adsorbed excess shell particles and a residual solution containing shell particle-coated composite particles, b) removing the supernatant solution, c) re-dispersing the residual solution in a pure aqueous solution, and d) repeating steps a) through c) as necessary until the excess shell particles are substantially eliminated. ### Claim 8 (depends on 7) A process for preparing composite particle dispersions according to claim 7, wherein the shell particles have a diameter between 1 and 100 nm. ### Claim 9 (depends on 8) A process for preparing composite particle dispersions according to claim 8, wherein the core and shell particles are selected from the group consisting of metal oxides, metal carbides and metal nitrides. ### Claim 10 (depends on 9) A process for preparing composite particle dispersions according to claim 9, wherein the polymer is selected from the group consisting of polyacrylic acid, polyvinyl alcohol, polyamides and polypeptides. ### Claim 11 (depends on 10) A process for preparing composite particles according to claim 10, wherein the polymer is polyacrylic acid. ### Claim 12 (depends on 11) A process for preparing composite particle dispersions according to claim 11, wherein the polymer has a molecular weight in the range of about 2,000 to about 150,000. ### Claim 13 (depends on 10) A process for preparing composite particle dispersions according to claim 10, wherein the first aqueous solution and the second aqueous solution comprise less than 0.10M of a salt. ### Claim 14 (depends on 2) A process for preparing composite particle dispersions according to claim 2, wherein the polymer has a molecular weight in the range of about 2,000 to about 150,000. ### Claim 15 (depends on 1) A process for preparing composite particle dispersions according to claim 1 consisting essentially of: dispersing a plurality of core particles having an average diameter between 0.1 and 100 microns in a first aqueous solution having a pH sufficiently different from the isoelectric point such that the core particle zeta potential is at least +/-20 millivolts, adding an amount of a polymer to the dispersion of core particles, the polymer having a chemical affinity for the dispersed core particles, and removing excess polymer by a) centrifuging the solution, thereby forming a supernatant solution which comprises non-adsorbed excess polymer and a residual solution containing polymer-coated core particles, b) removing the supernatant solution, c) re-dispersing the residual solution in a pure aqueous solution, and d) repeating steps a) through c) as necessary until the excess polymer in the supernatant solution is substantially eliminated. ### Claim 16 (depends on 15) A process for preparing composite particle dispersions according to claim 15, wherein the polymer has a molecular weight in the range of about 2,000 to about 150,000. ### Claim 17 A composite particle dispersion prepared by a process which consisting essentially of: dispersing a plurality of core particles in a first solution wherein the core particles do not irreversibly self-flocculate, adding an amount of a polymer to the dispersion of core particles wherein the polymer has an affinity for the dispersed core particles, and removing the excess polymer by a solid/liquid separation process.