# US 8,785,523 B2 · Phosphorus loaded particles and methods for their preparation and use > Agents: this data is available as JSON from the patentgrep API and MCP server — see https://patentgrep.com/llms.txt - Number: US 8,785,523 B2 - Document ID: US8785523B2 - Status: Granted - Kind: B2 - Application number: 13/604,781 - Filed: 2012-09-06 - Published: 2013-06-06 - Granted: 2014-07-22 - Earliest claimed: 2012-09-06 - Assignees: Empire Technology Development LLC - Applicants: Seth Adrian Miller - Inventors: Seth Adrian Miller - Web page: https://patentgrep.com/patent/US8785523B2 ## CPC - C08J 3/212: {and solid additives} - C08K 3/016: Flame-proofing or flame-retarding additives - C08J: WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H (working, e.g. shaping, of plastics B29) - C08K: Use of inorganic or non-macromolecular organic substances as compounding ingredients (paints, inks, varnishes, dyes, polishes, adhesives C09) ## Abstract A flame retardant additive includes red phosphorus adsorbed into a porous carrier. The carrier may be mixed with white phosphorus above its melting point (41° C.), so that liquid phosphorus is pulled into the pores of the carrier by capillary action. The phosphorus-loaded carrier may be heated above 250° C. to convert the white phosphorus to red phosphorus. The resulting red phosphorus-loaded carrier may retain flame retardant activity, and may also be protected from the environment for easier handling and formulation. By employing a carrier of a suitably small particle size, it is practical to incorporate the flame retardant red phosphorus-loaded carrier in thin films. ## Claims ### Claim 1 A flame retardant composition comprising: a noncombustible particulate dispersed in a polymer film, the noncombustible particulate including nanoscale pores; and red phosphorus adsorbed into the nanoscale pores of the noncombustible particulate, wherein the flame retardant composition is characterized by a total red phosphorus content substantially comprising the adsorbed red phosphorus. ### Claim 2 (depends on 1) The composition of claim 1, wherein the red phosphorous is present in the composition at about 30% to about 90% by weight. ### Claim 3 (depends on 1) The composition of claim 1, wherein the noncombustible particulate includes one or more of silica gel, alumina, a zeolite, and an aerogel. ### Claim 4 (depends on 1) The composition of claim 1, wherein the noncombustible particulate is characterized by an average particle diameter of about 0.1 micrometers to about 100 micrometers. ### Claim 5 (depends on 1) The composition of claim 1, wherein the noncombustible particulate is characterized by an average nanoscale pore diameter of about 0.001 micrometers to about 10 micrometers. ### Claim 6 (depends on 1) The composition of claim 1, wherein the noncombustible particulate is characterized by a surface area by weight of about 20 square meters per gram to about 2,000 square meters per gram. ### Claim 7 (depends on 1) The composition of claim 1, wherein a water reactivity of the red phosphorus adsorbed by the noncombustible particulate is less than a water reactivity of a pure red phosphorus particulate, the pure red phosphorus particulate having an average particle diameter of 100 micrometers. ### Claim 8 A polymer composition comprising: at least one polymer configured as a film; and a flame retardant composition dispersed in the polymer, the flame retardant composition including: a noncombustible particulate that includes nanoscale pores; and red phosphorus adsorbed into the nanoscale pores of the noncombustible particulate, wherein the flame retardant composition is characterized by a total red phosphorus content substantially comprising the adsorbed red phosphorus. ### Claim 9 (depends on 8) The polymer composition of claim 8, characterized by an average film thickness of equal to or less than about 100 micrometers. ### Claim 10 (depends on 8) The polymer composition of claim 8, wherein the noncombustible particulate is characterized by an average particle diameter that is less than a thickness of the film. ### Claim 11 (depends on 8) The polymer composition of claim 8, wherein the red phosphorus adsorbed by the noncombustible particulate is about 0.1% by weight to about 20% by weight of the polymer composition. ### Claim 12 (depends on 8) The polymer composition of claim 8, wherein the polymer includes one or more of a polyolefin, a polyalkylene, a polyoxyalkylene, a polyvinylene, a polyarylene, a polyheteroarylene, a polyester, a polyalkylene terephthalate, a polyacrylonitrile, a polyacrylate, a polystyrene, a poly acrylonitrile-butadiene polystyrene, a polycarbonate, a polyether, a polyurethane, an epoxy, mixtures thereof, and copolymers thereof ### Claim 13 A method of making a flame retardant composition, the method comprising: providing a noncombustible particulate that includes nanoscale pores; providing a fluid that includes phosphorus; contacting the fluid and the noncombustible particulate; adsorbing the phosphorus from the fluid into the nanoscale pores of the noncombustible particulate to produce the flame retardant composition comprising solid red phosphorus adsorbed by the noncombustible particulate; and separating unadsorbed phosphorus from the flame retardant composition after adsorbing the phosphorus into the nanoscale pores of the noncombustible particulate. ### Claim 14 (depends on 13) The method of claim 13, wherein: providing the fluid that includes phosphorus comprises heating white phosphorus to a temperature greater than about 44° C. to form the fluid as molten white phosphorus; and adsorbing the phosphorus from the fluid includes adsorbing the molten white phosphorus into the nanoscale pores of the noncombustible particulate. ### Claim 15 (depends on 13) The method of claim 13, wherein: providing the fluid that includes phosphorus comprises: providing a solution of phosphorus in: carbon disulfide, liquid ammonia, liquid sulfur dioxide, liquid carbon dioxide, phosphorus tribromide, phosphorus trichloride, an organic solvent, or a mixture thereof; and adsorbing the phosphorus from the fluid includes adsorbing dissolved phosphorus from the solution of phosphorus into the nanoscale pores of the noncombustible particulate and removing the solvent to form the flame retardant composition. ### Claim 16 (depends on 13) The method of claim 13, wherein the phosphorus is adsorbed from the fluid as white phosphorus, further comprising forming the solid red phosphorus in the nanoscale pores of the noncombustible particulate from the white phosphorus by: heating the white phosphorus to a temperature greater than about 250° C.; heating the white phosphorus to a temperature greater than about 170° C. in the presence of phosphorus trichloride, phosphorus tribromide, phosphorus triiodide, bromine, or iodine; orexposing the white phosphorus to light. ### Claim 17 A method of making a polymer composition, the method comprising: providing a polymer configured as a film; providing a flame retardant that includes: a noncombustible particulate that includes nanoscale pores; and red phosphorus adsorbed into the nanoscale pores of the noncombustible particulate, wherein unadsorbed phosphorus is separated from the flame retardant composition after the phosphorus adsorbed into the nanoscale pores of the noncombustible particulate; and contacting the polymer and the flame retardant to form the polymer composition. ### Claim 18 (depends on 17) The method of claim 17, wherein: providing the polymer includes providing an organic solvent solution of the polymer; and contacting the polymer and the flame retardant to form the polymer composition includes contacting the organic solvent solution of the polymer and the flame retardant and removing the organic solvent to form the polymer composition. ### Claim 19 (depends on 17) The method of claim 17, wherein providing the polymer includes: providing a monomer of the polymer; contacting the monomer and the flame retardant; and polymerizing the monomer to form the polymer in contact with the flame retardant. ### Claim 20 (depends on 17) The method of claim 17, wherein providing the polymer includes: providing the polymer in molten form; mixing the polymer in molten form with the flame retardant; and cooling the polymer in molten form with the flame retardant to form the flame retardant polymer composition.