[특허]Freeze indicators, components therefor and preparative processes

Temptime Corporation

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Freeze indicators, components therefor and preparative processes

특허상세정보
국가/구분	United States(US) Patent 등록
국제특허분류(IPC7판)	G01N-025/20 G01K-011/12
미국특허분류(USC)	422/082.12; 422/420; 422/430; 436/147; 436/164; 116/216; 374/106; 252/962
출원번호	US-0511025 (2009-07-28)
등록번호	US-8128872 (2012-03-06)
발명자 / 주소	Lentz, Carl Smith, Dawn E. Taylor, Dene H.
출원인 / 주소	Temptime Corporation
대리인 / 주소	K&L Gates LLP
인용정보	피인용 횟수 : 48 인용 특허 : 13

초록
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Freeze indicators can include an indicator dispersion, a liquid medium, indicator particles dispersed in the liquid medium and a particulate inorganic nucleating agent to inhibit supercooling of the liquid medium. The inorganic nucleating agent can have an ionic surface coating which can help provide a sharp end point. Optionally, freeze indicators can include indicator particles comprising an organic material and a softener to soften the indicator particles and provide the freeze indication with an enhanced visual appearance. Another option is to provide a temperature-sensitive stabilizer to inhibit coagulation of the indicator dispersion at temperatures above the liquid medium frozen state melting point while permitting coagulation of the indicator dispersion at the liquid medium frozen state melting point.

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1. A freeze indicator comprising an indicator dispersion having an initial appearance, the indicator dispersion comprising: (a) an aqueous liquid medium having a melting point determined from the frozen state of the liquid medium;(b) solid indicator particles comprising an organic material and a softener to soften the indicator particles at the aqueous liquid medium melting point, wherein the softener is intimately admixed with the organic material and the indicator particles have a softness of at least about 20 dmm, as determined at 25° C. by Needle Penetration Test ASTM D1321, and are dispersed in the liquid medium; and(c) a particulate nucleating agent to inhibit supercooling of the liquid medium below the liquid medium melting point;wherein in the frozen state of the liquid medium the indicator particles are coalesced providing the indicator dispersion with a different appearance from the initial appearance and the coalescence and the different appearance are irreversible. 2. A freeze indicator according to claim 1 wherein the organic material comprises a wax material selected from the group consisting of a paraffin wax, a microcrystalline wax, carnauba wax, beeswax, Chinese wax, shellac wax, spermaceti, tallow, palm wax, soy wax, lanolin, wool grease, and mixtures of any two or more of the foregoing wax materials. 3. A freeze indicator according to claim 2 wherein the softener comprises a wax softener selected from the group consisting of an ethylene-vinyl acetate copolymer, an ethylene-acrylic acid copolymer, a microcrystalline wax, polyethylene, cholesterol, short-chain alkanes, paraffinic oil, naphthenic oil, aromatic oil, glycerol, mineral oil, a fatty acid, a fatty-acid derivative, a fatty alcohol, a fatty acid ester, a hydrogenated fatty acid, a partially hydrogenated fatty acid, a lipid, a hydrophilic softener and a hydrophilic long-chain hydrocarbon comprising at least one ester group. 4. A freeze indicator according to claim 1 wherein the organic material comprises a soft solid or a semi-solid material selected from the group consisting of rubbery polymers, styrene-butadiene latex, natural rubber latex, rubbery polyurethane, rubbery acrylic polymers and copolymers, rubbery nitrile polymers and copolymers, rubbery polychloroprene, rubbery vinyl pyridine polymers, rubbery styrene polymers, rubbery styrene/butadiene copolymers, rubbery styrene/acrylic acid copolymers, rubbery vinyltoluene/tertiary-butyl-styrene copolymers, rubbery vinylidene chloride/vinyl chloride copolymers and mixtures of two or more of the foregoing polymeric materials. 5. A freeze indicator according to claim 4 wherein the softener comprises a plasticizer and the organic indicator material has a glass transition temperature below about 20° C. or below the liquid medium frozen state melting point or has a glass transition temperature above about 20° C. 6. A freeze indicator according to claim 1 wherein the indicator particles have a softness of at least about 30 dmm. 7. A freeze indicator according to claim 1 wherein the liquid medium is aqueous and the nucleating agent comprises ice-nucleating particles. 8. A freeze indicator according to claim 7 wherein the nucleating agent is selected from the group consisting of an ice-nucleating protein, an ice-nucleating microorganism, Pseudomonas syringae microorganisms, Pseudomonas syringae nucleating proteins, and mixtures of two or more of the foregoing nucleating agents. 9. A freeze indicator according to claim 1 wherein the indicator dispersion comprises a dispersion stabilizer wherein the dispersion stabilizer inhibits coagulation of the indicator dispersion at temperatures above the liquid medium frozen state melting point and permits coagulation of the indicator dispersion at the liquid medium frozen state melting point. 10. A freeze indicator according to claim 9 wherein the indicator dispersion comprises a high-molecular weight, low-temperature destabilizer to promote freeze-related coagulation without causing premature coagulation at temperatures above the liquid medium frozen state melting point wherein the low-temperature destabilizer has a molecular weight in the range of from about 1,000 to about 100,000 dalton. 11. A freeze indicator according to claim 1 wherein the indicator dispersion comprises a proportion of indicator particles of from about 5 to about 60 percent by weight based upon the weight of the indicator dispersion and a proportion of nucleating agent of at least about 0.1 percent by weight based upon the weight of the indicator dispersion. 12. A freeze indicator according to claim 3 wherein the liquid medium is aqueous, the nucleating agent comprises an ice-nucleating protein, the indicator dispersion comprises a proportion of indicator particles of from about 5 to about 60 percent by weight and a proportion of ice-nucleating protein of at least about 0.01 percent by weight, both ranges of proportions of ice-nucleating protein being based upon the weight of the indicator dispersion, and the indicator particles have a softness of at least about 20 dmm. 13. A freeze indicator according to claim 1 comprising a proportion of the softener of from about 5 to about 50 percent by weight based upon the combined weights of the softener and the organic indicator material. 14. A freeze indicator according to claim 10 wherein the dispersion stabilizer comprises a nonpolar surfactant and no polar surfactant is present. 15. A freeze indicator according to claim 10 wherein the dispersion stabilizer comprises a surfactant in a concentration calculated to provide less than monolayer coverage of the surfaces of the indicator particles. 16. A freeze indicator according to claim 10 wherein the dispersion stabilizer comprises a surfactant having enhanced efficacy in a specified pH range and wherein the indicator dispersion has a pH outside the specified pH range. 17. A freeze indicator according to claim 16 wherein the surfactant is nonpolar, the specified pH range is from about pH 6 to about pH 8 and the indicator dispersion has a pH of less than about 5 or greater than about 9. 18. A freeze indicator according to claim 16 wherein the surfactant is anionic, the specified pH range is above about pH 7 and the indicator dispersion has a pH of less than about 6. 19. A freeze indicator according to claim 16 wherein the surfactant is cationic, the specified pH range is below about pH 7 and the indicator dispersion has a pH of greater than about 8. 20. A freeze indicator according to claim 10 wherein the low-temperature destabilizer is present in a proportion by weight relative to the proportion of dispersion stabilizer of from about 0.2 to 1 to about 1 to 1.3. 21. A freeze indicator according to claim 20 wherein the dispersion stabilizer is polar and the low-temperature destabilizer carries a charge opposite to the charge of the dispersion stabilizer. 22. A freeze indicator according to claim 20 wherein the low-temperature destabilizer is a cationic, anionic, zwitterionic or an uncharged compound or compounds. 23. A freeze indicator according to claim 20 wherein the low-temperature destabilizer comprises a high molecular weight polyacrylamide, a high molecular weight polyvinyl alcohol, a high molecular weight polyvinyl pyrrolidone, a high molecular weight polyacrylic acid or a mixture of two or more of the foregoing compounds. 24. A freeze indicator according to claim 10 wherein the indicator particles comprise a wax material, the indicator dispersion comprises an anionic surfactant, and the low-temperature destabilizer comprises a cationic polymer, a cationically modified hydroxyethyl cellulose polyquaternium-4, or a low molecular weight cationically charged polymeric flocculant. 25. A freeze indicator according to claim 10 wherein the indicator particles comprise a wax material, the indicator dispersion comprises a cationic surfactant, and the low-temperature destabilizer comprises an anionic polymer, a polyacrylic acid or a polymethacrylic acid or a mixture of two or more of the foregoing low-temperature destabilizers. 26. A freeze indicator according to claim 10 wherein the indicator particles comprise a wax material, the indicator dispersion comprises a zwitterionic surfactant, and the low-temperature destabilizer comprises a cationic, anionic or zwitterionic surfactant or a mixture of two or more of the foregoing low-temperature destabilizers. 27. A freeze indicator according to claim 10 wherein the dispersion stabilizer comprises an anionic surfactant selected from the group consisting of sodium stearate, potassium stearate, sodium myristate, sodium oleate, sodium dodecyl sulfate, ammonium lauryl sulfate, sodium lauryl ether sulfate, sodium dodecyl 3-mole ether sulfate, sodium dodecyl benzene sulfonate, sodium nonylphenol 2-mole ethoxylate sulfonate, bis(2-ethylhexyl)sodium sulfosuccinate and mixtures of two or more of the foregoing anionic surfactants. 28. A freeze indicator according to claim 10 wherein the dispersion stabilizer comprises a cationic surfactant selected from the group consisting of dodecyl trimethyl ammonium chloride, hexadecyl trimethyl ammonium bromide, cetylpyridinium chloride, polyethoxylated tallow amine, benzalkonium chloride, benzethonium chloride and mixtures of two or more of the foregoing cationic surfactants. 29. A freeze indicator according to claim 10 wherein the dispersion stabilizer comprises a zwitterionic surfactant selected from the group consisting of lauryl amido propyl dimethyl betaine, dodecyl betaine, dodecyl dimethylamine oxide, cocamidopropyl betaine, coco amphoglycinate and mixtures of two or more of the foregoing zwitterionic surfactants. 30. A freeze indicator according to claim 10 wherein the dispersion stabilizer comprises a nonpolar surfactant selected from the group consisting of fatty acid ethoxylates, sorbitan esters, sorbitan ester derivatives, sorbitan monolaurate, copolymers of poly(ethylene oxide) and poly(propylene oxide), fatty alcohols, cetyl alcohol, oleyl alcohol and mixtures of two or more of the foregoing nonpolar surfactants. 31. A freeze indicator according to claim 1 wherein the liquid medium is an aqueous liquid medium consisting essentially of water or of deuterium oxide or of a mixture of water and deuterium oxide, wherein the organic particles having a softness of at least about 20 dmm, and wherein the indicator dispersion comprises a polar dispersion stabilizer, and a high-molecular weight, low-temperature destabilizer carrying a charge opposite to the charge on the dispersion stabilizer to promote freeze-related coagulation, the low-temperature destabilizer having a molecular weight in the range of from about 1,000 dalton to about 100,000 dalton. 32. A freeze indicator according to claim 31 wherein the dispersion stabilizer is an anionic surfactant and the low-temperature destabilizer carries a cationic charge or the dispersion stabilizer is a cationic surfactant and the low-temperature destabilizer carries an anionic charge. 33. A freeze indicator according to claim 1 in combination with a freeze-sensitive host product, the freeze indicator being associated with the host product to indicate possible exposure of the host product to a temperature at or near the liquid medium melting point. 34. A freeze indicator according to claim 1 wherein the nucleating agent comprises an ice-nucleating protein. 35. A freeze indicator according to claim 7 wherein the liquid medium consists essentially of water or of deuterium oxide or of a mixture of water and deuterium oxide. 36. A freeze indicator according to claim 10 comprising a proportion of dispersion stabilizer of from about 0.01 percent to about 5 percent by weight based on the weight of the indicator dispersion. 37. A freeze indicator according to claim 15 wherein the surfactant is selected from the group consisting of nonpolar, anionic, cationic and zwitterionic surfactants. 38. A freeze indicator according to claim 1 wherein the organic material comprises a wax having a melting point in the range of from about 40° C. to about 80° C. 39. A freeze indicator according to claim 1 wherein the indicator particles are solid particles of homogenous material. 40. A freeze indicator according to claim 1 wherein the organic material comprises a wax material selected from the group consisting of a waxy polymer, a waxy copolymer, a waxy polyolefin, a waxy polyethylene, a waxy polypropylene, a waxy ethylene-vinyl acetate copolymer, a waxy ethylene-acrylic acid copolymer and mixtures of any two or more of the foregoing wax materials. 41. A freeze indicator according to claim 1 wherein the indicator dispersion comprises a proportion of indicator particles of from about 10 to about 20 percent by weight based upon the weight of the indicator dispersion and a proportion of nucleating agent of from about 1 percent to about 2 percent by weight based upon the weight of the indicator dispersion. 42. A freeze indicator according to claim 1 comprising a proportion of the softener of from about 20 to about 30 percent by weight based upon the combined weights of the softener and the organic indicator material. 43. A freeze indicator according to claim 2 wherein the indicator particles lack dyes and pigments.

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