WO2010062893A1 - Composition de revêtement antibuée, film antibuée et article - Google Patents

Composition de revêtement antibuée, film antibuée et article Download PDF

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Publication number
WO2010062893A1
WO2010062893A1 PCT/US2009/065703 US2009065703W WO2010062893A1 WO 2010062893 A1 WO2010062893 A1 WO 2010062893A1 US 2009065703 W US2009065703 W US 2009065703W WO 2010062893 A1 WO2010062893 A1 WO 2010062893A1
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weight
antifogging
composition according
polymer
aqueous solution
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PCT/US2009/065703
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English (en)
Inventor
Bangwei Xi
Naiyong Jing
Dang XIE
Gaowa Wuyun
Zhigang Yu
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3M Innovative Properties Company
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Publication of WO2010062893A1 publication Critical patent/WO2010062893A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/18—Materials not provided for elsewhere for application to surfaces to minimize adherence of ice, mist or water thereto; Thawing or antifreeze materials for application to surfaces

Definitions

  • the present invention relates to an antifogging coating composition, an antifogging film and an antifogging article, and particularly, to an antifogging coating composition being particularly applicable to high-temperature high-humidity environment, an antifogging film comprising a coating made of the composition and an article comprising the antifogging film, such as mask for medical operation.
  • Plastics or inorganic transparent materials are often used in our daily life.
  • a common problem resided in this type of materials is that after fogging, the transparency thereof will be affected greatly.
  • an inestimable aftereffect may be produced in the operation.
  • various antifogging coatings are developed.
  • the antifogging property of coatings will decrease with the increment of temperature and humidity, and especially, humidity has a great affect on the antifogging property of coatings.
  • this type of antifogging products commonly requires a certain expiration date, and if there is a mass of moisture or high temperature during the process of storage or transport, the products are likely to be out of service. For example, under 5O 0 C and a relative humidity of 90%, the antifogging performance will be lost in less than 12 hours.
  • Testing equipments such as blood sugar test strip, pregnancy test strip, urinalysis test strip and the like, are also required to have a stable hydrophilic surface.
  • An object of the invention is to provide an antifogging coating composition particularly applicable to a high-temperature high-humidity environment, and particularly, to provide an antifogging coating composition particularly applicable to a high-temperature high-humidity environment which can be not only antifogging but also antisticking.
  • Another object of the invention is to provide a hydrophilic antifogging film comprising a coating made of the present composition.
  • a further object of the invention is to provide an article comprising the stable hydrophilic antifogging film, for example, mask, eye glasses, advertising box, displaying shopwindow, pick-up lens and testing equipment.
  • a coating composition obtained by using polyvinyl alcohol as a main component and adding a specific amount of anionic surfactant can provide an antifogging coating with excellent performance which not only can endure the aging due to high temperature or high humidity, but also has improved antisticking ability.
  • the film formed by coating the coating composition of the invention on a substrate can be placed in the form of a web or a stack without a blocking phenomenon.
  • the first aspect of the invention provides an antifogging coating composition comprising: at least a hydrophilic polymer;
  • said polymer is at least one selected from cellulose, polyvinylpyrrolidone, polyacrylic acid, polyacrylamide and polyvinyl alcohol.
  • Another aspect of the invention provides a hydrophilic antifogging film comprising: a substrate; and a coating which is provided on at least a part of at least one surface of said substrate and made of the antifogging composition.
  • a further aspect of the invention provides an article comprising the stable hydrophilic antifogging film of the invention, for example, mask, eye glasses, advertising box, displaying shopwindow, pick-up lens and testing equipment.
  • high temperature means a temperature of 4O 0 C or more
  • high humidity means a humidity of 80% or more
  • centimeter grade means that an average particle diameter of a particle is 150 nm or less.
  • surfactant as used herein describes molecules comprising hydrophilic (polar) and hydrophobic (non-polar) regions on the same molecule which are capable of reducing the surface tension of the coating solution.
  • useful surfactants may include those disclosed in U.S. 6,040,053 (Scholz et al.), incorporated herein by reference.
  • An aspect of the invention provides an antifogging coating composition comprising: at least a hydrophilic polymer;
  • said hydrophilic polymer is at least one selected from a group consisting of cellulose, polyvinylpyrrolidone, polyacrylic acid, polyacrylamide and polyvinyl alcohol.
  • the polymer has a molecular weight of 9,000-150,000.
  • hydrophilic polymer is polyvinyl alcohol.
  • Polyvinyl alcohol is a familiar macromolecule with a good hydrophilic antifogging performance due to the abundant hydroxyl groups accumulating on the side chains thereof. However, the antifogging performance thereof will decrease sharply with the increment of temperature and humidity.
  • a further problem of using polyvinyl alcohol as an antifogging coating is stickness, and especially under a condition of high temperature and high humidity, the mutual contact between polyvinyl alcohol coatings will produce adherence, and thus result in the destroy of the coatings.
  • the inventors have found that, by using a combination of a specific amount of anionic surfactant and polyvinyl alcohol, the problem of antifogging performance decrease and the problem of stickness for the coating under a condition of high temperature and high humidity can be avoided simultaneously and effectively.
  • Useful anionic surfactants include, but not limited to, those with molecular structures comprising (1) at least one hydrophobic moiety, such as from about C 6 - to about C 2 o-alkyl, alkylaryl, and/or alkenyl groups; (2) at least one anionic group, such as sulfate, sulfonate, phosphate, polyoxyethylene sulfate, polyoxyethylene sulfonate, polyoxyethylene phosphate, and the like; and/or (3) the salts of such anionic groups, wherein said salts include alkali metal salts, ammonium salts, tertiary amino salts and the like.
  • useful anionic surfactants include: sodium dodecyl benzene sulfonate (such as, available from Rhone-Poulenc, Inc., Cranberry, N.J. under a trade name of SIPONATE DS-IO), sodium lauryl sulfate, (such as, available from Henkel Inc., Wilmington, Del. under a trade name of TEXAPON L-IOO or from Stepan Chemical Co, Northfield, 111. under a trade name of POLYSTEP B-3), sodium lauryl ether sulfate (such as, available from Stepan Chemical Co, Northfield, 111.
  • sodium dodecyl benzene sulfonate such as, available from Rhone-Poulenc, Inc., Cranberry, N.J. under a trade name of SIPONATE DS-IO
  • sodium lauryl sulfate such as, available from Henkel Inc., Wilmington, Del. under a trade name of TEXAPON L-IOO
  • POLYSTEP B- 12 ammonium lauryl sulfate (such as, available from Henkel Inc., Wilmington, Del. under a trade name of STANDAPOLA), and sodium 1, 4-bis(2-ethylhexyl)-sulfonate (such as, available from Dow Chemical (China) Co. Ltd. under a trade name of GR-5M).
  • ammonium lauryl sulfate such as, available from Henkel Inc., Wilmington, Del. under a trade name of STANDAPOLA
  • sodium 1, 4-bis(2-ethylhexyl)-sulfonate such as, available from Dow Chemical (China) Co. Ltd. under a trade name of GR-5M.
  • the uniformity of the coating can be increased by adding another wetting agent without the antifogging performance.
  • useful wetting agents include polyethoxylated alkyl alcohols (e.g. "BrijTM 30," and “BrijTM 35,” commercially available from ICI Americas, Inc.; “TergitolTM TMN-6TM Specialty Surfactant,” commercially available from Union Carbide Chemical and Plastics Co.), polyethoxylated alkylphenols (e.g., "TritonTM X-IOO", commercially available from Union Carbide Chemical and Plastics Co.; "IconolTM NP-70", commercially available from BASF Corp.) and polyethylene glycol/polypropylene glycol block copolymer (all commercially available from BASF, Corp.
  • any added wetting agent must be included at a level which will not destroy anti-fogging properties of the coating.
  • the wetting agent is used in amounts of less than about 0.1 percent by weight of the coating composition, preferably between about 0.003 and 0.05 percent by weight of the coating composition depending on the amount of silica nanoparticles. Rinsing or steeping the coated article in water may be desirable to remove excess surfactant or wetting agent.
  • the anionic surfactants applicable to the invention include, but not limited to, carboxylate type, sulphate type, phosphate type (including monoester and diester), fluorine-containing anionic surfactant and sulfonic acid type or sulphonate type surfactant.
  • carboxylate type e.g., carboxylate type
  • phosphate type including monoester and diester
  • fluorine-containing anionic surfactant sulfonic acid type or sulphonate type surfactant.
  • sulfonic acid type and sulphonate type anionic surfactant are preferred.
  • sec. -alkyl sulfonate salt such as sodium sec.
  • alkyl benzene sulfonic acid such as dodecyl benzene sulfonic acid and alkyl benzene sulfonate such as sodium dodecyl benzene sulfonate
  • sulfosuccinate salt such as sodium 1 , 4-bi(2-ethylhexyl) sulfonate are more preferred.
  • the invention uses dodecyl benzene sulfonic acid and/or sodium dodecyl benzene sulfonate as the anionic surfactant.
  • These two surfactants are especially excellent in increasing the antisticking effect of polyvinyl alcohol coating.
  • this kind of surfactant of dodecyl benzene sulfonic acid itself can act as an acid for acidifying polyvinyl alcohol which will contribute to the inner cross-linking of polyvinyl alcohol and thus the antisticking effect of polyvinyl alcohol is further increased.
  • sodium dodecyl benzene sulfonate is used, the antisticking effect of polyvinyl alcohol coating can also be further increased by acidification.
  • the pH range of the solution can be 1 to 14. According to certain preferable embodiments, the pH value of the described composition is 1-7, more preferably 2-4.
  • organic or inorganic acids can be used, wherein sulfonic acid type organic acid surfactant is preferred, such as dodecyl benzene sulfonic acid.
  • the addition amount of the surfactant can be selected in dependence on specific situation so that the coating has a prominent aging antifogging performance under high-temperature and high-humidity.
  • the addition amount reaches a certain ratio, the aging antifogging performance under high-temperature and high-humidity will not be increased prominently by further increasing the addition amount of the surfactant. Therefore, according to certain preferable embodiments, the addition of the anionic surfactant is 1.0 wt% to 20 wt%, more preferably 1.5 wt% to 15 wt% relative to 100% by weight of the polymer.
  • the amount of the anionic surfactant is too much, the interaction between the anionic surfactant and polyvinyl alcohol will make the spreading of the coating on PET surface inferior and disadvantageous Iy affect the appearance of the coating. If the amount is too less, the best aging antifogging effect under high-temperature and high-humidity can not be achieved.
  • the surfactant applicable to the invention can be a combination of two or more kinds of different anionic surfactants, wherein at least one anionic surfactant such as sodium sec.-alkyi sulfonate is mainly used for improving the antifogging appearance, while other type of anionic surfactant such as dodecyl benzene sulfonic acid is mainly used for increasing the antisticking performance of the coating.
  • anionic surfactant such as sodium sec.-alkyi sulfonate
  • other type of anionic surfactant such as dodecyl benzene sulfonic acid
  • the composition of the invention further comprises nontoxic or low poisonous inorganic oxide particles, such as silica, zinc oxide, alumina, zirconia, calcium oxide, magnesium oxide and titanium oxide, and it is preferably nanometer grade silica with an average particle diameter of 1 nm to 150 nm.
  • the adequate addition Of SiO 2 nanoparticles into the composition consisted of polyvinyl alcohol and an anionic surfactant can further increase the antisticking ability of the composition of the invention so as to simultaneously obtain the best antifogging property under high temperature and high moisture.
  • Silica can be used in a manner of aqueous solution.
  • the silica being applicable to the invention, for example, can be purchased from Nalco Company.
  • SiO 2 nanoparticles with various particles diameters can all be applicable to the invention, for example, the SiO 2 nanoparticles purchased from Nalco Company include, but not limited to: 1115 (4 nm), 2326 (5 nm), 1130 (8 nm), 1030 (13 nm), 1050 (20 nm), 2327 (20 nm), TXl 1561 (45 nm), 1060 (60 nm) and 2329 (75 nm).
  • the particle diameter and the addition amount of nanoparticles have great effect on the performance of coating. Nanometer grade SiO 2 with large particle diameter has a better antisticking effect. The larger the particle diameter is, the lesser the SiO 2 amount required will be.
  • the addition of the described silica is 5% to 60% relative to 100% by weight of the polymer. If the addition amount of SiO 2 is too low, the increment of the antisticking effect is not prominent, and if the addition amount is too high, coating clouding will be caused while the increment degree of the antifogging performance of the coating will be affected.
  • the composition of the invention further comprises a cross-linking agent, such as tetraethyl orthosilicate or a prepolymer thereof, or glycidyletherpropyltrimethoxyl silane or a prepolymer thereof.
  • the cross-linking agent is used in the invention for increasing the cross-linking degree thereof so as to increase the physical performance of the coating, such as increasing the wet-rub resistance ability of the coating.
  • the addition amount of this kind of cross-linking agents should not exceed 2% of the weight of the polymer such as polyvinyl alcohol.
  • the concentration of the polymer in the composition of the invention is no specific limitation on the concentration of the polymer in the composition of the invention.
  • the polymer is 3% to 10% of the total weight of said composition.
  • the described polyvinyl alcohol in the composition of the invention has an alcoho lysis degree of 60-100%, preferably 86% to 100%. This is because the water-proofing ability of the polyvinyl alcohol with a low alcoho lysis degree may be poor. Under a high-humidity condition, a case of mutual adherence is easily occurred after coatings contact each other. However, a low alcoholysis degree will not affect the high-temperature high-humidity aging antifogging performance of the coating.
  • the solvent in the composition of the invention is preferably an aqueous solvent and more preferably water.
  • One or more other polar solvents can be added on a basis of water to mix with water, and examples of said other polar solvents include ethanol, methanol, ⁇ o-propanol, acetone and the like.
  • the invention further provides a film comprising: a substrate; and a dried adherent coating which is provided on at least a part of at least one surface of said substrate and made from the antifogging coating composition of the invention.
  • the antifogging coating can be coated on single side or both sides of the substrate.
  • Said substrate includes transparent or translucent materials in the visible light region, for example, polyester (e.g., polyethylene terephthalate(PET), polybutylene terephthalate (PBT)), polycarbonate(PC), allyldiglycolcarbonate, polyacrylates (such as polymethylmethacrylate), polystyrene, polysulfone resin, polyethersulfone resin, homo-epoxy polymers, epoxy addition polymers with polydiamines, epoxy addition polymers with polydiols, polyethylene and copolymers thereof, fluorinated surfaces, cellulose esters such as cellulose acetate and cellulose butyrate or the like, glass, ceramic, organic and inorganic composite surfaces and the like, and blends and laminates consisted of the above described materials.
  • polyester e.g., polyethylene terephthalate(PET), polybutylene terephthalate (PBT)
  • PC polycarbonate
  • allyldiglycolcarbonate polyacrylates (such as polymethylmeth
  • the substrate is in the form of film, sheet or block material and may be a part of an article such as ophthalmic lenses, architectural glass, decorative glass frames, vehicle windows and windshields, and protective eye wear such as surgical masks and face shields.
  • the coatings may, optionally if desired, cover only a portion of the article, e.g., only the section immediately adjacent the eyes in a mask may be coated.
  • the substrate may be of flat, curved or various shapes.
  • the article to be coated may be produced by methods of blowing, casting, extrusion, or injection molding and the like.
  • said substrate in the film of the invention is at least one transparent material selected from polyethylene terephthalate (PET), polyethylene glycol naphthalene dicarboxylate, polybutylene terephthalate (PBT), polycarbonate (PC), polyolefm, polystyrene, glass and polymethyl methacrylate (PMMA), and various compositions constituted of the materials described above.
  • PET polyethylene terephthalate
  • PBT polyethylene glycol naphthalene dicarboxylate
  • PC polycarbonate
  • PMMA polymethyl methacrylate
  • the invention further provides an article which comprises the film according to the invention.
  • the article of the invention is applicable to all situations requiring antifogging, especially a situation of hydrophilic antifogging.
  • the article of the invention is in a manner selected from mask, eye glasses, advertising box, displaying shopwindow, diagnostic test strip and pick-up lens.
  • Mask is more preferable, which includes, but not limited to, mask for medical operation, protecting mask for mining, protecting mask for welding and protecting mask for smeltery.
  • Eye glasses is also a preferable article of the invention, which includes, but not limited to, glasses for daily, glasses for swimming, glasses for laboratory and glass for medical applications.
  • the antifogging coating composition of the invention can be prepared by using conventional methods and the invention has no limitation on the preparation method thereof.
  • the antifogging coating composition of the invention can be prepared by dissolving predetermined amount of a polymer or the solution thereof with an arbitrary concentration in a solvent to form a polymer solution, and then adding thereto required amount of an anionic surfactant and optional nontoxic or low poisonous metal oxide particles and mixing uniformly.
  • the preparation method for the antifogging coating composition of the invention will be described in detail, for example, by taking polyvinyl alcohol as the polymer component and taking water as the solvent component in the composition of the invention.
  • the antifogging coating composition of the invention can be prepared by adding an anionic surfactant and various of optional additives such as nanometer grade SiO 2 solution and the like into a required amount of polyvinyl alcohol solution and keeping stirring for at least 30 min.
  • the film of the invention can be prepared by coating the antifogging coating composition of the invention onto at least a part of at least one surface of a substrate by utilizing a conventional coating method, such as, wire rod coating, roll coating, curtain coating, rotogravure coating, spray coating, dip coating, air knife coating or the like.
  • the preferred coating methods include wire rod coating, rotogravure coating, or air knife coating so as to control the thickness of coating.
  • the film of the invention can be prepared by coating the obtained coating composition of the invention on a PET surface (such as, using a 4 ⁇ m wire rod), and then drying for a proper time under a predetermined temperature.
  • the corona and harding temperature can be selected according to the demand. Generally, the higher the corona value is, the better the bonding between the obtained coating and the substrate will be. Corona and harding temperature have no remarkable effect on the antifogging performance of the coating.
  • the article of the invention can be obtained by situating the film of the invention at various application situations.
  • Aging experiment is carried out in an aging chamber with a relative humidity of 90% at 5O 0 C.
  • the test for antifogging performance is performed by taking a sample out of the aging chamber and then breath was applied to the film side with the antifogging coating, It is a passing standard that there isn't any fog appears on the surface of the sample. It will be determined to be un-antifogging that any visual fog appears on the surface of the sample, regardless how fast the disappearing speed of the fog on the surface of the sample will be.
  • the distance between the mouth and the surface of the film at blowing should not exceed 2 centimeters.
  • Antisticking experiment is also carried out in an aging chamber with a relative humidity of 90% at 5O 0 C. Two films are superposed together (the sides with the antifogging coating contact each other), and six 5 cmxlO cm stainless steel plates with a total weight of 220 grams are placed thereon.
  • the PETs used for the experiments are all from Shanghai Zicheng Packing Material Co. Ltd. (Shanghai, China).
  • the polyvinyl alcohols used include GM-14 and N-300 produced by Nippon Gohsei Company (Japan).
  • GM-14 has an alcoholysis degree of 86.5% to 89% and a molecular weight between 44,000 and 66,000.
  • N-300 has an alcoholysis degree of 98% to 99% and a molecular weight of 66,000 or more. Unless stated otherwise, all of the parts, ratios and percentages are on a basis of weight. Specif ⁇ c examples
  • Methylol cellulose (Molecular weight 98,000, Shanghai Jiachen Chemical Co. Ltd., Shanghai, China)
  • Polyacrylic acid (Molecular weight 15,000, Jinsheng Chemical Co. Ltd., Xinxiang City, Henan province, China)
  • Comparative Example IA and IB 250 mg of 10% polyoxy ethylene octylphenol was added into 10 g of 3% polyvinyl alcohol aqueous solution (GM- 14 for Comparative Example IA and N-300 for Example IB) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET films were 2 for both Comparative Examples IA and IB under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Comparative Example 2 A and 2B cationic surfactant: 250 mg of a complex of 10% alkyl dimethyl benzyl ammonium chloride was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14 for Comparative Example 2 A and N-300 for Example 2B) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET films were 0 for both Comparative Examples 2A and 2B under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Comparative Example 3 A and 3 B non-ionic surfactant: 250 mg of D-glucopyranose (oligomeric, decyl octyl glucose) was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14 for Comparative Example 3 A and N-300 for Example 3B) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET films were 2 for both Comparative Examples 3 A and 3B under a circumstance with a relative humidity of 90% at 5O 0 C.
  • D-glucopyranose oligomeric, decyl octyl glucose
  • Comparative Example 4 A and 4B non-ionic surfactant: 250 mg of 10% hydrogenated castor oil was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14 for Comparative Example 4 A and N-300 for Example 4B) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET films were 1 for both Comparative Examples 4A and 4B under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Comparative Example 5 A and 5 B non-ionic surfactant: 250 mg of 10% aliphatic polyethenoxy ether aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14 for Comparative Example 5A and N-300 for Example 5B) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET films were 2 for both Comparative Examples 5 A and 5B under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Example 1 (anionic surfactant): 250 mg of 10% dodecyl benzene sulfonic acid aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET film was 6 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • anionic surfactant 250 mg of 10% dodecyl benzene sulfonic acid aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET film was
  • Example 3 (anionic surfactant): 250 mg of 10% sodium dodecyl sulfonate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET film was 7 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • GM- 14 polyvinyl alcohol aqueous solution
  • Example 4 A and Example 4B(anionic surfactant) 250 mg of 10% sodium sec.-alkyi sulfonate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14 for Example 4 A and N-300 for Example 4B) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET films were 10 for both Example 4 A and 4B under a circumstance with a relative humidity of 90% at 5O 0 C.
  • anionic surfactant 250 mg of 10% sodium sec.-alkyi sulfonate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14 for Example 4 A and N-300 for Example 4B) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then
  • Example 5 A and 5B anionic surfactant: 250 mg of 10% sodium 1, 4-bi(2-ethylhexyl) sulfonate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM-14 for Example 5A and N-300 for Example 5B) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET films were 10 for both Example 5 A and 5 B under a circumstance with a relative humidity of 90% at 5O 0 C.
  • anionic surfactant 250 mg of 10% sodium 1, 4-bi(2-ethylhexyl) sulfonate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM-14 for Example 5A and N-300 for Example 5B) and stirred for 30 min. The obtained solution was coated on
  • Example 6 A and 6B anionic surfactant: 250 mg of 10% sodium dodecyl sulphate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM-14 for Example 6A and N-300 for Example 6B) and stirred for 30 min. The obtained solutions were coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performances of the finally obtained PET films were 5 for both Example 6A and 6B, under a circumstance with a relative humidity of 90% at 5O 0 C.
  • anionic surfactant 250 mg of 10% sodium dodecyl sulphate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM-14 for Example 6A and N-300 for Example 6B) and stirred for 30 min. The obtained solutions were coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O
  • Example 8 A and 8B anionic surfactant: 250 mg of 10% Sodium N-oleoylpolypeptide aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM-14 for Example 8 A and N-300 for Example 8B) and stirred for 30 min. The obtained solutions were coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performances of the finally obtained PET films were 4 for both Example 8 A and 8B, under a circumstance with a relative humidity of 90% at 5O 0 C.
  • anionic surfactant 250 mg of 10% Sodium N-oleoylpolypeptide aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM-14 for Example 8 A and N-300 for Example 8B) and stirred for 30 min. The obtained solutions were coated on a PET surface by a 4 ⁇ m wire rod and then placed into
  • Example 9 (anionic surfactant): 250 mg of 10% dodecyl benzene sulfonic acid aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (N-300) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET film was 10 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Example 11 (anionic surfactant): 250 mg of 10% sodium dodecyl sulfonate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (N-300) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET film was 9 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Example 12 100 mg of 10% sodium 1, 4-bi(2-ethylhexyl) sulfonate aqueous solution was added into 10 g of 3% polyvinyl alcohol aqueous solution (GM- 14) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET film was 10 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Example 13 150 mg of 10% sodium 1, 4-bi(2-ethylhexyl) sulfonate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET film was 10 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Example 14 300 mg of 10% sodium 1, 4-bi(2-ethylhexyl) sulfonate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14) and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antifogging performance of the finally obtained PET film was 10 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Example 15 350 mg of 10% dodecyl benzene sulfonic acid aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14) and stirred for 30 min. The pH of the solution was about 2.5. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antisticking performance of the finally obtained PET film was 4 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Example 16 450 mg of 10% dodecyl benzene sulfonic acid aqueous solution was added into 10 g of 10% polyvinyl alcohol aqueous solution (GM- 14) and stirred for 30 min. The pH of the solution was about 2. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antisticking performance of the finally obtained PET film was 4 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • Example 17 350 mg of 10% sodium dodecyl benzene sulfonate aqueous solution was added into 1O g of 7% polyvinyl alcohol aqueous solution (GM- 14). The solution was adjusted to be a pH value of 2 by phosphoric acid and stirred for 30 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The aging antisticking performance of the finally obtained PET film was 4 under a circumstance with a relative humidity of 90% at 5O 0 C.
  • GM- 14 polyvinyl alcohol aqueous solution
  • Example 18 400 mg of 10% sodium dodecyl benzene sulfonate aqueous solution was added into 10 g of 5% N-300 aqueous solution and stirred for 30 min. The obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min. The finally obtained antifogging PET film had an aging antifogging performance of 10 and an aging antisticking performance of 6 under a relative humidity of 90% at 5O 0 C.
  • Example 19 400 mg of 10% dodecyl benzene sulfonic acid aqueous solution was added into 10 g of 5% N-300 aqueous solution and stirred for 1 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the finally obtained antifogging PET film had an aging antifogging performance of 7 and an aging antisticking performance of 10 under a relative humidity of 90% at 5O 0 C.
  • Example 20 400 mg of 10% dodecyl benzene sulfonic acid aqueous solution was added into 10 g of 5% N-300 aqueous solution and stirred for 1 min.
  • 4 g of the acidified 2326 solution was added into the aforementioned solution of N-300 and dodecyl benzene sulfonic acid and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking performances of the finally obtained antifogging PET film are both 10 under a relative humidity of 90% at 5O 0 C.
  • Example 21 400 mg of 10% dodecyl benzene sulfonic acid aqueous solution was added into 10 g of 5% N-300 aqueous solution and stirred for 1 min.
  • 4 g of the acidified 1130 solution was added into the aforementioned solution of N-300 and dodecyl benzene sulfonic acid and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking performances of the finally obtained antifogging PET film are both 10 under a relative humidity of 90% at 5O 0 C.
  • Example 22 400 mg of 10% dodecyl benzene sulfonic acid aqueous solution was added into 10 g of 5% N-300 aqueous solution and stirred for 1 min.
  • 3 g of the acidified 1030 solution was added into the aforementioned solution of N-300 and dodecyl benzene sulfonic acid and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking performances of the finally obtained antifogging PET film are both 10 under a relative humidity of 90% at 5O 0 C.
  • Example 23 400 mg of 10% sodium dodecyl benzene sulfonate aqueous solution was added into 1O g of 5% N-300 aqueous solution and stirred for 1 min.
  • a nanometer grade SiO 2 2327 origin liquid (with a particle diameter of 20 nm and a concentration of 40%) was diluted to be 5% by deionized water.
  • 2.5 g of the 5% 2327 solution was added into the aforementioned solution of N-300 and sodium dodecyl benzene sulfonate and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking results of the finally obtained antifogging PET film are both 10 under a relative humidity of 90% at 5O 0 C.
  • Example 24 400 mg of 10% sodium dodecyl benzene sulfonate aqueous solution was added into 1O g of 5% N-300 aqueous solution and stirred for 1 min.
  • a nanometer grade SiO 2 1050 origin liquid (with a particle diameter of 20 nm and a concentration of 50%) was diluted to be 5% by deionized water.
  • 2.5 g of the 5% 1050 solution was added into the aforementioned solution of N-300 and sodium dodecyl benzene sulfonate and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking results of the finally obtained antifogging PET film are both 10 under a relative humidity of 90% at 5O 0 C.
  • Example 25 400 mg of 10% sodium dodecyl benzene sulfonate aqueous solution was added into 1O g of 5% N-300 aqueous solution and stirred for 1 min.
  • a nanometer grade SiO 2 TXl 1561 origin liquid (with a particle diameter of 45 nm and a concentration of 40%) was diluted to be 5% by deionized water.
  • 2 g of the 5% TXl 1561 solution was added into the aforementioned solution of N-300 and sodium dodecyl benzene sulfonate and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking results of the finally obtained antifogging PET film are both 10 under a relative humidity of 90% at 5O 0 C.
  • Example 26 400 mg of 10 % sodium dodecyl benzene sulfonate aqueous solution was added into 10 g of 5 % N-300 aqueous solution and stirred for 1 min.
  • a nanometer grade SiO 2 1060 origin liquid (with a particle diameter of 60 nm and a concentration of 50 %) was diluted to be 5 % by deionized water.
  • 1.5 g of the 5 % 1060 solution was added into the aforementioned solution of N-300 and sodium dodecyl benzene sulfonate and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking results of the finally obtained antifogging PET film are both 10 under a relative humidity of 90 % at 5O 0 C.
  • Example 27 400 mg of 10 % sodium dodecyl benzene sulfonate aqueous solution was added into 10 g of 5 % N-300 aqueous solution and stirred for 1 min.
  • a nanometer grade SiO 2 2329 origin liquid (with a particle diameter of 75 nm and a concentration of 40 %) was diluted to be 5 % by deionized water.
  • 1 g of the 5 % 2329 solution was added into the aforementioned solution of N-300 and sodium dodecyl benzene sulfonate and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking results of the finally obtained antifogging PET film are both 10 under a relative humidity of 90 % at 5O 0 C.
  • Example 28 400 mg of 10 % sodium 1, 4-bi(2-ethylhexyl) sulfonate aqueous solution and 350mg of 10% dodecyl benzene sulfonic acid aqueous solution were added into 10 g of 7 % GM- 14 aqueous solution and stirred for 30 min.
  • the obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min.
  • the finally obtained PET film had a good aging antifogging effect, that is, had an aging antifogging performance of 10 and an aging antisticking performance of 4 under a circumstance with a relative humidity of 90 % at 5O 0 C.
  • Example 29 200 mg of 10 % sodium sec. -alkyl sulfonate aqueous solution and 250 mg of 10 % dodecyl benzene sulfonic acid aqueous solution were added into 1O g of 3 % GM-14 aqueous solution and stirred for 30 min.
  • the obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min.
  • the finally obtained PET film had an aging antifogging performance of 10 and an aging antisticking performance of 4 under a circumstance with a relative humidity of 90 % at 5O 0 C.
  • Example 30 150 mg of 10 % dodecyl benzene sulfonic acid aqueous solution were added into 10 g of 10 % N-300 aqueous solution and stirred for 1 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the finally obtained antifogging PET film had an aging antifogging performance of 10 and an aging antisticking performance of 8 under a relative humidity of 90 % at 5O 0 C.
  • Example 31 150 mg of 10 % dodecyl benzene sulfonic acid aqueous solution were added into 10 g of 10 % N-300 aqueous solution and stirred for 1 min.
  • Example 32 400 mg of 10 % dodecyl benzene sulfonic acid aqueous solution were added into 10 g of 7 % N-300 aqueous solution and stirred for 1 min.
  • 4 g of the acidified 2326 solution was added into the aforementioned solution of N-300 and dodecyl benzene sulfonic acid and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking performances of the finally obtained antifogging PET film are both 10 under a relative humidity of 90 % at 5O 0 C.
  • Example 33 600 mg of 10 % dodecyl benzene sulfonic acid aqueous solution were added into 10 g of 3 % N-300 aqueous solution and stirred for 1 min.
  • 3.6 g of the acidified 2326 solution was added into the aforementioned solution of N-300 and dodecyl benzene sulfonic acid and stirred for 30 min.
  • Example 34 400 mg of 10 % sodium dodecyl benzene sulfonate aqueous solution were added into 10 g of 10 % N-300 aqueous solution and stirred for 1 min. A nanometer grade SiO 2 2329 origin liquid (75 nm, 40 %) was diluted to be 5 % by deionized water.
  • Example 35 400 mg of 10 % sodium sec. -alkyl sulfonate aqueous solution were added into 10 g of 3 % N-300 aqueous solution and stirred for 1 min.
  • a nanometer grade SiO 2 2329 origin liquid (75 nm, 40 %) was diluted to be 5 % by deionized water.
  • 2 g of 5 % 2329 solution was added into the aforementioned solution of N-300 and sodium sec. -alkyl sulfonate and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a PET surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking results of the finally obtained PET film are both 10 under a relative humidity of 90 % at 5O 0 C.
  • Example 37 250 mg of 10 % sodium sec. -alkyl sulfonate aqueous solution and 0.1O g of 10 % tetraethyl orthosilicate solution in ethanol were added into 10 g of 5 % N-300 aqueous solution.
  • the obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 30 min.
  • the finally obtained antifogging PET film can endure 5 times of wet-rubbing without falling off.
  • the aging antifogging performance was 7 under a circumstance with a relative humidity of 90 % at 5O 0 C.
  • Example 38 250 mg of 10 % sodium sec. -aikyi sulfonate aqueous solution and 0.05 g of 10 % tetraethyl orthosilicate solution in ethanol were added into 10 g of 5 % N-300 aqueous solution.
  • the obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 30 min.
  • the finally obtained antifogging PET film can endure 3 times of wet-rubbing without falling off.
  • the aging antifogging performance was 9 under a circumstance with a relative humidity of 90 % at 5O 0 C.
  • Example 39 300 mg of 10 % sodium sec. -aikyi sulfonate aqueous solution was added into 10 g of 10 % GM- 14 aqueous solution and stirred for 30 min. The obtained solution was coated on a polycarbonate (PC) surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The finally obtained antifogging PC film has a good aging antifogging effect, that is, the aging antifogging performance was 10 under a circumstance with a relative humidity of 90 % at 5O 0 C.
  • PC polycarbonate
  • Example 40 400 mg of 10 % sodium dodecyl benzene sulfonate aqueous solution was added into 10 g of 5 % N-300 aqueous solution and stirred for 1 min.
  • a nanometer grade SiO 2 2329 origin liquid (75 nm, 40 %) was diluted to be 5 % by deionized water.
  • 1.5 g of the 5 % 2329 solution was added into the aforementioned solution of N-300 and sodium dodecyl benzene sulfonate and stirred for 30 min.
  • the obtained solution was coated by a 4 ⁇ m wire rod on a polycarbonate surface treated by 1.7 KW corona and then placed into a heating oven at 14O 0 C for 1 min.
  • the aging antifogging and antisticking results of the finally obtained PC film are both 10 under a relative humidity of 90 % at 5O 0 C.
  • Example 41 200 mg of 10 % sodium sec. -aikyi sulfonate aqueous solution was added into 10 g of 3 % GM- 14 aqueous solution and stirred for 30 min. The obtained solution was coated on a glass surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The finally obtained glass has a good aging antifogging effect, that is, the aging antifogging performance was 10 under a circumstance with a relative humidity of 90 % at 5O 0 C.
  • Example 42 150 mg of 10 % sodium sec. -aikyi sulfonate aqueous solution was added into 10 g of 5 % methylol cellulose aqueous solution and stirred for 1 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The finally obtained PET film has an aging antifogging result of 10 under a relative humidity of 90 % at 5O 0 C.
  • Example 43 400 mg of 10 % sodium sec. -alkyl sulfonate aqueous solution was added into 10 g of 10 % polyacrylic acid aqueous solution and stirred for 1 min. The obtained solution was coated on a PET surface by a 4 ⁇ m wire rod and then placed into a heating oven at 12O 0 C for 1 min. The finally obtained PET film has an aging antifogging result of 10 under a relative humidity of 90 % at 5O 0 C.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
  • Paints Or Removers (AREA)
  • Laminated Bodies (AREA)
  • Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)

Abstract

L’invention concerne une composition de revêtement antibuée qui comprend un polymère hydrophile, 0,5 à 25 % en poids d’un tensioactif anionique pour 100 % en poids du polymère, 0 à 60 % en poids de particules d’oxyde inorganique pour 100 % en poids du polymère et un solvant aqueux. Le polymère peut être la cellulose, la polyvinylpyrrolidone, l’acide polyacrylique, le polyacrylamide ou l’alcool polyvinylique. L’invention concerne également un film antibuée qui comprend un substrat et un revêtement qui est placé sur au moins une partie d’une surface sur au moins un côté du substrat et qui est fabriqué à partir de la présente composition. L’invention concerne également un article qui comprend le film, tel qu’un masque pour une opération médicale, des lunettes, un masque protecteur pour l’exploitation minière, une boîte d’emballage pour produits alimentaires ou un sac d’emballage pour produits alimentaires.
PCT/US2009/065703 2008-11-28 2009-11-24 Composition de revêtement antibuée, film antibuée et article WO2010062893A1 (fr)

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US9926458B2 (en) 2013-05-30 2018-03-27 3M Innovative Properties Company Poly(vinyl alcohol)-containing and silica nanoparticle multilayer coatings and methods
US11154735B2 (en) 2013-08-20 2021-10-26 3M Innovative Properties Company Personal respiratory protection device
US11247079B2 (en) 2013-08-20 2022-02-15 3M Innovative Properties Company Personal respiratory protection device
CN103409110A (zh) * 2013-08-20 2013-11-27 南通市通州区益君劳务有限公司 一种去污玻璃防雾剂
US11241595B2 (en) 2013-08-20 2022-02-08 3M Innovative Properties Company Personal respiratory protection device
US10639506B2 (en) 2013-08-20 2020-05-05 3M Innovative Properties Company Personal respiratory protection device
WO2018142253A1 (fr) 2017-02-03 2018-08-09 3M Innovative Properties Company Composition de revêtement protecteur pour substrats siliceux
EP3357880A1 (fr) 2017-02-03 2018-08-08 3M Innovative Properties Company Composition de revêtement de protection pour substrats siliceux
CN110904733A (zh) * 2019-12-04 2020-03-24 江苏双冠新材料科技有限公司 一种雾面pet离型纸的制备方法
CN112280447A (zh) * 2020-11-12 2021-01-29 唐波 防雾涂层组合物及其制备方法和应用
WO2023111743A1 (fr) * 2021-12-15 2023-06-22 SCG Chemicals Public Company Limited Composition de revêtement antibuée
CN115160987A (zh) * 2022-07-11 2022-10-11 国网吉林省电力有限公司电力科学研究院 一种护目镜专用防雾剂及其制备方法
CN115418144A (zh) * 2022-08-19 2022-12-02 复旦大学 超低醇解度聚乙烯醇防雾涂膜材料及其制造方法
CN115418144B (zh) * 2022-08-19 2023-10-31 复旦大学 超低醇解度聚乙烯醇防雾涂膜材料及其制造方法
CN116814126A (zh) * 2023-08-03 2023-09-29 燕山大学 一种可自愈合光催化的超亲水防雾涂层的制备方法
CN116814126B (zh) * 2023-08-03 2024-05-10 燕山大学 一种可自愈合光催化的超亲水防雾涂层的制备方法

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