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) (51) International Patent Classification: TR), OAPI (BF, BJ

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) (51) International Patent Classification: TR), OAPI (BF, BJ ) ( 1 (51) International Patent Classification: TR), OAPI (BF, BJ, CF, CG, Cl, CM, GA, GN, GQ, GW, C O- 26/02 (2006.0 1) C04B 35/46 (2006.01) KM, ML, MR, NE, SN, TD, TG). CO-IB 26/0-1 (2006.0 1) C04B 35/48 (2006.01) C04B 35/01 (2006.01) C04B 35/486 (2006.01) Declarations under Rule 4.17: C04B 35/111 (2006.01) C04B 35/50 (2006.01) — as to applicant's entitlement to apply for and be granted a C04B 35/12 (2006.01) C04B 35/626 (2006.01) patent (Rule 4.17(H)) C04B 35/14 (2006.01) C04B 35/638 (2006.01) — of inventorship (Rule 4.17(iv)) C04B 35/453 (2006.01) C04B 38/00 {2006.01) Published: (21) International Application Number: — with international search report (Art. 21(3)) PCT/EP2020/056173 (22) International Filing Date: 09 March 2020 (09.03.2020) (25) Filing Language: English (26) Publication Language: English (30) Priority Data: 62/817,192 12 March 2019 (12.03.2019) US (71) Applicant: BASF SE [DE/DE]; Carl-Bosch-Strasse 38, 67056 Ludwigshafen am Rhein (DE). (72) Inventors: FINNEGAN, Gerard; 540 White Plains Road, Tarrytown, New York 10591 (US). THOMPSON, Thomas; 540 White Plains Road, Tarrytown, New York 10591 (US). CAPOTE, Juan; 540 White Plains Road, Tar¬ rytown, New York 10591 (US). DARJI, Rupa; 540 White Plains Road, Tarrytown, New York 10591 (US). (74) Agent: BASF IP ASSOCIATION et al.; BASF SE, GBI - C006, 67056 Ludwigshafen (DE). (81) Designated States (unless otherwise indicated, for every kind of national protection available) : AE, AG, AL, AM, AO, AT, AU, AZ, BA, BB, BG, BH, BN, BR, BW, BY, BZ, CA, CH, CL, CN, CO, CR, CU, CZ, DE, DJ, DK, DM, DO, DZ, EC, EE, EG, ES, FI, GB, GD, GE, GH, GM, GT, HN, HR, HU, ID, IL, IN, IR, IS, JO, JP, KE, KG, KH, KN, KP, KR, KW, KZ, LA, LC, LK, LR, LS, LU, LY, MA, MD, ME, MG, MK, MN, MW, MX, MY, MZ, NA, NG, NI, NO, NZ, OM, PA, PE, PG, PH, PL, PT, QA, RO, RS, RU, RW, SA, SC, SD, SE, SG, SK, SL, ST, SV, SY, TH, TJ, TM, TN, TR, TT, TZ, UA, UG, US, UZ, VC, VN, WS, ZA, ZM, ZW. (84) Designated States (unless otherwise indicated, for every kind of regional protection available) : ARIPO (BW, GH, GM, KE, LR, LS, MW, MZ, NA, RW, SD, SL, ST, SZ, TZ, UG, ZM, ZW), Eurasian (AM, AZ, BY, KG, KZ, RU, TJ, TM), European (AL, AT, BE, BG, CH, CY, CZ, DE, DK, EE, ES, FI, FR, GB, GR, HR, HU, IE, IS, IT, LT, LU, LV, MC, MK, MT, NL, NO, PL, PT, RO, RS, SE, SI, SK, SM, (54) Title: SHAPED ARTIFICIAL POLYMER ARTICLES (57) Abstract: Use of porous metal oxide microspheres as light stabilizers for shaped artificial polymer articles, wherein the porous metal oxide microspheres are prepared via a process comprising forming a liquid dispersion of polymer nanoparticles and a metal oxide; forming liquid droplets of the dispersion; drying the droplets to provide polymer template microspheres comprising polymer nanospheres; and removing the polymer nanospheres from the template microspheres to provide the porous metal oxide microspheres. Shaped Artificial Polymer Articles The present invention relates to the use of specific porous metal oxide spheres (e.g., micro¬ spheres) as light stabilizers for a shaped artificial polymer article, and corresponding shaped artificial polymer articles and corresponding extruded, casted, spun, molded or calendered pol¬ ymer compositions. Certain porous metal oxide spheres have now been found to be especially efficacious towards stabilizing polymers against degradation, especially degradation induced by UV light. In addi¬ tion, it has been found that these show a synergistic effect with respect to such stabilization in combination with other UV absorbers. The present invention relates in particular to the use of porous metal oxide spheres as light sta¬ bilizers for a shaped artificial polymer article, wherein the polymer is a synthetic polymer and/or a natural or synthetic elastomer and the porous metal oxide spheres comprise a metal oxide and are prepared, e.g., by a method comprising forming a liquid dispersion of polymer particles (e.g., nanoparticles) and a metal oxide; forming liquid droplets of the dispersion; drying the liquid droplets to provide polymer templatespheres (e.g., microspheres) comprising polymer spheres (e.g., nanospheres) and metal oxide; and removing the polymer spheres from the template microspheres to provide the porous metal ox¬ ide spheres, and wherein the spheres have, e.g., an average diameter of from 0.5 pm to 100 pm, an average porosity of from 0.10 to 0.80 and an average pore diameter of from 50 nm to 999 nm. Brief Description of the Drawings The disclosure described herein is illustrated by way of example and not by way of limitation in the accompanying figures. For simplicity and clarity of illustration, features illustrated in the fig¬ ures are not necessarily drawn to scale. For example, the dimensions of some features may be exaggerated relative to other features for clarity. Further, where considered appropriate, refer¬ ence labels have been repeated among the figures to indicate corresponding or analogous ele¬ ments. Fig. 1 shows a general outline for the preparation of porous microspheres according to an em¬ bodiment of the invention. Fig. 2 is a scanning electron microscope (SEM) image of a polymer template microsphere, ac¬ cording to an embodiment of the invention. Fig. 3 is a SEM image of a porous silica microsphere, according to an embodiment of the inven¬ tion. Fig. 4 is a representation of a spray-drying process according to some embodiments of the in¬ vention. Figs. 5 to 12 show transmission curves as results of the UV measurement for the indicated ap¬ plication examples. Detailed Description Present porous metal oxide spheres, or photonic balls, may be prepared with the use of a poly¬ meric sacrificial template. In one embodiment, an aqueous colloid dispersion containing poly¬ mer particles and a metal oxide is prepared, the polymer particles typically being nano-scaled. The aqueous colloidal dispersion cab be mixed with a continuous oil phase, for instance within a microfluidic device, to produce a water-in-oil emulsion. Emulsion aqueous droplets are pre¬ pared, collected and dried to form spheres (typically microscaled) containing polymer particles and metal oxide. The polymer particles (spheres) are then removed, for instance via calcina¬ tion, to provide spherical, metal oxide particles (spheres) containing a high degree of porosity and pores that are typically nanoscaled. The spheres may contain uniform pore diameters, a result of the polymer particles being spherical and monodisperse. Fig. 1 shows a general outline for the preparation of present porous microspheres. A n emul¬ sion droplet containing polymer nanospheres and metal oxide is dried to remove solvent, providing an assembled microsphere containing polymer nanospheres with metal oxide in the interstitial spaces between the polymer nanospheres (template microsphere or “direct struc¬ ture”). The polymer nanospheres define the interstitial space. Calcination results in removal of the polymer, providing a present metal oxide microsphere with high porosity, or void volume (inverse structure). The porous metal oxide spheres are advantageously sintered, resulting in a continuous solid structure which is thermally and mechanically stable. In some embodiments, droplet formation and collection occurs within a microfluidic device. Mi¬ crofluidic devices are for instance narrow channel devices having a micron-scaled droplet junc¬ tion adapted to produce uniform size droplets connected to a collection reservoir. Microfluidic devices for example contain a droplet junction having a channel width of from about 10 pm to about 100 pm. The devices are for instance made of polydimethylsiloxane (PDMS) and may be prepared for example via soft lithography. A n emulsion may be prepared within the device via pumping an aqueous dispersed phase and oil continuous phase at specified rates to the device where mixing occurs to provide emulsion droplets. Alternatively, an oil-in-water emulsion may be employed. In some embodiments, vibrating nozzle techniques may be employed. In these techniques, a liquid dispersion is prepared, droplets are formed and are dropped into a bath of a continuous phase. The droplets are then dried followed by removal of the polymer. Vibrating nozzle equipment is available from Buchi and comprises for instance a syringe pump and a pulsation unit. Vibrating nozzle equipment may also comprise a pressure regulation valve. The polymer particles for instance have an average diameter of from about 50 nm to about 999 nm and are monodisperse. Suitable template polymers for the spheres include thermoplastic polymers. For example, tem¬ plate polymers are selected from the group consisting of poly(meth)acrylic acid, poly(meth)acrylates, polystyrenes, polyacrylamides, polyvinyl alcohol, polyvinyl acetate, polyes¬ ters, polyurethanes, polyethylene, polypropylene, polylactic acid, polyacrylonitrile, polyvinyl ethers, derivatives thereof, salts thereof, copolymers thereof and combinations thereof. For example, the polymer is selected from the group consisting of polymethyl methacrylate, poly¬ ethyl methacrylate, poly(n-butyl methacrylate), polystyrene, poly(chloro-styrene), poly(alpha- methylstyrene), poly(N-methylolacrylamide), styrene/methyl methacrylate copolymer, polyalkyl- ated acrylate, polyhydroxyl acrylate, polyamino acrylate, polycyanoacrylate, polyfluorinated acrylate, poly(N-methylolacrylamide), polyacrylic acid, polymethacrylic acid, methyl methacry¬ late/ethyl acrylate/acrylic acid copolymer, styrene/methyl methacrylate/acrylic acid copolymer, polyvinyl acetate, polyvinylpyrrolidone, polyvinylcaprolactone, polyvinylcaprolactam, derivatives thereof, salts thereof, and combinations thereof. In certain embodiments, polymer templates include polystyrenes, including polystyrene and pol¬ ystyrene copolymers. Polystyrene copolymers include copolymers with water-soluble mono¬ mers, for example polystyrene/acrylic acid, polystyrene/poly(ethylene glycol) methacrylate, and polystyrene/styrene sulfonate. Present metal oxides include oxides of transition metals, metalloids and rare earths, for exam¬ ple silica, titania, alumina, zirconia, ceria, iron oxides, zinc oxide, indium oxide, tin oxide, chro¬ mium oxide, mixed metal oxides, combinations thereof, and the like.
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