SI23900A - Dispersions based on nanocrystalline titanium (IV) oxide in crystalline form anatas for facade coating systems - Google Patents
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Abstract
Preložen izum se nanaša na sintezo disperzij na osnovi nano titanovega (IV) oksida v kristalni strukturi anatas, z ozko porazdelitvijo velikosti delcev v območju med 10 nm in 50 nm, postopek hidrolize komercialno dostopne raztopine titanilovega sulfata (TiOSO4), obarjanja netopnega hidratiziranega titanovega dioksida (Ti02.xH20.yS03) z dialkilamidnim obarjalnim reagentom, sedimentacije oborjenih hidratiziranih nanodelcev z dodatkom vodne raztopine anionskega poliakrilamidnega flokulacijskega sredstva,termične obdelave nanodelcev hidratiziranega titanovega (IV) oksida v zračni atmosferi, deaglomeracije termično obdelanega titanovega (IV) oksida v kristalni strukturi anatas v disolverju, visoko energetskega mletja v horizontalnem atritorskem cirkonijevem mlinu s fazo dezintegracije vodne suspenzije termično obdelanih nano delcev titanovega (IV) oksida v kristalni obliki anatas s cirkonijevimi krogelnimi mlevnimi telesi, tehnologijo površinske obdelave nano delcev titanovega (IV) oksida v kristalnistrukturi anatas z organskimi površinsko aktivnimi snovmi ter tehnologijo vgradnje površinsko obdelanih nano delcev titanovega (IV) oksida v kristalni strukturi anatas v organske nosilne medije, ki zagotavljajo stabilnost končnega disperzijskega sistema v območju pH vrednosti med 5 in 9 in zeta potencialom manjšim od - 30 eV ter pod vplivom UV-svetlobe sprožijo redukcijsko ciklične površinsko aktivne procese in mineralizacijo organskih polutantov pri fotokatalitičnem odstranjevanju nečistoč inmikroorganizmov v fasadnih premaznih sistemih.The present invention relates to the synthesis of nano titanium (IV) oxide dispersions in crystalline structure of anatases, with a narrow particle size distribution in the range of 10 nm to 50 nm, a hydrolysis process of commercially available titanium sulfate solution (TiOSO4), precipitation of insoluble hydrated titanium dioxide (Ti02.xH20.yS03) with dialkylamide precipitation reagent, sedimentation of precipitated hydrated nanoparticles by addition of aqueous solution of an anionic polyacrylamide flocculation agent, thermal treatment of nanoparticles of hydrated titanium (IV) oxide in an air atmosphere, deagglomeration of thermally treated titanium (IV) oxide in the crystal structure of anatases in a dysolver, high-energy grinding in a horizontal atritor zircon mill with the phase of disintegration of the aqueous suspension of thermally treated nanoparticles of titanium (IV) oxide in crystalline form, anatases with zirconium ball milling bodies, surface treatment of nanoparticles of titanium (IV) oxides in crystalline structure of anatases with organic surfactants and the technology of incorporation of surface-treated nanoparticles of titanium (IV) oxide in crystalline structure of anatases into organic carrier media that ensure the stability of the final dispersion system in the range of pH values between 5 and 9 and zeta potential less than - 30 eV and under the influence of UV light trigger reduction cyclic surface active processes and mineralization of organic pollutants in the photocatalytic removal of impurities of inorganic organisms in façade coating systems.
Description
DISPERZIJE NA OSNOVI NANOKRISTALINIČNEGA TITANOVEGA (IV) OKSIDA V KRISTALNI OBLIKI ANATAS ZA FASADNE PREMAZNE SISTEMEDISPERSIONS ON THE BASIS OF NANOCRYSTALINIC TITANIUM (IV) OXIDE IN ANATAS CRYSTAL FORM FOR COATING COATING SYSTEMS
Predmet izuma je sinteza disperzij na osnovi nanokristaliničnega titanovega (IV) oksida v kristalni obliki anatas, s povprečno velikostjo delcev v območju med 10 nm in 50 nm, ki zaradi visoke oksidacij ske sposobnosti, hidrofilnosti in kemijske obstojnosti pod vplivom UV-svetlobe sproži redukcijsko ciklične površinsko aktivne procese ter mineralizacijo organskih polutantov pri fotokatalitičnem odstranjevanju nečistoč in mikroorganizmov v fasadnih premaznih sistemih.The subject of the invention is the synthesis of nanocrystalline titanium (IV) oxide dispersions in anatas crystalline form, with an average particle size in the range of 10 nm to 50 nm, which, due to its high oxidation ability, hydrophilicity and chemical stability, under the influence of UV light surface active processes and mineralization of organic pollutants in photocatalytic removal of impurities and microorganisms in facade coating systems.
Uporabne lastnosti nanokristaliničnega titanovega (IV) oksida v kristalni obliki anatsa, izvirajo iz njegove fotokatalitske sposobnosti zaščite materialov pred svetlobnimi in vremenskimi vplivi ter so v osnovi določene z velikostjo in obliko nanodelcev, kristalno strukturo in kemijsko sestavo ter prilagojene pogojem uporabe za fasadne premazne sisteme.The useful properties of crystalline titanium (IV) oxide nanocrystalline oxide originate from its photocatalytic ability to protect materials from light and weather, and are fundamentally determined by the size and shape of the nanoparticles, crystal structure and chemical composition and adapted to the conditions of use for facade coating systems.
Učinkovita izraba lastnosti nanokristaliničnega titanovega (IV) oksida v kristalni strukturi anatas je mogoča zaradi prilagojenih pogojev postopka izdelave ter načina in pogojev dispergiranja nanodelcev v stabilne disperzijske sisteme.The efficient utilization of the properties of nanocrystalline titanium (IV) oxide in the crystalline structure of anatas is possible due to the adapted conditions of the manufacturing process and the manner and conditions of dispersing the nanoparticles in stable dispersion systems.
Po standardni patentni klasifikaciji sodi izum v 01. razred - kemični proizvodi za industrijo in znanost.According to the standard patent classification, the invention belongs to the 1st class - chemical products for industry and science.
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Tehnični problem, ki ga omenjeni izum rešuje, je sinteza disperzij na osnovi nanokristaliničnega titanovega (IV) oksida v kristalni obliki anatas, ki vključuje postopek hidrolize komercialno dostopne 12 % - 15 % raztopine titanilovega sulfata (T1OSO4), z gostoto 1,4 g/ml in pH vrednostjo < 1, obarjanja netopnega hidratiziranega titanovega dioksida (TiO2'xH2O‘ySO3) z dialkilamidnim obarjalnim reagentom v koncentracijskem območju od 5,0 mol/l do 12,0 mol/l,, sedimentacijo oborjenih hidratiziranih nanodelcev z dodatkom vodne raztopine anionskega poliakrilamidnega flokulacij skega sredstva v koncentracijskem območju med 0,01 ut.% in 0,5 ut.%, ter procesne parametre obarjanja hidratiziranega titanovega (IV) oksida v temperaturnem območju (100 ± 2)°C, časa zadrževanja na maksimalni temperaturi od 1 do 5 ur, termične obdelave nanodelcev hidratiziranega titanovega (IV) oksida v zračni atmosferi v temperaturnem območju med 500°C in 1000°C, z 1 do 3 urnim zadrževanjem na maksimalni temperaturi, deaglomeracijo termično obdelanega titanovega (IV) oksida v kristalni strukturi anatas v masnem razmerju demineralizirana voda: nano delci titanovega (IV) oksida v kristalni strukturi anatas 1:1 v disolverju, v časovnem območju od 30 minut do 120 minut, visoko energetskega mletja v horizontalnem atritorskem cirkonijevem mlinu s fazo dezintegracije termično obdelanih nano delcev titanovega (IV) oksida v kristalni obliki anatas v območju od 0,5 ure do 6 ur pri pH vrednosti v območju med 6,0 in 11,5 s cirkonijevimi krogelnimi mlevnimi telesi dimenzije v območju Φ = 2 mm do 6 mm, fazo površinske obdelave nano delcev titanovega (IV) oksida z organskimi površinsko aktivnimi snovmi v razmerju suha snov/organska komponenta 1:0,04-0,2 ter fazo vgradnje površinsko obdelanih nano delcev titanovega (IV) oksida v kristalni strukturi anatas v organski nosilni medij v masnem razmerju, površinsko obdelani nano delci/organski nosilni medij 1:10-15 v disolverju, v območju od 60 minut doA technical problem to be solved by the present invention is the synthesis of nanocrystalline titanium (IV) oxide dispersions in anatas crystalline form, which involves the hydrolysis process of a commercially available 12% - 15% solution of titanyl sulfate (T1OSO4), with a density of 1.4 g / ml and pH <1, precipitation of insoluble hydrated titanium dioxide (TiO2'xH 2 O'ySO3) with dialkylamide precipitation reagent in a concentration range from 5.0 mol / l to 12.0 mol / l ,, sedimentation of precipitated hydrated nanoparticles with the addition of aqueous solutions of the anionic polyacrylamide flocculation agent in a concentration range between 0.01 wt% and 0.5 wt%, and the process parameters for precipitation of hydrated titanium (IV) oxide in the temperature range (100 ± 2) ° C, holding time at maximum temperature from 1 to 5 hours, thermal treatment of hydrated titanium (IV) oxide nanoparticles in an air atmosphere in the temperature range between 500 ° C and 1000 ° C, with a maximum holding time of 1 to 3 hours low temperature, deagglomeration of thermally treated titanium (IV) oxide in anatas crystalline structure by mass demineralized water: nano particles of titanium (IV) oxide in anatas crystal structure 1: 1 in disolver, in the time range from 30 minutes to 120 minutes, high energy grinding in a horizontal zirconia grinder with the disintegration phase of thermally treated nano-particles of titanium (IV) oxide in anatas crystalline form in the range of 0.5 hours to 6 hours at a pH in the range of 6.0 to 11.5 with zirconium ball mills dimensions in the range Φ = 2 mm to 6 mm, the surface treatment of titanium (IV) oxide nano-particles with organic surfactants in a dry matter / organic component ratio of 1: 0.04-0.2 and the incorporation phase of surface-treated nano-particles of titanium (IV) oxides in the crystal structure of anatas to organic carrier medium by mass ratio, surface treated nano particles / organic carrier medium 1: 10-15 in disolver, in the range from 60 minutes to
180 minut, pri pH vrednosti 7 ter v visoko energetskem atritorskem cirkonijevem mlinu s cirkonijevimi krogelnimi mlevnimi telesi dimenzije v območju Φ = 2 mm do 6 mm, časa homogenizacije v območju od 0,5 ure do 6 ur, pri pH vrednosti v območju od 5 do 9, ki zagotavljajo stabilnost končnega disperzij skega sistema v območju pH vrednosti med 5 in 9 in zeta potencialom manjšim od - 30 eV.180 minutes, at pH 7 and in a high-energy zirconia grinder with zirconia ball mills with dimensions in the range of Φ = 2 mm to 6 mm, homogenization time in the range of 0.5 hours to 6 hours, at a pH in the range of 5 to 9, providing stability of the final dispersion system in the pH range between 5 and 9 and a zeta potential of less than - 30 eV.
Način in pogoji priprave nanokristaliničnega titanovega (IV) oksida v kristalni obliki anatas v veliki meri določajo končne uporabne lastnosti, ki so odvisne od oblike in velikosti, kristalne strukture in kemijske sestave. Razvoj na področju sinteze nanokristaliničnega titanovega (IV) oksida, se usmerja v tehnologije priprave sferičnih nanodelcev z visoko specifično površino in ozko porazdelitvijo velikosti.The method and conditions for the preparation of nanocrystalline titanium (IV) oxide in the crystalline form of anatas largely determine the end-use properties, which depend on the shape and size, crystal structure and chemical composition. Development in the field of synthesis of nanocrystalline titanium (IV) oxide is focused on technologies for the preparation of spherical nanoparticles with a high specific surface area and a narrow size distribution.
Po doslej znanih literatumih podatkih, poteka priprava titanovega (IV) oksida v svetu v dveh glavnih komercialnih oblikah. Starejša in količinsko bistvena je proizvodnja mikronskega pigmenta, medtem ko je proizvodnja ultrafinega oziroma nano pigmenta predmet intenzivnih razvojnih raziskav.According to the literature so far, titanium (IV) oxide is being prepared worldwide in two major commercial forms. The production of micron pigment is of older and quantitative importance, while the production of ultrafine or nano pigment is the subject of intensive developmental research.
Priprava mikronskega pigmentnega titanovega (IV) oksida v kristalni obliki anatas, poteka po komercialno najbolj uveljavljenem sulfatnem in kloridnem postopku. Sulfatni postopek priprave titanovega (IV) oksida se prične z razklopom rud, obogatenih s titanom, z žvepleno (VI) kislino. Nastane titanilov sulfat (TiOSO4), ki se večstopenjsko čisti in hidrolizira, da se dobi hidratiziran gel, ki se mu pred fazo kalcinacije dodajo ustrezne snovi za usmerjeno rast kristalov v želeno kristalno obliko (anatas, rutil). Sledi postopek površinske obdelave primarnih delcev titanovega (IV) oksida, da se izboljšajo končne pigmentne lastnosti. Kloridni postopek, kije novejši in zahtevnejši od sulfatnega, temelji na kloriranju ustreznih, s titanom obogatenih surovin, v temperaturnem območju med 700 °C in 1200 °C. Nastane titanov tetraklorid (TiCl4), ki ga po fazi čiščenja z neposredno oksidacijo v temperaturnem območju med 900 °C in 1400 °C v kisikovi atmosferi ali s postopkom termične hidrolize, prevedejo v titanov (IV) oksid v kristalno strukturo rutil.The preparation of micron pigment titanium (IV) oxide in the crystalline form of anatas is carried out by the most commercially available sulfate and chloride process. The sulfate process for the preparation of titanium (IV) oxide begins with the decomposition of titanium-enriched ores with sulfuric acid. Titanyl sulphate (TiOSO 4 ) is formed, which is purified and hydrolyzed in several stages to give a hydrated gel, which is added to the desired crystalline form (anatas, rutile) prior to the calcination phase. The process of surface treatment of primary titanium (IV) oxide particles is followed to improve the final pigment properties. The chloride process, which is newer and more demanding than sulfate, is based on the chlorination of suitable titanium-enriched feedstocks in the temperature range between 700 ° C and 1200 ° C. Titanium tetrachloride (TiCl 4 ) is formed which, after the purification step, is converted into titanium (IV) oxide into the crystalline structure of rutile by direct oxidation in the temperature range between 900 ° C and 1400 ° C in an oxygen atmosphere or by thermal hydrolysis.
Skupno obema postopkoma je nastanek odpadnih stranskih produktov, kar zahteva ustrezno deponiranje, pojavljajo se problemi visokih temperatur, korozije in toksičnosti, zaradi česar sta lahko postopka tudi ekološko sporna in ne omogočata priprave titanovega (IV) oksida v obliki nanodelcev, zahtevane oblike, velikosti in porazdelitve velikosti.Common to both processes is the generation of waste by-products, which requires proper disposal, high temperature, corrosion and toxicity problems, which can also be environmentally controversial and do not allow the preparation of titanium (IV) oxide in the form of nanoparticles, the required shape, size, and size distributions.
V primerjavi z doslej znanimi postopki priprave disperzij na osnovi nanokristaliničnega titanovega (IV) oksida v kristalni obliki anatas, se predmet izuma od njih razlikuje v postopku priprave nanodelcev hidratiziranega titanovega dioksida (TiO2xH2OySO3), visoko-temperatumi termični obdelavi hidratiziranega titanovega (IV) oksida, načinu in pogojih homogeniziranja in mletja termično obdelanega nanokristaliničnega titanovega (IV) oksida v kristalni strukturi anatas, površinski obdelavi z organskimi površinsko aktivnimi snovmi in vgradnja površinsko obdelanih nano delcev titanovega (IV) oksida v kristalni strukturi anatas v organske nosilne medije, kar vpliva na končne fizikalnokemijske lastnosti nanokristaliničnega titanovega (IV) oksida v kristalni strukturi anatas ter zagotavljajo stabilnost končnih disperzij za fasadne premazne sisteme.Compared with the known methods of preparing dispersions based on nanocrystalline titanium (IV) oxide in anatas crystalline form, the object of the invention differs from them in the process of preparing nanoparticles of hydrated titanium dioxide (TiO 2 xH 2 OySO3), high temperature thermal treatment of hydrated titanium IV) oxide, mode and conditions of homogenization and milling of thermally treated nanocrystalline titanium (IV) oxide in anatas crystalline structure, surface treatment with organic surfactants and incorporation of surface treated nano particles of titanium (IV) oxide in anatas crystalline structure into organic carrier media which affects the final physicochemical properties of nanocrystalline titanium (IV) oxide in the crystal structure of anatas and provide stability of the final dispersions for the facade coating systems.
Izum se nanaša na uporabljene vhodne surovine in kemijsko sestavo, tehnologijo termične obdelave hidratiziranega nano titanovega dioksida, tehnologijo deaglomeriranja termično obdelanega nano titanovega (IV) oksida v kristalni obliki • · anatas v disolverju ter visoko energetskem horizontalnem atritorskem cirkonijevem mlinu, z uporabo cirkonijevih krogelnih mlevnih teles, tehnologijo površinske obdelave nano delcev titanovega (IV) oksida v kristalni obliki anatas z različnimi organskimi površinsko aktivnimi snovmi ter tehnologijo vgradnje površinsko obdelanih nano delcev titanovega (IV) oksida v kristalni obliki anatas v organske nosilne medije, kar zagotavlja stabilnost končnega disperzijskega sistema v območju pH vrednosti med 5 in 9 in zeta potencialom manjšim kot - 30 e V.The invention relates to the input materials used and the chemical composition, technology of heat treatment of hydrated nano titanium dioxide, technology of deagglomeration of thermally treated nano titanium (IV) oxide in crystalline form. bodies, the technology of surface treatment of titanium (IV) oxide nanoparticles in anatas crystalline form with various organic surfactants, and the technology of incorporation of surface treated nano particle titanium (IV) oxide in crystalline anatas into organic carrier media, which ensures the stability of the final dispersion system in pH range between 5 and 9 and zeta potential less than - 30 e V.
Po izumu je naloga rešena z izdelavo disperznij na osnovi nanokristaliničnega titanovega (IV) oksida v kristalni obliki anatas, iz:According to the invention, the problem is solved by the production of dispersions based on nanocrystalline titanium (IV) oxide in crystalline anatas form, from:
• 12 - 15 % raztopine titanilovega sulfata (TiOSO4), z gostoto 1,4 g/ml in pH vrednostjo < 1.• 12-15% titanium sulphate solution (TiOSO 4 ), with a density of 1.4 g / ml and a pH value of <1.
• Vodne raztopine dialkilamida kot obarjalni reagent v koncentracijskem območju med 5,0 mol/1 in 12,0 mol/1.• Aqueous dialkylamide solutions as a precipitating reagent in a concentration range between 5.0 mol / l and 12.0 mol / l.
• Vodne raztopine anionskega poliakrilamidnega flokulacij skega sredstva v koncentracijskem območju med 0,01 ut% in 0,5 ut%.• Aqueous solutions of the anionic polyacrylamide flocculation agent in a concentration range between 0.01 wt% and 0.5 wt%.
• Organskih površinsko aktivnih snovi na osnovi natrijevega poliakrilata in etanolamina v koncentracijskem območju med 1 ut% in 10 ut% • Organskega nosilnega medija na osnovi vodne raztopine polisiloksana v koncentacijskem območju med 50 ut% in 90 ut % • Procesnih parametrov postopka obarjanja hidratiziranega titanovega (IV) oksida v temperaturnem območju (100 ± 2) °C ter 1 do 5 urnega zadrževanja na maksimalni temperaturi, termične obdelave hidratiziranega titanovega (IV) oksida v temperaturnem območju med 400 °C in 1000 °C v zračni atmosferi ter 1 do 3 urnem zadrževanjem na maksimalni temperaturi, deaglomeracije termično obdelanega titanovega (IV) oksida v kristalni• Organic surfactants based on sodium polyacrylate and ethanolamine in a concentration range between 1 wt% and 10 wt% • Organic carrier medium based on aqueous polysiloxane solution in a concentration range between 50 wt% and 90 wt% • Process parameters of the process of precipitation of hydrated titanium ( IV) oxide in the temperature range (100 ± 2) ° C and 1 to 5 hours maximum temperature retention, thermal treatment of hydrated titanium (IV) oxide in the temperature range between 400 ° C and 1000 ° C in air atmosphere and 1 to 3 hours holding at maximum temperature, deagglomeration of thermally treated titanium (IV) oxide in crystalline
strukturi anatas v masnem razmerju demineralizirana voda: nano delci titanovega (IV) oksida v kristalni strukturi anatas 1:1 v disolverju, v časovnem območju od 30 minut do 120 minut, visoko energetskega mletja v horizontalnem atritorskem cirkonijevem mlinu s fazo dezintegracije vodne suspenzije termično obdelanih nano delcev titanovega (IV) oksida v kristalni obliki anatas v območju od 30 minut do 6 ur pri pH vrednosti v območju med 6,0 in 11,5 s cirkonijevimi krogelnimi mlevnimi telesi dimenzije v območju Φ = 2 mm do 6 mm, fazo površinske obdelave nano delcev titanovega (IV) oksida v kristalni obliki anatas z organskimi površinsko aktivnimi snovmi na osnovi natrijevega poliakrilata in etanolamina v razmerju suha snov: organska komponenta 1: 0,04 - 0,2 ter fazo vgradnje površinsko obdelanih nano delcev titanovega (IV) oksida v kristalni strukturi anatas v organski nosilni medij na osnovi vodne raztopine polisiloksana v razmerju površinsko obdelani nano delci titanovega (IV) oksida v kristalni strukturi anatas : organska komponenta 1: 10-15 v disolverju v območju med 60 minut in 180 minut pri pH vrednosti 7 in visokoenergetskem horizontalnem atritorskem cirkonijevem mlinu s cirkonijevimi krogelnimi mlevnimi telesi dimenzije v območju Φ = 2 mm do 6 mm, časa homogenizacije v območju med 30 minut do 6 ur, pri pH vrednosti v območju od 5 do 9.Anatas structure by weight demineralised water: Nano particles of titanium (IV) oxide in anatas 1: 1 crystal structure in a disolver, in the time range from 30 minutes to 120 minutes, high-energy grinding in a horizontal zirconia grinder with the disintegration phase of the aqueous suspension of heat treated nano-particles of titanium (IV) oxide in anatas crystalline form in the range of 30 minutes to 6 hours at a pH in the range of 6.0 to 11.5 with zirconium ball mills with dimensions in the range of Φ = 2 mm to 6 mm, surface phase of the treatment of anatas crystalline titanium (IV) oxide nanoparticles with organic surfactants based on sodium polyacrylate and ethanolamine in the dry matter ratio: organic component 1: 0.04 - 0.2 and the incorporation of titanium (IV) surface-treated nano particles of oxide in the crystal structure of anatas into an organic carrier medium based on an aqueous solution of polysiloxane in the ratio of surface treated nano particles of titanium (IV) oxide in anatas crystalline structure: organic component 1: 10-15 in disolver in the range of 60 minutes to 180 minutes at pH 7 and high-energy horizontal zirconia grinder with zirconia ball mills with dimensions in the range Φ = 2 mm to 6 mm, time homogenization in the range of 30 minutes to 6 hours, with a pH in the range of 5 to 9.
Natančna razmerja posameznih komponent ter pripadajoči procesni parametri sinteze so navedeni v izvedbenih primerih.The exact proportions of the individual components and the corresponding process parameters of the synthesis are given in the embodiments.
IZVEDBENI PRIMER 1EXAMPLE 1
V reakcijsko posodo, opremljeno z mešalom, odmerimo 245 litrov 10 - 12 %Weigh 245 liters of 10 - 12% in a reaction vessel equipped with a mixer
Ί raztopine titanilovega sulfata (T1OSO4), z gostoto 1,4 g/ml in pH vrednostjo < 1, 490 litrov demineralizirane vode ter 265 litrov 11,04 molame vodne raztopine obarjalnega reagenta dialkilamida. Sinteza poteka 120 minut pri konstantni temperaturi (100 ± 2) °C in hitrosti mešanja 150 vrt./minuto. Po zaključku sinteze oborjene delce hidratiziranega titanovega (IV) oksida (TiO2xH2OySO3) sedimentiramo z dodatkom 0,1 vol % 0,33 % vodne raztopine anionskega poliakriamidnega flokulanta in filtrat ločimo z dekantiranjem. Sediment nanodelcev hidratiziranega titanovega (IV) oksida, ki vsebuje cca 50 % vlage termično obdelamo pri temperaturi 600 °C v zračni atmosferi z zadrževalnim časom 2 uri na maksimalni temperaturi, da se formira kristalna struktura anatas.Tit titanyl sulphate solution (T1OSO4), with a density of 1.4 g / ml and a pH value of <1.490 liters of demineralized water and 265 liters of 11.04 molar aqueous solution of the dialkylamide precipitation reagent. Synthesis is carried out for 120 minutes at a constant temperature (100 ± 2) ° C and a stirring speed of 150 rpm. Upon completion of the synthesis, the precipitated particles of hydrated titanium (IV) oxide (TiO 2 xH2OySO3) were sedimented with 0.1 vol% 0.33% aqueous anionic polyacriamide flocculant and the filtrate was separated by decantation. The sediment of the nanoparticles of hydrated titanium (IV) oxide containing approximately 50% moisture is thermally treated at 600 ° C in an air atmosphere with a holding time of 2 hours at maximum temperature to form the crystalline structure of anatas.
Termično obdelane nano delce titanovega (IV) oksida v kristalni obliki anatas v prvi fazi deaglomeriramo v disolverju. Disolver med mešanjem s 500 obrati/ min napolnimo z demineralizirano vodo ter termično obdelanimi nanodelci titanovega (IV) oksida v kristalni strukturi anatas v masnem razmerju demineralizirana voda: termično obdelani nanodelci titanovega (IV) oksida v kristalni strukturi anatas 1:1. Po končanem doziranju zvišamo obrate mešalnika disolverja na 1000 obratov/ min. Dispergiramo 60 minut pri pH =7. Disperziji dodamo 2,6 ut.% vodne raztopine natrijevega poliakrilata ter s hitrostjo 1000 obratov/ min dispergiramo še 60 minut. Disperzijo prečrpamo v visokoenergetski horizontalni atritorski cirkonijev mlin ter v prvi fazi deaglomeriramo z uporabo cirkonijevih krogelnih mlevnih teles velikosti Φ = 5 mm pri mlevskem razmerju: 1 masni delež disperzije nanodelcev titanovega (IV) oksida v kristalni strukturi anatas ter 0,5 masnega deleža cirkonijevih krogelnih mlevnih teles dimenzije Φ = 5 mm s hitrostjo črpalke 35 obratov minuto ter hitrostjo mešala 400 obratov na minuto. Med fazo mletja vzdržujemo pH vrednost v območju med 6,5 in 7,5 (pH vrednost uravnavamo z dodatkom NH4OH) ter meljemo 1 uro do končne stabilne disperzije nano titanovega (IV) oksida v kristalni anatas.The thermally treated nano particles of titanium (IV) oxide in the crystalline anatas form are deagglomerated in a disolver in the first phase. The disolver is filled with demineralised water and thermally treated titanium (IV) oxide nanoparticles in anatas crystalline structure in a mass ratio of anatas in a mass ratio of dematerialized water: thermally treated titanium (IV) oxide nanoparticles in anatas crystalline structure during mixing at 500 rpm. After dosing is completed, the revolutions of the disolver mixer are increased to 1000 rpm. Disperse for 60 minutes at pH = 7. 2.6 wt% aqueous polyacrylate solution was added to the dispersion and dispersed at a speed of 1000 rpm for another 60 minutes. The dispersion is pumped into a high-energy horizontal zirconia grinder and in the first phase is deagglomerated using zirconium ball mills of size Φ = 5 mm at a grinding ratio: 1 particle dispersion of titanium (IV) oxide nanoparticles in the crystal structure of anatas and 0.5 mass fraction of zirconia grinding bodies of dimension Φ = 5 mm at a pump speed of 35 rpm and a mixer speed of 400 rpm. During the milling phase, the pH was maintained in the range of 6.5 to 7.5 (pH adjusted by the addition of NH4OH) and milled for 1 hour to the final stable dispersion of nano titanium (IV) oxide in crystalline anatase.
Nanodelce titanovega (IV) oksida v kristalni obliki anatas karakteriziramo z rentgensko praškovno difrakcijo (XRD), določimo specifično površino in velikost delcev z metodo BET, pH vrednost in zeta potencial.The anatase crystalline titanium (IV) oxide nanoparticles are characterized by X-ray powder diffraction (XRD), the specific surface area and particle size are determined by the BET method, pH value and zeta potential.
Po izumu je problem rešen z določitvijo fazne sestave z rentgensko praškovno diffakcijo (XRD), specifično površino delcev (ABet) in velikostjo delcev (DBet) z metodo BET, pH vrednostjo in zeta potencialom stabilne disperzije nano titanovega (IV) oksida v kristalni obliki anatas.According to the invention, the problem is solved by determining the phase composition by X-ray powder diffraction (XRD), specific particle surface (A B et) and particle size (D B et) by the BET method, pH value and zeta potential of stable dispersion of nano titanium (IV) oxide in the crystalline form of anatas.
IZVEDBENI PRIMER 2EXAMPLE 2
V reakcijsko posodo, opremljeno z mešalom, odmerimo 245 litrov 10 - 12 % raztopine titanilovega sulfata (TiOSCf), z gostoto 1,4 g/ml in pH vrednostjo < 1, 490 litrov demineralizirane vode ter 265 litrov 11,04 molame vodne raztopine obarj alnega reagenta dialkilamida. Sinteza poteka 120 minut pri konstantni temperaturi (100 ± 2) °C in hitrosti mešanja 150 vrt./minuto. Po zaključku sinteze oborjene delce hidratiziranega titanovega (IV) oksida (ΤίΟ2·χΗ2Ο·γ8θ3) sedimentiramo z dodatkom 0,1 vol % 0,33 % vodne raztopine anionskega poliakriamidnega flokulanta in filtrat ločimo z dekantiranjem. Sediment nanodelcev hidratiziranega titanovega (IV) oksida, ki vsebuje cca 50 % vlage termično obdelamo pri temperaturi 600 °C v zračni atmosferi z zadrževalnim časom 2 uri na maksimalni temperaturi, da se formira kristalna oblika anatas. Vodno raztopino organskega nosilnega medija na osnovi polisiloksana in termično obdelane nanodelce titanovega (IV) oksida v kristalni obliki anatas z masnim razmerjem vodna raztopina organskega nosilnega medija : termično obdelani nanodelci titanovega (IV) oksida v kristalni strukturi anatas 1: 0,087 doziramo v pretočni homogenizator visokoenergetskega horizontalnega atritorskega cirkonijevega mlina, ki ima 50 % volumna mlevne posode napolnjenene s cirkonijevimi krogelnimi mlevnimi telesi velikosti Φ = 5 mm ter z nastavitvijo hitrosti črpalke na 30 obratov na minuto in mešala v mlevni posodi na 400 obratov na minuto, homogeniziramo 10 minut. Nato dodamo 0,9 ut. % etanoiamina preračunano na količino uporabljene vodne raztopine organskega nosilnega medija na osnovi polisiloksana ter homogeniziramo 30 minut do končne stabilne disperzije nano titanovega (IV) oksida v kristalni anatas. Med fazo mletja vzdržujemo pH vrednost v območju med 7,5 in 8,5 (pH vrednost uravnavamo z dodatkom NH4OH).Pour 245 liters of 10-12% titanium sulphate solution (TiOSCf), with a density of 1.4 g / ml and a pH of <1, 490 liters of demineralized water and 265 liters of 11.04 molar precipitate aqueous solution into the reaction vessel equipped with the agitator. dialkylamide reagent. Synthesis is carried out for 120 minutes at a constant temperature (100 ± 2) ° C and a stirring speed of 150 rpm. After synthesis, the precipitated particles of hydrated titanium (IV) oxide (ΤίΟ 2 · χΗ 2 Ο · γ8θ3) were sedimented with the addition of 0.1 vol% 0.33% aqueous anionic polyacriamide flocculant and the filtrate was separated by decantation. The sediment of the nanoparticles of hydrated titanium (IV) oxide containing approximately 50% moisture is thermally treated at 600 ° C in an air atmosphere with a holding time of 2 hours at maximum temperature to form anatas crystalline form. Polysiloxane-based aqueous solution of organic carrier medium and thermally treated titanium (IV) oxide nanoparticles in anatas crystalline form by weight aqueous solution of organic carrier medium: Titanium (IV) oxide nanoparticles in anatase crystal structure 1: 0.087 are dosed in a high-energy homogenizer a horizontal zirconia grinder having 50% of the volume of a grinding vessel filled with zirconia ball bodies of size velikosti = 5 mm and adjusting the pump speed to 30 rpm and stirring in a grinding vessel to 400 rpm is homogenized for 10 minutes. Then 0.9 wt. % ethanoiamine calculated on the amount of aqueous solution of the polysiloxane-based organic carrier medium used and homogenized for 30 minutes until the final stable dispersion of nano titanium (IV) oxide in crystalline anatase. During the milling phase, the pH is maintained in the range of 7.5 to 8.5 (pH is adjusted by the addition of NH4OH).
Nanodelce titanovega (IV) oksida v kristalni obliki anatas pred izdelavo disperzije karakteriziramo z rentgensko praškovno difrakcijo (XRD) in določimo specifično površino in velikost delcev z metodo BET.Titanium (IV) oxide nanoparticles in anatas crystalline form were characterized by X-ray powder diffraction (XRD) prior to dispersion and the specific surface area and particle size were determined by the BET method.
Po izumu je problem rešen z določitvijo fazne sestave z rentgensko praškovno difrakcijo (XRD), specifično površino delcev (ABet) in velikostjo delcev (Dret) z metodo BET.According to the invention, the problem is solved by determining the phase composition by X-ray powder diffraction (XRD), specific particle surface (A B et) and particle size (Dret) by the BET method.
Andrei/ŽnidaršiČ^Andrei / ŽnidaršiČ ^
Nevenka RajnarNevenka Reinar
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