CZ300800B6 - Process for preparing transparent photocatalytically active particles of titanium dioxide - Google Patents
Process for preparing transparent photocatalytically active particles of titanium dioxide Download PDFInfo
- Publication number
- CZ300800B6 CZ300800B6 CZ20060270A CZ2006270A CZ300800B6 CZ 300800 B6 CZ300800 B6 CZ 300800B6 CZ 20060270 A CZ20060270 A CZ 20060270A CZ 2006270 A CZ2006270 A CZ 2006270A CZ 300800 B6 CZ300800 B6 CZ 300800B6
- Authority
- CZ
- Czechia
- Prior art keywords
- titanium
- solution
- titanium dioxide
- photocatalytically active
- active particles
- Prior art date
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000002245 particle Substances 0.000 title claims abstract description 20
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title abstract description 4
- 150000003608 titanium Chemical class 0.000 claims abstract description 7
- 238000000034 method Methods 0.000 claims description 12
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical group Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims description 7
- 229920002338 polyhydroxyethylmethacrylate Polymers 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 4
- 238000006460 hydrolysis reaction Methods 0.000 claims description 4
- XFVGXQSSXWIWIO-UHFFFAOYSA-N chloro hypochlorite;titanium Chemical group [Ti].ClOCl XFVGXQSSXWIWIO-UHFFFAOYSA-N 0.000 claims description 3
- 239000012266 salt solution Substances 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 abstract description 5
- 229920002818 (Hydroxyethyl)methacrylate Polymers 0.000 abstract 2
- WOBHKFSMXKNTIM-UHFFFAOYSA-N Hydroxyethyl methacrylate Chemical compound CC(=C)C(=O)OCCO WOBHKFSMXKNTIM-UHFFFAOYSA-N 0.000 abstract 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract 1
- RCJVRSBWZCNNQT-UHFFFAOYSA-N dichloridooxygen Chemical compound ClOCl RCJVRSBWZCNNQT-UHFFFAOYSA-N 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 3
- 239000003973 paint Substances 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 2
- 101150106083 hemA1 gene Proteins 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 239000011541 reaction mixture Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- -1 titanium alkoxides Chemical class 0.000 description 2
- 101150007870 HEMA3 gene Proteins 0.000 description 1
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 235000005811 Viola adunca Nutrition 0.000 description 1
- 240000009038 Viola odorata Species 0.000 description 1
- 235000013487 Viola odorata Nutrition 0.000 description 1
- 235000002254 Viola papilionacea Nutrition 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 101150072032 hemA2 gene Proteins 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 239000004922 lacquer Substances 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000001038 titanium pigment Substances 0.000 description 1
- 238000001238 wet grinding Methods 0.000 description 1
Landscapes
- Catalysts (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Paints Or Removers (AREA)
Abstract
Description
Způsob výroby transparentních fotokatalyticky aktivních částic oxidu titaničítéhoProcess for the production of transparent photocatalytically active titanium dioxide particles
Oblast technikyTechnical field
Vynález se týká způsobu výroby transparentních fotokatalyticky aktivních částic oxidu titaničitého.The invention relates to a process for the production of transparent photocatalytically active titanium dioxide particles.
io Dosavadní stav technikyBACKGROUND OF THE INVENTION
Transparentní částice oxidů kovů mají využití v mnoha oborech, např. jako pigmenty v připraví nátěrových hmot, v kosmetice jako ochranný faktor proti UV záření, při přípravě tenkých vrstev atd.Transparent metal oxide particles are used in many fields, eg as pigments in paints, in cosmetics as a protective factor against UV radiation, in the preparation of thin films, etc.
Pro přípravu transparentních částic oxidu titaničítého (resp. transparentních vrstev) se s výhodou používá řízená hydrolýza alkoxidů titanu. Další známou metodou je adsorpce organických makromolekul na povrchu částic oxidu titaničítého, které pak tyto částice izolují od vodné fáze a zabraňují vzniku aglomerátů - prakticky se to provádí např. hydrolýzou v prostředí polyethylen20 glykolu. Také je možné změnou hodnoty pH povrch částice nabít na mnohonásobný kladný či záporný náboj a tím zabránit srážkám, které by vedly ke vzniku aglomerátů. Jinou možnou metodou přípravy je mokré mleti titanových pigmentů.For the preparation of transparent titanium dioxide particles (or transparent layers), controlled hydrolysis of titanium alkoxides is preferably used. Another known method is the adsorption of organic macromolecules on the surface of titanium dioxide particles, which then isolate the particles from the aqueous phase and prevent agglomerates from forming - for example, by hydrolysis in polyethylene 20 glycol. It is also possible, by changing the pH value, to charge the particle surface to a multiple positive or negative charge, thereby avoiding precipitation that would lead to agglomerates. Another possible preparation method is wet grinding of titanium pigments.
Podstata vynálezuSUMMARY OF THE INVENTION
Podstata způsobu výroby transparentních fotokatalyticky aktivních částic oxidu titaničítého podle vynálezu spočívá v tom, že roztok soli titanu je hydrolyzován za normální nebo za zvýšené teploty v prostředí polyhydroxyethylmethakrylátu (HEMA).The principle of the process for producing transparent photocatalytically active titanium dioxide particles according to the invention is that the titanium salt solution is hydrolyzed at normal or elevated temperature in a polyhydroxyethyl methacrylate (HEMA) medium.
Solí titanu může být především chlorid titanitý, chlorid titaničitý nebo oxychlorid titanitý.The titanium salt may in particular be titanium tetrachloride, titanium tetrachloride or titanium oxychloride.
Hydrolýza se s výhodou provádí při teplotě do 100° C.The hydrolysis is preferably carried out at a temperature of up to 100 ° C.
Přínosem způsobu podle vynálezu oproti dosavadním postupům je jednoduchost přípravy, relativně levná surovinová základna a absolutně bezodpadová technologie. Základní výhodou potom je, že transparentní fotokatalytické částice oxidu titaničítého se získají v prostředí, se kterým tvoří vhodný prekurzor se specifickými vlastnostmi např. pro nátěrové hmoty a povrchové transparentní laky.The advantages of the process according to the invention over the prior art processes are simplicity of preparation, relatively cheap raw material base and absolutely waste-free technology. The basic advantage is that transparent photocatalytic titanium dioxide particles are obtained in an environment with which they form a suitable precursor with specific properties, for example, for paints and surface transparent lacquers.
Příklady provedeni vynálezuDETAILED DESCRIPTION OF THE INVENTION
K bližšímu objasnění způsobu výroby podle vynálezu slouží následující příklady.The following examples serve to illustrate the process of the invention in more detail.
Příklad 1 g kovového titanu bylo rozpuštěno ve 100 ml koncentrované kyseliny chlorovodíkové za vzni50 ku chloridu titanitého a doplněno na celkový objem 100 ml (Roztok 1). 50 ml připraveného Roztoku 1 bylo pak přidáno ke směsi vzniklé smícháním 200 ml roztoku HEMA1 (20% roztok polyhydroxyethylmethakrylátu v ethanolu) a 600 ml ethanolu; čirý reakční roztok se zabarvil do modrofialova. Reakční směs byla potom za stálého míchání zahřívána na teplotu 70 °C. Jakmile došlo k odbarvení roztoku, bylo zahřívání ukončeno a roztok byl míchán až do vychladnutí na laboratorní teplotu.Example 1 g of titanium metal was dissolved in 100 ml of concentrated hydrochloric acid to form titanium tetrachloride and made up to a total volume of 100 ml (Solution 1). 50 ml of the prepared Solution 1 was then added to the mixture formed by mixing 200 ml of a solution of HEMA1 (20% solution of polyhydroxyethyl methacrylate in ethanol) and 600 ml of ethanol; the clear reaction solution turned blue-violet. The reaction mixture was then heated to 70 ° C with stirring. Once the solution had decolorized, heating was stopped and the solution was stirred until it cooled to room temperature.
Produktem je čirá, opaleskující kapalina s obsahem transparentních částic oxidu titaničitého 5 o velikostí 70-80 nm. Tyto částice byly zviditelněny v laserovém paprsku na základě Tyndallova jevu.The product is a clear opalescent liquid containing 70-80 nm transparent titanium dioxide 5 particles. These particles were visualized in the laser beam based on the Tyndall effect.
Příklad 2Example 2
K 50 ml roztoku HEMA2 (20% roztok polyhydroxyethylmethakrylátu v ethanolu s 10 % kyseliny methakrylové bylo přidáno 150 ml ethanolu a 25 ml roztoku chloridu titanitého (15% roztok Sigma-Aldrich). Reakční směs byla pak intenzivně míchána za laboratorní teploty. Jakmile došlo k odbarvení roztoku, bylo míchání ukončeno.To 50 ml of HEMA2 solution (20% polyhydroxyethyl methacrylate solution in ethanol with 10% methacrylic acid) was added 150 ml ethanol and 25 ml titanium tetrachloride solution (15% Sigma-Aldrich solution) and the reaction mixture was then stirred vigorously at room temperature. decolourizing the solution, stirring was complete.
Produktem je čirá, opaleskující kapalina s obsahem transparentních částic oxidu titaničitého o velikosti 60 - 70 nm.The product is a clear, opalescent liquid containing 60 - 70 nm transparent titanium dioxide particles.
Příklad 3Example 3
K 50 ml roztoku HEMA3 (40% roztok polyhydroxyethylmethakrylátu v ethanolu) bylo přidáno 150 ml ethanolu a 50 ml 0,1 M roztoku chloridu titaničitého v kyselině chlorovodíkové. Reakční roztok byl intenzivně míchán za laboratorní teploty a laserovým paprskem byl sledován vznik částic. Po jejich vzniku byl pak roztok míchán ještě jednu hodinu.To 50 ml of HEMA3 solution (40% solution of polyhydroxyethyl methacrylate in ethanol) was added 150 ml of ethanol and 50 ml of a 0.1 M solution of titanium tetrachloride in hydrochloric acid. The reaction solution was vigorously stirred at room temperature and the formation of particles was monitored by laser beam. After formation, the solution was stirred for an additional hour.
Produktem je čirá, opaleskující kapalina s obsahem transparentních částic oxidu titaničitého o velikosti 60 - 100 nm.The product is a clear, opalescent liquid containing 60 - 100 nm transparent titanium dioxide particles.
Příklad 4Example 4
K 50 ml roztoku HEMA1 (20% roztok polyhydroxyethylmethakrylátu v ethanolu) bylo přidáno 150 ml ethanolu a 25 ml roztoku oxychloridu titanitého. Reakční roztok byl intenzivně míchán za laboratorní teploty a laserovým paprskem byl sledován vznik částic. Po jejich vzniku byl pak roztok míchán ještě jednu hodinu.To 50 mL of HEMA1 solution (20% polyhydroxyethyl methacrylate solution in ethanol) was added 150 mL of ethanol and 25 mL of titanium oxychloride solution. The reaction solution was vigorously stirred at room temperature and the formation of particles was monitored by laser beam. After formation, the solution was stirred for an additional hour.
Produktem je čirá, opaleskující kapalina s obsahem transparentních částic oxidu titaničitého o velikosti 60- 100 nm.The product is a clear, opalescent liquid containing 60-100 nm transparent titanium dioxide particles.
Průmyslová využitelnostIndustrial applicability
Roztok koloidních (transparentních) částic oxidu titaničitého je možno využít při přípravě foto45 katalyticky aktivních transparentních nátěrů nebo jako prekurzorů nátěrových hmot.The solution of colloidal (transparent) titanium dioxide particles can be used in preparing photo45 catalytically active transparent coatings or as paint precursors.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CZ20060270A CZ300800B6 (en) | 2006-04-27 | 2006-04-27 | Process for preparing transparent photocatalytically active particles of titanium dioxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CZ20060270A CZ300800B6 (en) | 2006-04-27 | 2006-04-27 | Process for preparing transparent photocatalytically active particles of titanium dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CZ2006270A3 CZ2006270A3 (en) | 2007-11-07 |
| CZ300800B6 true CZ300800B6 (en) | 2009-08-12 |
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| Application Number | Title | Priority Date | Filing Date |
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| CZ20060270A CZ300800B6 (en) | 2006-04-27 | 2006-04-27 | Process for preparing transparent photocatalytically active particles of titanium dioxide |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW241278B (en) * | 1992-11-04 | 1995-02-21 | Henkel Corp | |
| US6610135B1 (en) * | 1998-08-19 | 2003-08-26 | Showa Denko K.K. | Titanium-containing finely divided particulate material, aqueous sol composition and coating liquid containing same, process for producing same, and shaped article having film thereof |
| CZ293442B6 (en) * | 1999-12-07 | 2004-04-14 | Precheza A. S. | Stabilization process of calcining mode of operation when preparing pigmentary titanium dioxide |
| CZ297774B6 (en) * | 2005-05-25 | 2007-03-28 | Ceské technologické centrum pro anorganické pigmenty, akciová spolecnost | Process for producing nanofibers of photocatalytically active titanium dioxide |
-
2006
- 2006-04-27 CZ CZ20060270A patent/CZ300800B6/en not_active IP Right Cessation
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TW241278B (en) * | 1992-11-04 | 1995-02-21 | Henkel Corp | |
| US6610135B1 (en) * | 1998-08-19 | 2003-08-26 | Showa Denko K.K. | Titanium-containing finely divided particulate material, aqueous sol composition and coating liquid containing same, process for producing same, and shaped article having film thereof |
| CZ293442B6 (en) * | 1999-12-07 | 2004-04-14 | Precheza A. S. | Stabilization process of calcining mode of operation when preparing pigmentary titanium dioxide |
| CZ297774B6 (en) * | 2005-05-25 | 2007-03-28 | Ceské technologické centrum pro anorganické pigmenty, akciová spolecnost | Process for producing nanofibers of photocatalytically active titanium dioxide |
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| Publication number | Publication date |
|---|---|
| CZ2006270A3 (en) | 2007-11-07 |
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| MM4A | Patent lapsed due to non-payment of fee |
Effective date: 20180427 |