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Patent US5981425 - Photocatalyst-containing coating composition - Google PatentsSearch Images Maps Play YouTube News Gmail Drive More »Sign inPatentsA coating composition which is excellent in water resistance, weatherability and durability and can maintain its appearance for a prolonged period of time can be provided. A coating composition comprising a coating component and a photocatalyst containing calcium phosphate and titanium oxide is disclosed....http://www.google.com/patents/US5981425?utm_source=gb-gplus-sharePatent US5981425 - Photocatalyst-containing coating compositionAdvanced Patent SearchTry the new Google Patents, with machine-classified Google Scholar results, and Japanese and South Korean patents.Publication numberUS5981425 APublication typeGrantApplication numberUS 09/285,056Publication dateNov 9, 1999Filing dateApr 2, 1999Priority dateApr 14, 1998Fee statusPaidAlso published asDE69940450D1, EP0963789A2, EP0963789A3, EP0963789B1Publication number09285056, 285056, US 5981425 A, US 5981425A, US-A-5981425, US5981425 A, US5981425AInventorsHiroshi Taoda, Toru Nonami, Takaaki Fujiwa, Masahiro KagotaniOriginal AssigneeAgency Of Industrial Science & Tech., Daicel Chemical Ind., Ltd., H. Taoda, T. NonamiExport CitationBiBTeX, EndNote, RefManPatent Citations (1), Referenced by (117), Classifications (18), Legal Events (5) External Links: USPTO, USPTO Assignment, EspacenetPhotocatalyst-containing coating composition
US 5981425 AAbstract
A coating composition which is excellent in water resistance, weatherability and durability and can maintain its appearance for a prolonged period of time can be provided. A coating composition comprising a coating component and a photocatalyst containing calcium phosphate and titanium oxide is disclosed. As the photocatalyst, use is made of titanium oxide particles partially covered thereon with calcium phosphate, or porous body coated thereon with a film of titanium oxide, the film of titanium oxide being further covered partially thereon with calcium phosphate. The crystal form of titanium oxide is preferably anatase. The organic coating includes vinyl-type synthetic resin emulsions, and the inorganic coating is e.g. a solution containing a metal alkoxide for forming a film by a sol-gel method.
1. A coating composition comprising a coating component and a photocatalyst containing calcium phosphate and titanium oxide.
WO 96/29375 discloses a photocatalytic hydrophilic film comprising silica and a photocatalytic material selected from TiO2, ZnO, SnO2, SrTiO3, WO3, Bi2 O3 and Fe2 O3.
In addition, if an organic coating is used as a coating component, the organic coating component comes into direct contact with TiO2 etc., so there is also the problem of coating deterioration.
Accordingly, the object of the present invention is to provide a coating composition which is excellent in water resistance, weatherability and durability and capable of maintaining the appearance thereof for a long period of time, thus solving the above problems in the prior art.
First, the photocatalyst used in the present invention is described. In the present invention, a photocatalyst containing calcium phosphate and titanium oxide is used. Although the form of this photocatalyst is not particularly limited, but taking it into consideration that calcium phosphate is excellent in the ability to absorb proteins and a wide variety of aqueous dirt components and also that titanium oxide is superior in photocatalytic functions, the form of the photocatalyst having covering of calcium phosphate on a part of the surface of titanium oxide is preferable.
The calcination is conducted preferably by gradually heating the porous body at room temperature to a temperature of a final temperature of 600° C. to 700° C. or by heating it at a temperature of 400° C. to 600° C. By this procedure, the titania sol with which the porous body has been covered is converted into titanium oxide as a high-performance photocatalyst whose crystal form is anatase. In this step, if the porous body is calcinated by heating at a temperature of 600° C. to 700° C. directly or at a calcination temperature of less than 400° C. or more than 700° C., there is brought about low-active rutile as a photocatalyst or partially amorphous titanium oxide.
Covering with calcium phosphate may be conducted by immersing titanium oxide particles or particles coated with titanium oxide in an aqueous solution containing at least Ca and P, followed by drying them. The aqueous solution may be a pseudo-humor. The pseudo-humor preferably contains ions such as, for example, Na, K, Cl, Ca, P, and Mg, etc. In particular, it is preferably at pH 7 to 8, more preferably at pH 7.3 to 7.7. Immersion in the aqueous solution is conducted for example at 20 to 60° C. for 10 minutes to 30 days or so, preferably at 30 to 40° C. for 20 minutes to 24 hours or so.
(R11)n Si(OR12)4-n                     (1)
In this formula, R11, represents an optionally substituted lower alkyl group or an optionally substituted aryl group, R12 represents a lower alkyl group, R11 and R12 may be different depending on n. n is an integer of 0 or 1. The lower alkyl group represented by R11 and R12 is usually an alkyl group containing about 1 to 4 carbons, and includes methyl, ethyl, propyl, isopropyl, butyl, isobutyl and sec-butyl groups.
If an organic solvent is used as a coating component, the organic coating component hardly comes into direct contact with TiO2, thus making the coating stable.
Hereinafter, the present invention is described in more detail by reference to the Examples, which however are not intended to limit the present invention. Hereinafter, the term "parts" refers to parts by weight unless otherwise specified.
Preparative Example of Vinyl Type Synthetic Resin Emulsion
TABLE 1______________________________________Preparative Example of Vinyl Type Synthetic Resin Emulsion______________________________________Deionized water          100.6 parts  2-Ethylhexylacrylate  33 parts  Methyl methacrylate 24.5 parts  Styrene  40 parts  Acrylic acid   2 parts  Itaconic acid 0.5 parts  &#947;-Methacryloyloxypropyltrimethoxysilane 0.2 parts  (Emulsifier)  Polyoxyalkylene styrene phenyl ether (n = 10) 0.5 parts  Polyoxyalkylene styrene phenyl ether (n = 50) 3.5 parts  Sulfate soda of polyoxyethylene nonyl phenyl ether 0.5 parts  (n = 6)  Sodium styrenesulfonate 0.2 parts  (Polymerization initiator)  Ammonium persulfate 0.5 parts  Sodium bisulfite 0.5 parts______________________________________
40 parts of deionized water were introduced into a four-necked flask and heated to 80° C. in a nitrogen stream, and the polymerization initiator was added thereto. Separately, the polymerizable monomer was emulsified in an aqueous solution of the emulsifier dissolved in the remainder of water, and this emulsion was dropped for 3 hours into it the flask. The reaction temperature at the time of dropping was regulated within 78 to 82° C.
Preparation of a Photocatalyst Covered Partially with Calcium Phosphate
45 g of titanium tetraisopropoxide was diluted with 400 ml absolute ethanol, and 15 g of triethanolamine and 4 g of water were added thereto under stirring. Further, 4 g of polyethylene glycol with a molecular weight of 1500 was added thereto under stirring to prepare a transparent sol solution. Spherical silica gel with a diameter of about 10 μm was then coated with said sol solution by dropping. That is, a small amount of this sol solution was dropped onto the surface of the spherical silica gel, and an excess of the solution was removed, and the gel was dried and then heated gradually from room temperature to a temperature 600° C. for calcination. This was repeated 5 times so that a film of titanium oxide was formed on the surface of the spherical silica gel. As a result of examination of the crystal structure of the resulting film of titanium oxide by X-ray diffraction, the structure was composed of 100% anatase. Observation of the surface under an electron microscope indicated that it had pores with a size of about 20 nm.
The resulting particles coated with the film of titanium oxide was suspended in 1 L pseudo-humor, left for 2 hours at 37° C. and then dried at 100° C. The pseudo-humor contained 8000 mg sodium chloride, 200 mg potassium chloride, 1150 mg sodium monohydrogen phosphate, 200 mg potassium dihydrogen phosphate and 200 mg calcium chloride per litter of water. In this manner, a photocatalyst having a part (about 12% under an electron microscope) of the surface of the film of titanium oxide covered with calcium phosphate was obtained.
Preparation of a Photocatalyst Partially Covered with Calcium Phosphate
10 g of anatase-type titanium oxide (Super Titania, an average particle diameter of 30 nm, Showa Denko, K. K.) was suspended in 1 L of the same pseudo-humor as in Reference Example 2, left for 2 hours at 37° C. and then dried at 100° C. In this manner, a photocatalyst having a part (about 2% under an electron microscope) of the surface of the titanium oxide particles covered with calcium phosphate was obtained.
The synthetic resin emulsion obtained in Reference Example 1 was formed into a coating with the formulation shown in Table 2. That is, as the photocatalyst, TiO2 covered with calcium phosphate obtained in Reference Example 2 was used in Example 1, TiO2 covered with calcium phosphate obtained in Reference Example 3 was used in Example 2, TiO2 R630 (average particle diameter of 0.24 μm, produced by Ishihara Sangyo Kaisha, Ltd.) was used in Reference Example 1, and anatase-type TiO2 ST41 (average particle diameter of 0.1 μm, produced by Ishihara Sangyo Kaisha, Ltd.) was used in Reference Example 2.
Each coating was applied by a bar coater # 420 onto an aluminum plate and burned at 120° C. for 30 minutes to prepare a test piece. (Weatherability)
Using a black aqueous ink, a line of 2 mm in width was drawn on the coating film on each test piece. A promotion test was conducted under the conditions of QUV 3000 hours, 60° C. and humidity of 20%, and the degree of decomposition of the black ink (%) was determined using a Macbeth densitometer. That is, higher degrees of decomposition of the ink (%) indicate higher stain resistance.
Degree of decomposition of ink (%) 100×[(density of the black ink before the promotion test)-(density of the black ink after the promotion test)]/(density of the black ink before the promotion test)
TABLE 2__________________________________________________________________________               Comparative                     Comparative  Coating ingredients Example 1 Example 2 Example 1 Example 2__________________________________________________________________________Water               7.8 parts                     7.8 parts                              7.8 parts                                   7.8 parts  HEC SP600 0.27 parts 0.27 parts 0.27 parts 0.27 parts  (Dicel Chemical Industries, Ltd.)  Primal 850 (Rhoom &amp; Haas) 0.65 parts 0.65 parts 0.65 parts 0.65 parts                                    SN defoamer 315 (Sunnopco) 0.40                                   parts 0.40 parts 0.40 parts 0.40                                   parts  TiO2 R630 31.4 parts -- -- --  (Ishihara Sangyo Kaisha, Ltd.)  Anatase-type TiO2 ST41 -- 31.4 parts -- --  (Ishihara Sangyo Kaisha, Ltd.)  Calcium phosphate-covered TiO2 -- -- 31.4 parts --  (Reference Example 2)  Calcium phosphate-covered TiO2 -- -- -- 31.4 parts  (Reference Example 3)  Synthetic resin emulsion 100 parts 100 parts 100 parts 100 parts                                    (Reference Example 1)  CS 12 (Chisso Corporation) 4.0 parts 4.0 parts 4.0 parts 4.0 parts                                    Weatherability: Degree of gloss                                   retention (%) 80 50 80 80                                      (Film deterioration)  Stain resistance: 10 35 50 50  Degree of decomposition of ink (%)__________________________________________________________________________
As can be seen from Table 2, because TiO2 was covered partially with calcium phosphate in Examples 1 and 2, the coating component in the coating did not come in direct contact with TiO2, so the coating was stable and superior in weatherability to that of Comparative Example 2 where usual anatase-type TiO2 was used. Further, in Examples 1 and 2, the aqueous ink was absorbed into calcium phosphate and the decomposition of the ink was promoted, so the coating was also superior in stain resistance.
100 parts of methyltrimethoxysilane, 10 parts of tetraethoxysilane, 90 parts of organosilica gel, 30 parts of dimethyldimethoxysilane and 100 parts of isopropyl alcohol were mixed, and then 90 parts of water and 40 parts of the TiO2 covered partially with calcium phosphate in Reference Example 2 were added thereto and stirred. Thereafter, this suspension was regulated in a thermostatic bath at 60° C. such that its weight average molecular weight became 1500, to give a photocatalyst-containing inorganic coating.
An inorganic coating film was prepared in the same manner as in Example 2 except that as the photocatalyst, TiO2 (Nippon Aerosol K: P-25) was used in place of the TiO2 covered partially with calcium phosphate in Reference Example 2.
Ares silicon (Kansai Paint Co., Ltd.) was used as a solvent-type, two-pack crosslinked acrylic silicon resin. The TiO2 covered with calcium phosphate obtained in Reference Example 3 was dispersed in the clear base of said Ares silicon such that its content was 10% by weight in the total resin. An Ares silicon hardener was added at the ratio of 1 part of said hardener to 14 parts of said clear base, and the mixture was applied in a thickness of 20 μm onto an aluminum plate and hardened at room temperature for 1 week whereby a test piece was prepared.
A test piece was prepared in the same manner as in Example 4 except that as the photocatalyst, anatase-type TiO2 STL41 (Ishihara Sangyo Kaisha, Ltd.: average particle diameter of 0.1 μm) was used in place of the TiO2 covered partially with calcium phosphate in Reference Example 3.
As can be seen from Table 4, because the TiO2 covered with calcium phosphate was used as the photocatalyst in Example 4, its film was stable and superior in weatherability to that of Comparative Example 4 where the conventional anatase-type TiO2 was used. Further, in Example 4, the decomposition of the ink was also promoted, and the film was also superior in stain resistance.
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Grace & Co.-Conn.Composite inorganic particles and methods of making and using the same* Cited by examinerClassifications U.S. Classification502/208, 502/233, 502/237, 502/214, 502/232, 502/238, 502/159, 502/527.12, 502/349, 502/350, 502/239, 502/527.15, 502/527.13International ClassificationB01J35/00Cooperative ClassificationB01J35/002, B01J35/004European ClassificationB01J35/00D6, B01J35/00DLegal EventsDateCodeEventDescriptionApr 2, 1999ASAssignmentOwner name: AGENCY OF INDUSTRIAL SCIENCE AND TECHNOLOGY, JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:TAODA, HIROSHI;NONAMI, TORU;FUJIWA, TAKAAKI;AND OTHERS;REEL/FRAME:009891/0235;SIGNING DATES FROM 19990310 TO 19990324Owner name: DAICEL CHEMICAL INDUSTRIES, LTD., JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:TAODA, HIROSHI;NONAMI, TORU;FUJIWA, TAKAAKI;AND OTHERS;REEL/FRAME:009891/0235;SIGNING DATES FROM 19990310 TO 19990324Owner name: NONAMI, TORU, JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:TAODA, HIROSHI;NONAMI, TORU;FUJIWA, TAKAAKI;AND OTHERS;REEL/FRAME:009891/0235;SIGNING DATES FROM 19990310 TO 19990324Owner name: TAODA, HIROSHI, JAPANFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNORS:TAODA, HIROSHI;NONAMI, TORU;FUJIWA, TAKAAKI;AND OTHERS;REEL/FRAME:009891/0235;SIGNING DATES FROM 19990310 TO 19990324Apr 18, 2003FPAYFee paymentYear of fee payment: 4Apr 13, 2007FPAYFee paymentYear of fee payment: 8Dec 16, 2009ASAssignmentOwner name: NATIONAL INSTITUTE OF ADVANCED INDUSTRIAL SCIENCEFree format text: ASSIGNMENT OF ASSIGNORS INTEREST;ASSIGNOR:DAICEL CHEMICAL INDUSTRIES, LTD.;REEL/FRAME:023660/0001Effective date: 20091209Apr 8, 2011FPAYFee paymentYear of fee payment: 12RotateOriginal ImageGoogle Home - Sitemap - USPTO Bulk Downloads - Privacy Policy - Terms of Service - About Google Patents - Send FeedbackData provided by IFI CLAIMS Patent Services