201020296 六、發明說明: 【發明所屬之技術領域】 本發明涉及一種複合塗料的技術’特別涉及一種複合塗料 的製備方法及其產品。 【先前技術】 获,溶膠凝膠沄201020296 VI. Description of the Invention: [Technical Field] The present invention relates to a technique for composite coatings, and particularly to a method for preparing a composite coating and a product thereof. [Prior Art] obtained, sol-gel 沄
用方法,其化學均勻性好、製程簡單、操作方便、成本低,同 時具有向的透光度並適用於各種基材,可以塗佈於大型複雜的 基體上’因此於業界得到廣泛的應用,但在其製備的過程中往 往需要給予一定的高溫加熱以利最終成膜。 複合塗料製成之複合薄膜通常具有兩種或兩種以上普通 薄膜的優點’常見的無機薄臈其組成成份為—含有兩種以 無機金屬氧化物,例如:氧化辞、二氧切、二氧化鈦、二氧 =及二氧化二鋁等,此薄膜的優勢為可包括兩種以上的複數 ^’不_組成成份會有不同功能性的表現,例如 化欽和二氧化石々+為人、人 5 一乳 薄膜之光觸媒材二製成之複合薄膜既具有二氧化鈦 效.AM 還具有膜之抗刮耐磨功 化嫩㈣狀複合㈣既具有氧 效:因氧化㈣—功 I二二!1複合塗料在成膜過程中—般f要進行高溫加 【發明内容】〜加_成膜時間長’製成之薄膜的強度差。 本發明的g β & 複合塗料的製備習知技術存在之缺陷提供-種 方法及其產品,以該方法製備之產品可在不經 201020296 高溫加熱的條件下快速成膜且製成之薄膜的強度好。 為實現上述目的,本發明所提供複合塗料的製備方法包括 如下步驟: (1) 首先,將一定容量作為前驅物的非矽類無機金屬鹽 加入到醇類溶劑,並攪拌30〜60分鐘; (2) 其次,在加入有非矽類無機金屬鹽的醇類溶劑内加 入一定容量的矽類無機金屬鹽,並攪拌30〜60分鐘; (3) 嗣後,在上述第(2)步驟中所混合的溶液内加入水 及作為觸媒用且濃度為10%〜40%的酸溶液或鹼溶液,將混和 〇 物攪拌4〜8小時,使其充分進行水解縮合反應; (4) 最後,將上述混合溶液於室溫或於低於100°C的加 熱條件下靜置24小時,最終得到一穩定複合塗料。 如上所述,本發明複合塗料的製備方法所製得的塗料產品 在塗佈於基材表面後,可在常溫或於低於l〇〇°C的加熱條件下 經30〜60分鐘後乾燥便可在基材表面形成一強度好、穩定性高 的複合薄膜。 【實施方式】 Q 為詳細說明本發明之技術内容及其所達成之目的與功 效,下面將結合實施例詳予說明。 本發明複合塗料的製備方法包括如下步驟: (1)將作為前驅物的非矽類無機金屬鹽以一定容量加入 到醇類溶劑内,並攪拌30-60分鐘;其中適量的醇類溶劑可以 為乙醇和異丙醇中之一種或兩種;非矽類無機金屬鹽可從以下 各組無機金屬鹽的一組或多組選得,且每組無機金屬鹽中選擇 一種或多種: (a) Ti(OC2H5)4、Ti(OCH(CH3)2)4 ; 201020296 (b) Al(OC3H7)3、Al[OCH(CH3)C2H5]3 ; (c) Zr(OC2H5)4、Zr(OCH2CH2CH3)4、Zr[OC(CH3)3]4 ; (d) Zn(CH3C00)2-2H20。 (2) 其次,在第(1)步驟所混合的溶液中加入以一定容量 作為前驅物的矽類無機金屬鹽,並攪拌30〜60分鐘;其中梦類 無機金屬鹽可以為 Si(OC2H5)4、C2H5Si(OC2H5)3、 C2H5Si(OCH3)3、CH3Si(OC2H5)3、H2C=CHSi(OC2H5)3、 H2C=CHSi(OCH3)3、CH3Si(OCH3)3 中的任意一種或多種。 (3) 嗣後,在第(2)步驟所混合的溶液中再加入水及作為 ® 觸媒且濃度為10%〜40%的酸溶液或鹼溶液,並將混和物挽拌 4〜8小時,使其充分進行水解縮合反應;其中水可以為去離子 水;酸溶液為鹽酸溶液、醋酸溶液和硝酸溶液之一種或一種以 上的混和物;鹼溶液可為氫氧化铵溶液。 (4) 最後,於室溫下靜置24小時,最終得到一穩定複合 塗料。 下面以製備Si02/Al203複合塗料的製備方法和 Si02/Ti02/Al203複合塗料製備方法為例對本發明詳細說明。 ❹ 實施例一:製備Si02/Al20複合塗料 首先將2毫升Al(OC3H7)3加入於300毫升的乙醇溶劑中, 並於室溫下攪拌30分鐘;隨後加入50毫升Si(OC2H5)4、50 毫升 C2H5Si(OC2H5)3、50 毫升 H2C=CHSi(OCH3)3 並於室溫下 攪拌30分鐘;再加入1〇毫升濃度為10%的鹽酸及15毫升去 離子水’並持續攪拌4小時;最後於室溫下靜置24小時形成 穩定的Si02/Al203複合塗料。將此Si02/Al203複合塗料塗佈於 基材表面,經過30分鐘後自然乾燥後便可在基材表面上形成 強度好、穩定性高的Si02/Al203複合薄膜。 實施例二:製備Si02/Ti02/Al203複合塗料 5 201020296 首先,將1.5毫升Al[OCH(CH3)C2H5]3和1.5毫升 Ti(OCH(CH3)2)4加入300毫升的乙醇溶劑中並於室溫下攪拌3〇 分鐘;其次,再加入50毫升Si(OC2H5)4、50毫升 H2C=CHSi(OC2H5)3 和 50 毫升 H2C=CHSi(OCH3)3 並於室溫下 攪拌30分鐘;嗣後,加入1〇毫升濃度為1〇 %的鹽酸及15毫 升去離子水,並持續攪拌4小時後停止攪拌;最後於室溫下靜 置24小時便可得到穩定的SiOz/TiOz/AIzO3複合塗料。將此 SKVTKVAbO3複合塗料塗佈於基材表面,於5〇〇c下加熱3 分鐘’即可在基材表面上形成強度好、穩定性高的 ® Si02/Ti02/Al203 複合薄膜。 如上所述,經由本發明複合塗料的製備方法所製得的塗料 產品在塗佈於基材表面後,可在常溫或於低於“^匸的加熱條 件下經30〜60分鐘後乾燥便可形成一強度好、穩定性高的複合 薄膜。 。The method has the advantages of good chemical uniformity, simple process, convenient operation, low cost, simultaneous transmittance and suitable for various substrates, and can be applied to large and complex substrates, so it is widely used in the industry. However, in the process of its preparation, it is often necessary to give a certain high temperature heating to facilitate the final film formation. Composite films made from composite coatings usually have the advantage of two or more ordinary films. The common inorganic thin ruthenium consists of two inorganic metal oxides, such as oxidized, dioxic, and titanium dioxide. Dioxane = and Al2O2, etc., the advantage of this film is that it can include more than two kinds of complex elements. The composition of the compound has different functionalities, such as Huachin and sulphur dioxide 々+ for humans and humans. The composite film made of the photocatalyst of a milk film has the effect of titanium dioxide. The AM also has the anti-scratch and abrasion resistance of the film (four) composite (four) has the oxygen effect: due to oxidation (four) - work II two! (1) In the film-forming process, the composite coating is subjected to high-temperature addition. [Invention] The film produced by the filming process has a low strength. The preparation of the g β & composite coating of the present invention has the defects of the prior art to provide a method and a product thereof, and the product prepared by the method can be rapidly formed into a film without heating at a high temperature of 201020296 and the film is prepared. Good strength. In order to achieve the above object, the preparation method of the composite coating provided by the present invention comprises the following steps: (1) First, a non-steroidal inorganic metal salt having a certain capacity as a precursor is added to an alcohol solvent and stirred for 30 to 60 minutes; 2) Next, a certain amount of an inert inorganic metal salt is added to an alcohol solvent having a non-indole inorganic metal salt and stirred for 30 to 60 minutes; (3) after mixing, mixed in the above step (2) To the solution, water and an acid solution or an alkali solution having a concentration of 10% to 40% as a catalyst are added, and the mixed mixture is stirred for 4 to 8 hours to sufficiently carry out a hydrolysis condensation reaction; (4) Finally, the above The mixed solution was allowed to stand at room temperature or under heating conditions of less than 100 ° C for 24 hours to finally obtain a stable composite coating. As described above, the coating product prepared by the method for preparing the composite coating of the present invention can be dried after being applied to the surface of the substrate at room temperature or under heating conditions of less than 10 ° C for 30 to 60 minutes. A composite film having high strength and high stability can be formed on the surface of the substrate. [Embodiment] Q is a detailed description of the technical contents of the present invention and the objects and effects achieved thereby, which will be described in detail below with reference to the embodiments. The preparation method of the composite coating of the invention comprises the following steps: (1) adding a non-indole inorganic metal salt as a precursor to an alcohol solvent in a certain volume and stirring for 30-60 minutes; wherein an appropriate amount of the alcohol solvent may be One or two of ethanol and isopropanol; the non-indole inorganic metal salt may be selected from one or more groups of the following groups of inorganic metal salts, and one or more of each group of inorganic metal salts are selected: (a) Ti(OC2H5)4, Ti(OCH(CH3)2)4; 201020296 (b) Al(OC3H7)3, Al[OCH(CH3)C2H5]3; (c) Zr(OC2H5)4, Zr(OCH2CH2CH3)4 Zr[OC(CH3)3]4; (d) Zn(CH3C00)2-2H20. (2) Next, in the solution mixed in the step (1), a bismuth-based inorganic metal salt having a certain capacity as a precursor is added and stirred for 30 to 60 minutes; wherein the dream inorganic metal salt may be Si(OC2H5)4. Any one or more of C2H5Si(OC2H5)3, C2H5Si(OCH3)3, CH3Si(OC2H5)3, H2C=CHSi(OC2H5)3, H2C=CHSi(OCH3)3, and CH3Si(OCH3)3. (3) After the enthalpy, add water and an acid solution or an alkali solution as a catalyst with a concentration of 10% to 40% in the solution mixed in the step (2), and mix the mixture for 4 to 8 hours. The hydrolysis reaction is sufficiently carried out; wherein the water may be deionized water; the acid solution is a mixture of one or more of a hydrochloric acid solution, an acetic acid solution and a nitric acid solution; and the alkali solution may be an ammonium hydroxide solution. (4) Finally, it was allowed to stand at room temperature for 24 hours to finally obtain a stable composite coating. The following is a detailed description of the preparation method of the SiO 2 /Al 2 2 composite coating and the preparation method of the SiO 2 /TiO 2 /Al 2 2 composite coating.实施 Example 1: Preparation of SiO 2 /Al 20 composite coating First, 2 ml of Al(OC3H7) 3 was added to 300 ml of ethanol solvent and stirred at room temperature for 30 minutes; then 50 ml of Si(OC2H5) 4, 50 ml was added. C2H5Si(OC2H5)3, 50 ml H2C=CHSi(OCH3)3 and stirred at room temperature for 30 minutes; add 1 ml of 10% hydrochloric acid and 15 ml of deionized water' and continue stirring for 4 hours; The mixture was allowed to stand at room temperature for 24 hours to form a stable SiO 2 /Al 2 2 composite coating. The SiO 2 /Al 2 2 composite coating was applied to the surface of the substrate, and after 30 minutes, it was naturally dried to form a SiO 2 /Al 2 2 composite film having high strength and high stability on the surface of the substrate. Example 2: Preparation of SiO 2 /Ti02 / Al 203 composite coating 5 201020296 First, 1.5 ml of Al[OCH(CH3)C2H5]3 and 1.5 ml of Ti(OCH(CH3)2)4 were added to 300 ml of ethanol solvent and placed in a chamber. Stir for 3 minutes at room temperature; secondly, add 50 ml of Si(OC2H5)4, 50 ml of H2C=CHSi(OC2H5)3 and 50 ml of H2C=CHSi(OCH3)3 and stir at room temperature for 30 minutes; 1 〇ml of 1% by weight hydrochloric acid and 15 ml of deionized water, and stirring was continued for 4 hours, then the stirring was stopped; finally, standing at room temperature for 24 hours, a stable SiOz/TiOz/AIzO3 composite coating was obtained. This SKVTKVAbO3 composite coating is applied to the surface of the substrate and heated at 5 °c for 3 minutes to form a high-strength, high-stability ® Si02/Ti02/Al203 composite film on the surface of the substrate. As described above, the coating product obtained by the preparation method of the composite coating of the present invention can be dried after being applied to the surface of the substrate at room temperature or under a heating condition of less than 30 to 60 minutes. Forming a composite film with good strength and high stability.