TWI396722B - Preparation of the composite coatings - Google Patents
Preparation of the composite coatings Download PDFInfo
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- TWI396722B TWI396722B TW97146429A TW97146429A TWI396722B TW I396722 B TWI396722 B TW I396722B TW 97146429 A TW97146429 A TW 97146429A TW 97146429 A TW97146429 A TW 97146429A TW I396722 B TWI396722 B TW I396722B
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- composite coating
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- 239000002131 composite material Substances 0.000 title claims description 38
- 238000000576 coating method Methods 0.000 title claims description 33
- 238000002360 preparation method Methods 0.000 title description 10
- 239000011248 coating agent Substances 0.000 claims description 32
- 229910052751 metal Inorganic materials 0.000 claims description 15
- 239000002184 metal Substances 0.000 claims description 15
- 150000003839 salts Chemical class 0.000 claims description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 5
- 239000002253 acid Substances 0.000 claims description 5
- 239000003513 alkali Substances 0.000 claims description 5
- 239000002243 precursor Substances 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 3
- 238000006482 condensation reaction Methods 0.000 claims description 3
- 230000007062 hydrolysis Effects 0.000 claims description 3
- 238000006460 hydrolysis reaction Methods 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 229910052797 bismuth Inorganic materials 0.000 claims description 2
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims description 2
- 229910017604 nitric acid Inorganic materials 0.000 claims description 2
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 2
- 239000000243 solution Substances 0.000 claims 9
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims 2
- 229910052787 antimony Inorganic materials 0.000 claims 2
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims 2
- 239000011259 mixed solution Substances 0.000 claims 1
- 239000010408 film Substances 0.000 description 20
- 229910004298 SiO 2 Inorganic materials 0.000 description 10
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 9
- 239000000758 substrate Substances 0.000 description 9
- 238000003756 stirring Methods 0.000 description 7
- SIKJAQJRHWYJAI-UHFFFAOYSA-N Indole Chemical compound C1=CC=C2NC=CC2=C1 SIKJAQJRHWYJAI-UHFFFAOYSA-N 0.000 description 6
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 6
- 229910010413 TiO 2 Inorganic materials 0.000 description 5
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 5
- 229910000420 cerium oxide Inorganic materials 0.000 description 4
- BMMGVYCKOGBVEV-UHFFFAOYSA-N oxo(oxoceriooxy)cerium Chemical compound [Ce]=O.O=[Ce]=O BMMGVYCKOGBVEV-UHFFFAOYSA-N 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- PZOUSPYUWWUPPK-UHFFFAOYSA-N indole Natural products CC1=CC=CC2=C1C=CN2 PZOUSPYUWWUPPK-UHFFFAOYSA-N 0.000 description 3
- RKJUIXBNRJVNHR-UHFFFAOYSA-N indolenine Natural products C1=CC=C2CC=NC2=C1 RKJUIXBNRJVNHR-UHFFFAOYSA-N 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 239000011787 zinc oxide Substances 0.000 description 3
- 238000005299 abrasion Methods 0.000 description 2
- 230000000844 anti-bacterial effect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- 239000004408 titanium dioxide Substances 0.000 description 2
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 1
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 description 1
- 150000004056 anthraquinones Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 1
- RVTZCBVAJQQJTK-UHFFFAOYSA-N oxygen(2-);zirconium(4+) Chemical compound [O-2].[O-2].[Zr+4] RVTZCBVAJQQJTK-UHFFFAOYSA-N 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 230000003637 steroidlike Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
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Description
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。 The invention relates to a composite coating technology, in particular to a preparation method of a composite coating.
按，溶膠凝膠法(Sol-Gel法)是一種製備無機薄膜的常用方法，其化學均勻性好、製程簡單、操作方便、成本低，同時具有高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。 According to the sol-gel method (Sol-Gel method), it is a common method for preparing inorganic thin films, which has good chemical uniformity, simple process, convenient operation, low cost, high transmittance and suitable for various substrates. It can be applied to large and complex substrates, so it is widely used in the industry, but it is often necessary to give a certain high temperature heating during the preparation process to facilitate the final film formation.
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，常見的無機薄膜其組成成份為一含有兩種以上的無機金屬氧化物，例如：氧化鋅、二氧化矽、二氧化鈦、二氧化鋯及三氧化二鋁等，此薄膜的優勢為可包括兩種以上的複數功能，不同的組成成份會有不同功能性的表現，例如：含二氧化鈦和二氧化矽之複合塗料製成之複合薄膜既具有二氧化鈦薄膜之光觸媒材料功能，還具有二氧化矽薄膜之抗刮耐磨功效；含氧化鋅和二氧化矽之複合塗料製成之複合薄膜既具有氧化鋅薄膜之抗菌抑菌功能，還具有二氧化矽薄膜之抗刮耐磨功效；因此，複合塗料得到了廣泛使用。 A composite film made of a composite coating generally has the advantages of two or more ordinary films, and a common inorganic film has a composition of two or more inorganic metal oxides such as zinc oxide, cerium oxide, titanium oxide, Zirconium dioxide and aluminum oxide, etc., the advantage of this film is that it can include more than two complex functions, different compositions have different functional properties, such as: composite coating containing titanium dioxide and cerium oxide The composite film not only has the function of the photocatalytic material of the titanium dioxide film, but also has the anti-scratch and abrasion resistance effect of the cerium oxide film; the composite film made of the composite coating containing zinc oxide and cerium oxide has the antibacterial and antibacterial function of the zinc oxide film. It also has the scratch and abrasion resistance of the ruthenium dioxide film; therefore, the composite coating is widely used.
惟，當前之複合塗料在成膜過程中一般需要進行高溫加熱；不進行高溫加熱則成膜時間長，製成之薄膜的強度差。 However, the current composite coating generally needs to be heated at a high temperature during the film formation process; the film formation time is long without heating at a high temperature, and the strength of the produced film is poor.
本發明的目的是針對上述習知技術存在之缺陷提供一種複合塗料的製備方法，以該方法製備之產品可在不經高溫加熱 的條件下快速成膜且製成之薄膜的強度好。 The object of the present invention is to provide a method for preparing a composite coating according to the defects of the above-mentioned prior art, and the product prepared by the method can be heated without high temperature. The film is formed quickly under the conditions and the strength of the film produced is good.
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內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內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條件下靜置24小時，最終得到一穩定複合塗料。 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) Secondly, adding a certain volume of anthraquinone inorganic metal salt to an alcohol solvent having a non-indole inorganic metal salt and stirring for 30 to 60 minutes; (3) after mixing, mixing in the above step (2) To the solution, water and an acid solution or an alkali solution having a concentration of 10% to 40% are used as a catalyst, and the mixture is stirred for 4 to 8 hours to sufficiently carry out a hydrolysis condensation reaction; (4) Finally, the above mixing is carried out. The solution was allowed to stand at room temperature for 24 hours to finally obtain a stable composite coating.
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，可在室溫的條件下經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。 As described above, the coating product prepared by the method for preparing the composite coating of the present invention can be formed on the surface of the substrate after being dried at room temperature for 30 to 60 minutes after being applied to the surface of the substrate. A composite film with high stability.
為詳細說明本發明之技術內容及其所達成之目的與功效，下面將結合實施例詳予說明。 The details of the technical contents of the present invention and the objects and effects achieved by the present invention will be described in detail below with reference to the embodiments.
本發明複合塗料的製備方法包括如下步驟： The preparation method of the composite coating of the invention comprises the following steps:
(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內，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；(b)Al(OC3H7)3、Al[OCH(CH3)C2H5]3； (c)Zr(OC2H5)4、Zr(OCH2CH2CH3)4、Zr[OC(CH3)3]4；(d)Zn(CH3COO)2．2H2O。 (1) adding a non-indole inorganic metal salt as a precursor to an alcohol solvent in a certain volume and stirring for 30 to 60 minutes; wherein an appropriate amount of the alcohol solvent may be one or both of ethanol and isopropanol The non-indole inorganic metal salt may be selected from one or more of the following groups of inorganic metal salts, and one or more of each group of inorganic metal salts are selected: (a) Ti(OC 2 H 5 ) 4 , Ti ( OCH(CH 3 ) 2 ) 4 ; (b) Al(OC 3 H 7 ) 3 , Al[OCH(CH 3 )C 2 H 5 ] 3 ; (c) Zr(OC 2 H 5 ) 4 , Zr(OCH 2 CH 2 CH 3 ) 4 , Zr[OC(CH 3 ) 3 ] 4 ; (d) Zn(CH 3 COO) 2 . 2H 2 O.
(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；其中矽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。 (2) Next, a ruthenium-based inorganic metal salt having a certain capacity as a precursor is added to the solution mixed in the step (1), and stirred for 30 to 60 minutes; wherein the bismuth-based inorganic metal salt may be Si (OC 2 H). 5 ) 4 , C 2 H 5 Si(OC 2 H 5 ) 3 , C 2 H 5 Si(OCH 3 ) 3 , CH 3 Si(OC 2 H 5 ) 3 , H 2 C=CHSi(OC 2 H 5 ) 3. Any one or more of H 2 C=CHSi(OCH 3 ) 3 and CH 3 Si(OCH 3 ) 3 .
(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，並將混和物攪拌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；鹼溶液可為氫氧化銨溶液。 (3) After the enthalpy, add water and a solution of 10% to 40% acid or alkali as a catalyst in the solution mixed in the step (2), and stir the mixture for 4 to 8 hours. The hydrolysis condensation 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)最後，於室溫下靜置24小時，最終得到一穩定複合塗料。 (4) Finally, it was allowed to stand at room temperature for 24 hours to finally obtain a stable composite coating.
下面以製備SiO2/Al2O3複合塗料的製備方法和SiO2/TiO2/Al2O3複合塗料製備方法為例對本發明詳細說明。 The following is a detailed description of the preparation method of the SiO 2 /Al 2 O 3 composite coating and the preparation method of the SiO 2 /TiO 2 /Al 2 O 3 composite coating as an example.
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10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SiO2/Al2O3複合塗料。將此SiO2/Al2O3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SiO2/Al2O3複合薄膜。 First, 2 ml of Al(OC 3 H 7 ) 3 was added to 300 ml of ethanol solvent and stirred at room temperature for 30 minutes; then 50 ml of Si(OC 2 H 5 ) 4 , 50 ml of C 2 H 5 Si was added. (OC 2 H 5 ) 3 , 50 ml of H 2 C=CHSi(OCH 3 ) 3 and stirred at room temperature for 30 minutes; then add 10 ml of 10% hydrochloric acid and 15 ml of deionized water, and continue to stir 4 Hour; finally stood at room temperature for 24 hours to form a stable SiO 2 /Al 2 O 3 composite coating. The SiO 2 /Al 2 O 3 composite coating was applied onto the surface of the substrate, and after drying for 30 minutes, a SiO 2 /Al 2 O 3 composite film having high strength and high stability was formed on the surface of the substrate.
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30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10毫升濃度為10%的鹽酸及15毫升去離子水，並持續攪拌4小時後停止攪拌；最後於室溫下靜置24小時便可得到穩定的SiO2/TiO2/Al2O3複合塗料。將此SiO2/TiO2/Al2O3複合塗料塗佈於基材表面，於50℃下加熱3分鐘，即可在基材表面上形成強度好、穩定性高的SiO2/TiO2/Al2O3複合薄膜。 First, 1.5 ml of Al[OCH(CH 3 )C 2 H 5 ] 3 and 1.5 ml of Ti(OCH(CH 3 ) 2 ) 4 were added to 300 ml of ethanol solvent and stirred at room temperature for 30 minutes; secondly, Add 50 ml of Si(OC 2 H 5 ) 4 , 50 ml of H 2 C=CHSi(OC 2 H 5 ) 3 and 50 ml of H 2 C=CHSi(OCH 3 ) 3 and stir at room temperature for 30 minutes; Add 10 ml of 10% hydrochloric acid and 15 ml of deionized water, and continue stirring for 4 hours, then stop stirring. Finally, stand at room temperature for 24 hours to obtain stable SiO 2 /TiO 2 /Al 2 O 3 composite. coating. The SiO 2 /TiO 2 /Al 2 O 3 composite coating is applied to the surface of the substrate and heated at 50 ° C for 3 minutes to form SiO 2 /TiO 2 with good strength and high stability on the surface of the substrate. Al 2 O 3 composite film.
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。 As described above, the coating product obtained by the preparation method of the composite coating of the present invention can be dried at a normal temperature for 30 to 60 minutes after being applied to the surface of the substrate to form a strong and stable one. Composite film.
Claims (7)
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| TW97146429A TWI396722B (en) | 2008-11-28 | 2008-11-28 | Preparation of the composite coatings |
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| TWI396722B true TWI396722B (en) | 2013-05-21 |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1201479A (en) * | 1995-11-09 | 1998-12-09 | 美国3M公司 | Water spreading coating with metal oxide coated silica particle surface |
| TWI261615B (en) * | 2004-12-31 | 2006-09-11 | Ind Tech Res Inst | Hydrophobic structure on the surface of substrate and its manufacturing method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1201479A (en) * | 1995-11-09 | 1998-12-09 | 美国3M公司 | Water spreading coating with metal oxide coated silica particle surface |
| TWI261615B (en) * | 2004-12-31 | 2006-09-11 | Ind Tech Res Inst | Hydrophobic structure on the surface of substrate and its manufacturing method |
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