JPH0258986B2 - - Google Patents
Info
- Publication number
- JPH0258986B2 JPH0258986B2 JP29048786A JP29048786A JPH0258986B2 JP H0258986 B2 JPH0258986 B2 JP H0258986B2 JP 29048786 A JP29048786 A JP 29048786A JP 29048786 A JP29048786 A JP 29048786A JP H0258986 B2 JPH0258986 B2 JP H0258986B2
- Authority
- JP
- Japan
- Prior art keywords
- film
- water
- coating agent
- contact
- curing
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired
Links
- 238000000034 method Methods 0.000 claims description 13
- 239000011248 coating agent Substances 0.000 claims description 9
- 229910000077 silane Inorganic materials 0.000 claims description 6
- -1 silane compound Chemical class 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 239000000758 substrate Substances 0.000 claims description 4
- 239000010936 titanium Substances 0.000 claims description 3
- 239000003054 catalyst Substances 0.000 claims description 2
- 229910052719 titanium Inorganic materials 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 21
- 238000007654 immersion Methods 0.000 description 5
- 239000000428 dust Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 229910052782 aluminium Inorganic materials 0.000 description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 2
- 239000012298 atmosphere Substances 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 2
- 239000012530 fluid Substances 0.000 description 2
- 125000000956 methoxy group Chemical group [H]C([H])([H])O* 0.000 description 2
- 238000004528 spin coating Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000003746 surface roughness Effects 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 238000005299 abrasion Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 238000007664 blowing Methods 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- 238000003618 dip coating Methods 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 150000004756 silanes Chemical class 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
Landscapes
- Application Of Or Painting With Fluid Materials (AREA)
- Surface Treatment Of Glass (AREA)
- Paints Or Removers (AREA)
Description
〔産業上の利用分野〕
本発明は、耐熱性、耐薬品性、耐沸騰水性など
に優れ、基板との密着性の優れた無機系コーテイ
ング剤を均一な皮膜として形成する方法を提供す
るものである。
〔発明の背景〕
従来、一般式
RxSi（OR）4-x
（式中、Ｒは−CH3、
[Field of Industrial Application] The present invention provides a method for forming a uniform film of an inorganic coating agent that has excellent heat resistance, chemical resistance, boiling water resistance, etc., and excellent adhesion to a substrate. be. [Background of the Invention] Conventionally, the general formula R x Si (OR) 4-x (wherein R is -CH 3 ,
本発明は以下の構造式で示されるシラン化合物
（CH3）xSi（OCH3）4-x
（式中、ｘは１または２を表わす）
の部分加水分解物を主成分として含む組成物に、
アルコキシチタンを触媒として添加した無機系コ
ーテイング剤の皮膜形成方法について、新規の製
膜方法を提供することを目的とするものである。
本発明の方法によれば、上記無機系コーテイン
グ剤は、優れた耐熱性、耐摩耗性、高硬度な皮膜
特性を維持し、かつ、優れた表面平滑性・均一性
とを有する皮膜として提供される。
〔発明の構成〕
本発明に用いられる上記無機系コーテイング剤
は、従来、これをガラス、金属、プラスチツクな
どの基板に、刷毛塗り、回転塗布、浸漬塗布、ス
プレーなどの方法により湿潤膜として形成したの
ち、乾燥・硬化させることにより皮膜としてい
る。
本発明は、上記皮膜形成プロセスにおいて、湿
潤膜が乾燥する前にこれを高濃度の水分、例えば
水または水を含む液体に接触する処理を加えるこ
とにより、乾燥・硬化したあとの皮膜の均一性・
平滑性が著しく向上することを見い出したことに
基づいている。
本発明において、「高濃度の水分を接触させる」
とは、例えば水または水を含む液体と接触させる
処理を意味し、この処理には
(1) 水中に浸漬させる
(2) スチームと接触させる
(3) 加湿器などによる霧状の水と接触させる
などの方法が使用できる。
本発明に用いられる無機系コーテイング剤の湿
潤膜は、大気中の水分と接触すると直ちにその表
面が白く不透明化し、これを乾燥・硬化させる
と、ふたたび透明な皮膜となる性質があることは
従来より知られていたが、ここで驚くべきこと
に、例えば水中にこの湿潤膜を浸漬するような急
激な高濃度の水分との接触による湿潤膜の不透明
化は、結果として皮膜の平滑化・均一化をもたら
すことを見い出した。
この現象の原理については十分に明らかではな
いが、上記湿潤膜が水中浸漬のような方法により
高濃度の水と急激に接触することにより、その表
面に非水溶性で非流動性のスキン層が生成する一
方、その内部が流動性の良好な状態に保たれてい
るため、乾燥・硬化過程でのレベリングが容易と
なり、その結果、皮膜の平滑化・均一化が起こる
ものと考えられる。同時に、一般に、水中の塵・
ゴミなどの除去は簡単であるからそのような水中
で表面凝固させて非粘着性となつた皮膜はその表
面にゴミの付着がなく、また大気中での乾燥・硬
化過程でゴミが付着しにくくなることも表面の平
滑性を良くする原因であると考えられる。
〔実施例〕
以下、本発明を実施例により詳細に説明する。
実施例 １
CH3Si（OCH3）3400ｇ、（CH3）2Si（OCH3）2200
ｇ、
The present invention relates to a composition containing as a main component a partial hydrolyzate of a silane compound (CH 3 ) x Si(OCH 3 ) 4-x (in the formula, x represents 1 or 2) represented by the following structural formula. ,
The purpose of this invention is to provide a new method for forming a film using an inorganic coating agent containing alkoxy titanium as a catalyst. According to the method of the present invention, the inorganic coating agent is provided as a film that maintains excellent heat resistance, abrasion resistance, and high hardness film properties, and has excellent surface smoothness and uniformity. Ru. [Structure of the Invention] The above-mentioned inorganic coating agent used in the present invention has conventionally been formed as a wet film on a substrate such as glass, metal, or plastic by a method such as brush coating, spin coating, dip coating, or spraying. It is then dried and cured to form a film. The present invention improves the uniformity of the film after drying and curing by adding a treatment in which the wet film is brought into contact with a high concentration of water, such as water or a liquid containing water, before drying in the film forming process.・
This is based on the discovery that smoothness is significantly improved. In the present invention, "contact with high concentration moisture"
means, for example, a treatment in which the product is brought into contact with water or a liquid containing water, and this treatment includes (1) immersion in water, (2) contact with steam, and (3) contact with water mist from a humidifier. Methods such as this can be used. It has been known from the past that the surface of the wet film of the inorganic coating agent used in the present invention immediately becomes white and opaque when it comes into contact with moisture in the atmosphere, and when it dries and hardens, it becomes a transparent film again. However, what is surprising here is that the opacity of the wet film due to rapid contact with high-concentration water, such as when the wet film is immersed in water, results in smoothing and homogenization of the film. I found that it brings about Although the principle behind this phenomenon is not fully clear, when the above-mentioned wet film rapidly comes into contact with high-concentration water by a method such as immersion in water, a water-insoluble and non-fluid skin layer forms on its surface. While forming, the inside of the film is maintained in a fluid state, which facilitates leveling during the drying and curing process, and as a result, it is thought that the film becomes smooth and uniform. At the same time, in general, dust and
Since it is easy to remove dust, etc., a film that has become non-adhesive by coagulating its surface in water will not have dust adhering to its surface, and it will also be difficult for dust to adhere to it during the drying and curing process in the atmosphere. This is also thought to be a cause of improving the surface smoothness. [Example] Hereinafter, the present invention will be explained in detail with reference to Examples. Example 1 CH 3 Si (OCH 3 ) 3 400g, (CH 3 ) 2 Si (OCH 3 ) 2 200
g,
【式】100ｇか
らなるシラン化合物の混合物に、純水100ｇと氷
酢酸10ｇの混合物を滴下して室温で反応させた。
反応は急激な発熱を伴つて進行し、数分〜数10分
で終了する。これに稀釈剤としてメタノール150
ｇとダイアセトンアルコール50ｇを加え、シラン
加水分解物（）をえた。このシラン加水分解物
（）にテトラブトキシチタン（TBT）、Ti
（OC4H9）4を、シラン化合物の５重量％に相当す
る量で添加した。反応は急激で、激しい発熱を伴
つた。
この反応生成物をアルミニウム円盤に回転塗布
法により塗布し、直ちに、清浄な純水に浸漬し
た。この浸漬約30〜60秒で表面に皮膜が形成され
たところで、水から取り出し回転遠心力でその皮
膜の表面に付着している水分を除去する。この場
合、水と反応してできた表面の皮膜は袋状になつ
て膜を形成しており、それが回転遠心力によつて
外周方向に押しやられるため、膜の内面にレベリ
ング効果をもたらし、円の外周の末端の部分が破
られて未反応の液が吹き飛ばされる効果がある。
この効果は回転のスピードを調整したり、純水に
浸漬する時間を増減することによつて調節できる
ものである。その後、150℃で２時間硬化を行つ
た。硬化した皮膜は、鉛筆硬さが9Hと硬く、ク
ラツクのない膜厚が0.05mmで表面粗さRaが0.02ミ
クロンと平滑な均一透明膜であり、アルミ基板の
硬度や耐スクラツチ性が著しく改善された。
なお、本実施例１において浸水処理を行わない
ほかは実施例１と同様とした場合には表面粗さ
Raは0.08ミクロンとやや大きい値であつた。
実施例 ２
CH3Si（OCH3）340ｇ、（CH3）2Si（OCH3）220ｇ、
[Formula] A mixture of 100 g of pure water and 10 g of glacial acetic acid was added dropwise to a mixture of 100 g of a silane compound and reacted at room temperature.
The reaction proceeds with rapid exotherm and is completed in a few minutes to several tens of minutes. Add 150 methanol to this as a diluent.
g and 50 g of diacetone alcohol were added to obtain a silane hydrolyzate (). This silane hydrolyzate () contains tetrabutoxytitanium (TBT) and Ti.
(OC 4 H 9 ) 4 was added in an amount corresponding to 5% by weight of the silane compound. The reaction was rapid and accompanied by a strong exotherm. This reaction product was applied to an aluminum disk by a spin coating method, and immediately immersed in clean pure water. When a film is formed on the surface after about 30 to 60 seconds of immersion, it is taken out of the water and the water adhering to the surface of the film is removed by rotating centrifugal force. In this case, the film on the surface that reacts with water becomes bag-shaped and forms a film, which is pushed toward the outer circumference by the rotating centrifugal force, creating a leveling effect on the inner surface of the film. This has the effect of blowing away unreacted liquid by breaking the outer edge of the circle.
This effect can be adjusted by adjusting the rotation speed or increasing or decreasing the immersion time in pure water. Thereafter, curing was performed at 150°C for 2 hours. The cured film has a pencil hardness of 9H, a smooth, uniform transparent film with a crack-free film thickness of 0.05 mm and a surface roughness Ra of 0.02 micron, which significantly improves the hardness and scratch resistance of aluminum substrates. Ta. In addition, if this Example 1 is the same as Example 1 except that the water immersion treatment is not performed, the surface roughness
Ra was a rather large value of 0.08 micron. Example 2 CH3Si ( OCH3 ) 3 40g, ( CH3 ) 2Si ( OCH3 ) 2 20g,
以上述べたところから明らかなように、本発明
によれば、耐熱性、耐薬品性、耐沸騰水性などに
優れ、耐摩耗性で高硬度の無機系コーテイング皮
膜を、表面平滑性・均一性に優れた形で形成する
方法が提供される。
As is clear from the above description, according to the present invention, an inorganic coating film with excellent heat resistance, chemical resistance, boiling water resistance, etc., wear resistance, and high hardness can be used to improve surface smoothness and uniformity. A method of forming an improved shape is provided.
Claims (1)
て含む組成物に、アルコキシチタンを硬化触媒と
して添加した無機系コーテイング剤の皮膜形成方
法において、基板上に上記コーテイング剤を塗布
したのち、高濃度の水分と接触させ、ついで乾
燥・硬化させることを特徴とする皮膜形成方法。[Claims] 1. A partial hydrolyzate of a silane compound (CH 3 ) x Si(OCH 3 ) 4-x (in the formula, x represents 1 or 2) represented by the following structural formula or a mixture thereof. In a method for forming a film of an inorganic coating agent in which alkoxy titanium is added as a curing catalyst to a composition containing it as a main component, the coating agent is applied onto a substrate, and then brought into contact with high concentration moisture, followed by drying and curing. A film forming method characterized by the following.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29048786A JPS63143978A (en) | 1986-12-08 | 1986-12-08 | Film forming method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP29048786A JPS63143978A (en) | 1986-12-08 | 1986-12-08 | Film forming method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63143978A JPS63143978A (en) | 1988-06-16 |
| JPH0258986B2 true JPH0258986B2 (en) | 1990-12-11 |
Family
ID=17756657
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP29048786A Granted JPS63143978A (en) | 1986-12-08 | 1986-12-08 | Film forming method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS63143978A (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2876068B2 (en) * | 1989-12-19 | 1999-03-31 | 住友精化株式会社 | How to prevent mold from building materials |
| US5508062A (en) * | 1994-12-02 | 1996-04-16 | Dow Corning Corporation | Method for forming an insoluble coating on a substrate |
| KR102882355B1 (en) * | 2019-02-13 | 2025-11-10 | 케메탈 게엠베하 | An improved method for applying a silane-based coating to a solid surface, particularly a metal surface. |
-
1986
- 1986-12-08 JP JP29048786A patent/JPS63143978A/en active Granted
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63143978A (en) | 1988-06-16 |
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