JP2911378B2 - Manufacturing method of water-repellent composite particles - Google Patents
Manufacturing method of water-repellent composite particlesInfo
- Publication number
- JP2911378B2 JP2911378B2 JP7001182A JP118295A JP2911378B2 JP 2911378 B2 JP2911378 B2 JP 2911378B2 JP 7001182 A JP7001182 A JP 7001182A JP 118295 A JP118295 A JP 118295A JP 2911378 B2 JP2911378 B2 JP 2911378B2
- Authority
- JP
- Japan
- Prior art keywords
- water
- repellent
- composite particles
- particles
- substrate
- 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 - Fee Related
Links
Landscapes
- Glanulating (AREA)
- Surface Treatment Of Glass (AREA)
- Silicon Compounds (AREA)
- Physical Or Chemical Processes And Apparatus (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
Description
【０００１】[0001]
【産業上の利用分野】本発明は、撥水性複合粒子の製造
法およびその得られた該粒子を用いて基材表面に撥水層
を形成する方法に関する。The present invention relates to a method for producing water-repellent composite particles and a method for forming a water-repellent layer on the surface of a substrate using the obtained particles.
【０００２】[0002]
【従来技術】フッ素系樹脂は優れた撥水性を有し防水、
防汚等を目的として多くの分野で実用化されている。し
かしながら、フッ素系樹脂の中で最も撥水性の高いＰＴ
ＦＥでさえ、表面に付着する水滴を完全に防止するほど
の撥水効果はなく、その表面に水滴を残し、そこに付着
するダスト等により表面が汚染されてその撥水効果が著
しく低減されるような問題点がある。PRIOR ART Fluorine resin has excellent water repellency and waterproof,
It has been put to practical use in many fields for antifouling and the like. However, the most water-repellent PT among fluororesins
Even FE does not have a water-repellent effect enough to completely prevent water droplets adhering to the surface, leaving water droplets on the surface and contaminating the surface with dust and the like adhering thereto, thereby significantly reducing the water-repellent effect. There is such a problem.
【０００３】また、フッ素系樹脂は撥水性が高いものほ
ど他の材料との接着性が悪くなるため、基材表面をコー
トすることが非常に困難であり、たとえコートしても摩
擦などに対する耐久性が低いものとなる。従来はＰＴＦ
Ｅ等のシートの片面を金属ナトリウムにより処理して表
面を活性化して接着強度をあげる方法やグロー放電等に
よりＰＴＦＥシート表面を粗面化して、アンカー効果に
より接着強度をあげる方法が用いられてきた。しかしな
がら、このような方法では処理が複雑である上に、ＰＴ
ＦＥシートでは複雑な形状のものに対応することが困難
である。[0003] In addition, the higher the water repellency of the fluororesin, the worse the adhesion to other materials, and it is very difficult to coat the surface of the base material. The property is low. Conventionally, PTF
A method in which one side of a sheet such as E is treated with metallic sodium to activate the surface and increase the adhesive strength, or a method in which the PTFE sheet surface is roughened by glow discharge or the like to increase the adhesive strength by an anchor effect has been used. . However, such a method is complicated in processing and PT
It is difficult for an FE sheet to cope with a complicated shape.
【０００４】[0004]
【問題点を解決するための具体的手段】本発明者らは、
かかる従来技術の問題点に鑑み鋭意検討の結果、低分子
量ＰＴＦＥより機械的強度の大きい粒子上に被覆されて
なる撥水性複合粒子を用いることにより優れた撥水性を
持つことを見出し本発明に到達したものである。[Specific means for solving the problem]
As a result of intensive studies in view of the problems of the prior art, the present inventors have found that using the water-repellent composite particles coated on particles having higher mechanical strength than low-molecular-weight PTFE has excellent water repellency, and reached the present invention. It was done.
【０００５】すなわち本発明は、低分子量ＰＴＦＥを２
５０〜５００℃の温度で溶融液化した後、低分子量ＰＴ
ＦＥより機械的強度が大きい一次粒子を該溶融した液中
に投入して混合、冷却後、解砕または粉砕することを特
徴とする基材表面塗布用撥水性複合粒子の製造法で、ま
た低分子量ＰＴＦＥを加熱、蒸発させたものを低分子量
ＰＴＦＥより機械的強度が大きい一次粒子表面に析出さ
せることにより被覆し、得られた複合粒子を解砕または
粉砕することを特徴とする基材表面塗布用撥水性複合粒
子の製造法であり、さらに、該製造法により得られた撥
水性複合粒子を基材表面にエポキシ樹脂層またはウレタ
ン樹脂層を介して、粗面が形成されるように塗布するこ
とを特徴とする撥水層の形成方法および該製造法により
得られた撥水性複合粒子を樹脂に混合して基材表面に塗
布して硬化させることを特徴とする撥水層の形成方法を
提供するものである。[0005] That is, the present invention relates to low molecular weight PTFE
After being melted and liquefied at a temperature of 50 to 500 ° C., the low molecular weight PT
A method for producing water-repellent composite particles for coating on the surface of a substrate, characterized in that primary particles having higher mechanical strength than FE are put into the molten liquid, mixed, cooled, and then crushed or pulverized. Heating and evaporating high molecular weight PTFE, depositing it on the surface of primary particles having higher mechanical strength than low molecular weight PTFE, coating the obtained composite particles, and crushing or pulverizing the obtained composite particles. And a method for producing water-repellent composite particles, and further, applying the water-repellent composite particles obtained by the production method to a surface of a substrate via an epoxy resin layer or a urethane resin layer so that a rough surface is formed. A method for forming a water-repellent layer, comprising: mixing a water-repellent composite particle obtained by the production method with a resin; applying the mixture to a substrate surface; and curing the mixture. To provide .
【０００６】本発明による撥水性複合粒子を施した基材
表面は表面の粗面化の効果により、水滴と表面との接触
面積が小さくなり、ベースの低分子量ＰＴＦＥ単独より
も撥水性が著しく高くなり、水滴の付着をほぼ完全に防
止できる。また、ＰＴＦＥよりも機械的強度が大きい粒
子を複合しているため、摩擦等の外的な力に対する耐久
性も著しく向上する。[0006] The surface of the substrate coated with the water-repellent composite particles according to the present invention has a small contact area between water droplets and the surface due to the effect of surface roughening, and has significantly higher water repellency than the low molecular weight PTFE alone. Thus, the adhesion of water droplets can be almost completely prevented. In addition, since particles having mechanical strength larger than that of PTFE are compounded, durability against external forces such as friction is significantly improved.
【０００７】さらに強力な撥水性を発現させるため、ま
たは、撥水性材料に透明性を付与する場合には、撥水性
粒子の粒径を１μｍ以下まで小さくすることが必要とな
るがＰＴＦＥ粒子自体は柔らかいために一般の粉砕方法
では、粒子間で融着が起こるなどの理由から１μｍ以下
の粒子を得ることは困難である。そこで、本発明では、
２種類の方法により、１μｍ以下の撥水性微粒子を得る
ことを可能としている。一方は１μｍ以下の微粒子に本
発明における複合化を施すことにより、容易に１μｍ以
下の撥水性微粒子を得るという方法であり、もう一方は
１μｍ以上の粒子に本発明における複合化を施した後
に、粉砕することにより粒子間の融着を防ぎ、１μｍ以
下の撥水性微粒子を得るという方法である。In order to exhibit stronger water repellency or to impart transparency to the water repellent material, it is necessary to reduce the particle size of the water repellent particles to 1 μm or less. Because of the softness, it is difficult to obtain particles of 1 μm or less by a general pulverization method because of the fact that fusion occurs between particles. Therefore, in the present invention,
Two types of methods make it possible to obtain water-repellent fine particles of 1 μm or less. One is a method of easily obtaining water-repellent fine particles of 1 μm or less by subjecting the fine particles of 1 μm or less to complexation in the present invention, and the other is a method of subjecting the fine particles of 1 μm or more to complexation in the present invention. This is a method in which fusion between particles is prevented by pulverization to obtain water-repellent fine particles of 1 μm or less.
【０００８】また、撥水性複合粒子を用いる場合、接着
層が完全に硬化する前に撥水性複合粒子の表面エネルギ
ーの低さゆえに、組成物表面に粒子が浮上してくるた
め、この段階で圧力を加えることにより、粒子が接着層
に食い込み、十分な接着性が得られる。ここでＰＴＦＥ
単独の粒子の場合、粒子に強度が無いため表面の粗面を
維持できない上に食い込みも不十分であるため、接着性
が得られないうえに耐久性も不十分である。When the water-repellent composite particles are used, the particles float on the surface of the composition before the adhesive layer is completely cured due to the low surface energy of the water-repellent composite particles. By adding the particles, the particles penetrate into the adhesive layer, and sufficient adhesiveness can be obtained. Where PTFE
In the case of a single particle, since the particle has no strength, a rough surface cannot be maintained and the bite is insufficient, so that adhesion is not obtained and durability is also insufficient.
【０００９】本発明にて使用する低分子量ＰＴＦＥとし
ては本出願人が、すでに提案した製造法（特公平１−４
９４０４号）で得られる平均分子量が５００〜１５００
０のＰＴＦＥ、好ましくは５００〜１５００のＰＴＦＥ
を使用する。平均分子量が１５０００を越えるものは溶
融粘度が高く、本発明の特徴である粒子との複合化が困
難であるため好ましくない。As the low molecular weight PTFE used in the present invention, the production method already proposed by the present applicant (JP-B 1-4)
9404) is 500 to 1500.
0 PTFE, preferably 500-1500 PTFE
Use Those having an average molecular weight of more than 15,000 are not preferred because the melt viscosity is high and it is difficult to form a composite with the particles which is a feature of the present invention.
【００１０】本発明の高強度撥水性複合粒子を形成する
ために用いる粒子としてはＰＴＦＥよりも強度の大きい
ものであればよい。例えば、ＳｉＯ2 、Ａｌ2 Ｏ3 等の
セラミック系材料やＦｅ、Ｎｉ等の金属材料、エポキシ
樹脂、ポリカーボネート等のポリマー材料、そのほか塗
料原料用顔料やカーボン材料、ＣａＦ2 等の無機化合物
が挙げられる。ただし、多孔質粒子のほうがより強いア
ンカー効果が期待できるため好ましい。これらの粒子の
粒径については０．０１μｍ以上、１ｍｍ以下が好まし
く、これ以上の粒径では複合粒子を基材の表面に被覆し
た場合、撥水効果により水は球状になるものの、粒子間
に水滴が入り込み表面より落下しにくくなることもある
ため好ましくない。The particles used to form the high-strength water-repellent composite particles of the present invention may be any particles having a higher strength than PTFE. For example, ceramic materials such as SiO 2 and Al 2 O 3 , metal materials such as Fe and Ni, polymer materials such as epoxy resin and polycarbonate, and pigments and carbon materials for paint raw materials, and inorganic compounds such as CaF 2 can be used. . However, porous particles are preferable because a stronger anchor effect can be expected. The particle size of these particles is preferably 0.01 μm or more and 1 mm or less. When the particle size is larger than this, when the composite particles are coated on the surface of the base material, water becomes spherical due to the water-repellent effect, but between the particles. It is not preferable because water droplets may enter and hardly fall from the surface.
【００１１】本発明の撥水性複合粒子の作製法について
は、液相で行う方法と気相で行う方法の二種類があり、
液相法では容易に複合粒子が作製できるものの低分子量
ＰＴＦＥを完全に溶融するために系内を２５０℃以上に
保持する必要があるため、樹脂等の耐熱性の低い材料へ
の被覆法としては適さない。そこでもう一つの方法であ
る気相法を用いれば、耐熱性の低い材料への応用も可能
となる。以下、その作製法について詳述する。There are two methods for preparing the water-repellent composite particles of the present invention: a method in a liquid phase and a method in a gas phase.
In the liquid phase method, composite particles can be easily prepared. However, since the inside of the system must be maintained at 250 ° C. or higher in order to completely melt the low molecular weight PTFE, a method for coating a material having low heat resistance such as a resin is as follows. Not suitable. Therefore, if a gas phase method, which is another method, is used, it can be applied to a material having low heat resistance. Hereinafter, the manufacturing method will be described in detail.
【００１２】まず液相法は、低分子量ＰＴＦＥを加熱溶
融し、その中に上記のＰＴＦＥよりも強度の大きい粒子
を投入して、よく混合した後に室温まで冷却する。ここ
で、複合粒子は固結して塊状になるが、これは粉砕機等
で容易に解砕することができる。First, in the liquid phase method, low-molecular-weight PTFE is heated and melted, and particles having a strength higher than that of the above-mentioned PTFE are charged therein, mixed well, and then cooled to room temperature. Here, the composite particles are consolidated into a mass, which can be easily crushed by a crusher or the like.
【００１３】次に気相法であるが、複合化に用いる粒子
中に低分子量ＰＴＦＥを加熱、蒸発させたものを導入
し、粒子表面に低分子量ＰＴＦＥを析出させることによ
り被覆する。その際、粒子が固結する場合もあるが、こ
れは粉砕機等で容易に解砕することができる。Next, in the case of the gas phase method, a material obtained by heating and evaporating low-molecular-weight PTFE is introduced into particles used for compounding, and the particles are coated by depositing low-molecular-weight PTFE on the surface of the particles. At this time, the particles may be solidified, but can be easily broken by a crusher or the like.
【００１４】本発明の撥水性複合粒子により、被覆され
る基材の材質や形状は特に限定はなく、一般に塗装が可
能なものであればどのようなものにでも使用できる。ま
た、接着層についてはエポキシ樹脂、ウレタン樹脂等の
一般の接着や塗装に用いられるものでよい。その接着層
の厚みは使用する複合粒子の半径以上であることが好ま
しく、それ以下であると十分な接着強度が得られない。The material and shape of the substrate to be coated with the water-repellent composite particles of the present invention are not particularly limited, and any material that can be generally coated can be used. Further, the adhesive layer may be an epoxy resin, a urethane resin or the like used for general bonding or painting. The thickness of the adhesive layer is preferably not less than the radius of the composite particles to be used, and if it is less than that, sufficient adhesive strength cannot be obtained.
【００１５】以上のようにして得られた撥水性複合粒子
を用いて基材上に撥水層を形成した撥水性材料は従来の
ものよりも著しく高い撥水性を示し、水滴の付着をほぼ
完全に防止できる。しかも、基材との接着性にも優れて
いる。The water-repellent material obtained by forming a water-repellent layer on a substrate using the water-repellent composite particles obtained as described above exhibits remarkably higher water repellency than conventional ones, and almost completely prevents the attachment of water droplets. Can be prevented. Moreover, the adhesiveness to the substrate is excellent.
【００１６】[0016]
【実施例】以下実施例により本発明を具体的に説明する
が、本発明はかかる実施例により限定されるものではな
い。EXAMPLES The present invention will be specifically described below with reference to examples, but the present invention is not limited to these examples.
【００１７】実施例１〜１８、比較例１〜４ 表１における実施例１〜７は、以下のように実施した。
低分子量ＰＴＦＥを分子量５００と１５００のものは２
６０℃で、分子量１５０００のものは４５０℃で加熱溶
融して、その中に低分子量ＰＴＦＥよりも機械的強度の
大きい粒子（以下、複合化材と呼ぶ）を投入し、十分に
混合した後、室温まで冷却し、固結した複合粒子を乳鉢
により解砕することにより撥水性複合粒子を得た。次に
ガラス基板（実施例２〜４、７、比較例１はアルミ基
板、実施例５、６はニッケル基板）上に一液性エポキシ
樹脂（チバガイギー製：ＸＮＲ３５０１）をコートし、
その上に上記の方法で得られた撥水性複合粒子を表面が
完全に覆われるように、過剰量を均一に散布した。樹脂
層が硬化する前にこの表面にガラス板を重ねて圧力を加
えた後に１５０℃にて樹脂層を完全に硬化させ、表面の
余分な撥水性粒子を除去することにより、撥水性材料
（塗膜）を得た。この撥水性材料の撥水性の評価を直径
２ｍｍの水滴に対する接触角、水滴の落下しやすさを表
す転落角の測定により、また、耐久性の評価を粘着テー
プによる剥離テストにより実施した。Examples 1 to 18 and Comparative Examples 1 to 4 Examples 1 to 7 in Table 1 were carried out as follows.
Low molecular weight PTFE having a molecular weight of 500 or 1500 has 2
At 60 ° C., those having a molecular weight of 15000 are heated and melted at 450 ° C., and particles having a higher mechanical strength than the low-molecular-weight PTFE (hereinafter, referred to as a composite material) are put therein, and after sufficiently mixed, The mixture was cooled to room temperature, and the consolidated composite particles were crushed with a mortar to obtain water-repellent composite particles. Next, a one-component epoxy resin (XNR3501 manufactured by Ciba-Geigy) was coated on a glass substrate (Examples 2 to 4 and 7, Comparative Example 1 was an aluminum substrate, and Examples 5 and 6 were nickel substrates).
An excess amount of the water-repellent composite particles obtained by the above method was evenly sprayed thereon such that the surface was completely covered. Before the resin layer is cured, a glass plate is overlaid on the surface, pressure is applied thereto, and the resin layer is completely cured at 150 ° C., and excess water-repellent particles on the surface are removed. Film). The water repellency of this water repellent material was evaluated by measuring a contact angle with respect to a water drop having a diameter of 2 mm and a falling angle representing the ease of dropping the water drop, and the durability was evaluated by a peel test using an adhesive tape.
【００１８】表１の比較例１は粒径１μｍの純粋な低分
子量ＰＴＦＥ粒子のみで、実施例１〜７と同様に撥水性
材料を形成し、それを評価したものである。実施例１〜
７と、比較例１を比較すると、接触角はどの材料も１６
０゜と大きいが、転落角と剥離試験後の接触角で差がみ
られ、比較例１は転落角が大きく、剥離試験により簡単
に劣化することがわかる。すなわち、実施例１〜７のほ
うが撥水性および耐久性が優れていると考えられる。Comparative Example 1 in Table 1 was formed by forming a water-repellent material in the same manner as in Examples 1 to 7 using only pure low-molecular-weight PTFE particles having a particle size of 1 μm and evaluating the same. Example 1
7 and Comparative Example 1, the contact angle was 16 for all materials.
Although it was as large as 0 °, a difference was observed between the falling angle and the contact angle after the peeling test. It can be seen that Comparative Example 1 had a large falling angle and was easily deteriorated by the peeling test. That is, it is considered that Examples 1 to 7 have better water repellency and durability.
【００１９】[0019]
【表１】 [Table 1]
【００２０】表２における実施例８〜１６は、以下のよ
うに実施した。まず、実施例１〜７と同様の方法によ
り、撥水性複合粒子を調整した。この撥水性複合粒子を
有機溶媒（酢酸ブチル）と１：１の割合で混合する。こ
れに一液性エポキシ樹脂（チバガイギー製：ＸＮＲ３５
０１）を添加し十分に混合して撥水性樹脂とした。Examples 8 to 16 in Table 2 were carried out as follows. First, water-repellent composite particles were prepared in the same manner as in Examples 1 to 7. The water-repellent composite particles are mixed with an organic solvent (butyl acetate) at a ratio of 1: 1. Add one-part epoxy resin (Ciba Geigy: XNR35)
01) was added and mixed well to obtain a water-repellent resin.
【００２１】次に、作成した撥水性樹脂をガラス基板上
に塗布し、塗板は１５０℃で乾燥させ樹脂層を完全に硬
化させる。次に、このようにして得た撥水性材料（塗
膜）の直径２ｍｍの水滴に対する接触角の測定を行い、
また、この撥水性材料表面の機械的な耐久性試験は、図
１に示した機械的耐久性試験装置を用いて測定した。攪
拌機４に柄を切った歯ブラシ２を用いて、台秤３に基板
１をセットし、基板材料表面上約５００ｇの負荷で回転
させた後、再び直径２ｍｍの水滴に対する接触角を測定
して、試験前の接触角と比較した。実施例８、１０、お
よび１３の結果は、図２に歯ブラシの回転数と接触角と
の関係で示した。Next, the prepared water-repellent resin is applied on a glass substrate, and the coated plate is dried at 150 ° C. to completely cure the resin layer. Next, the contact angle of the water-repellent material (coating film) thus obtained with respect to a water droplet having a diameter of 2 mm was measured.
The mechanical durability test on the surface of the water-repellent material was measured using the mechanical durability test apparatus shown in FIG. The substrate 1 was set on the platform scale 3 using the toothbrush 2 having the handle cut into the stirrer 4 and rotated at a load of about 500 g on the surface of the substrate material. It was compared with the previous contact angle. The results of Examples 8, 10, and 13 are shown in FIG. 2 in the relationship between the number of rotations of the toothbrush and the contact angle.
【００２２】表２における比較例３は低分子量ＰＴＦＥ
のみ、比較例４は低分子量ＰＴＦＥとゼオライトの単純
な混合物をそれぞれ、実施例８〜１６と同様の方法によ
り、撥水性材料（塗膜）とし、評価したものである。そ
の結果は図３に示した。Comparative Example 3 in Table 2 shows low molecular weight PTFE
Only in Comparative Example 4, a simple mixture of low-molecular-weight PTFE and zeolite was evaluated as a water-repellent material (coating) in the same manner as in Examples 8 to 16, respectively. The results are shown in FIG.
【００２３】図２と図３および表２中の各実施例、比較
例を比較すると、明らかに本発明の撥水性複合粒子が機
械的な耐久性において優位性を有することがわかる。表
２における実施例１７は複合化材に粒径８μｍのゼオラ
イトを用い、実施例１〜７と同様の方法により、撥水性
複合粒子を調整し、次にこの撥水性複合粒子を比較例２
と同様の方法により、粉砕して粒径を０．２μｍとした
ものである。さらに、実施例８〜１６と同様の方法によ
り、撥水性材料（塗膜）とし、評価した。A comparison of the examples and comparative examples in FIGS. 2 and 3 and Table 2 clearly shows that the water-repellent composite particles of the present invention have superior mechanical durability. In Example 17 in Table 2, water-repellent composite particles were prepared in the same manner as in Examples 1 to 7, using zeolite having a particle size of 8 μm as the composite material.
In the same manner as described above, the powder was pulverized to a particle size of 0.2 μm. Furthermore, a water-repellent material (coating) was evaluated in the same manner as in Examples 8 to 16, and evaluated.
【００２４】ここで、実施例１７と実施例１２そして比
較例２を比較すると明らかなように本発明は、１μｍ以
下の撥水性微粒子を得る方法としても有効である。表２
における実施例１８は、実施例１で得た供試体を実施例
８〜１７と同様の機械的耐久性試験により、評価したも
のである。Here, as is clear from comparison between Example 17 and Example 12 and Comparative Example 2, the present invention is also effective as a method for obtaining water-repellent fine particles of 1 μm or less. Table 2
In Example 18, the specimen obtained in Example 1 was evaluated by the same mechanical durability test as in Examples 8 to 17.
【００２５】[0025]
【表２】 [Table 2]
【００２６】[0026]
【発明の効果】従来の複雑な方法で製造していた撥水性
材料を、本発明による撥水性複合粒子を用いることによ
り、容易に防水、防汚等に優れた撥水性材料を得ること
を可能にした。By using the water-repellent composite particles according to the present invention, a water-repellent material excellent in waterproofness, stain-proofing and the like can be easily obtained from the water-repellent material produced by the conventional complicated method. I made it.
【図１】歯ブラシによる機械的強度試験装置を示す。FIG. 1 shows a mechanical strength test device using a toothbrush.
【図２】実施例８、１０、１３の撥水性材料に対する歯
ブラシの回転数と接触角との関係を示す。FIG. 2 shows the relationship between the rotation speed of the toothbrush and the contact angle for the water-repellent materials of Examples 8, 10 and 13.
【図３】比較例３、４の撥水性材料に対する歯ブラシの
回転数と接触角との関係を示す。FIG. 3 shows the relationship between the rotation speed of the toothbrush and the contact angle for the water-repellent materials of Comparative Examples 3 and 4.
１．基板 ２．ブラシ ３．台秤 ４．攪拌機 1. Substrate 2. Brush 3 Platform scale 4. Stirrer
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ // Ｃ０９Ｋ 3/18 １０２ Ｃ０９Ｋ 3/18 １０２ (72)発明者 喜田 康 山口県宇部市大字沖宇部5253番地 セン トラル硝子株式会社宇部研究所内 (56)参考文献 特開 昭63−312989（ＪＰ，Ａ) 特開 平２−82455（ＪＰ，Ａ) 特開 平７−90691（ＪＰ，Ａ) 特公 昭45−40790（ＪＰ，Ｂ１) (58)調査した分野(Int.Cl.6，ＤＢ名) B01J 2/00 B01J 19/00 C09K 3/18 C25D 15/00 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 6 Identification code FI // C09K 3/18 102 C09K 3/18 102 (72) Inventor Yasushi Kida 5253 Oki Ube, Daiji, Ube City, Yamaguchi Prefecture Central Glass Stock (56) References JP-A-63-312989 (JP, A) JP-A-2-82455 (JP, A) JP-A-7-90691 (JP, A) JP-B-45-40790 (JP) , B1) (58) Fields investigated (Int. Cl. 6 , DB name) B01J 2/00 B01J 19/00 C09K 3/18 C25D 15/00
Claims (4)
温度で溶融液化した後、低分子量ＰＴＦＥより機械的強
度が大きい一次粒子を該溶融した液中に投入して混合、
冷却後、解砕または粉砕することを特徴とする基材表面
塗布用撥水性複合粒子の製造法。1. After low-molecular-weight PTFE is melted and liquefied at a temperature of 250 to 500 ° C., primary particles having higher mechanical strength than the low-molecular-weight PTFE are charged into the molten liquid and mixed.
A method for producing water-repellent composite particles for coating on the surface of a substrate, comprising crushing or pulverizing after cooling.
のを低分子量ＰＴＦＥより機械的強度が大きい一次粒子
表面に析出させることにより被覆し、得られた複合粒子
を解砕または粉砕することを特徴とする基材表面塗布用
撥水性複合粒子の製造法。2. A method of heating and evaporating low-molecular-weight PTFE, coating it by depositing it on primary particle surfaces having higher mechanical strength than low-molecular-weight PTFE, and crushing or pulverizing the obtained composite particles. For producing water-repellent composite particles for coating on a substrate surface.
より得られた撥水性複合粒子を基材表面にエポキシ樹脂
層またはウレタン樹脂層を介して、粗面が形成されるよ
うに塗布することを特徴とする撥水層の形成方法。3. The water-repellent composite particles obtained by the production method according to claim 1 or 2 are applied to the surface of a substrate via an epoxy resin layer or a urethane resin layer so that a rough surface is formed. A method for forming a water-repellent layer, comprising:
より得られた撥水性複合粒子を樹脂に混合して基材表面
に塗布して硬化させることを特徴とする撥水層の形成方
法。4. A method for forming a water-repellent layer, wherein the water-repellent composite particles obtained by the production method according to claim 1 are mixed with a resin, applied to the surface of a substrate, and cured. .
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7001182A JP2911378B2 (en) | 1994-01-26 | 1995-01-09 | Manufacturing method of water-repellent composite particles |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP721694 | 1994-01-26 | ||
| JP6-7216 | 1994-01-26 | ||
| JP7001182A JP2911378B2 (en) | 1994-01-26 | 1995-01-09 | Manufacturing method of water-repellent composite particles |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH07251060A JPH07251060A (en) | 1995-10-03 |
| JP2911378B2 true JP2911378B2 (en) | 1999-06-23 |
Family
ID=26334363
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7001182A Expired - Fee Related JP2911378B2 (en) | 1994-01-26 | 1995-01-09 | Manufacturing method of water-repellent composite particles |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2911378B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0825241B1 (en) | 1996-08-16 | 2003-03-26 | Nippon Telegraph And Telephone Corporation | Water repellent coating composition, method for preparing the same, and coating films and coated articles using the same |
| WO2003059812A1 (en) * | 2002-01-11 | 2003-07-24 | Mikuni Shikiso Kabushiki Kaisha | Carbonaceous material and dispersion containing the same |
-
1995
- 1995-01-09 JP JP7001182A patent/JP2911378B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH07251060A (en) | 1995-10-03 |
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