JPH0692501B2 - Filler for synthetic resin, method for producing the same, and synthetic resin using the same - Google Patents
Filler for synthetic resin, method for producing the same, and synthetic resin using the sameInfo
- Publication number
- JPH0692501B2 JPH0692501B2 JP63166128A JP16612888A JPH0692501B2 JP H0692501 B2 JPH0692501 B2 JP H0692501B2 JP 63166128 A JP63166128 A JP 63166128A JP 16612888 A JP16612888 A JP 16612888A JP H0692501 B2 JPH0692501 B2 JP H0692501B2
- Authority
- JP
- Japan
- Prior art keywords
- synthetic resin
- fine particles
- silane
- fiber
- oxide
- 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
- Compositions Of Macromolecular Compounds (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
Description
【発明の詳細な説明】 産業上の利用分野 本発明は、合成樹脂の改質あるいは増量等に用いる合成
樹脂用充填材とその製造方法およびそれを用いた合成樹
脂に関するものである。Description: TECHNICAL FIELD The present invention relates to a synthetic resin filler used for modifying or increasing the amount of a synthetic resin, a method for producing the same, and a synthetic resin using the same.
従来の技術 従来合成樹脂の改質あるいは増量は、一般にSiO2やAl2O
3のような酸化物、あるいはFeやAlの微粒子や繊維を樹
脂中に分散する方法が用いられている。Conventional technology Conventional synthetic resins are generally modified or increased in volume with SiO 2 or Al 2 O.
A method of dispersing oxides such as 3 or fine particles or fibers of Fe or Al in a resin is used.
発明が解決しようとする課題 しかしながら、この方法では製造が容易である反面、充
填材は樹脂中に単に混ざっているだけであり、長時間使
用していると微粒子や繊維表面より樹脂材料が剥離して
しまいひび割れや白濁が生じる欠点があった。DISCLOSURE OF THE INVENTION Problems to be Solved by the Invention However, while this method is easy to manufacture, the filler is simply mixed in the resin, and when used for a long time, the resin material peels from the fine particles or the fiber surface. There was a defect that it caused cracks and white turbidity.
本発明の目的は、充填用の微粒子や繊維の表面に界面活
性剤を化学結合することにより、長期間使用しても品質
の劣化しない合成樹脂を製造する方法を提供し、合成樹
脂の信頼性を向上させることにある。An object of the present invention is to provide a method for producing a synthetic resin which does not deteriorate in quality even after long-term use by chemically bonding a surfactant to the surface of fine particles or fibers for filling, and the reliability of the synthetic resin is improved. To improve.
課題を解決するための手段 本発明は、微粒子や繊維の表面に直接シラン界面活性剤
を単分子膜状に化学吸着させる工程を含む合成樹脂用充
填材の製造方法とその方法を用いて製造された充填材、
さらに前記単分子膜が形成された充填材を樹脂原料に分
散させたことを特徴とする合成樹脂を提供するものであ
る。Means for Solving the Problems The present invention is manufactured by using a method for manufacturing a synthetic resin filler including a step of chemically adsorbing a silane surfactant in the form of a monomolecular film directly on the surface of fine particles or fibers, and a method for manufacturing the same. Filling material,
Further, the present invention provides a synthetic resin characterized in that the filler having the monomolecular film formed thereon is dispersed in a resin raw material.
作用 従って、本発明の方法を用いれば、充填材表面に直接化
学結合した状態の単分子状の有機薄膜を形成できるの
で、単分子状の有機薄膜は剥離することも無く、樹脂と
の密着性を極めて高く保つことができる作用がある。Action Therefore, by using the method of the present invention, it is possible to form a monomolecular organic thin film in a state of being chemically bonded directly to the surface of the filler, so that the monomolecular organic thin film does not peel off and the adhesiveness to the resin is improved. Has the effect of keeping the value extremely high.
実施例 以下、実施例を第1〜4図を用いて説明する。例えば、
第1図に示すように、大きさが数ミクロン程度の微粒子
または繊維1(アルミナ(Al2O3)、シリカ、ガラス、F
e2O3、あるいはFe3O4等の酸化物やFe、Al等の金属の微
粒子または繊維)の表面に、化学吸着法により全面シラ
ン界面活性剤を吸着反応させてシラン界面活性剤よりな
る単分子の保護膜2を形成する。例えば、シラン界面活
性剤としてCH3−(CH2)n−SiCl3(n:整数。10〜25程
度が最も扱いやすい)を用い、2×10-3〜5×10-2Mol/
l程度の濃度で溶かした80%n−ヘキサン、12%四塩化
炭素、8%クロロホルム溶液を調整し、前記微粒子また
は繊維1を浸漬する。このとき、金属の微粒子または繊
維では表面にナチュラルオキサイドが形成されており、
また酸化物は当然表面が酸化物であるためいずれも表面
には−OH基が含まれている。従って、−SiCl3基と−OH
が脱塩酸反応して の結合が生成され、シラン界面活性剤による単分膜3が
磁性体微粒子表面に1層(20〜30Åの厚み)形成され
る。(第2図) 次に、この微粒子や繊維を合成樹脂材料(例えば、アク
リル、またはポリカーボネート、塩化ビニル、ポリアミ
ド、ポリエステル樹脂材料)中に均一に分散した後、全
体を硬化すると合成樹脂、即ちいわゆる繊維強化樹脂
(FRP)が製造できる。Example Hereinafter, an example will be described with reference to FIGS. For example,
As shown in FIG. 1, fine particles or fibers 1 (alumina (Al 2 O 3 ), silica, glass, F
e 2 O 3 or oxide such as Fe 3 O 4 or fine particles or fibers of metal such as Fe or Al) is made up of silane surfactant by adsorbing and reacting the entire surface with silane surfactant by chemisorption method A monomolecular protective film 2 is formed. For example, CH 3 — (CH 2 ) n-SiCl 3 (n: integer; about 10 to 25 is the easiest to handle) is used as the silane surfactant, and 2 × 10 −3 to 5 × 10 −2 Mol /
A solution of 80% n-hexane, 12% carbon tetrachloride and 8% chloroform dissolved at a concentration of about 1 is prepared and the fine particles or fiber 1 is immersed. At this time, natural oxide is formed on the surface of the metal fine particles or fibers,
In addition, since the surface of the oxide is of course an oxide, the surface of each of them contains an -OH group. Therefore, --SiCl 3 group and --OH
Dehydrochlorination reaction Are formed, and a monolayer 3 made of a silane surfactant is formed on the surface of the magnetic fine particles (thickness of 20 to 30 Å). (FIG. 2) Next, the fine particles and fibers are uniformly dispersed in a synthetic resin material (for example, acrylic, polycarbonate, vinyl chloride, polyamide, polyester resin material), and then the whole is cured to obtain a synthetic resin, that is, a so-called Fiber reinforced resin (FRP) can be manufactured.
なお、シラン界面活性材として樹脂材料としてCH2=CH
−(CH2)n−SiCl3またはCH=CH−(CH2)n−SiCl
3(n:整数。10〜25程度が最も扱いやすい)を用いた場
合には、表面にCH2=CH−基4またはCH=CH−基が並ん
だ状態の単分子膜3′を形成できる。(第3図)従って
これら充填材は直接アクリル、またはポリカーボネー
ト、塩化ビニル、ポリアミド、ポリエステル等の樹脂材
料と化学結合を形成できるので密着性を大幅に向上でき
る。In addition, CH 2 = CH as the resin material as the silane surfactant
- (CH 2) n-SiCl 3 or CH = CH- (CH 2) n -SiCl
When 3 (n: integer; about 10 to 25 is the easiest to handle), it is possible to form a monomolecular film 3 ′ in which CH 2 ═CH— groups 4 or CH═CH— groups are arranged on the surface. . (FIG. 3) Accordingly, these fillers can directly form a chemical bond with a resin material such as acrylic, polycarbonate, vinyl chloride, polyamide, polyester, etc., so that the adhesiveness can be greatly improved.
また、樹脂材料としてフッ素樹脂を用いる場合には、シ
ラン界面活性剤として末端に−CF3基等のフッ素原子を
含む物質(例えば、CF3−(CH2)n−SiCl3(n:整数。1
0〜25程度が最も扱いやすい))用いると第4図に示す
ように−CF基5が表面に並んだ状態の単分子膜を形成で
き、フッ素樹脂との相溶性を向上できる。When a fluororesin is used as the resin material, a substance containing a fluorine atom such as a —CF 3 group at the end as a silane surfactant (for example, CF 3 — (CH 2 ) n-SiCl 3 (n: integer. 1
If 0 to 25 is the easiest to handle)), a monomolecular film in which -CF groups 5 are arranged on the surface can be formed as shown in FIG. 4, and the compatibility with the fluororesin can be improved.
さらにまた、微粒子或は繊維としてシリカを用い、合成
樹脂材料としてアクリル、またはポリカーボネートを用
いれば極めて透明性がよく信頼性の高いガラス様樹脂板
等が得られる。Furthermore, when silica is used as the fine particles or fibers and acrylic or polycarbonate is used as the synthetic resin material, a highly transparent and highly reliable glass-like resin plate or the like can be obtained.
なお、化学吸着用の材料としては、−OH基に対して結合
性を有する基 を含んでいれば、実施例で示したシラン系界面活性剤に
限定されるものではない。In addition, as the material for chemisorption, a group having a bondability to the --OH group is used. Is not limited to the silane-based surfactants shown in the examples.
発明の効果 本発明の方法を用いれば、充填材表面は単分子状の有機
薄膜が直接化学結合した状態で高密度に形成されている
ため、樹脂との密着性が極めて高く、これを充填された
合成樹脂はたとえば水分を含んだ雰囲気中で使用しても
劣化することがない。単分子膜は直接充填材表面に化学
結合し、かつ均一な厚みで非常に薄く形成されているた
め長時間使用しても界面活性剤が剥離することも無く信
頼性が高い。また、充填材の特性を損なうこともない。EFFECTS OF THE INVENTION When the method of the present invention is used, since the surface of the filler is formed at a high density in the state where the monomolecular organic thin film is directly chemically bonded, the adhesiveness with the resin is extremely high and the filler is filled with the resin. The synthetic resin does not deteriorate even when used in an atmosphere containing water, for example. Since the monomolecular film is chemically bonded directly to the surface of the filler and is formed to have a uniform thickness and is extremely thin, the surfactant is not peeled off even if it is used for a long time and is highly reliable. Further, the characteristics of the filler are not impaired.
【図面の簡単な説明】 第1図〜第4図は本発明の方法を説明するための微粒子
または繊維の断面図、第1図は概念図、第2図〜第4図
は吸着単分子膜の形成された微粒子または繊維で第1図
に示したO印A部を分子レベルまで拡大した図である。 1……充填用微粒子または繊維、2……微粒子または繊
維の表面のOH基、3……単分子膜。BRIEF DESCRIPTION OF THE DRAWINGS FIGS. 1 to 4 are sectional views of fine particles or fibers for explaining the method of the present invention, FIG. 1 is a conceptual diagram, and FIGS. 2 to 4 are adsorption monolayers. It is the figure which expanded the O mark A part shown in FIG. 1 to the molecular level by the formed fine particle or fiber. 1 ... Filling fine particles or fibers, 2 ... OH group on the surface of fine particles or fibers, 3 ... Monomolecular film.
Claims (9)
面に化学結合したシラン系界面活性剤よりなる単分子吸
着膜で表面が覆われた金属または酸化物の微粒子または
繊維よりなることを特徴とした合成樹脂用充填材。1. A fine particle or fiber of metal or oxide, the surface of which is covered with a monomolecular adsorption film of a silane-based surfactant chemically bonded to the surface through a —SiO— bond by a dehydrochlorination reaction. Characteristic synthetic resin filling material.
ーボン鎖を含んでいることを特徴とした特許請求の範囲
第1項記載の合成樹脂用充填材。2. The filler for synthetic resin according to claim 1, wherein the silane-based surfactant contains a linear hydrocarbon chain.
微粒子または繊維表面が互いに化学結合していることを
特徴とした特許請求の範囲第1項又は第2項記載の合成
樹脂用充填材。3. The synthetic resin filler according to claim 1 or 2, wherein the silane-based surfactant and the metal or oxide fine particles or the fiber surface are chemically bonded to each other. .
微粒子または繊維表面にシラン系界面活性剤を脱塩酸反
応により化学吸着させ、前記微粒子または繊維表面に直
接前記活性剤のシリコンを介して化学結合させて単分子
膜を形成する工程とを含むことを特徴とした合成樹脂用
充填材の製造方法。4. A silane-based surfactant is chemically adsorbed on the surface of fine particles of metal or oxide or fiber in a non-aqueous organic solvent by a dehydrochlorination reaction, and silicon of the active agent is directly added to the surface of the fine particles or fiber. And a step of chemically bonding to form a monomolecular film.
囲第4項記載の合成樹脂用充填材の製造方法。5. As a silane surfactant, at the end The method for producing a synthetic resin filler according to claim 4, characterized in that a chemical substance containing is used.
SiCl3(n:整数)で表される化学物質または、CH2=CH−
(CH2)n−SiCl3(n:整数)で表される化学物質を用い
ることを特徴とした特許請求の範囲第4項記載の合成樹
脂充填材の製造方法。6. CH 3- (CH 2 ) n-- as a silane surfactant
Chemical substance represented by SiCl 3 (n: integer) or CH 2 = CH−
The method for producing a synthetic resin filler according to claim 4, characterized in that a chemical substance represented by (CH 2 ) n-SiCl 3 (n: integer) is used.
たはシリカまたはガラスであることを特徴とした特許請
求の範囲第4項記載の合成樹脂用充填材の製造方法。7. The method for producing a synthetic resin filler according to claim 4, wherein the fine particles or fibers are alumina (Al 2 O 3 ), silica or glass.
微粒子または繊維表面にシラン系界面活性剤を脱塩酸反
応により化学吸着させ、前記微粒子または繊維表面に直
接前記活性剤のシリコンを介して化学結合させて単分子
膜を形成した酸化物の微粒子または繊維を合成樹脂中に
分散させたことを特徴とした合成樹脂。8. A silane-based surfactant is chemically adsorbed on the surface of fine particles of metal or oxide or fiber by a dehydrochlorination reaction in a non-aqueous organic solvent, and silicon of the active agent is directly added to the surface of the fine particles or fiber. A synthetic resin characterized in that fine particles or fibers of an oxide, which are chemically bonded to form a monomolecular film, are dispersed in the synthetic resin.
ラン系界面活性剤のハイドロカーボン鎖の一部にフッ素
原子を含んでいることを特徴とした特許請求の範囲第8
項記載の合成樹脂。9. A fluorine resin is used as a synthetic resin material, and a fluorine atom is contained in a part of a hydrocarbon chain of the silane-based surfactant.
The synthetic resin according to the item.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63166128A JPH0692501B2 (en) | 1988-07-04 | 1988-07-04 | Filler for synthetic resin, method for producing the same, and synthetic resin using the same |
| US07/781,673 US5209976A (en) | 1988-07-04 | 1991-10-24 | Structure having a surface covered with a monomolecular film |
| US08/021,910 US5445886A (en) | 1988-07-04 | 1993-02-24 | Structure having a surface covered with a monomolecular film |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63166128A JPH0692501B2 (en) | 1988-07-04 | 1988-07-04 | Filler for synthetic resin, method for producing the same, and synthetic resin using the same |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0216134A JPH0216134A (en) | 1990-01-19 |
| JPH0692501B2 true JPH0692501B2 (en) | 1994-11-16 |
Family
ID=15825555
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63166128A Expired - Fee Related JPH0692501B2 (en) | 1988-07-04 | 1988-07-04 | Filler for synthetic resin, method for producing the same, and synthetic resin using the same |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0692501B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3531805B2 (en) * | 2000-05-25 | 2004-05-31 | 富士高分子工業株式会社 | Sheet containing thermal conductive silicone gel |
| JP5813297B2 (en) * | 2010-07-02 | 2015-11-17 | 株式会社ブリヂストン | Tire manufacturing method |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5550975A (en) * | 1978-10-11 | 1980-04-14 | Toyota Motor Corp | Plasma arc welding starting method |
| JPS5639820A (en) * | 1979-04-23 | 1981-04-15 | Azumi Kk | Hob with inserted carbide tips |
| JPH0788438B2 (en) * | 1986-09-03 | 1995-09-27 | 株式会社資生堂 | Resin composition |
-
1988
- 1988-07-04 JP JP63166128A patent/JPH0692501B2/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0216134A (en) | 1990-01-19 |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| LAPS | Cancellation because of no payment of annual fees |