JPH0216134A - Filler for synthetic resin, its production and synthetic resin filled therewith - Google Patents
Filler for synthetic resin, its production and synthetic resin filled therewithInfo
- Publication number
- JPH0216134A JPH0216134A JP16612888A JP16612888A JPH0216134A JP H0216134 A JPH0216134 A JP H0216134A JP 16612888 A JP16612888 A JP 16612888A JP 16612888 A JP16612888 A JP 16612888A JP H0216134 A JPH0216134 A JP H0216134A
- Authority
- JP
- Japan
- Prior art keywords
- synthetic resin
- filler
- fibers
- fine particles
- silane surfactant
- 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.)
- Granted
Links
- 229920003002 synthetic resin Polymers 0.000 title claims abstract description 27
- 239000000057 synthetic resin Substances 0.000 title claims abstract description 27
- 239000000945 filler Substances 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- 239000000835 fiber Substances 0.000 claims abstract description 25
- 239000004094 surface-active agent Substances 0.000 claims abstract description 20
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 18
- 229910000077 silane Inorganic materials 0.000 claims abstract description 18
- 239000000126 substance Substances 0.000 claims abstract description 8
- 239000011356 non-aqueous organic solvent Substances 0.000 claims abstract 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract 2
- 239000010419 fine particle Substances 0.000 claims description 20
- 239000000463 material Substances 0.000 claims description 10
- 239000002184 metal Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical group O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 claims description 3
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 125000001153 fluoro group Chemical group F* 0.000 claims description 2
- 239000000377 silicon dioxide Substances 0.000 claims description 2
- 125000001183 hydrocarbyl group Chemical group 0.000 claims 2
- 229910052710 silicon Inorganic materials 0.000 claims 2
- 239000010703 silicon Substances 0.000 claims 2
- 239000012190 activator Substances 0.000 claims 1
- 239000013543 active substance Substances 0.000 claims 1
- 239000011521 glass Substances 0.000 claims 1
- 239000002356 single layer Substances 0.000 claims 1
- 229920005989 resin Polymers 0.000 abstract description 14
- 239000011347 resin Substances 0.000 abstract description 14
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical compound ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 239000013528 metallic particle Substances 0.000 abstract 2
- 239000004925 Acrylic resin Substances 0.000 abstract 1
- 229920000178 Acrylic resin Polymers 0.000 abstract 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052782 aluminium Inorganic materials 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 239000003365 glass fiber Substances 0.000 abstract 1
- 230000003014 reinforcing effect Effects 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000010408 film Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 3
- 229920000515 polycarbonate Polymers 0.000 description 3
- 239000004417 polycarbonate Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000007033 dehydrochlorination reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 239000002923 metal particle Substances 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Structures Or Materials For Encapsulating Or Coating Semiconductor Devices Or Solid State Devices (AREA)
Abstract
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。DETAILED DESCRIPTION OF THE INVENTION Field of Industrial Application The present invention relates to a filler for synthetic resins used for modifying or increasing the amount of synthetic resins, 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５ｆｏ２や
ＡｌａＯ３のような酸化物、あるいはＦｅやＡＩ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。2. Description of the Related Art Conventionally, synthetic resins have been modified or increased in quantity by dispersing oxides such as 5fo2 or AlaO3, or fine particles or fibers of Fe or AI into the resin.
発明が解決しようとした課題
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。Problems that the invention sought to solve However, while this method is easy to manufacture, the filler is simply mixed in the resin, and if used for a long time, the resin material may peel off from the surface of the particles or fibers. This had the disadvantage of causing cracks and cloudiness.
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
脂の信願性を向上させることにある。The purpose of the present invention is to provide a method for producing synthetic resin that does not deteriorate in quality even after long-term use by chemically bonding a surfactant to the surface of fine particles or fibers used for filling, and to improve the reputation of synthetic resins. It is about improving sexuality.
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した合成樹脂を提供するものである
。Means for Solving the Problems The present invention provides a method for producing a filler for synthetic resins, which includes a step of chemically adsorbing a silane surfactant directly onto the surface of fine particles or fibers in the form of a single molecule, and a method produced using the method. The present invention provides a synthetic resin characterized in that a filler and a filler on which the monomolecular film is formed are 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。Effect: Therefore, by using the method of the present invention, it is possible to form a monomolecular organic thin film that is chemically bonded directly to the surface of the filler, so the monomolecular organic thin film does not peel off and has good adhesion to the resin. It has the ability to keep the temperature extremely high.
実施例 以下、実施例を第１〜４図を用いて説明する。Example Examples will be described below with reference to FIGS. 1 to 4.
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（Ａ１２０ｓ）、シリ
カ、ガラス％ Ｆ ｅ ２ ｋ あるいはＦｅ３Ｏ
４等の酸化物やＦ ８％ Ａ Ｉ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ＣＨａ−（ＣＨ２）ｎ−３ｉ Ｃｌ ａ （ａ：整
数。１０〜２５程度が最も扱いやすい）を用い、２Ｘ
１ ｏ−ｉ〜ｓｘ １０−’Ｍｏｌ／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一〇Ｈ基
が含まれている。For example, as shown in FIG.
A monomolecular protective film 2 made of a silane surfactant is formed by adsorbing and reacting a silane surfactant over the entire surface of oxides such as oxides such as F 8% A, or metal particles or fibers such as F 8% A I using a chemical adsorption method. Form. For example, using CHa-(CH2)n-3iCl a (a: an integer; approximately 10 to 25 is easiest to handle) as a silane surfactant, 2X
A solution of 80% n-hexane, 12% carbon tetrachloride, and 8% chloroform dissolved at a concentration of about 1 o-i~sx 10-'Mol/l is prepared, and the fine particles or fibers 1 are immersed therein. At this time, natural oxide is formed on the surface of the metal fine particles or fibers, and since the surface of the oxide is naturally an oxide, the surface of each of them contains 10H groups.
従って、Ｓ ｔ Ｃｌ ａ基と−ＯＨが脱塩酸反応して
シラン界面活性剤による半分膜３が磁性体微粒子表面に
１層（２０〜３０Ａ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。Therefore, the S t Cla group and -OH undergo a dehydrochlorination reaction, and a half film 3 of the silane surfactant is formed on the surface of the magnetic fine particles (with a thickness of 20 to 30 Å). (Figure 2) Next, after uniformly dispersing these fine particles and fibers in a synthetic resin material (for example, acrylic, polycarbonate, vinyl chloride, polyamide, or polyester resin material), the whole is cured to form 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ＣＨ＊＝
ＣＨ−（ＣＨ２）ｎ。−ＳｉＣｌ３またはＣＨ＝ＣＨ−
（ＣＨ２）ｎｎ−３ｉ Ｃｌ 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*= as a resin material as a silane surfactant
CH-(CH2)n. -SiCl3 or CH=CH-
(CH2)nn-3i Cl3(n: integer. 10~
25 is the easiest to handle), it is possible to form a monomolecular film of 3 degrees with CH2''CH- groups or CH=CH- groups arranged on the surface. (Figure 3) Therefore, these fillings Since the material can directly form chemical bonds with acrylic or resin materials such as polycarbonate, vinyl chloride, polyamide, and polyester, adhesion 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一〇Ｆ３基等のフッ素原子
を含む物質（例えば、ＣＦ３−（ＣＨ２）ｎ−３Ｉ Ｃ
Ｉ ３ （ｎ： 整数。１０〜２５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。In addition, when using a fluororesin as the resin material, a substance containing a fluorine atom such as 10F3 group at the end (for example, CF3-(CH2)n-3I C
When I 3 (n: an integer; approximately 10 to 25 is easiest to handle)), a monomolecular film with -CF groups 5 arranged on the surface can be formed as shown in Figure 4, and the compatibility with fluororesin is high. 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, if silica is used as the fine particles or fibers and acrylic or polycarbonate is used as the synthetic resin material, a glass-like resin plate with extremely good transparency and high reliability can be obtained.
なお、化学吸着用の材料としては、−ＯＨ基にを含んで
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。Note that the chemical adsorption material is not limited to the silane surfactants shown in the examples as long as it contains -OH groups.
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。Effects of the Invention When the method of the present invention is used, the surface of the filler is formed with a high density of monomolecular organic thin films directly chemically bonded to each other, so it has extremely high adhesion to the resin, and the surface of the filler is filled with Synthetic resins do not deteriorate even when used in an atmosphere containing moisture.
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期間使用しても界
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。The monomolecular film is chemically bonded directly to the filler surface and is extremely thin with a uniform thickness, so the surfactant does not peel off even after long-term use, making it highly reliable. Moreover, the properties of the filler are not impaired.
第１図〜第４図は本発明の詳細な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。
代理人の氏名 弁理士 粟野重孝 はか１名Ｍ１図
第３図
第
図
′−どFigures 1 to 4 are cross-sectional views of fine particles or fibers for detailed explanation of the present invention, Figure 1 is a conceptual diagram, and Figures 2 to 4 are fine particles or fibers on which an adsorbed monomolecular film has been formed. 1 is an enlarged view of the O-marked section A shown in FIG. 1 to the molecular level. 1...Fine particles or fibers for filling, 2...
・OH groups on the surface of fine particles or fibers, 3... Monomolecular film. Name of agent: Patent attorney Shigetaka Awano (1 person)
Claims (9)
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 filler for synthetic resins characterized by being made of fine particles or fibers of metal or oxide whose surface is covered with a monomolecular adsorption film made of a silane surfactant.
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 resins according to claim 1, wherein the silane surfactant contains a linear hydrocarbon chain.
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 filler for synthetic resins according to claim 1 or 2, wherein the silane surfactant and the surface of metal or oxide fine particles or fibers are chemically bonded to each other.
または繊維表面にシラン系界面活性剤を化学吸着させ、
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を１層形成する工程とを
含むことを特徴とした合成樹脂用充填材の製造方法。(4) chemically adsorbing a silane surfactant onto the surface of metal or oxide fine particles or fibers in a non-aqueous organic solvent;
A method for producing a filler for a synthetic resin, comprising the step of forming a single layer of a single molecule by directly chemically bonding the active agent to the surface of the fine particles or fibers via silicon.
範囲第４項記載の合成樹脂用充填材の製造方法。(5) As the silane surfactant, a chemical substance containing a ▲ mathematical formula, chemical formula, table, etc. at the end is used. .
）＿ｎ−ＳｉＣｌ＿３（ｎ：整数）で表される化学物質
または、ＣＨ＿２：ＣＨ−（ＣＨ＿２）＿ｎ−ＳｉＣｌ
＿３（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項記載の合成樹脂用充填材
の製造方法。(6) As a silane surfactant, CH_3-(CH_2
)_n-SiCl_3 (n: integer) or CH_2:CH-(CH_2)_n-SiCl
5. The method for producing a synthetic resin filler according to claim 4, characterized in that a chemical substance represented by _3 (n: an integer) is used.
ま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) Fine particles or fibers are alumina (Al_2O_3)
5. The method for producing a synthetic resin filler according to claim 4, wherein the filler is silica or glass.
または繊維表面にシラン系界面活性剤を化学吸着させ、
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を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) Chemically adsorbing a silane surfactant onto the surface of metal or oxide fine particles or fibers in a non-aqueous organic solvent;
A synthetic resin characterized by dispersing in a synthetic resin fine particles or fibers of an oxide, which are chemically bonded directly to the surface of the fine particles or fibers to form a single molecule via silicon as the activator.
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) The synthetic resin according to claim 8, characterized in that a fluororesin is used as the synthetic resin material, and a part of the hydrocarbon chain of the silane surfactant contains a fluorine atom. .
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 true JPH0216134A (en) | 1990-01-19 |
| JPH0692501B2 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) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001329173A (en) * | 2000-05-25 | 2001-11-27 | Fuji Kobunshi Kogyo Kk | Heat-conductive silicone gel composition |
| JP2012011718A (en) * | 2010-07-02 | 2012-01-19 | Bridgestone Corp | Method of producing resin-metal composite material, resin-metal composite material, and tire |
Citations (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 |
| JPS6363751A (en) * | 1986-09-03 | 1988-03-22 | Shiseido Co Ltd | Resin composition |
-
1988
- 1988-07-04 JP JP63166128A patent/JPH0692501B2/en not_active Expired - Fee Related
Patent Citations (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 |
| JPS6363751A (en) * | 1986-09-03 | 1988-03-22 | Shiseido Co Ltd | Resin composition |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001329173A (en) * | 2000-05-25 | 2001-11-27 | Fuji Kobunshi Kogyo Kk | Heat-conductive silicone gel composition |
| JP2012011718A (en) * | 2010-07-02 | 2012-01-19 | Bridgestone Corp | Method of producing resin-metal composite material, resin-metal composite material, and tire |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0692501B2 (en) | 1994-11-16 |
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