JPH059897A - Papers having modified surface - Google Patents
Papers having modified surfaceInfo
- Publication number
- JPH059897A JPH059897A JP14208791A JP14208791A JPH059897A JP H059897 A JPH059897 A JP H059897A JP 14208791 A JP14208791 A JP 14208791A JP 14208791 A JP14208791 A JP 14208791A JP H059897 A JPH059897 A JP H059897A
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- Japan
- Prior art keywords
- papers
- plasma
- paper
- gas
- atmospheric pressure
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- 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.)
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- Treatments Of Macromolecular Shaped Articles (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
- Paper (AREA)
- Treatment Of Fiber Materials (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は表面改質された紙類に関
する。FIELD OF THE INVENTION The present invention relates to surface-modified papers.
【０００２】[0002]
【従来の技術】従来より本来の木材パルプから作られる
紙の他、包装用、衣料用、建築用、その他産業用資材と
して種々の用途に用いられる合成紙、化学繊維紙等があ
る。これらの紙類はそれ自体で広範囲な用途にもちいら
れているが、これらを原料としてさらに二次加工を施し
特殊な機能をもたせた加工紙として多分野に利用されて
いる。とくに疎水性、摩耗性を付与するために、ペレッ
ト状ポリマーの加熱押出し塗工、ロッド塗工、電着塗工
等の特殊塗工や、複数のフィルム、箔、布等のラミネー
トや、薬液中に浸漬して薬剤を基材中に定着させたり、
スパッタリング法や、イオンプレーテイング法等の基材
表面を真空中で金属めっきする真空蒸着等の加工がなさ
れている。2. Description of the Related Art Conventionally, in addition to papers made from original wood pulp, there are synthetic papers, chemical fiber papers, etc. which are used for various purposes as packaging materials, clothing materials, construction materials, and other industrial materials. Although these papers are used in a wide range of applications by themselves, they are used in various fields as processed papers that have been subjected to secondary processing using these as raw materials to have special functions. In particular, in order to impart hydrophobicity and abrasion resistance, special coating such as heat extrusion coating of pelletized polymer, rod coating, electrodeposition coating, lamination of multiple films, foils, cloths, etc. To fix the drug in the substrate,
Processing such as sputtering and ion plating is performed such as vacuum deposition of metal plating the surface of a base material in vacuum.
【０００３】一方、繊維に対して疎水性、磨耗性、風
合、光沢、帯電防止、粗面化等の性質を付与するために
プラズマ処理が行われている。例えば特開昭６２−２５
７４５５号には、合成繊維の粗面化（エッチング処理）
を行う目的で、低圧におけるプラズマ装置と処理方法が
開示されている。また、特開昭６２−１７２０３５号で
は低圧におけるプラズマ処理により、繊維表面を親水化
し、再汚染性（黒ずみ）防止を行う方法が開示されてい
る。また、プラズマ処理により繊維及び織物に疎水性を
付与する場合には、通常上記と同様な低圧プラズマ処理
装置を使用して繊維及び織物上に疎水性の物質、例えば
シリコーン系あるいはフッ素系の重合膜を形成させるこ
とが一般的に行われている。On the other hand, plasma treatment is carried out to impart properties such as hydrophobicity, abrasion resistance, feeling, luster, antistatic property and surface roughening to the fibers. For example, JP-A-62-25
No. 7455 has roughened synthetic fibers (etching treatment).
For the purpose of carrying out, a plasma device and a processing method at low pressure are disclosed. Further, JP-A-62-172035 discloses a method in which the fiber surface is made hydrophilic by plasma treatment at low pressure to prevent recontamination (darkening). When imparting hydrophobicity to fibers and fabrics by plasma treatment, a low-pressure plasma treatment apparatus similar to the above is usually used to form hydrophobic substances on the fibers and fabrics, such as silicone-based or fluorine-based polymerized films. Is generally performed.
【０００４】[0004]
【発明が解決すべき課題】これら従来のプラズマ処理
は、紙類には未だ適用されたことがなかった。これらの
繊維及び織物に成されるプラズマ処理は低圧において処
理するので、装置の機密性のためシーリングに特に留意
し、また紙類等を処理する場合には、これらの紙類に含
まれる水分や油脂分、その他紙類に含まれる様々な揮発
成分の装置内を汚染するものの除去を行うために乾燥と
いう前処理が必要であり、これら前処理及びシーリング
は共に装置製作コストを著しく高めている。These conventional plasma treatments have never been applied to papers. Since the plasma treatment performed on these fibers and fabrics is performed at a low pressure, pay particular attention to sealing because of the airtightness of the device, and when treating papers, etc., the moisture and moisture contained in these papers should be taken into consideration. Pretreatment such as drying is necessary to remove oil and fats and other various volatile components contained in papers that contaminate the inside of the apparatus. Both of these pretreatments and sealing significantly increase the manufacturing cost of the apparatus.
【０００５】また、この前処理を行なわずに装置内へ紙
類を挿入すると、長時間にわたりこれらの水分や吸収物
質が気相に蒸発し、処理条件を調整することが極めて困
難であった。特に低圧グロー放電の場合には放電自身が
装置内に拡散するので、上記含有物質による装置壁への
汚染は工業的利用において運転継続上の障害であった。Further, if papers are inserted into the apparatus without performing this pretreatment, these moisture and absorbing substances evaporate in the vapor phase for a long time, and it is extremely difficult to adjust the treatment conditions. Particularly in the case of low-pressure glow discharge, the discharge itself diffuses into the device, and thus the contamination of the device wall with the above-mentioned contained substances has been an obstacle to continuous operation in industrial use.
【０００６】[0006]
【発明の目的】本発明の目的は、セラミックス、金属あ
るいはプラスチックと比べ含揮発成分率が高く、このた
め従来のプラズマ処理では困難あるいは工程が煩雑であ
った紙類のプラズマ処理を容易にし、処理ムラの無い、
均一な表面改質がなされた疎水性紙類を提供することを
目的とする。It is an object of the present invention to facilitate the plasma treatment of papers, which has a higher volatile component content than ceramics, metals or plastics, and which has been difficult or complicated in the conventional plasma treatment. Uniform,
It is an object of the present invention to provide hydrophobic papers having a uniform surface modification.
【０００７】[0007]
【課題を解決するための手段】一般にグロー放電は低気
圧における放電であったが、本発明は、低圧下のグロー
プラズマでは困難であった紙類の均一な表面改質を大気
圧におけるグロープラズマを用いることにより達成する
ことができた。従来からグロー放電は、一般に低気圧で
の放電形式であるとされてきたが、近年下部放電電極を
誘電体で覆い、他方の極に多針型極を用いることにより
大気圧でも安定なグロープラズマ放電を生じさせること
が本発明者により提案されている（特開昭６３−１３８
６３０号）。Generally, glow discharge was discharge at low pressure, but the present invention provides uniform surface modification of papers at low pressure which was difficult with glow plasma under low pressure. Could be achieved by using Conventionally, glow discharge has been generally regarded as a low pressure discharge type, but in recent years a glow plasma that is stable even at atmospheric pressure has been obtained by covering the lower discharge electrode with a dielectric and using a multi-needle electrode on the other pole. It has been proposed by the present inventor to generate an electric discharge (Japanese Patent Laid-Open No. 63-138).
630).
【０００８】しかし、この際の被処理物が金属の場合の
み、多針型電極からの放電がアークに転移する欠点があ
った。更にこの欠点を改善し金属、非金属の如何を問わ
ず安定なグロー放電プラズマを発生できる方法（特願昭
６３−２０２９７７号）、更には、このプラズマ内電界
を均一にする方法（特願昭６３−１６６５９９号）を共
同発明者が発明した。However, there is a drawback in that the discharge from the multi-needle electrode is transferred to an arc only when the object to be treated is a metal. Further, a method of improving this defect to generate stable glow discharge plasma regardless of metal or non-metal (Japanese Patent Application No. 63-202977), and a method of making the electric field in the plasma uniform (Japanese Patent Application No. 63-166599) was invented by a joint inventor.
【０００９】この大気圧グロー放電法を用いることによ
り水分やその他の揮発成分を含んだ天然の紙、合成紙、
化学繊維紙等の紙類でも、処理中に揮発成分の蒸発の影
響がなく、プラズマの生成に対して悪影響を与えず、均
一な処理が可能であることの知見を得て本発明を完成さ
せた。即ち、本発明の表面改質紙類は、含フッ素化合物
と不活性ガスの混合ガスを用いて大気圧グロープラズマ
処理することにより均一な疎水性表面を持つようにした
ものである。By using this atmospheric pressure glow discharge method, natural paper containing water and other volatile components, synthetic paper,
Even with papers such as chemical fiber paper, the present invention has been completed with the knowledge that there is no effect of evaporation of volatile components during processing, does not adversely affect plasma generation, and uniform processing is possible. It was That is, the surface-modified papers of the present invention have a uniform hydrophobic surface by being subjected to atmospheric pressure glow plasma treatment using a mixed gas of a fluorine-containing compound and an inert gas.
【００１０】ここで、プラズマ発生方法としては図１に
示す内部電極方式が最適であり、ＫＨｚからの低周波放
電、高周波放電、導波管型方式によるマイクロ波放電お
よび電子サイクロトロン共鳴放電等があるが、これらに
限らずプラズマを発生し、かつこれにより表面に反応を
起こす方法であれば他の方法も使用することができる。
図１は本発明の表面改質紙類を製造するプラズマ処理装
置の一例を示す説明図であり、以下図面に示すプラズマ
放電装置を用いた本発明の表面改質紙類を製造する方法
を説明する。Here, the internal electrode method shown in FIG. 1 is most suitable as a plasma generating method, and there are low frequency discharge from KHz, high frequency discharge, microwave discharge by a waveguide type method, electron cyclotron resonance discharge and the like. However, not limited to these, other methods can be used as long as they generate plasma and cause a reaction on the surface.
FIG. 1 is an explanatory view showing an example of a plasma treatment apparatus for producing the surface-modified papers of the present invention, and a method for producing the surface-modified papers of the present invention using a plasma discharge device shown in the drawings will be described below. To do.
【００１１】図１において、プラズマ処理装置２内に、
プラズマ発生系６に接続された上部電極３及び下部電極
４（アノード側）が平行に設置されており、この下部電
極４上に紙類から成る基材１を設置する。大気圧で安定
なグロープラズマを発生させるために使用する電極は少
なくとも一方の電極が誘電体５で覆われている必要があ
る。電極の形状は平行平板型電極でもよいが、高速で大
容量エネルギーの注入を目的とする場合、より均一なプ
ラズマ処理をおこなうには上部電極３は多針型、下部電
極４は誘電体で覆われた平板型電極を用いることが好ま
しい（特願昭６３−２０２９７７号）。In FIG. 1, in the plasma processing apparatus 2,
An upper electrode 3 and a lower electrode 4 (anode side) connected to a plasma generation system 6 are installed in parallel, and a base material 1 made of paper or the like is installed on the lower electrode 4. At least one of the electrodes used to generate stable glow plasma at atmospheric pressure must be covered with the dielectric 5. The shape of the electrode may be a parallel plate type electrode, but in order to inject a large amount of energy at high speed, the upper electrode 3 should be covered with a multi-needle type and the lower electrode 4 should be covered with a dielectric material in order to perform more uniform plasma treatment. It is preferable to use a flat plate type electrode (Japanese Patent Application No. 63-202977).
【００１２】但し、紙類が導電性を有する際は、平板型
または多針型で更に誘電体により覆われた上部電極５ａ
を用いることが好ましい（図２）。誘電体で覆われた多
針型電極であれば電界も均一となり、導電性、誘電体い
ずれの試料にも適用できる。使用する含フッ素化合物は
基本的には処理時にガス化するもであればよい。しか
し、安全性を考慮し低毒性で不燃性のＣＦ4、Ｃ2Ｆ
6等、また不燃性で非腐食性のＳＦ6、ＮＦ3等が好まし
い。また、含フッ素化合物に混合する不活性ガスとして
は、ヘリウム、アルゴン、窒素、ネオン等またはそれら
の混合したものが使用できるが、発生するプラズマの安
定性からヘリウムを主体として使用することが好まし
い。However, when the paper is electrically conductive, the upper electrode 5a is of flat plate type or multi-needle type and is covered with a dielectric material.
Is preferably used (FIG. 2). A multi-needle type electrode covered with a dielectric material has a uniform electric field and can be applied to both conductive and dielectric samples. The fluorine-containing compound used may basically be gasified during processing. However, in consideration of safety, low toxicity and nonflammable CF 4 , C 2 F
6 and the like, and nonflammable and non-corrosive SF 6 , NF 3 and the like are preferable. Further, as the inert gas mixed with the fluorine-containing compound, helium, argon, nitrogen, neon, or the like or a mixture thereof can be used, but it is preferable to use helium as a main component because of stability of generated plasma.
【００１３】基材１とする紙類としては、天然紙、合成
紙、不織布、化学繊維紙が挙げられる。また、本発明は
紙類が種々の加工処理した後、表面に液相あるいは蒸気
相を有する場合でも（濡れている状態でも）プラズマ処
理できる利点が有り、例えば不織布の製造工程中に本発
明を適用することができる。Examples of the paper used as the base material 1 include natural paper, synthetic paper, non-woven fabric, and chemical fiber paper. Further, the present invention has an advantage that after various kinds of processing of papers, plasma processing can be performed even when the surface has a liquid phase or a vapor phase (even in a wet state). Can be applied.
【００１４】本発明の紙類に成される表面改質に必要な
フッ素の量は、プラスチック材料に成されるフッ素化と
異なり可燃性物としての処理であり、フッ素化されるの
が最外表面のみであるため極く少量である。得られる表
面改質紙類は包装用、建築用、産業用、地図用等極めて
広範囲な用途に使用可能であって、全体が疎水性を付与
されるのみならず、目的によっては、スリット状の用具
を使用することにより任意の柄や形に疎水性部分を制御
することができる。これにより染色、染着、印刷等も可
能となる。The amount of fluorine required for the surface modification of the papers of the present invention is a treatment as a combustible substance unlike the fluorination of plastic materials, and the fluorination is the outermost. Since it is only the surface, it is extremely small. The surface-modified papers obtained can be used in an extremely wide range of applications such as packaging, construction, industry, and maps, and not only is the entire surface imparted with hydrophobicity, but depending on the purpose, it may be slit-shaped. By using the tool, the hydrophobic portion can be controlled to have an arbitrary pattern or shape. This enables dyeing, dyeing, printing and the like.
【００１５】[0015]
【作用】本発明における紙類はその表面がフッ素化され
ることによって疎水性を付与されており、このフッ素化
は紙類表面の表面近傍での水素−フッ素の引き抜き置換
反応と考えられ、疎水性を与えるための積層膜を生成さ
せる場合と比べると接着性を考慮する必要のないこと、
またフッ素の使用量が少なく大気圧でのプラズマ処理で
あることから低圧におけるプラズマ処理と比べてシーリ
ング、即ち一定の真空度を保つことに対する考慮は格段
に少なくてすむことからランニングコストも安価な未だ
かつて得られたことがない表面改質紙類を提供すること
ができる。The paper of the present invention is rendered hydrophobic by the surface thereof being fluorinated, and this fluorination is considered to be a hydrogen-fluorine abstraction substitution reaction near the surface of the paper surface. It is not necessary to consider the adhesiveness as compared with the case of generating a laminated film for giving the property,
In addition, since the amount of fluorine used is small and the plasma treatment is performed at atmospheric pressure, the running cost is still low because the sealing, that is, maintaining a certain degree of vacuum, is much less important than the plasma treatment at low pressure. It is possible to provide surface-modified papers that have never been obtained.
【００１６】[0016]
実施例１ 市販のコピー用紙を下部電極４上に設置し、ガス供給路
７、８よりガス混合器１０を通してＣＦ4：Ｈｅ＝１：
５０の混合ガスを装置内のガス圧が７６５Torrになるよ
うに導入し、以後混合ガスの導入を続けながら、ガス圧
力が７６５Torrを保つように排気路９を開き、次いで周
波数１５ＫＨｚ、３０Ｗ／ｃｍ2の電力を電極に印荷し
グロープラズマを発生させ、約３分間処理を行った。Example 1 A commercially available copy sheet was placed on the lower electrode 4, and CF 4 : He = 1: through the gas mixers 10 through the gas supply paths 7 and 8.
The mixed gas of 50 was introduced so that the gas pressure in the apparatus was 765 Torr, and while continuing the introduction of the mixed gas, the exhaust passage 9 was opened so that the gas pressure was maintained at 765 Torr, and then the frequency was 15 KHz and 30 W / cm 2 Was applied to the electrodes to generate glow plasma, and the treatment was performed for about 3 minutes.
【００１７】このようにして得られたコピー用紙は、純
水の接触角が１０４度となり、高い撥水性を示した。 実施例２ 市販の和紙を下部電極４上に設置し、ガス供給路７、８
よりガス混合器１０を通してＣＦ4：Ｈｅ＝１：７０の
混合ガスを装置内のガス圧が７６５Torrになるように導
入し、以後混合ガスの導入を続けながら、ガス圧力が７
６５Torrを保つように排気路９を開き、次いで周波数１
５ＫＨｚ、３０Ｗ／ｃｍ2の電力を電極に印荷しグロー
プラズマを発生させ、約３分間処理を行った。The copy paper thus obtained had a contact angle of pure water of 104 degrees and showed high water repellency. Example 2 Commercially available Japanese paper is placed on the lower electrode 4 and the gas supply paths 7 and 8 are used.
Further, a mixed gas of CF 4 : He = 1: 70 was introduced through the gas mixer 10 so that the gas pressure in the apparatus became 765 Torr. While continuing to introduce the mixed gas thereafter, the gas pressure became 7
Open the exhaust passage 9 so as to maintain 65 Torr, then frequency 1
An electric power of 5 KHz and 30 W / cm 2 was applied to the electrodes to generate glow plasma, which was then treated for about 3 minutes.
【００１８】このようにして得られた和紙は、純水の接
触角が１１０度となり、高い撥水性を示した。The thus-obtained Japanese paper had a contact angle of pure water of 110 degrees and showed high water repellency.
【００１９】[0019]
【発明の効果】本発明は、大気圧でグロープラズマ処理
を行うようにしたことから、水分やその他の揮発成分を
含んだ紙類でも前処理の必要が無く、装置的なメンテナ
ンス等も廉価であり、結果的に安価な疎水性表面を持つ
紙類が提供できる。According to the present invention, since the glow plasma treatment is carried out at atmospheric pressure, there is no need for pretreatment even for papers containing water and other volatile components, and maintenance for the apparatus is inexpensive. As a result, inexpensive papers having a hydrophobic surface can be provided.
【図１】本発明の表面改質紙類を製造するプラズマ処理
装置の一例を示す説明図FIG. 1 is an explanatory view showing an example of a plasma processing apparatus for producing surface-modified papers of the present invention.
【図２】本発明の表面改質紙類を製造するプラズマ処理
装置の要部の一例を示す説明図FIG. 2 is an explanatory view showing an example of a main part of a plasma processing apparatus for producing surface-modified papers of the present invention.
１………基材（紙類） ２………プラズマ処理装置 ７………ガス供給路（含フッ素ガス） ８………ガス供給路（不活性ガス） 1 ... Base material (paper) 2 ... Plasma processing device 7 ... Gas supply path (fluorine-containing gas) 8 ... Gas supply path (inert gas)
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.5 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｄ０６Ｍ 10/08 15/256 Ｄ２１Ｈ 27/00 7199−3Ｂ Ｄ０６Ｍ 10/00 Ｇ 7199−3Ｂ 15/256 (72)発明者 小駒 益弘 埼玉県和光市下新倉843番15 (72)発明者 吹田 隆文 埼玉県与野市鈴谷４丁目６番35号 株式会 社きもと開発研究所内 (72)発明者 木村 剛久 埼玉県与野市鈴谷４丁目６番35号 株式会 社きもと開発研究所内─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 5 Identification code Internal reference number FI Technical display location D06M 10/08 15/256 D21H 27/00 7199-3B D06M 10/00 G 7199-3B 15/256 (72) Inventor Masuhiro Ogoma 843-15 Shimoarakura, Wako-shi, Saitama Prefecture (72) Inventor Takafumi Suita 4-63 Suzuya, Yono City, Saitama Prefecture Kimoto Development Research Institute (72) Inventor Takehisa Kimura Saitama Prefecture 4-6-35 Suzuya, Yono-shi, Kimoto Development Research Institute, Inc.
Claims (1)
用いて大気圧グロープラズマ処理することにより均一な
疎水性表面を持つことを特徴とする表面改質紙類。Claims: 1. Surface-modified papers having a uniform hydrophobic surface by an atmospheric pressure glow plasma treatment using a mixed gas of a fluorine-containing compound and an inert gas.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14208791A JPH059897A (en) | 1991-06-13 | 1991-06-13 | Papers having modified surface |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP14208791A JPH059897A (en) | 1991-06-13 | 1991-06-13 | Papers having modified surface |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH059897A true JPH059897A (en) | 1993-01-19 |
Family
ID=15307129
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP14208791A Withdrawn JPH059897A (en) | 1991-06-13 | 1991-06-13 | Papers having modified surface |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH059897A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102409527A (en) * | 2011-10-20 | 2012-04-11 | 浙江理工大学 | Plasma finishing method for endowing fabric durable super-hydrophobic property |
| US8425943B2 (en) | 2007-10-17 | 2013-04-23 | Biova, L.L.C. | Method of treatment using solubilized protein composition obtained from eggshell membrane |
| CZ306256B6 (en) * | 2005-11-18 | 2016-11-02 | Masarykova Univerzita | Method of and apparatus for surface activation of cellulose fiber layers, materials based on paper and carton boards |
-
1991
- 1991-06-13 JP JP14208791A patent/JPH059897A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CZ306256B6 (en) * | 2005-11-18 | 2016-11-02 | Masarykova Univerzita | Method of and apparatus for surface activation of cellulose fiber layers, materials based on paper and carton boards |
| US8425943B2 (en) | 2007-10-17 | 2013-04-23 | Biova, L.L.C. | Method of treatment using solubilized protein composition obtained from eggshell membrane |
| CN102409527A (en) * | 2011-10-20 | 2012-04-11 | 浙江理工大学 | Plasma finishing method for endowing fabric durable super-hydrophobic property |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A300 | Withdrawal of application because of no request for examination |
Free format text: JAPANESE INTERMEDIATE CODE: A300 Effective date: 19980903 |