JP2005256221A - Method for coating carbon nanotube onto natural fiber - Google Patents
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本発明は天然繊維に従来有していない特性、例えば導電性，熱伝導性等を付与するためカーボンナノチューブを天然繊維表面に付着させ、被覆する方法に関するものである。
The present invention relates to a method for attaching and coating a carbon nanotube on the surface of a natural fiber in order to give the natural fiber characteristics such as conductivity and thermal conductivity which have not been conventionally provided.
天然繊維素材はしなやかで強いという特長をもち、使用中も使用後も環境負荷が少なく、しかも繊維を構成する分子の構造上、その表面には親水性の官能基が多く存在するため、保水性や環境との調和性では合成繊維素材より優れており、また、官能基の存在により化学結合を介して様々な染料，顔料をのせることができることから、古くから現在に至るまで衣料用のみならず産業用にも幅広く利用されているが、天然繊維素材はその性質上、制電性はあるにしても、導電性，熱伝導性は具有していない。
Natural fiber material has the characteristics of being supple and strong, has little environmental impact during and after use, and has many hydrophilic functional groups on its surface due to the structure of the molecules that make up the fiber. It is superior to synthetic fiber materials in terms of harmony with the environment, and since various dyes and pigments can be placed through chemical bonds due to the presence of functional groups, it can only be used for clothing from ancient times to the present Although it is widely used for industrial purposes, natural fiber materials are not conductive or heat conductive due to their properties, even though they are antistatic.
しかし、近年、ＩＴ技術の発展により高い電磁波シールドや高い制電性を求める風潮が強く、上記特性を有する天然繊維に対しても、その特性を保持したまま、導電性，熱伝導性を併せ有する素材への関心が昂まって来た。
However, in recent years, with the development of IT technology, there is a strong trend for high electromagnetic shielding and high anti-static properties, and even natural fibers having the above characteristics have both conductivity and heat conductivity while retaining the characteristics. My interest in materials has grown.
ところで、繊維に導電性等を与える手段としては従来、導電性成分を共重合するか、混合紡糸する方法や、繊維に炭素粒子を侵入させたり、銀，銅などの金属で被覆する方法などが知られている。（例えば非特許文献文献１参照）
また、熱可塑性樹脂を炭素繊維に付着させたり、炭素繊維に対し気相成長炭素繊維及び／又はカーボンナノチューブを付着することも提案されている。（例えば特許文献１）
By the way, as means for imparting conductivity to the fiber, conventionally, there are a method of copolymerizing conductive components or a mixed spinning method, a method of infiltrating carbon particles into the fiber, and a method of coating with a metal such as silver or copper. Are known. (For example, see Non-Patent Document 1)
It has also been proposed to attach a thermoplastic resin to carbon fibers or to attach vapor grown carbon fibers and / or carbon nanotubes to carbon fibers. (For example, Patent Document 1)
しかし、上記各導電性付与手法は何れも合成繊維、あるいは炭素繊維に加工を施すものであり、綿糸の如き天然繊維ならびに天然繊維構造物に対し導電性，熱伝導性を付与することについては触れていない。
However, each of the above-mentioned methods for imparting electrical conductivity is to process synthetic fibers or carbon fibers, and mention about imparting electrical conductivity and thermal conductivity to natural fibers such as cotton yarn and natural fiber structures. Not.
そこで、本発明者らはカーボンナノチューブの利用に着目し、天然繊維素材に対し導電性，熱伝導性を付与することを試みた。
カーボンナノチューブは黒鉛のシートを巻いて筒状にした形状で、直径はおよそ数ｎｍから数十ｎｍ，長さは数μｍであり、導電性，熱伝導性，耐酸化性などの炭素材料が示す高機能を保持した粉体状の物質である。
従って、この物質を天然繊維上に加工するか、または天然繊維素材上に被覆することができれば、天然素材のしなやかさと、カーボンナノチューブの機能を併せ持つ新機能材料を得ることができる可能性がある。
しかし、カーボンナノチューブは水系には極めて分散しにくい性質を持ち、そのままでは天然繊維表面に加工，被覆することは困難であり、何らかの処理が必要となる。
また、天然繊維である綿糸等の表面には脂分が残留しているため、未処理のままでは水系との親和性は低い。
そのため、カーボンナノチューブを天然繊維に被覆する場合には、なお種々の問題があり、とりわけ以下の２つの課題を解決することが不可欠であることを知見した。
（１）天然繊維への被覆力を持った安定したカーボンナノチューブ分散系を得ること。
（２）カーボンナノチューブ被覆に適した天然繊維の表面改質法を開発すること。
また、炭素系の優れた機能を発現させるためには、カーボンナノチューブを繊維表面に規則正しく配列させることが必要である。
Accordingly, the inventors focused on the use of carbon nanotubes and tried to impart conductivity and thermal conductivity to the natural fiber material.
Carbon nanotubes are formed by rolling graphite sheets into cylinders, with diameters ranging from several nanometers to several tens of nanometers and lengths of several micrometers, and are indicated by carbon materials such as conductivity, thermal conductivity, and oxidation resistance. It is a powdery substance with high functionality.
Therefore, if this substance can be processed on natural fiber or coated on a natural fiber material, there is a possibility that a new functional material having both the flexibility of the natural material and the function of carbon nanotubes can be obtained.
However, carbon nanotubes are extremely difficult to disperse in aqueous systems, and as such, it is difficult to process and coat the natural fiber surface, and some kind of treatment is required.
Moreover, since fat remains on the surface of cotton yarn or the like that is a natural fiber, the affinity with water is low if it is left untreated.
For this reason, it has been found that there are still various problems when carbon nanotubes are coated on natural fibers, and in particular, it is essential to solve the following two problems.
(1) To obtain a stable carbon nanotube dispersion system having covering power to natural fibers.
(2) To develop a surface modification method for natural fibers suitable for carbon nanotube coating.
Further, in order to develop an excellent carbon-based function, it is necessary to regularly arrange the carbon nanotubes on the fiber surface.
本発明は上述の如き実状に対し、特に上記課題の解決を見出すことにより天然繊維素材に欠如している導電性及び熱伝導性を付与し、天然繊維の特質を保持し、現在使用されている炭素繊維よりも高機能を有する材料を提供することを目的とするものである。
The present invention gives the conductivity and thermal conductivity that are lacking in the natural fiber material by finding the solution of the above-mentioned problems to the actual situation as described above, and retains the characteristics of the natural fiber and is currently used. The object is to provide a material having a higher function than carbon fiber.
即ち、上記目的を達成する本発明の特徴は、カーボンナノチューブに質量比で該カーボンナノチューブの５〜２０倍の界面活性剤を混合し、更に蒸留水を加えてスラリー状のカーボンナノチューブを分散させた処理液を作り、天然繊維素材をこの処理液の中に浸漬・含浸させ天然繊維素材の表面にカーボンナノチューブを被覆せしめる方法にある。
ここで混合する界面活性剤はアニオン系，ノニオン系，カチオン系の何れでもよいが、好ましくはアニオン系，ノニオン系の界面活性剤である。
That is, the feature of the present invention that achieves the above object is that carbon nanotubes are mixed with a surfactant having a mass ratio of 5 to 20 times that of the carbon nanotubes, and distilled water is added to disperse the slurry-like carbon nanotubes. There is a method in which a treatment liquid is prepared and a natural fiber material is immersed and impregnated in the treatment liquid to cover the surface of the natural fiber material with carbon nanotubes.
The surfactant to be mixed here may be any of anionic, nonionic and cationic, but is preferably anionic or nonionic surfactant.
従来、疎水性粒子を水系に分散させる方法としては、界面活性剤を少量水系に添加し、安定な分散液を作ることが行われてきた。
カーボンナノチューブ分散系についてもこの手法を適用することはできるが、安定な分散系が得られてもこれがカーボンナノチューブと天然繊維との間に十分な結合力をもたらすものとは限らない。
Conventionally, as a method for dispersing hydrophobic particles in an aqueous system, a small amount of a surfactant is added to an aqueous system to form a stable dispersion.
Although this method can be applied to a carbon nanotube dispersion system, even if a stable dispersion system is obtained, this does not necessarily provide a sufficient bonding force between the carbon nanotube and the natural fiber.
そこで、本発明は、カーボンナノチューブに所要量、特にカーボンナノチューブの５〜２０倍の界面活性剤を混合し、スラリー状として処理液を作り、この中に天然繊維を浸漬し、含浸させることによりその表面にカーボンナノチューブを被覆固定せしめるようにした。
ここで、混合する界面活性剤としては前記の如くアニオン系，ノニオン系，カチオン系の何れも使用可能であるが、なかでもアニオン系，ノニオン系、特にノニオン系界面活性剤が好ましく、ポリオキシエチレン誘導体を始め、既知の界面活性剤が用いられる。
しかし、アニオン系，カチオン系の各種界面活性剤も使用することができる。
Therefore, the present invention mixes a required amount of carbon nanotubes with a surfactant, in particular 5 to 20 times that of carbon nanotubes, creates a treatment liquid as a slurry, and immerses and impregnates natural fibers in the treatment liquid. Carbon nanotubes were fixed on the surface by coating.
Here, as the surfactant to be mixed, any of anionic, nonionic, and cationic surfactants can be used as described above, and among them, anionic and nonionic surfactants, particularly nonionic surfactants are preferred, and polyoxyethylene Known surfactants are used, including derivatives.
However, various anionic and cationic surfactants can also be used.
上記本発明方法によれば、天然繊維素材の表面にカーボンナノチューブを十分な結合力をもって付着、被覆することができ、天然繊維の特性を保持し、しかも導電性，熱伝導性を備えた新機能材料を得ることができ、衣料用，産業用として各種用途への利用が期待される。
According to the method of the present invention, carbon nanotubes can be attached and coated on the surface of a natural fiber material with a sufficient binding force, and the new function that retains the properties of natural fibers and has conductivity and thermal conductivity. Materials can be obtained, and it is expected to be used for various purposes as clothing and industrial use.
上述したように本発明は、基本的に天然繊維にカーボンナノチューブを付着させるのに適した処理液の調製と、効果的に処理液からカーボンナノチューブを天然繊維に付着させるために不可欠な天然繊維の表面改質によって構成される。
As described above, the present invention is basically a preparation of a treatment liquid suitable for attaching carbon nanotubes to natural fibers, and the natural fibers essential for effectively attaching carbon nanotubes to natural fibers from the treatment liquid. Constructed by surface modification.
カーボンナノチューブは、嵩密度が低く非常に微細な粒子であり、取り扱いには十分な注意が必要である。
そのため、本発明で実施する天然繊維への付着・被覆の場合には、カーボンナノチューブを直接、付着させることは事実上、不可能であり、従って、ここで示すように処理液にカーボンナノチューブを分散させておき、その中に天然繊維を含浸させ被覆する方法が採用される。
しかしながら、カーボンナノチューブ自体は疎水性が極めて強く、水には容易に分散ではない。そこでカーボンナノチューブ表面を親水化する方法として、プラズマ処理や薬品による酸化処理が考えられるが、処理後の洗浄・処理に使う薬品の除去などに余分な工程が必要となるので好ましくない。
また、界面活性剤の疎水基をカーボンナノチューブ表面と結合させることによりカーボンナノチューブを親水化することはできるが、カーボンナノチューブの表面は９９％以上が疎水性のグラフェン面であるので、安定した分散系を得るためには少量の活性剤添加では効果を発揮できない。
そこで、本発明においては前記の如く特に質量比でカーボンナノチューブに対し５〜２０倍の界面活性剤を混合したスラリーを処理液に使用するようにした。
Carbon nanotubes are very fine particles with a low bulk density and must be handled with care.
For this reason, in the case of adhesion / coating to natural fibers performed in the present invention, it is practically impossible to attach carbon nanotubes directly. Therefore, as shown here, the carbon nanotubes are dispersed in the treatment liquid. In addition, a method of impregnating and coating natural fibers therein is employed.
However, carbon nanotubes themselves are extremely hydrophobic and are not easily dispersed in water. Thus, plasma treatment or chemical oxidation treatment can be considered as a method for hydrophilizing the carbon nanotube surface, but it is not preferable because an extra step is required for cleaning and removal of chemicals used for the treatment after the treatment.
In addition, it is possible to hydrophilize carbon nanotubes by bonding the hydrophobic group of the surfactant to the surface of the carbon nanotube. However, since the surface of the carbon nanotube is 99% or more of a hydrophobic graphene surface, a stable dispersion system In order to obtain a small amount of activator, the effect cannot be exhibited.
Therefore, in the present invention, as described above, a slurry in which a surfactant having a mass ratio of 5 to 20 times that of carbon nanotubes is mixed is used as the treatment liquid.
次に、本発明におけるスラリー状処理液の具体的な調製手順の概要を示す。
（１）先ず、容器にカーボンナノチューブを適宜量を計りとり、ここに界面活性剤を添加する。この場合、カーボンナノチューブと界面活性剤との配合割合としては、界面活性剤がカーボンナノチューブに対し所要適量であることが必要であり、例えばカーボンナノチューブ量に対し界面活性剤を５〜２０倍程度の割合で添加する。
そして、上記得られた添加物に次に蒸留水を所定量、好ましくはカーボンナノチューブと界面活性剤の総量の２倍程度の蒸留水を加え、これらを混合し、次いで蓋付きガラス容器に移して３０分×４回程度、超音波照射を行い均一化する。
（２）天然繊維の前処理１−脱脂・官能基の活性化
一方、天然繊維に対し、夫々試料を作成し、所要時間、例えば１時間又は６４時間、アルカリ溶液、例えば水酸化ナトリウム又はカリウム溶液に浸漬する。この場合、水酸化ナトリウム又はカリウムの濃度としては通常、０．３〜０．７ｍｏｌ／Ｌ程度が好ましい。
そして、浸漬後、取り出して十分に水洗し、蒸留水中に保存する。
（３）カーボンナノチューブ被覆操作の手順
かくして、上記の手順を経た後、前記カーボンナノチューブを分散したスラリー状の処理液に（２）に示した前処理を施した天然繊維を夫々浸漬し、所要時間後に引き上げ、過剰となった液を除き、６０℃前後の恒温乾燥機で所要時間、例えば２時間乾燥する。
Next, the outline of the specific preparation procedure of the slurry-like processing liquid in the present invention is shown.
(1) First, an appropriate amount of carbon nanotubes is measured in a container, and a surfactant is added thereto. In this case, as a mixing ratio of the carbon nanotube and the surfactant, it is necessary that the surfactant is an appropriate amount with respect to the carbon nanotube. For example, the surfactant is about 5 to 20 times the amount of the carbon nanotube. Add in proportions.
Then, a predetermined amount of distilled water is added to the additive obtained above, preferably about twice the total amount of carbon nanotubes and surfactant, mixed, and then transferred to a glass container with a lid. Uniform by performing ultrasonic irradiation for about 30 minutes × 4 times.
(2) Pretreatment of natural fiber 1-degreasing and functional group activation
On the other hand, a sample is prepared for each natural fiber and immersed in an alkaline solution such as sodium hydroxide or potassium solution for a required time, for example, 1 hour or 64 hours. In this case, the concentration of sodium hydroxide or potassium is usually preferably about 0.3 to 0.7 mol / L.
And after immersion, it is taken out, sufficiently washed with water, and stored in distilled water.
(3) Procedure for carbon nanotube coating operation
Thus, after passing through the above procedure, each of the natural fibers subjected to the pretreatment shown in (2) is immersed in a slurry-like treatment liquid in which the carbon nanotubes are dispersed, and the excess liquid is pulled up after the required time. Except for this, it is dried in a constant temperature dryer at about 60 ° C. for a required time, for example, 2 hours.
なお、上記本発明において天然繊維とは、天然に得られる繊維の外、天然で得られる素材を加工，再生した繊維を総称し、綿，麻の如き植物性繊維，絹，羊毛の如き動物性繊維，石綿の如き鉱物性繊維及びトウモロコシ，大豆等より作られた再生繊維や動植物性タンパクから作られた再生繊維が含まれるが、特に綿，麻の如き植物性繊維が最も効果的であり、綿糸，麻糸など、糸に限らず該繊維による織物，編物，不織布などの各構造体も含むものである。
In the present invention, the natural fiber is a generic term for fibers obtained by processing and regenerating natural materials, in addition to fibers obtained in nature, and plant-like fibers such as cotton and hemp, and animal properties such as silk and wool. Fibers, mineral fibers such as asbestos, and regenerated fibers made from corn, soybean, etc. and regenerated fibers made from animal and vegetable proteins are included, but vegetable fibers such as cotton and hemp are especially effective. It includes not only yarns, such as cotton yarn and hemp yarn, but also various structures such as woven fabrics, knitted fabrics and nonwoven fabrics.
以下、更に本発明の実施例として実験例を述べる。
先ず容器に表１に示す組成割合でカーボンナノチューブ２ｇにノニオン系界面活性剤３０ｇを添加し、更に蒸留水を７０ｇ加えて処理液を作成した。
Hereinafter, experimental examples will be described as examples of the present invention.
First, 30 g of a nonionic surfactant was added to 2 g of carbon nanotubes at a composition ratio shown in Table 1, and 70 g of distilled water was further added to prepare a treatment liquid.
一方、天然繊維として綿番手１０番手の綿糸を１０ｃｍ位の長さにカットして試料１，２を作り、夫々を０．５ｍｏｌ／Ｌの水酸化ナトリウム溶液に浸漬し、１時間後、試料１を、また６４時間後、試料２を夫々液中より取り出し、蒸留水中に保存した。
次いで、前記のカーボンナノチューブを分散したスラリー状処理液に前記前処理を施した夫々の綿糸を浸漬し５分後、綿糸を処理液より引き上げ、過剰となった液を除き、６０℃の恒温乾燥機で２時間乾燥した。
上記のようにしてカーボンナノチューブを被覆後、乾燥した綿糸表面は図１の走査型電子顕微鏡写真に示す如くであった。
同写真より本発明において綿糸表面がカーボンナノチューブを含む処理液で均一に被覆されていることが観察される。
次に上記の処理された綿糸を利用し、織物を作成したものは天然繊維のしなやかさ及び感触にカーボンナノチューブによる炭素特有の特性が付加され、今後の各用途への利用に十分期待できることが確認された。
On the other hand, 10 yarns of cotton count as natural fibers were cut to a length of about 10 cm to prepare Samples 1 and 2, and each was immersed in a 0.5 mol / L sodium hydroxide solution, and after 1 hour, Sample 1 After 64 hours, Sample 2 was taken out from the liquid and stored in distilled water.
Next, the respective pretreated cotton yarns are immersed in the slurry-like treatment liquid in which the carbon nanotubes are dispersed, and after 5 minutes, the cotton yarn is pulled up from the treatment liquid, and the excess liquid is removed, followed by constant temperature drying at 60 ° C. Dried for 2 hours.
After coating the carbon nanotubes as described above, the surface of the dried cotton yarn was as shown in the scanning electron micrograph of FIG.
From the photograph, it is observed that the surface of the cotton yarn is uniformly coated with the treatment liquid containing carbon nanotubes in the present invention.
Next, using the above-treated cotton yarn, weaving fabrics confirmed that carbon fiber-specific characteristics are added to the suppleness and feel of natural fibers, and that it can be fully expected for future use. It was done.
Claims (2)
カーボンナノチューブに、質量比で該カーボンナノチューブの５〜２０倍の界面活性剤を混合し、次いで蒸留水を加えてスラリー状処理液とし、該処理液に天然繊維を浸漬・含浸させ、天然繊維表面にカーボンナノチューブを被覆せしめることを特徴とするカーボンナノチューブを天然繊維へ被覆する方法。
A carbon nanotube is mixed with a surfactant having a mass ratio of 5 to 20 times that of the carbon nanotube, and then distilled water is added to form a slurry-like treatment liquid. A method of coating a natural fiber with a carbon nanotube, comprising coating a carbon nanotube with a carbon nanotube.
界面活性剤がアニオン系又はノニオン系界面活性剤である請求項１記載のカーボンナノチューブを天然繊維へ被覆する方法。
The method for coating a natural fiber with carbon nanotubes according to claim 1, wherein the surfactant is an anionic or nonionic surfactant.
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Cited By (13)
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| WO2009054415A1 (en) * | 2007-10-23 | 2009-04-30 | Tokushu Paper Mfg. Co., Ltd. | Sheet-like article and method for producing the same |
| JP2010040730A (en) * | 2008-08-05 | 2010-02-18 | Tokushu Paper Mfg Co Ltd | Sheet-like article |
| WO2010026937A1 (en) * | 2008-09-02 | 2010-03-11 | 国立大学法人 北海道大学 | Electroconductive fibers with carbon nanotubes deposited thereon, electroconductive threads, fiber structure, and process for producing same |
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