JPH06287355A - Molding containing ultrafine particle dispersed therein - Google Patents
Molding containing ultrafine particle dispersed thereinInfo
- Publication number
- JPH06287355A JPH06287355A JP5076812A JP7681293A JPH06287355A JP H06287355 A JPH06287355 A JP H06287355A JP 5076812 A JP5076812 A JP 5076812A JP 7681293 A JP7681293 A JP 7681293A JP H06287355 A JPH06287355 A JP H06287355A
- Authority
- JP
- Japan
- Prior art keywords
- resin
- ultrafine particles
- fibers
- dispersed
- fiber
- 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.)
- Withdrawn
Links
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は超微粒子が均一に分散し
ている繊維と樹脂成形物に関する。繊維や樹脂成形物に
超微粒子を添加することにより、様々な機能、例えば、
抗菌性・防カビ性・防臭性、難燃性、紫外線防止、蓄熱
性、表面性の改善、清涼感等を付与することが行われ
る。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fiber and a resin molded product in which ultrafine particles are uniformly dispersed. By adding ultrafine particles to fibers and resin molded products, various functions such as
Antibacterial / mold / deodorant properties, flame retardancy, UV protection, heat storage properties, surface property improvement, and refreshing feeling are provided.
【０００２】[0002]
【従来の技術】粒径がミクロンオーダの無機微粒子を繊
維や樹脂成形物に添加することにより、様々な機能を付
与することが、従来より行われている。例えば、抗菌性
・防カビ性・防臭性、難燃性、紫外線防止、蓄熱性、表
面性の改善、清涼感の付与などである。2. Description of the Related Art It has been conventionally practiced to add various functions by adding inorganic fine particles having a particle size on the order of micron to a fiber or a resin molded product. For example, antibacterial / mold / deodorant properties, flame retardancy, UV protection, heat storage, surface property improvement, and refreshing sensation.
【０００３】しかしながら、平均粒径が２００ｎｍ未満
の超微粒子を用いた場合、繊維や樹脂成形物に添加する
際に超微粒子が繊維や成形物の作製時に凝集してしま
い、均一に分散させることが困難であった。However, when ultrafine particles having an average particle size of less than 200 nm are used, the ultrafine particles aggregate during the production of the fiber or molded product when added to the fiber or resin molded product, and can be dispersed uniformly. It was difficult.
【０００４】[0004]
【発明が解決しようとする課題】本発明は、均一性の優
れた超微粒子分散繊維及び樹脂成形物を提供することを
目的とする。SUMMARY OF THE INVENTION It is an object of the present invention to provide ultrafine particle-dispersed fibers and resin molded products having excellent uniformity.
【０００５】[0005]
【課題を解決するための手段】繊維や樹脂成形物を作製
する際の溶融混練工程などの工程に於いて直接に超微粒
子粉体を添加すると、超微粒子が凝集してしまい、超微
粒子が均一に分散していない。ところが、成形物の原料
である高分子中で直接超微粒子を作製すると均一な分散
状態を実現できることを見出し、本発明を完成するに到
った。[Means for Solving the Problems] When ultrafine particle powder is directly added in a step such as a melt-kneading step in producing a fiber or a resin molded product, the ultrafine particles are agglomerated and the ultrafine particles are uniform. Not dispersed in. However, they have found that a uniform dispersion state can be realized by directly producing ultrafine particles in a polymer, which is a raw material for a molded product, and have completed the present invention.
【０００６】すなわち、本発明は平均粒径が２００ｎｍ
未満１ｎｍ以上の超微粒子が分散している成形物におい
て、超微粒子の粒径分布及び分散状態が均一に維持され
ていることを特徴とする成形物である。本発明におい
て、成形物とは繊維及び樹脂成形物である。繊維として
は綿、羊毛、絹、麻などの天然繊維、レーヨン繊維、キ
ュプラ繊維などの再生繊維、アセテート繊維、ビニロン
繊維、ナイロン繊維、ビニリデン繊維、ポリ塩化ビニル
繊維、ポリエステル繊維、ポリエチレン繊維、アクリル
繊維、ポリプロピレン繊維などの合成繊維及びガラス繊
維などの無機繊維などを挙げることができる。That is, the present invention has an average particle size of 200 nm.
In a molded product in which ultrafine particles having a size of less than 1 nm are dispersed, the particle size distribution and dispersed state of the ultrafine particles are maintained uniformly. In the present invention, the molded product is a fiber or resin molded product. The fibers include natural fibers such as cotton, wool, silk and hemp, recycled fibers such as rayon fibers and cupra fibers, acetate fibers, vinylon fibers, nylon fibers, vinylidene fibers, polyvinyl chloride fibers, polyester fibers, polyethylene fibers, acrylic fibers. , Synthetic fibers such as polypropylene fibers, and inorganic fibers such as glass fibers.
【０００７】樹脂としては、熱可塑性樹脂、熱硬化性樹
脂などを用いることができる。具体的には熱可塑性樹脂
としては、ＡＡＳ樹脂、ＡＥＳ樹脂、ＡＳ樹脂、イソフ
チレンー無水マレイン酸共重合樹脂、ＡＢＳ樹脂、ＡＣ
Ｓ樹脂、エチレンー塩ビ共重合樹脂、塩化ビリニデン樹
脂、塩化ビニル樹脂、クマロン樹脂、ケトン樹脂、酢酸
ビニル樹脂、フェノキシ樹脂、ブタジエン樹脂、フッ素
樹脂、ポリアセタール、ポリアミド、ポリアミドイミ
ド、ポリアリレート、ポリエーテルイミド、ポリエーテ
ルエーテルケトン、ポリエチレン、ポリエチレンテレフ
タレート、ポリカーボネート、ポリスチレン、ポリサル
ホン、ポリパラメチルスチレン、ポリビニルアルコー
ル、ポリビニルエーテル、ポリビニルブチラール、ポリ
ビニルホルマール、ポリフェニレンエーテル、ポリフェ
ニレンサルファイド、ポリプロピレン、ポリメチレペン
テン、メタクリル樹脂、液晶ポリマーなどを挙げること
ができる。As the resin, a thermoplastic resin, a thermosetting resin or the like can be used. Specific examples of the thermoplastic resin include AAS resin, AES resin, AS resin, isophthalene-maleic anhydride copolymer resin, ABS resin, and AC resin.
S resin, ethylene-vinyl chloride copolymer resin, vinylidene chloride resin, vinyl chloride resin, coumarone resin, ketone resin, vinyl acetate resin, phenoxy resin, butadiene resin, fluororesin, polyacetal, polyamide, polyamideimide, polyarylate, polyetherimide, Polyether ether ketone, polyethylene, polyethylene terephthalate, polycarbonate, polystyrene, polysulfone, polyparamethylstyrene, polyvinyl alcohol, polyvinyl ether, polyvinyl butyral, polyvinyl formal, polyphenylene ether, polyphenylene sulfide, polypropylene, polymethylene pentene, methacrylic resin, liquid crystal polymer And so on.
【０００８】熱硬化性樹脂としては、ＤＦＫ樹脂、エポ
キシ樹脂、キシレン樹脂、フェノール樹脂、ポリイミ
ド、ポリウレタン、メラニン樹脂、ユリア樹脂、ビニル
エステル樹脂、不飽和ポリエステル樹脂などを挙げるこ
とができる。更にメチルセルロース、エチルセルロー
ス、アセテートプラスチック、酢酸セルロースなどの天
然高分子を挙げることができる。Examples of the thermosetting resin include DFK resin, epoxy resin, xylene resin, phenol resin, polyimide, polyurethane, melanin resin, urea resin, vinyl ester resin and unsaturated polyester resin. Further, natural polymers such as methyl cellulose, ethyl cellulose, acetate plastic, cellulose acetate and the like can be mentioned.
【０００９】本発明の樹脂成形物とは上記樹脂を射出成
形、押し出し成形、圧縮成形などの成形法を用いて様々
な形に成形した樹脂成形物である。本発明の超微粒子の
材質としては特に限定されないが、金属、半導体、酸化
物、硫化物、有機物などが挙げられる。好ましくは銀、
金、銅、パラジウム、ロジウム、白金などの金属や酸化
銀、酸化銅、酸化チタン、酸化亜鉛などの酸化物、硫化
カドミウム、セレン化カドミウム、硫化亜鉛、セレン化
亜鉛、シリコン、ゲルマニウムなどの半導体を挙げるこ
とができる。より好ましくは銀、金、銅、パラジウム、
ロジウム、白金などの金属や酸化銀、酸化銅などの酸化
物である。The resin molded product of the present invention is a resin molded product obtained by molding the above resin into various shapes using a molding method such as injection molding, extrusion molding or compression molding. The material of the ultrafine particles of the present invention is not particularly limited, and examples thereof include metals, semiconductors, oxides, sulfides and organic substances. Preferably silver,
Metals such as gold, copper, palladium, rhodium and platinum, oxides such as silver oxide, copper oxide, titanium oxide and zinc oxide, semiconductors such as cadmium sulfide, cadmium selenide, zinc sulfide, zinc selenide, silicon and germanium. Can be mentioned. More preferably silver, gold, copper, palladium,
Metals such as rhodium and platinum and oxides such as silver oxide and copper oxide.
【００１０】平均粒径は、次のように測定した。作製し
た繊維や樹脂成形物をウルトラミクロトームを用いて、
超薄切片を作製し、この切片をコロジオン支持膜を張り
付けた銅製グリッド上に載物し、カーボン蒸着処理を行
って透過型電子顕微鏡観察用試料とした。超薄切片の厚
みは５０ｎｍ以上１００ｎｍ以下である。透過型電子顕
微鏡（日本電子（株）製 ＪＥＭ−４０００ＦＸ）を用
いて、加速電圧２００ｋＶで観察倍率５万倍あるいは１
０万倍で行い、写真倍率２０万倍あるいは４０万倍にし
た写真を用いた。次に、この写真を用いて、画像解析装
置写真中の一定範囲内の近接する超微粒子１００個の直
径を測定し、その算術平均を平均粒径とした。但し、写
真内に超微粒子が１００個に満たない場合は、異なる場
所の透過型電子顕微鏡写真を必要枚数用いて１００個に
し、平均粒径とした。The average particle size was measured as follows. Using an ultramicrotome for the produced fibers and resin molded products,
An ultrathin section was prepared, and this section was placed on a copper grid to which a collodion support film was attached, and carbon vapor deposition treatment was performed to obtain a sample for transmission electron microscope observation. The thickness of the ultrathin section is 50 nm or more and 100 nm or less. Using a transmission electron microscope (JEM-4000FX, manufactured by JEOL Ltd.), an observation magnification of 50,000 times or 1 at an acceleration voltage of 200 kV.
Photographs were taken at a magnification of 200,000 and a magnification of 200,000 or 400,000 was used. Next, using this photograph, the diameters of 100 adjacent ultrafine particles within a certain range in the photograph of the image analyzer were measured, and the arithmetic average thereof was taken as the average particle diameter. However, when the number of ultrafine particles in the photograph was less than 100, the required number of transmission electron micrographs at different locations were used to obtain 100 particles, and the average particle diameter was obtained.
【００１１】粒径分布が均一であるとは、平均粒径Ｒと
したときに、測定した超微粒子の直径が０．５Ｒ以上
１．５Ｒ以下の範囲に、測定した超微粒子の５０％以上
が存在していることを意味する。より粒径分布が均一な
場合は７５％以上が存在している。分散状態が均一であ
るとは、平均粒径測定用の電子顕微鏡写真において、平
均粒径測定に使用した１００個の粒子のうち、重なって
いる粒子が３０個以下である状態である。より分散状態
が均一である場合は重なっている粒子が１０個以下であ
る。Uniform particle size distribution means that when the average particle size is R, 50% or more of the measured ultrafine particles are in the range of 0.5R or more and 1.5R or less. It means that it exists. When the particle size distribution is more uniform, 75% or more is present. The uniform dispersion state means a state in which, in the electron micrograph for measuring the average particle diameter, out of 100 particles used for measuring the average particle diameter, 30 or less overlapped particles. When the dispersed state is more uniform, the number of overlapping particles is 10 or less.
【００１２】分散状態が均一な部分は局在化していても
構わない。もちろん、全体の分散状態が均一であっても
一向に構わない。局在化しているとは、例えば、表面付
近にのみあるいは中央付近にのみ、超微粒子が存在し、
その部分で上記の分散状態が均一であることを意味して
いる。材料中の超微粒子の量としては、何に分散するか
によってまた、どのような性能を与えるかによって当然
異なる。たとえば繊維や樹脂などの高分子に分散する場
合は５ｗｔ％以下０．１ｐｐｍ以上である。The portion where the dispersion state is uniform may be localized. Of course, it does not matter if the entire dispersion state is uniform. Localized means that, for example, ultrafine particles exist only near the surface or only near the center,
This means that the dispersed state is uniform in that portion. The amount of ultrafine particles in the material naturally depends on what is dispersed and what performance is given. For example, when dispersed in a polymer such as fiber or resin, the content is 5 wt% or less and 0.1 ppm or more.
【００１３】本発明において、超微粒子の平均粒径は２
００ｎｍ未満１ｎｍ以上であることが必要である。平均
粒径が１ｎｍ未満の超微粒子は上述のような分散状態で
は現在作製できていない。上記の分散状態や粒径分布を
達成するための手段としては、上記の条件が達成できれ
ば特に限定されないが、好ましい方法としては繊維や樹
脂成形物を作製するための原料である高分子固相中で超
微粒子を作製する方法などを挙げることができる。例え
ば、金属塩と還元剤などを溶解あるいは含浸させた高分
子ペレットなどの高分子原料を加熱処理することによ
り、高分子原料中で還元させ、高分子原料内に超微粒子
を作製する方法を用いることができる。また、溶剤に可
溶な高分子を溶剤に溶解させた後、金属塩と還元剤を添
加して還元反応により超微粒子を作製し、その後溶剤を
除去させ、超微粒子が分散した高分子原料を作製する方
法、高分子原料中に金属塩のみを溶解あるいは含浸させ
たのち、加熱処理をすることにより、金属塩を還元させ
超微粒子を高分子原料中に作製する方法を用いることが
できる。In the present invention, the average particle size of the ultrafine particles is 2
It is necessary to be less than 00 nm and 1 nm or more. Ultrafine particles having an average particle size of less than 1 nm cannot be currently produced in the dispersed state as described above. The means for achieving the above-mentioned dispersed state and particle size distribution is not particularly limited as long as the above conditions can be achieved, but a preferable method is in a polymer solid phase which is a raw material for producing fibers and resin molded products. And a method for producing ultrafine particles. For example, a method of producing ultrafine particles in a polymer raw material by heating a polymer raw material such as a polymer pellet in which a metal salt and a reducing agent are dissolved or impregnated to reduce the polymer raw material be able to. Also, after dissolving a polymer soluble in a solvent in a solvent, ultrafine particles are prepared by a reduction reaction by adding a metal salt and a reducing agent, and then the solvent is removed to prepare a polymer raw material in which the ultrafine particles are dispersed. It is possible to use a method of producing, in which the metal salt alone is dissolved or impregnated in the polymer raw material, and then heat treatment is performed to reduce the metal salt to produce ultrafine particles in the polymer raw material.
【００１４】そして、この高分子原料を用いて、繊維に
加工することもできる。また、この高分子原料を用い
て、射出成形、押し出し成形、ブロウ成形などを行うこ
とにより、様々な樹脂成形品を作製することができる。
繊維や樹脂成形品などの表面に超微粒子を分散させる場
合には、繊維や樹脂成形品などに直接金属塩などを含浸
させ、加熱処理あるいは、還元処理をすることにより、
表面に高濃度に分散させることも可能である。The polymer raw material can be used to process into fibers. Further, various resin molded products can be produced by performing injection molding, extrusion molding, blow molding and the like using this polymer raw material.
When ultrafine particles are dispersed on the surface of fibers or resin molded products, the fibers or resin molded products are directly impregnated with a metal salt or the like, and subjected to heat treatment or reduction treatment,
It is also possible to disperse in high concentration on the surface.
【００１５】[0015]
【実施例】以下の実施例によって本発明を更に詳細に説
明するが、本発明はこれらの実施例によって限定される
ものではない。The present invention will be described in more detail with reference to the following examples, but the present invention is not limited to these examples.
【００１６】[0016]
【実施例１】次のようにしてマスターバッチを作製し
た。下記に示す組成の塗布液を作製した。 ポリスチレン １０ｇ ヘプタフルオロ酪酸銀 ０．０１ｇ 2-t-ブチル-6-(3-t-ブチル-2- ヒドロキシ-5- メチルベンジル）-4- メチルフェ ニルアクリレート ０．０２ｇ メチルエチルケトン ６０ｇ トルエン ３０ｇ この塗布液を平均孔径０．２μｍのフィルターを通して
ろ過した後、ブレードコータを用いて乾燥後の膜厚が６
μｍになるように、ポリエチレンテレフタレート（ＰＥ
Ｔ）フィルム上に均一に塗布し、自然乾燥させた。その
後オーブンを用いて１５０℃で３０分間加熱処理をした
後、スチレン膜をＰＥＴフィルムから剥離させ、このス
チレン膜をマスターバッチとした。このマスターバッチ
を用いて、銀量が０．０５ｗｔ％になるようにポリスチ
レンと混ぜて、射出成形をおこない、抗菌性評価サンプ
ルを作製した。Example 1 A masterbatch was prepared as follows. A coating liquid having the composition shown below was prepared. Polystyrene 10 g Silver heptafluorobutyrate 0.01 g 2-t-butyl-6- (3-t-butyl-2-hydroxy-5-methylbenzyl) -4-methylphenyl acrylate 0.02 g Methyl ethyl ketone 60 g Toluene 30 g After filtering through a filter with an average pore size of 0.2 μm, the film thickness after drying was 6 using a blade coater.
Polyethylene terephthalate (PE
T) A film was evenly applied and naturally dried. After that, heat treatment was performed for 30 minutes at 150 ° C. in an oven, and then the styrene film was peeled off from the PET film, and this styrene film was used as a masterbatch. Using this masterbatch, it was mixed with polystyrene so that the amount of silver was 0.05 wt%, and injection molding was performed to prepare an antibacterial property evaluation sample.
【００１７】電子顕微鏡写真を用いて、粒径を測定した
ところ平均粒径は９ｎｍであった。また、測定した１０
０個の銀微粒子はすべて独立に分散していた。粒径分布
に関しては粒径は４．５ｎｍ以上１３．５ｎｍ以下の範
囲に８５％の粒子が存在していた。When the particle size was measured using an electron micrograph, the average particle size was 9 nm. Also, measured 10
All 0 silver particles were dispersed independently. Regarding the particle size distribution, 85% of particles were present in the range of 4.5 nm to 13.5 nm.
【００１８】[0018]
【実施例２】次のようにしてマスターバッチを作製し
た。下記に示す組成の液を作製した。 トリフルオロ酢酸銀 ０．１ｇ メタノール １５ｇ この液に一晩ナイロン６のペレットを浸漬させた後、溶
液からペレットを取り出し、溶媒を除去した後、オーブ
ンを用いて１５０℃で３０分間加熱処理をした。このマ
スターバッチを用いて、銀量が約０．０１ｗｔ％になる
ようにナイロン６６チップを混ぜて、１０デニールの糸
を作製した。その後、この糸を用いて布を作製した。電
子顕微鏡写真を用いて、粒径を測定したところ平均粒径
は１９ｎｍであった。測定した銀微粒子１００個すべて
は独立に分散していた。粒径分布に関しては、粒径が
９．５ｎｍ以上２８．５ｎｍ以下の範囲に７５％の超微
粒子が存在していた。Example 2 A masterbatch was prepared as follows. A liquid having the composition shown below was prepared. Silver trifluoroacetate 0.1 g Methanol 15 g After immersing the nylon 6 pellets in this solution overnight, the pellets were taken out from the solution, the solvent was removed, and then heat treatment was performed at 150 ° C. for 30 minutes using an oven. Using this masterbatch, nylon 66 chips were mixed so that the amount of silver was about 0.01 wt%, to prepare a 10 denier yarn. Then, a cloth was produced using this thread. When the particle size was measured using an electron micrograph, the average particle size was 19 nm. All 100 fine silver particles measured were independently dispersed. Regarding the particle size distribution, 75% of ultrafine particles were present in the range of particle size 9.5 nm or more and 28.5 nm or less.
【００１９】[0019]
【実施例３】下記の成分からなる塗工液を作製した。 塩化金酸ナトリウム ０．１ｇ ポリウレタン １００ｇ イソプロピルアルコール ７００ｇ メチルアルコール １００ｇ トルエン ４００ｇ この塗工液を平均孔径０．２μｍのフィルタ−を通して
ろ過した後、ブレードコ−タによって乾燥後、膜厚６μ
ｍになるように、旭化成製のナイロン６（品番１１６
２）布上に均一に塗布し、温度３０℃、湿度４５％RHの
条件で乾燥した。このサンプルを１５０℃で２０分間加
熱した。このサンプルをミクロトームを用いて透過型電
子顕微鏡用切片を作製し、電子顕微鏡を用いて観察し
た。電子顕微鏡は（株）日立製作所製Ｈ−５００を用い
て検鏡した。写真より１００個の金微粒子の直径を測定
したところ算術平均粒径は２８ｎｍであった。１００個
の金微粒子は９５個が独立に分散していた。粒径分布に
関しては、１４ｎｍ以上４２ｎｍ以下の範囲に９０％の
超微粒子が存在していた。Example 3 A coating solution containing the following components was prepared. Sodium chloroaurate 0.1 g Polyurethane 100 g Isopropyl alcohol 700 g Methyl alcohol 100 g Toluene 400 g After filtering this coating solution through a filter having an average pore size of 0.2 μm, it was dried with a blade coater to give a film thickness of 6 μm.
Asahi Kasei nylon 6 (Part No. 116
2) It was evenly applied onto a cloth and dried under the conditions of a temperature of 30 ° C. and a humidity of 45% RH. The sample was heated at 150 ° C. for 20 minutes. A section for a transmission electron microscope was prepared from this sample using a microtome and observed using an electron microscope. As an electron microscope, H-500 manufactured by Hitachi, Ltd. was used. When the diameter of 100 fine gold particles was measured from the photograph, the arithmetic average particle diameter was 28 nm. 95 of 100 gold particles were dispersed independently. Regarding the particle size distribution, 90% of ultrafine particles were present in the range of 14 nm to 42 nm.
【００２０】[0020]
【発明の効果】超微粒子の粒径分布がシャープであり、
かつ超微粒子の凝集が少なく独立に存在している均一性
の高い新しい繊維や樹脂成形物を提供することができ
る。EFFECT OF THE INVENTION The particle size distribution of ultrafine particles is sharp,
In addition, it is possible to provide a highly uniform new fiber or resin molded product in which ultrafine particles have little aggregation and exist independently.
Claims (1)
超微粒子が分散している成形物において、超微粒子の粒
径分布及び分散状態が均一に維持されていることを特徴
とする成形物。1. A molded article in which ultrafine particles having an average particle size of less than 200 nm and 1 nm or more are dispersed, wherein the particle size distribution and dispersed state of the ultrafine particles are maintained uniformly.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5076812A JPH06287355A (en) | 1993-04-02 | 1993-04-02 | Molding containing ultrafine particle dispersed therein |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5076812A JPH06287355A (en) | 1993-04-02 | 1993-04-02 | Molding containing ultrafine particle dispersed therein |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH06287355A true JPH06287355A (en) | 1994-10-11 |
Family
ID=13616088
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5076812A Withdrawn JPH06287355A (en) | 1993-04-02 | 1993-04-02 | Molding containing ultrafine particle dispersed therein |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH06287355A (en) |
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- 1993-04-02 JP JP5076812A patent/JPH06287355A/en not_active Withdrawn
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