JP7500104B1 - Treatment agent for producing carbon fiber-containing nonwoven fabric, carbon fiber-containing nonwoven fabric, and method for producing carbon fiber-containing nonwoven fabric - Google Patents
Treatment agent for producing carbon fiber-containing nonwoven fabric, carbon fiber-containing nonwoven fabric, and method for producing carbon fiber-containing nonwoven fabric Download PDFInfo
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- JP7500104B1 JP7500104B1 JP2023069461A JP2023069461A JP7500104B1 JP 7500104 B1 JP7500104 B1 JP 7500104B1 JP 2023069461 A JP2023069461 A JP 2023069461A JP 2023069461 A JP2023069461 A JP 2023069461A JP 7500104 B1 JP7500104 B1 JP 7500104B1
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- JP
- Japan
- Prior art keywords
- carbon fiber
- nonwoven fabric
- treatment agent
- mass
- containing nonwoven
- 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.)
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- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 87
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 83
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 83
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000004745 nonwoven fabric Substances 0.000 title claims abstract description 55
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 150000001875 compounds Chemical class 0.000 claims abstract description 58
- 239000004593 Epoxy Substances 0.000 claims abstract description 41
- -1 ester compound Chemical class 0.000 claims description 57
- 239000002736 nonionic surfactant Substances 0.000 claims description 34
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 16
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 12
- DNIAPMSPPWPWGF-GSVOUGTGSA-N (R)-(-)-Propylene glycol Chemical compound C[C@@H](O)CO DNIAPMSPPWPWGF-GSVOUGTGSA-N 0.000 claims description 6
- 150000001732 carboxylic acid derivatives Chemical class 0.000 claims description 6
- ZZTCPWRAHWXWCH-UHFFFAOYSA-N diphenylmethanediamine Chemical compound C=1C=CC=CC=1C(N)(N)C1=CC=CC=C1 ZZTCPWRAHWXWCH-UHFFFAOYSA-N 0.000 claims description 3
- 239000000835 fiber Substances 0.000 description 27
- 238000000034 method Methods 0.000 description 23
- 125000002947 alkylene group Chemical group 0.000 description 15
- 238000009960 carding Methods 0.000 description 12
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 8
- 239000003063 flame retardant Substances 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- 239000000126 substance Substances 0.000 description 7
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- 150000001735 carboxylic acids Chemical class 0.000 description 6
- 230000000694 effects Effects 0.000 description 6
- VKOBVWXKNCXXDE-UHFFFAOYSA-N icosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCC(O)=O VKOBVWXKNCXXDE-UHFFFAOYSA-N 0.000 description 6
- 238000011156 evaluation Methods 0.000 description 5
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- 239000012209 synthetic fiber Substances 0.000 description 4
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- PUPZLCDOIYMWBV-UHFFFAOYSA-N (+/-)-1,3-Butanediol Chemical compound CC(O)CCO PUPZLCDOIYMWBV-UHFFFAOYSA-N 0.000 description 2
- OBETXYAYXDNJHR-SSDOTTSWSA-M (2r)-2-ethylhexanoate Chemical compound CCCC[C@@H](CC)C([O-])=O OBETXYAYXDNJHR-SSDOTTSWSA-M 0.000 description 2
- YWWVWXASSLXJHU-AATRIKPKSA-N (9E)-tetradecenoic acid Chemical compound CCCC\C=C\CCCCCCCC(O)=O YWWVWXASSLXJHU-AATRIKPKSA-N 0.000 description 2
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- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 description 2
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- BTVWZWFKMIUSGS-UHFFFAOYSA-N 2-methylpropane-1,2-diol Chemical compound CC(C)(O)CO BTVWZWFKMIUSGS-UHFFFAOYSA-N 0.000 description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 description 2
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- 229930185605 Bisphenol Natural products 0.000 description 2
- FERIUCNNQQJTOY-UHFFFAOYSA-N Butyric acid Chemical compound CCCC(O)=O FERIUCNNQQJTOY-UHFFFAOYSA-N 0.000 description 2
- QUSNBJAOOMFDIB-UHFFFAOYSA-N Ethylamine Chemical compound CCN QUSNBJAOOMFDIB-UHFFFAOYSA-N 0.000 description 2
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- AMQJEAYHLZJPGS-UHFFFAOYSA-N N-Pentanol Chemical compound CCCCCO AMQJEAYHLZJPGS-UHFFFAOYSA-N 0.000 description 2
- REYJJPSVUYRZGE-UHFFFAOYSA-N Octadecylamine Chemical compound CCCCCCCCCCCCCCCCCCN REYJJPSVUYRZGE-UHFFFAOYSA-N 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 description 2
- 239000004952 Polyamide Substances 0.000 description 2
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 description 2
- 125000005233 alkylalcohol group Chemical group 0.000 description 2
- OBETXYAYXDNJHR-UHFFFAOYSA-N alpha-ethylcaproic acid Natural products CCCCC(CC)C(O)=O OBETXYAYXDNJHR-UHFFFAOYSA-N 0.000 description 2
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Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
【課題】炭素繊維の折れを低減できる炭素繊維含有不織布製造用の処理剤、炭素繊維含有不織布、及び炭素繊維含有不織布の製造方法を提供する。【解決手段】本発明の炭素繊維含有不織布製造用の処理剤は、エポキシ化合物(A)を含有することを特徴とする。【選択図】なしThe present invention provides a treatment agent for producing a carbon fiber-containing nonwoven fabric, which can reduce breakage of carbon fibers, a carbon fiber-containing nonwoven fabric, and a method for producing a carbon fiber-containing nonwoven fabric. The treatment agent for producing a carbon fiber-containing nonwoven fabric of the present invention is characterized by containing an epoxy compound (A). [Selected Figures] None
Description
本発明は、炭素繊維含有不織布製造用の処理剤、かかる処理剤が付着している炭素繊維含有不織布、及びかかる処理剤を用いた炭素繊維含有不織布の製造方法に関する。 The present invention relates to a treatment agent for producing carbon fiber-containing nonwoven fabric, a carbon fiber-containing nonwoven fabric to which such a treatment agent is attached, and a method for producing a carbon fiber-containing nonwoven fabric using such a treatment agent.
一般に、炭素繊維は、例えばエポキシ樹脂等のマトリクス樹脂と組み合わせた炭素繊維複合材料又は難燃・防炎素材として、建材、輸送機器等の各分野において広く利用されている。例えば、炭素繊維は、炭素繊維前駆体として、例えばアクリル繊維を紡糸する工程、繊維を延伸する工程、耐炎化工程、及び炭素化工程を経て製造される。 In general, carbon fibers are widely used in various fields such as building materials and transportation equipment as carbon fiber composite materials combined with matrix resins such as epoxy resins or as flame-retardant and fire-resistant materials. For example, carbon fibers are produced through a process of spinning acrylic fibers as a carbon fiber precursor, a process of drawing the fibers, a flame-retardant process, and a carbonization process.
炭素繊維は、織物の他、ローラーカード(カード機)を使用して得られる不織布等に成形して用いられることがある。不織布を製造する際、原料繊維に対してカード通過性等の各種特性を付与する観点から、繊維の表面に不織布用処理剤を付着させる処理が行われることがある。従来、特許文献1に開示される処理剤が知られている。 Carbon fibers may be used in the form of woven fabrics or nonwoven fabrics obtained using a roller card (carding machine). When producing nonwoven fabrics, a treatment may be applied to the surface of the raw fiber to impart various properties such as carding properties to the fiber. A treatment disclosed in Patent Document 1 is known.
しかし、処理剤が付与された炭素繊維がカード機を通過する際、炭素繊維の折れが生ずることがあった。炭素繊維含有不織布製造用の処理剤について、炭素繊維の折れの低減効果の更なる向上が求められていた。 However, when the carbon fibers to which the treatment agent was applied passed through a carding machine, the carbon fibers sometimes broke. There was a demand for further improvements in the effect of reducing breakage of carbon fibers in treatment agents used in the production of carbon fiber-containing nonwoven fabrics.
本発明者らは、前記の課題を解決するべく研究した結果、炭素繊維含有不織布製造用の処理剤において、エポキシ化合物(A)を配合した構成が好適であることを見出した。
上記課題を解決する各態様を記載する。
As a result of research aimed at solving the above problems, the present inventors have found that a treatment agent for producing a carbon fiber-containing nonwoven fabric containing an epoxy compound (A) is preferably used.
Various aspects for solving the above problems will be described below.
態様1の炭素繊維含有不織布製造用の処理剤は、エポキシ化合物(A)、ノニオン界面活性剤(B)、及びエステル化合物(C)を含有する炭素繊維含有不織布製造用の処理剤であって、前記処理剤の不揮発分における前記エポキシ化合物(A)の含有割合が5質量%以上60質量%以下であり、前記エステル化合物(C)の含有割合が5~50質量%であり、前記エポキシ化合物(A)は、主骨格としてビスフェノールA、ビスフェノールF、及びジアミノジフェニルメタンから選ばれる少なくとも一種を有することを特徴とする。 The treatment agent for producing a carbon fiber-containing nonwoven fabric of Aspect 1 is a treatment agent for producing a carbon fiber-containing nonwoven fabric, comprising an epoxy compound (A) , a nonionic surfactant (B) , and an ester compound (C) , characterized in that the content of the epoxy compound (A) in the nonvolatile matter of the treatment agent is 5 mass% or more and 60 mass% or less, the content of the ester compound (C) is 5 to 50 mass%, and the epoxy compound (A) has at least one compound selected from bisphenol A, bisphenol F, and diaminodiphenylmethane as a main skeleton.
エステル化合物(C):1価脂肪族アルコールと1価カルボン酸とからなるエステル化合物。
態様2の炭素繊維含有不織布製造用の処理剤は、エポキシ化合物(A)、ノニオン界面活性剤(B)、及びエステル化合物(C)を含有する炭素繊維含有不織布製造用の処理剤であって、前記処理剤の不揮発分における前記ノニオン界面活性剤(B)の含有割合が30質量%以上60質量%以下であり、前記エステル化合物(C)の含有割合が5~40質量%であり、前記エポキシ化合物(A)は、主骨格としてビスフェノールA及びビスフェノールFから選ばれる少なくとも一種を有することを特徴とする。
Ester compound (C): An ester compound consisting of a monohydric aliphatic alcohol and a monobasic carboxylic acid.
The treatment agent for producing a carbon fiber-containing nonwoven fabric of Aspect 2 contains an epoxy compound (A) , a nonionic surfactant (B) , and an ester compound (C) , characterized in that the content of the nonionic surfactant (B) in the nonvolatile matter of the treatment agent is 30 mass % or more and 60 mass % or less , the content of the ester compound (C) is 5 to 40 mass %, and the epoxy compound (A) has at least one compound selected from bisphenol A and bisphenol F as a main skeleton.
エステル化合物(C):1価脂肪族アルコールと1価カルボン酸とからなるエステル化合物。
態様3は、態様1に記載の炭素繊維含有不織布製造用の処理剤において、前記エポキシ化合物(A)が、ビスフェノールA骨格、及びビスフェノールF骨格から選ばれる少なくとも1つを有する。
Ester compound (C): An ester compound consisting of a monohydric aliphatic alcohol and a monobasic carboxylic acid.
In a third aspect, in the treating agent for producing a carbon fiber-containing nonwoven fabric according to the first aspect, the epoxy compound (A) has at least one selected from a bisphenol A skeleton and a bisphenol F skeleton .
態様4は、態様2に記載の炭素繊維含有不織布製造用の処理剤において、前記処理剤の不揮発分における前記エポキシ化合物(A)の含有割合が5~60質量%である。
態様5は、態様1又は3に記載の炭素繊維含有不織布製造用の処理剤において、前記処理剤の不揮発分における前記ノニオン界面活性剤(B)の含有割合が5~60質量%である。
In a fourth aspect, in the treating agent for producing a carbon fiber-containing nonwoven fabric according to the second aspect, the content of the epoxy compound (A) in the non-volatile matter of the treating agent is 5 to 60 mass %.
Aspect 5 is the treating agent for producing a carbon fiber-containing nonwoven fabric according to Aspect 1 or 3, in which the content of the nonionic surfactant (B) in the nonvolatile matter of the treating agent is 5 to 60 mass %.
態様6は、態様1,3,及び5のいずれか一態様に記載の炭素繊維含有不織布製造用の処理剤において、前記エポキシ化合物(A)、前記ノニオン界面活性剤(B)、及び前記エステル化合物(C)の含有割合の合計を100質量%とすると、前記エポキシ化合物(A)を5~90質量%、前記ノニオン界面活性剤(B)を5~60質量%、及び前記エステル化合物(C)を5~50質量%の割合で含有する。 Aspect 6 is the treatment agent for producing a carbon fiber-containing nonwoven fabric according to any one of Aspects 1, 3, and 5 , wherein the treatment agent contains the epoxy compound (A) in an amount of 5 to 90 mass%, the nonionic surfactant (B) in an amount of 5 to 60 mass%, and the ester compound (C) in an amount of 5 to 50 mass%, assuming that the total content of the epoxy compound (A), the nonionic surfactant (B), and the ester compound (C) is 100 mass% .
態様7は、態様2又は4に記載の炭素繊維含有不織布製造用の処理剤において、前記エポキシ化合物(A)、前記ノニオン界面活性剤(B)、及び前記エステル化合物(C)の含有割合の合計を100質量%とすると、前記エポキシ化合物(A)を5~60質量%、前記ノニオン界面活性剤(B)を30~60質量%、及び前記エステル化合物(C)を5~50質量%の割合で含有する。 Aspect 7 is the treatment agent for producing a carbon fiber-containing nonwoven fabric according to Aspect 2 or 4 , wherein the treatment agent contains the epoxy compound (A) in an amount of 5 to 60 mass%, the nonionic surfactant (B) in an amount of 30 to 60 mass%, and the ester compound (C) in an amount of 5 to 50 mass%, assuming that the total content of the epoxy compound (A), the nonionic surfactant (B), and the ester compound (C) is 100 mass% .
態様8の炭素繊維含有不織布は、態様1~7のいずれか一態様に記載の処理剤が付着していることを特徴とする。
態様9の炭素繊維含有不織布の製造方法は、態様1~7のいずれか一態様に記載の処理剤を、炭素繊維の短繊維に付着させる工程を含むことを特徴とする。
The carbon fiber-containing nonwoven fabric of Aspect 8 is characterized in that the treating agent according to any one of Aspects 1 to 7 is adhered thereto.
A method for producing a carbon fiber-containing nonwoven fabric according to Aspect 9 is characterized by comprising a step of adhering the treating agent according to any one of Aspects 1 to 7 to short carbon fibers.
本発明によれば、炭素繊維含有不織布製造用の処理剤が付与された炭素繊維の折れを低減できる。 According to the present invention, it is possible to reduce breakage of carbon fibers to which a treatment agent for producing carbon fiber-containing nonwoven fabric has been applied.
<第1実施形態>
以下、本発明の炭素繊維含有不織布製造用の処理剤(以下、処理剤という)を具体化した第1実施形態を説明する。本実施形態の処理剤は、下記のエポキシ化合物(A)及びノニオン界面活性剤(B)を含有し、さらにエステル化合物(C)を含有する。
First Embodiment
Hereinafter, a first embodiment of the treating agent for producing a carbon fiber-containing nonwoven fabric of the present invention (hereinafter, referred to as the treating agent) will be described. The treating agent of this embodiment contains the following epoxy compound (A) and nonionic surfactant (B), and further contains an ester compound (C).
(エポキシ化合物(A))
エポキシ化合物(A)は、分子中にエポキシ基を有する化合物である。エポキシ化合物(A)は、分子中にエポキシ基を1つ有するモノエポキシ化合物、又は2以上有する多官能エポキシ化合物のいずれであってもよい。
(Epoxy compound (A))
The epoxy compound (A) is a compound having an epoxy group in the molecule. The epoxy compound (A) may be either a monoepoxy compound having one epoxy group in the molecule or a multifunctional epoxy compound having two or more epoxy groups in the molecule.
また、主鎖としては、例えばジフェニルメタンが挙げられ、より具体的にはビスフェノールが挙げられる。ビスフェノールの具体例としては、例えばビスフェノールA,AP,AF,B,BP,C,E,F,G,M,S,P,PH,TMC,Z等が挙げられる。これら中で、炭素繊維の折れをより低減できる観点から、エポキシ化合物(A)は、ビスフェノールA骨格、及びビスフェノールF骨格を有するものが好ましい。 The main chain may be, for example, diphenylmethane, more specifically, bisphenol. Specific examples of bisphenol include bisphenol A, AP, AF, B, BP, C, E, F, G, M, S, P, PH, TMC, and Z. Among these, from the viewpoint of further reducing the breakage of carbon fibers, it is preferable that the epoxy compound (A) has a bisphenol A skeleton and a bisphenol F skeleton.
本発明においては、エポキシ化合物(A)は、主骨格としてジフェニルメタン骨格を含む化合物が用いられる。主骨格としてジフェニルメタン骨格を含む化合物としては、例えばビスフェノールA骨格、ビスフェノールF骨格、ジアミノジフェニルメタン骨格、及クレゾールノボラック骨格から選ばれる少なくとも1つを含む化合物等が挙げられる。以下、本発明のエポキシ化合物(A)以外の化合物は、参考例とする。 In the present invention, the epoxy compound (A) is a compound containing a diphenylmethane skeleton as the main skeleton. Examples of compounds containing a diphenylmethane skeleton as the main skeleton include compounds containing at least one skeleton selected from a bisphenol A skeleton, a bisphenol F skeleton, a diaminodiphenylmethane skeleton, and a cresol novolac skeleton. Hereinafter, compounds other than the epoxy compound (A) of the present invention are provided as reference examples.
エポキシ化合物(A)の具体例としては、例えばポリオキシアルキレン付加p-tert-ブチルフェノールモノグリシジルエーテル、ビスフェノールAジグリシジルエーテル、レゾルシノールジグリシジルエーテル、ポリプロピレングリコールジグリシジルエーテル、トリメチロールプロパンポリグリシジルエーテル、ペンタエリスリトールポリグリシジルエーテル、ネオペンチルグリコールジグリシジルエーテル、1,6-ヘキサンジオールジグリシジルエーテル、ポリエチレングリコールジグリシジルエーテル、ポリグリセロールポリグリシジルエーテル、アルキルグリシジルエーテル、ポリオキシアルキレン付加アルキルグリシジルエーテル、フェニルグリシジルエーテル、ポリオキシアルキレン付加フェニルグリシジルエーテル、トリグリシジルアミン、テトラグリシジルアミン等の重合体等のアミン型エポキシ化合物等が挙げられる。 Specific examples of epoxy compounds (A) include amine-type epoxy compounds such as polyoxyalkylene-added p-tert-butylphenol monoglycidyl ether, bisphenol A diglycidyl ether, resorcinol diglycidyl ether, polypropylene glycol diglycidyl ether, trimethylolpropane polyglycidyl ether, pentaerythritol polyglycidyl ether, neopentyl glycol diglycidyl ether, 1,6-hexanediol diglycidyl ether, polyethylene glycol diglycidyl ether, polyglycerol polyglycidyl ether, alkyl glycidyl ether, polyoxyalkylene-added alkyl glycidyl ether, phenyl glycidyl ether, polyoxyalkylene-added phenyl glycidyl ether, triglycidylamine, tetraglycidylamine, and other polymers.
また、エポキシ化合物(A)として、市販品を使用してもよい。市販品の具体例としては、例えばjER828(三菱ケミカル株式会社製), jER834(三菱ケミカル株式会社製), jER1001(三菱ケミカル株式会社製), jER1002(三菱ケミカル株式会社製), エポトートYD-128(日鉄ケミカル&マテリアル製), エポトートYD-011(日鉄ケミカル&マテリアル製), エポトートYD-012(日鉄ケミカル&マテリアル製), スミエポキシELM-434(住友化学株式会社製), EPICRON N-660(DIC株式会社製)等が挙げられる。 In addition, commercially available products may be used as the epoxy compound (A). Specific examples of commercially available products include jER828 (manufactured by Mitsubishi Chemical Corporation), jER834 (manufactured by Mitsubishi Chemical Corporation), jER1001 (manufactured by Mitsubishi Chemical Corporation), jER1002 (manufactured by Mitsubishi Chemical Corporation), Epotohto YD-128 (manufactured by Nippon Steel Chemical & Material Co., Ltd.), Epotohto YD-011 (manufactured by Nippon Steel Chemical & Material Co., Ltd.), Epotohto YD-012 (manufactured by Nippon Steel Chemical & Material Co., Ltd.), Sumiepoxy ELM-434 (manufactured by Sumitomo Chemical Co., Ltd.), EPICRON N-660 (manufactured by DIC Corporation), and the like.
これらのエポキシ化合物(A)は、一種類を単独で使用してもよいし、又は二種以上を適宜組み合わせて使用してもよい。
処理剤の不揮発分中におけるエポキシ化合物(A)の含有割合は、例えば3~100質量%、5~90質量%である。かかる範囲に規定することにより本発明の効果をより向上できる。なお、上記の上限及び下限を任意に組み合わせた範囲も想定される。また、不揮発分とは、処理剤を105℃で2時間熱処理して揮発性成分を十分に除去したものをいう。以下、不揮発分の定義は、同じ条件を採用するものとする。
These epoxy compounds (A) may be used alone or in appropriate combination of two or more.
The content of the epoxy compound (A) in the non-volatile content of the treatment agent is, for example, 3 to 100% by mass , or 5 to 90% by mass. By specifying the content within such ranges, the effects of the present invention can be further improved. Any range combining the above upper and lower limits is also envisioned. The non-volatile content refers to the treatment agent that has been heat-treated at 105°C for 2 hours to thoroughly remove volatile components. Hereinafter, the definition of non-volatile content will adopt the same conditions.
(ノニオン界面活性剤(B))
処理剤は、さらにノニオン界面活性剤(B)を含有してもよい。処理剤中にノニオン界面活性剤(B)が含まれることにより、処理剤が付与された炭素繊維から得られた不織布の強さが向上する。
(Nonionic Surfactant (B))
The treatment agent may further contain a nonionic surfactant (B). By including the nonionic surfactant (B) in the treatment agent, the strength of the nonwoven fabric obtained from the carbon fibers to which the treatment agent has been applied is improved.
ノニオン界面活性剤(B)としては、例えばアルコール類又はカルボン酸類にアルキレンオキサイドを付加させた(ポリ)オキシアルキレン構造を有する化合物、カルボン酸類と多価アルコールとのエステル化合物にアルキレンオキサイドを付加させた(ポリ)オキシアルキレン構造を有するエーテル・エステル化合物、天然油脂にアルキレンオキサイドを付加させた化合物又はその化合物とカルボン酸類とをエステル化させた化合物、アミン化合物として例えば一級有機アミンにアルキレンオキサイドを付加させた(ポリ)オキシアルキレン構造を有する化合物、脂肪酸アミド類にアルキレンオキサイドを付加させた(ポリ)オキシアルキレン構造を有する化合物、アミン化合物とカルボン酸類とを縮合されたアミド化合物、カルボン酸類と多価アルコール等との部分エステル化合物等が挙げられる。 Examples of nonionic surfactants (B) include compounds having a (poly)oxyalkylene structure in which alkylene oxides are added to alcohols or carboxylic acids, ether/ester compounds having a (poly)oxyalkylene structure in which alkylene oxides are added to ester compounds of carboxylic acids and polyhydric alcohols, compounds in which alkylene oxides are added to natural fats and oils or compounds in which such compounds are esterified with carboxylic acids, amine compounds such as compounds having a (poly)oxyalkylene structure in which alkylene oxides are added to primary organic amines, compounds having a (poly)oxyalkylene structure in which alkylene oxides are added to fatty acid amides, amide compounds in which amine compounds and carboxylic acids are condensed, partial ester compounds of carboxylic acids and polyhydric alcohols, etc.
ノニオン界面活性剤(B)の原料として用いられるアルコール類の具体例としては、例えば、(1)メタノール、エタノール、プロパノール、ブタノール、ペンタノール、ヘキサノール、オクタノール、ノナノール、デカノール、ウンデカノール、ドデカノール、トリデカノール、テトラデカノール、ペンタデカノール、ヘキサデカノール、ヘプタデカノール、オクタデカノール、ノナデカノール、エイコサノール、ヘンエイコサノール、ドコサノール、トリコサノール、テトラコサノール、ペンタコサノール、ヘキサコサノール、ヘプタコサノール、オクタコサノール、ノナコサノール、トリアコンタノール等の直鎖アルキルアルコール、(2)イソプロパノール、イソブタノール、イソヘキサノール、2-エチルヘキサノール、イソノナノール、イソデカノール、イソドデカノール、イソトリデカノール、イソテトラデカノール、イソトリアコンタノール、イソヘキサデカノール、イソヘプタデカノール、イソオクタデカノール、イソノナデカノール、イソエイコサノール、イソヘンエイコサノール、イソドコサノール、イソトリコサノール、イソテトラコサノール、イソペンタコサノール、イソヘキサコサノール、イソヘプタコサノール、イソオクタコサノール、イソノナコサノール、イソペンタデカノール等の分岐アルキルアルコール、(3)テトラデセノール、ヘキサデセノール、ヘプタデセノール、オクタデセノール、ノナデセノール等の直鎖アルケニルアルコール、(4)イソヘキサデセノール、イソオクタデセノール等の分岐アルケニルアルコール、(5)シクロペンタノール、シクロヘキサノール等の環状アルキルアルコール、(6)フェノール、ノニルフェノール、ベンジルアルコール、モノスチレン化フェノール、ジスチレン化フェノール、トリスチレン化フェノール等の芳香族系アルコール等が挙げられる。 Specific examples of alcohols used as raw materials for the nonionic surfactant (B) include, for example, (1) linear alkyl alcohols such as methanol, ethanol, propanol, butanol, pentanol, hexanol, octanol, nonanol, decanol, undecanol, dodecanol, tridecanol, tetradecanol, pentadecanol, hexadecanol, heptadecanol, octadecanol, nonadecanol, eicosanol, heneicosanol, docosanol, tricosanol, tetracosanol, pentacosanol, hexacosanol, heptacosanol, octacosanol, nonacosanol, and triacontanol; (2) isopropanol, isobutanol, isohexanol, 2-ethylhexanol, isononanol, isodecanol, isododecanol, isotridecanol, isotetradecanol, isotriacontanol, and isoheptadecanol; (3) branched alkyl alcohols such as tetradecenol, hexadecanol, heptadecanol, octadecanol, isononadecanol, isoeicosanol, isoheneicosanol, isodocosanol, isotricosanol, isotetracosanol, isopentacosanol, isohexacosanol, isoheptacosanol, isooctacosanol, isononacosanol, and isopentadecanol; (4) branched alkenyl alcohols such as isohexadecenol and isooctadecenol; (5) cyclic alkyl alcohols such as cyclopentanol and cyclohexanol; and (6) aromatic alcohols such as phenol, nonylphenol, benzyl alcohol, monostyrenated phenol, distyrenated phenol, and tristyrenated phenol.
ノニオン界面活性剤(B)の原料として用いられるカルボン酸類の具体例としては、例えば、(1)オクチル酸、ノナン酸、デカン酸、ウンデカン酸、ドデカン酸、トリデカン酸、テトラデカン酸、ペンタデカン酸、ヘキサデカン酸、ヘプタデカン酸、オクタデカン酸、ノナデカン酸、エイコサン酸、ヘンエイコサン酸、ドコサン酸等の直鎖アルキルカルボン酸、(2)2-エチルヘキサン酸、イソドデカン酸、イソトリデカン酸、イソテトラデカン酸、イソヘキサデカン酸、イソオクタデカン酸等の分岐アルキルカルボン酸、(3)オクタデセン酸、オクタデカジエン酸、オクタデカトリエン酸等の直鎖アルケニルカルボン酸、(4)安息香酸等の芳香族系カルボン酸、(5)リシノール酸等のヒドロキシカルボン酸等が挙げられる。 Specific examples of carboxylic acids used as raw materials for the nonionic surfactant (B) include (1) linear alkyl carboxylic acids such as octylic acid, nonanoic acid, decanoic acid, undecanoic acid, dodecanoic acid, tridecanoic acid, tetradecanoic acid, pentadecanoic acid, hexadecanoic acid, heptadecanoic acid, octadecanoic acid, nonadecanoic acid, eicosanoic acid, heneicosanoic acid, and docosanoic acid, (2) branched alkyl carboxylic acids such as 2-ethylhexanoic acid, isododecanoic acid, isotridecanoic acid, isotetradecanoic acid, isohexadecanoic acid, and isooctadecanoic acid, (3) linear alkenyl carboxylic acids such as octadecenoic acid, octadecadienoic acid, and octadecatrienoic acid, (4) aromatic carboxylic acids such as benzoic acid, and (5) hydroxycarboxylic acids such as ricinoleic acid.
ノニオン界面活性剤(B)の(ポリ)オキシアルキレン構造を形成する原料として用いられるアルキレンオキサイドとしては、炭素数2以上4以下のアルキレンオキサイドが好ましい。アルキレンオキサイドの具体例としては、例えばエチレンオキサイド、プロピレンオキサイド、ブチレンオキサイド等が挙げられる。アルキレンオキサイドの付加モル数は、適宜設定されるが、好ましくは0.1モル以上150モル以下、より好ましくは1モル以上100モル以下、さらに好ましくは2モル以上50モル以下である。上記の上限及び下限を任意に組み合わせた範囲も想定される。なお、アルキレンオキサイドの付加モル数は、仕込み原料中における付加対象化合物1モルに対するアルキレンオキサイドのモル数を示す。アルキレンオキサイドは、一種類のアルキレンオキサイドを単独で使用してもよいし、又は二種以上のアルキレンオキサイドを適宜組み合わせて使用してもよい。アルキレンオキサイドが二種類以上適用される場合、それらの付加形態は、ブロック付加、ランダム付加、及びブロック付加とランダム付加の組み合わせのいずれでもよく、特に制限はない。 As the alkylene oxide used as a raw material for forming the (poly)oxyalkylene structure of the nonionic surfactant (B), an alkylene oxide having 2 to 4 carbon atoms is preferred. Specific examples of alkylene oxide include, for example, ethylene oxide, propylene oxide, and butylene oxide. The number of moles of alkylene oxide added is set appropriately, but is preferably 0.1 to 150 moles, more preferably 1 to 100 moles, and even more preferably 2 to 50 moles. Any combination of the above upper and lower limits is also possible. The number of moles of alkylene oxide added indicates the number of moles of alkylene oxide per mole of the compound to be added in the raw material. As the alkylene oxide, one type of alkylene oxide may be used alone, or two or more types of alkylene oxides may be used in appropriate combination. When two or more types of alkylene oxide are used, the addition form may be any of block addition, random addition, and a combination of block addition and random addition, and is not particularly limited.
ノニオン界面活性剤(B)の原料として用いられる多価アルコールの具体例としては、例えばエチレングリコール、プロピレングリコール、1,3-プロパンジオール、1,2-ブタンジオール、1,3-ブタンジオール、1,4-ブタンジオール、2-メチル-1,2-プロパンジオール、1,5-ペンタンジオール、1,6-ヘキサンジオール、2,5-ヘキサンジオール、2-メチル-2,4-ペンタンジオール、2,3-ジメチル-2,3-ブタンジオール、グリセリン、ジグリセリン、2-メチル-2-ヒドロキシメチル-1,3-プロパンジオール、トリメチロールプロパン、ソルビタン、ペンタエリスリトール、ソルビトール等が挙げられる。 Specific examples of polyhydric alcohols used as raw materials for the nonionic surfactant (B) include ethylene glycol, propylene glycol, 1,3-propanediol, 1,2-butanediol, 1,3-butanediol, 1,4-butanediol, 2-methyl-1,2-propanediol, 1,5-pentanediol, 1,6-hexanediol, 2,5-hexanediol, 2-methyl-2,4-pentanediol, 2,3-dimethyl-2,3-butanediol, glycerin, diglycerin, 2-methyl-2-hydroxymethyl-1,3-propanediol, trimethylolpropane, sorbitan, pentaerythritol, and sorbitol.
ノニオン界面活性剤(B)の原料として用いられる脂肪族アミン又は一級有機アミンの具体例として、例えばメチルアミン、エチルアミン、ブチルアミン、オクチルアミン、ラウリルアミン、オクタデシルアミン(ステアリルアミン)、オクタデセニルアミン、ヤシアミン等が挙げられる。 Specific examples of aliphatic amines or primary organic amines used as raw materials for the nonionic surfactant (B) include methylamine, ethylamine, butylamine, octylamine, laurylamine, octadecylamine (stearylamine), octadecenylamine, and coconut amine.
ノニオン界面活性剤(B)の原料として用いられる脂肪酸アミドの具体例としては、例えばオクチル酸アミド、ラウリン酸アミド、パルミチン酸アミド、ステアリン酸アミド、オレイン酸アミド、ベヘン酸アミド、リグノセリン酸アミド、脂肪酸とジエタノールアミンとのアミド、脂肪酸とエチレンアミンとのアミド等が挙げられる。 Specific examples of fatty acid amides used as raw materials for the nonionic surfactant (B) include octyl acid amide, lauric acid amide, palmitic acid amide, stearic acid amide, oleic acid amide, behenic acid amide, lignoceric acid amide, amides of fatty acids and diethanolamine, and amides of fatty acids and ethyleneamine.
これらのノニオン界面活性剤(B)は、一種類を単独で使用してもよいし、又は二種以上を適宜組み合わせて使用してもよい。
処理剤の不揮発分中において、ノニオン界面活性剤(B)の含有割合は、例えば3~70質量%、5~60質量%である。かかる含有割合の範囲に規定することにより、処理剤が付与された炭素繊維から得られた不織布の強さが向上する。なお、上記の上限及び下限を任意に組み合わせた範囲も想定される。
These nonionic surfactants (B) may be used alone or in appropriate combination of two or more kinds.
The content of the nonionic surfactant (B) in the nonvolatile matter of the treatment agent is, for example , 3 to 70 mass % , or 5 to 60 mass %. By specifying the content within such a range, the strength of the nonwoven fabric obtained from the carbon fiber to which the treatment agent is applied is improved. Note that any combination of the above upper and lower limits is also envisioned.
(エステル化合物(C))
本実施形態の処理剤に供するエステル化合物(C)は、1価脂肪族アルコールと1価カルボン酸とからなるエステル化合物が適用される。このエステル化合物(C)を適用することにより、処理剤が付与された炭素繊維から得られた不織布の強さが向上する。
(Ester Compound (C))
The ester compound (C) used in the treatment agent of this embodiment is an ester compound composed of a monohydric aliphatic alcohol and a monovalent carboxylic acid. By using this ester compound (C), the strength of the nonwoven fabric obtained from the carbon fiber to which the treatment agent is applied is improved.
エステル化合物(C)を構成する1価カルボン酸としては、飽和脂肪族カルボン酸であっても、不飽和脂肪族カルボン酸であってもよい。また、直鎖状のものであっても、分岐鎖構造を有するものであってもよい。 The monovalent carboxylic acid constituting the ester compound (C) may be a saturated aliphatic carboxylic acid or an unsaturated aliphatic carboxylic acid. In addition, it may be a straight-chain or branched-chain structure.
飽和脂肪族カルボン酸の具体例としては、例えばギ酸、酢酸、プロピオン酸、酪酸、吉草酸、ヘキサン酸(カプロン酸)、オクチル酸(2-エチルヘキサン酸)、オクタン酸(カプリル酸)、ノナン酸、デカン酸(カプリン酸)、ドデカン酸(ラウリン酸)、テトラデカン酸(ミリスチン酸)、ヘキサデカン酸(パルミチン酸)、オクタデカン酸(ステアリン酸)、イソオクタデカン酸(イソステアリン酸)、エイコサン酸(アラキジン酸)、ドコサン酸(ベヘン酸)、テトラコサン酸等が挙げられる。 Specific examples of saturated aliphatic carboxylic acids include formic acid, acetic acid, propionic acid, butyric acid, valeric acid, hexanoic acid (caproic acid), octylic acid (2-ethylhexanoic acid), octanoic acid (caprylic acid), nonanoic acid, decanoic acid (capric acid), dodecanoic acid (lauric acid), tetradecanoic acid (myristic acid), hexadecanoic acid (palmitic acid), octadecanoic acid (stearic acid), isooctadecanoic acid (isostearic acid), eicosanoic acid (arachidic acid), docosanoic acid (behenic acid), and tetracosanoic acid.
不飽和脂肪族カルボン酸の具体例としては、例えばクロトン酸、ミリストレイン酸、パルミトレイン酸、オレイン酸、バクセン酸、エイコセン酸、リノール酸、αリノレン酸、γリノレン酸、アラキドン酸等が挙げられる。 Specific examples of unsaturated aliphatic carboxylic acids include crotonic acid, myristoleic acid, palmitoleic acid, oleic acid, vaccenic acid, eicosenoic acid, linoleic acid, alpha-linolenic acid, gamma-linolenic acid, and arachidonic acid.
1価脂肪族アルコールの具体例としては、上述したノニオン界面活性剤(B)の原料として用いられるアルコール類のうち1価脂肪族アルコールの具体例が挙げられる。
これらのエステル化合物(C)は、1種を単独で使用してもよく、2種以上を組み合わせて使用してもよい。
Specific examples of the monohydric aliphatic alcohol include the specific examples of the monohydric aliphatic alcohols among the alcohols used as raw materials for the nonionic surfactant (B) described above.
These ester compounds (C) may be used alone or in combination of two or more.
処理剤の不揮発分中において、エステル化合物(C)の含有割合は、例えば3~60質量%、5~50質量%である。かかる含有割合の範囲に規定することにより、処理剤が付与された炭素繊維から得られた不織布の強さが向上する。なお、上記の上限及び下限を任意に組み合わせた範囲も想定される。 The content of the ester compound (C) in the non-volatile matter of the treatment agent is, for example , 3 to 60 mass % , or 5 to 50 mass %. By specifying the content within such a range, the strength of the nonwoven fabric obtained from the carbon fiber to which the treatment agent is applied is improved. Note that ranges that combine the above upper and lower limits in any way are also envisioned.
処理剤中において、エポキシ化合物(A)、ノニオン界面活性剤(B)、及びエステル化合物(C)の含有割合の合計を100質量%とすると、エポキシ化合物(A)を5~90質量%、ノニオン界面活性剤(B)を5~60質量%、及びエステル化合物(C)を5~50質量%の割合で含有することが好ましい。かかる含有割合の範囲に規定することにより、本発明の効果をより向上できる。なお、上記の上限及び下限を任意に組み合わせた範囲も想定される。 In the treatment agent, if the total content of the epoxy compound (A), the nonionic surfactant (B), and the ester compound (C) is taken as 100% by mass, it is preferable that the epoxy compound (A) is contained in an amount of 5 to 90% by mass, the nonionic surfactant (B) is contained in an amount of 5 to 60% by mass, and the ester compound (C) is contained in an amount of 5 to 50% by mass. By specifying the content ratios in such a range, the effect of the present invention can be further improved. Note that ranges that combine the above upper and lower limits in any desired manner are also contemplated.
<第2実施形態>
次に、本発明に係る炭素繊維含有不織布(以下、単に不織布という)を具体化した第2実施形態について説明する。本実施形態の不織布は、不織布に第1実施形態の処理剤が付着している。本実施形態の不織布は、まず第1実施形態の処理剤を炭素繊維に付着させる工程が行われ、次にカーディングによるウェブ形成工程を行うことにより製造される。不織布に対する処理剤の付着量については特に制限はないが、不織布に処理剤(溶媒を含まない)が好ましくは0.01~10質量%、より好ましくは0.1~2質量%となるよう付着している。
Second Embodiment
Next, a second embodiment of the carbon fiber-containing nonwoven fabric (hereinafter simply referred to as nonwoven fabric) according to the present invention will be described. In the nonwoven fabric of this embodiment, the treatment agent of the first embodiment is adhered to the nonwoven fabric. The nonwoven fabric of this embodiment is manufactured by first carrying out a step of adhering the treatment agent of the first embodiment to carbon fibers, and then carrying out a web formation step by carding. There is no particular restriction on the amount of treatment agent adhered to the nonwoven fabric, but the treatment agent (not including the solvent) is preferably adhered to the nonwoven fabric in an amount of 0.01 to 10 mass %, more preferably 0.1 to 2 mass %.
不織布を構成する炭素繊維の種類としては、特に制限はないが、例えば、アクリル繊維を原料として得られたPAN系繊維、ピッチを原料として得られたピッチ系繊維の他、化学分解・熱分解法等によって、炭素繊維複合材料から取り出されたリサイクル炭素繊維、ポリエステル繊維、ポリエチレン樹脂、フェノール樹脂、セルロース樹脂、リグニン樹脂等を原料として得られる炭素繊維等が挙げられる。例えばアクリル繊維が用いられる場合、アクリル繊維としては、少なくとも90モル%以上のアクリロニトリルと、10モル%以下の耐炎化促進成分とを共重合させて得られるポリアクリロニトリルを主成分とする繊維から構成されることが好ましい。耐炎化促進成分としては、例えばアクリロニトリルに対して共重合性を有するビニル基含有化合物が好適に使用できる。原料繊維の単繊維繊度については、特に限定はないが、性能及び製造コストのバランスの観点から、好ましくは0.1~2.0dTexである。また、原料繊維の繊維束を構成する単繊維の本数についても特に限定はないが、性能及び製造コストのバランスの観点から、好ましくは1,000~96,000本である。 The type of carbon fiber constituting the nonwoven fabric is not particularly limited, but examples include PAN-based fibers obtained from acrylic fibers, pitch-based fibers obtained from pitch, recycled carbon fibers extracted from carbon fiber composite materials by chemical decomposition or thermal decomposition, polyester fibers, carbon fibers obtained from polyethylene resins, phenolic resins, cellulose resins, lignin resins, etc. For example, when acrylic fibers are used, the acrylic fibers are preferably composed of fibers mainly composed of polyacrylonitrile obtained by copolymerizing at least 90 mol% or more of acrylonitrile and 10 mol% or less of a flame retardant promoting component. As the flame retardant promoting component, for example, a vinyl group-containing compound that is copolymerizable with acrylonitrile can be suitably used. There is no particular limit to the single fiber fineness of the raw fiber, but from the viewpoint of the balance between performance and production cost, it is preferably 0.1 to 2.0 dTex. In addition, there is no particular limit to the number of single fibers constituting the fiber bundle of the raw fiber, but from the viewpoint of the balance between performance and production cost, it is preferably 1,000 to 96,000.
本実施形態の炭素繊維の製造方法は、まず上述した原料繊維を得た後、製糸する製糸工程が行われる。次に、その製糸工程で製造された繊維束を200~300℃、好ましくは230~270℃の酸化性雰囲気中で耐炎化繊維に転換する耐炎化処理工程が行われる。さらに炭素繊維を得る場合、前記耐炎化繊維をさらに300~2000℃、好ましくは300~1300℃の不活性雰囲気中で炭化させる炭素化処理工程が行われる。炭素化処理工程は、耐炎化処理工程に続けて行ってもよい。 In the method for producing carbon fiber of this embodiment, first, the raw fiber described above is obtained, and then a spinning process is carried out to spin the raw fiber. Next, a flame-retardant treatment process is carried out to convert the fiber bundle produced in the spinning process into a flame-retardant fiber in an oxidizing atmosphere at 200 to 300°C, preferably 230 to 270°C. When further obtaining carbon fiber, a carbonization process is carried out to carbonize the flame-retardant fiber in an inert atmosphere at 300 to 2000°C, preferably 300 to 1300°C. The carbonization process may be carried out subsequent to the flame-retardant treatment process.
本実施形態の不織布の製造方法は、上述したようにまず第1実施形態の処理剤を炭素繊維に付着させる工程が行われる。炭素繊維に処理剤を付着させる方法は、公知の方法を適宜採用できる。例えば、浸漬給油法、ローラー浸漬法、ローラー接触法、スプレー法、抄紙法、計量ポンプを用いたガイド給油法等、一般に工業的に用いられている方法を適用できる。 As described above, the method for producing the nonwoven fabric of this embodiment first involves a step of adhering the treatment agent of the first embodiment to the carbon fibers. The method for adhering the treatment agent to the carbon fibers can be any known method. For example, methods that are generally used industrially, such as the immersion oiling method, roller immersion method, roller contact method, spray method, papermaking method, and guide oiling method using a metering pump, can be used.
第1実施形態の処理剤を繊維に付着させる際の形態としては、例えば有機溶媒溶液、水性液等が挙げられる。処理剤は、好ましくは水性のエマルション液の状態で炭素繊維に付着される。処理剤が適用される繊維の長さは、特に限定されず、一般にステープルと呼ばれる短繊維、一般にフィラメントと呼ばれる長繊維のものが挙げられる。また、2種類以上の異なったステープルを混ぜ合わせて混紡した炭素繊維を使用してもよい。混紡する合成繊維としては、例えば6ナイロン、66ナイロン、ポリアミド9T、ポリアミド10等のポリアミド繊維、ポリプロピレン、ポリエチレン等が挙げられる。混紡する際の合成繊維と炭素繊維の比率としては、特に限定されないが、好ましくは10:90~90:10、より好ましくは20:80~80:20である。混紡する場合において、処理剤は、炭素繊維と合成繊維を混紡させる前後どちらで付着させてもよい。 The form in which the treatment agent of the first embodiment is applied to the fiber includes, for example, an organic solvent solution, an aqueous liquid, and the like. The treatment agent is preferably applied to the carbon fiber in the form of an aqueous emulsion liquid. The length of the fiber to which the treatment agent is applied is not particularly limited, and examples thereof include short fibers generally called staples and long fibers generally called filaments. In addition, carbon fiber in which two or more different types of staples are mixed and spun may be used. Examples of synthetic fibers to be spun include polyamide fibers such as nylon 6, nylon 66, polyamide 9T, and polyamide 10, polypropylene, and polyethylene. The ratio of synthetic fibers to carbon fibers when spun is not particularly limited, but is preferably 10:90 to 90:10, and more preferably 20:80 to 80:20. In the case of spun, the treatment agent may be applied either before or after the carbon fiber and synthetic fiber are spun.
続いて、乾燥処理し、処理剤の溶液に含まれている水等の溶媒の除去を行うことにより、処理剤が付着した炭素繊維を得ることができる。ここでの乾燥処理は、例えば、熱風、熱板、ローラー、各種赤外線ヒーター等を熱媒として利用した方法を採用できる。 Then, the carbon fiber with the treatment agent attached can be obtained by drying the carbon fiber and removing the solvent, such as water, contained in the solution of the treatment agent. For the drying process, for example, a method using hot air, a hot plate, a roller, or various infrared heaters as a heat medium can be used.
次に、ウェブ形成工程が行われる。ウェブ形成工程は、上記処理剤が付着した炭素繊維にカーディングを行い、不織布からなるウェブを製造する工程である。カーディングは、公知のカード機を用いて行うことができる。例えばフラットカード、コンビネーションカード、ローラーカード等が挙げられる。 Next, a web forming process is carried out. In the web forming process, the carbon fibers to which the treatment agent is applied are carded to produce a web made of nonwoven fabric. Carding can be carried out using a known carding machine. Examples include flat cards, combination cards, and roller cards.
本実施形態の処理剤及び不織布の効果について説明する。
(1)本実施形態の処理剤では、エポキシ化合物(A)を配合して構成した。したがって、カード機を通過する際、処理剤が付与された炭素繊維の折れを低減することができる。また、処理剤が付与された炭素繊維から得られた不織布の強さを向上できる。
The effects of the treatment agent and nonwoven fabric of this embodiment will be described.
(1) The treatment agent of this embodiment is constituted by blending an epoxy compound (A). Therefore, when passing through a carding machine, it is possible to reduce breakage of the carbon fiber to which the treatment agent is applied. In addition, it is possible to improve the strength of the nonwoven fabric obtained from the carbon fiber to which the treatment agent is applied.
(2)処理剤が、所定量のノニオン界面活性剤(B)又はエステル化合物(C)を含有する場合、処理剤が付与された炭素繊維から得られた不織布の強さをより向上できる。
なお、上記実施形態は以下のように変更してもよい。上記実施形態及び以下の変更例は、技術的に矛盾しない範囲で互いに組み合わせて実施できる。
(2) When the treating agent contains a predetermined amount of the nonionic surfactant (B) or the ester compound (C), the strength of the nonwoven fabric obtained from the carbon fibers to which the treating agent has been applied can be further improved.
The above embodiment may be modified as follows: The above embodiment and the following modifications may be combined with each other to the extent that no technical contradiction occurs.
・上記実施形態の処理剤には、本発明の効果を阻害しない範囲内において、処理剤の品質保持のための安定化剤、制電剤、つなぎ剤、酸化防止剤、紫外線吸収剤等の通常処理剤に用いられる成分をさらに配合してもよい。 - The treatment agent of the above embodiment may further contain components that are typically used in treatment agents, such as stabilizers for maintaining the quality of the treatment agent, antistatic agents, binders, antioxidants, and ultraviolet absorbers, within the scope that does not impair the effects of the present invention.
以下、本発明の構成及び効果をより具体的にするため、実施例等を挙げるが、本発明がこれらの実施例に限定されるというものではない。尚、以下の実施例及び比較例において、部は質量部を、また%は質量%を意味する。 The following examples are provided to more specifically illustrate the configuration and effects of the present invention, but the present invention is not limited to these examples. In the following examples and comparative examples, parts means parts by mass, and % means % by mass.
試験区分1(処理剤の調製)
表1に示すように、エポキシ化合物(A)、ノニオン界面活性剤(B)、エステル化合物(C)、その他成分(D)を、固形分濃度が30%となるように撹拌しながら水又は有機溶媒を徐々に加えることにより各例の処理剤を調製した。
Test section 1 (preparation of treatment agent)
As shown in Table 1, the treatment agent of each example was prepared by gradually adding water or an organic solvent to an epoxy compound (A), a nonionic surfactant (B), an ester compound (C), and other components (D) while stirring so that the solid content concentration became 30%.
試験区分2(炭素繊維不織布の製造)
試験区分1で調製した処理剤を用いて、炭素繊維不織布を製造した。
調製した各処理剤の水性液又は有機溶媒溶液を更に水希釈し、各処理剤の1~4%水性液とした。この水性液を繊維長45mmの炭素短繊維にスプレー給油法で付着させた。その後、105℃の熱風乾燥機に60分間入れて乾燥し、処理剤を付着させた処理済み炭素短繊維を得た。得られた処理済み炭素短繊維を25℃で65%RHの雰囲気に一夜調湿して評価に供した。なお、実施例47等は、表に記載の合成繊維を所定の割合で混紡した。
Test Section 2 (Manufacturing of Carbon Fiber Nonwoven Fabric)
Using the treatment agent prepared in Test Section 1, a carbon fiber nonwoven fabric was produced.
The aqueous or organic solvent solution of each treatment agent thus prepared was further diluted with water to obtain a 1 to 4% aqueous solution of each treatment agent. This aqueous solution was applied to short carbon fibers having a fiber length of 45 mm by a spray oiling method. The fibers were then dried in a hot air dryer at 105°C for 60 minutes to obtain treated short carbon fibers having the treatment agent applied thereto. The treated short carbon fibers thus obtained were conditioned overnight in an atmosphere of 25°C and 65% RH and then subjected to evaluation. In addition, in Example 47 and the like, the synthetic fibers shown in the table were blended in a predetermined ratio.
上記で得られた処理済み炭素短繊維10kgを、2山コンデンサー付きカードに供した。カード工程は、25℃×65%RHの雰囲気下、紡出スピード=18.0m/分、紡出ゲレン=1g/m、揉み回数=30回/インチの条件で運転した。それによりウェブとして炭素繊維不織布を得た。 10 kg of the treated short carbon fibers obtained above were subjected to a carding process with a two-ridge condenser. The carding process was carried out under the following conditions: 25°C x 65% RH, spinning speed = 18.0 m/min, spinning radius = 1 g/m, and number of kneading = 30 times/inch. As a result, a carbon fiber nonwoven fabric was obtained as a web.
試験区分3(炭素繊維の折れ抑制)
カード前後で炭素繊維の長さが何%になったかを測定することにより炭素繊維の折れ具合を評価した。50mmに揃えた短繊維を、カードを通した後に、短繊維の長さをn=50で測定し、平均値を求めた。(カード後の長さ平均/カード前の長さ平均)×100を値とし、下記の基準で評価した。
Test category 3 (carbon fiber breakage prevention)
The degree of folding of the carbon fibers was evaluated by measuring the percentage of the length of the carbon fibers before and after carding. After passing short fibers of 50 mm length through a card, the lengths of the short fibers were measured for n=50 fibers and the average value was calculated. The value was calculated by (average length after carding/average length before carding)×100 and evaluated according to the following criteria.
・炭素繊維の折れ抑制の評価基準
◎(良好):90%以上
○(可):70%以上、90%未満
×(不可):70%未満
試験区分4(製造したウェブの強さ)
得られたウェブを把持して引っ張り、切れた時の倍率を測定することにより、製造したウェブの強さを評価した。作製したウェブを用い、引っ張り強伸度試験機を用いて把持長10cm、引張速度10cm/minで1分間延伸し、その間にウェブの切断が発生するか否かを確認した。下記の基準で評価した。
・Evaluation criteria for carbon fiber breakage prevention ◎ (Good): 90% or more ○ (Acceptable): 70% or more, less than 90% × (Not acceptable): Less than 70% Test category 4 (Strength of manufactured web)
The obtained web was held and pulled, and the ratio at which it broke was measured to evaluate the strength of the produced web. The produced web was stretched for 1 minute using a tensile strength and elongation tester at a grip length of 10 cm and a pulling speed of 10 cm/min, and it was confirmed whether the web broke during that time. Evaluation was made according to the following criteria.
・製造したウェブの強さの評価基準
◎◎(優れる):延伸中にウェブが切断しない場合
◎(良好):延伸中、50秒以上60秒未満の間に、ウェブが切断する場合
○(可):延伸中、40秒以上50秒未満の間に、ウェブが切断する場合
×(不可):延伸中、40秒未満でウェブが切断する場合
上記表の各比較例に対する各実施例の評価結果からも明らかなように、本発明の処理剤によると、処理剤が付与された炭素繊維がカード通過する際の折れを低減できる。また、処理剤が付与された炭素繊維から得られたウェブの強さを向上できる。
Evaluation criteria for strength of produced web: Excellent (excellent): when the web is not broken during stretching, Good (good): when the web is broken between 50 and 60 seconds during stretching, Fair (fair): when the web is broken between 40 and 50 seconds during stretching, Poor (unfair): when the web is broken in less than 40 seconds during stretching. As is clear from the evaluation results of each example and each comparative example in the above table, the treatment agent of the present invention can reduce breakage of carbon fiber to which the treatment agent is applied when passing through a card. Also, the strength of the web obtained from carbon fiber to which the treatment agent is applied can be improved.
Claims (9)
エステル化合物(C):1価脂肪族アルコールと1価カルボン酸とからなるエステル化合物。 A treatment agent for producing a carbon fiber-containing nonwoven fabric, comprising an epoxy compound (A) , a nonionic surfactant (B) , and an ester compound (C) , characterized in that the content of the epoxy compound (A) in a non-volatile matter of the treatment agent is 5% by mass or more and 60% by mass or less, the content of the ester compound (C) is 5 to 50% by mass, and the epoxy compound (A) has at least one compound selected from bisphenol A, bisphenol F, and diaminodiphenylmethane as a main skeleton.
Ester compound (C): An ester compound consisting of a monohydric aliphatic alcohol and a monobasic carboxylic acid.
エステル化合物(C):1価脂肪族アルコールと1価カルボン酸とからなるエステル化合物。 A treatment agent for producing a carbon fiber-containing nonwoven fabric, comprising an epoxy compound (A) , a nonionic surfactant (B) , and an ester compound (C) , characterized in that the content of the nonionic surfactant (B) in a non-volatile matter of the treatment agent is 30 mass % or more and 60 mass % or less , the content of the ester compound (C) is 5 to 40 mass %, and the epoxy compound (A) has at least one member selected from bisphenol A and bisphenol F as a main skeleton.
Ester compound (C): An ester compound consisting of a monohydric aliphatic alcohol and a monobasic carboxylic acid.
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JP2016194175A (en) | 2015-04-01 | 2016-11-17 | トヨタ自動車株式会社 | Resin-coated carbon fiber and carbon fiber reinforced composite material of the same |
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