JP5913996B2 - Oil and fat-containing rayon fiber, method for producing the same, and fiber structure - Google Patents
Oil and fat-containing rayon fiber, method for producing the same, and fiber structure Download PDFInfo
- Publication number
- JP5913996B2 JP5913996B2 JP2012005144A JP2012005144A JP5913996B2 JP 5913996 B2 JP5913996 B2 JP 5913996B2 JP 2012005144 A JP2012005144 A JP 2012005144A JP 2012005144 A JP2012005144 A JP 2012005144A JP 5913996 B2 JP5913996 B2 JP 5913996B2
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- Prior art keywords
- oil
- fiber
- fat
- mass
- rayon fiber
- Prior art date
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Landscapes
- Artificial Filaments (AREA)
Description
本発明は、特定の油脂を含有するレーヨン繊維、その製造方法及び繊維構造物に関する。 The present invention relates to a rayon fiber containing a specific fat and oil, a method for producing the same, and a fiber structure.
再生セルロースを用いたレーヨン繊維は、例えばビスコース法、銅アンモニア法、溶剤紡糸法等様々な方法で製造されることが知られている。レーヨン繊維は基質がセルロースであるため、それ自体肌に優しい性質を有する。従来から、上記レーヨン繊維の性質をさらに発揮させるため、様々な提案がされている。例えば、脂肪酸(油脂分)を練り込んだ再生セルロース繊維に関する提案として、オレイン酸又はオレイン酸の金属塩を練り込む提案(特許文献1)、γ−リノレン酸乳化液を練り込む提案(特許文献2〜3)、ドコサヘキサエン酸(DHA)乳化液を練り込む提案(特許文献4)、γ−リノレン酸の乳化物を練り込む提案(特許文献5)、オレイン酸又はその塩を練り込み、セル状領域を形成したレーヨン繊維の提案(特許文献6)、脂肪酸又はその塩と脂溶性の酸化防止剤を練り込み、セル状領域を形成したレーヨン繊維の提案(特許文献7)、こめ油、γ−オリザノール、フェルラ酸を含む乳化液を練り込む提案(特許文献8)、オリーブオイル乳化液を練り込む提案(特許文献9)、相変化材料をマイクロカプセルに封入して添加したセルロース系繊維の提案(特許文献10)等がある。また、特許文献11には、スクワラン等の油分を含むレーヨン繊維等の含油繊維を原料繊維として用いた化粧・美容用不織布が提案されている。 It is known that rayon fibers using regenerated cellulose are produced by various methods such as a viscose method, a copper ammonia method, and a solvent spinning method. Since rayon fiber is made of cellulose as a substrate, it itself has a gentle nature to the skin. Conventionally, various proposals have been made to further exhibit the properties of the rayon fiber. For example, as proposals regarding regenerated cellulose fibers kneaded with fatty acids (oils and fats), proposals for kneading oleic acid or metal salts of oleic acid (Patent Document 1), proposals for kneading γ-linolenic acid emulsion (Patent Document 2) -3), proposal to knead docosahexaenoic acid (DHA) emulsion (Patent Document 4), proposal to knead emulsion of γ-linolenic acid (Patent Document 5), knead oleic acid or salt thereof, cellular region Proposal of Rayon Fiber (Patent Document 6) Formed with Cation, Proposal of Rayon Fiber Formed with Cellulose Region by Kneading Fatty Acid or its Salt and Fat-soluble Antioxidant (Patent Document 7), Rice Oil, γ-Oryzanol , A proposal to knead an emulsion containing ferulic acid (Patent Document 8), a proposal to knead an olive oil emulsion (Patent Document 9), and added a phase change material enclosed in a microcapsule Proposal of cellulose fibers (Patent Document 10), and the like. Patent Document 11 proposes a non-woven fabric for cosmetics and beauty using oil-containing fibers such as rayon fibers containing oil such as squalane as raw material fibers.
特許文献1〜7で用いている脂肪酸は融点が14℃以下であるために常温で液体であり、容易に乳化することが可能である。また、特許文献8で用いているこめ油及び特許文献9で用いているオリーブオイルも不飽和脂肪酸を多く含むために低融点であり、容易に乳化可能である。特許文献10では、油脂あるいは脂肪酸をマイクロカプセル化して添加している。特許文献11で油分として用いているスクワランは、常温で液体であり、容易に乳化することが可能である。 Since the fatty acid used in Patent Documents 1 to 7 has a melting point of 14 ° C. or lower, it is liquid at room temperature and can be easily emulsified. In addition, the rice oil used in Patent Document 8 and the olive oil used in Patent Document 9 contain a large amount of unsaturated fatty acids, so have a low melting point and can be easily emulsified. In Patent Document 10, fats and oils or fatty acids are added as microcapsules. Squalane used as an oil component in Patent Document 11 is liquid at room temperature and can be easily emulsified.
上述したように、20℃以下で液体(融点が20℃以下)の油脂は、流動性が高く、肌になじみやすい性質を有し、乳化は比較的容易である。しかしながら、20℃以下で液体の油脂は二重結合を含む不飽和脂肪酸の含有量が多く、酸化が生じやすい。そのため、20℃以下で液体の油脂を繊維中に含有させる場合には、油脂の酸化を防止する必要がある。そこで、油脂の酸化を防止するため、油脂に酸化防止剤を添加する技術が提案されている。例えば、特許文献2〜5では、酸化防止剤として3,5−ジ−ブチルヒドロキシトルエン、イオウ系酸化防止剤、トコフェロール類を脂肪酸と併用することが開示されている。また、油脂としてこめ油を用いている特許文献8では、フェルラ酸を0.5〜2重量%含有させること、特許文献7では脂溶性の酸化防止剤を脂肪酸に含有させることが提案されている。 As described above, oils and fats that are liquid at 20 ° C. or lower (melting point: 20 ° C. or lower) have high fluidity and are easy to adjust to the skin, and are relatively easy to emulsify. However, liquid fats and oils at 20 ° C. or less have a high content of unsaturated fatty acids containing double bonds, and are likely to be oxidized. Therefore, when liquid fats and oils are contained in the fiber at 20 ° C. or lower, it is necessary to prevent the fats and oils from being oxidized. Therefore, in order to prevent the oxidation of fats and oils, a technique for adding an antioxidant to the fats and oils has been proposed. For example, Patent Documents 2 to 5 disclose that 3,5-di-butylhydroxytoluene, a sulfur-based antioxidant, and tocopherols are used in combination with a fatty acid as an antioxidant. Further, in Patent Document 8 using rice bran oil as an oil and fat, it is proposed that 0.5 to 2% by weight of ferulic acid is contained, and in Patent Document 7 that a fat-soluble antioxidant is contained in a fatty acid. .
しかしながら、例えば、20℃以下で液体の油脂を酸化防止剤とともにビスコース中に乳化して添加しようとすると十分に微細なエマルジョン化が困難であった。 However, for example, if an attempt is made to emulsify liquid oil and fat together with an antioxidant in viscose at 20 ° C. or less, it is difficult to make a sufficiently fine emulsion.
本発明は、従来の問題を解決するため、融点が20℃以下の油脂を酸化安定性が良好な状態でレーヨン繊維を構成するセルロース内に微分散させた油脂含有レーヨン繊維、その製造方法及び繊維構造物を提供する。 In order to solve the conventional problems, the present invention provides a fat-containing rayon fiber in which a fat having a melting point of 20 ° C. or less is finely dispersed in cellulose constituting the rayon fiber in a state of good oxidation stability, a method for producing the same, and a fiber Provide a structure.
本発明の油脂含有レーヨン繊維は、レーヨン繊維内に油脂及び酸化防止剤が含有された油脂含有レーヨン繊維であり、上記油脂は、脂肪酸及びそのグリセリンエステルから選ばれる少なくとも一つの脂肪酸成分を含み、且つ20℃において液体であり(ただし、こめ油を除く)、上記油脂において、リノレン酸の含有量は1質量%以下であり、上記酸化防止剤は、天然トコフェロールであり、上記レーヨン繊維内のセルロースと上記油脂とは非相溶状態で、且つ上記油脂は上記セルロース中に微分散されており、上記レーヨン繊維内の上記油脂を含有する粒子の平均粒子径が0.02〜0.8μmであることを特徴とする。
The oil-containing rayon fiber of the present invention is an oil-containing rayon fiber in which oil and fat and an antioxidant are contained in the rayon fiber, and the oil contains at least one fatty acid component selected from fatty acids and glycerin esters thereof, and It is liquid at 20 ° C. (except koji oil), and in the fats and oils, the content of linolenic acid is 1% by mass or less, the antioxidant is natural tocopherol, and the cellulose in the rayon fiber The fats and oils are in an incompatible state, the fats and oils are finely dispersed in the cellulose, and the average particle size of the particles containing the fats and oils in the rayon fiber is 0.02 to 0.8 μm. It is characterized by.
本発明の油脂含有レーヨン繊維の製造方法は、脂肪酸及びそのグリセリンエステルから選ばれる少なくとも一つの脂肪酸成分を含み、且つ20℃において液体である油脂(ただし、こめ油を除く)に、酸化防止剤と、HLB(Hydrophile−Lipophile Balance)が14.5〜19である第一乳化剤と、HLBが6〜12.5である第二乳化剤とを加えて、平均粒子径が0.02〜1μmのエマルジョン液を調製し、上記油脂において、リノレン酸の含有量は1質量%以下であり、上記酸化防止剤は、天然トコフェロールであり、セルロースを含むビスコース原液に、上記エマルジョン液を混合して紡糸用ビスコース液を調製し、上記紡糸用ビスコース液をノズルより押し出して紡糸し、凝固再生することを特徴とする。
The method for producing an oil-containing rayon fiber according to the present invention comprises at least one fatty acid component selected from a fatty acid and a glycerin ester thereof, and is an oil / fat that is liquid at 20 ° C. ( except for koji oil ), an antioxidant and An emulsion liquid having an average particle size of 0.02 to 1 μm by adding a first emulsifier having an HLB (Hydrophile-Lipophile Balance) of 14.5 to 19 and a second emulsifier having an HLB of 6 to 12.5 In the oil and fat, the content of linolenic acid is 1% by mass or less, the antioxidant is natural tocopherol, and the emulsion solution is mixed with a viscose stock solution containing cellulose to produce a spinning screw. A course liquid is prepared, and the spinning viscose liquid is extruded through a nozzle, spun, and coagulated and regenerated. .
本発明の油脂含有レーヨン繊維紡糸用ビスコース液は、脂肪酸及びそのグリセリンエステルから選ばれる少なくとも一つの脂肪酸成分を含み、且つ20℃において液体である油脂(ただし、こめ油を除く)に、酸化防止剤と、HLBが14.5〜19である乳化剤と、HLBが6〜12.5である乳化剤とを加えて調製した平均粒子径が0.02〜1μmのエマルジョン液を、セルロースを含むビスコース原液に混合しており、上記油脂において、リノレン酸の含有量は1質量%以下であり、上記酸化防止剤は、天然トコフェロールであることを特徴とする。 The viscose liquid for spinning oil-containing rayon fibers of the present invention contains at least one fatty acid component selected from fatty acids and glycerin esters thereof, and is an antioxidant for oils and fats ( except koji oil ) that are liquid at 20 ° C. Viscose containing cellulose, an emulsion having an average particle size of 0.02 to 1 μm, prepared by adding an agent, an emulsifier having an HLB of 14.5 to 19 and an emulsifier having an HLB of 6 to 12.5 The linolenic acid content is 1% by mass or less in the oil and fat, and the antioxidant is natural tocopherol .
本発明の繊維構造物は、上記油脂含有レーヨン繊維を含むものである。 The fiber structure of the present invention includes the oil-and-fat-containing rayon fiber.
本発明の油脂含有レーヨン繊維は、脂肪酸成分を含み、且つ常温(20℃)で液体である油脂を酸化防止剤と併用してレーヨン繊維中に含有させることにより、肌への馴染みが良好なレーヨン繊維とすることができる。また、酸化防止剤とともに油脂が繊維中に微分散されて多数存在することにより、油脂の酸化安定性が向上し、油脂自体のもつ機能が発揮され、ソフトな風合いの繊維となるとともに、油脂の酸化に伴う繊維強度の低下も防止できる。 The oil-containing rayon fiber of the present invention contains a fatty acid component and contains oil and fat that are liquid at room temperature (20 ° C.) in combination with an antioxidant in the rayon fiber, so that the rayon has good familiarity to the skin. It can be a fiber. In addition, the presence of a large number of oils and fats that are finely dispersed in the fiber together with the antioxidant improves the oxidation stability of the oils and fats, the functions of the oils and fats themselves are exhibited, and the fibers have a soft texture. A decrease in fiber strength accompanying oxidation can also be prevented.
本発明の製造方法は、油脂に酸化防止剤を添加する際に、HLBの異なる第一乳化剤と、第二乳化剤を併合して加えることで微細なエマルジョン化ができ、即ち平均粒子径が0.02〜1μmのエマルジョン液を調製することができ、セルロースを含むビスコース原液に上記エマルジョン液を混合して紡糸用ビスコース液、即ち本発明の油脂含有レーヨン繊維紡糸用ビスコース液とすることにより、酸化されやすい融点が20℃以下の油脂であっても、酸化安定性が良好な状態で繊維中に微分散して含有させることができる。 In the production method of the present invention, when an antioxidant is added to fats and oils, a first emulsifier having a different HLB and a second emulsifier can be added together to form a fine emulsion. An emulsion liquid of 02 to 1 μm can be prepared. By mixing the above emulsion liquid with a viscose stock solution containing cellulose, a viscose liquid for spinning, that is, a viscose liquid for spinning oil-containing rayon fiber of the present invention is obtained. Even oils and fats having a melting point of 20 ° C. or less that are easily oxidized can be finely dispersed in the fiber with good oxidation stability.
本発明の繊維構造物は、肌に優しく、ヌメリ感があり、ソフトな風合いとすることができる。 The fiber structure of the present invention is gentle to the skin, has a slimy feeling, and can have a soft texture.
本発明のレーヨン繊維は、レーヨン繊維内に油脂及び酸化防止剤が含有された油脂含有レーヨン繊維である。 The rayon fiber of the present invention is an oil and fat-containing rayon fiber in which oil and fat and an antioxidant are contained in the rayon fiber.
(油脂)
本発明に用いられる油脂は、脂肪酸及びそのグリセリンエステルから選ばれる少なくとも一つの脂肪酸成分を含み、且つ20℃において液体である。上記脂肪酸としては、飽和脂肪酸、不飽和脂肪酸が挙げられ、上記脂肪酸のグリセリンエステルとしては、飽和脂肪酸のグリセリンエステル、飽和脂肪酸の混合グリセリンエステル、不飽和脂肪酸のグリセリンエステル、不飽和脂肪酸の混合グリセリンエステル、飽和脂肪酸と不飽和脂肪酸の混合グリセリンエステル等が挙げられる。一般に脂肪酸は、炭素数が増加すると融点が上がり、同じ炭素数の場合、飽和脂肪酸に比べて不飽和脂肪酸の融点は低い傾向にある。脂肪酸成分を含有し、20℃において液体の天然由来の油脂は融点が20℃以下であるものが多く、常温で固体状の油脂に比べて流動性が高く、肌になじみやすい効果を与えることができる。本発明において、20℃において液体である油脂とは、油脂の融点が20℃以下であることを意味する。
(Oil and fat)
The fats and oils used in the present invention contain at least one fatty acid component selected from fatty acids and glycerin esters thereof and are liquid at 20 ° C. Examples of the fatty acids include saturated fatty acids and unsaturated fatty acids. Examples of the glycerin esters of the fatty acids include saturated fatty acid glycerin esters, saturated fatty acid mixed glycerin esters, unsaturated fatty acid glycerin esters, and unsaturated fatty acid mixed glycerin esters. And mixed glycerin ester of saturated fatty acid and unsaturated fatty acid. In general, when the number of carbon atoms increases, the melting point of the fatty acid increases. When the number of carbon atoms is the same, the melting point of the unsaturated fatty acid tends to be lower than that of the saturated fatty acid. It contains a fatty acid component, and many of naturally occurring oils and fats that are liquid at 20 ° C. have a melting point of 20 ° C. or less, and are more fluid than normal oils and fats at room temperature, giving an effect that is easy to adjust to the skin. it can. In the present invention, the oil that is liquid at 20 ° C. means that the melting point of the oil is 20 ° C. or less.
本発明に用いられる油脂に含まれる脂肪酸成分は、飽和脂肪酸、不飽和脂肪酸及びそれらのグリセリンエステルのいずれであってもよい。脂肪酸の炭素数としては、特に限定されないが、例えば、炭素数16〜22であることが好ましい。上記不飽和脂肪酸としては、パルミトレイン酸、オレイン酸、リノール酸、リノレン酸、エイコセン酸、エルシン酸等から選ばれる少なくとも1種を含むことが好ましい。上記飽和脂肪酸としては、パルミチン酸、ステアリン酸、アラキジン酸、ペヘニン酸等から選ばれる少なくとも1種を含むことが好ましい。 The fatty acid component contained in the fats and oils used in the present invention may be any of saturated fatty acids, unsaturated fatty acids, and glycerin esters thereof. Although it does not specifically limit as carbon number of a fatty acid, For example, it is preferable that it is C16-22. The unsaturated fatty acid preferably contains at least one selected from palmitoleic acid, oleic acid, linoleic acid, linolenic acid, eicosenoic acid, erucic acid and the like. The saturated fatty acid preferably contains at least one selected from palmitic acid, stearic acid, arachidic acid, pehenic acid and the like.
上記油脂は、飽和脂肪酸及び不飽和脂肪酸を含むことが好ましく、飽和脂肪酸の含有量が10〜40質量%、不飽和脂肪酸の含有量が60〜90質量%であることがより好ましい。飽和脂肪酸及び不飽和脂肪酸を含むと、それぞれの脂肪酸の持つ様々な効果を享受できる点で好ましい。 The fats and oils preferably contain saturated fatty acids and unsaturated fatty acids, more preferably 10 to 40% by mass of saturated fatty acids and 60 to 90% by mass of unsaturated fatty acids. When saturated fatty acid and unsaturated fatty acid are included, it is preferable at the point which can receive the various effects which each fatty acid has.
通常、油脂の融点は、油脂に含まれる脂肪酸の融点に依存する。例えば、複数の脂肪酸を含む油脂であれば、油脂として測定したときの融点をいい、その融点が20℃以下であれば20℃において液体である油脂に含まれる。 Usually, the melting point of fats and oils depends on the melting point of fatty acids contained in the fats and oils. For example, in the case of fats and oils containing a plurality of fatty acids, the melting point when measured as fats and oils is used. If the melting point is 20 ° C. or less, the fats and oils are liquid at 20 ° C.
上記油脂が天然由来の油脂である場合、飽和脂肪酸及び/又は不飽和脂肪酸のグリセリンエステルとして存在していることがある。グリセリンエステルとして存在することにより、各々の脂肪酸の有する機能を幅広く発揮することができる。また、融点について、油脂の融点が低いことにより、流動性が高くなり肌になじみやすくなる。具体的には、天然由来の油脂の融点は、−30〜20℃であることが好ましい。より好ましくは、−25〜15℃である。 When the said fats and oils are naturally derived fats and oils, it may exist as a glycerol ester of a saturated fatty acid and / or an unsaturated fatty acid. By being present as a glycerin ester, the functions of each fatty acid can be exhibited widely. Moreover, about melting | fusing point, when the melting | fusing point of fats and oils is low, fluidity | liquidity becomes high and becomes easy to adapt to skin. Specifically, the melting point of naturally derived fats and oils is preferably -30 to 20 ° C. More preferably, it is −25 to 15 ° C.
上記天然由来の油脂としては、例えば、オリーブ果実より得られるオリーブオイル(通常、パルミチン酸9〜18%、パルミトレイン酸0〜3%、ステアリン酸2〜4%、オレイン酸60〜80%、リノール酸4〜16%、リノレン酸0〜1%を含む)、ブドウ種子より得られるグレープシードオイル(通常、パルミチン酸6〜8%、ステアリン酸3〜10%、オレイン酸18〜20%、リノール酸67〜71%、リノレン酸0〜1%を含む)、トウモロコシ胚芽より得られるコーンオイル(通常、パルミチン酸9〜12%、ステアリン酸1〜3%、オレイン酸25〜33%、リノール酸50〜60%、リノレン酸0〜2%を含む)、大豆種子より得られる大豆油(通常、パルミチン酸10〜12%、ステアリン酸2〜5%、オレイン酸20〜25%、リノール酸50〜57%、リノレン酸5〜9%を含む)、米糠より得られる米油(通常、ミリチリン酸0〜1%、パルミチン酸16〜17%、ステアリン酸1〜2%、オレイン酸40〜44%、リノール酸35〜37%、リノレン酸0〜2%、アラキジン酸0〜1%を含む)、ワタの種子より得られる綿実油(通常、ミリチリン酸0〜3%、パルミチン酸20〜30%、ステアリン酸1〜5%、オレイン酸15〜30%、リノール酸40〜52%、アラキジン酸0〜1%を含む)、くるみの種子より得られるくるみ油(通常、パルミチン酸6〜8%、ステアリン酸1〜3%、オレイン酸14〜21%、リノール酸57〜72%リノレン酸10%を含む)、落花生の種子から得られる落花生油(通常、パルミチン酸10〜12%、ステアリン酸2〜5%、オレイン酸40〜49%、リノール酸30〜37%、リノレン酸0〜2%、アラキジン酸1〜2%、エイコセン酸0〜2%、ベヘン酸0〜4%、リグノセリン酸0〜2%を含む)、アブラナの種子より得られる菜種油(通常、ローエルシックタイプではパルミチン酸3〜6%、ステアリン酸1〜3%、オレイン酸46〜59%、リノール酸21〜32%、リノレン酸9〜16%、アラキジン酸0〜1%、エルシン酸1〜5%を含む)、ツバキ科のヤブツバキの種子から得られる椿油(通常、パルミチン酸8%、ステアリン酸2%、オレイン酸79〜85%、リノール酸3〜9%、リノレン酸0〜1%を含む)等が挙げられる。 Examples of the natural fats and oils include olive oil obtained from olive fruit (usually palmitic acid 9 to 18%, palmitoleic acid 0 to 3%, stearic acid 2 to 4%, oleic acid 60 to 80%, linoleic acid 4-16%, including linolenic acid 0-1%), grape seed oil obtained from grape seeds (usually palmitic acid 6-8%, stearic acid 3-10%, oleic acid 18-20%, linoleic acid 67 -71%, including linolenic acid 0-1%), corn oil obtained from corn germ (usually 9-12% palmitic acid, 1-3% stearic acid, 25-33% oleic acid, 50-60 linoleic acid %, Including linolenic acid 0-2%), soybean oil obtained from soybean seed (usually 10-12% palmitic acid, 2-5% stearic acid, oleic acid 20 25%, including linoleic acid 50-57%, linolenic acid 5-9%), rice oil obtained from rice bran (usually 0 to 1% myristic acid, 16 to 17% palmitic acid, 1 to 2% stearic acid, 40-44% oleic acid, 35-37% linoleic acid, 0-2% linolenic acid, 0-1% arachidic acid, cottonseed oil obtained from cotton seeds (usually 0-3% myrrhilic acid, palmitic acid 20-30%, stearic acid 1-5%, oleic acid 15-30%, linoleic acid 40-52%, arachidic acid 0-1% included), walnut oil obtained from walnut seeds (usually palmitic acid 6 -8%, stearic acid 1-3%, oleic acid 14-21%, linoleic acid 57-72% linolenic acid 10% included), peanut oil obtained from peanut seeds (usually 10-12% palmitic acid, The Aric acid 2-5%, oleic acid 40-49%, linoleic acid 30-37%, linolenic acid 0-2%, arachidic acid 1-2%, eicosenoic acid 0-2%, behenic acid 0-4%, lignoserine Rapeseed oil obtained from oilseed rape seeds (usually 3-6% palmitic acid, 1-3% stearic acid, 46-59% oleic acid, 21-32% linoleic acid in low L chic type) , Linolenic acid 9-16%, arachidic acid 0-1%, erucic acid 1-5%), camellia oil obtained from camellia seeds (usually palmitic acid 8%, stearic acid 2%, oleic acid) 79-85%, linoleic acid 3-9%, and linolenic acid 0-1%).
中でも好ましい油脂は椿油である。椿油はツバキ科カメリア属植物の種子から得られる植物性油脂であり、常温(20℃)で液状の油脂である。日本では伊豆大島や長崎五島を中心に栽培されているツバキ節のヤブツバキの種子から生産されている。また、同じくツバキ節のトウツバキ種子から生産されるトウツバキ油の他、サザンカ節のサザンカやユチャ、チャ節のチャノキ等の種子から得られるものが挙げられる。椿油の成分は、オレイン酸を含む不飽和脂肪酸のグリセリンエステルが主成分で、他にトコロフェノール、サポニンも微量に含まれる。椿油を用いることにより、オレイン酸の有する角質層保護、乾燥肌改善効果を持たせることができる。 Among them, preferred oil is fat oil. Camellia oil is a vegetable oil obtained from the seeds of the Camellia family Camellia, and is a liquid oil at room temperature (20 ° C.). In Japan it is produced from camellia seeds of camellia knots that are cultivated mainly in Izu Oshima and Nagasaki Goto. In addition, other than the camellia oil produced from camellia seeds of camellia, there are those obtained from seeds such as sasanqua and yucha of sasanqua, or chanoki of tea. The components of coconut oil are mainly composed of glycerin esters of unsaturated fatty acids including oleic acid, and also contain trace amounts of tocopherol and saponin. By using cocoon oil, stratum corneum protection and dry skin improvement effect possessed by oleic acid can be provided.
椿油の脂肪酸組成は、椿油の産地、収穫時期、気候条件等によって原料品質が変動するが、飽和脂肪酸が10〜30質量%、不飽和脂肪酸が70〜90質量%であることが好ましい。上記範囲内にあると、各脂肪酸成分の機能を有効に発揮することができる。 Although the raw material quality of the fatty acid composition of camellia oil varies depending on the production area, harvest time, climatic conditions, etc., it is preferable that the saturated fatty acid is 10 to 30% by mass and the unsaturated fatty acid is 70 to 90% by mass. Within the above range, the function of each fatty acid component can be effectively exhibited.
(酸化防止剤)
油脂と酸化防止剤を併用することによって、油脂の酸化を防止することができ、ひいては油脂の酸化による繊維強度の低下を防止できる。上記酸化防止剤としては、例えば、脂溶性の酸化防止剤及び水溶性の酸化防止剤のいずれを用いてもよい。油脂との相溶性の観点から、酸化防止剤は脂溶性酸化防止剤であることが好ましい。
(Antioxidant)
By using fats and oils together with antioxidants, the fats and oils can be prevented from being oxidized, and as a result, the fiber strength can be prevented from lowering due to the fats and oils being oxidized. As the antioxidant, for example, either a fat-soluble antioxidant or a water-soluble antioxidant may be used. From the viewpoint of compatibility with fats and oils, the antioxidant is preferably a fat-soluble antioxidant.
上記脂溶性酸化防止剤としては、例えばトコフェロール、β−カロチン及びユビキノール(CoQ10)等の天然の酸化防止剤、並びにBHT(ジブチルヒドロキシルトルエン)、及びBHA(ブチルヒドロキシアニソール)等の合成酸化防止剤が挙げられる。中でも、
皮膚に対する低刺激性の観点から、天然酸化防止剤であることが好ましい。上記トコフェロール類としては、天然トコフェロール及び合成トコフェロールのいずれを使用してもよい。天然トコフェロールは、一般に植物油等から抽出、濃縮、精製されるもので、光学異性体を含まない(D体のみ)。一方、合成トコフェロールは、一般に工業的に合成されたもので、光学異性体はD体とL体が混合した状態のものである。上記合成トコフェロールとしては、例えば酢酸トコフェロール等が挙げられる。酸化防止性により優れるという観点では、天然トコフェロールであることが好ましい。また、トコフェロール類には、α型、β型、γ型、δ型があるが、酸化防止性により優れるという観点から、δ型トコフェロールを含むことが好ましい。β−カロチン、ユビキノール(CoQ10)、BHT、及びBHAは、トコフェロール類と同等の作用効果がある。
Examples of the fat-soluble antioxidant include natural antioxidants such as tocopherol, β-carotene and ubiquinol (CoQ10), and synthetic antioxidants such as BHT (dibutylhydroxyl toluene) and BHA (butylhydroxyanisole). Can be mentioned. Above all,
From the viewpoint of low irritation to the skin, a natural antioxidant is preferable. As the tocopherols, either natural or synthetic tocopherols may be used. Natural tocopherols are generally extracted, concentrated and purified from vegetable oils and the like, and do not contain optical isomers (D-form only). On the other hand, synthetic tocopherols are generally synthesized industrially, and optical isomers are in a state where D-form and L-form are mixed. Examples of the synthetic tocopherol include tocopherol acetate. From the standpoint of superior antioxidant properties, natural tocopherol is preferred. In addition, the tocopherols include α-type, β-type, γ-type, and δ-type, and it is preferable that δ-type tocopherol is included from the viewpoint of superior antioxidant properties. β-carotene, ubiquinol (CoQ10), BHT, and BHA have the same effects as tocopherols.
上記水溶性の酸化防止剤としては、例えばアスコルビン酸、イソアスコルビン酸;カテキン、アントシアニン、タンニン、クエルセチン(ルチン、クエルシトリン等の各種配糖体、酵素処理イソクエルシトリン等の酵素処理及び化学処理を加えたものを含む)、ミリシトリン、ミリセチン、イソフラボン等のフラボノイド;クロロゲン酸、エラグ酸、クルクミン等のフェノール酸;リンゴポリフェノール、カカオマスポリフェノール等のポリフェノール;アスタキサンチン、ルテイン等の水に可溶なカルテノイドから選ばれる少なくとも1つであることが好ましい。また、上記水溶性の酸化防止剤を含む植物抽出物は、例えば、茶、ローズマリー、葡萄、柿やヤマモモ等の抽出物であってもよい。上記植物抽出物は、特に制限されないが、例えば、上記植物を粉末にした後、水や含水アルコール等の溶媒を用いて抽出する植物の溶媒抽出液やそれを濃縮若しくは乾燥したもの等が挙げられる。また、アントシアニンを含む市販の葡萄果汁や、ブドウ果皮色素等を用いてもよい。 Examples of the water-soluble antioxidant include ascorbic acid, isoascorbic acid; catechin, anthocyanin, tannin, quercetin (various glycosides such as rutin and quercitrin, and enzyme treatment and chemical treatment such as enzyme-treated isoquercitrin. Flavonoids such as myricitrin, myricetin and isoflavone; phenolic acids such as chlorogenic acid, ellagic acid and curcumin; polyphenols such as apple polyphenol and cacao mass polyphenol; It is preferable that at least one selected. In addition, the plant extract containing the water-soluble antioxidant may be an extract of tea, rosemary, strawberries, strawberries, bayberry, etc., for example. The plant extract is not particularly limited, and examples thereof include a plant solvent extract obtained by powdering the plant and then using a solvent such as water or hydrous alcohol, or a solution obtained by concentrating or drying the plant extract. . Moreover, you may use the commercially available persimmon fruit juice containing anthocyanin, grape skin pigment | dye, etc.
上記油脂含有レーヨン繊維において、上記油脂は上記セルロース中に微分散されており、上記レーヨン繊維内の上記油脂を含有する粒子の平均粒子径が0.02〜0.8μmである。繊維中に均一に微分散されることで油脂の特性が発揮できるという観点から、上記油脂を含有する粒子の平均粒子径が0.04〜0.5μmであることが好ましく、0.06〜0.25μmであることがより好ましい。 In the oil and fat-containing rayon fiber, the oil and fat is finely dispersed in the cellulose, and the average particle diameter of the particles containing the oil and fat in the rayon fiber is 0.02 to 0.8 μm. From the viewpoint that the characteristics of fats and oils can be exhibited by being finely dispersed uniformly in the fiber, the average particle diameter of the particles containing fats and oils is preferably 0.04 to 0.5 μm, and 0.06 to 0 More preferably, it is 25 μm.
上記油脂含有レーヨン繊維内の上記油脂を含有する粒子の平均粒子径は、脱油処理後の上記油脂含有レーヨン繊維を用いて測定することができる。具体的には、脱油処理後の上記油脂含有レーヨン繊維における空隙部の平均孔径を測定することで、上記油脂含有レーヨン繊維内の上記油脂を含有する粒子の平均粒子径を確認することができる。脱油処理後の上記油脂含有レーヨン繊維における空隙部は、脱油処理により微分散していた油脂が抜けることにより形成されるものであるため、脱油処理後の上記油脂含有レーヨン繊維における空隙部の平均孔径を測定することで、上記油脂含有レーヨン繊維内の上記油脂を含有する粒子の平均粒子径を確認することができる。上記油脂含有レーヨン繊維の脱油処理後の空隙部の平均孔径は、脱油処理後の繊維の断面写真(走査型電子顕微鏡写真、倍率3000倍)を用いて測定する。具体的には、脱油処理後の繊維の断面写真(走査型電子顕微鏡写真、倍率3000倍)を画像処理により倍率9010倍に拡大し、印刷した紙面上から任意の繊維の断面をサンプリングし、その繊維断面における繊維の外周から3μm内部までの間に存在する空隙部の直径を計測し、計測した100個の空隙部の直径を平均して空隙部の平均孔径とする。なお、楕円状の空隙部は長径及び短径を計測して算出した面積から真円直径に換算し、空隙部の直径とする。上記において、脱油処理は、下記のように行う。
(I)試料約2.3gを精秤し、底部に小さい穴の空いた試料管に詰める。
(II)底部の穴を塞ぎ、抽出溶媒としてメタノール10mlを試料管に注加し、一定時間静置し浸透させてからプレス装置によりメタノール処理液を抽出する。
(III)同じ試料を使用して上記の操作(II)による抽出を20回繰り返した後、試料管から取り出した試料を水洗し、105℃、2時間で乾燥して脱油処理後の繊維を得た。
The average particle diameter of the particles containing the oil and fat in the oil and fat-containing rayon fiber can be measured using the oil and fat-containing rayon fiber after the deoiling treatment. Specifically, by measuring the average pore diameter of the voids in the oil-containing rayon fiber after deoiling treatment, the average particle diameter of the particles containing the oil in the oil-containing rayon fiber can be confirmed. . Since the voids in the oil-containing rayon fiber after deoiling treatment are formed by the removal of the oil and fat finely dispersed by deoiling treatment, the voids in the oil-containing rayon fiber after deoiling treatment By measuring the average pore diameter, the average particle diameter of the particles containing the oil and fat in the oil and fat-containing rayon fiber can be confirmed. The average pore diameter of the voids after the deoiling treatment of the oil-and-fat-containing rayon fiber is measured using a cross-sectional photograph (scanning electron micrograph, magnification 3000 times) of the fiber after the deoiling treatment. Specifically, the cross-sectional photograph of the fiber after deoiling treatment (scanning electron micrograph, magnification 3000 times) is magnified to a magnification of 9010 by image processing, and the cross-section of any fiber is sampled from the printed paper, The diameter of the void existing between the outer periphery of the fiber and the inside of 3 μm in the fiber cross section is measured, and the average diameter of the 100 measured voids is taken as the average pore diameter of the void. In addition, an elliptical space | gap part is converted into a perfect circle diameter from the area calculated by measuring a long diameter and a short diameter, and is set as the diameter of a space | gap part. In the above, the deoiling process is performed as follows.
(I) About 2.3 g of a sample is precisely weighed and packed in a sample tube having a small hole at the bottom.
(II) The bottom hole is closed, and 10 ml of methanol as an extraction solvent is poured into the sample tube, allowed to stand for a certain period of time and allowed to permeate, and then the methanol treatment liquid is extracted by a press device.
(III) Using the same sample, the extraction by the above operation (II) was repeated 20 times, and then the sample taken out from the sample tube was washed with water, dried at 105 ° C. for 2 hours, and the fiber after deoiling treatment Obtained.
以下、図面を用いて説明する。図1Aは、繊維断面を走査型電子顕微鏡により倍率3000倍で観察した顕微鏡写真である。図1Bは、図1Aを部分的に拡大した画像である(倍率9010倍)。図1A−Bにおける黒い点が空隙部であり、微分散していた油脂が脱油により抜けた後の微小領域部分である。図1A−Bからレーヨン繊維内のセルロースと油脂とは非相溶状態で、且つ上記油脂は上記セルロース中に微分散されていることがわかる。 Hereinafter, it demonstrates using drawing. FIG. 1A is a photomicrograph of a fiber cross section observed with a scanning electron microscope at a magnification of 3000 times. FIG. 1B is an image obtained by partially enlarging FIG. 1A (magnification 9010 times). The black dots in FIGS. 1A and 1B are voids, and are minute regions after finely dispersed oils and fats are removed by deoiling. 1A-B show that the cellulose and the fats and oils in the rayon fiber are in an incompatible state, and the fats and oils are finely dispersed in the cellulose.
本発明の油脂含有レーヨン繊維は、特に限定されないが、下記のように製造することが好ましい。油脂をエマルジョン化して得られたエマルジョン液を、セルロースを含むビスコース原液に添加して紡糸用ビスコース液を調製し、得られた紡糸用ビスコース液を紡糸して油脂含有レーヨン繊維を得ることができる。 The fat and oil-containing rayon fiber of the present invention is not particularly limited, but is preferably produced as follows. An emulsion obtained by emulsifying oil and fat is added to a viscose stock solution containing cellulose to prepare a viscose solution for spinning, and the obtained viscose solution for spinning is spun to obtain an oil-containing rayon fiber. Can do.
(油脂のエマルジョン化)
上記油脂を、HLBの異なる第一乳化剤と第二乳化剤を併用して乳化させてエマルジョン液を得る。その際に、上記酸化防止剤も油脂と併せて添加する。上記酸化防止剤のエマルジョン液中に占める割合は、0.2〜20質量%であることが好ましい。より好ましくは1.5〜15質量%、さらに好ましくは好適には2.5〜10質量%である。上記範囲内にあると、油脂の酸化安定性が向上して、油脂自体のもつ機能が発揮され、ソフトな風合いの繊維となるとともに、油脂の酸化に伴う繊維強度の低下を防止できる。乳化方法としては転相乳化法、強制乳化方法等既知の乳化法を用いることができる。
(Emulsion of fats and oils)
The said fats and oils are emulsified by using together the 1st emulsifier and 2nd emulsifier from which HLB differs, and an emulsion liquid is obtained. In that case, the said antioxidant is also added together with fats and oils. The proportion of the antioxidant in the emulsion is preferably 0.2 to 20% by mass. More preferably, it is 1.5-15 mass%, More preferably, it is 2.5-10 mass% suitably. If it is within the above range, the oxidation stability of fats and oils is improved, the functions of the fats and oils themselves are exhibited, the fibers become soft and the fiber strength can be prevented from being lowered due to the oxidation of the fats and oils. As the emulsification method, known emulsification methods such as phase inversion emulsification method and forced emulsification method can be used.
<第一乳化剤>
上記第一乳化剤としては、HLBが14.5〜19の乳化剤を用い、好ましくはHLBが16〜18の乳化剤を用いる。上記第一乳化剤としては、例えば、ポリオキシエチレンアルキルエーテル等のポリオキシアルキレンアルキルエーテル、ポリオキシエチレンアルケニルエーテル等のポリオキシアルキレンアルケニルエーテル、ポリオキシアルキレンアルキルフェニルエーテル、ポリオキシアルキレンスチレン化ルフェニルエーテル、ポリオキシアルキレンアルキルスチレン化ルフェニルエーテル、ポリオキシアルキレンクミルフェニルエーテル、ポリオキシアルキレンβ-ナフチルエーテル、ポリオキシアルキレンひまし油エーテル、ポリオキシアルキレン硬化ひまし油エーテル等が挙げられる。特に、ポリオキシエチレンアルキルエーテル及び/又はポリオキシエチレンアルケニルエーテルであることが好ましい。上記HLB範囲を満たすポリオキシエチレンアルキル及びポリオキシエチレンアルケニルエーテルは、ポリオキシエチレンとして重合度が好ましくは30〜200、より好ましくは40〜150であり、且つアルキル及びアルケニル鎖の炭素数が好ましくは12〜22、より好ましくは16〜18である。また、上記第一乳化剤としては、例えば上記ポリオキシエチレン・ポリオキシアルキレングリコールブロックポリマー(PAG)を用いてもよい。前記PAGは、乳化安定を補助する助剤として用いられる。上記第一乳化剤の添加量は、油脂に対して5〜35質量%であることが好ましく、5〜15質量%であることがより好ましい。また、上記ポリオキシエチレン・ポリオキシアルキレングリコールブロックポリマーの添加量は、油脂に対して0.5〜3.0質量%であることが好ましい。
<First emulsifier>
As said 1st emulsifier, the emulsifier whose HLB is 14.5-19 is used, Preferably the emulsifier whose HLB is 16-18 is used. Examples of the first emulsifier include polyoxyalkylene alkyl ethers such as polyoxyethylene alkyl ethers, polyoxyalkylene alkenyl ethers such as polyoxyethylene alkenyl ethers, polyoxyalkylene alkylphenyl ethers, and polyoxyalkylene styrenated ruphenyl ethers. , Polyoxyalkylene alkyl styrenated ruphenyl ether, polyoxyalkylene cumyl phenyl ether, polyoxyalkylene β-naphthyl ether, polyoxyalkylene castor oil ether, polyoxyalkylene hardened castor oil ether, and the like. In particular, polyoxyethylene alkyl ether and / or polyoxyethylene alkenyl ether are preferable. The polyoxyethylene alkyl and polyoxyethylene alkenyl ether satisfying the above HLB range preferably have a degree of polymerization of 30 to 200, more preferably 40 to 150 as polyoxyethylene, and the number of carbon atoms in the alkyl and alkenyl chains is preferably It is 12-22, More preferably, it is 16-18. Moreover, as said 1st emulsifier, you may use the said polyoxyethylene polyoxyalkylene glycol block polymer (PAG), for example. The PAG is used as an auxiliary agent that assists in emulsion stability. The amount of the first emulsifier added is preferably 5 to 35% by mass and more preferably 5 to 15% by mass with respect to the fats and oils. Moreover, it is preferable that the addition amount of the said polyoxyethylene polyoxyalkylene glycol block polymer is 0.5-3.0 mass% with respect to fats and oils.
<第二乳化剤>
上記第二乳化剤としては、HLBが6〜12.5の乳化剤を用い、好ましくはHLBが6〜12、より好ましくはHLBが8〜11の乳化剤を用いる。上記第二乳化剤としては、例えばポリオキシエチレンアルキルエーテル等のポリオキシアルキレンアルキルエーテル、ポリオキシアルキレンアルケニルエーテル、ポリオキシアルキレンクミルフェニルエーテル、ポリオキシアルキレンβ-ナフチルエーテル、ポリオキシアルキレンフェニルエーテル、ポリオキシアルキレンベンジルエーテル等を用いることができる。上記HLB範囲を満たすポリオキシエチレンアルキルエーテルは、ポリオキシエチレンとして重合度が好ましくは1〜8、より好ましくは2〜4で、且つアルキル鎖の炭素数が好ましくは4〜12、より好ましくは6〜8である。上記第二乳化剤の添加量は、油脂に対して2〜25質量%であることが好ましく、2〜15質量%であることがより好ましい。
<Second emulsifier>
As said 2nd emulsifier, the emulsifier whose HLB is 6-12.5 is used, Preferably the HLB is 6-12, More preferably, the emulsifier whose HLB is 8-11 is used. Examples of the second emulsifier include polyoxyalkylene alkyl ethers such as polyoxyethylene alkyl ether, polyoxyalkylene alkenyl ethers, polyoxyalkylene cumyl phenyl ethers, polyoxyalkylene β-naphthyl ethers, polyoxyalkylene phenyl ethers, Oxyalkylene benzyl ether and the like can be used. The polyoxyethylene alkyl ether satisfying the above HLB range preferably has a polymerization degree of 1 to 8, more preferably 2 to 4, and preferably 4 to 12, more preferably 6 carbon atoms in the alkyl chain as polyoxyethylene. ~ 8. The amount of the second emulsifier added is preferably 2 to 25% by mass and more preferably 2 to 15% by mass with respect to the fat.
上記第一乳化剤と上記第二乳化剤のHLBの差は3以上であることが好ましく、5以上であることがより好ましい。より乳化良好で且つ安定性良好なエマルジョン液が得られる。 The difference in HLB between the first emulsifier and the second emulsifier is preferably 3 or more, and more preferably 5 or more. An emulsion liquid with better emulsification and better stability can be obtained.
上述したようにHLBの異なる乳化剤を併用することで、乳化良好で且つ安定性良好な微細なエマルジョン液が得られる。第一乳化剤と第二乳化剤の混合比は、質量比で、1:1〜20:1であることが好ましい。より好ましくは1.5:1〜10:1、さらにより好ましくは2:1〜5:1である。HLBの相対的に低い第二乳化剤が油脂の極性に影響を与え、HLBの相対的に高い第一乳化剤と併用することにより安定で粒子径の小さいエマルジョンが得られる。なお、本発明における所定のエマルジョンが得られる範囲において、第一乳化剤と第二乳化剤に加えてHLBが13以上14.5未満の第三乳化剤を添加してもよい。 As described above, by using an emulsifier having a different HLB in combination, a fine emulsion liquid having good emulsification and good stability can be obtained. The mixing ratio of the first emulsifier and the second emulsifier is preferably 1: 1 to 20: 1 by mass ratio. More preferably, it is 1.5: 1 to 10: 1, and still more preferably 2: 1 to 5: 1. The second emulsifier having a relatively low HLB affects the polarity of the oil and fat, and a stable emulsion having a small particle diameter can be obtained by using it together with the first emulsifier having a relatively high HLB. In addition, in the range in which the predetermined emulsion in this invention is obtained, you may add the 3rd emulsifier whose HLB is 13 or more and less than 14.5 in addition to the 1st emulsifier and the 2nd emulsifier.
<第三乳化剤>
第三乳化剤は、HLBが13以上14.5未満であり、13.3〜14.2であることが好ましい。第三乳化剤としては、例えば、ポリオキシエチレンひまし油エーテル等のポリオキシアルキレンひまし油エーテル、ポリオキシエチレン硬化ひまし油エーテル等のポリオキシアルキレン硬化ひまし油エーテル等(以下において、これらを総称してひまし油エーテル系の乳化剤とも記す。)を用いることができる。特に、上記ひまし油エーテル系の乳化剤は、油脂の乳化、可溶化に効果があり、油脂を効果的に乳化することができる。大豆油、椿油等脂肪酸組成がオレイン酸リッチな油脂については、第一乳化剤と第二乳化剤に加えて、親水基を有するひまし油エーテル系の乳化剤を併用することが好ましい。上記第三乳化剤の添加量は、油脂に対して20質量%以下であることが好ましく、5〜15質量%であることがより好ましい。
<Third emulsifier>
The third emulsifier has an HLB of 13 or more and less than 14.5, and preferably 13.3 to 14.2. Examples of the third emulsifier include polyoxyalkylene castor oil ethers such as polyoxyethylene castor oil ether, polyoxyalkylene cured castor oil ethers such as polyoxyethylene hydrogenated castor oil ether, and the like (hereinafter collectively referred to as castor oil ether emulsifiers). Can also be used.). In particular, the castor oil ether emulsifier is effective in emulsifying and solubilizing fats and oils, and can effectively emulsify fats and oils. For fats and oils rich in oleic acid such as soybean oil and coconut oil, it is preferable to use a castor oil ether emulsifier having a hydrophilic group in addition to the first emulsifier and the second emulsifier. The addition amount of the third emulsifier is preferably 20% by mass or less, more preferably 5 to 15% by mass with respect to the fats and oils.
乳化をより良好にするという観点から、第一乳化剤としてHLB14.5〜19のポリオキシアルキレンエーテル及びHLB14.5〜19のポリオキシアルキレン(硬化)ひまし油エーテルを併合して用いることや、第一乳化剤としてHLB14.5〜19のポリオキシアルキレンエーテルを用い、第三乳化剤としてHLB13以上14.5未満のポリオキシアルキレン(硬化)ひまし油エーテルを併合して用いることが好ましい。上記の乳化剤の組み合わせにおいて、ポリオキシアルキレン(硬化)ひまし油エーテルはHLB13〜16であることがより好ましい。酸化防止剤の含有量が多くなった場合、特に効果的に乳化できる。 From the viewpoint of making the emulsification better, HLB 14.5-19 polyoxyalkylene ether and HLB 14.5-19 polyoxyalkylene (cured) castor oil ether are used in combination as the first emulsifier, It is preferable to use polyoxyalkylene ethers of HLB 14.5 to 19 as HLB, and to use polyoxyalkylene (hardened) castor oil ethers of HLB 13 or more and less than 14.5 as the third emulsifier. In the combination of the above emulsifiers, the polyoxyalkylene (cured) castor oil ether is more preferably HLB 13-16. When the content of the antioxidant increases, it can be emulsified particularly effectively.
上記第一乳化剤、第二乳化剤、第三乳化剤を含む乳化剤のトータル添加量は、油脂に対して7〜60質量%であることが好ましい。より好ましくは15〜50質量%であり、さらに好ましくは15〜35質量%である。乳化剤のトータル添加量が7質量%以上であれば安定性が良好なエマルジョン液が得られやすい。また、乳化剤のトータル添加量が60質量%以下であれば、精練工程で泡が多く発生することを抑制し、精練異常になりにくい。 The total amount of the emulsifier including the first emulsifier, the second emulsifier, and the third emulsifier is preferably 7 to 60% by mass with respect to the fat and oil. More preferably, it is 15-50 mass%, More preferably, it is 15-35 mass%. If the total addition amount of the emulsifier is 7% by mass or more, an emulsion liquid having good stability is easily obtained. Moreover, if the total addition amount of an emulsifier is 60 mass% or less, generation | occurrence | production of many foams will be suppressed in a scouring process, and it will be hard to become abnormal scouring.
上記エマルジョン液におけるエマルジョンの平均粒子径は、0.02〜1μmであることが好ましい。より好ましい平均粒子径は、0.05〜0.8μm、さらに好ましくは0.08〜0.6μm、さらにより好ましくは0.1〜0.4μmであり、特には0.3μm未満であるとよい。平均粒子径が上記範囲内にあると、油脂が微分散され、微小領域を多数含むレーヨン繊維が得られるので、好ましい。平均粒子径は、乳化剤の組成、乳化剤の添加量及び乳化条件によりコントロールすることができる。また、上記エマルジョン液は、エマルジョンの粒子径が3μm以上の粒子が3%以下であることが好ましい。より好ましくは、1%以下であり、さらに好ましくは0.1%以下である。エマルジョンの粒子径が上記範囲内にあると、油脂が微分散され、微小領域を多数含むレーヨン繊維が得られるので、好ましい。本発明において、エマルジョンの粒子径及び平均粒子径は、光散乱法で測定・算出したものをいう。 The average particle size of the emulsion in the emulsion is preferably 0.02 to 1 μm. The more preferable average particle diameter is 0.05 to 0.8 μm, more preferably 0.08 to 0.6 μm, still more preferably 0.1 to 0.4 μm, and particularly preferably less than 0.3 μm. . When the average particle diameter is within the above range, oil and fat are finely dispersed, and rayon fibers including a large number of fine regions are obtained, which is preferable. The average particle size can be controlled by the composition of the emulsifier, the added amount of the emulsifier, and the emulsification conditions. The emulsion liquid preferably contains 3% or less of particles having an emulsion particle diameter of 3 μm or more. More preferably, it is 1% or less, More preferably, it is 0.1% or less. When the particle diameter of the emulsion is within the above range, oil and fat are finely dispersed, and rayon fibers containing a large number of fine regions are obtained, which is preferable. In the present invention, the particle diameter and average particle diameter of the emulsion are those measured and calculated by a light scattering method.
(紡糸条件)
紡糸液(ビスコース液)としては、セルロースが7〜10質量%、水酸化ナトリウムが5〜8質量%、二硫化炭素が2〜3.5質量%のビスコース原液を調製して用いるとよい。このとき、必要に応じて、エチレンジアミン四酢酸(EDTA)、二酸化チタン等の添加剤を使用することもできる。紡糸液(ビスコース液)の温度は19〜23℃に保持するのが好ましい。上記セルロースを含むビスコース原液に、上記で得られたエマルジョン液を混合して紡糸用ビスコース液(油脂含有用レーヨン繊維紡糸用ビスコース液)を調製する。
(Spinning conditions)
As the spinning solution (viscose solution), a viscose stock solution containing 7 to 10% by mass of cellulose, 5 to 8% by mass of sodium hydroxide, and 2 to 3.5% by mass of carbon disulfide may be prepared and used. . At this time, additives such as ethylenediaminetetraacetic acid (EDTA) and titanium dioxide can be used as necessary. The temperature of the spinning solution (viscose solution) is preferably maintained at 19 to 23 ° C. The emulsion solution obtained above is mixed with the viscose stock solution containing cellulose to prepare a spinning viscose solution (oil-containing rayon fiber spinning viscose solution).
上記油脂の添加量は、セルロースに対して0.5〜15質量%の範囲が好ましい。より好ましくは、0.8〜14質量%であり、さらに好ましくは1〜10質量%の範囲である。上記範囲であれば、皮膚の乾燥、老化防止、オレイン酸による角質層保護、乾燥肌改善、リノール酸による新陳代謝促進、リノレン酸による皮膚の細胞機能正常化等の効果を期待できる。 The addition amount of the fat is preferably in the range of 0.5 to 15% by mass with respect to cellulose. More preferably, it is 0.8-14 mass%, More preferably, it is the range of 1-10 mass%. If it is the said range, effects, such as drying of skin, prevention of aging, stratum corneum protection by oleic acid, improvement of dry skin, promotion of metabolism by linoleic acid, normalization of skin cell function by linolenic acid, can be expected.
紡糸浴(ミューラー浴)は、例えば、硫酸を95〜130g/リットル、硫酸亜鉛を10〜17g/リットル、硫酸ナトリウムを290〜370g/リットル含み、温度が45〜60℃であることが好ましい。より好ましい硫酸濃度は、100〜120g/リットルである。紡糸ノズルとしては、例えば、通常の円形ノズルを用いることができる。紡糸ノズルの選定は、目的とする生産量にもよるが、直径0.05〜0.12mmの円形ノズルを1000〜20000ホール有するものが好ましい。 The spinning bath (Mueller bath) preferably contains 95 to 130 g / liter of sulfuric acid, 10 to 17 g / liter of zinc sulfate, 290 to 370 g / liter of sodium sulfate, and preferably has a temperature of 45 to 60 ° C. A more preferable sulfuric acid concentration is 100 to 120 g / liter. As the spinning nozzle, for example, a normal circular nozzle can be used. The selection of the spinning nozzle depends on the target production amount, but preferably has a circular nozzle having a diameter of 0.05 to 0.12 mm and 1000 to 20000 holes.
上記紡糸ノズルを用いて、上記で得られた紡糸用ビスコース液を紡糸浴中に押し出して紡糸し、凝固再生させる。紡糸速度は35〜70m/分の範囲が好ましい。また、延伸率は39〜50%が好ましい。ここで延伸率とは、延伸前の長さを100%としたとき、延伸後の長さが何%伸びたかを示すものである。倍率で示すと、延伸前が1、延伸後は1.39〜1.50倍となる。 Using the spinning nozzle, the spinning viscose solution obtained above is extruded into a spinning bath, spun, and coagulated and regenerated. The spinning speed is preferably in the range of 35 to 70 m / min. Further, the stretching ratio is preferably 39 to 50%. Here, the stretch ratio indicates how many percent the stretched length is increased when the stretched length is 100%. In terms of magnification, the ratio is 1 before stretching and 1.39 to 1.50 after stretching.
上記のようにして得られたレーヨン繊維糸条を所定の長さにカットし、精練処理を行う。精練工程は、通常の方法で、熱水処理、水硫化処理、漂白、酸洗い及び油剤付与の順で行うとよい。 The rayon fiber yarn obtained as described above is cut into a predetermined length and subjected to a scouring treatment. The scouring step is preferably performed in the order of hot water treatment, hydrosulfurization treatment, bleaching, pickling, and oil application.
その後、必要に応じて圧縮ローラーや真空吸引等の方法で余分な油剤、水分を繊維から除去した後、乾燥処理を施して本発明の油脂含有レーヨン繊維を得ることができる。 Then, after removing excess oil agent and water | moisture content from a fiber by methods, such as a compression roller and a vacuum suction, as needed, it can dry-process and can obtain the fat-containing rayon fiber of this invention.
本発明の油脂含有レーヨン繊維は、繊度が0.3〜6.0dtexであることが好ましい。より好ましくは0.6〜4.0dtexであり、さらに好ましくは0.9〜3.3dtexである。繊度が0.3dtex未満であると、延伸時の単繊維切れが発生しやすい傾向にある。繊度が6.0dtexを越えると、衣料用途には使いにくい恐れがある。 The oil-containing rayon fiber of the present invention preferably has a fineness of 0.3 to 6.0 dtex. More preferably, it is 0.6-4.0 dtex, More preferably, it is 0.9-3.3 dtex. If the fineness is less than 0.3 dtex, single fiber breakage tends to occur during stretching. If the fineness exceeds 6.0 dtex, it may be difficult to use for clothing.
本発明の油脂含有レーヨン繊維は、長繊維状(例えば、トウ、フィラメント、不織布等)、短繊維状(例えば、湿式抄紙用原綿、エアレイド不織布用原綿、カード用原綿等)の形態で提供され、繊維構造物を形成することが好ましい。上記繊維構造物としては、例えば、トウ、フィラメント、紡績糸、中綿(詰め綿)、紙、不織布、織物、編物が好ましく、紡績糸、編物、織物及び不織布からなる群から選ばれる一種であることがより好ましい。 The fat and oil-containing rayon fiber of the present invention is provided in the form of long fibers (for example, tow, filament, nonwoven fabric, etc.), short fibers (for example, raw paper for wet papermaking, raw cotton for airlaid nonwoven fabric, raw cotton for cards, etc.) It is preferable to form a fiber structure. The fiber structure is preferably, for example, tow, filament, spun yarn, batting (padded cotton), paper, non-woven fabric, woven fabric, or knitted fabric, and is a kind selected from the group consisting of spun yarn, knitted fabric, woven fabric, and non-woven fabric. Is more preferable.
本発明の繊維構造物は、上記レーヨン繊維が油脂を含むため、風合いが良好である。かかる風合いを詳細に説明すると、本発明の油脂含有レーヨン繊維を用いると、従来のレーヨン繊維に比べて繊維構造物にしたときに表面にヌメリ感があり、且つソフトな風合いが発現するので、肌に優しい風合いで商品に格段の高級感効果が発揮できる(以下において、風合い効果とも記す。)。また、本発明の油脂含有レーヨン繊維では油脂を繊維内に練り込んでいるので、本発明の風合い効果は、従来の繊維構造物の最終仕上げの段階で柔軟剤を付与する、いわゆる後加工仕上げと比較して抜群の洗濯耐久性を有する。 The fiber structure of the present invention has a good texture because the rayon fiber contains fats and oils. This texture will be described in detail. When the oil-containing rayon fiber of the present invention is used, the surface has a slimy feeling and a soft texture is expressed when it is made into a fiber structure as compared with the conventional rayon fiber. The product has a gentle texture and can produce a very high-class effect on the product (hereinafter also referred to as the texture effect). In addition, since the fat and oil-containing rayon fiber of the present invention is kneaded with fats and oils in the fiber, the texture effect of the present invention is a so-called post-processing finish that imparts a softener at the final finishing stage of a conventional fiber structure. Compared with outstanding washing durability.
本発明の繊維構造物として、例えば、紡績糸とした場合、上記油脂含有レーヨン繊維単独、又はその他の再生セルロース繊維、コットン、麻、ウール、アクリル、ポリエステル、ポリアミド、ポリオレフィン、ポリウレタン等の他の繊維と混紡、複合することが好ましい。このような紡績糸は、例えば織物や編物に加工されて衣料等に用いることができる。 As the fiber structure of the present invention, for example, in the case of a spun yarn, the above oil-containing rayon fiber alone or other regenerated cellulose fibers, cotton, hemp, wool, acrylic, polyester, polyamide, polyolefin, polyurethane, and other fibers It is preferable to be blended with and mixed with. Such spun yarn can be processed into a woven fabric or a knitted fabric and used for clothing or the like.
本発明の繊維構造物として、織物や編物とした場合、織物や編物の組織は特に限定されない。例えば、編物では、丸編み、横編み、経編み(トリコット)が、織物では、平織、綾織、繻子織が、本発明の風合い効果がよく発揮できることから好ましい繊維構造物の形態である。 When the fiber structure of the present invention is a woven fabric or a knitted fabric, the structure of the woven fabric or the knitted fabric is not particularly limited. For example, circular knitting, weft knitting, and warp knitting (tricot) are preferable for knitting, and plain weaving, twill weaving, and satin weaving are preferable forms of the fiber structure because the texture effect of the present invention can be exhibited well.
本発明の繊維構造物として、例えば、不織布とした場合、上記油脂含有レーヨン繊維単独、又はその他の再生セルロース繊維、コットン、麻、ウール、アクリル、ポリエステル、ポリアミド、ポリオレフィン、ポリウレタン等の他の繊維と混綿して用いることができる。不織布の形態としては、例えば、湿式不織布(湿式抄紙)、エアレイド不織布、水流交絡不織布、ニードルパンチ不織布等が挙げられる。このような不織布は、例えば、ウェットティッシュ、対人・対物用ワイパー等のウェットシート、水解シート等に用いることができる。また、化粧パフ、吸収体等の衛生シートに用いることができる。 As the fiber structure of the present invention, for example, when it is a non-woven fabric, the above oil and fat-containing rayon fiber alone or other regenerated cellulose fibers, cotton, hemp, wool, acrylic, polyester, polyamide, polyolefin, polyurethane and other fibers Can be used after blending. Examples of the form of the nonwoven fabric include a wet nonwoven fabric (wet papermaking), an airlaid nonwoven fabric, a hydroentangled nonwoven fabric, and a needle punched nonwoven fabric. Such a nonwoven fabric can be used, for example, for wet tissues, wet sheets such as interpersonal / objective wipers, hydrolytic sheets, and the like. Moreover, it can be used for sanitary sheets such as cosmetic puffs and absorbent bodies.
本発明の繊維構造物において、他の繊維と混用する場合は、上記油脂含有レーヨン繊維は10質量%以上含有させることが好ましい。より好ましくは15質量%以上、さらに好ましくは20質量%以上、特に好ましくは30質量%以上である。混用する場合の油脂含有レーヨン繊維の含有量の上限は、90質量%であることが好ましい。油脂含有レーヨン繊維が10質量%未満の場合は、上述したソフトな風合いが得られにくくなる傾向にある。また、90質量%を超える場合は、レーヨン繊維の比率が多くなるため、上述した風合い効果に加えて、吸湿性、放湿性、吸湿発熱性、及びドレープ性が高いが、レーヨン繊維本来の低強度、低乾燥性(乾きにくい)、保温性が低い、低ストレッチ性となる傾向にあり、かかる性能を補うには、他の繊維と複合することが好ましい。 In the fiber structure of the present invention, when mixed with other fibers, the oil-and-fat-containing rayon fibers are preferably contained in an amount of 10% by mass or more. More preferably, it is 15 mass% or more, More preferably, it is 20 mass% or more, Most preferably, it is 30 mass% or more. The upper limit of the content of the oil-and-fat-containing rayon fiber when mixed is preferably 90% by mass. When the oil and fat-containing rayon fiber is less than 10% by mass, the above-mentioned soft texture tends to be hardly obtained. In addition, when it exceeds 90% by mass, the ratio of the rayon fiber increases, so in addition to the above-mentioned hand effect, the moisture absorption, moisture release, moisture absorption heat generation, and drape properties are high, but the inherent low strength of rayon fiber. It tends to be low dryness (hard to dry), low heat retention, and low stretchability. To supplement such performance, it is preferably combined with other fibers.
上記油脂含有レーヨン繊維に複合する他の繊維は、目的に応じて適宜選択することができ、特に限定されない。例えば、強度を向上させるにはポリエステル繊維を複合することが好ましく、上記油脂含有レーヨン短繊維とポリエステル繊維を混紡する方法、あるいは上記油脂含有レーヨン繊維とポリエステル繊維を長繊維同士で合撚、交編、交織することで複合することが好ましい。また、汗や洗濯の低乾燥性改善にはポリエステル繊維を複合することが好ましい。保温性改善には、ポリアクリル繊維が好ましい。低ストレッチ性改善には、ポリウレタン系弾性繊維が好ましい。発色性アップや屈曲強度改善には、ポリアミド繊維が好ましい。また、コットン(綿)の硬い風合いを改善することやウールの暖かさを加味できるので、かかる繊維を用途、要求に合わせてそれぞれ複合することが好ましい。 Other fibers combined with the oil-and-fat-containing rayon fiber can be appropriately selected according to the purpose, and are not particularly limited. For example, in order to improve the strength, it is preferable to combine polyester fibers, the method of blending the fat-containing rayon short fibers and the polyester fibers, or the oil-containing rayon fibers and the polyester fibers are twisted and knitted together with the long fibers. It is preferable to make a composite by interweaving. Moreover, it is preferable to combine a polyester fiber in order to improve the low drying property of sweat or laundry. For improving heat retention, polyacrylic fibers are preferred. For improving the low stretchability, polyurethane elastic fibers are preferred. Polyamide fibers are preferred for improving color development and improving flexural strength. Further, since the hard texture of cotton can be improved and the warmth of wool can be taken into account, it is preferable to combine such fibers in accordance with the application and requirements.
本発明の油脂含有レーヨン繊維を使用形態は、混率20〜50質量%で他の繊維との混紡が好ましく用いられ、特にニット(編地)あるいは織布に加工して用いると、アウター衣料においては風合いが良好であり、ボトム、インナー衣料、靴下等においては保湿性、風合いが良好である。 The use form of the fat and oil-containing rayon fiber of the present invention is preferably mixed with other fibers at a blending ratio of 20 to 50% by mass. Especially when processed into a knit (knitted fabric) or woven fabric, it is used in outer clothing. The texture is good, and the bottom, inner garment, socks, etc. have good moisture retention and texture.
以下、実施例により本発明をさらに具体的に説明する。本発明は、下記の実施例に限定されるものではない。なお、下記の実施例で添加量を単に%と表記した場合は、質量%を意味する。 Hereinafter, the present invention will be described more specifically with reference to examples. The present invention is not limited to the following examples. In addition, when the addition amount is simply expressed as% in the following examples, it means mass%.
まず、測定方法について説明する。 First, the measurement method will be described.
(融点)
示差走査熱量分析計(DSC)を使用し、フローガスとして窒素ガスを30ml/min速度で流し、−68℃から20℃まで昇温速度5℃/分で測定し、吸熱開始前の直線部延長線と吸熱中の直線部延長線の交点の温度を融点(℃)として求めた。
(Melting point)
Using a differential scanning calorimeter (DSC), flow nitrogen gas as a flow gas at a rate of 30 ml / min, measure from -68 ° C to 20 ° C at a rate of temperature increase of 5 ° C / min, and extend the straight line before starting the endotherm The temperature at the intersection of the line and the straight line extension line during endotherm was determined as the melting point (° C).
(平均粒子径)
エマルジョン液の平均粒子径は、(株)堀場製作所製のレーザー回折/散乱式粒子分布測定装置LA−950V2を使用し、測定した。
(Average particle size)
The average particle size of the emulsion was measured using a laser diffraction / scattering particle distribution measuring apparatus LA-950V2 manufactured by Horiba, Ltd.
(低温貯蔵安定性)
エマルジョン液の低温安定性を以下の方法で評価した。エマルジョン液10mlをガラス容器に入れ、−5℃の恒温槽内で16時間静置した後、手で上下方向に10秒程度の強振を行なった際の乳化状態を確認し、以下評価基準に従って低温安定性の判定を行った。
[評価基準]
良好: 強振後も液状で、さらに凝集物も確認されない
可: 強振後も液状であるが、凝集物が確認された
不可: 固化もしくは分離する
(Low temperature storage stability)
The low temperature stability of the emulsion was evaluated by the following method. 10ml of the emulsion is put in a glass container and left in a thermostatic bath at -5 ° C for 16 hours, and then the emulsified state is confirmed by shaking for about 10 seconds in the vertical direction by hand. Judgment of stability was performed.
[Evaluation criteria]
Good: Liquid after strong shaking and no agglomerates observed. Possible: Liquid after strong shaking but no agglomerates confirmed. Solidified or separated.
(ヨウ素価)
絶乾綿100gあたりに反応するヨウ素量をヨウ素価[I2(mg)/綿(100g)]として、以下の手順により測定した。
(1)試料原綿の水分率を測定する。
(2)油脂量としておよそ0.1gとなるように原綿試料を精秤し、三角フラスコに入れる。
(3)シクロヘキサン20mlを加えて撹拌し、さらにウィス試薬(一塩化ヨウ素の酢酸水溶液)10mlとイオン交換水20mlを加える。
(4)ときどき撹拌しつつ、30分間常温暗所にて静置する。
(5)10質量%のヨウ化カリウム溶液20mlと、イオン交換水20mlを加えた後、0.1Nのチオ硫酸ナトリウムで滴定する。
(6)液の色が薄くなってきたらデンプン指示薬を加えて滴定を続け、デンプン指示薬の呈色が消失した時の0.1Nのチオ硫酸ナトリウム滴定量を終点として読み取る。
(7)試料を入れずに同様の試験を行い、空試験とする。
(8)次式によりヨウ素価を算出する。
繊維のヨウ素価[I2(mg)/綿(100g)]=(空試験滴定量−滴定量)×絶乾綿質量
(Iodine number)
The amount of iodine reacted per 100 g of absolutely dry cotton was measured as the iodine value [I 2 (mg) / cotton (100 g)] according to the following procedure.
(1) The moisture content of the sample raw cotton is measured.
(2) A raw cotton sample is precisely weighed so that the amount of oil and fat is about 0.1 g, and placed in an Erlenmeyer flask.
(3) Add 20 ml of cyclohexane and stir, and further add 10 ml of Wis reagent (iodine aqueous solution of iodine monochloride) and 20 ml of ion-exchanged water.
(4) Leave at room temperature in a dark place for 30 minutes with occasional stirring.
(5) After adding 20 ml of 10% by mass potassium iodide solution and 20 ml of ion-exchanged water, titration is performed with 0.1 N sodium thiosulfate.
(6) When the color of the solution becomes lighter, the starch indicator is added and the titration is continued, and 0.1N sodium thiosulfate titration when the color of the starch indicator disappears is read as the end point.
(7) Do the same test without putting a sample, and make a blank test.
(8) The iodine value is calculated by the following formula.
Iodine value of fiber [I 2 (mg) / cotton (100 g)] = (blank test titration-titration) × absolute dry cotton mass
(繊維の繊度)
繊維の繊度を、JIS L 1015に準じて測定した。
(Fine fineness)
The fineness of the fiber was measured according to JIS L 1015.
(繊維の強度及び伸度)
繊維の強度(乾強度、湿強度)及び伸度(乾伸度及び湿伸度)を、JIS L 1015に準じて測定した。
(Fiber strength and elongation)
The strength (dry strength, wet strength) and elongation (dry elongation and wet elongation) of the fiber were measured according to JIS L 1015.
(促進試験)
原綿を70℃、70%RH(恒温恒湿器、ヤマト科学(株)社製の“IG420”型)の環境下で20日間放置した後に繊維強度を測定、処理前後の比較により繊維の経時促進状態の評価を行った。
(Accelerated test)
Fiber strength is measured after leaving raw cotton in an environment of 70 ° C. and 70% RH (constant temperature and humidity chamber, “IG420” manufactured by Yamato Scientific Co., Ltd.) for 20 days, and fiber aging is accelerated by comparing before and after treatment. The state was evaluated.
(洗濯耐久性)
繊維を中性洗剤(繊維製品新機能評価協議会標準洗剤)及びアルカリ洗剤を使用してそれぞれ5回洗濯、10回洗濯を行った後、ヨウ素価を測定した。洗濯試験はJIS L 0217 103法に準じて実施した。
(Washing durability)
The fibers were washed 5 times and 10 times respectively using a neutral detergent (textile product new function evaluation council standard detergent) and an alkaline detergent, and then the iodine value was measured. The washing test was conducted according to JIS L 0217 103 method.
(脱油処理後のレーヨン繊維における空隙部の平均孔径)
脱油処理後の繊維の断面写真(走査型電子顕微鏡写真、倍率3000倍)を用いて、脱油処理後のレーヨン繊維における空隙部の平均孔径を測定した。具体的には、脱油処理後の繊維の断面写真(走査型電子顕微鏡写真、倍率3000倍)を画像処理により倍率9010倍に拡大し、印刷した紙面上から任意の繊維の断面をサンプリングし、その断面上の空隙部の直径を計測し、計測した100個の空隙部の直径を平均して空隙部の平均孔径とした。なお、楕円状の空隙は長径及び短径を計測して算出した面積から真円直径に換算し、空隙部の直径とした。
[脱油処理]
(I)試料約2.3gを精秤し、底部に小さい穴の空いた試料管に詰めた。
(II)底部の穴を塞ぎ、抽出溶媒としてメタノール10mlを試料管に注加し、一定時間静置し浸透させてからプレス装置によりメタノール処理液を抽出した。
(III)同じ試料を使用して上記の操作(II)による抽出を20回繰り返した後、試料管から取り出した試料を水洗し、105℃、2時間で乾燥して脱油処理後の繊維を得た。
(Average pore diameter of voids in rayon fiber after deoiling treatment)
The average pore diameter of the voids in the rayon fiber after deoiling treatment was measured using a cross-sectional photograph of the fiber after deoiling treatment (scanning electron micrograph, magnification 3000 times). Specifically, the cross-sectional photograph of the fiber after deoiling treatment (scanning electron micrograph, magnification 3000 times) is magnified to a magnification of 9010 by image processing, and the cross-section of any fiber is sampled from the printed paper, The diameter of the voids on the cross section was measured, and the average diameter of the 100 measured voids was used as the average pore diameter of the voids. In addition, the elliptical space | gap was converted into the perfect circle diameter from the area calculated by measuring the long diameter and the short diameter, and it was set as the diameter of the space | gap part.
[Deoiling treatment]
(I) About 2.3 g of a sample was precisely weighed and packed in a sample tube having a small hole at the bottom.
(II) The bottom hole was closed, 10 ml of methanol was poured into the sample tube as an extraction solvent, allowed to stand for a certain period of time and permeated, and then the methanol treatment liquid was extracted with a press device.
(III) Using the same sample, the extraction by the above operation (II) was repeated 20 times, and then the sample taken out from the sample tube was washed with water, dried at 105 ° C. for 2 hours, and the fiber after deoiling treatment Obtained.
(製造例1〜13)
[エマルジョン液の調製]
油脂として下記表1に示す脂肪酸組成を有し、且つ融点が−11.6℃である精製椿油(五島産)又は脂肪酸組成としてリノール酸を主成分とし、且つ20℃において液体である大豆油を用い、乳化剤として下記表2〜表3に示す乳化剤を用い、下記表2〜表3に示す配合割合で油脂と乳化剤を混合して、製造例1〜13のエマルジョン液を調製した。酸化防止剤として、天然トコフェロールを50質量%含む液体を用いた。
(Production Examples 1 to 13)
[Preparation of emulsion]
Refined bran oil (from Goto) having a fatty acid composition shown in Table 1 below as fat and oil and having a melting point of -11.6 ° C, or soybean oil having linoleic acid as a main component and fatty acid composition at 20 ° C as a fatty acid composition Using the emulsifiers shown in Tables 2 to 3 below as emulsifiers, the fats and oils and the emulsifiers were mixed at the blending ratios shown in Tables 2 to 3 below to prepare emulsion liquids of Production Examples 1 to 13. As an antioxidant, a liquid containing 50% by mass of natural tocopherol was used.
上記表2〜表3のとおり、製造例1〜10では、乳化剤として、HLBが14.5〜19の第一乳化剤とHLBが6〜12.5の第二乳化剤を併用することにより、平均粒子径が1μm以下と小さく、微分散されているエマルジョン液を調製することができた。一方、第二乳化剤を含んでいない製造例11のエマルジョン液は、低温安定性が悪かった。また、第一乳化剤を含んでいない製造例12及び製造例13の場合は、乳化不良の状態となり、微分散されているエマルジョン液を調製することができなかった。 As shown in Tables 2 to 3, in Production Examples 1 to 10, the average particle is obtained by using a first emulsifier having an HLB of 14.5 to 19 and a second emulsifier having an HLB of 6 to 12.5 as an emulsifier. A finely dispersed emulsion liquid having a diameter as small as 1 μm or less could be prepared. On the other hand, the emulsion liquid of Production Example 11 containing no second emulsifier had poor low-temperature stability. Moreover, in the case of the manufacture example 12 and the manufacture example 13 which do not contain the 1st emulsifier, it became the state of emulsification failure and the emulsion liquid finely dispersed was not able to be prepared.
(実施例1)
<紡糸用ビスコース液の調製>
製造例1で調製したエマルジョン液を、油脂含有量がセルロースに対して3質量%になるように、原料ビスコースへ添加し、混合機にて攪拌混合を行い、紡糸用ビスコース液を調製した。温度は20℃に保った。原料ビスコースとしては、セルロース8.5質量%、水酸化ナトリウム5.7質量%、二硫化炭素2.7質量%を含むビスコース原液を用いた。
Example 1
<Preparation of spinning viscose liquid>
The emulsion liquid prepared in Production Example 1 was added to the raw material viscose so that the fat content was 3% by mass with respect to cellulose, and stirred and mixed in a mixer to prepare a spinning viscose liquid. . The temperature was kept at 20 ° C. As the raw material viscose, a viscose stock solution containing 8.5% by mass of cellulose, 5.7% by mass of sodium hydroxide, and 2.7% by mass of carbon disulfide was used.
<紡糸条件>
得られた紡糸用ビスコース液を、2浴緊張紡糸法により、紡糸速度60m/分、延伸率50%で紡糸して、繊度が約1.4dtexの椿油含有レーヨン繊維を得た。紡糸浴としては、硫酸100g/L、硫酸亜鉛15g/L、硫酸ナトリウム350g/L含むミューラー浴(50℃)を用いた。また、ビスコースを吐出する紡糸口金には、孔径0.06mmのホールを4000個有する円形ノズルを用いた。紡糸中、単糸切れ等の不都合は生じず、混合ビスコースの紡糸性は良好であった。
<Spinning conditions>
The obtained viscose liquid for spinning was spun at a spinning speed of 60 m / min and a draw ratio of 50% by a two-bath tension spinning method to obtain a cocoon oil-containing rayon fiber having a fineness of about 1.4 dtex. As the spinning bath, a Mueller bath (50 ° C.) containing 100 g / L of sulfuric acid, 15 g / L of zinc sulfate, and 350 g / L of sodium sulfate was used. In addition, a circular nozzle having 4000 holes having a hole diameter of 0.06 mm was used as a spinneret for discharging viscose. During spinning, there was no inconvenience such as single yarn breakage, and the spinnability of the mixed viscose was good.
<精練条件>
上記で得られたビスコースレーヨンの糸条を、繊維長38mmにカットし、精練処理を行った。精練工程では、熱水処理後に水洗を行い、油剤を付与した後圧縮ローラーで余分な水分と油剤を繊維から落とし、その後、乾燥処理(60℃、7時間)を施して、実施例1の油脂含有レーヨン繊維を得た。
<Scouring conditions>
The viscose rayon yarn obtained above was cut into a fiber length of 38 mm and scoured. In the scouring step, after washing with hot water, washing with water, applying an oil agent, dropping excess moisture and oil agent from the fiber with a compression roller, and then performing a drying treatment (60 ° C., 7 hours), the fat and oil of Example 1 A contained rayon fiber was obtained.
(実施例2〜4)
製造例2〜4で得られたエマルジョン液を、それぞれ油脂含有量がセルロースに対して3質量%になるように、原料ビスコースへ添加した以外は実施例1と同様にして、実施例2〜4の油脂含有レーヨン繊維を得た。
(Examples 2 to 4)
In the same manner as in Example 1, except that the emulsion liquids obtained in Production Examples 2 to 4 were added to the raw material viscose so that the oil content was 3% by mass with respect to cellulose, respectively. 4 oil and fat-containing rayon fibers were obtained.
(実施例5)
製造例4で得られたエマルジョン液を、油脂含有量がセルロースに対して1.5質量%になるように、原料ビスコースへ添加した以外は実施例1と同様にして、実施例5の油脂含有レーヨン繊維を得た。
(Example 5)
The fats and oils of Example 5 were obtained in the same manner as in Example 1 except that the emulsion liquid obtained in Production Example 4 was added to the raw material viscose so that the fat and oil content was 1.5% by mass with respect to cellulose. A contained rayon fiber was obtained.
(実施例6)
製造例5で得られたエマルジョン液を、油脂含有量がセルロースに対して3.0質量%になるように、原料ビスコースへ添加した以外は実施例1と同様にして、実施例6の油脂含有レーヨン繊維を得た。
(Example 6)
The fats and oils of Example 6 were obtained in the same manner as in Example 1 except that the emulsion liquid obtained in Production Example 5 was added to the raw material viscose so that the fat and oil content was 3.0% by mass with respect to cellulose. A contained rayon fiber was obtained.
(実施例7)
製造例10で得られたエマルジョン液を、油脂含有量がセルロースに対して3.0質量%になるように、原料ビスコースへ添加した以外は実施例1と同様にして、実施例7の油脂含有レーヨン繊維を得た。
(Example 7)
The fats and oils of Example 7 were obtained in the same manner as in Example 1 except that the emulsion liquid obtained in Production Example 10 was added to the raw material viscose so that the fat and oil content was 3.0% by mass with respect to cellulose. A contained rayon fiber was obtained.
(参考例1)
参考例1として、レギュラーレーヨン(ダイワボウレーヨン株式会社製)を用いた。
(Reference Example 1)
As Reference Example 1, regular rayon (manufactured by Daiwabo Rayon Co., Ltd.) was used.
実施例1〜7と参考例1のレーヨン繊維の繊度、乾強度、湿強度、乾伸度及び湿伸度を上記のように測定し、その結果を下記表4に示した。また、実施例1〜7と参考例1のレーヨン繊維のヨウ素価を測定し、その結果を下記表4に示した。また、実施例1、4及び5と参考例1のレーヨン繊維を用いて促進試験を行い、その結果を下記表4に示した。また、実施例5のレーヨン繊維の洗濯耐久性を評価し、その結果を下記表4に示した。 The fineness, dry strength, wet strength, dry elongation and wet elongation of the rayon fibers of Examples 1 to 7 and Reference Example 1 were measured as described above, and the results are shown in Table 4 below. Moreover, the iodine value of the rayon fiber of Examples 1-7 and Reference Example 1 was measured, and the results are shown in Table 4 below. Further, accelerated tests were conducted using the rayon fibers of Examples 1, 4 and 5 and Reference Example 1, and the results are shown in Table 4 below. Moreover, the washing durability of the rayon fiber of Example 5 was evaluated, and the results are shown in Table 4 below.
表4から分かるように、促進試験による実施例の油脂含有レーヨン繊維の繊維強度低下率は、レギュラーレーヨンよりも低かった。この結果から、実施例の油脂含有レーヨン繊維において、油脂は酸化安定性が良好な状態でレーヨン繊維を構成するセルロース内に微分散していることが分かる。また、中性洗剤で5回洗濯した場合、中性洗剤で10回洗濯した場合、アルカリ洗剤で5回洗濯した場合、アルカリ洗剤で10回洗濯した場合のいずれの洗濯試験でも、実施例の油脂含有レーヨン繊維のヨウ素価は変化しないことから、洗濯しても油脂は脱落せずセルロース中に存在している、即ち実施例の油脂含有レーヨン繊維は洗濯耐久性に優れることが確認できた。 As can be seen from Table 4, the fiber strength-decreasing rate of the oil-and-fat-containing rayon fiber of the example by the acceleration test was lower than that of the regular rayon. From this result, it can be seen that in the oil-containing rayon fibers of the examples, the oils and fats are finely dispersed in the cellulose constituting the rayon fibers with good oxidation stability. In addition, when the laundry was washed 5 times with a neutral detergent, washed 10 times with a neutral detergent, washed 5 times with an alkaline detergent, or washed 10 times with an alkaline detergent, the fats and oils of the examples were used. Since the iodine value of the contained rayon fibers did not change, it was confirmed that the fats and oils did not fall off even after washing and existed in the cellulose, that is, the fat and oil-containing rayon fibers of the examples were excellent in washing durability.
また、実施例4のレーヨン繊維を脱油処理した後、走査型電子顕微鏡(日立製作所社製「S−3500N」)で観察し、顕微鏡観察結果を図1に示した。図1Aは、脱油処理後の実施例4のレーヨン繊維における繊維断面の走査型電子顕微鏡写真である(倍率3000倍)。図1Bは、図1Aの顕微鏡観察結果を画像処理により倍率が9010倍になるように部分的拡大した画像である。図1及び2の繊維断面の顕微鏡写真において、繊維断面内の島部分は空隙部であり、この空隙部内部に微分散した油脂が存在していたと考えられる。即ち、脱油処理後の上記レーヨン繊維の繊維断面における空隙部は、微分酸していた油脂が脱油により抜けた後の微小領域部分である。図1A−Bからレーヨン繊維内のセルロースと油脂とは非相溶状態で、且つ上記油脂は上記セルロース中に微分散されていることが分かった。そして、実施例4の繊維について、図1Bの画像を用いて100個の空隙部の孔径を測定したところ、平均孔径は0.14μmであった。また、実施例5のレーヨン繊維についても、同様に測定したところ、繊維断面における空隙部の平均孔径は0.15μmであった。 Moreover, after deoiling the rayon fiber of Example 4, it observed with the scanning electron microscope ("S-3500N" by Hitachi, Ltd.), and the microscope observation result was shown in FIG. FIG. 1A is a scanning electron micrograph of the fiber cross section of the rayon fiber of Example 4 after deoiling treatment (magnification 3000 times). FIG. 1B is an image obtained by partially enlarging the microscope observation result of FIG. 1A by image processing so that the magnification is 9010 times. In the micrographs of the fiber cross section of FIGS. 1 and 2, the island portion in the fiber cross section is a void, and it is considered that finely dispersed oil and fat existed in the void. That is, the void portion in the fiber cross section of the rayon fiber after the deoiling treatment is a minute region portion after the oil and fat that have been differentiated acid are removed by deoiling. From FIG. 1A-B, it was found that the cellulose and the fats and oils in the rayon fiber were in an incompatible state, and the fats and oils were finely dispersed in the cellulose. And about the fiber of Example 4, when the hole diameter of 100 space | gap parts was measured using the image of FIG. 1B, the average hole diameter was 0.14 micrometer. Moreover, when the rayon fiber of Example 5 was also measured in the same manner, the average pore diameter of the voids in the fiber cross section was 0.15 μm.
また、実施例1〜7の油脂含有レーヨン繊維の風合いを官能(触感)試験で評価したところ、ヌメリ感がありソフトな風合いであった。 Moreover, when the texture of the fat and oil-containing rayon fibers of Examples 1 to 7 was evaluated by a sensory (tactile feeling) test, the texture was soft and soft.
本発明の油脂含有レーヨン繊維は、例えば、紡績糸、編物、織物、不織布、トウ、フィラメント、中綿(詰め綿)、紙等の繊維構造物に用いることができる。また、本発明の繊維構造物は、衣料、化粧パフ、吸収体等の衛生材料、ウェットティッシュ、対人・対物ワイパー等のウェットシート、水解性シート、ドライワイパー、フィルター等に用いることができる。 The oil and fat-containing rayon fiber of the present invention can be used for fiber structures such as spun yarn, knitted fabric, woven fabric, non-woven fabric, tow, filament, batting (padded cotton), paper and the like. Further, the fiber structure of the present invention can be used for clothes, cosmetic puffs, hygiene materials such as absorbent bodies, wet tissues, wet sheets such as interpersonal / objective wipers, water-degradable sheets, dry wipers, filters, and the like.
Claims (10)
前記油脂は、脂肪酸及びそのグリセリンエステルから選ばれる少なくとも一つの脂肪酸成分を含み、且つ20℃において液体であり(ただし、こめ油を除く)、
前記油脂において、リノレン酸の含有量は1質量%以下であり、
前記酸化防止剤は、天然トコフェロールであり、
前記レーヨン繊維内のセルロースと前記油脂とは非相溶状態で、且つ前記油脂は前記セルロース中に微分散されており、
前記レーヨン繊維内の前記油脂を含有する粒子の平均粒子径が0.02〜0.8μmであることを特徴とする油脂含有レーヨン繊維。 It is a fat and oil-containing rayon fiber containing fat and antioxidant in the rayon fiber,
The fats and oils include at least one fatty acid component selected from fatty acids and glycerin esters thereof, and are liquid at 20 ° C. (except koji oil),
In the oil and fat, the content of linolenic acid is 1% by mass or less,
The antioxidant is natural tocopherol,
The cellulose and the fat / oil in the rayon fiber are in an incompatible state, and the fat / oil is finely dispersed in the cellulose,
Fat-containing rayon fibers having an average particle size of particles containing pre SL oil in said rayon fiber is characterized in that it is a 0.02~0.8Myuemu.
脂肪酸及びそのグリセリンエステルから選ばれる少なくとも一つの脂肪酸成分を含み、且つ20℃において液体である油脂(ただし、こめ油を除く)に、酸化防止剤と、HLBが14.5〜19である乳化剤と、HLBが6〜12.5である乳化剤とを加えて、平均粒子径が0.02〜1μmのエマルジョン液を調製し、前記油脂において、リノレン酸の含有量は1質量%以下であり、前記酸化防止剤は、天然トコフェロールであり、
セルロースを含むビスコース原液に、前記エマルジョン液を混合して紡糸用ビスコース液を調製し、
前記紡糸用ビスコース液をノズルより押し出して紡糸し、凝固再生することを特徴とする油脂含有レーヨン繊維の製造方法。 It is a manufacturing method of oil and fat content rayon fiber given in any 1 paragraph of Claims 1-4,
Fats and oils (however, except koji oil) containing at least one fatty acid component selected from fatty acids and glycerin esters thereof and being liquid at 20 ° C., an antioxidant, and an emulsifier having an HLB of 14.5 to 19 And an emulsifier having an HLB of 6 to 12.5 to prepare an emulsion having an average particle size of 0.02 to 1 μm. In the oil, the content of linolenic acid is 1% by mass or less, The antioxidant is natural tocopherol,
A viscose solution for spinning is prepared by mixing the emulsion solution with a viscose stock solution containing cellulose,
A method for producing an oil-containing rayon fiber, wherein the spinning viscose liquid is extruded from a nozzle, spun, and coagulated.
他の繊維として、ポリエステル繊維、ポリアクリル繊維、ポリアミド繊維、ポリウレタン系弾性繊維、コットン及びウールからなる群から選ばれる少なくとも一つの繊維を複合した請求項8に記載の繊維構造物。 Containing 10 to 90% by mass of the oil-containing rayon fiber,
The fiber structure according to claim 8, wherein at least one fiber selected from the group consisting of polyester fiber, polyacrylic fiber, polyamide fiber, polyurethane elastic fiber, cotton and wool is compounded as the other fiber.
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