JP2018153632A - Sheet for being impregnated with drug solution - Google Patents
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Abstract
Description
本発明は、湿潤時の透明度が高く、湿潤時の取扱性や密着性に優れており、肌に刺激が少なくフェイスマスクとして使用したときに一体感を感じることができる薬液含浸用シートに関する。 The present invention relates to a chemical-impregnated sheet that has high transparency when wet, excellent handling properties and adhesion when wet, and has little irritation to the skin and can feel a sense of unity when used as a face mask.
従来、セルロース繊維不織布は美容向けのフェイスマスクとして広く使用されている。例えば、銅アンモニアレーヨン原液を流下緊張法によりウエブ化し、ウエブ化時に繊維が自己接着した後、水流交絡処理により模様付けした再生セルロース連続長繊維不織布は、化学的および物理的刺激性が少なく透明度が高い。例えば、下記特許文献１を参照のこと。
また、空隙率を制御することで透明度を高くしたセルロース短繊維不織布（例えば、下記特許文献２を参照のこと）、屈折率を制御することで透明度を高くした不織布（例えば、下記特許文献３と４を参照のこと）も開発されている。
Conventionally, a cellulose fiber nonwoven fabric has been widely used as a face mask for beauty. For example, a regenerated cellulose continuous long-fiber non-woven fabric that is made from a copper ammonia rayon stock solution by web flow tension method and the fibers self-adhering at the time of web formation and then patterned by hydroentanglement treatment has little chemical and physical irritation and transparency. high. For example, see Patent Document 1 below.
Moreover, the cellulose short fiber nonwoven fabric which raised transparency by controlling the porosity (for example, refer to the following patent document 2), and the nonwoven fabric which raised transparency by controlling the refractive index (for example, the following patent document 3) 4) has also been developed.
しかしながら、近年需要が拡大してきた、美容向けの薬液含浸用シートの開発は充分でなく、以下のような問題点があった。
（１）湿潤時に透明度の高い不織布が求められるが、厚みに応じて透明度が下がってしまう。
（２）薄くして透明性を改善した不織布は形態安定性が悪く湿潤状態での取扱性が悪くなってしまう。
（３）フェイスマスクとして着用した際、顔に異物が載っているような違和感がある。
（４）湿潤時での肌への密着性が満足できていない。
However, the development of a sheet for impregnating chemicals for beauty, whose demand has been increasing in recent years, has not been sufficiently developed, and has the following problems.
(1) Although a non-woven fabric with high transparency is required when wet, the transparency decreases depending on the thickness.
(2) A thin nonwoven fabric with improved transparency has poor shape stability and poor handling in a wet state.
(3) When worn as a face mask, there is a sense of incongruity that foreign matter is on the face.
(4) Adhesion to the skin when wet is not satisfactory.
上記従来技術の問題点に鑑み、本発明が解決しようとする課題は、湿潤時の透明度が高く、湿潤時の取扱性や密着性に優れており、肌に刺激が少なくフェイスマスクとして使用したときに一体感を感じることができる薬液含浸用シートを提供することである。 In view of the above-mentioned problems of the prior art, the problem to be solved by the present invention is high transparency when wet, excellent handling and adhesion when wet, and when used as a face mask with little irritation to the skin It is an object of the present invention to provide a sheet for impregnating a chemical solution that can feel a sense of unity.
本発明者らは、上記課題を解決すべく鋭意研究し実験を重ねた結果、再生セルロース系繊維の紡糸時において、凝固速度、再生速度を最適化することで、繊維表面の屈折率が１．０００以上１．５３６以下であり、湿潤時の繊維表面にミクロフィブリルが２０ｎｍ以上１３０ｎｍ以下の間隔で存在し、かつ、平均繊維直径が1μｍ以上２０μｍである薬液含浸用シートを得ることができることを予想外に見出し、本発明を完成するに至ったものである。 As a result of diligent research and experiments to solve the above problems, the present inventors have optimized the coagulation rate and the regeneration rate during spinning of the regenerated cellulosic fiber so that the refractive index of the fiber surface is 1. It is expected that a sheet impregnated with a chemical solution having a microfibril on the fiber surface at the time of wetness of 20 to 130 nm and an average fiber diameter of 1 to 20 μm can be obtained. It found out and came to complete this invention.
即ち、本発明は以下の通りのものである。
［１］再生セルロース系繊維不織布からなる薬液含浸用シートであって、下記（Ａ）〜（Ｃ）の特徴：
（Ａ）該再生セルロース系繊維表面の屈折率が１．０００以上１．５３６以下である；
（Ｂ）湿潤時の該再生セルロース系繊維の表面にミクロフィブリルが２０ｎｍ以上１３０ｎｍ以下の間隔で存在する；
（Ｃ）該再生セルロース系繊維の平均繊維直径が１μｍ以上２０μｍ以下である；
を有する前記薬液含浸用シート。
［２］前記再生セルロース系繊維の繊維断面が丸型断面構造を有する、前記［１］に記載の薬液含浸用シート。
［３］前記再生セルロース系繊維不織布の水抽出物量が５００ｐｐｍ以下である、前記［１］又は［２］に記載の薬液含浸用シート。
［４］前記再生セルロース系繊維不織布の厚み方向と垂直な一辺をＤａ方向とし、該厚み方向と該Ｄａ方向とにそれぞれ垂直な一辺をＤｂ方向とし、かつ、一定荷重で引っ張った際の伸び率がＤａ＞ＤｂであるところのＤａ方向における、該再生セルロース系繊維不織布の湿潤時のＫＥＳ引張回復率（ＲＴ）が、２１％以上６５％以下である、前記［１］〜［３］のいずれかに記載の薬液含浸用シート。
［５］前記再生セルロース系繊維が連続長繊維である、前記［１］〜［４］のいずれかに記載の薬液含浸用シート。
［６］前記［１］〜［５］のいずれかに記載の薬液含浸用シート１００重量部に対して、液体化粧料が１００重量部以上２０００重量部以下の割合で含浸されているフェイスマスク。
That is, the present invention is as follows.
[1] A sheet for impregnating a chemical solution made of a regenerated cellulose fiber nonwoven fabric, which is characterized by the following (A) to (C):
(A) The refractive index of the surface of the regenerated cellulose fiber is 1.000 or more and 1.536 or less;
(B) Microfibrils are present at intervals of 20 nm to 130 nm on the surface of the regenerated cellulosic fiber when wet;
(C) The regenerated cellulosic fiber has an average fiber diameter of 1 μm or more and 20 μm or less;
The said chemical | medical solution impregnation sheet | seat which has.
[2] The sheet for impregnating a chemical solution according to [1], wherein a fiber cross section of the regenerated cellulose fiber has a round cross section.
[3] The sheet for chemical liquid impregnation according to the above [1] or [2], wherein the amount of water extract of the regenerated cellulose fiber nonwoven fabric is 500 ppm or less.
[4] Elongation rate when one side perpendicular to the thickness direction of the regenerated cellulose fiber nonwoven fabric is defined as the Da direction, and one side perpendicular to the thickness direction and the Da direction is defined as the Db direction. Any of the above-mentioned [1] to [3], wherein the regenerated cellulose fiber nonwoven fabric has a KES tensile recovery rate (RT) of 21% or more and 65% or less in the Da direction where Da> Db. A sheet for impregnating a chemical solution according to claim 1.
[5] The sheet for impregnation with a chemical solution according to any one of [1] to [4], wherein the regenerated cellulose fiber is a continuous long fiber.
[6] A face mask in which the liquid cosmetic is impregnated at a ratio of 100 parts by weight or more and 2000 parts by weight or less with respect to 100 parts by weight of the chemical liquid impregnated sheet according to any one of [1] to [5].
本発明に係る薬液含浸用シートは、湿潤時の透明度が高く、湿潤時の取扱性や密着性に優れており、肌に刺激が少なくフェイスマスクとして使用したときに一体感を感じることができるものである。 The liquid impregnated sheet according to the present invention has high transparency when wet, excellent handling and adhesion when wet, and is less irritating to the skin and can feel a sense of unity when used as a face mask. It is.
以下、本発明の実施形態について詳細に説明する。
本実施形態で用いる再生セルロース系繊維としては、特に制限はなく、銅アンモニアレーヨン、ビスコースレーヨン、テンセル（リヨセル）、ポリノジック等の再生セルロース繊維や溶剤セルロース繊維が挙げられる。再生セルロース系繊維は連続長繊維でも短繊維でも構わないが、連続長繊維は短繊維のものよりも物理的刺激が少なく肌への密着性に優れ、吸液性にも優れている。
Hereinafter, embodiments of the present invention will be described in detail.
The regenerated cellulose fiber used in the present embodiment is not particularly limited, and examples thereof include regenerated cellulose fibers such as copper ammonia rayon, viscose rayon, tencel (lyocell), polynosic, and solvent cellulose fibers. The regenerated cellulosic fiber may be either a continuous long fiber or a short fiber, but the continuous long fiber has less physical irritation than that of the short fiber and has excellent adhesion to the skin and excellent liquid absorption.
本実施形態においては、不織布を構成する再生セルロース系繊維の平均繊維直径は１．０μｍ以上２０．０μｍ以下であり、好ましくは２．０μｍ以上１９．０μｍ以下、より好ましくは４．０μｍ以上１６μｍ以下である。平均繊維直径が１．０μｍ未満の場合、湿潤時の強度が小さくなるため、湿潤時の取扱性が悪くなる。他方、２０．０μｍよりも大きい場合、透明度が低下する。
本実施形態の再生セルロース系繊維不織布としては、バインダーや界面活性剤を付与した再生セルロース系繊維不織布では吸水性の低下や成分の溶出が懸念されるため、ノーバインダーのセルロース不織布を用いることが好ましい。
In the present embodiment, the average fiber diameter of the regenerated cellulose fiber constituting the nonwoven fabric is 1.0 μm or more and 20.0 μm or less, preferably 2.0 μm or more and 19.0 μm or less, more preferably 4.0 μm or more and 16 μm or less. It is. When the average fiber diameter is less than 1.0 μm, the strength when wet is reduced, and the handleability when wet is deteriorated. On the other hand, when larger than 20.0 micrometers, transparency will fall.
As the regenerated cellulosic fiber nonwoven fabric of the present embodiment, it is preferable to use a cellulosic nonwoven fabric with no binder because the regenerated cellulosic fiber nonwoven fabric to which a binder or a surfactant is added is liable to decrease in water absorption or elution of components. .
本実施形態の再生セルロース系繊維不織布の目付は、３０ｇ／ｍ２以上１５０ｇ／ｍ２以下であり、好ましくは、３５ｇ／ｍ２以上１１０ｇ／ｍ２以下であり、より好ましくは３５ｇ／ｍ２以上９０ｇ／ｍ２以下である。再生セルロース系繊維不織布の目付が３０ｇ／ｍ２未満の場合、薄すぎるために取扱い性が著しく低下し、実用的でなく、他方、１５０ｇ／ｍ２より大きい場合、取扱い性は優れるが、透明度が低下する。 The basis weight of the regenerated cellulose fiber nonwoven fabric of this embodiment is 30 g / m 2 or more and 150 g / m 2 or less, preferably 35 g / m 2 or more and 110 g / m 2 or less, more preferably 35 g / m 2 or more. 90 g / m 2 or less. When the basis weight of the regenerated cellulose fiber nonwoven fabric is less than 30 g / m 2 , the handleability is remarkably lowered because it is too thin and is not practical. On the other hand, when the basis weight is greater than 150 g / m 2 , the handleability is excellent, but the transparency is high. descend.
本実施形態の再生セルロース系繊維不織布の厚みは、０．２０ｍｍ以上１．００ｍｍ以下であり、好ましくは、０．２５ｍｍ以上０．８０ｍｍ以下であり、より好ましくは０．２５ｍｍ以上０．６０ｍｍ以下である。再生セルロース系繊維不織布の厚みが０．２０ｍｍ未満の場合、薄すぎるために取扱性が低下する。他方、１．００ｍｍよりも大きい場合、透明度の低下や肌への密着性が低下する。 The thickness of the regenerated cellulose fiber nonwoven fabric of this embodiment is 0.20 mm or more and 1.00 mm or less, preferably 0.25 mm or more and 0.80 mm or less, more preferably 0.25 mm or more and 0.60 mm or less. is there. When the thickness of the regenerated cellulose fiber nonwoven fabric is less than 0.20 mm, the handleability decreases because it is too thin. On the other hand, when larger than 1.00 mm, the transparency fall and the adhesiveness to skin fall.
本実施形態の再生セルロース系繊維不織布繊維表面の屈折率が１．０００以上１．５３６以下である。好ましくは１．２５０以上１．５３０以下であり、より好ましくは１．３００以上１．５２０以下である。繊維表面の屈折率が１．０００未満の場合、湿潤時の透明性が低下する。他方、１．５３６よりも大きい場合も湿潤時の透明性が低下する。 The refractive index of the surface of the regenerated cellulose-based nonwoven fabric fiber of this embodiment is 1.000 or more and 1.536 or less. Preferably it is 1.250 or more and 1.530 or less, More preferably, it is 1.300 or more and 1.520 or less. When the refractive index of the fiber surface is less than 1.000, transparency when wet is lowered. On the other hand, when it is larger than 1.536, the transparency when wet is lowered.
図１に示すように、本実施形態の再生セルロース系繊維不織布は、湿潤時の繊維表面においてミクロフィブリルが２０ｎｍ以上１３０ｎｍ以下の間隔で存在する。本明細書中、ミクロフィブリルとは、湿潤時の繊維表面のＳＥＭ画像において、幅８００ｎｍ以下のヒダ状又はウロコ状の形態を有する物を指し、この幅は、ミクロフィブリルの間隔と同義である。換言すれば、本実施形態の再生セルロース系繊維不織布の湿潤時の繊維表面には、２０〜１３０ｎｍの間隔で、ミクロフィブリルのヒダ状物が存在している。ミクロフィブリルの間隔は、好ましくは３０ｎｍ以上１２５ｎｍ以下であり、より好ましくは３５ｎｍ以上１２５ｎｍ以下である。湿潤時の繊維表面におけるミクロフィブリル間隔が２０ｎｍ未満の場合、繊維表面が緻密な構造となり硬いため肌への密着性が低下してしまう。他方、１３０ｎｍよりも大きい場合、光の散乱が抑制できずに透明性が低下してしまう。 As shown in FIG. 1, in the regenerated cellulose fiber nonwoven fabric of this embodiment, microfibrils are present at intervals of 20 nm to 130 nm on the fiber surface when wet. In the present specification, the microfibril refers to an object having a wrinkle-like or scale-like shape having a width of 800 nm or less in the SEM image of the fiber surface when wet, and this width is synonymous with the interval of the microfibrils. In other words, microfibril folds are present at intervals of 20 to 130 nm on the wet fiber surface of the regenerated cellulose fiber nonwoven fabric of this embodiment. The interval between microfibrils is preferably 30 nm to 125 nm, and more preferably 35 nm to 125 nm. When the microfibril spacing on the fiber surface when wet is less than 20 nm, the fiber surface has a dense structure and is hard, so the adhesion to the skin is reduced. On the other hand, when it is larger than 130 nm, light scattering cannot be suppressed and transparency is lowered.
本実施形態の再生セルロース系繊維不織布の繊維断面は丸型断面構造であることが好ましい。丸型断面とは、繊維断面の真円度が７０％以上１００％以下であることを意味し、より好ましくは８５％以上１００％以下である。真円度が７０％未満の場合、光の乱反射を抑制できずに透明性が低下してしまう。 The fiber cross section of the regenerated cellulose fiber nonwoven fabric of this embodiment preferably has a round cross section. The round cross section means that the roundness of the fiber cross section is 70% or more and 100% or less, more preferably 85% or more and 100% or less. When the roundness is less than 70%, the irregular reflection of light cannot be suppressed and the transparency is lowered.
本実施形態の再生セルロース系繊維不織布の水抽出物量は、５００ｐｐｍ以下であることが好ましく、より好ましくは４５０ｐｐｍ以下であり、さらに好ましくは４００ｐｐｍ以下である。水抽出物の成分としては低分子量のヘミセルロース、バインダー、親水剤などが考えられる。水抽出物量が５００ｐｐｍよりも大きい場合、湿潤時の肌刺激性が高く、不純物の影響により透明性が低下してしまう。 The amount of the water extract of the regenerated cellulose fiber nonwoven fabric of this embodiment is preferably 500 ppm or less, more preferably 450 ppm or less, and still more preferably 400 ppm or less. As a component of the water extract, low molecular weight hemicellulose, a binder, a hydrophilic agent, and the like can be considered. When the amount of water extract is larger than 500 ppm, the skin irritation when wet is high, and the transparency is lowered due to the influence of impurities.
本明細書中、「液体化粧料」とは、特に制限はなく、化粧品成分を含んだ水のことを言う。 In the present specification, the “liquid cosmetic” is not particularly limited and refers to water containing a cosmetic ingredient.
本実施形態の再生セルロース系繊維不織布の湿潤時の透明度は８０％以上９９％以下であることが好ましく、より好ましくは８０％以上９５％以下である。湿潤時の透明度が８０％未満の場合、フェイスマスクとして着用した際に、顔に異物が載っているように違和感を覚えてしまう。他方、９９％よりも大きい場合、肌に貼り付けた不織布が見辛くなり剥がしにくいため好ましくない。 The wet cellulose transparency of the regenerated cellulose fiber nonwoven fabric of this embodiment is preferably 80% or more and 99% or less, and more preferably 80% or more and 95% or less. When the transparency when wet is less than 80%, when worn as a face mask, the user feels a sense of incongruity as if foreign matter is on the face. On the other hand, when it is larger than 99%, the non-woven fabric attached to the skin is difficult to see and is difficult to peel off.
本実施形態の再生セルロース系繊維不織布の湿潤時のＤａ方向−１０％モジュラスは、０．４５Ｎ／５０ｍｍ以上１．５０Ｎ／５０ｍｍ以下であることが好ましく、より好ましくは０．４７Ｎ／５０ｍｍ以上１．３０Ｎ／５０ｍｍ以下である。湿潤時のＤａ方向−１０％モジュラスが０．４５Ｎ／５０ｍｍ未満の場合、形態安定性が悪く湿潤状態での取扱性が悪くなってしまう。他方、１．５０Ｎ／５０ｍｍよりも大きい場合、肌に密着した際に硬く感じることで不快感を覚えることがある。
尚、「Ｄａ方向」とは、前記再生セルロース系繊維不織布の厚み方向と垂直な一辺をＤａ方向とし、該厚み方向と該Ｄａ方向とにそれぞれ垂直な一辺をＤｂ方向とし、かつ、一定荷重で引っ張った際の伸び率がＤａ＞Ｄｂであるところの方向である。
The Da direction −10% modulus of the regenerated cellulose fiber nonwoven fabric of this embodiment is preferably 0.45 N / 50 mm or more and 1.50 N / 50 mm or less, more preferably 0.47 N / 50 mm or more. 30 N / 50 mm or less. When the Da direction -10% modulus when wet is less than 0.45 N / 50 mm, the form stability is poor and the handleability in the wet state is poor. On the other hand, when it is larger than 1.50 N / 50 mm, it may feel uncomfortable by feeling hard when it is in close contact with the skin.
The “Da direction” means that one side perpendicular to the thickness direction of the regenerated cellulose fiber nonwoven fabric is the Da direction, one side perpendicular to the thickness direction and the Da direction is the Db direction, and at a constant load. This is the direction in which the elongation percentage when pulled is Da> Db.
本実施形態の再生セルロース系繊維不織布の湿潤時のＤａ方向−ＫＥＳ引張回復率（ＲＴ）は２１％以上６５％以下であることが好ましく、より好ましくは２４％以上６０％以下である。湿潤時のＤａ方向−ＫＥＳ引張回復率が２１％未満の場合、形態安定性が悪く湿潤状態での取扱性が悪くなってしまう。他方、６５％よりも大きい場合、フェイスマスクとして着用した際、肌とシートが密着していた部位がフェイスマスク着用中にずれてしまうため好ましくない。 The Da direction-KES tensile recovery rate (RT) when wet of the regenerated cellulose fiber nonwoven fabric of the present embodiment is preferably 21% or more and 65% or less, more preferably 24% or more and 60% or less. When the direction of Da during wet-KES tensile recovery is less than 21%, the form stability is poor and the handleability in the wet state is poor. On the other hand, when it is larger than 65%, the portion where the skin and the sheet are in close contact with each other when worn as a face mask shifts during wearing the face mask, which is not preferable.
本実施形態の再生セルロース系繊維不織布の湿潤時のＤａ方向−ＫＥＳせん断ヒステリシス（２ＨＧ）は１．００ｇｆ／ｃｍ以上５．００ｇｆ／ｃｍ以下であることが好ましく、より好ましくは１．３０ｇｆ／ｃｍ以上４．６ｇｆ／ｃｍ以下である。湿潤時のＤａ方向−ＫＥＳせん断ヒステリシスが１．００ｇｆ／ｃｍ未満の場合、フェイスマスクとして着用した際、肌とシートが密着していた部位がフェイスマスク着用中にずれてしまうため好ましくない。他方、５．００ｇｆ／ｃｍよりも大きい場合、せん断方向の回復性が低くなるため、形態安定性が悪く湿潤状態での取扱性が悪く、また、目開きが生じることで液体保持能力が低下する場合もあるため好ましくない。 The Da direction-KES shear hysteresis (2HG) when wet of the regenerated cellulose fiber nonwoven fabric of this embodiment is preferably 1.00 gf / cm or more and 5.00 gf / cm or less, more preferably 1.30 gf / cm or more. It is 4.6 gf / cm or less. When the wet direction Da direction-KES shear hysteresis is less than 1.00 gf / cm, it is not preferable because the portion where the skin and the sheet are in close contact with each other is worn while wearing the face mask. On the other hand, if it is larger than 5.00 gf / cm, the recovery property in the shear direction is low, so that the form stability is poor and the handling property in a wet state is poor, and the liquid holding ability is reduced due to the opening. In some cases, it is not preferable.
本実施形態の再生セルロース系繊維不織布は、紡出した糸をネット上に振り落してシート状に積層した後、水流交絡させ、乾燥工程を経ることで製造することができる。本実施形態の再生セルロース系繊維不織布の製法上の特徴としては、例えば、銅アンモニアレーヨンの場合は紡糸工程において紡糸温度を３０℃以下することで凝固速度を下げたことを挙げることができる。紡糸温度を３０℃以下にすることでセルロース繊維表面の屈折率を従来のセルロース繊維不織布と比較して小さくすることができた。また、精練工程において弱酸を用いて再生速度を下げることも特徴の一つとして挙げることができる。再生速度を下げることで繊維表面にヒダ状のミクロフィブリルが多く存在する再生セルロース系繊維不織布を得ることができた。凝固速度・再生速度を最適化することで、低分子量セルロースの発生を少なくすることができたため、乾燥後に純水洗浄することなく従来の水流交絡行程において水抽出物質を除去することが可能となった。この製法上の特徴により、空隙率や厚みに関係なく透明性が高い再生セルロース系繊維不織布を得ることができた。 The regenerated cellulosic fiber nonwoven fabric of this embodiment can be produced by shaking the spun yarn onto a net and laminating it into a sheet, then hydroentangling and passing through a drying step. For example, in the case of copper ammonia rayon, the characteristics of the regenerated cellulose fiber nonwoven fabric according to this embodiment can be reduced by lowering the coagulation rate by lowering the spinning temperature to 30 ° C. or less in the spinning process. By setting the spinning temperature to 30 ° C. or less, the refractive index of the cellulose fiber surface could be reduced as compared with the conventional cellulose fiber nonwoven fabric. In addition, it can be mentioned as one of the characteristics that the regeneration rate is lowered by using a weak acid in the scouring process. By reducing the regeneration speed, a regenerated cellulosic fiber nonwoven fabric with many pleated microfibrils on the fiber surface could be obtained. By optimizing the coagulation rate and regeneration rate, it was possible to reduce the generation of low molecular weight cellulose, making it possible to remove the water extract material in the conventional hydroentanglement process without washing with pure water after drying. It was. Due to the characteristics of this production method, it was possible to obtain a regenerated cellulose fiber nonwoven fabric having high transparency regardless of the porosity and thickness.
以下、本発明を実施例などにより具体的に説明するが、本発明はこれらの実施例のみに何ら限定されるものではない。まず、実施例等で用いた測定方法を以下に示す。 EXAMPLES Hereinafter, although an Example etc. demonstrate this invention concretely, this invention is not limited to only these Examples at all. First, measurement methods used in Examples and the like are shown below.
（１）目付（ｇ／ｍ２）
０．０５ｍ２以上の面積の再生セルロース系繊維不織布を、１０５℃で一定質量になるまで乾燥後、２０℃、６５％ＲＨの恒温室に１６時間以上放置してその質量を測定し、不織布のｍ２当たりの質量（ｇ）を求めた。
(1) Weight per unit area (g / m 2 )
After drying the regenerated cellulosic fiber nonwoven fabric having an area of 0.05 m 2 or more to a constant mass at 105 ° C., the mass is measured by leaving it in a constant temperature room at 20 ° C. and 65% RH for 16 hours or more. The mass (g) per m 2 was determined.
（２）厚み（ｍｍ）
再生セルロース系繊維不織布を、ＪＩＳ−Ｌ１０９６準拠の厚み試験にて荷重を１．９６ｋＰａとして測定した。
(2) Thickness (mm)
The regenerated cellulose fiber nonwoven fabric was measured with a load of 1.96 kPa in a thickness test in accordance with JIS-L1096.
（３）繊維直径（μｍ）
再生セルロース系繊維不織布表面を、走査型電子顕微鏡、日本電子製ＪＳＭ−６３８０を用いて１００００倍の倍率で観察し、任意の１００本を選び測定した平均値を繊維直径とした。
(3) Fiber diameter (μm)
The surface of the regenerated cellulose fiber nonwoven fabric was observed with a scanning electron microscope and JSM-6380 manufactured by JEOL Ltd. at a magnification of 10,000 times, and an average value obtained by selecting and measuring 100 arbitrary fibers was defined as a fiber diameter.
（４）繊維表面の屈折率
常温で４８時間以上真空乾燥させた再生セルロース系繊維不織布にセダー油とシンナムアルデヒドの混合液を含浸させてデシケータ中で一晩放置した。前記混合液はセダー油とシンナムアルデヒドを屈折率が０．００２刻みとなるように作製した。混合液を含浸させた試料は偏光顕微鏡（Ｏｌｙｍｐｕｓ ＢＸ５１、偏光子＝入射側のみ、観察方法＝透過法、対物レンズ＝５０倍）を用いてベッケ線を観察することにより以下の式：
屈折率（ｎｉｓｏ）＝（ｎ// ＋ ２ｎ⊥）／３
で求められる不織布の屈折率（ｎｉｓｏ）を算出した。尚、測定は３０本の繊維に対して行い、ステージを下げる方向に動かした際、ベッケ線が内側から外側へ変化した繊維の本数比率と外側から内側へ変化した本数比率の入れ替わりを確認した。ベッケ線の見え方が逆転する直前・直後の混合液の屈折率の中間値を繊維表面の屈折率（ｎ//・ｎ⊥）とした。繊維軸に対して平行方向の屈折率（ｎ//）は入射側の偏光子に対して平行方向に向いている繊維のベッケ線を観察することにより得られる。繊維軸に対して垂直方向の屈折率（ｎ⊥）は、入射側の偏光子に対して垂直方向に向いている繊維のベッケ線を観察することにより得られる。［参考：高分子素材の変更顕微鏡入門（粟屋裕）アグネ技術センターｐ９７］
(4) Refractive index of fiber surface A regenerated cellulose fiber nonwoven fabric that had been vacuum-dried at room temperature for 48 hours or longer was impregnated with a mixed solution of cedar oil and cinnamaldehyde and left in a desiccator overnight. The mixed solution was made of cedar oil and cinnamaldehyde so that the refractive index was in increments of 0.002. The sample impregnated with the mixed solution was observed by using a polarizing microscope (Olympus BX51, polarizer = incident side only, observation method = transmission method, objective lens = 50 times), and the following formula:
Refractive index ( niso ) = (n // + 2n⊥ ) / 3
The refractive index ( niso ) of the nonwoven fabric calculated | required by (1) was computed. The measurement was performed on 30 fibers, and when the stage was moved in the lowering direction, it was confirmed that the number ratio of the fibers whose Becke line changed from the inside to the outside and the ratio of the number of fibers changed from the outside to the inside were confirmed. The refractive index of the fiber surface (n // · n ⊥ ) was defined as the intermediate value of the refractive index of the liquid mixture immediately before and after the appearance of the Becke line was reversed. The refractive index (n // ) in the direction parallel to the fiber axis can be obtained by observing the Becke line of the fiber oriented in the direction parallel to the polarizer on the incident side. The refractive index (n ⊥ ) in the direction perpendicular to the fiber axis is obtained by observing the Becke line of the fiber oriented in the direction perpendicular to the polarizer on the incident side. [Reference: Introduction to Changing Microscope of Polymer Materials (Hiroshi Hiroya) Agne Technology Center p97]
（５）湿潤時の繊維表面におけるミクロフィブリル間隔（ｎｍ）
再生セルロース系繊維不織布を蒸留水に浸漬後、徐々にイオン液体水溶液に置換した。遠心分離（１５０００ｒｐｍ／２０ｍｉｎ．）し過剰に存在しているイオン液体を除去した後、走査型電子顕微鏡ＨＩＴＡＣＨＩ Ｓ−４８００を用いて加速電圧５００Ｖ、ＷＤ（焦点距離）１．１〜１．８ｍｍで任意の１０本を選び観察した。得られた繊維表面画像は解析ソフト（ＩｍａｇｅＪ）を用いて二値化し、ミクロフィブリル（幅８００ｎｍ以下のヒダ状物：二値化後の画像上では黒色部分）の間隔を繊維方向と垂直の方向で１００ヶ所測定しその平均値を湿潤時の繊維表面におけるミクロフィブリル間隔とした。
(5) Microfibril spacing on the fiber surface when wet (nm)
The regenerated cellulose fiber nonwoven fabric was immersed in distilled water and then gradually replaced with an ionic liquid aqueous solution. After centrifuging (15000 rpm / 20 min.) To remove excess ionic liquid, using a scanning electron microscope HITACHI S-4800 at an acceleration voltage of 500 V and a WD (focal length) of 1.1 to 1.8 mm. Arbitrary 10 pieces were selected and observed. The obtained fiber surface image is binarized using analysis software (ImageJ), and the interval between microfibrils (folded objects having a width of 800 nm or less: black portions on the binarized image) is perpendicular to the fiber direction. 100 locations were measured, and the average value was defined as the microfibril spacing on the fiber surface when wet.
（６）真円度（％）
再生セルロース系繊維不織布断面を、走査型電子顕微鏡、日本電子製ＪＳＭ−６３８０を用いて２０００倍の倍率で観察し、最大外接円の直径Ａ（μｍ）、最大内接円の直径Ｂ（μｍ）を測定し、次式：
真円度（％）＝｛１−（Ａ−Ｂ）／繊維直径｝×１００
により真円度（％）を算出した。測定は任意の１００本を選び行った。
(6) Roundness (%)
The cross section of the regenerated cellulose fiber nonwoven fabric was observed with a scanning electron microscope and JSM-6380 manufactured by JEOL Ltd. at a magnification of 2000 times. The maximum circumscribed circle diameter A (μm) and the maximum inscribed circle diameter B (μm) Measure the following formula:
Roundness (%) = {1− (A−B) / fiber diameter} × 100
Was used to calculate the roundness (%). The measurement was performed by selecting 100 arbitrary pieces.
（７）水抽出物量（ｐｐｍ）
再生セルロース系繊維不織布４０ｇを入れたガラス瓶に蒸留水６４０ｇを加え、蓋をして１６時間放置する。抽出液は、濾過することによって繊維くずを取り除き、質量Ｃ（ｇ）を測定する。その後、濾過した抽出液は減圧蒸留を行い、抽出物（固体）の質量Ｄ（ｇ）を測定し、次式：
抽出物量 ＝ Ｄ／｛（Ｃ／６４０）×４０｝×１００００００
により抽出物量を算出した。
(7) Amount of water extract (ppm)
Add 640 g of distilled water to a glass bottle containing 40 g of the regenerated cellulose fiber nonwoven fabric, close the lid, and leave it for 16 hours. The extract is filtered to remove fiber waste, and the mass C (g) is measured. Thereafter, the filtered extract is distilled under reduced pressure, and the mass D (g) of the extract (solid) is measured.
Extract amount = D / {(C / 640) × 40} × 1000000
Was used to calculate the amount of extract.
（８）湿潤時の透明度（％）
５ｃｍ×５ｃｍの再生セルロース系繊維不織布をメッシュ（１０メッシュ、線径０．５ｍｍ）の上に載せ、これをバットに入れた水の中に入れて３０秒間浸漬する。その後、メッシュを引き上げて１０分間放置した後、過剰な水、水溶液を濾紙などで拭き取る。含水状態の不織布をガラス板に挟み、スガ試験機株式会社製積分球方式ＳＭ−Ｔを用いてＬ値を５回測定し、その平均値Ｅを用いて次式：
湿潤時の透明度 ＝ １００−（Ｅ−Ｆ）
により湿潤時の透明度（％）を算出した。この時、ガラス板のみのＬ値も５回測定し、その平均値をＦとしている。
(8) Transparency when wet (%)
A 5 cm × 5 cm regenerated cellulose fiber non-woven fabric is placed on a mesh (10 mesh, wire diameter 0.5 mm), placed in water in a vat and immersed for 30 seconds. Thereafter, the mesh is pulled up and left for 10 minutes, and then excess water and an aqueous solution are wiped off with a filter paper or the like. A non-woven fabric in a water-containing state is sandwiched between glass plates, and the L value is measured 5 times using an integrating sphere method SM-T manufactured by Suga Test Instruments Co., Ltd.
Transparency when wet = 100- (EF)
Was used to calculate the transparency (%) when wet. At this time, the L value of the glass plate alone was also measured five times, and the average value was taken as F.
（９）湿潤時のＤａ方向−１０％モジュラス（Ｎ／５０ｍｍ）
ＪＩＳ Ｌ １０９６に準拠して、厚み方向と垂直な一辺（Ｄａ方向）１５ｃｍ、厚み方向、且つ、Ｄａ方向に垂直な一辺（Ｄｂ方向）５ｃｍの試験片をＤａ方向に把握長１０ｃｍとなる様に試験機にセットし、滴り始める程度の水を付与した。定速伸長型引張り試験機（商品名：テンシロンＵＣＴ−１ｔ（オリエンテック株式会社製））を用いて不織布の伸長性を有する方向に、１０％伸長させたときの応力を測定した。測定は任意に１０試料サンプリングして行った。
(9) Da direction when wet-10% modulus (N / 50mm)
In accordance with JIS L 1096, a specimen having a side of 15 cm perpendicular to the thickness direction (Da direction) and a thickness of 5 cm and a side perpendicular to the Da direction (Db direction) of 5 cm is 10 cm long in the Da direction. The tester was set and water was added to the extent that it would begin to drip. Using a constant speed extension type tensile tester (trade name: Tensilon UCT-1t (manufactured by Orientec Co., Ltd.)), the stress was measured when the nonwoven fabric was extended by 10% in the direction having the extensibility. Measurement was performed by arbitrarily sampling 10 samples.
（１０）湿潤時のＤａ方向−ＫＥＳ引張回復率：ＲＴ（％）
カトーテック株式会社製のＫＥＳ-ＦＢ１引張試験機を用いて評価した。厚み方向と垂直な一辺（Ｄａ方向）１０ｃｍ、厚み方向、且つ、Ｄａ方向に垂直な一辺（Ｄｂ方向）２０ｃｍの試験片をＤａ方向に把握長５ｃｍとなるように試験機にセットし、霧吹きを用いて滴り始める程度の水を付与した後、荷重５０ｇｆ／ｃｍ下で引張回復率（ＲＴ）を測定した。測定は任意の試料を１０回行った。
(10) Da direction when wet-KES tensile recovery rate: RT (%)
Evaluation was performed using a KES-FB1 tensile tester manufactured by Kato Tech Co., Ltd. Set a test piece of 10 cm in one side (Da direction) perpendicular to the thickness direction, and 20 cm in one side (Db direction) perpendicular to the Da direction (Db direction) on the testing machine so that the grasping length is 5 cm in the Da direction, and spray After applying water enough to start dripping, the tensile recovery rate (RT) was measured under a load of 50 gf / cm. The measurement was performed 10 times for any sample.
（１１）湿潤時のＤａ方向−ＫＥＳせん断ヒステリシス：２ＨＧ（ｇｆ／ｃｍ）
カトーテック株式会社製のＫＥＳ-ＦＢ１せん断試験機を用いて評価した。厚み方向と垂直な一辺（Ｄａ方向）１０ｃｍ、厚み方向、且つ、Ｄａ方向に垂直な一辺（Ｄｂ方向）２０ｃｍをＤａ方向に把握長５ｃｍとなるように試験機にセットし、霧吹きを用いて滴り始める程度の水を付与した後、荷重５０ｇｆ／ｃｍ下でせん断ヒステリシス（２ＨＧ）を測定した。測定は任意の試料を１０回行った。
(11) Da direction when wet-KES shear hysteresis: 2HG (gf / cm)
Evaluation was performed using a KES-FB1 shear tester manufactured by Kato Tech Co., Ltd. Set 10cm in one side (Da direction) perpendicular to the thickness direction and 20cm in the thickness direction and 20cm side (Db direction) perpendicular to the Da direction on the test machine so that the grasping length is 5cm in the Da direction. After applying water to the extent that it begins, shear hysteresis (2HG) was measured under a load of 50 gf / cm. The measurement was performed 10 times for any sample.
（１２）着用感（点）
被験者２０人で着用感の官能評価を行った。評価方法及び判定水準は以下のとおりであり、２０人の平均値をそのサンプルの取扱いの官能評価の値とした。
評価方法：フェイスマスク型に抜いたセルロース不織布を４つ折りにし、通常のフェイスマスク商品同様に湿潤させたサンプルを顔に貼り付けた際の密着感や浸透感を以下の判定基準に従って評価した。
＜判定基準＞
５：着用時の不快感がなく、着用中に肌全体に潤っている感じがある。
４：着用時にサラサラした刺激を感じるが、着用中に肌全体に潤っている感じがある。
３：着用時にサラサラした刺激を感じ、着用中に肌の一部を除いて潤っている感じがある。
２：着用時にチクチクした刺激を感じ、着用中に肌の一部を除いて潤っている感じがある。
１：着用時にチクチクした刺激を感じ、着用中に肌の３か所以上において潤いを感じない部分がある。
(12) Wearing feeling (point)
Sensory evaluation of wearing feeling was performed with 20 test subjects. The evaluation method and the judgment level are as follows, and an average value of 20 people was used as a sensory evaluation value for handling the sample.
Evaluation method: Cellulose nonwoven fabric extracted into a face mask mold was folded in four, and the adhesion and penetration feeling when a wet sample was applied to the face in the same manner as a normal face mask product was evaluated according to the following criteria.
<Criteria>
5: There is no discomfort at the time of wearing, and there is a feeling that the whole skin is moistened during wearing.
4: Feels a smooth irritation when worn, but feels moist throughout the skin during wear.
3: A feeling of smooth irritation at the time of wearing is felt, and there is a feeling of moistening except for a part of the skin during wearing.
2: Feeling tingling when worn, feels moistened except for a part of skin during wearing.
1: There is a portion that does not feel moisturized at three or more places on the skin while wearing and feels a tingling stimulus.
（１３）取扱性（点）
被験者２０人で取扱性の官能評価を行った。評価方法及び判定水準は以下のとおりであり、２０人の平均値をそのサンプルの取扱いの官能評価の値とした。
評価方法：フェイスマスク型に抜いたセルロース不織布を４つ折りにし、通常のフェイスマスク商品同様に湿潤させたサンプルの開きやすさを以下の判定基準に従って評価した。
＜判定基準＞
５：皺が入ることなく広げられる
４：皺は入るがイライラせずに広げられる
３：普通
２：イライラするが時間をかければ広げられる
１：広げることができない
(13) Handleability (points)
Sensory evaluation of handleability was performed with 20 subjects. The evaluation method and the judgment level are as follows, and an average value of 20 people was used as a sensory evaluation value for handling the sample.
Evaluation method: The cellulose non-woven fabric extracted into a face mask mold was folded in four, and the ease of opening of the wet sample was evaluated according to the following criteria, as in the case of ordinary face mask products.
<Criteria>
5: Can be spread without spears 4: Can be speared but can be spread without frustration 3: Normal 2: Frustrated but can be spread over time 1: Cannot be spread
（１４）化学的刺激性
純水１５０ｍＬが入ったビーカーに、サンプル５ｇを浸漬させる。５分後、ビーカーを１分間振りながら撹拌する。１００ｍＬのメスシリンダーに６０ｍＬの抽出液を取り、蓋をして上下に２０回振る。メスシリンダーを立てて１分間放置した時の泡立ちの状態を見て下記基準により化学的刺激性を評価した。
＜判定基準＞
○：泡が無い状態か、ほとんど泡が目立たず液面に薄い筋状の泡が残る程度で壁面には泡は付着しない。
×：液面上に明らかに泡と分かる層が形成されており、シリンダーの壁面にも泡が付着している。
(14) Chemical irritation 5 g of the sample is immersed in a beaker containing 150 mL of pure water. After 5 minutes, stir while shaking the beaker for 1 minute. Take 60 mL of extract in a 100 mL graduated cylinder, cap and shake 20 times up and down. Chemical irritation was evaluated according to the following criteria by looking at the state of foaming when the measuring cylinder was stood and left for 1 minute.
<Criteria>
○: No bubbles on the wall surface, with no bubbles, or almost no bubbles are noticeable and thin streaky bubbles remain on the liquid surface.
X: The layer which can be recognized as a bubble clearly is formed on the liquid level, and the bubble adheres also to the wall surface of the cylinder.
（１５）密着性（点）
被験者２０人で密着性の官能評価を行った。評価方法及び判定水準は以下のとおりであり、２０人の平均値をそのサンプルの密着感の官能評価の値とした。
評価方法：５ｃｍ角の試料を湿潤（液が滴る直前量の純水を含浸）させて、手の甲に載せる。５分後の密着感を以下の判定基準に従って評価した。
＜判定基準＞
５：剥がれることが無く、皮膚が引き締まる感じがある。
４：端面に浮は生じるが、皮膚が引き締まる感じがある。
３：剥がれることは無いが、皮膚の引き締め感は感じられない。
２：端面に浮が生じ、皮膚の引き締め感も感じられない。
１：手の甲に乗らないくらい浮いており、結果、引き締め感もない。
(15) Adhesion (point)
Sensory evaluation of adhesion was performed with 20 test subjects. The evaluation method and the judgment level are as follows, and an average value of 20 persons was used as a sensory evaluation value of the adhesion feeling of the sample.
Evaluation method: A sample of 5 cm square is moistened (impregnated with an amount of pure water just before dripping) and placed on the back of the hand. The adhesion after 5 minutes was evaluated according to the following criteria.
<Criteria>
5: The skin does not peel off and the skin feels tight.
4: Although floating occurs on the end face, there is a feeling that the skin is tightened.
3: Although it does not peel off, it does not feel the tightness of the skin.
2: The end face floats, and the skin does not feel tight.
1: It floats so as not to get on the back of the hand, and as a result, there is no feeling of tightening.
［実施例１］
コットンリンター（重合度９００〜１０００）を銅アンモニア溶液で溶解し（コットンリンター１０ｗｔ％、アンモニア７ｗｔ％、銅３ｗｔ％）紡糸原液を準備した。原液吐出孔が直径０．６ｍｍ、４５個／ｃｍ２である紡糸口金を用い１ホール当たりの吐出量が０．０９ｃｃ／ｍｉｎにて、流下緊張下（水温２８℃）で連続してネット上に５層重ねで紡糸してセルロース連続長繊維ウエブを得た。得られたセルロース連続長繊維ウエブをリン酸（三価）で再生し、水洗後４０メッシュのコンベアネット（支持体）上にて水流交絡処理を行い１００℃の熱風にて乾燥させた。ネットスピードは２５ｍ／ｍｉｎ．であった。得られた不織布は、目付３７．５ｇ／ｍ２、繊維直径１４．３μｍ、屈折率１．４２８２、ＷＥＴミクロフィブリル間隔８１ｎｍであった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Example 1]
Cotton linter (degree of polymerization 900-1000) was dissolved with a copper ammonia solution (cotton linter 10 wt%, ammonia 7 wt%, copper 3 wt%) to prepare a spinning dope. Using a spinneret having a stock solution discharge hole of 0.6 mm in diameter and 45 pieces / cm 2 , the discharge amount per hole is 0.09 cc / min, and continuously on the net under flowing tension (water temperature 28 ° C.). A cellulose continuous long fiber web was obtained by spinning in five layers. The obtained continuous cellulose continuous fiber web was regenerated with phosphoric acid (trivalent), washed with water, hydroentangled on a 40 mesh conveyor net (support), and dried with hot air at 100 ° C. Net speed is 25m / min. Met. The obtained nonwoven fabric had a basis weight of 37.5 g / m 2 , a fiber diameter of 14.3 μm, a refractive index of 1.4282, and a WET microfibril spacing of 81 nm. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［実施例２］
原液吐出孔が直径０．３ｍｍ、１８０個／ｃｍ2である紡口を用い、１ホール当たりの吐出量が０．０２ｃｃ／ｍｉｎ．であること、水温１５℃であること以外は実施例１と同様の条件にて不織布を得た。得られた不織布は、目付４０．２ｇ／ｍ２、繊維直径４．３μｍ、屈折率１．４８５０、ＷＥＴミクロフィブリル間隔３６ｎｍであった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Example 2]
Using a spinning nozzle having a stock solution discharge hole with a diameter of 0.3 mm and 180 pieces / cm 2 , the discharge amount per hole is 0.02 cc / min. The nonwoven fabric was obtained under the same conditions as in Example 1 except that the water temperature was 15 ° C. The obtained nonwoven fabric had a basis weight of 40.2 g / m 2 , a fiber diameter of 4.3 μm, a refractive index of 1.4850, and a WET microfibril spacing of 36 nm. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［実施例３］
ネットスピードを１３ｍ／ｍｉｎ．であること以外は実施例１と同様の条件にて不織布を得た。得られた不織布は、目付８０．５ｇ／ｍ２、繊維直径１３．９μｍ、屈折率１．４５７３、ＷＥＴミクロフィブリル間隔６６ｎｍであった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Example 3]
Net speed is 13m / min. The nonwoven fabric was obtained on the conditions similar to Example 1 except being. The obtained nonwoven fabric had a basis weight of 80.5 g / m 2 , a fiber diameter of 13.9 μm, a refractive index of 1.4573, and a WET microfibril spacing of 66 nm. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［実施例４］
Ｎ−メチルモルホリンＮ−オキシドを溶媒として溶媒温度７６℃で紡糸された溶媒紡糸セルロースフィラメントから形成されたウエブに水流交絡処理を行い１００℃の熱風にて乾燥させた。得られた不織布は、目付３５．１ｇ／ｍ２、繊維直径２．５μｍ、屈折率１．５２１４、ＷＥＴミクロフィブリル間隔１２１ｎｍであった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Example 4]
A web formed from solvent-spun cellulose filaments spun at a solvent temperature of 76 ° C. using N-methylmorpholine N-oxide as a solvent was subjected to hydroentanglement treatment and dried with hot air at 100 ° C. The obtained nonwoven fabric had a basis weight of 35.1 g / m 2 , a fiber diameter of 2.5 μm, a refractive index of 1.5214, and a WET microfibril spacing of 121 nm. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［実施例５］
実施例１と同様な条件にて得られたセルロース連続長繊維糸を３８ｍｍにカットした。得られたカット綿をカーディングした後、水流交絡処理を行い１００℃の熱風にて乾燥させた。得られた不織布は、目付４５．２ｇ／ｍ２、繊維直径１０．２μｍ、屈折率１．５０６９、ＷＥＴミクロフィブリル間隔１１１ｎｍであった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Example 5]
A cellulose continuous long fiber yarn obtained under the same conditions as in Example 1 was cut into 38 mm. After carding the obtained cut cotton, it was subjected to hydroentanglement treatment and dried with hot air at 100 ° C. The obtained nonwoven fabric had a basis weight of 45.2 g / m 2 , a fiber diameter of 10.2 μm, a refractive index of 1.5069, and a WET microfibril spacing of 111 nm. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［実施例６］
実施例４と同様な条件にて得られたセルロース連続長繊維糸を３５ｍｍにカットした。得られたカット綿をカーディングした後、水流交絡処理を行い１００℃の熱風にて乾燥させた。得られた不織布は、目付４５．３ｇ／ｍ２、繊維直径８．７μｍ、屈折率１．５２９１、ＷＥＴミクロフィブリル間隔１２９ｎｍであった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Example 6]
The cellulose continuous long fiber yarn obtained under the same conditions as in Example 4 was cut into 35 mm. After carding the obtained cut cotton, it was subjected to hydroentanglement treatment and dried with hot air at 100 ° C. The obtained nonwoven fabric had a basis weight of 45.3 g / m 2 , a fiber diameter of 8.7 μm, a refractive index of 1.5291, and a WET microfibril spacing of 129 nm. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［実施例７］
１ホール当たりの吐出量が０．１５ｃｃ／ｍｉｎ、連続してネット上に４層重ねで紡糸、ネットスピードが２２ｍ／ｍｉｎ．であること以外は実施例１と同様の条件にて不織布を得た。得られた不織布は、目付６０．２ｇ／ｍ２、繊維直径１７．８μｍ、屈折率１．２８９０、ＷＥＴミクロフィブリル間隔４５ｎｍであった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Example 7]
The discharge amount per hole is 0.15 cc / min, and spinning is continuously performed by four layers on the net, and the net speed is 22 m / min. The nonwoven fabric was obtained on the conditions similar to Example 1 except being. The obtained nonwoven fabric had a basis weight of 60.2 g / m 2 , a fiber diameter of 17.8 μm, a refractive index of 1.2890, and a WET microfibril spacing of 45 nm. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［比較例１］
公知の方法によりキュプラ不織布を紡糸（水温４５℃）、精練した水流交絡させた後、乾燥させた。尚、ネットスピードは２６ｍ／ｍｉｎ．であった。得られた不織布は、目付３８．１ｇ／ｍ２、繊維直径１２．６μｍ、屈折率１．５３２０、ＷＥＴミクロフィブリル間隔１３１ｎｍであった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Comparative Example 1]
A cupra nonwoven fabric was spun by a known method (water temperature: 45 ° C.), scoured with water and entangled, and then dried. The net speed is 26 m / min. Met. The obtained nonwoven fabric had a basis weight of 38.1 g / m 2 , a fiber diameter of 12.6 μm, a refractive index of 1.5320, and a WET microfibril spacing of 131 nm. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［比較例２］
紡糸原液吐出口径を１／２のサイズに、水温３８℃であること以外は比較性１と同様の条件にて不織布を得た。得られた不織布は、目付３８．６ｇ／ｍ２、繊維直径４．５μｍ、屈折率１．５３６５、ＷＥＴミクロフィブリル間隔９３ｎｍであった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Comparative Example 2]
A nonwoven fabric was obtained under the same conditions as in Comparative Example 1 except that the spinning solution discharge port diameter was halved and the water temperature was 38 ° C. The obtained nonwoven fabric had a basis weight of 38.6 g / m 2 , a fiber diameter of 4.5 μm, a refractive index of 1.5365, and a WET microfibril spacing of 93 nm. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［比較例３］
市販の溶剤セルロース繊維不織布（リヨセル製不織布）の特性測定と評価を行なった。目付３６．９ｇ／ｍ２、繊維直径１０．１μｍ、屈折率１．５４４５、ＷＥＴミクロフィブリルはなかった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Comparative Example 3]
Characteristic measurement and evaluation of a commercially available solvent cellulose fiber nonwoven fabric (Lyocell nonwoven fabric) were performed. The basis weight was 36.9 g / m 2 , the fiber diameter was 10.1 μm, the refractive index was 1.5445, and there was no WET microfibril. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［比較例４］
市販の再生セルロース不織布（レーヨン製不織布）の特性測定と評価を行なった。目付６４．６ｇ／ｍ２、繊維直径１６．３μｍ、屈折率１．５３６５、ＷＥＴミクロフィブリルはなかった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Comparative Example 4]
Characteristic measurement and evaluation of a commercially available recycled cellulose nonwoven fabric (rayon nonwoven fabric) were performed. The basis weight was 64.6 g / m 2 , the fiber diameter was 16.3 μm, the refractive index was 1.5365, and there was no WET microfibril. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［比較例５］
市販の天然セルロース不織布（コットン製不織布）の特性測定と評価を行なった。目付６５．０ｇ／ｍ２、繊維直径２５．０μｍ、屈折率１．５５６８、ＷＥＴミクロフィブリルはなかった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Comparative Example 5]
Characteristic measurement and evaluation of a commercially available natural cellulose nonwoven fabric (cotton nonwoven fabric) were performed. The basis weight was 65.0 g / m 2 , the fiber diameter was 25.0 μm, the refractive index was 1.5568, and there was no WET microfibril. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
［比較例６］
公知の方法により得られた再生セルロース不織布（キュプラ不織布３８ｇ／ｍ２）の上から目付２ｇ／ｍ２の微細セルロース繊維不織布層を形成させた。得られた不織布は、目付４０．１ｇ／ｍ２、繊維直径０．１μｍ、屈折率１．５４８２、ＷＥＴミクロフィブリルはなかった。得られた不織布の特性、透明性などの評価結果を以下の表１と２に示す。
[Comparative Example 6]
A fine cellulose fiber nonwoven fabric layer having a basis weight of 2 g / m 2 was formed on the regenerated cellulose nonwoven fabric (cupra nonwoven fabric 38 g / m 2 ) obtained by a known method. The obtained nonwoven fabric had a basis weight of 40.1 g / m 2 , a fiber diameter of 0.1 μm, a refractive index of 1.5482, and no WET microfibrils. The evaluation results such as the properties and transparency of the obtained nonwoven fabric are shown in Tables 1 and 2 below.
表２から分かるように、本実施形態の再生セルロース系繊維不織布は、湿潤時の透明度が高く、湿潤時の取扱性や密着性に優れており、肌に刺激が少ないものであった。 As can be seen from Table 2, the regenerated cellulosic fiber nonwoven fabric of this embodiment has high transparency when wet, excellent handleability and adhesion when wet, and is less irritating to the skin.
本発明の薬液含浸用シートは、湿潤時の透明度が高く、湿潤時の取扱性や密着性に優れており、肌に刺激が少なくフェイスマスクとして使用したときに一体感を感じることができるため、湿潤状態で肌に触れるフェイスマスク用不織布として好適に利用可能である。 The liquid-impregnated sheet of the present invention has high transparency when wet, and is excellent in handleability and adhesion when wet, because it can feel a sense of unity when used as a face mask with little irritation to the skin, It can be suitably used as a non-woven fabric for a face mask that touches the skin in a wet state.
Claims (6)
（Ａ）該再生セルロース系繊維表面の屈折率が１．０００以上１．５３６以下である；
（Ｂ）湿潤時の該再生セルロース系繊維の表面にミクロフィブリルが２０ｎｍ以上１３０ｎｍ以下の間隔で存在する；
（Ｃ）該再生セルロース系繊維の平均繊維直径が１μｍ以上２０μｍ以下である；
を有する前記薬液含浸用シート。 A sheet for impregnating a chemical solution comprising a regenerated cellulose fiber nonwoven fabric, the following features (A) to (C):
(A) The refractive index of the surface of the regenerated cellulose fiber is 1.000 or more and 1.536 or less;
(B) Microfibrils are present at intervals of 20 nm to 130 nm on the surface of the regenerated cellulosic fiber when wet;
(C) The regenerated cellulosic fiber has an average fiber diameter of 1 μm or more and 20 μm or less;
The said chemical | medical solution impregnation sheet | seat which has.
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| WO2020226181A1 (en) * | 2019-05-09 | 2020-11-12 | 旭化成株式会社 | Recycled cellulosic fiber nonwoven fabric, chemical impregnation sheet, and face mask |
| WO2021210531A1 (en) * | 2020-04-14 | 2021-10-21 | 第一三共ヘルスケア株式会社 | Face mask and sheet-shaped base material |
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| JP2014205924A (en) * | 2013-04-10 | 2014-10-30 | 旭化成せんい株式会社 | Sheet impregnated with chemical |
| JP2015070968A (en) * | 2013-10-03 | 2015-04-16 | 旭化成せんい株式会社 | Nonwoven fabric for face mask |
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| JPH1037055A (en) * | 1996-07-19 | 1998-02-10 | Asahi Chem Ind Co Ltd | Composite nonwoven fabric |
| JP2011255122A (en) * | 2010-06-11 | 2011-12-22 | Unicharm Corp | Method for quantitative evaluation of comfortableness of disposable diaper |
| JP2014205924A (en) * | 2013-04-10 | 2014-10-30 | 旭化成せんい株式会社 | Sheet impregnated with chemical |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2020226181A1 (en) * | 2019-05-09 | 2020-11-12 | 旭化成株式会社 | Recycled cellulosic fiber nonwoven fabric, chemical impregnation sheet, and face mask |
| JPWO2020226181A1 (en) * | 2019-05-09 | 2021-11-18 | 旭化成株式会社 | Regenerated cellulose fiber non-woven fabric, chemical impregnated sheet, and face mask |
| CN113677238A (en) * | 2019-05-09 | 2021-11-19 | 旭化成株式会社 | Regenerated cellulose fiber nonwoven fabric, sheet impregnated with chemical solution, and face mask |
| JP7101879B2 (en) | 2019-05-09 | 2022-07-15 | 旭化成株式会社 | Regenerated cellulose fiber non-woven fabric, chemical impregnated sheet, and face mask |
| CN113677238B (en) * | 2019-05-09 | 2024-06-11 | 旭化成株式会社 | Regenerated cellulose fiber nonwoven fabric, sheet impregnated with chemical solution, and mask |
| WO2021210531A1 (en) * | 2020-04-14 | 2021-10-21 | 第一三共ヘルスケア株式会社 | Face mask and sheet-shaped base material |
| CN115426920A (en) * | 2020-04-14 | 2022-12-02 | 第一三共健康事业株式会社 | Mask pack and sheet-like substrate |
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