JP2013234408A - Cellulose fiber for inner cotton and method for producing the same - Google Patents
Cellulose fiber for inner cotton and method for producing the same Download PDFInfo
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- JP2013234408A JP2013234408A JP2012108277A JP2012108277A JP2013234408A JP 2013234408 A JP2013234408 A JP 2013234408A JP 2012108277 A JP2012108277 A JP 2012108277A JP 2012108277 A JP2012108277 A JP 2012108277A JP 2013234408 A JP2013234408 A JP 2013234408A
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- 229920003043 Cellulose fiber Polymers 0.000 title claims abstract description 57
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 229920000742 Cotton Polymers 0.000 title abstract description 8
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims description 31
- 238000000034 method Methods 0.000 claims description 30
- 125000004432 carbon atom Chemical group C* 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000002736 nonionic surfactant Substances 0.000 claims description 8
- 239000007764 o/w emulsion Substances 0.000 claims description 7
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 125000002947 alkylene group Chemical group 0.000 claims description 4
- 125000000962 organic group Chemical group 0.000 claims description 4
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 4
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 claims description 3
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 24
- 238000005406 washing Methods 0.000 abstract description 19
- 239000000839 emulsion Substances 0.000 abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 7
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 239000000463 material Substances 0.000 abstract description 4
- 229920002678 cellulose Polymers 0.000 abstract description 2
- 239000001913 cellulose Substances 0.000 abstract description 2
- 230000003578 releasing effect Effects 0.000 abstract 1
- 239000004094 surface-active agent Substances 0.000 abstract 1
- 239000003921 oil Substances 0.000 description 36
- -1 polysiloxane Polymers 0.000 description 8
- 238000012360 testing method Methods 0.000 description 7
- 238000011156 evaluation Methods 0.000 description 6
- 238000011282 treatment Methods 0.000 description 6
- 210000003746 feather Anatomy 0.000 description 5
- 229920000433 Lyocell Polymers 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 239000011247 coating layer Substances 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 229920002994 synthetic fiber Polymers 0.000 description 3
- 239000012209 synthetic fiber Substances 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- IDCBOTIENDVCBQ-UHFFFAOYSA-N TEPP Chemical compound CCOP(=O)(OCC)OP(=O)(OCC)OCC IDCBOTIENDVCBQ-UHFFFAOYSA-N 0.000 description 2
- 229920013822 aminosilicone Polymers 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007257 malfunction Effects 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 125000000022 2-aminoethyl group Chemical group [H]C([*])([H])C([H])([H])N([H])[H] 0.000 description 1
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 description 1
- 229920002972 Acrylic fiber Polymers 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 229920001407 Modal (textile) Polymers 0.000 description 1
- 229920000297 Rayon Polymers 0.000 description 1
- 229920002125 Sokalan® Polymers 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 239000003599 detergent Substances 0.000 description 1
- 239000004205 dimethyl polysiloxane Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 125000000816 ethylene group Chemical group [H]C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 150000003840 hydrochlorides Chemical class 0.000 description 1
- 150000002431 hydrogen Chemical group 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000001771 impaired effect Effects 0.000 description 1
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 1
- 239000004584 polyacrylic acid Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000002964 rayon Substances 0.000 description 1
- 239000004627 regenerated cellulose Substances 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 230000035807 sensation Effects 0.000 description 1
- 230000015541 sensory perception of touch Effects 0.000 description 1
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 description 1
- 229920002545 silicone oil Polymers 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 239000002344 surface layer Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000013519 translation Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Landscapes
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
Description
本発明は、洗濯耐久性のある柔らかい風合い、制電性に優れた嵩高反発性を有し、羽毛調で吸湿性に優れたふとん綿素材として最適な中綿用セルロース繊維とその製造方法に関する。 The present invention relates to a cellulose fiber for batting which has a soft texture with washing durability, a bulky resilience excellent in antistatic properties, and is suitable as a futon material excellent in feather tone and moisture absorption, and a method for producing the same.
従来、合成繊維や再生セルロースを含むセルロース繊維、その他の天然繊維に洗濯耐久性、柔らかな風合い、制電性、嵩高反発性、吸湿性などを付与するために、中綿用に限らず各種の処理方法が提案されている。たとえば特公昭６３−５５１号公報（特許文献１）にはポリシロキサンとアミノシラン化合物及び金属塩を必須とした処理剤を用いて、洗濯による脱落の少ない羽毛調を呈する詰綿用合成繊維の処理剤が提案されている。 Conventionally, various treatments are used not only for batting, but to give washing durability, soft texture, antistatic, bulky resilience, hygroscopicity, etc. to cellulose fibers including synthetic fibers and regenerated cellulose, and other natural fibers A method has been proposed. For example, Japanese Examined Patent Publication No. 63-551 (Patent Document 1) uses a treating agent essentially composed of a polysiloxane, an aminosilane compound and a metal salt, and a treating agent for synthetic fibers for wadding, which has a feather tone with less dropout due to washing. Has been proposed.
しかしながらこの方法による処理剤に含まれる金属塩は亜鉛や錫、鉛などの塩酸塩、硫酸塩などが使用されており、環境問題や、安全、安心の面での懸念が完全に払拭できない欠点がある。 However, the metal salt contained in the treatment agent by this method uses zinc, tin, lead and other hydrochlorides, sulfates, etc., and there is a drawback that environmental problems and safety and security concerns cannot be completely eliminated. is there.
また、アミノシリコーンとアミノシラン等を使用して、安全性を確保し、柔らかい風合いを持ちながら洗濯耐久性を併せ持つ処理方法も提案されている（特許文献２）。しかしながら、この方法による処理は、抗菌性を付与させるためにカチオン系界面活性剤を用いており、アルカリ性洗剤による洗濯耐久性に劣る欠点があると同時に、アクリル繊維には比較的好結果をもたらすが、セルロース系繊維には効果が少ない欠点を有する。 In addition, a treatment method that uses aminosilicone and aminosilane, etc., to ensure safety and to have washing durability while having a soft texture has also been proposed (Patent Document 2). However, the treatment by this method uses a cationic surfactant to impart antibacterial properties, and has the disadvantage of being inferior in washing durability with an alkaline detergent, while at the same time providing relatively good results for acrylic fibers. Cellulose fibers have drawbacks that are less effective.
また、カルボキシ変性シリコーン、アミノ変性シリコーン、アミノアルコキシシランを必須成分とした油剤により処理することで、洗濯後も易滑風合いに優れたポリエステル短繊維を得る方法が提案されている（特許文献３）。しかしながらこの方法では、繊維表面に樹脂化した被覆層が形成され、洗濯耐久性は向上するものの柔らかな風合いを損ねる欠点を有する。 In addition, a method has been proposed in which polyester short fibers having excellent slipperiness after washing are obtained by treating with an oil agent containing carboxy-modified silicone, amino-modified silicone, and aminoalkoxysilane as essential components (Patent Document 3). . However, in this method, a resinized coating layer is formed on the fiber surface, and although the washing durability is improved, there is a defect that the soft texture is impaired.
さらにまた、一定条件でセルロース系繊維をクリンプ処理したのち、アミノ官能基を有するシリコーン油で処理して、羽毛との混合に最適な、改善された開繊特性を付与させる方法が提案されている（特許文献４）。しかしながらこの方法においてはクリンプによる機械的な強度劣化の問題が完全に払拭されないため、洗濯の繰り返しにより嵩高反発性が低下する欠点が解消されない。 Furthermore, a method has been proposed in which cellulosic fibers are crimped under certain conditions and then treated with silicone oil having an amino functional group to provide improved opening characteristics that are optimal for mixing with feathers. (Patent Document 4). However, in this method, the problem of mechanical strength deterioration due to crimping is not completely wiped out, so that the disadvantage that bulkiness rebound is reduced by repeated washing is not solved.
安全性が高く、風合い及び洗濯耐久性を付与する繊維処理剤を提供する方法も、提案されている（特許文献５）。しかしながら、この方法においても、使用されるポリビニルアルコール系重合体とポリアクリル酸系共重合体が樹脂化して、繊維表面に硬い被覆層が形成され、洗濯耐久性は向上するものの柔らかい風合いが、やや犠牲にされる欠点を有する。 A method for providing a fiber treatment agent that is highly safe and imparts a texture and washing durability has also been proposed (Patent Document 5). However, even in this method, the polyvinyl alcohol polymer and the polyacrylic acid copolymer to be used are converted into a resin, and a hard coating layer is formed on the fiber surface. Has the disadvantage of being sacrificed.
特許文献１〜５に示された従来の方法では、環境問題や、安全、安心の面で懸念があったり、一定の合成繊維では効果があるがセルロース系繊維においては効果が低減したり、繊維表面に樹脂化した被覆層が形成され、洗濯耐久性は向上するものの柔らかな風合いを損ねたり、機械的な強度劣化の問題が完全に払拭されないため、嵩高反発性が、繰り返しにより低下する欠点など、問題点があった。 In the conventional methods shown in Patent Documents 1 to 5, there are concerns in terms of environmental problems, safety and security, and certain synthetic fibers are effective, but the effects are reduced in cellulosic fibers, or fibers. A resinized coating layer is formed on the surface, and although washing durability is improved, the soft texture is damaged, and the problem of mechanical strength deterioration is not completely wiped out, so the bulky rebound is reduced due to repetition etc. There was a problem.
本発明の目的は、環境問題や、安全、安心の面で懸念がなく、洗濯耐久性を有しながらも、柔らかい風合いを併せ持ち、良好な制電性及び優れた嵩高反発性を有し、羽毛調で吸放湿性の優れたふとん綿素材として最適なセルロース繊維を提供することにある。 The object of the present invention is not concerned with environmental problems, safety and security, and has a soft texture while having washing durability, good antistaticity and excellent bulky resilience, and feathers The object is to provide an optimum cellulose fiber as a futon material with excellent tone and moisture absorption.
本発明は、上記の課題を解決するものとして、以下のことを特徴とする。 The present invention is characterized by the following in order to solve the above problems.
１．中綿用セルロース繊維の製造方法であって、次の第１工程〜第３工程：
（第１工程）下記のＡ成分と下記のＢ成分をＡ成分／Ｂ成分＝９９／１〜９０／１０の質量比で含有する油剤の油剤濃度が０．１質量％〜２．０質量％の水中油滴エマルションを調製し、前記水中油滴エマルションをセルロース繊維に含侵させて給油する工程；
（第２工程）前記第１工程の後に、前記セルロース繊維を絞り率５０％〜１５０％にて遠心脱水し、前記油剤を前記セルロース繊維に対して０．２質量％〜１．５質量％の割合で付着させる工程；
（第３工程）前記第２工程の後に、前記セルロース繊維を減圧下で加熱処理する工程
を経ることを特徴とする前記製造方法。
Ａ成分：アミノ当量が３０００グラム／ｍｏｌ〜１５０００グラム／ｍｏｌである式（１）で示
されるアミノ変性シリコーン
Ｒは、式（２）
で示される有機基であり、
ｘは、１〜２０の整数であり、そして、
ｙは、４０〜１０００の整数である。
Ｂ成分：式（３）で示されるノニオン型界面活性剤
２．前記第２工程の後の前記セルロース繊維に対する前記油剤の付着量が０．５質量％〜１．０質量％である上記１記載の中綿用セルロース繊維の製造方法。
３．前記第３工程での圧力が７２０ｍｍＨｇ以下である上記１又は２に記載の中綿用セルロース繊維の製造方法。
４．前記第３工程での加熱温度が１１０℃〜１３０℃である上記１〜３のいずれかに記載の中綿用セルロース繊維の製造方法。
５．上記１〜４のいずれかに記載の製造方法により得られる中綿用セルロース繊維。
1. It is a manufacturing method of the cellulose fiber for batting, Comprising: The following 1st process-3rd process:
(1st process) Oil agent concentration of the oil agent which contains the following A component and the following B component by the mass ratio of A component / B component = 99/1-90/10 is 0.1 mass%-2.0 mass% Preparing an oil-in-water emulsion, and impregnating the oil-in-water emulsion with cellulose fibers to supply oil;
(Second step) After the first step, the cellulose fibers are centrifugally dehydrated at a drawing rate of 50% to 150%, and the oil agent is 0.2% by mass to 1.5% by mass with respect to the cellulose fibers. Applying at a rate;
(Third step) The method according to claim 3, wherein after the second step, the cellulose fiber is subjected to a heat treatment under reduced pressure.
Component A: amino-modified silicone represented by formula (1) having an amino equivalent of 3000 to 15000 g / mol
R is the formula (2)
An organic group represented by
x is an integer from 1 to 20, and
y is an integer of 40 to 1000.
Component B: Nonionic surfactant represented by the formula (3)
2. The manufacturing method of the cellulose fiber for batting of said 1 whose adhesion amount of the said oil agent with respect to the said cellulose fiber after the said 2nd process is 0.5 mass%-1.0 mass%.
3. The manufacturing method of the cellulose fiber for batting of said 1 or 2 whose pressure in the said 3rd process is 720 mmHg or less.
4). The manufacturing method of the cellulose fiber for batting in any one of said 1-3 whose heating temperature in the said 3rd process is 110 to 130 degreeC.
5. A cellulose fiber for batting obtained by the production method according to any one of 1 to 4 above.
本発明により、洗濯耐久性のある柔らかい風合い、良好な制電性及び優れた嵩高反発性を有するセルロース繊維、さらに詳しくは羽毛調で吸放湿性の優れたふとん綿素材として最適なセルロース繊維を提供することができる。 According to the present invention, a cellulose fiber having a soft texture with durability to washing, a good antistatic property and an excellent bulky resilience, and more specifically, a cellulose fiber that is optimal as a futon material with feather tone and excellent moisture absorption and desorption properties is provided. can do.
本発明は上記の特徴を持つものであるが、以下にその実施の形態について説明する。
本発明の中綿用セルロース繊維の製造方法で、まず、第１工程で使用されるＡ成分のアミノ変性シリコーンの好ましいアミノ当量は３０００グラム／ｍｏｌ〜１５０００グラム／ｍｏｌであり、より好ましくは３５００グラム／ｍｏｌ〜１００００グラム／ｍｏｌである。３０００グラム／ｍｏｌ未満だと嵩高性が低下し、セルロース繊維が着色するという不具合が生じ、１５０００グラム／ｍｏｌを超えると嵩高性が低下し、セルロース繊維に十分な柔らかい風合いが得られないという不具合が生じる。
第１工程で使用されるＡ成分のアミノ変性シリコーンにおいて、式（１）のＭは、水素又はメチル基であり、それぞれ同じでも異なっていてもよい。
The present invention has the above-described features, and an embodiment thereof will be described below.
In the method for producing cellulose fibers for batting of the present invention, first, the preferred amino equivalent of the amino-modified silicone of component A used in the first step is 3000 g / mol to 15000 g / mol, more preferably 3500 g / mol. mol-10000 g / mol. If it is less than 3000 g / mol, the bulkiness decreases and the cellulose fiber is colored, and if it exceeds 15000 g / mol, the bulkiness decreases, and the cellulose fiber cannot have a sufficiently soft texture. Arise.
In the amino-modified silicone of component A used in the first step, M in the formula (1) is hydrogen or a methyl group, and may be the same or different.
第１工程で使用されるＡ成分のアミノ変性シリコーンにおいて、式（１）のｘは、１〜２０の整数であり、より好ましくは１〜１０の整数であり、更に好ましくは１〜３の整数である。ｘが０だと嵩高性が低下し、セルロース繊維に柔らかい風合いが得られないという不具合が生じ、ｘが２０を超えると嵩高性が低下し、セルロース繊維が着色するという不具合が生じる。 In the amino-modified silicone of component A used in the first step, x in the formula (1) is an integer of 1 to 20, more preferably an integer of 1 to 10, and still more preferably an integer of 1 to 3. It is. When x is 0, the bulkiness is lowered, and a problem that a soft texture cannot be obtained on the cellulose fiber occurs. When x exceeds 20, the bulkiness is lowered and the cellulose fiber is colored.
第１工程で使用されるＡ成分のアミノ変性シリコーンにおいて、式（１）のｙは、４０〜１０００の整数であり、より好ましくは５０〜６００の整数であり、更に好ましくは５０〜４００の整数である。ｙが４０未満だと嵩高性が低下し、セルロース繊維に十分な柔らかい風合いが得られないという不具合が生じ、ｙが１０００を超えると水に溶解できず、水中油滴エマルションを作製できないため、セルロース繊維に給油することができないという不具合が生じる。 In the amino-modified silicone of component A used in the first step, y in the formula (1) is an integer of 40 to 1000, more preferably an integer of 50 to 600, still more preferably an integer of 50 to 400. It is. When y is less than 40, the bulkiness is lowered, and there is a problem that a sufficiently soft texture cannot be obtained for the cellulose fiber. When y exceeds 1000, it cannot be dissolved in water and an oil-in-water emulsion cannot be produced. There is a problem that the fiber cannot be refueled.
第１工程で使用されるＡ成分のアミノシリコーンにおいて、式（１）のＲは式（２）で示される有機基であり、式（２）のｚは、０又は１である。ｚが１を超えるとセルロース繊維が着色するという不具合が生じる。 In the aminosilicone of component A used in the first step, R in the formula (1) is an organic group represented by the formula (2), and z in the formula (2) is 0 or 1. When z exceeds 1, the malfunction that a cellulose fiber will color arises.
式（２）で示される有機基のＲ1及びＲ2は、炭素数２〜４のアルキレン基であり、それぞれ同じでも異なっていてもよい。アルキレン基の炭素数が２未満、或いは炭素数４を超えると油剤製品の安定性が保てないという不具合が生じる。 R 1 and R 2 of the organic group represented by the formula (2) are alkylene groups having 2 to 4 carbon atoms, and may be the same or different. If the alkylene group has less than 2 carbon atoms or more than 4 carbon atoms, there is a problem that the stability of the oil product cannot be maintained.
本発明の中綿用セルロース繊維の製造方法で、第１工程で使用されるＢ成分のノニオン型界面活性剤において、式（３）のｎは、８〜１８の整数であり、より好ましくは１０〜１５の整数である。ｎが８未満、或いはｎが１８を超えると、安定なエマルションを作製できないという不具合が生じる。同じく式（３）において、ｍは３〜３０の整数であり、より好ましくは３〜２０の整数である。ｍが３未満、或いはｍが３０を超えると、安定なエマルションを作製できないという不具合が生じる。 In the manufacturing method of the cellulose fiber for batting of this invention, in the nonionic surfactant of B component used at a 1st process, n of Formula (3) is an integer of 8-18, More preferably, it is 10-10. It is an integer of 15. When n is less than 8 or n exceeds 18, there is a problem that a stable emulsion cannot be produced. Similarly in Formula (3), m is an integer of 3-30, More preferably, it is an integer of 3-20. When m is less than 3 or m exceeds 30, there is a problem that a stable emulsion cannot be produced.
本発明の中綿用セルロース繊維の製造方法で使用されるＡ成分とＢ成分の質量比は、９９／１〜９０／１０であり、より好ましくは９６／４〜９０／１０である。質量比が９９／１よりもＡ成分が増大すると安定なエマルションを作製できないという不具合が生じ、９０／１０よりもＢ成分が増大するとセルロース繊維に十分な柔らかい風合いが得られないという不具合が生じる。 The mass ratio of A component and B component used by the manufacturing method of the cellulose fiber for batting of this invention is 99 / 1-90 / 10, More preferably, it is 96 / 4-90 / 10. When the A component increases from 99/1, a problem that a stable emulsion cannot be produced occurs. When the B component increases from 90/10, a problem arises that a sufficiently soft texture cannot be obtained for cellulose fibers.
本発明の中綿用セルロース繊維の製造方法において、第１工程で、上記質量比で混合された油剤を、水に分散させ、油剤濃度が０．１〜２．０重量％の水中油滴エマルションを調製し、これをセルロース繊維に含侵させて給油する。エマルションの油剤濃度が０．１質量％未満だとセルロース繊維への給油量が少なくなり、セルロース繊維に十分な柔らかい風合いが得られない不具合が生じる。エマルションの油剤濃度が２．０質量％を超えると給油量が過大となり、嵩高性及び洗濯耐久性が低下する。 In the manufacturing method of the cellulose fiber for batting of this invention, the oil agent mixed by the said mass ratio is disperse | distributed to water at the 1st process, and the oil-in-water emulsion whose oil agent density | concentration is 0.1 to 2.0 weight% is obtained. It is prepared and impregnated into cellulose fibers and oiled. When the oil agent concentration of the emulsion is less than 0.1% by mass, the amount of oil supplied to the cellulose fibers is reduced, and there is a problem that a sufficiently soft texture cannot be obtained for the cellulose fibers. When the oil agent concentration of the emulsion exceeds 2.0% by mass, the amount of oil supply becomes excessive, and the bulkiness and washing durability deteriorate.
本発明において原料として使用できるセルロース繊維は、セルロースを主成分とする繊維である。具体的には、例えば、テンセル（登録商標）（レンチング社製）、レーヨン、ポリノジック、リネン、綿等が挙げられる。 The cellulose fiber that can be used as a raw material in the present invention is a fiber mainly composed of cellulose. Specific examples include Tencel (registered trademark) (manufactured by Lenzing), rayon, polynosic, linen, and cotton.
本発明の中綿用セルロース繊維の製造方法で、第２工程でのセルロース繊維への油剤付着量は、該繊維に対し０．２質量％〜１．５質量％であり、より好ましくは０．５質量％〜１．０質量％である。０．２質量％未満だとセルロース繊維への給油量が少なくなり、セルロース繊維に十分な柔らかい風合いが得られず、嵩高性が低下し、制電性も不十分になる。１．５質量％を超えると給油量が過大となり、嵩高性及び洗濯耐久性が低下するという不具合が生じる。 In the method for producing the cellulose fiber for batting of the present invention, the amount of the oil agent attached to the cellulose fiber in the second step is 0.2% by mass to 1.5% by mass with respect to the fiber, more preferably 0.5%. It is mass%-1.0 mass%. If the amount is less than 0.2% by mass, the amount of oil supplied to the cellulose fiber is reduced, and a sufficiently soft texture cannot be obtained for the cellulose fiber, the bulkiness is lowered, and the antistatic property is also insufficient. When it exceeds 1.5 mass%, the amount of oil supply becomes excessive, resulting in a problem that bulkiness and washing durability are lowered.
本発明の中綿用セルロース繊維の製造方法において、第２工程で、セルロース繊維を絞り率５０％〜１５０％にて遠心脱水する。絞り率をこの範囲に制御することにより、最適の油剤付着量が得
られる。ここで、絞り率は次の式（４）で求めた。
本発明の中綿用セルロース繊維の製造方法において、次に第３工程で、油剤付着セルロース繊維を７６０ｍＨｇ未満の減圧下で加熱処理するが、その圧力は７２０ｍｍＨｇ以下であることが好ましい。７６０ｍＨｇを超える加圧下では、洗濯耐久性や風合いが不十分となり、嵩高反発性が低下し、制電性も不十分となる。 In the method for producing cellulose fiber for batting of the present invention, the oil agent-attached cellulose fiber is then heat-treated at a reduced pressure of less than 760 mHg in the third step, and the pressure is preferably 720 mmHg or less. Under pressure exceeding 760 mHg, washing durability and texture are insufficient, bulky resilience is reduced, and antistatic properties are also insufficient.
第３工程の加熱温度が、１１０℃〜１３０℃の範囲にあればセルロース繊維はより優れたものになる。１１０℃未満だと、洗濯耐久性や風合いが不十分となり、嵩高反発性が低下し、制電性が不十分となる。また、１３０℃を超えるとセルロース繊維が着色するという不具合が生じる。本発明における上記減圧下での熱処理の効果発現は、油剤が繊維表面層にとどまらず、一部が内部に浸潤するためであると推定される。 If the heating temperature in the third step is in the range of 110 ° C. to 130 ° C., the cellulose fibers will be more excellent. When it is less than 110 ° C., washing durability and texture are insufficient, bulky resilience is lowered, and antistatic properties are insufficient. Moreover, when it exceeds 130 degreeC, the malfunction that a cellulose fiber will color arises. The effect of the heat treatment under reduced pressure in the present invention is presumed to be because the oil agent does not stay in the fiber surface layer but partially infiltrates inside.
以下、実施例によって本発明をさらに詳細に説明するが、本発明は該実施例に限定されるものではない。尚、以下の実施例等において、別に記載しない限り部は質量部を示し、％は質量％を示す。 EXAMPLES Hereinafter, although an Example demonstrates this invention further in detail, this invention is not limited to this Example. In the following examples and the like, unless otherwise indicated, parts indicate parts by mass, and% indicates mass%.
試験区分１（アミノ変性シリコーンの合成）
ハイドロジェンポリジメチルシロキサン（両末端ヒドロキシル基、ジメチルシロキサン単位５０個から構成されたもの）３７１８ｇ（１モル）、３−アミノプロピルメチルジメトキシシラン１６４ｇ（１モル）及び触媒として水酸化カリウム３．９ｇ（仕込み量の０．１質量％）を反応容器に仕込み、反応系の温度を１２０℃に保ち、２時間重合反応を行った後、１２０℃で２時間減圧脱水処理し、生成物を得た。これを分析したところ、ｘが１、ｙが５０、Ｍが水素、Ｒが３−アミノプロピル基である式（１）のアミノ変性シリコーン（Ｐ−１）であった。
Test Category 1 (Synthesis of amino-modified silicone)
Hydrogen polydimethylsiloxane (consisting of hydroxyl groups at both ends, 50 dimethylsiloxane units) 3718 g (1 mol), 164 g (1 mol) of 3-aminopropylmethyldimethoxysilane and 3.9 g of potassium hydroxide as a catalyst ( 0.1 mass% of the charged amount) was charged into a reaction vessel, the temperature of the reaction system was kept at 120 ° C., and a polymerization reaction was carried out for 2 hours, followed by vacuum dehydration treatment at 120 ° C. for 2 hours to obtain a product. When this was analyzed, it was an amino-modified silicone (P-1) of the formula (1) in which x is 1, y is 50, M is hydrogen, and R is a 3-aminopropyl group.
アミノ変性シリコーン（Ｐ−１）と同様にして、アミノ変性シリコーン（Ｐ−２）〜（Ｐ−７）及び（ｐ−１）〜（ｐ−２）を合成した。合成した各アミノ変性シリコーンの内容を表１に示す。 In the same manner as amino-modified silicone (P-1), amino-modified silicones (P-2) to (P-7) and (p-1) to (p-2) were synthesized. The contents of each amino-modified silicone synthesized are shown in Table 1.
表１において、ＡＭ−１は３−アミノプロピル基（式（２）中、Ｒ１が炭素数３のプロピレン基、ｚ＝０）、ＡＭ−２はＮ−（２−アミノエチル）−３−アミノプロピル基（式（２）中、Ｒ１が炭素数３のプロピレン基、Ｒ２が炭素数２のエチレン基、ｚ＝１）を表す。 In Table 1, AM-1 is a 3-aminopropyl group (in formula (2), R 1 is a propylene group having 3 carbon atoms, z = 0), and AM-2 is N- (2-aminoethyl) -3- An aminopropyl group (in formula (2), R 1 represents a propylene group having 3 carbon atoms, R 2 represents an ethylene group having 2 carbon atoms, z = 1).
試験区分２（油剤の調製）
Ａ成分としてアミノ変性シリコーン（Ｐ−１）を３０部、アミノ変性シリコーン（Ｐ−２）を３０部、及びアミノ変性シリコーン（Ｐ−３）を３０部と、Ｂ成分として、式（３）で示されるノニオン型界面活性剤（Ｎ−１）を４部及び式（３）で示されるノニオン型界面活性剤（Ｎ−２）を６部とを２０℃〜２５℃の温度で均一になるまで混合した後、撹拌しながら２０℃〜２５℃の水を加え、均一に分散された分散液として油剤（Ｓ−１）を調製した。
Test Category 2 (Preparation of oil)
30 parts of amino-modified silicone (P-1) as component A, 30 parts of amino-modified silicone (P-2), 30 parts of amino-modified silicone (P-3), and B component as formula (3) 4 parts of the nonionic surfactant (N-1) shown and 6 parts of the nonionic surfactant (N-2) shown by formula (3) until uniform at a temperature of 20 ° C to 25 ° C. After mixing, water at 20 ° C. to 25 ° C. was added with stirring to prepare an oil agent (S-1) as a uniformly dispersed dispersion.
油剤（Ｓ−１）と同様にして、油剤（Ｓ−２）〜（Ｓ−７）及び（ｓ−１）〜（ｓ−２）を調製した。これらの油剤の構成成分を表２に示す。 In the same manner as the oil agent (S-1), oil agents (S-2) to (S-7) and (s-1) to (s-2) were prepared. The components of these oils are shown in Table 2.
表２において、数字の単位は部であり、Ｎ−１は、ｎ＝１２、ｍ＝３である式（３）で示されるノニオン型界面活性剤であり、Ｎ−２は、ｎ＝１２、ｍ＝１０である式（３）で示されるノニオン型界面活性剤であり、Ｎ−３は、ｎ＝１２、ｍ＝２０である式（３）で示されるノニオン型界面活性剤である。 In Table 2, the unit of the number is part, N-1 is a nonionic surfactant represented by the formula (3) in which n = 12, m = 3, N-2 is n = 12, It is a nonionic surfactant represented by the formula (3) in which m = 10, and N-3 is a nonionic surfactant represented by the formula (3) in which n = 12, m = 20.
試験区分３（繊維への油剤の付着）
（１）セルロース繊維への油剤の付着
２０〜２５℃に温調した水を撹拌しておき、そこへ試験区分２で調製した等量の油剤を加え、均一な油剤水溶液となるまで撹拌を継続して５０質量％の油剤水溶液を調製し、その後更に水を添加して０．５重量％の水中油滴エマルションを調製した。その中にテンセル（登録商標）（レンチング社製）を含侵させて給油し、その後、遠心脱水させ、最後に密閉式の釜で７００ｍｍＨｇにて減圧し、１２０℃で１時間加熱処理した。
Test category 3 (attachment of oil to fibers)
(1) Adhesion of oil agent to cellulose fiber Stirring water adjusted to 20 to 25 ° C., adding an equal amount of oil agent prepared in Test Category 2, and continuing stirring until a uniform oil agent aqueous solution is obtained. Then, a 50 mass% oil solution was prepared, and then water was further added to prepare a 0.5 wt% oil-in-water emulsion. Tencel (registered trademark) (manufactured by Lenzing Co., Ltd.) was impregnated therein and oiled, and then centrifugal dehydration was performed. Finally, the pressure was reduced at 700 mmHg in a sealed kettle, and heat treatment was performed at 120 ° C. for 1 hour.
（２）ポリエステル繊維への油剤の付着
「テンセル（登録商標）」と同様にして、「テイジン（登録商標）テトロン（登録商標）」（帝人ファイバー社製）へ油剤を付着させた。
(2) Attachment of oil agent to polyester fiber The oil agent was attached to "Teijin (registered trademark) Tetron (registered trademark)" (manufactured by Teijin Fibers Ltd.) in the same manner as "Tencel (registered trademark)".
実施例１〜５、比較例１〜６
種々の油剤及び繊維を組み合わせて得られた本発明の実施例と比較例との比較を行った。各例における油剤の内容、繊維の種類、減圧加熱処理の有無、繊維に対する油剤の付着量を表３に示す。
Examples 1-5, Comparative Examples 1-6
The example of the present invention obtained by combining various oils and fibers was compared with the comparative example. Table 3 shows the contents of the oil agent, the type of fiber, the presence / absence of heat treatment under reduced pressure, and the amount of oil agent attached to the fiber in each example.
表３において、ポリエステルは、帝人ファイバー社製のテイジン（登録商標）テトロン（登録商標）ＴＴ９４Ｖである。 In Table 3, the polyester is Teijin (registered trademark) Tetron (registered trademark) TT94V manufactured by Teijin Fibers Limited.
実施例及び比較例により得られた繊維について、嵩高反発性、制電性、洗濯耐久性及び風合いについて以下の方法で評価した。
＜嵩高反発性＞
試験区分３で減圧下、加熱処理した試料綿をＪＩＳＬ１０９７−１９８２ ５．２及び５．３に記載の方法により比容積、圧縮率を測定して次の式（５）より嵩高反発度を求め、表４の基準で評価した結果を表５に示した。
嵩高反発度＝圧縮率／比容積 （５）
About the fiber obtained by the Example and the comparative example, the following methods evaluated the bulk resilience, antistatic property, washing durability, and texture.
<Bulky resilience>
Under the reduced pressure in Test Category 3, the sample cotton that had been heat-treated was measured for specific volume and compressibility by the method described in JISL 1097-1982 5.2 and 5.3, and the bulk resilience was obtained from the following equation (5). The results of evaluation based on the criteria in Table 4 are shown in Table 5.
Bulkiness rebound = compression ratio / specific volume (5)
＜制電性＞
試験区分３で減圧下、加熱処理した試料綿１００ｇを温度２５℃、相対湿度４０％の条件下で１２時間静置した後、該温湿度条件で、繊維を平行にそろえる工程（カード工程）において５０ｍ／分の速度で走行しているウェブ上１０ｃｍの帯電圧を測定し、表４の基準で評価した結果を表５に示した。
<Electrical control>
In a process (card process) in which 100 g of sample cotton heat-treated under reduced pressure in Test Category 3 is allowed to stand for 12 hours at a temperature of 25 ° C. and a relative humidity of 40%, and then the fibers are aligned in parallel under the temperature and humidity conditions. Table 5 shows the results of measuring the charged voltage of 10 cm on the web running at a speed of 50 m / min and evaluating it according to the criteria shown in Table 4.
＜洗濯耐久性及び風合い＞
試験区分３で減圧下、加熱処理した試料綿２０ｇを温度２５℃、相対湿度６５％の条件下で１２時間静置した後、該温湿度条件でのカード工程において５０ｍ／分の速度で走行して作製したウェブをコットン製の袋（１５ｃｍ×３０ｃｍ）に入れ、洗濯及び乾燥はＪＩＳＬ１０９６−１９９０ ６．２３．１のＡ法にて行い、１０回洗濯した後、風合いを触感により５段階で判定し、羽毛調のヌメリ感のあることを望ましいとした。触感評価は１０名で行い、５が最も羽毛調のヌメリ感があるとし、１０名の評価の平均値を求め、表４の基準で評価した結果を表５に示した。
<Washing durability and texture>
20 g of sample cotton heat-treated under reduced pressure in Test Category 3 was allowed to stand for 12 hours under conditions of a temperature of 25 ° C. and a relative humidity of 65%, and then traveled at a speed of 50 m / min in the card process under the temperature and humidity conditions. The web prepared in this way is put in a cotton bag (15cm x 30cm), washed and dried by the method A of JISL 1096-1990 6.23.1, washed 10 times, and the texture is determined by tactile sense in 5 stages. In addition, it is desirable that there is a feeling of feathery tone. Evaluation of tactile sensation was performed by 10 people, 5 is the most feathery slime feeling, the average value of the evaluation of 10 people was obtained, and the results of evaluation based on the criteria in Table 4 are shown in Table 5.
表３の試料について上述の評価を行い、その結果を表４に示した。また、評価については、◎は優秀、○は良好、△はやや不良、×は不可とした４段階で判定を行った。 The above-described evaluation was performed on the samples in Table 3, and the results are shown in Table 4. In addition, the evaluation was made in four stages, with ◎ being excellent, ○ being good, Δ being slightly poor, and × being impossible.
本発明のセルロース系繊維は、布団、枕、ぬいぐるみ、クッションなどの日用品や、ダウンジャケットなどの衣料分野など幅広い分野で利用できる。 The cellulosic fiber of the present invention can be used in a wide range of fields such as daily necessities such as futons, pillows, stuffed animals, and cushions, and clothing such as down jackets.
Claims (5)
（第１工程）下記のＡ成分と下記のＢ成分をＡ成分／Ｂ成分＝９９／１〜９０／１０の質量比で含有する油剤の油剤濃度が０．１質量％〜２．０質量％の水中油滴エマルションを調製し、前記水中油滴エマルションをセルロース繊維に含侵させて給油する工程；
（第２工程）前記第１工程の後に、前記セルロース繊維を絞り率５０％〜１５０％にて遠心脱水し、前記油剤を前記セルロース繊維に対して０．２質量％〜１．５質量％の割合で付着させる工程；
（第３工程）前記第２工程の後に、前記セルロース繊維を減圧下で加熱処理する工程
を経ることを特徴とする前記製造方法。
Ａ成分：アミノ当量が３０００グラム／ｍｏｌ〜１５０００グラム／ｍｏｌである式（１）で示されるアミノ変性シリコーン
Ｒは、式（２）
で示される有機基であり、
ｘは、１〜２０の整数であり、そして、
ｙは、４０〜１０００の整数である。）
Ｂ成分：式（３）で示されるノニオン型界面活性剤
(1st process) Oil agent concentration of the oil agent which contains the following A component and the following B component by the mass ratio of A component / B component = 99/1-90/10 is 0.1 mass%-2.0 mass% Preparing an oil-in-water emulsion, and impregnating the oil-in-water emulsion with cellulose fibers to supply oil;
(Second step) After the first step, the cellulose fibers are centrifugally dehydrated at a drawing rate of 50% to 150%, and the oil agent is 0.2% by mass to 1.5% by mass with respect to the cellulose fibers. Applying at a rate;
(Third step) The method according to claim 3, wherein after the second step, the cellulose fiber is subjected to a heat treatment under reduced pressure.
Component A: amino-modified silicone represented by formula (1) having an amino equivalent of 3000 to 15000 g / mol
R is the formula (2)
An organic group represented by
x is an integer from 1 to 20, and
y is an integer of 40 to 1000. )
Component B: Nonionic surfactant represented by the formula (3)
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014043665A (en) * | 2012-07-30 | 2014-03-13 | Asahi Kasei Fibers Corp | Cellulose fiber cotton and treatment method |
| TWI618975B (en) * | 2016-12-28 | 2018-03-21 | Micro Lithography Inc | Photomask dustproof frame structure |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01266277A (en) * | 1988-04-19 | 1989-10-24 | Mitsubishi Rayon Co Ltd | Antimicrobial treatment of yarn |
| WO2005085517A1 (en) * | 2004-03-03 | 2005-09-15 | Sumitomo Corporation | Method for making fibrous structure hydrophobic |
| JP2008196082A (en) * | 2007-02-14 | 2008-08-28 | Shin Etsu Chem Co Ltd | Fiber-treating agent |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH01266277A (en) * | 1988-04-19 | 1989-10-24 | Mitsubishi Rayon Co Ltd | Antimicrobial treatment of yarn |
| WO2005085517A1 (en) * | 2004-03-03 | 2005-09-15 | Sumitomo Corporation | Method for making fibrous structure hydrophobic |
| JP2008196082A (en) * | 2007-02-14 | 2008-08-28 | Shin Etsu Chem Co Ltd | Fiber-treating agent |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014043665A (en) * | 2012-07-30 | 2014-03-13 | Asahi Kasei Fibers Corp | Cellulose fiber cotton and treatment method |
| TWI618975B (en) * | 2016-12-28 | 2018-03-21 | Micro Lithography Inc | Photomask dustproof frame structure |
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