JP7357353B2 - Method for producing liquid crystal emulsion for kneading rayon and rayon fiber - Google Patents
Method for producing liquid crystal emulsion for kneading rayon and rayon fiber Download PDFInfo
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Description
本発明は、レーヨン練り込み用液晶乳化型エマルションの作製方法及びレーヨン繊維に関するものである。 The present invention relates to a method for producing a liquid crystal emulsion for kneading rayon, and to rayon fibers.
セルロースは周知のとおり、地球上に最も多く存在するバイオマス資源であり、環境配慮型素材として注目されている。 As is well known, cellulose is the most abundant biomass resource on earth and is attracting attention as an environmentally friendly material.
このセルロースを用いて製造されるレーヨン繊維は、古くから、衣料等の用途に用いられており、さらに、スクワラン、椿油等の油成分（非水溶性機能性物質）を練り込んだ機能性物質を含有するレーヨン繊維も提案されている（例えば、特許文献１参照。）。 Rayon fibers manufactured using this cellulose have been used for clothing and other purposes since ancient times, and are also made with functional substances kneaded with oil components (water-insoluble functional substances) such as squalane and camellia oil. A rayon fiber containing rayon fibers has also been proposed (for example, see Patent Document 1).
一方、油成分（非水溶性機能性物質）以外の機能性物質、特に、水溶性機能性物質は、従来の油成分（非水溶性機能性物質）を含有するレーヨン繊維の製造方法では、レーヨン繊維の製造工程中でその成分が繊維系外に流出してしまい、レーヨン繊維中に水溶性機能性物質が残存させることが困難であった。 On the other hand, functional substances other than oil components (water-insoluble functional substances), especially water-soluble functional substances, cannot be used in conventional methods for producing rayon fibers containing oil components (water-insoluble functional substances). During the fiber manufacturing process, the components flow out of the fiber system, making it difficult to allow water-soluble functional substances to remain in the rayon fibers.
本発明は、従来の油成分（非水溶性機能性物質）を含有するレーヨン繊維の製造方法では製造することができなかった、水溶性機能性物質を含有するレーヨン繊維を製造するためのレーヨン練り込み用液晶乳化型エマルションの作製方法を提供することを目的とする。 The present invention is a rayon kneading method for producing rayon fibers containing water-soluble functional substances, which could not be produced using conventional methods for producing rayon fibers containing oil components (water-insoluble functional substances). The object of the present invention is to provide a method for producing a liquid crystal emulsion for liquid crystal emulsion.
上記目的を達成するため、本発明のレーヨン練り込み用液晶乳化型エマルションの作製方法は、水溶性機能性物質及び非イオン系界面活性剤を含む液晶乳化用混合物を作製し、該液晶乳化用混合物に有極性シリコンオイルを滴下し、液晶乳化原体を作製し、該液晶乳化原体に水を滴下してレーヨン練り込み用Ｏ／Ｗ型液晶乳化型エマルションを作製することを特徴とする。 In order to achieve the above object, the method for producing a liquid crystal emulsion type emulsion for kneading rayon of the present invention includes producing a liquid crystal emulsion mixture containing a water-soluble functional substance and a nonionic surfactant, A liquid crystal emulsion base material is prepared by dropping polar silicone oil onto the liquid crystal emulsion base material, and water is dropped onto the liquid crystal emulsion base material to produce an O/W type liquid crystal emulsion type emulsion for kneading rayon.
この場合において、前記水溶性機能性物質に、生薬成分を用いることができる。 In this case, a crude drug component can be used as the water-soluble functional substance.
本発明の水溶性機能性物質を含有するレーヨン練り込み用液晶乳化型エマルションの製造方法によって作製されるレーヨン練り込み用液晶乳化型エマルションを用いることによって、従来の油成分（非水溶性機能性物質）を含有するレーヨン繊維の製造方法では製造することができなかった、水溶性機能性物質を含有するレーヨン繊維を製造することができる。 By using the liquid crystal emulsion type emulsion for rayon kneading produced by the manufacturing method of the liquid crystal emulsion type emulsion type for rayon kneading containing the water-soluble functional substance of the present invention, the conventional oil component (water-insoluble functional substance ) It is possible to produce rayon fibers containing water-soluble functional substances, which could not be produced using methods for producing rayon fibers containing water-soluble functional substances.
以下、本発明のセルロース溶液の作製方法の実施の形態を説明する。 Hereinafter, embodiments of the method for producing a cellulose solution of the present invention will be described.
本発明の水溶性機能性物質を含有するレーヨン練り込み用液晶乳化型エマルションの作製方法は、従来の油成分（非水溶性機能性物質）を含有するレーヨン繊維の製造方法では製造することができなかった、水溶性機能性物質を含有するレーヨン繊維を製造するために用いる、レーヨン練り込み用Ｏ／Ｗ型（水を連続相とする水中油滴型）液晶乳化型エマルションを作製するものである。 The method for producing the liquid crystal emulsion for kneading into rayon containing the water-soluble functional substance of the present invention cannot be produced using the conventional method for producing rayon fiber containing an oil component (water-insoluble functional substance). This is to create an O/W type (oil-in-water type with water as a continuous phase) liquid crystal emulsion type emulsion for kneading rayon, which is used to manufacture rayon fibers containing water-soluble functional substances. .
ここで、従来、例えば、繊維加工剤において、Ｗ／Ｏ型（油を連続相とする油中水滴型）のエマルション加工剤は、加工剤の作りやすさから汎用されているが、水溶性機能性物質を担持するＯ／Ｗ型エマルションは、作製に技術的な難易度が高いため、作製が試みられていなかった。 Conventionally, for example, in textile processing agents, W/O type (water-in-oil type with oil as a continuous phase) emulsion processing agent has been widely used because it is easy to make a processing agent, but it has a water-soluble function. No attempt has been made to produce an O/W type emulsion that supports a sexual substance because it is technically difficult to produce.
本発明の水溶性機能性物質を含有するレーヨン練り込み用液晶乳化型エマルションの作製方法は、水溶性機能性物質及び非イオン系界面活性剤を含む液晶乳化用混合物を作製し、該液晶乳化用混合物に有極性シリコンオイルを滴下し、液晶乳化原体を作製し、該液晶乳化原体に水を滴下してレーヨン練り込み用Ｏ／Ｗ型液晶乳化型エマルションを作製するものである。 The method for producing a liquid crystal emulsion type emulsion for kneading rayon containing a water-soluble functional substance of the present invention includes preparing a liquid crystal emulsion mixture containing a water-soluble functional substance and a nonionic surfactant, and Polar silicone oil is added dropwise to the mixture to prepare a liquid crystal emulsion base material, and water is added dropwise to the liquid crystal emulsion base material to prepare an O/W type liquid crystal emulsion type emulsion for kneading rayon.
ここで、水溶性機能物質（Ａ）としては、生薬成分の高麗人参エキス、甘草エキス、ウコンエキス、アロエエキス等、水溶性アミノ酸のアスパラギン、アスパラギン酸、システィン、グルタミン、グリシン、リシン、ヒスチジン、アルギニン、トレオニン、セリン、チロシン等、水溶性ビタミンのアスコルビン酸、ナイアシン、パントテン酸、葉酸等を挙げることができるが、これらに限定されるものではない。 Here, the water-soluble functional substances (A) include crude drug ingredients such as ginseng extract, licorice extract, turmeric extract, and aloe extract, and water-soluble amino acids asparagine, aspartic acid, cysteine, glutamine, glycine, lysine, histidine, and arginine. , threonine, serine, tyrosine, etc., water-soluble vitamins such as ascorbic acid, niacin, pantothenic acid, folic acid, etc., but are not limited to these.
また、非イオン系界面活性剤（Ｂ）としては、ポリオキシエチレンラウリルエーテル、ポリオキシエチレンステアリルエーテル、ポリオキシエチレンオレイルエーテル、ポリオキシエチレンセチルエーテル、ポリオキシエチレンセカンダリーアルコールエーテル、ポリオキシエチレンスチレン化フェニルエーテル、ポリオキシエチレンイソデシルエーテル、ポリオキシアルキレントリデシルエーテル等を挙げることができるが、これらに限定されるものではない。 In addition, as the nonionic surfactant (B), polyoxyethylene lauryl ether, polyoxyethylene stearyl ether, polyoxyethylene oleyl ether, polyoxyethylene cetyl ether, polyoxyethylene secondary alcohol ether, polyoxyethylene styrenated Examples include, but are not limited to, phenyl ether, polyoxyethylene isodecyl ether, polyoxyalkylene tridecyl ether, and the like.
また、有極性シリコンオイル（Ｃ）としては、アミノ変性シリコンオイル、カルボニル変性シリコンオイル、カルビノール変性シリコンオイル、ポリエーテル変性シリコンオイル、メチルハイドロジェンポリシロキサン、アミノ／アルコキシ変性シリコンオイルエポキシ／ポリエーテルシリコンオイル、アミノ／ポリエーテルシリコンオイル等を挙げることができるが、これらに限定されるものではない。
ここで、有極性シリコンオイルを用いると、レーヨン練り込み用Ｏ／Ｗ型液晶乳化型エマルションを作製することができるが、例えば、無極性シリコンオイルを用いても、安定したＯ／Ｗ型液晶乳化型エマルションを作製することができない。
In addition, as the polar silicone oil (C), amino-modified silicone oil, carbonyl-modified silicone oil, carbinol-modified silicone oil, polyether-modified silicone oil, methyl hydrogen polysiloxane, amino/alkoxy-modified silicone oil epoxy/polyether Examples include, but are not limited to, silicone oil, amino/polyether silicone oil, and the like.
Here, if a polar silicone oil is used, an O/W type liquid crystal emulsion for kneading rayon can be produced, but even if a nonpolar silicone oil is used, a stable O/W type liquid crystal emulsion can be produced. It is not possible to make a mold emulsion.
また、水溶性機能物質（Ａ）及び非イオン系界面活性剤（Ｂ）並びに有極性シリコンオイル（Ｃ）の配合割合は、（Ａ）を５～３０重量部、好ましくは１０～２０重量部、（Ｂ）を５～１５重量部、好ましくは８～１２重量部、（Ｃ）を２０～４０重量部、好ましくは、２０～３５重量部で、水（「湯」を含む。以下、同じ。）を加え１００重量部とする配合割合がよい。この配合割合を外れると安定したＯ／Ｗ型液晶乳化型エマルションを作製することができないか、あるいは、粘度が高まりレーヨン練り込みの用途に使用することが困難となる。 In addition, the blending ratio of the water-soluble functional substance (A), the nonionic surfactant (B), and the polar silicone oil (C) is 5 to 30 parts by weight, preferably 10 to 20 parts by weight, (B) in an amount of 5 to 15 parts by weight, preferably 8 to 12 parts by weight, and (C) in an amount of 20 to 40 parts by weight, preferably 20 to 35 parts by weight, and water (including "hot water"). The same applies hereinafter. ) is preferably added to make 100 parts by weight. If the blending ratio is outside this range, a stable O/W type liquid crystal emulsion cannot be produced, or the viscosity increases, making it difficult to use it for kneading rayon.
ここで、水溶性機能性物質（Ａ）及び非イオン系界面活性剤（Ｂ）を含む液晶乳化用混合物を作製するに当たっては、必要に応じて、少量（０．０５～１．０重量部、好ましくは０．１～０．５重量部）の酢酸、コハク酸、カルボン酸、乳酸、マロン酸、リンゴ酸、酒石酸、クエン酸等の酸を加えることで、錯体物質を形成させ、乳化を行いやすくすることができる。 Here, when preparing a liquid crystal emulsifying mixture containing a water-soluble functional substance (A) and a nonionic surfactant (B), a small amount (0.05 to 1.0 parts by weight, By adding an acid such as acetic acid, succinic acid, carboxylic acid, lactic acid, malonic acid, malic acid, tartaric acid, citric acid, etc. (preferably 0.1 to 0.5 parts by weight), a complex substance is formed and emulsified. It can be made easier.
水溶性機能性物質及び非イオン系界面活性剤を含む液晶乳化用混合物は、水溶性機能性物質及び非イオン系界面活性剤の混合物に水を滴下することで作製することができる。 A liquid crystal emulsifying mixture containing a water-soluble functional substance and a nonionic surfactant can be prepared by dropping water into a mixture of the water-soluble functional substance and nonionic surfactant.
また、液晶乳化用混合物、液晶乳化原体及び液晶乳化型エマルションの作製には、ホモジナイザ等の従来汎用されている各種の混合撹拌機を用いることができる。 In addition, various conventionally used mixing and stirring machines such as a homogenizer can be used to prepare the liquid crystal emulsion mixture, the liquid crystal emulsion raw material, and the liquid crystal emulsion type emulsion.
以下、本発明の水溶性機能性物質を含有するレーヨン練り込み用液晶乳化型エマルションの作製方法を実施例によって詳細に説明する。 EXAMPLES Hereinafter, a method for producing a liquid crystal emulsion for kneading into rayon containing a water-soluble functional substance of the present invention will be explained in detail with reference to Examples.
＜Ｏ／Ｗ型液晶乳化型エマルションを作製方法＞
水溶性機能物質（Ａ）として高麗人参エキスを１５重量部、非イオン系界面活性剤（Ｂ）としてポリオキシエチレンセカンダリーアルコールエーテルを１０重量部、９０％酢酸０．２重量部に、同量程度の水を加えて液晶乳化用混合物を作製し、その中に有極性シリコンオイル（Ｃ）としてアミノ変性シリコンオイル３０重量部を少量ずつ加え、Ｗ／Ｏ型液晶乳化原体を作製し、その中に水を滴下して、固形分濃度４８％の高麗人参エキスを含有するレーヨン練り込み用Ｏ／Ｗ型液晶乳化型エマルションを作製した。
<Method for producing O/W type liquid crystal emulsion>
15 parts by weight of ginseng extract as the water-soluble functional substance (A), 10 parts by weight of polyoxyethylene secondary alcohol ether as the nonionic surfactant (B), and 0.2 parts by weight of 90% acetic acid, about the same amount. of water to prepare a liquid crystal emulsifying mixture, and 30 parts by weight of amino-modified silicone oil as polar silicone oil (C) was added little by little to the mixture to prepare a W/O type liquid crystal emulsifying raw material. Water was added dropwise to prepare an O/W type liquid crystal emulsion type emulsion for kneading into rayon containing ginseng extract with a solid content concentration of 48%.
＜実施例１：高麗人参エキス練り込みレーヨン繊維の製造方法＞
原料パルプを約１８％の苛性ソーダ水溶液に浸漬し、圧搾・粉砕によりアルカリセルロースを得た。
これを老成し、その後、二硫化炭素を反応させセルロースザンテートとし、これを希苛性ソーダ溶液に溶解させてビスコースを調製した。このビスコースは、セルロース含有率８．６％、アルカリ含有率４．８％で、粘度が５０秒（落球粘度）である。
このビスコース溶液に、作製した高麗人参エキスを含有するレーヨン練り込み用Ｏ／Ｗ型液晶乳化型エマルションを、セルロース重量に対して５．０重量％添加し、均一に混合して紡糸原液を調製した。
得られた紡糸原液をノズル径０．０６ｍｍ、孔数１３０００ホールのノズルから、紡糸速度６０ｍ／分にて凝固浴中へ紡糸し、次いで、延伸、切断を行い、繊度１．４デシテックス、繊維長３８ｍｍのレーヨン繊維を得た。凝固浴は、硫酸９５ｇ／Ｌ、硫酸ナトリウム３５０ｇ／Ｌ、硫酸亜鉛１２．５ｇ／Ｌ含有したもので、温度は４７℃にしたものである。
<Example 1: Method for producing rayon fiber mixed with ginseng extract>
The raw material pulp was immersed in an approximately 18% aqueous solution of caustic soda, and then compressed and crushed to obtain alkali cellulose.
This was aged and then reacted with carbon disulfide to form cellulose xanthate, which was dissolved in dilute caustic soda solution to prepare viscose. This viscose has a cellulose content of 8.6%, an alkali content of 4.8%, and a viscosity of 50 seconds (falling ball viscosity).
To this viscose solution, 5.0% by weight of the O/W type liquid crystal emulsion for kneading into rayon containing the prepared Korean ginseng extract was added to the cellulose weight, and the mixture was uniformly mixed to prepare a spinning dope. did.
The obtained spinning stock solution was spun into a coagulation bath at a spinning speed of 60 m/min through a nozzle with a nozzle diameter of 0.06 mm and 13,000 holes, and then stretched and cut to obtain a fineness of 1.4 dtex and fiber length. A 38 mm rayon fiber was obtained. The coagulation bath contained 95 g/L of sulfuric acid, 350 g/L of sodium sulfate, and 12.5 g/L of zinc sulfate, and was kept at a temperature of 47°C.
＜実施例２：高麗人参エキス練り込みレーヨン繊維の製造方法＞
上記ビスコース溶液に、作製した高麗人参エキスを含有するレーヨン練り込み用Ｏ／Ｗ型液晶乳化型エマルションを、セルロース重量に対して１０．０重量％添加し、均一に混合して紡糸原液を調製した。
得られた紡糸原液をノズル径０．０６ｍｍ、孔数１３０００ホールのノズルから、紡糸速度６０ｍ／分にて凝固浴中へ紡糸し、次いで、延伸、切断を行い、繊度１．４デシテックス、繊維長３８ｍｍのレーヨン繊維を得た。凝固浴は、硫酸９５ｇ／Ｌ、硫酸ナトリウム３５０ｇ／Ｌ、硫酸亜鉛１２．５ｇ／Ｌ含有したもので、温度は４７℃にしたものである。
<Example 2: Method for producing rayon fiber mixed with ginseng extract>
To the above viscose solution, 10.0% by weight of the O/W liquid crystal emulsion for kneading into rayon containing the prepared Korean ginseng extract was added to the cellulose weight, and mixed uniformly to prepare a spinning dope. did.
The obtained spinning stock solution was spun into a coagulation bath at a spinning speed of 60 m/min through a nozzle with a nozzle diameter of 0.06 mm and 13,000 holes, and then stretched and cut to obtain a fineness of 1.4 dtex and fiber length. A 38 mm rayon fiber was obtained. The coagulation bath contained 95 g/L of sulfuric acid, 350 g/L of sodium sulfate, and 12.5 g/L of zinc sulfate, and was kept at a temperature of 47°C.
＜レーヨン繊維中の高麗人参エキスの定性試験＞
実施例１及び２で得たレーヨン繊維が、水溶性機能性物質の高麗人参エキスを含有するレーヨン繊維であることを、以下の試験方法によって確認した。
実施例１及び２で得たレーヨン繊維を、５０％メタノール水溶液で１時間リフラックス抽出を実施した。その上澄み液を採取し、エバポレーションにより約２ｍｌに濃縮し、不溶物をメンブレンフィルタでろ過して、そのろ液を液体クロマトグラフィー質量分析機（島津製作所社製ＬＣ２０シリーズ）にて分析を行った。
その結果、６５．２分付近に高麗人参エキス特有のピークがみられ、レーヨン繊維中に高麗人参エキスが含有されていることを確認した。
<Qualitative test of ginseng extract in rayon fiber>
It was confirmed by the following test method that the rayon fibers obtained in Examples 1 and 2 were rayon fibers containing ginseng extract, which is a water-soluble functional substance.
The rayon fibers obtained in Examples 1 and 2 were subjected to reflux extraction for 1 hour with a 50% methanol aqueous solution. The supernatant liquid was collected and concentrated to approximately 2 ml by evaporation, insoluble matter was filtered with a membrane filter, and the filtrate was analyzed using a liquid chromatography mass spectrometer (LC20 series manufactured by Shimadzu Corporation). .
As a result, a peak unique to ginseng extract was observed around 65.2 minutes, and it was confirmed that ginseng extract was contained in the rayon fiber.
以上、本発明の水溶性機能性物質を含有するレーヨン練り込み用液晶乳化型エマルションの作製方法について、その実施の形態に基づいて説明したが、本発明は上記実施の形態に記載した構成に限定されるものではなく、その趣旨を逸脱しない範囲において適宜その構成を変更することができるものである。 The method for producing a liquid crystal emulsion for kneading rayon containing a water-soluble functional substance of the present invention has been described above based on the embodiment, but the present invention is limited to the configuration described in the above embodiment. However, the configuration may be changed as appropriate without departing from the spirit of the invention.
本発明の水溶性機能性物質を含有するレーヨン練り込み用液晶乳化型エマルションの作製方法によれば、レーヨン練り込み用液晶乳化型エマルションの作製方法を提供するもので、油成分（非水溶性機能性物質）を含有するレーヨン繊維の製造方法では製造することができなかった、水溶性機能性物質を含有するレーヨン繊維を製造するために好適に用いることができる。 According to the method for producing a liquid crystal emulsion type emulsion for kneading rayon containing a water-soluble functional substance of the present invention, a method for producing a liquid crystal emulsion type emulsion for kneading rayon is provided. It can be suitably used to produce rayon fibers containing water-soluble functional substances, which could not be produced using methods for producing rayon fibers containing water-soluble functional substances.
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| JP2010037683A (en) | 2008-08-05 | 2010-02-18 | Toray Ind Inc | Denim fabric |
| JP2010116656A (en) | 2008-11-14 | 2010-05-27 | Daiwabo Holdings Co Ltd | Functionalizing agent-containing rayon fiber and method for producing the rayon fiber |
| JP2010121229A (en) | 2008-11-18 | 2010-06-03 | Daiwabo Holdings Co Ltd | Rayon fiber containing tea-originated component and method for producing the same |
| CN105381766A (en) | 2015-12-09 | 2016-03-09 | 山传雷 | Preparation method and applications of isatis root extract, vitamin and protein composite microcapsule |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2010037683A (en) | 2008-08-05 | 2010-02-18 | Toray Ind Inc | Denim fabric |
| JP2010116656A (en) | 2008-11-14 | 2010-05-27 | Daiwabo Holdings Co Ltd | Functionalizing agent-containing rayon fiber and method for producing the rayon fiber |
| JP2010121229A (en) | 2008-11-18 | 2010-06-03 | Daiwabo Holdings Co Ltd | Rayon fiber containing tea-originated component and method for producing the same |
| CN105381766A (en) | 2015-12-09 | 2016-03-09 | 山传雷 | Preparation method and applications of isatis root extract, vitamin and protein composite microcapsule |
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