JP2018178352A - Treatment agent for polyester based synthetic fiber and polyester based synthetic fiber - Google Patents
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本発明は、ポリエステル系合成繊維用処理剤及びかかるポリエステル系合成繊維用処理剤が付着したポリエステル系合成繊維に関する。 The present invention relates to a polyester-based synthetic fiber treating agent and a polyester-based synthetic fiber to which such a polyester-based synthetic fiber treating agent is attached.
従来、ポリエステル系合成繊維処理剤として、有機リン酸エステルアルカリ金属塩、特定のワックス又は線状ポリオルガノシロキサン、特定の非イオン界面活性剤を含有する処理剤(特許文献1)、有機リン酸エステルアルカリ金属塩、特定のワックス、特定の線状ポリオルガノシロキサン、特定の非イオン界面活性剤を含有する処理剤(特許文献2)、アルキルリン酸エステルのアルカリ金属塩、特定の非イオン界面活性剤、リン酸金属塩を含有する処理剤(特許文献3)等が提案されている。 Conventionally, an organic phosphate ester alkali metal salt, a specific wax or linear polyorganosiloxane, a specific non-ionic surfactant-containing treatment agent (Patent Document 1), an organic phosphate ester as a polyester-based synthetic fiber treatment agent Alkali metal salts, specific waxes, specific linear polyorganosiloxanes, treatment agents containing specific nonionic surfactants (Patent Document 2), alkali metal salts of alkyl phosphates, specific nonionic surfactants And treating agents containing a metal salt of phosphoric acid (Patent Document 3) and the like have been proposed.
また、特定のアルキルリン酸エステルカリウム塩と、特定のアルキルリン酸エステルカリウム塩と、ポリオキシアルキレンアルキルエーテル、ポリオキシアルキレンアルケニルエーテル及びポリオキシアルキレン(アルキルフェニル)エーテルから選ばれる少なくとも1種とを含有して成る繊維処理剤(特許文献4)、特定のアルキルリン酸エステルカリウム塩と、アクリル樹脂とを特定の比率で含有する繊維処理剤(特許文献5)が開示されている。更に、リン酸類のアルカリ金属塩を重要成分として添加含有する合成繊維処理用油剤(特許文献6)が開示されている。 In addition, a specific alkyl phosphate ester potassium salt, a specific alkyl phosphate ester potassium salt, and at least one selected from polyoxyalkylene alkyl ether, polyoxyalkylene alkenyl ether and polyoxyalkylene (alkylphenyl) ether A fiber treatment agent (Patent Document 5) containing a fiber treatment agent (Patent Document 4), a specific alkyl phosphoric acid ester potassium salt, and an acrylic resin in a specific ratio is disclosed. Furthermore, an oil for synthetic fiber treatment (Patent Document 6) is disclosed, which contains an alkali metal salt of phosphoric acid as an important component.
上記特許文献に例示したように種々の繊維用処理剤が提案されている。しかしながら、高性能な処理剤として、市場では、紡糸工程での優れたトウの集束性、延伸工程での優れた延伸性を兼ね備え、更に、紡績工程での発生電気の抑制が可能であるポリエステル合成繊維、並びにその処理剤が切望されている。 Various fiber treatment agents have been proposed as exemplified in the above-mentioned patent documents. However, as a high-performance processing agent, in the market, polyester synthesis that combines excellent tow focusing in the spinning process and excellent stretchability in the drawing process, and can further suppress generated electricity in the spinning process Fibers, as well as their treatment, are desired.
本発明は上記背景に鑑みてなされたものであり、紡糸工程でのトウの優れた集束性および延伸工程での優れた延伸性を兼ね備え、且つ紡績工程での発生電気の抑制が可能なポリエステル系合成繊維用処理剤、並びにかかるポリエステル系合成繊維用処理剤が付着したポリエステル系合成繊維を提供することを課題とする。 The present invention has been made in view of the above background, and it is a polyester system which has both excellent focusing property of tow in the spinning process and excellent stretchability in the drawing process, and can suppress generated electricity in the spinning process. An object of the present invention is to provide a synthetic fiber treating agent, and a polyester synthetic fiber to which such a polyester synthetic fiber treating agent is attached.
本発明者らが鋭意研究を重ねた結果、特定の3成分と非イオン界面活性剤を特定の割合で含有して成るポリエステル系合成繊維用処理剤を用いることにより本発明の課題を解決できることを見出し、本発明を完成するに至った。 As a result of intensive studies by the present inventors, it is possible to solve the problems of the present invention by using a polyester-based synthetic fiber treatment agent comprising specific three components and a nonionic surfactant in a specific ratio. The present invention has been completed.
すなわち本発明は、下記の長鎖アルキルリン酸エステル塩を20〜88.99質量%、下記の短鎖アルキルリン酸エステル塩を1〜10質量%、下記の無機リン酸塩を0.01〜10質量%及び非イオン界面活性剤を10〜65質量%(合計100質量%)の割合で含有して成ることを特徴とするポリエステル系合成繊維用処理剤及びかかるポリエステル系合成繊維用処理剤が付着したポリエステル系合成繊維に係る。 That is, according to the present invention, 20 to 88.99% by mass of the following long chain alkyl phosphate ester salt, 1 to 10% by mass of the following short chain alkyl phosphate ester salt, and 0.01 to 50% by mass of the following inorganic phosphate A treating agent for a polyester based synthetic fiber characterized by comprising 10% by mass and 10 to 65% by mass (totally 100% by mass) of a nonionic surfactant and such a treating agent for a polyester based synthetic fiber Pertaining to attached polyester synthetic fiber.
長鎖アルキルリン酸エステル塩:アルキル基の炭素数が16〜18のアルキルリン酸エステルのアルカリ金属塩。 Long chain alkyl phosphoric acid ester salt: Alkali metal salt of alkyl phosphoric acid ester having 16 to 18 carbon atoms in alkyl group.
短鎖アルキルリン酸エステル塩:アルキル基の炭素数が4〜8のアルキルリン酸エステルのアルカリ金属塩。 Short-chain alkyl phosphate ester salt: Alkali metal salt of alkyl phosphate ester having 4 to 8 carbon atoms in alkyl group.
無機リン酸塩:リン酸水素二金属塩及びリン酸三金属塩から選ばれる少なくとも一つ。 Inorganic phosphate: at least one selected from bimetallic hydrogen phosphate and trimetallic phosphoric acid.
先ず、本発明に係るポリエステル系合成繊維用処理剤(以下、本発明の処理剤ともいう)について説明する。本発明の処理剤は、特定の3成分と非イオン界面活性剤を特定の割合で含有して成るポリエステル系合成繊維用処理剤である。 First, the polyester-based synthetic fiber treatment agent according to the present invention (hereinafter, also referred to as the treatment agent of the present invention) will be described. The treating agent of the present invention is a treating agent for polyester based synthetic fibers comprising a specific three component and a nonionic surfactant in a specific ratio.
本発明の処理剤に供する長鎖アルキルリン酸エステル塩としては、ヘキサデシルリン酸エステルアルカリ金属塩、オクタデシルリン酸エステルアルカリ金属塩、イソステアリルリン酸エステルアルカリ金属塩等の、アルキル基の炭素数が16〜18のアルキルリン酸エステルのアルカリ金属塩が挙げられる。 As long-chain alkyl phosphate ester salts to be used for the treatment agent of the present invention, carbon number of alkyl group such as hexadecyl phosphate alkali metal salt, octadecyl phosphate alkali metal salt, isostearyl phosphate alkali metal salt, etc. And an alkali metal salt of an alkyl phosphoric acid ester of 16-18.
本発明の処理剤に供する短鎖アルキルリン酸エステル塩としては、ノルマルブチルリン酸エステルアルカリ金属塩、ヘキシルリン酸エステルアルカリ金属塩、オクチルリン酸エステルアルカリ金属塩等のアルキル基の炭素数が4〜8のアルキルリン酸エステルのアルカリ金属塩が挙げられる。こらのなかでもノルマルブチルリン酸エステルアルカリ金属塩、ヘキシルリン酸エステルアルカリ金属塩等のアルキル基の炭素数が4〜6の短鎖アルキルリン酸エステル塩が好ましい。 The short chain alkyl phosphoric acid ester salt to be used in the treatment agent of the present invention includes 4 to 25 carbon atoms of alkyl group such as normal butyl phosphoric acid ester alkali metal salt, hexyl phosphoric acid ester alkali metal salt, octyl phosphoric acid ester alkali metal salt and the like. Alkali metal salts of alkyl phosphates of 8 can be mentioned. Among these, short-chain alkyl phosphate ester salts having 4 to 6 carbon atoms in the alkyl group such as normal butyl phosphate ester alkali metal salts and hexyl phosphate ester alkali metal salts are preferable.
本発明の処理剤に供する無機リン酸塩は、リン酸水素二金属塩及びリン酸三金属塩から選ばれる少なくとも一つであるが、なかでもリン酸水素二金属塩が好ましい。具体的にリン酸水素二金属塩としてはリン酸水素二カリウム塩、リン酸水素二ナトリウム塩等が挙げられ、リン酸三金属塩としてはリン酸三カリウム塩、リン酸三ナトリウム塩等が挙げられる。 The inorganic phosphate to be used for the treatment agent of the present invention is at least one selected from hydrogen phosphate bimetallic salts and phosphoric acid trimetallic salts, and among them, hydrogen phosphate bimetallic salts are preferable. Specifically, examples of the bimetallic hydrogen phosphate include dipotassium hydrogen phosphate and disodium hydrogen phosphate, and examples of the trimetallic phosphate include tripotassium phosphate and trisodium phosphate. Be
本発明の処理剤に供する非イオン界面活性剤としては、α−ドデシル−ω−ヒドロキシポリオキシエチレン(n=10)、α−ドデシル−ω−ヒドロキシポリオキシエチレンポリオキシプロピレン(n+m=10)、α−ドデシルアミノ−ω−ヒドロキシポリオキシエチレン(n=10)、α−ノニルフェニル−ω−ヒドロキシポリオキシエチレン(n=10)、α−ドデシルアミノ−ω−ヒドロキシポリオキシエチレン(n=10)等が挙げられる。ここでnはオキシエチレン単位の数を意味し、n+mはオキシエチレン単位の数とオキシプロピレン単位の数の合計数を意味し、以降同様とする。 As a nonionic surfactant to be provided for the treatment agent of the present invention, α-dodecyl-ω-hydroxypolyoxyethylene (n = 10), α-dodecyl-ω-hydroxypolyoxyethylene polyoxypropylene (n + m = 10), α-dodecylamino-ω-hydroxypolyoxyethylene (n = 10), α-nonylphenyl-ω-hydroxypolyoxyethylene (n = 10), α-dodecylamino-ω-hydroxypolyoxyethylene (n = 10) Etc. Here, n means the number of oxyethylene units, n + m means the total number of oxyethylene units and the number of oxypropylene units, and so on.
本発明の処理剤は、前記の長鎖アルキルリン酸エステル塩を20〜88.99質量%、短鎖アルキルリン酸エステル塩を1〜10質量%、無機リン酸塩を0.01〜10質量%及び非イオン界面活性剤を10〜65質量%(合計100質量%)の割合で含有して成るものである。無機リン酸塩の含有割合は、より好ましくは0.1〜5.0質量%であり、更に好ましくは0.3〜3.0質量%である。 The treatment agent of the present invention contains 20 to 88.99 mass% of the above long chain alkyl phosphate ester salt, 1 to 10 mass% of short chain alkyl phosphate ester salt, and 0.01 to 10 mass of inorganic phosphate. % And nonionic surfactant in a ratio of 10 to 65% by mass (total 100% by mass). The content ratio of the inorganic phosphate is more preferably 0.1 to 5.0% by mass, and still more preferably 0.3 to 3.0% by mass.
本発明の処理剤は、更に下記のワックス及び下記の線状ポリオルガノシロキサンから選ばれるものを本発明の処理剤全体の12質量%未満の割合で含有することができる。 The treatment agent of the present invention may further contain one selected from the following waxes and the following linear polyorganosiloxane in a proportion of less than 12% by mass of the entire treatment agent of the present invention.
ワックス:炭素数16〜22の脂肪族1価アルコールと炭素数6〜22の脂肪族モノカルボン酸とから得られるエステル化合物及びパラフィンワックスから選ばれる少なくとも一つであって、融点が50〜120℃のもの。 Wax: at least one selected from an ester compound obtained from an aliphatic monohydric alcohol having 16 to 22 carbon atoms and an aliphatic monocarboxylic acid having 6 to 22 carbon atoms and paraffin wax, and having a melting point of 50 to 120 ° C. Things.
線状ポリオルガノシロキサン:30℃の動粘度が1×10−3〜100×10−3m2/sのもの。 Linear polyorganosiloxane: one having a kinematic viscosity of 1 × 10 −3 to 100 × 10 −3 m 2 / s at 30 ° C.
具体的にワックスとしては、セチルアルコール、ステアリルアルコール、アラキジルアルコール、ベヘニルアルコール等の炭素数16〜22の脂肪族1価アルコールと、カプロン酸、カプリル酸、カプリン酸、ラウリン酸、ミリスチン酸、パルミチン酸、ステアリン酸、アラキジン酸、ベヘン酸等の炭素数6〜22の脂肪族モノカルボン酸とから得られるエステル化合物や、融点が65℃のパラフィンワックス等が挙げられる。また線状ポリオルガノシロキサンとしては、30℃の動粘度が10×10−3m2/sのポリジメチルシロキサン、30℃の動粘度が50×10−3m2/sのポリジメチルシロキサン等が挙げられる。 Specifically, as the wax, aliphatic monohydric alcohols having 16 to 22 carbon atoms such as cetyl alcohol, stearyl alcohol, arachidyl alcohol, behenyl alcohol, caproic acid, caprylic acid, capric acid, lauric acid, myristic acid, palmitic acid Examples thereof include ester compounds obtained from aliphatic monocarboxylic acids having 6 to 22 carbon atoms such as stearic acid, arachidic acid and behenic acid, and paraffin waxes having a melting point of 65 ° C. Moreover, as linear polyorganosiloxane, polydimethylsiloxane having a kinematic viscosity of 10 × 10 −3 m 2 / s at 30 ° C., and polydimethylsiloxane having a kinematic viscosity of 50 × 10 −3 m 2 / s at 30 ° C. It can be mentioned.
本発明の処理剤は、1質量%水溶液の表面張力が45mN/m未満のものが好ましい。表面張力は、イオン交換水を用いて調製した本発明の処理剤の1質量%水溶液を垂直板法表面張力測定装置に供して求めることができる。 The treatment agent of the present invention preferably has a surface tension of less than 45 mN / m in a 1% by mass aqueous solution. The surface tension can be determined by applying a 1% by mass aqueous solution of the treatment agent of the present invention prepared using ion-exchanged water to a vertical plate method surface tension measurement device.
最後に、本発明に係るポリエステル系合成繊維(以下、本発明の合成繊維ともいう)について説明する。本発明の合成繊維は、本発明の処理剤が付着しているポリエステル系合成繊維である。 Finally, a polyester-based synthetic fiber according to the present invention (hereinafter, also referred to as a synthetic fiber according to the present invention) will be described. The synthetic fiber of the present invention is a polyester synthetic fiber to which the treatment agent of the present invention is attached.
ポリエステル系合成繊維としては、ポリエチレンテレフタレート繊維、ポリトリメチレンテレフタレート繊維等が挙げられるが、なかでもポリエチレンテレフタレート繊維が好ましい。本発明の処理剤を繊維に付着させる割合に特に制限はないが、本発明の処理剤を繊維に対し0.01〜0.5質量%の割合となるよう付着させることが好ましい。また本発明の処理剤を付着させる工程は、紡糸工程、延伸工程、捲縮工程等のいずれでもよいが、紡糸工程又は捲縮工程の前或いは後に付着させるのが好ましい。付着方法は、浸漬給油法、スプレー給油法、ローラー給油法、計量ポンプを用いたガイド給油法等のいずれでもよいが、浸漬給油法、スプレー給油法又はローラー給油法が好ましい。 Examples of polyester-based synthetic fibers include polyethylene terephthalate fibers and polytrimethylene terephthalate fibers. Among them, polyethylene terephthalate fibers are preferable. There is no particular limitation on the rate at which the treatment agent of the present invention is attached to the fiber, but it is preferable to attach the treatment agent of the present invention to the fiber in a proportion of 0.01 to 0.5% by mass. The step of depositing the treatment agent of the present invention may be any of a spinning step, a stretching step, a crimping step and the like, but it is preferred to be deposited before or after the spinning step or crimping step. The adhesion method may be any of an immersion oiling method, a spray oiling method, a roller oiling method, a guide oiling method using a measuring pump, etc., but an immersion oiling method, a spray oiling method or a roller oiling method is preferable.
本発明によれば、紡糸工程でのトウの優れた集束性、および延伸工程での優れた延伸性を兼ね備え、且つ紡績工程での発生電気の抑制が可能なポリエステル系合成繊維用処理剤及びポリエステル系合成繊維を提供できるという優れた効果を奏する。 According to the present invention, a polyester-based synthetic fiber treating agent and polyester capable of suppressing the generated electricity in the spinning process while combining the excellent convergence of the tow in the spinning process and the excellent stretchability in the drawing process. The excellent effect of providing a synthetic fiber is exhibited.
以下、本発明の構成及び効果をより具体的にするため、実施例等を挙げるが、本発明はこれらの実施例に限定されるというものではない。尚、以下の実施例及び比較例において、部は質量部を、また%は質量%を意味する。 Hereinafter, examples and the like will be described in order to make the configuration and effects of the present invention more specifically, but the present invention is not limited to these examples. In the following examples and comparative examples, "part" means "mass part" and "%" means mass%.
試験区分1(ポリエステル系合成繊維用処理剤の調製と表面張力の測定)
・実施例1
オクタデシルリン酸エステルカリウム塩(A−1)69.0部、ブチルリン酸エステルカリウム塩(A−4)5.0部、リン酸水素二カリウム塩(B−1)1.0部及びα−ドデシル−ω−ヒドロキシポリオキシエチレン(n=10)/α−ドデシル−ω−ヒドロキシポリオキシエチレンポリオキシプロピレン(n+m=10)/α−ドデシルアミノ−ω−ヒドロキシポリオキシエチレン(n=10)=25/25/50(質量比)の混合物(C−1)25.0部を、80℃に加熱した所定量の半量のイオン交換水に撹拌下で加えて完全に溶解させた。溶解後、残りの半量のイオン交換水を一気に加えて均一になるまで撹拌し、合成繊維用処理剤の1%水性液を200g調製した。この水溶液のpHを測定したところ、9.0であった。調製した合成繊維用処理剤の1%水性液を垂直板法表面張力測定装置(協和界面科学社製の商品名KYOWA CBVP SURFACE TENSIONMETER)に供して、20℃における表面張力を測定するという操作を5回行い、かくして求めた5回の測定値の平均値(mN/m)を算出したところ、39.7mN/mであった。
Test division 1 (Preparation of polyester-based synthetic fiber treatment agent and measurement of surface tension)
Example 1
69.0 parts of octadecyl phosphoric acid ester potassium salt (A-1), 5.0 parts of butyl phosphoric acid ester potassium salt (A-4), 1.0 part of dipotassium hydrogen phosphate (B-1) and α-dodecyl -Ω-hydroxypolyoxyethylene (n = 10) / α-dodecyl-ω-hydroxypolyoxyethylene polyoxypropylene (n + m = 10) / α-dodecylamino-ω-hydroxypolyoxyethylene (n = 10) = 25 25.0 parts of a mixture (C-1) of / 25/50 (mass ratio) was completely dissolved in a predetermined amount of half amount of ion exchange water heated to 80 ° C. with stirring. After dissolution, the remaining half amount of ion-exchanged water was added at a stretch and stirred until uniform, to prepare 200 g of a 1% aqueous solution of a synthetic fiber treatment agent. It was 9.0 when pH of this aqueous solution was measured. A 1% aqueous solution of the prepared synthetic fiber treatment agent is subjected to a vertical plate method surface tension measurement device (trade name KYOWA CBVP SURFACE TENSION METER manufactured by Kyowa Interface Science Co., Ltd.) to measure the surface tension at 20 ° C. 5 The average value (mN / m) of the five measured values determined in this manner was calculated to be 39.7 mN / m.
・実施例2〜15、参考例1及び比較例1〜13
実施例1と同様にして、表1に記載の内容で、実施例2〜15、参考例1及び比較例1〜13の合成繊維用処理剤の1%水溶液を各200g調製し、表面張力を測定して、平均値を算出した。実施例1も含め、各例の内容及び表面張力の平均値を表1にまとめて示した。尚、実施例2の水溶液のpHは8.4であり、また比較例9の水溶液のpHは10.5であった。
-Examples 2-15, the reference example 1, and the comparative examples 1-13
In the same manner as in Example 1, 200 g of a 1% aqueous solution of each of the synthetic fiber treating agents of Examples 2 to 15, Reference Example 1 and Comparative Examples 1 to 13 was prepared with the contents described in Table 1 and surface tension It measured and calculated the average value. Table 1 summarizes the contents of each example and the surface tension, including Example 1. The pH of the aqueous solution of Example 2 was 8.4, and the pH of the aqueous solution of Comparative Example 9 was 10.5.
表1において、
A−1:オクタデシルリン酸エステルカリウム塩
A−2:セチルリン酸エステルカリウム塩
A−3:ラウリルリン酸エステルカリウム塩
A−4:ブチルリン酸エステルカリウム塩
A−5:ヘキシルリン酸エステルカリウム塩
A−6:ポリオキシエチレン(n=7)セチルリン酸エステルカリウム塩
B−1:リン酸水素二カリウム塩
B−2:リン酸三カリウム塩
B−3:リン酸水素二ナトリウム塩
C−1:α−ドデシル−ω−ヒドロキシポリオキシエチレン(n=10)/α−ドデシル−ω−ヒドロキシポリオキシエチレンポリオキシプロピレン(n+m=10)/α−ドデシルアミノ−ω−ヒドロキシポリオキシエチレン(n=10)=25/25/50(質量比)の混合物
C−2:α−ノニルフェニル−ω−ヒドロキシポリオキシエチレン(n=10)/α−ドデシルアミノ−ω−ヒドロキシポリオキシエチレン(n=10)=70/30(質量比)の混合物
C−3:ポリオキシエチレン(n=7)ラウリルエーテル
C−4:ポリオキシエチレン(n=10)ラウリルエーテル/ポリオキシエチレン(n=25)ラウリルエーテル/ポリオキシエチレン(n=5)オレイルエーテル/ポリエチレングリコール(分子量1100)モノラウレート=55/10/20/15
C−5:ポリエチレングリコール(平均分子量400)モノラウレート
D−1:融点が60℃のパラフィンワックス
D−2:融点が61℃のステアリン酸ステアリル
E−1:30℃の粘度が10×10−3m2/sの線状ポリジメチルシロキサン
In Table 1,
A-1: octadecyl phosphate potassium salt A-2: cetyl phosphate potassium salt A-3: lauryl phosphate potassium salt A-4: butyl phosphate potassium salt A-5: hexyl phosphate potassium salt A-6 : Polyoxyethylene (n = 7) cetyl phosphate ester potassium salt B-1: Dipotassium hydrogen phosphate B-2: Tripotassium phosphate B-3: Disodium hydrogen phosphate C-1: α-dodecyl -Ω-hydroxypolyoxyethylene (n = 10) / α-dodecyl-ω-hydroxypolyoxyethylene polyoxypropylene (n + m = 10) / α-dodecylamino-ω-hydroxypolyoxyethylene (n = 10) = 25 / 25/50 (mass ratio) mixture C-2: α-nonylphenyl-ω-hydroxypolyoxyethylen A mixture of (n = 10) / α-dodecylamino-ω-hydroxypolyoxyethylene (n = 10) = 70/30 (mass ratio) C-3: polyoxyethylene (n = 7) lauryl ether C-4: Polyoxyethylene (n = 10) lauryl ether / polyoxyethylene (n = 25) lauryl ether / polyoxyethylene (n = 5) oleyl ether / polyethylene glycol (molecular weight 1100) monolaurate = 55/10/20/15
C-5: polyethylene glycol (average molecular weight 400) monolaurate D-1: paraffin wax having a melting point of 60 ° C. D-2: stearyl stearate having a melting point of 61 ° C. E-1: Viscosity at 10 ° C. of 10 × 10 − 3 m 2 / s linear polydimethylsiloxane
試験区分2(ポリエステル系合成繊維用処理剤の評価)
試験区分1で調製した各例のポリエステル系合成繊維用処理剤について、次のようにトウ集束性、延伸性及び発生電気を評価し、結果を表2にまとめて示した。
Test category 2 (Evaluation of processing agent for polyester synthetic fiber)
With respect to the polyester-based synthetic fiber treatment agent of each example prepared in Test Category 1, the tow bundling ability, stretchability and generated electricity were evaluated as follows, and the results are summarized in Table 2.
・トウ集束性の評価
トウ集束性は、ポリエステル系合成繊維用処理剤の動的表面張力を代用して次のように評価した。試験区分1で調製した各例のポリエステル系合成繊維用処理剤の1%水溶液を20℃で一晩静置した後、動的表面張力測定装置(Chem−Dyne Reserch Corporation社製の商品名QC6000)を用いて、25℃で65%RHの雰囲気下に動的表面張力を5Bubble/秒の条件で測定し、トウ集束性を以下の基準で評価した。
Evaluation of tow focusing property The tow focusing property was evaluated as follows by substituting the dynamic surface tension of the polyester-based synthetic fiber treatment agent. A 1% aqueous solution of the treating agent for polyester synthetic fiber prepared in Test Category 1 is allowed to stand overnight at 20 ° C., and then a dynamic surface tension measuring device (trade name QC6000 manufactured by Chem-Dyne Research Corporation) The dynamic surface tension was measured at 25 ° C. and an atmosphere of 65% RH under the condition of 5 Bubbles / second, and the toe focusing was evaluated based on the following criteria.
トウ集束性の評価基準
◎:動的表面張力が40mN/m未満
○:動的表面張力が40mN/m以上45mN/m未満
×:動的表面張力が45mN/m以上
Evaluation criteria for tow focusing ◎: Dynamic surface tension less than 40 mN / m ○: Dynamic surface tension greater than 40 mN / m and less than 45 mN / m ×: Dynamic surface tension greater than 45 mN / m
・延伸性の評価
図1に略示した試験装置を用いて、次のように延伸性を評価した。図1において、1は容器、2はポリエステル系合成繊維用処理剤の1%水溶液、3は円筒状の金属製摩擦体、3及び5はフリーローラー、6はポリエステルフィラメントである、各例のポリエステル系合成繊維用処理剤の1%水溶液について、図1の状態で、ポリエステルフィラメント6を図1中の矢印方向へ50m/分の速度で引っ張り、このときのフリーローラー4の上流部及びフリーローラー5の下流部における張力T1及びT2を20℃の雰囲気下で測定して、T2/T1の比から、延伸性を以下の基準で評価した。
Evaluation of Stretchability The stretchability was evaluated as follows using the test apparatus schematically shown in FIG. In FIG. 1, 1 is a container, 2 is a 1% aqueous solution of a polyester-based synthetic fiber treating agent, 3 is a cylindrical metal friction body, 3 and 5 are free rollers, and 6 is a polyester filament. With respect to a 1% aqueous solution of the synthetic fiber treating agent, the polyester filament 6 is pulled in the direction of the arrow in FIG. 1 at a speed of 50 m / min in the state of FIG. The tension T1 and T2 in the downstream part of the above were measured in an atmosphere at 20 ° C., and the stretchability was evaluated based on the following criteria from the ratio of T2 / T1.
延伸性の評価基準
◎:T2/T1=6.00未満
○:T2/T1=6.00以上6.30未満
×:T2/T1=6.30以上
Evaluation criteria for stretchability ◎: T2 / T1 = less than 6.00 ○: T2 / T1 = 6.00 or more and less than 6.30 ×: T2 / T1 = 6.30 or more
・発生電気の評価
試験区分1で調製した各例のポリエステル系合成繊維用処理剤の1%水性液を更にイオン交換水で希釈し、ポリエステル系合成繊維用処理剤の0.5%水性液を調製した。調製したポリエステル系合成繊維用処理剤の0.5%水性液を製綿工程で得られた繊度1.3×10−4g/m(1.2デニール)で繊維長38mmのセミダルのポリエステルステープル繊維に、ポリエステル系合成繊維用処理剤としての付着量が0.15%となるようにスプレー給油法で付着させ、80℃の熱風乾燥機で2時間乾燥した後、25℃×40%RHの雰囲気下に一夜調湿して、ポリエステル系合成繊維用処理剤を付着させた処理済みポリエステルステープル繊維を得た。このようにして得られた処理済みポリエステルステープル繊維10kgを用い、25℃×40%RHの雰囲気下でフラットカード(豊和工業社製)に供し、紡出速度=140m/分の条件で通過させた。紡出されたカードウェブの発生電気を測定し、制電性を以下の基準で評価した。
· Evaluation of generated electricity The 1% aqueous solution of the treatment agent for polyester-based synthetic fiber prepared in Test Category 1 is further diluted with deionized water, and the 0.5% aqueous solution of the treatment agent for polyester-based synthetic fiber is prepared. Prepared. A semi-dal polyester staple of 38 mm in fiber length, with a fineness of 1.3 × 10 -4 g / m (1.2 denier), obtained in the cotton-making process with a 0.5% aqueous solution of the prepared treatment agent for polyester synthetic fiber After making it adhere to a fiber by a spray oiling method so that the adhesion amount as a processing agent for polyester based synthetic fiber is 0.15%, and drying with a hot air dryer at 80 ° C. for 2 hours, 25 ° C. × 40% RH The humidity was controlled overnight under an atmosphere to obtain a treated polyester staple fiber to which a treating agent for polyester synthetic fiber was attached. Using 10 kg of the treated polyester staple fiber thus obtained, it was subjected to a flat card (manufactured by Toyowa Kogyo Co., Ltd.) under an atmosphere of 25 ° C. × 40% RH and passed at a spinning speed of 140 m / min. . The generated electricity of the spun card web was measured, and the antistatic property was evaluated based on the following criteria.
発生電気の評価基準
◎:発生電気量が0.1kV未満
○:発生電気量が0.1kV以上0.3kV未満
×:発生電気量が0.3kV以上0.6kV未満
××:発生電気量が0.6kV以上
Evaluation criteria of generated electricity ◎: generated electricity is less than 0.1 kV ○: generated electricity is 0.1 kV or more and less than 0.3 kV ×: generated electricity is 0.3 kV or more and less than 0.6 kV × ×: generated electricity is 0.6 kV or more
表1に対応する表2の結果からも明らかなように、本発明によれば、紡糸工程でのトウの優れた集束性、および延伸工程での優れた延伸性を兼ね備え、更に紡績工程での発生電気を十分抑制できるという優れた効果がある。 As apparent from the results of Table 2 corresponding to Table 1, according to the present invention, the combination of the excellent focusing of the tow in the spinning step and the excellent stretchability in the drawing step are further combined, and further in the spinning step. There is an excellent effect that the generated electricity can be sufficiently suppressed.
1 容器
2 ポリエステル系合成繊維用処理剤の1%水溶液
3 円筒状の金属製摩擦体
4,5 フリーローラー
6 ポリエステルフィラメント
Reference Signs List 1
Claims (6)
長鎖アルキルリン酸エステル塩:アルキル基の炭素数が16〜18のアルキルリン酸エステルのアルカリ金属塩。
短鎖アルキルリン酸エステル塩:アルキル基の炭素数が4〜8のアルキルリン酸エステルのアルカリ金属塩。
無機リン酸塩:リン酸水素二金属塩及びリン酸三金属塩から選ばれる少なくとも一つ。 20 to 88.99% by mass of the following long chain alkyl phosphate ester salt, 1 to 10% by mass of the following short chain alkyl phosphate ester salt, 0.01 to 10% by mass of the following inorganic phosphate, and A treating agent for synthetic fibers based on polyester, comprising 10 to 65% by mass (total 100% by mass) of an ionic surfactant.
Long chain alkyl phosphoric acid ester salt: Alkali metal salt of alkyl phosphoric acid ester having 16 to 18 carbon atoms in alkyl group.
Short-chain alkyl phosphate ester salt: Alkali metal salt of alkyl phosphate ester having 4 to 8 carbon atoms in alkyl group.
Inorganic phosphate: at least one selected from bimetallic hydrogen phosphate and trimetallic phosphoric acid.
ワックス:炭素数16〜22の脂肪族1価アルコールと炭素数6〜22の脂肪族モノカルボン酸とから得られるエステル化合物及びパラフィンワックスから選ばれる少なくとも一つであって、融点が50〜120℃のもの。
線状ポリオルガノシロキサン:30℃の動粘度が1×10−3〜100×10−3m2/sのもの。 The polyester-based synthetic fiber treating agent according to claim 1, further comprising a wax selected from the following waxes and the following linear polyorganosiloxane in a proportion of less than 12% by mass of the whole.
Wax: at least one selected from an ester compound obtained from an aliphatic monohydric alcohol having 16 to 22 carbon atoms and an aliphatic monocarboxylic acid having 6 to 22 carbon atoms and paraffin wax, and having a melting point of 50 to 120 ° C. Things.
Linear polyorganosiloxane: one having a kinematic viscosity of 1 × 10 −3 to 100 × 10 −3 m 2 / s at 30 ° C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2022186001A (en) * | 2021-06-04 | 2022-12-15 | 松本油脂製薬株式会社 | Treatment agent for water-repellent fibers and use thereof |
| JP7223471B1 (en) | 2022-09-13 | 2023-02-16 | 竹本油脂株式会社 | Treatment agent for polyester synthetic fiber, composition containing treatment agent for polyester synthetic fiber, first treatment agent for polyester synthetic fiber, composition containing first treatment agent for polyester synthetic fiber, second treatment for polyester synthetic fiber agent, composition containing second treatment agent for polyester synthetic fibers, third treatment agent for polyester synthetic fibers, composition containing third treatment agent for polyester synthetic fibers, diluent of treatment agent for polyester synthetic fibers, polyester Synthetic fiber processing method and polyester synthetic fiber |
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|---|---|---|---|---|
| CN111684124B (en) * | 2018-06-15 | 2023-01-17 | 竹本油脂株式会社 | Treatment agent for polyester-based synthetic fibers and polyester-based synthetic fibers |
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53103099A (en) * | 1977-02-22 | 1978-09-07 | Takemoto Oil & Fat Co Ltd | Novel oil agent for treating synthetic fiber |
| JPS53106897A (en) * | 1977-02-22 | 1978-09-18 | Toyo Boseki | Antistatic finish for fire retardant polyester fiber |
| JP2002020971A (en) * | 2000-07-11 | 2002-01-23 | Takemoto Oil & Fat Co Ltd | Oil solution for high speed spinning of synthetic fiber and method for high speed spinning |
| JP2002030571A (en) * | 2000-07-12 | 2002-01-31 | Takemoto Oil & Fat Co Ltd | Lubricant for high-speed spinning of synthetic fiber and high-speed spinning method |
| JP2008063713A (en) * | 2006-08-09 | 2008-03-21 | Matsumoto Yushi Seiyaku Co Ltd | Fiber treatment agent and method for producing synthetic fiber using the same |
| WO2009098845A1 (en) * | 2008-02-07 | 2009-08-13 | Matsumoto Yushi-Seiyaku Co., Ltd. | Fiber-treating agent and process for production of synthetic fiber |
| JP2016216858A (en) * | 2015-05-21 | 2016-12-22 | 竹本油脂株式会社 | Treatment agent for polyester synthetic fiber, treatment method of polyester synthetic fiber and polyester synthetic fiber |
-
2018
- 2018-04-09 JP JP2018074869A patent/JP6348246B1/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS53103099A (en) * | 1977-02-22 | 1978-09-07 | Takemoto Oil & Fat Co Ltd | Novel oil agent for treating synthetic fiber |
| JPS53106897A (en) * | 1977-02-22 | 1978-09-18 | Toyo Boseki | Antistatic finish for fire retardant polyester fiber |
| JP2002020971A (en) * | 2000-07-11 | 2002-01-23 | Takemoto Oil & Fat Co Ltd | Oil solution for high speed spinning of synthetic fiber and method for high speed spinning |
| JP2002030571A (en) * | 2000-07-12 | 2002-01-31 | Takemoto Oil & Fat Co Ltd | Lubricant for high-speed spinning of synthetic fiber and high-speed spinning method |
| JP2008063713A (en) * | 2006-08-09 | 2008-03-21 | Matsumoto Yushi Seiyaku Co Ltd | Fiber treatment agent and method for producing synthetic fiber using the same |
| WO2009098845A1 (en) * | 2008-02-07 | 2009-08-13 | Matsumoto Yushi-Seiyaku Co., Ltd. | Fiber-treating agent and process for production of synthetic fiber |
| JP2016216858A (en) * | 2015-05-21 | 2016-12-22 | 竹本油脂株式会社 | Treatment agent for polyester synthetic fiber, treatment method of polyester synthetic fiber and polyester synthetic fiber |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2022186001A (en) * | 2021-06-04 | 2022-12-15 | 松本油脂製薬株式会社 | Treatment agent for water-repellent fibers and use thereof |
| JP2023132021A (en) * | 2022-03-10 | 2023-09-22 | 東レ株式会社 | thermoplastic long fiber |
| JP7223471B1 (en) | 2022-09-13 | 2023-02-16 | 竹本油脂株式会社 | Treatment agent for polyester synthetic fiber, composition containing treatment agent for polyester synthetic fiber, first treatment agent for polyester synthetic fiber, composition containing first treatment agent for polyester synthetic fiber, second treatment for polyester synthetic fiber agent, composition containing second treatment agent for polyester synthetic fibers, third treatment agent for polyester synthetic fibers, composition containing third treatment agent for polyester synthetic fibers, diluent of treatment agent for polyester synthetic fibers, polyester Synthetic fiber processing method and polyester synthetic fiber |
| WO2024058151A1 (en) * | 2022-09-13 | 2024-03-21 | 竹本油脂株式会社 | Treatment agent for polyester-based synthetic fibers, composition containing treatment agent for polyester-based synthetic fibers, first treatment agent for polyester-based synthetic fibers, composition containing first treatment agent for polyester-based synthetic fibers, second treatment agent for polyester-based synthetic fibers, composition containing second treatment agent for polyester-based synthetic fibers, third treatment agent for polyester-based synthetic fibers, composition containing third treatment agent for polyester-based synthetic fibers, diluted solution of treatment agent for polyester-based synthetic fibers, method for treating polyester-based synthetic fiber, and polyester-based synthetic fiber |
| JP2024040905A (en) * | 2022-09-13 | 2024-03-26 | 竹本油脂株式会社 | A treatment agent for polyester synthetic fibers, a composition containing a treatment agent for polyester synthetic fibers, a first treatment agent for polyester synthetic fibers, a composition containing a first treatment agent for polyester synthetic fibers, a second treatment for polyester synthetic fibers agent, composition containing a second processing agent for polyester synthetic fibers, third processing agent for polyester synthetic fibers, composition containing a third processing agent for polyester synthetic fibers, diluted solution of processing agent for polyester synthetic fibers, polyester Processing method for synthetic fibers and polyester synthetic fibers |
| KR20250044803A (en) * | 2022-09-13 | 2025-04-01 | 다께모도유시가부시끼가이샤 | Treatment agent for polyester-based synthetic fibers, composition containing treatment agent for polyester-based synthetic fibers, first treatment agent for polyester-based synthetic fibers, composition containing first treatment agent for polyester-based synthetic fibers, second treatment agent for polyester-based synthetic fibers, composition containing second treatment agent for polyester-based synthetic fibers, third treatment agent for polyester-based synthetic fibers, composition containing third treatment agent for polyester-based synthetic fibers, diluted solution of treatment agent for polyester-based synthetic fibers, method for treating polyester-based synthetic fibers, and polyester-based synthetic fibers |
| KR20250044946A (en) * | 2022-09-13 | 2025-04-01 | 다께모도유시가부시끼가이샤 | Treatment agent for polyester-based synthetic fibers, composition containing treatment agent for polyester-based synthetic fibers, first treatment agent for polyester-based synthetic fibers, composition containing first treatment agent for polyester-based synthetic fibers, second treatment agent for polyester-based synthetic fibers, composition containing second treatment agent for polyester-based synthetic fibers, diluted solution of treatment agent for polyester-based synthetic fibers, method for treating polyester-based synthetic fibers, and polyester-based synthetic fibers |
| KR102867182B1 (en) | 2022-09-13 | 2025-10-01 | 다께모도유시가부시끼가이샤 | Treatment agent for polyester-based synthetic fibers, composition containing treatment agent for polyester-based synthetic fibers, first treatment agent for polyester-based synthetic fibers, composition containing first treatment agent for polyester-based synthetic fibers, second treatment agent for polyester-based synthetic fibers, composition containing second treatment agent for polyester-based synthetic fibers, third treatment agent for polyester-based synthetic fibers, composition containing third treatment agent for polyester-based synthetic fibers, diluted solution of treatment agent for polyester-based synthetic fibers, method for treating polyester-based synthetic fibers, and polyester-based synthetic fibers |
| KR102880211B1 (en) | 2022-09-13 | 2025-11-03 | 다께모도유시가부시끼가이샤 | Treatment agent for polyester-based synthetic fibers, composition containing treatment agent for polyester-based synthetic fibers, first treatment agent for polyester-based synthetic fibers, composition containing first treatment agent for polyester-based synthetic fibers, second treatment agent for polyester-based synthetic fibers, composition containing second treatment agent for polyester-based synthetic fibers, diluted solution of treatment agent for polyester-based synthetic fibers, method for treating polyester-based synthetic fibers, and polyester-based synthetic fibers |
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