JP2009144271A - Hollow polyester multifilament and method for producing the same - Google Patents
Hollow polyester multifilament and method for producing the same Download PDFInfo
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- JP2009144271A JP2009144271A JP2007320919A JP2007320919A JP2009144271A JP 2009144271 A JP2009144271 A JP 2009144271A JP 2007320919 A JP2007320919 A JP 2007320919A JP 2007320919 A JP2007320919 A JP 2007320919A JP 2009144271 A JP2009144271 A JP 2009144271A
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- 229920000728 polyester Polymers 0.000 title claims abstract description 52
- 238000004519 manufacturing process Methods 0.000 title claims description 13
- WOZVHXUHUFLZGK-UHFFFAOYSA-N dimethyl terephthalate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C=C1 WOZVHXUHUFLZGK-UHFFFAOYSA-N 0.000 claims abstract description 36
- -1 polyethylene terephthalate units Polymers 0.000 claims abstract description 27
- 229920000642 polymer Polymers 0.000 claims abstract description 27
- 229920000139 polyethylene terephthalate Polymers 0.000 claims abstract description 24
- 239000005020 polyethylene terephthalate Substances 0.000 claims abstract description 24
- 238000005809 transesterification reaction Methods 0.000 claims abstract description 10
- 239000000835 fiber Substances 0.000 claims description 27
- 239000012510 hollow fiber Substances 0.000 claims description 9
- 208000024891 symptom Diseases 0.000 claims 1
- 239000004744 fabric Substances 0.000 abstract description 13
- 206010016322 Feeling abnormal Diseases 0.000 abstract description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-L terephthalate(2-) Chemical compound [O-]C(=O)C1=CC=C(C([O-])=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-L 0.000 abstract 1
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 17
- 208000028659 discharge Diseases 0.000 description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 238000009987 spinning Methods 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 description 4
- 238000004821 distillation Methods 0.000 description 4
- 238000009998 heat setting Methods 0.000 description 4
- 239000002699 waste material Substances 0.000 description 4
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 3
- 229920001283 Polyalkylene terephthalate Polymers 0.000 description 3
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 125000003118 aryl group Chemical group 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 239000007809 chemical reaction catalyst Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 150000002148 esters Chemical group 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 229920006267 polyester film Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- DNIAPMSPPWPWGF-VKHMYHEASA-N (+)-propylene glycol Chemical compound C[C@H](O)CO DNIAPMSPPWPWGF-VKHMYHEASA-N 0.000 description 1
- YPFDHNVEDLHUCE-UHFFFAOYSA-N 1,3-propanediol Substances OCCCO YPFDHNVEDLHUCE-UHFFFAOYSA-N 0.000 description 1
- ALQSHHUCVQOPAS-UHFFFAOYSA-N Pentane-1,5-diol Chemical compound OCCCCCO ALQSHHUCVQOPAS-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 125000002947 alkylene group Chemical group 0.000 description 1
- 239000002216 antistatic agent Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000012691 depolymerization reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- CJOJIAKIRLKBOO-UHFFFAOYSA-N dimethyl 2-hydroxybenzene-1,4-dicarboxylate Chemical compound COC(=O)C1=CC=C(C(=O)OC)C(O)=C1 CJOJIAKIRLKBOO-UHFFFAOYSA-N 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 150000002009 diols Chemical class 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 239000006224 matting agent Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- KYTZHLUVELPASH-UHFFFAOYSA-N naphthalene-1,2-dicarboxylic acid Chemical compound C1=CC=CC2=C(C(O)=O)C(C(=O)O)=CC=C21 KYTZHLUVELPASH-UHFFFAOYSA-N 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 238000001953 recrystallisation Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000013585 weight reducing agent Substances 0.000 description 1
- 238000004804 winding Methods 0.000 description 1
Images
Abstract
Description
本発明は、リサイクルポリマーを使用しながらでも衣料布帛での軽量感とソフト感を併せ持った細単糸繊度高中空ポリエステルマルチフィラメントに関するものである。 The present invention relates to a fine single yarn fine hollow polyester multifilament having both a lightweight feeling and a soft feeling in a garment fabric while using a recycled polymer.
ポリエステルはその優れた特性を生かし衣料用布帛素材として広く使用されている。衣生活の多様化、高級化、個性化と共に、天然繊維が持つ好ましい性能をポリエステル繊維に付与する試みが続けられている。中空繊維は布帛の軽量化が求められているなかでスポーツ衣料用途から婦人衣料用途まで古くから幅広く使用されており、近年では布帛のソフトな風合いを出すために単糸繊度が1.1デシテックス未満の細繊度の中空繊維も好まれて使用されている。例えば特開2004−124338号公報では単糸繊度が0.2〜1.0デニール、中空率が25〜40%の中空繊維が提案されており、ソフト性、軽量性等良好なものが得られている。 Polyester is widely used as a fabric material for clothing by taking advantage of its excellent properties. Along with the diversification, upgrading, and individualization of clothing life, attempts are being made to impart the desirable performance of natural fibers to polyester fibers. Hollow fibers have been widely used for a long time, from sports clothing to women's clothing, in light of the need to reduce the weight of fabrics. In recent years, the single yarn fineness is less than 1.1 decitex to give the fabric a soft texture. Hollow fibers with a fineness of less than are also preferred. For example, Japanese Patent Application Laid-Open No. 2004-124338 proposes a hollow fiber having a single yarn fineness of 0.2 to 1.0 denier and a hollow ratio of 25 to 40%, and a good softness and light weight can be obtained. ing.
そのようななかで商品のもつ地球環境に対する影響度に関心が高まり、例えばリサイクルポリマーを使用した細繊度の中空ポリエステル繊維などが望まれてきた。
一般的にいわれるリサイクルポリマーは回収されたPETボトルやポリエステルフィルム製品、更にはこれら製品の製造工程において発生する屑ポリマーなどを粉砕して再溶融するマテリアルリサイクルが知られているがポリマーの粘度斑などが原因で単糸繊度の細い中空繊維など高度に異型化された繊維を紡糸する際には糸切れが多発し、著しく生産性が低下することで商業生産が困難であった。
Recycled polymers that are generally referred to are recycled PET bottles and polyester film products, as well as material recycling that pulverizes and remelts scrap polymers generated in the manufacturing process of these products. When spinning highly atypical fibers such as hollow fibers with fine single yarn fineness due to the above, thread breakage frequently occurred, and the productivity was significantly reduced, making commercial production difficult.
本発明は、上記従来技術を背景になされたもので、その目的はマテリアルリサイクルではなくケミカルリサイクルポリマーを使用し布帛での軽量感及びソフト感を表現する事の出来る環境に配慮された細単糸繊度高中空ポリエステルマルチフィラメントを提供することにある。 The present invention has been made against the background of the above-mentioned prior art, and its purpose is to use an environment-friendly fine single yarn that can express a feeling of lightness and softness in a fabric using a chemical recycling polymer instead of material recycling. It is to provide a high-definition hollow polyester multifilament.
本発明者等は、上記課題を解決するために鋭意検討を重ねた結果、本発明に到達した、即ち本発明によれば、
第一の発明の態様として、繊維を構成するポリマー成分の80モル%以上がポリエチレンテレフタレート単位で構成される中空ポリエステルマルチフィラメントであって、該ポリエチレンテレフタレートがポリエチレンテレフタレートを解重合して得られたリサイクルされたテレフタル酸ジメチルをエステル交換反応に使用したポリエチレンテレフタレートからなり、単糸繊度が0.7〜1.1デシテックス、中空率が20〜40%であることを特徴とする中空ポリエステルマルチフィラメントであり、第二の発明の態様として、繊維を構成するポリマー成分の80モル%以上がポリエチレンテレフタレート単位で構成され、該ポリエチレンテレフタレートがポリエチレンテレフタレートを解重合して得られたリサイクルされたテレフタル酸ジメチルをエステル交換反応に使用したポリエチレンテレフタレートであり、単糸繊度が0.7〜1.1デシテックス、中空率が20〜40%である中空ポリエステルマルチフィラメントの製造方法において、複数のスリットからなる吐出孔を有する中空糸用紡糸口金を用い、吐出線速度3〜5cm/secの範囲で溶融ポリマーを吐出し、口金面から30〜50mmの付近より風速0.2〜0.8m/secで冷却固化したポリマー糸条を引き取り、そのまま又は一旦巻取り後に伸度25〜40%になるよう延伸処理することを特徴とする中空ポリエステルマルチフィラメントの製造方法により達成される。
As a result of intensive studies to solve the above problems, the present inventors have reached the present invention, that is, according to the present invention,
As an aspect of the first invention, a recycled material obtained by depolymerizing polyethylene terephthalate, in which 80 mol% or more of the polymer component constituting the fiber is a hollow polyester multifilament composed of polyethylene terephthalate units. It is a hollow polyester multifilament made of polyethylene terephthalate using dimethyl terephthalate used for transesterification, having a single yarn fineness of 0.7 to 1.1 dtex and a hollowness of 20 to 40%. As a second aspect of the invention, recycled terephthalic acid obtained by depolymerizing polyethylene terephthalate in which 80 mol% or more of the polymer component constituting the fiber is composed of polyethylene terephthalate units. Polyethylene terephthalate using methyl for transesterification, discharge consisting of a plurality of slits in a method for producing a hollow polyester multifilament having a single yarn fineness of 0.7 to 1.1 dtex and a hollowness of 20 to 40% Using a spinneret for hollow fibers having holes, the molten polymer is discharged at a discharge linear velocity in the range of 3 to 5 cm / sec, and cooled and solidified at a wind speed of 0.2 to 0.8 m / sec from around 30 to 50 mm from the die surface. It is achieved by a method for producing a hollow polyester multifilament characterized in that the polymer yarn is taken up and stretched to the extent of 25 to 40% as it is or once after winding.
本発明によりリサイクルされたテレフタル酸ジメチルをエステル交換反応に使用したポリエチレンテレフタレートにて製品の製造段階における環境への負荷を低減させ、軽量感とソフト感を併せ持った細単糸繊度高中空ポリエステルマルチフィラメントが安定して製造可能となる。 Polyethylene terephthalate using dimethyl terephthalate recycled according to the present invention for transesterification reduces the environmental burden in the production stage of the product, and has a single fiber fineness and high hollow polyester multifilament that combines lightness and softness. Can be manufactured stably.
以下本発明の実施形態について詳細に説明する。
本発明で用いるポリエステルとしては、テレフタル酸を主たるジカルボン酸成分とし、エチレングリコール、1,3−プロパンジオール、1,4−ブタンジオール、1,5−ペンタンジオール、1,6−ヘキサンジオールなどのアルキレングリコールを主たるジオール成分とするポリエステルを80重量%以上、好ましくは90重量%以上含有するポリエステルであり、該ポリエステルには、本発明の目的を損なわない範囲内で、例えばイソフタル酸、ナフタレンジカルボン酸、ジフェニルジカルボン酸などの芳香族ジカルボン酸成分や上記とは異なる他のグリコール成分を共重合していても良い。
Hereinafter, embodiments of the present invention will be described in detail.
As the polyester used in the present invention, terephthalic acid is the main dicarboxylic acid component, and alkylene such as ethylene glycol, 1,3-propanediol, 1,4-butanediol, 1,5-pentanediol, 1,6-hexanediol, etc. It is a polyester containing 80% by weight or more, preferably 90% by weight or more of a polyester having a glycol as a main diol component, and the polyester includes, for example, isophthalic acid, naphthalenedicarboxylic acid, within a range not impairing the object of the present invention. An aromatic dicarboxylic acid component such as diphenyldicarboxylic acid or another glycol component different from the above may be copolymerized.
該ポリエステルの固有粘度(オルソクロロフェノールを溶媒として使用し35℃で測定)は、通常衣料用布帛素材として使用されるポリエステルと同じ範疇の0.55〜0.80の範囲のものが好ましい。また、必要に応じて適宜艶消し剤、制電剤、安定剤などの添加剤またはアルカリ減量により繊維表面に微細孔やフィブリルを形成させる事の出来る添加剤などを含んでも良い。 The intrinsic viscosity (measured at 35 ° C. using orthochlorophenol as a solvent) of the polyester is preferably in the range of 0.55 to 0.80, which is the same category as the polyester used as a fabric material for clothing. Further, if necessary, an additive such as a matting agent, an antistatic agent and a stabilizer, or an additive capable of forming micropores and fibrils on the fiber surface by alkali weight reduction may be included.
本発明のポリエステルの製造方法は、芳香族ジカルボン酸のエステル形成誘導体をエステル交換反応触媒の存在下、アルキレングリコールとエステル交換反応せしめることによって製造する必要があるが、この出発原料物質であるテレフタル酸ジメチルは全カルボン酸成分の80mol%以上を占めることが好ましく、特に該原料であるテレフタル酸ジメチルは、ポリアルキレンテレフタレートを解重合することによって得られるケミカルリサイクルされたテレフタル酸ジメチルであることが必要である。ここで、該ポリアルキレンテレフタレートとしてはポリエチレンテレフタレートが好ましく、特に回収されたPETボトル、回収されたポリエステル繊維製品、回収されたポリエステルフィルム製品、更にはこれら製品の製造工程において発生する屑ポリマーなど回収されたポリエステルが好ましく用いられる。また上記回収されたポリアルキレンテレフタレートを解重合することによって得られるテレフタル酸ジメチルの製造方法について特に限定はなく、例えば、ポリエチレンテレフタレートをエチレングリコールで解重合した後、メタノールでエステル交換反応し、得られたテレフタル酸ジメチルを再結晶や蒸留で精製する方法等によって得ることができる。 In the method for producing the polyester of the present invention, it is necessary to produce an ester-forming derivative of an aromatic dicarboxylic acid by an ester exchange reaction with an alkylene glycol in the presence of an ester exchange reaction catalyst. It is preferable that dimethyl accounts for 80 mol% or more of the total carboxylic acid component. In particular, the raw material dimethyl terephthalate is required to be chemically recycled dimethyl terephthalate obtained by depolymerizing polyalkylene terephthalate. is there. Here, polyethylene terephthalate is preferable as the polyalkylene terephthalate. In particular, recovered PET bottles, recovered polyester fiber products, recovered polyester film products, and waste polymers generated in the manufacturing process of these products are recovered. Polyester is preferably used. There is no particular limitation on the method for producing dimethyl terephthalate obtained by depolymerizing the recovered polyalkylene terephthalate. For example, after depolymerizing polyethylene terephthalate with ethylene glycol, it is obtained by transesterification with methanol. Further, dimethyl terephthalate can be obtained by recrystallization or distillation.
本発明の中空ポリエステルマルチフィラメントは、単糸繊度が0.7〜1.1デシテックスであることが必要である。ここで単糸繊度が1.1デシテックス以上であれば単繊維での曲げ剛性が強すぎて布帛での風合いにおいてソフト感が不十分なものとなり、0.7デシテックス以下の場合は紡糸工程での断糸による工程通過性が著しく低下するので好ましくない。 The hollow polyester multifilament of the present invention needs to have a single yarn fineness of 0.7 to 1.1 dtex. Here, if the single yarn fineness is 1.1 dtex or more, the bending rigidity of the single fiber is too strong, and the soft feeling is insufficient in the texture in the fabric, and in the case of 0.7 dtex or less, in the spinning process This is not preferable because the process passability due to the yarn breakage is significantly reduced.
このような特性を有する本発明の中空ポリエステルマルチフィラメントとすることにより環境への負荷を低減させ、且つ軽量化とソフト感を併せ持った中空細繊度繊維とすることが可能となる。 By using the hollow polyester multifilament of the present invention having such characteristics, it is possible to reduce the burden on the environment, and to make a hollow fine fiber having both a light weight and a soft feeling.
中空繊維の中空率は20〜40%であることが必要である。ここで中空率が20%以下であれば布帛での軽量感が不十分なものとなり、40%以上の場合は紡糸工程での断糸による工程通過性が著しく低下するので好ましくない。 The hollow ratio of the hollow fiber needs to be 20 to 40%. Here, if the hollowness is 20% or less, the lightweight feeling of the fabric is insufficient, and if it is 40% or more, the process passability due to the yarn breakage in the spinning process is remarkably lowered.
中空率が20%以上となるような紡糸口金としては、例えば、図1(a)に示す吐出孔の場合は円弧状スリットのスリット巾及び円周配置直径(PCD)(図1の1)を変更することによって、任意に調整することができる。本発明においては、図1(a)の吐出孔の場合は円弧状のスリット巾を0.08mm以下、円周配置直径(PCD)を0.6mm以上とすれば、中空率20%以上とすることができる。しかし、中空率を40%以上とする場合は、複数のスリットから吐出される溶融ポリマー間での張り合わせが難しく、中空形成が困難となり断糸が多発する。なお、円弧状のスリットのほか、中空形成性能のある吐出孔であれば、例えば図1(b)に示すような形状のスリットを配置した吐出孔であってもよい。 As the spinneret having a hollow ratio of 20% or more, for example, in the case of the discharge hole shown in FIG. 1 (a), the slit width of the arc-shaped slit and the circumferential arrangement diameter (PCD) (1 in FIG. 1) By changing, it can be arbitrarily adjusted. In the present invention, in the case of the discharge hole of FIG. 1A, if the arc-shaped slit width is 0.08 mm or less and the circumferential arrangement diameter (PCD) is 0.6 mm or more, the hollowness is 20% or more. be able to. However, when the hollow ratio is set to 40% or more, it is difficult to bond the molten polymers discharged from the plurality of slits, and it is difficult to form a hollow, resulting in frequent breakage. In addition to the arc-shaped slit, as long as the discharge hole has a hollow forming performance, for example, a discharge hole in which a slit having a shape as shown in FIG.
次に本発明の中空ポリエステルマルチフィラメントの製造方法について説明する。中空糸用紡糸口金の複数のスリットからなる吐出孔からのポリマー吐出線速度を3〜5cm/secの範囲で吐出することが重要である。吐出線速度は、ポリマー吐出量に応じて、吐出スリットの総開口面積を変えることによって、任意に設定することができる。吐出線速度が3cm/sec未満の場合は、吐出線速度が遅過ぎることによる吐出斑(メルトフラクチャー)が発生し引き取られた繊維の繊度斑(U%ハーフイナート値)が悪化することによる布帛での染斑が目立つことによる品位の悪化が発生する。ポリマー吐出平均線速度が5m/min.を超える場合、繊維断面を高度に異型化することが出来なくなり中空断面割れや該繊維に必要な中空率が得られない。 Next, the manufacturing method of the hollow polyester multifilament of this invention is demonstrated. It is important that the polymer discharge linear velocity is discharged in the range of 3 to 5 cm / sec from the discharge holes formed by a plurality of slits of the spinneret for hollow fibers. The discharge linear velocity can be arbitrarily set by changing the total opening area of the discharge slit according to the polymer discharge amount. When the discharge linear velocity is less than 3 cm / sec, discharge irregularities (melt fracture) due to the discharge linear velocity being too slow are generated, and the fineness unevenness (U% half inert value) of the taken-off fiber is deteriorated. Deterioration of quality occurs due to the noticeable stains. Polymer discharge average linear velocity is 5 m / min. If it exceeds 1, the cross section of the fiber cannot be highly atypical, and the hollow cross section crack and the hollow ratio required for the fiber cannot be obtained.
口金面から30〜50mmの付近より風速0.2〜0.8m/secで冷却固化したポリマー糸条を引き取ることが重要である。口金面から30mm未満より冷却固化する場合、口金面の温度が著しく低下し、糸切れが多発することにより工程通過性が著しく低下する。口金面から50mm以上より冷却固化する場合、繊維断面を高度に異型化することが出来なくなり該繊維に必要な中空率が得られない。風速0.8m/sec以上で冷却固化する場合、口金面の温度が著しく低下し、糸切れが多発することにより工程通過性が著しく低下する。風速0.2m/sec未満で冷却固化する場合、繊維断面を高度に異型化することが出来なくなり該繊維に必要な中空率が得られない。 It is important to take up the polymer yarn cooled and solidified at a wind speed of 0.2 to 0.8 m / sec from around 30 to 50 mm from the base surface. In the case of cooling and solidifying from less than 30 mm from the die surface, the temperature of the die surface is remarkably lowered, and thread breakage frequently occurs, so that the process passability is remarkably lowered. When cooling and solidifying from 50 mm or more from the die surface, the cross section of the fiber cannot be highly atypical, and the hollowness required for the fiber cannot be obtained. When cooling and solidifying at a wind speed of 0.8 m / sec or more, the temperature of the die surface is remarkably lowered, and thread breakage occurs frequently, so that process passability is remarkably lowered. When cooling and solidifying at a wind speed of less than 0.2 m / sec, the cross section of the fiber cannot be made highly atypical and the hollowness required for the fiber cannot be obtained.
延伸処理後の伸度が25〜50%になることが重要である。伸度が25%以下の場合、延伸工程での毛羽や断糸が多発し、著しく工程通過性が低下する。伸度が50%以上の場合、得られた繊維の強度が不十分となり布帛での引き裂き強度低下の原因となる。 It is important that the elongation after the stretching treatment is 25 to 50%. When the elongation is 25% or less, fluff and yarn breakage frequently occur in the stretching process, and the process passability is significantly reduced. When the elongation is 50% or more, the strength of the obtained fiber becomes insufficient, which causes a decrease in tear strength in the fabric.
以下、実施例により、本発明を更に具体的に説明する。なお、実施例における各項目は次の方法で測定した。
(1)固有粘度
オルソクロロフェノールを溶媒として使用し35℃で測定した。
(2)中空率(%)及び中空率のばらつき
得られたポリエステルマルチフィラメントの断面写真(560倍)をとり、中空破れが認められる断面を除き、各単糸断面の中空部面積(A)および断面を囲む面積(B)を測定し、下記式で計算し、全測定値の平均値を中空率(%)として。
中空率(%)=A/B×100
(3)中空破れ発生率(%)
上記(2)で得た断面写真で、中空破れのある単糸断面を数え、全単糸断面に占める割合(%)を中空割れ発生率とした。
Hereinafter, the present invention will be described more specifically with reference to examples. In addition, each item in an Example was measured with the following method.
(1) Intrinsic viscosity Measured at 35 ° C. using orthochlorophenol as a solvent.
(2) Hollow ratio (%) and variation in hollow ratio Take a cross-sectional photograph (560 times) of the obtained polyester multifilament, except for the cross section where hollow breakage is observed, the hollow area (A) of each single yarn cross section The area (B) surrounding the cross-section is measured and calculated by the following formula, and the average value of all measured values is taken as the hollow ratio (%).
Hollow ratio (%) = A / B × 100
(3) Incidence rate of hollow breakage (%)
In the cross-sectional photograph obtained in (2) above, the single yarn cross-sections with hollow breakage were counted, and the ratio (%) to the total single-fiber cross-section was taken as the hollow crack occurrence rate.
[参考例]
回収テレフタル酸ジメチルの製造:エチレングリコール200部を500mlセパラブルフラスコに投入し、更に炭酸ソーダ1.5部、粉砕されたPETボトル等からなるポリエチレンテレフタレート屑50部を投入し、撹拌しながら昇温して、185℃とした。この状態を4時間保持したところ、ポリエチレンテレフタレート屑は溶解し解重合反応が完結した。得られた解重合物を減圧蒸留で濃縮し、留分としてエチレングリコール150部回収した。
[Reference example]
Production of recovered dimethyl terephthalate: 200 parts of ethylene glycol is put into a 500 ml separable flask, 1.5 parts of sodium carbonate and 50 parts of polyethylene terephthalate scraps such as crushed PET bottles are put in, and the temperature is increased while stirring. The temperature was 185 ° C. When this state was maintained for 4 hours, the polyethylene terephthalate waste was dissolved and the depolymerization reaction was completed. The obtained depolymerized product was concentrated by distillation under reduced pressure, and 150 parts of ethylene glycol was recovered as a fraction.
この濃縮液にエステル交換反応触媒として炭酸ソーダ0.5部とMeOH100部を投入し、常圧で液温を75℃、1時間撹拌し、エステル交換反応を実施した。
得られた混合物を40℃まで冷却し、ガラス製フィルターで濾過した。フィルター上に回収できた粗テレフタル酸ジメチルを100部のMeOH中に投入し、40℃に加温・撹拌洗浄し、再度ガラス製のフィルターで濾過した。この洗浄は2回繰り返した。
To this concentrated liquid, 0.5 part of sodium carbonate and 100 parts of MeOH were added as a transesterification reaction catalyst, and the liquid temperature was stirred at normal pressure at 75 ° C. for 1 hour to carry out the transesterification reaction.
The resulting mixture was cooled to 40 ° C. and filtered through a glass filter. The crude dimethyl terephthalate recovered on the filter was put into 100 parts of MeOH, heated to 40 ° C. with stirring and washed, and filtered again with a glass filter. This washing was repeated twice.
フィルター上に捕捉できた粗テレフタル酸ジメチルを蒸留装置に仕込み、圧力6.65kPa還流比0.5の条件で減圧蒸留を実施し、留分としてテレフタル酸ジメチルを得た。留分は47部回収できた。釜残を測定しテレフタル酸ジメチル量を測定すると2部であり、投入したポリエステルを基準にするとテレフタル酸ジメチルの反応率は93重量%であった。 Crude dimethyl terephthalate that could be captured on the filter was charged into a distillation apparatus and distilled under reduced pressure under a pressure of 6.65 kPa at a reflux ratio of 0.5 to obtain dimethyl terephthalate as a fraction. 47 parts of the fraction could be recovered. The residue in the kettle was measured and the amount of dimethyl terephthalate was measured to be 2 parts, and the reaction rate of dimethyl terephthalate was 93% by weight based on the charged polyester.
蒸留により精製された回収テレフタル酸ジメチル中には、2−ヒドロキシテレフタル酸ジメチルが0.5重量ppm検出された。精製された回収テレフタル酸ジメチルの品質は、純度99.9重量%以上であった。 In the recovered dimethyl terephthalate purified by distillation, 0.5 weight ppm of dimethyl 2-hydroxyterephthalate was detected. The purified recovered dimethyl terephthalate had a purity of 99.9% by weight or more.
[実施例1]
参考例のポリエチレンテレフタレートを解重合して得られたケミカルリサイクルされたテレフタル酸ジメチルをエステル交換反応に使用した固有粘度0.64のポリエチレンテレフタレートペレットを140℃で5時間乾燥した後、4つのスリットからなる吐出孔であり、吐出孔48ホールが一列同心円状に配列してある紡糸口金から、ポリマー吐出温度293℃とし、単一吐出孔でのポリマー吐出平均線速度が3.6cm/secとなるようとなるように押し出して、紡糸口金直下に設けた50〜290℃の雰囲気温度に保持した長さ3.7cmの保温領域を通過させて20℃、平均風速0.4m/sec.の冷却風により溶融マルチフィラメントを急冷して固体マルチフィラメントに変え、紡糸口金から600mmの位置にてオイリングノズルによるオイリングを行うと同時にマルチフィラメントの糸条を集束させて2900m/min.の速度で紡糸捲き取りを行い繊度56dTex、フィラメント数48、伸度110%の部分的未延伸中空ポリエステルマルチフィラメントを得た。得られた部分的未延伸中空ポリエステル繊維を余熱温度90℃、熱セット温度200℃で1.56倍の延伸処理をおこない繊度36dTex、フィラメント数48、単糸繊度0.75デシテックス、伸度27%の中空ポリエステルマルチフィラメントを得た。得られた中空ポリエステルマルチフィラメントの中空率は29%であり、48時間での紡糸断糸率及び中空破れ発生率が0%と良好な工程通過性であり、布帛での風合いもソフトなものであることを確認した。
[Example 1]
After drying polyethylene terephthalate pellets having an intrinsic viscosity of 0.64 using a chemically recycled dimethyl terephthalate obtained by depolymerizing the polyethylene terephthalate of the reference example for the transesterification reaction at 140 ° C. for 5 hours, From a spinneret in which 48 holes are arranged concentrically in a row, the polymer discharge temperature is set to 293 ° C., and the average linear velocity of the polymer discharged from the single discharge hole is 3.6 cm / sec. And passed through a 3.7 cm long heat retention region maintained at an atmospheric temperature of 50 to 290 ° C. provided directly below the spinneret, and 20 ° C. and an average wind speed of 0.4 m / sec. The melted multifilament is rapidly cooled by a cooling air of 5 to convert it into a solid multifilament, and oiling is performed by an oiling nozzle at a position 600 mm from the spinneret, and at the same time, the filaments of the multifilament are focused to 2900 m / min. Spinning was carried out at a speed of 5 to obtain partially unstretched hollow polyester multifilaments having a fineness of 56 dTex, a filament count of 48, and an elongation of 110%. The obtained partially unstretched hollow polyester fiber is stretched 1.56 times at a preheating temperature of 90 ° C. and a heat setting temperature of 200 ° C., and has a fineness of 36 dTex, a filament count of 48, a single yarn fineness of 0.75 dtex and an elongation of 27%. Of hollow polyester multifilament was obtained. The resulting hollow polyester multifilament has a hollowness of 29%, a spinning yarn breakage rate in 48 hours and a hollow breakage occurrence rate of 0% and good processability, and the fabric feel is soft. I confirmed that there was.
[実施例2]
単一吐出孔でのポリマー吐出平均線速度が4.2cm/secとなる以外は実施例1と同条件にて繊度64dTex、フィラメント数48、伸度116%の部分的未延伸中空ポリエステルマルチフィラメントを得た。得られた部分的未延伸中空ポリエステル繊維を余熱温度90℃、熱セット温度210℃で1.55倍の延伸処理をおこない繊度42dTex、フィラメント数48、単糸繊度0.87デシテックス、伸度30%の中空ポリエステルマルチフィラメントを得た。得られた中空ポリエステルマルチフィラメントの中空率は25%であり、48時間での紡糸断糸率及び中空破れ発生率が0%と良好な工程通過性であり、布帛での風合いもソフトなものであることを確認した。
[Example 2]
A partially unstretched hollow polyester multifilament having a fineness of 64 dTex, a filament count of 48, and an elongation of 116% under the same conditions as in Example 1 except that the polymer discharge average linear velocity at a single discharge hole was 4.2 cm / sec. Obtained. The obtained partially unstretched hollow polyester fiber was stretched 1.55 times at a preheating temperature of 90 ° C and a heat setting temperature of 210 ° C, a fineness of 42 dTex, a filament count of 48, a single yarn fineness of 0.87 dtex, and an elongation of 30%. Of hollow polyester multifilament was obtained. The hollow polyester multifilament obtained has a hollowness of 25%, a spinning yarn breakage rate and a hollow breakage occurrence rate of 48% in 48 hours and good process passability, and the fabric feel is soft. I confirmed that there was.
[比較例1]
ポリエチレンテレフタレート屑を粉砕して得られたマテリアルリサイクルされた固有粘度0.57のポリエチレンテレフタレートペレットを使用した以外は実施例1と同条件にて繊度56dTex、フィラメント数48の部分的未延伸中空ポリエステルマルチフィラメントを得ようと試みたが溶融吐出段階でのベンディングや単糸切れにより紡糸することができなかった。
[Comparative Example 1]
Partially unstretched hollow polyester multi having a fineness of 56 dTex and a filament number of 48 under the same conditions as in Example 1 except that polyethylene terephthalate pellets having an intrinsic viscosity of 0.57 obtained by grinding polyethylene terephthalate waste were used. Attempts were made to obtain filaments, but spinning was not possible due to bending or single yarn breakage in the melt discharge stage.
[比較例2]
単一吐出孔でのポリマー吐出平均線速度が2.7cm/secとなる以外は実施例1と同条件にて繊度56dTex、フィラメント数48、伸度83%の部分的未延伸中空ポリエステルマルチフィラメントを得たが、吐出斑(メルトフラクチャー)が発生しU%ハーフイナート値が3.7%と悪く延伸処理に値するものではなかった。
[Comparative Example 2]
A partially unstretched hollow polyester multifilament having a fineness of 56 dTex, a filament number of 48, and an elongation of 83% under the same conditions as in Example 1 except that the polymer discharge average linear velocity at a single discharge hole was 2.7 cm / sec. Although it was obtained, discharge spots (melt fracture) occurred, and the U% half inert value was 3.7%, which was not bad for stretching.
[比較例3]
単一吐出孔でのポリマー吐出平均線速度が8.4cm/secとなる以外は実施例1と同条件にて繊度56dTex、フィラメント数48、伸度112%の部分的未延伸中空ポリエステルマルチフィラメントを得た。得られた部分的未延伸中空ポリエステル繊維を余熱温度90℃、熱セット温度210℃で1.55倍の延伸処理をおこない繊度42dTex、フィラメント数48、単糸繊度0.75デシテックス中空ポリエステルマルチフィラメントを得たが中空率は18%であり目標とする中空率20%以上を達成できなかった。
中空破れが多発し延伸処理に値するものではなかった。
[Comparative Example 3]
A partially unstretched hollow polyester multifilament having a fineness of 56 dTex, a filament number of 48 and an elongation of 112% under the same conditions as in Example 1 except that the polymer discharge average linear velocity at a single discharge hole was 8.4 cm / sec. Obtained. The obtained partially unstretched hollow polyester fiber is stretched 1.55 times at a preheating temperature of 90 ° C. and a heat setting temperature of 210 ° C. to obtain a fineness of 42 dTex, a filament count of 48, and a single yarn fineness of 0.75 dtex hollow polyester multifilament. Although the hollowness was 18%, the target hollowness of 20% or more could not be achieved.
Hollow breakage occurred frequently and was not worthy of stretching treatment.
[比較例4]
紡糸口金直下に設けた50〜290℃の雰囲気温度に保持した長さ1.5cmの保温領域を通過させた以外は実施1と同様にして繊度56dTex、フィラメント数48の部分的未延伸中空ポリエステルマルチフィラメントを得ようと試みたが単糸切れにより紡糸することができなかった。
[Comparative Example 4]
A partially unstretched hollow polyester multi fiber having a fineness of 56 dTex and 48 filaments in the same manner as in Example 1 except that it was passed through a heat insulation region having a length of 1.5 cm and maintained at an atmospheric temperature of 50 to 290 ° C. provided immediately below the spinneret. An attempt was made to obtain a filament, but it could not be spun due to a single yarn breakage.
[比較例5]
紡糸口金直下に設けた50〜290℃の雰囲気温度に保持した長さ6.0cmの保温領域を通過させた以外は実施1と同様にして繊度56dTex、フィラメント数48、伸度126%の部分的未延伸中空ポリエステルマルチフィラメントを得た。得られた部分的未延伸中空ポリエステル繊維を余熱温度90℃、熱セット温度210℃で1.55倍の延伸処理をおこない繊度42dTex、フィラメント数48、単糸繊度0.87デシテックス中空ポリエステルマルチフィラメントを得たが中空率は14%であり目標とする中空率20%以上を達成できなかった。
[Comparative Example 5]
Partially having a fineness of 56 dTex, a filament number of 48, and an elongation of 126% in the same manner as in Example 1 except that it was passed through a heat-retaining region having a length of 6.0 cm held at an atmospheric temperature of 50 to 290 ° C. provided immediately below the spinneret. An unstretched hollow polyester multifilament was obtained. The obtained partially unstretched hollow polyester fiber is stretched 1.55 times at a preheating temperature of 90 ° C. and a heat setting temperature of 210 ° C. to obtain a fineness of 42 dTex, a filament count of 48, and a single yarn fineness of 0.87 dtex hollow polyester multifilament. Although the hollowness was 14%, the target hollowness of 20% or more could not be achieved.
ポリマー屑からケミカルリサイクルした原料を使用したポリエステルからなる細単糸繊度高中空ポリエステルマルチフィラメントとすることにより、地球環境に優しく且つ軽量感及びソフト感に優れた布帛とすることができる。 By using a thin single yarn fine hollow polyester multifilament made of polyester using a raw material chemically recycled from polymer waste, it is possible to obtain a fabric which is gentle to the global environment and excellent in lightness and softness.
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RU2531296C1 (en) * | 2010-09-02 | 2014-10-20 | Бэйцзинь Чунли Машинери Энджиниринг Ко., Лтд | Method of obtaining terylene fibre from polyether wastes |
KR101375750B1 (en) | 2012-11-05 | 2014-03-18 | 정근용 | Knited fabric for bedding with excellent exothermic |
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