TWI695097B - Colored polypropylene fiber and preparation method thereof - Google Patents
Colored polypropylene fiber and preparation method thereof Download PDFInfo
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- TWI695097B TWI695097B TW105118533A TW105118533A TWI695097B TW I695097 B TWI695097 B TW I695097B TW 105118533 A TW105118533 A TW 105118533A TW 105118533 A TW105118533 A TW 105118533A TW I695097 B TWI695097 B TW I695097B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
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Abstract
本發明公開了一種有色聚丙烯纖維，該纖維中含有組分a受阻酚類抗氧化劑以及組分b亞磷酸酯類抗氧化劑和/或組分c受阻胺類抗氧化劑，其中組分a占有色聚丙烯纖維的400至15000ppm；組分b與組分a的重量比為0.8至6.0：1，組分c占有色聚丙烯纖維的4000至50000ppm。所述有色聚丙烯纖維具有優異的抗氧化性能，裂解發熱少，應用廣泛。 The invention discloses a colored polypropylene fiber, which contains component a hindered phenolic antioxidant and component b phosphite antioxidant and/or component c hindered amine antioxidant, wherein component a possesses color 400 to 15000 ppm of polypropylene fibers; the weight ratio of component b to component a is 0.8 to 6.0:1, and component c occupies 4000 to 50000 ppm of colored polypropylene fibers. The colored polypropylene fiber has excellent oxidation resistance, less pyrolysis heat, and is widely used.
Description
本發明涉及一種抗氧化性好的有色聚丙烯纖維及其製備方法。 The invention relates to a colored polypropylene fiber with good oxidation resistance and a preparation method thereof.
聚丙烯纖維由於具有輕量、快乾等優點受到廣泛的利用。然而聚丙烯在光和熱的作用下會進行氧化分解，產生烷基自由基，而且這種反應會連續不斷的進行下去。通過這種被稱作自動氧化迴圈的連鎖反應，聚丙烯自身氧化裂解，同時該裂解反應為發熱反應，在自身發熱的作用下聚丙烯會發生熔融、發煙甚至燒毀。 Polypropylene fiber is widely used due to its advantages of light weight and quick drying. However, polypropylene will undergo oxidative decomposition under the action of light and heat to produce alkyl radicals, and this reaction will continue continuously. Through this chain reaction called auto-oxidation loop, polypropylene itself oxidizes and cracks, and at the same time, the cracking reaction is an exothermic reaction. Under the action of self-heating, polypropylene will melt, smoke, or even burn.
為了降低聚丙烯的氧化發熱問題，現有技術中的主要措施是添加抗氧化劑。如專利CN02112743.3公開了一種可透明化聚丙烯組合物，為了提高聚丙烯的抗氧化性能在其中加入了酚類及亞膦酸酯類或硫酸類抗氧化劑。然而不同於透明聚丙烯，有色聚丙烯的抗氧化性更差，同時有色聚丙烯中的著色劑如炭黑等對抗氧化劑有吸附作用，會影響抗氧化劑在聚丙烯中的分佈，削弱抗氧化劑的作用。 In order to reduce the oxidative heating of polypropylene, the main measure in the prior art is to add antioxidants. For example, the patent CN02112743.3 discloses a transparent polypropylene composition. In order to improve the oxidation resistance of polypropylene, phenolic and phosphonite or sulfuric acid antioxidants are added. However, unlike transparent polypropylene, colored polypropylene has poorer oxidation resistance. At the same time, the coloring agent in colored polypropylene, such as carbon black, has an antioxidant effect, which will affect the distribution of antioxidant in polypropylene and weaken the antioxidant. effect.
本發明的目的在於提供一種抗氧化性好的有色聚丙烯纖維。 The object of the present invention is to provide a colored polypropylene fiber with good oxidation resistance.
本發明的技術解決方法： 一種有色聚丙烯纖維，該聚丙烯纖維中含有組分a受阻酚類抗氧化劑以及組分b亞磷酸酯類抗氧化劑和/或組分c受阻胺類抗氧化劑，其中組分a占有色聚丙烯纖維的400至15000ppm；含有組分b時，組分b與組分a的重量比為0.8至6.0：1，較佳0.8至4.0：1；含有組分c時，組分c占有色聚丙烯纖維的4000至50000ppm，較佳4000至20000ppm。 The technical solution of the present invention: A colored polypropylene fiber containing component a hindered phenolic antioxidant and component b phosphite antioxidant and/or component c hindered amine antioxidant, wherein component a occupies colored polypropylene 400 to 15000 ppm of fiber; when component b is contained, the weight ratio of component b to component a is 0.8 to 6.0:1, preferably 0.8 to 4.0:1; when component c is contained, component c occupies color polypropylene 4000 to 50000 ppm of fiber, preferably 4000 to 20000 ppm.
當組分a占有色聚丙烯纖維的1100至15000ppm時，有色聚丙烯纖維的L值較佳小於20。 When component a occupies 1100 to 15000 ppm of colored polypropylene fibers, the L value of colored polypropylene fibers is preferably less than 20.
當組分a占有色聚丙烯纖維的400ppm以上、小於1100ppm時，有色聚丙烯纖維的L值較佳20至75。 When component a occupies 400 ppm or more and less than 1100 ppm of colored polypropylene fibers, the L value of the colored polypropylene fibers is preferably 20 to 75.
所述組分a較佳占有色聚丙烯纖維的500至8000ppm。 The component a preferably occupies 500 to 8000 ppm of colored polypropylene fibers.
該有色聚丙烯纖維中較佳同時含有組分a、組分b和組分c。 The colored polypropylene fiber preferably contains component a, component b and component c at the same time.
所述組分a受阻酚類抗氧化劑較佳為四[β-(3,5-二第三丁基-4-羥基苯基)丙酸]新戊四醇酯；β-(3,5-二第三丁基-4-羥基苯基)丙酸十八碳醇酯；1,3,5-三甲基-2,4,6-三(3,5-二第三丁基-4-羥基苄基)苯或1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
所述組分b亞磷酸酯類抗氧化劑較佳為聚(二丙二醇)苯基亞磷酸酯；雙(2,6-二第三丁基-4-甲基苯基)新戊四醇二磷酸酯；三(2,4-二第三丁基苯基)苯基亞磷酸酯；雙(2,4,6-三第三丁基苯基)新戊四醇二亞磷酸酯；四(2,4-二第三丁基酚)-4,4'-聯苯二亞磷酸酯或3,9-雙十八烷氧基-2,4,8,10-四氧-3,9-二磷螺環[5.5]十一烷中的至 少一種。 The component b phosphite antioxidant is preferably poly(dipropylene glycol) phenyl phosphite; bis(2,6-di-third-butyl-4-methylphenyl) neopentaerythritol diphosphate Ester; tris(2,4-di-tert-butylphenyl) phenyl phosphite; bis(2,4,6-tri-tert-butyl phenyl) neopentaerythritol diphosphite; tetra(2 ,4-di-tert-butylphenol)-4,4'-biphenyl diphosphite or 3,9-bisoctadecyloxy-2,4,8,10-tetraoxy-3,9-di Phosphoro Spiral [5.5] Undecane to One less.
所述組分c受阻胺類抗氧化劑較佳為聚{[6-[(1,1,3,3-四甲基丁基)胺基]]-1,3,5-三
本發明還公開了一種有色聚丙烯纖維的製備方法，將聚丙烯與組分a受阻酚類抗氧化劑以及組分b亞磷酸酯類抗氧化劑和/或組分c受阻胺類抗氧化劑混合均勻並擠出造粒得到有色聚丙烯混合物，然後將有色聚丙烯混合物進行熔融紡絲得到有色聚丙烯纖維，其中組分a占聚丙烯混合物的400至15000ppm，添加組分b時，組分b與組分a的重量比為0.8至6.0：1；添加組分c時，組分c占聚丙烯混合物的4000至50000ppm。 The invention also discloses a method for preparing colored polypropylene fibers. The polypropylene is mixed with component a hindered phenol antioxidant and component b phosphite antioxidant and/or component c hindered amine antioxidant. Extrusion and granulation to obtain a colored polypropylene mixture, and then the colored polypropylene mixture is melt-spun to obtain colored polypropylene fibers, in which component a accounts for 400 to 15000 ppm of the polypropylene mixture. When component b is added, component b and group The weight ratio of component a is 0.8 to 6.0:1; when component c is added, component c accounts for 4000 to 50000 ppm of the polypropylene mixture.
本發明所述的有色聚丙烯纖維具有優異的抗氧化性能，裂解發熱少，應用廣泛。 The colored polypropylene fiber of the present invention has excellent oxidation resistance, less pyrolysis heat, and is widely used.
聚丙烯本身的結構不穩定，容易被氧化，並且氧化過 程伴隨有發熱現象，因此會影響使用聚丙烯纖維的製品的安全性。雖然添加抗氧化劑可以提高聚丙烯的抗氧化性能，但是對於抗氧化性更差的含有著色劑的有色聚丙烯而言，由於著色劑對抗氧化劑的吸附，會影響抗氧化劑的效果。而添加過多的抗氧化劑又會降低聚丙烯製品的物理性能，且會導致有色聚丙烯製品容易黃變。 The structure of polypropylene itself is unstable, easily oxidized, and oxidized Cheng is accompanied by heat generation, which will affect the safety of products using polypropylene fibers. Although the addition of antioxidants can improve the antioxidant performance of polypropylene, for colored polypropylene with colorants that are less resistant to oxidation, the adsorption of the colorants to the anti-oxidants will affect the effectiveness of the anti-oxidants. Adding too much antioxidant will reduce the physical properties of polypropylene products, and will cause colored polypropylene products to easily turn yellow.
本發明提供的有色聚丙烯纖維不僅具有優良的抗氧化性能，纖維的物理性能如強度也較好，且不容易發生黃變。 The colored polypropylene fiber provided by the present invention not only has excellent oxidation resistance, but also has good physical properties such as strength, and is not prone to yellowing.
本發明的有色聚丙烯纖維中含有組分a受阻酚類抗氧化劑以及組分b亞磷酸酯類抗氧化劑和/或組分c受阻胺類抗氧化劑，組分a占有色聚丙烯纖維的400至15000ppm。當聚丙烯纖維含有組分b時，組分b與組分a的重量比為0.8至6.0：1；當聚丙烯纖維含有組分c時，組分c占有色聚丙烯纖維的4000至50000ppm。 The colored polypropylene fiber of the present invention contains component a hindered phenolic antioxidant and component b phosphite antioxidant and/or component c hindered amine antioxidant, and component a occupies 400 to 15000ppm. When the polypropylene fiber contains the component b, the weight ratio of the component b to the component a is 0.8 to 6.0:1; when the polypropylene fiber contains the component c, the component c occupies 4000 to 50000 ppm of the colored polypropylene fiber.
在聚丙烯氧化分解的過程中會生成烷基自由基和過氧化自由基，其中烷基自由基會進一步氧化成過氧化自由基。而過氧化自由基不穩定，一部分過氧化自由基又會進一步生成氫過氧化物，加速聚丙烯的氧化分解。上述組分a受阻酚類抗氧化劑可以捕捉過氧化自由基，組分b亞磷酸酯類抗氧化劑可以捕捉氫過氧化物，組分c受阻胺類抗氧化劑可以同時捕捉過氧化自由基和烷基自由基。 During the oxidative decomposition of polypropylene, alkyl radicals and peroxy radicals will be generated, wherein the alkyl radicals will be further oxidized into peroxy radicals. Peroxide free radicals are unstable, and some of the free radicals will further generate hydroperoxides, accelerating the oxidative decomposition of polypropylene. The above component a hindered phenol antioxidants can capture peroxide radicals, component b phosphite antioxidants can capture hydroperoxides, and component c hindered amine antioxidants can capture both peroxide radicals and alkyl groups Free radicals.
為了獲得具有一定抗氧化性的有色聚丙烯纖維，纖維中組分a受阻酚類抗氧化劑的含量必須在400ppm以上，否則組分a受阻酚類抗氧化劑大部分被纖維中的著色劑吸附後將難以提高有色聚丙烯纖維的抗氧化性能，同時著色劑本身的抗氧化性能也較差，會導致有色聚丙烯纖維抗氧化性能的進一步惡化。而當有色聚丙烯 纖維中組分a受阻酚類抗氧化劑含量高於15000ppm時，不僅會增加有色聚丙烯纖維的製備成本，同時過量的組分a受阻酚類抗氧化劑在空氣中會被氧化生成醌類化合物，導致有色聚丙烯纖維發生黃變。 In order to obtain colored polypropylene fibers with certain oxidation resistance, the content of the component a hindered phenolic antioxidant in the fiber must be above 400 ppm, otherwise most of the component a hindered phenolic antioxidant will be absorbed by the coloring agent in the fiber. It is difficult to improve the oxidation resistance of colored polypropylene fibers. At the same time, the oxidation resistance of the colorant itself is also poor, which will lead to further deterioration of the oxidation resistance of colored polypropylene fibers. And when colored polypropylene When the content of the hindered phenolic antioxidant in the fiber is higher than 15000ppm, it will not only increase the production cost of colored polypropylene fibers, but also the excessive hindered phenolic antioxidant in the component a will be oxidized in the air to generate quinone compounds, resulting in Colored polypropylene fibers become yellow.
當組分a占有色聚丙烯纖維的1100至15000ppm時，有色聚丙烯纖維的L值小於20；當組分a占有色聚丙烯纖維的400ppm以上、小於1100ppm時，有色聚丙烯纖維的L值為20至75。 When component a occupies 1100 to 15000 ppm of colored polypropylene fibers, the L value of colored polypropylene fibers is less than 20; when component a occupies more than 400 ppm of colored polypropylene fibers and less than 1100 ppm, the L value of colored polypropylene fibers 20 to 75.
本發明的有色聚丙烯纖維中組分a受阻酚類抗氧化劑含量較佳為500至8000ppm。 The content of the hindered phenolic antioxidant of component a in the colored polypropylene fiber of the present invention is preferably 500 to 8000 ppm.
組分b亞磷酸酯類抗氧化劑除了具有上述捕捉氫過氧化物的作用外，還可以有效地抑制組分a受阻酚類抗氧化劑在空氣中的氧化，從而抑制聚丙烯的黃變。為了同時達到上述效果，有色聚丙烯纖維中組分b與組分a的重量比為0.8至6.0：1。當組分b與組分a的重量比低於0.8：1時，不能有效抑制組分a受阻酚類抗氧化劑在空氣的氧化，無法避免聚丙烯纖維的黃變，同時也不能有效的捕獲氫過氧化物，聚丙烯的氧化分解加速嚴重。當組分b與組分a的重量比大於6.0：1時，相對於組分a受阻酚類抗氧劑會有較多的組分b亞磷酸酯類抗氧化劑殘留在有色聚丙烯纖維中，而由於已經沒有可供捕捉的氫過氧化物，這部分組分b亞磷酸酯類抗氧化劑無法引起抗氧化的作用，反而會增加有色聚丙烯纖維的製備成本，同時大量的組分b亞磷酸酯類抗氧化劑會使聚丙烯纖維的強度下降。在含有組分b亞磷酸酯類抗氧化劑時，本發明的有色聚丙烯纖維中組分b與組分a的重量比較佳為0.8至4.0：1。 In addition to the above-mentioned effect of trapping hydroperoxides, component b phosphite antioxidants can also effectively inhibit the oxidation of component a hindered phenol antioxidants in the air, thereby inhibiting the yellowing of polypropylene. In order to achieve the above effects at the same time, the weight ratio of component b to component a in the colored polypropylene fibers is 0.8 to 6.0:1. When the weight ratio of component b to component a is lower than 0.8:1, the oxidation of the hindered phenolic antioxidant of component a in air cannot be effectively suppressed, the yellowing of polypropylene fiber cannot be avoided, and hydrogen cannot be effectively captured Peroxide, the oxidative decomposition of polypropylene accelerates seriously. When the weight ratio of component b to component a is greater than 6.0:1, there will be more component b phosphite antioxidants remaining in colored polypropylene fibers relative to the hindered phenolic antioxidant of component a, Since there is no hydroperoxide to capture, this component b phosphite antioxidant cannot cause antioxidant effect, but will increase the production cost of colored polypropylene fiber, and a large amount of component b phosphite Ester antioxidants will reduce the strength of polypropylene fibers. When the component b phosphite antioxidant is contained, the weight of the component b and the component a in the colored polypropylene fiber of the present invention is preferably 0.8 to 4.0:1.
組分c受阻胺類抗氧化劑的作用為捕捉烷基自由基及過氧化自由基。當有色聚丙烯纖維中組分c受阻胺類抗氧化劑的含量低於4000ppm時，不能有效地捕捉烷基自由基及過氧化自由基，過多的烷基自由基會進一步氧化成過氧化自由基，而過氧化自由基又會生成大量的氫過氧化物，進一步加速聚丙烯的氧化，無法提高有色聚丙烯纖維的抗氧化性能。而當組分c受阻胺類抗氧化劑的含量高於50000ppm時，有色聚丙烯纖維的強度下降，同時成本也會增加。在含有組分c受阻胺類抗氧化劑時，本發明的有色聚丙烯纖維中組分c的含量較佳4000至20000ppm。 The role of component c hindered amine antioxidants is to capture alkyl radicals and peroxide radicals. When the content of the hindered amine antioxidant component c in the colored polypropylene fiber is less than 4000 ppm, it cannot effectively capture alkyl radicals and peroxide radicals, and excessive alkyl radicals will be further oxidized into peroxide radicals. Peroxide free radicals will generate a large amount of hydroperoxide, which further accelerates the oxidation of polypropylene, and cannot improve the oxidation resistance of colored polypropylene fibers. When the content of the hindered amine antioxidant of component c is higher than 50000ppm, the strength of the colored polypropylene fiber decreases, and the cost also increases. When the component c hindered amine antioxidant is contained, the content of the component c in the colored polypropylene fiber of the present invention is preferably 4,000 to 20,000 ppm.
本發明所述有色聚丙烯纖維中含有組分a受阻酚類抗氧化劑以及組分b亞磷酸酯類抗氧化劑和/或組分c受阻胺類抗氧化劑，也即存在三種情況：一是含有組分a和組分b，二是含有組分a和組分c，三是含有組分a、組分b和組分c。其中較佳第三種情況，即有色聚丙烯纖維中同時含有組分a受阻酚類抗氧化劑、組分b亞磷酸酯類抗氧化劑和組分c受阻胺類抗氧化劑。 The colored polypropylene fiber of the present invention contains component a hindered phenolic antioxidant and component b phosphite antioxidant and/or component c hindered amine antioxidant, that is, there are three cases: Divided a and component b, the second is containing component a and component c, the third is containing component a, component b and component c. Among them, the preferred third case is that the colored polypropylene fiber contains both the component a hindered phenol antioxidant, the component b phosphite antioxidant and the component c hindered amine antioxidant.
對所述組分a受阻酚類抗氧化劑沒有特別的限定，可以是β-(3,5-二第三丁基-4-羥基苯基)丙酸甲酯；N,N'-1,6-亞己基-雙[3-(3,5-二第三丁基-4-羥基苯基)丙醯胺]；1,3,5-三-(3,5-二環己基-4-羥基苄基)異氰尿酸酯；N,N'-雙[3-(3,5-二第三丁基-4-羥基苯基)丙醯]肼；3-(3,5-二第三丁基-4-羥基)丙酸十八酯；2,2'-亞甲基雙(4-甲基-6-第三丁基酚)；2,6-二第三丁基-4-甲基苯酚；4,4'-甲撐雙(2,6-二第三丁基苯酚)；2,2-硫代雙[3-(3,5-二第三丁基-4-羥基苯基)丙酸乙酯]；四[β-(3,5-二第三丁基-4-羥基苯基)丙酸]新戊四醇酯；β-(3,5-二第三丁基-4-羥基苯基)丙酸十八碳醇酯；1,3,5-三甲基-2,4,6-三
(3,5-二第三丁基-4-羥基苄基)苯或1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
對所述組分b亞磷酸酯類抗氧化劑沒有特別的限定，可以是二甲基亞磷酸酯、雙(2,4-二第三丁基苯基)苯基亞磷酸酯；三(1,2,2,6,6-五甲基哌啶醇)亞磷酸酯；三(壬基酚)亞磷酸酯；雙(2,4,6-三第三丁基苯基)新戊四醇二亞磷酸酯；雙(2,4,6-三第三丁基苯基)新戊四醇二亞磷酸酯；四(2,4-二第三丁基酚)-4,4'-聯苯二亞磷酸酯；二癸基苯基亞磷酸酯；二苯基異辛基亞磷酸酯；聚(二丙二醇)苯基亞磷酸酯；三(2,4-二第三丁基苯基)亞磷酸酯；3,9-雙十八烷氧基-2,4,8,10-四氧-3,9-二磷螺環[5.5]十一烷；三苄基亞磷酸酯或亞磷酸三(2-乙基己基)酯中的至少一種，其中較佳聚(二丙二醇)苯基亞磷酸酯；雙(2,6-二第三丁基-4-甲基苯基)新戊四醇二磷酸酯；三(2,4-二第三丁基苯基)亞磷酸酯；雙(2,4,6-三第三丁基苯基)新戊四醇二亞磷酸酯；四(2,4-二第三丁基酚)-4,4'-聯苯二亞磷酸酯或3,9-雙十八烷氧基-2,4,8,10-四氧-3,9-二磷螺環[5.5]十一烷中的至少一種。 The component b phosphite antioxidant is not particularly limited, and may be dimethyl phosphite, bis(2,4-di-tert-butylphenyl)phenyl phosphite; tri(1, 2,2,6,6-pentamethyl piperidinol) phosphite; tris(nonylphenol) phosphite; bis(2,4,6-tri-tert-butylphenyl) neopentaerythritol di Phosphite; bis(2,4,6-tri-tert-butylphenyl) neopentaerythritol diphosphite; tetra(2,4-di-tert-butylphenol)-4,4'-biphenyl Diphosphite; didecylphenyl phosphite; diphenyl isooctyl phosphite; poly(dipropylene glycol) phenyl phosphite; tri(2,4-di-tert-butylphenyl) phosphite Phosphate ester; 3,9-bisoctadecyloxy-2,4,8,10-tetraoxy-3,9-diphosphorane spiro[5.5]undecane; tribenzyl phosphite or triphosphite At least one of (2-ethylhexyl) esters, of which poly(dipropylene glycol) phenyl phosphite is preferred; bis(2,6-di-tert-butyl-4-methylphenyl) neopentaerythritol Diphosphate; tris(2,4-di-tert-butylphenyl) phosphite; bis(2,4,6-tri-tert-butylphenyl) neopentaerythritol diphosphite; tetra(2 ,4-di-tert-butylphenol)-4,4'-biphenyl diphosphite or 3,9-bisoctadecyloxy-2,4,8,10-tetraoxy-3,9-di At least one of phosphorus spiro [5.5] undecane.
對所述組分c受阻胺類抗氧化劑沒有特別的限定，可以是雙(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯；3-(2,2,6,6-四甲基哌啶-4-胺基)丙酸十二酯；2-(3',5'-二第三丁基-2'-羥基苯基)-5-氯苯并三唑；2,4,6-三氯-1,3,5-三
本發明所述的抗氧化劑，也可以與羥基胺類並用，其中可列舉的有二十八烷基羥胺。 The antioxidant described in the present invention can also be used in combination with hydroxylamines, among which octacosylhydroxylamine can be cited.
本發明還公開了一種有色聚丙烯纖維的製備方法，將聚丙烯與組分a受阻酚類抗氧化劑以及組分b亞磷酸酯類抗氧化劑和/或組分c受阻胺類抗氧化劑混合均勻並擠出造粒得到有色聚丙烯混合物，然後將有色聚丙烯混合物進行熔融紡絲得到有色聚丙烯纖維，其中組分a占聚丙烯混合物的400至15000ppm，添加組分b時，組分b與組分a的重量比為0.8至6：1；添加組分c時，組分c占聚丙烯混合物的4000至50000ppm。 The invention also discloses a method for preparing colored polypropylene fibers. The polypropylene is mixed with component a hindered phenol antioxidant and component b phosphite antioxidant and/or component c hindered amine antioxidant. Extrusion and granulation to obtain a colored polypropylene mixture, and then the colored polypropylene mixture is melt-spun to obtain colored polypropylene fibers, in which component a accounts for 400 to 15000 ppm of the polypropylene mixture. When component b is added, component b and group The weight ratio of component a is 0.8 to 6:1; when component c is added, component c accounts for 4,000 to 50,000 ppm of the polypropylene mixture.
本發明的有色聚丙烯纖維可以是在聚丙烯切片中共混著色劑母粒然後進行紡絲得到的纖維，也可以是聚丙烯切片和聚酯共混後再進行紡絲、染色得到的纖維。 The colored polypropylene fiber of the present invention may be a fiber obtained by blending a colorant masterbatch in polypropylene chips and then spinning, or a fiber obtained by blending polypropylene chips and polyester and then spinning and dyeing.
所述著色劑可以是顏料，也可以是染料，本發明對顏料和染料的種類不做特別的限定，可以是聚合物用各種顏料和染料，如炭黑、鈦白粉、鎘紅、群菁、酞菁綠、酞菁藍、水固紅、鋅黃、漢沙黃、TERATOP BLUE NFB GR、TERATOP RED NFR、TERATOP YELLOW NFG、TERASIL BLACK WW-KSN等。對聚丙烯纖維中著色劑的含量也不做特別的限定，在現有技術的公知範圍內，根據應用場合或市場需求可以做出相應的調整。另外，對著色劑的引入方式和時機也不作特別的限定，如引入方式可以是直接添加著色劑，也可以添加含有著色劑的母粒；引入時機可以是在聚丙烯與抗氧化劑共混時一起加入，也可以在聚丙烯與抗氧化劑共混擠出之後加入 混合再熔融紡絲。 The colorant may be a pigment or a dye. The present invention does not particularly limit the types of pigments and dyes, and may be various pigments and dyes for polymers, such as carbon black, titanium dioxide, cadmium red, ultramarine, Phthalocyanine green, phthalocyanine blue, water fast red, zinc yellow, Hansa yellow, TERATOP BLUE NFB GR, TERATOP RED NFR, TERATOP YELLOW NFG, TERASIL BLACK WW-KSN, etc. The content of the colorant in the polypropylene fiber is also not particularly limited. Within the known range of the prior art, the corresponding adjustment can be made according to the application occasion or market demand. In addition, the introduction method and timing of the colorant are not particularly limited. For example, the introduction method may be to add the colorant directly or to add the masterbatch containing the colorant; the introduction timing may be when the polypropylene and the antioxidant are blended together. It can also be added after polypropylene and antioxidant are blended and extruded Mix and then melt spinning.
本發明所述的有色聚丙烯纖維，由於其中不同組分抗氧劑之間的相互協同作用，使其具有優異的抗氧化性能，物性好，不易黃變。 The colored polypropylene fiber according to the present invention has excellent antioxidant properties due to the synergistic effect between antioxidants of different components, and has good physical properties and is not easily yellowed.
本發明所涉及的測試方法如下： The test methods involved in the present invention are as follows:
首先將有色聚丙烯纖維製備成筒編物，並按照JIS L 0217 103法進行前處理。然後依據《聚丙烯纖維的酸化發熱試驗方法(加速法)》(日本化學纖維協會法)進行測試並評價。當試驗時間到達100小時時，自身並未發熱，即判斷該聚丙烯纖維的耐氧化發熱性合格。否則，判定為不合格。 First, the colored polypropylene fiber is prepared into a knitted fabric, and pre-treated according to JIS L 0217 103 method. Then, it is tested and evaluated in accordance with "Acid Heating Test Method for Polypropylene Fiber (Acceleration Method)" (Japan Chemical Fiber Association Method). When the test time reaches 100 hours, it does not generate heat by itself, that is, the polypropylene fiber is judged to be qualified for oxidation and heat resistance. Otherwise, it is judged as unqualified.
在密閉容器中放入NOx氣體發生劑(85%磷酸及2%的亞硝酸水溶液)，然後將試樣及藍色標準染色佈置於容器內，當藍色標準染色布顏色褪為標準灰度板3號時，更換藍色標準染色布，當顏色再次達到標準灰度板3號時，將試樣取出，並清洗2次，晾乾。通過Datacolor 650分光光度儀對黃變值進行測定。 Put NOx gas generating agent (85% phosphoric acid and 2% nitrous acid aqueous solution) in the closed container, and then arrange the sample and blue standard dyeing in the container, when the color of the blue standard dyeing cloth fades to the standard gray board At No. 3, replace the blue standard dyed cloth. When the color reaches the standard gray plate No. 3 again, remove the sample, wash it twice, and dry it. The yellowing value was measured by Datacolor 650 spectrophotometer.
通過強伸度測試儀進行測試。測試速度為200mm/min，兩夾具之間的距離是200mm。 The test is carried out by a strong elongation tester. The test speed is 200mm/min, and the distance between the two fixtures is 200mm.
取纖維樣品，稱取重量為W1，用差示掃描量熱儀，在氣體氛圍為壓空、氣體流量為60±0.05ml條件下，從25℃開始以30℃/min的速度升溫至160℃，保持22小時，通過分析得出重量減少率，重 量減少率在10wt%以下的話，科肯法判斷為合格。重量減少率越低，表明抗氧化性越好。 Take a fiber sample, weigh it as W1, use a differential scanning calorimeter, under the condition of a gas atmosphere of air pressure and a gas flow rate of 60±0.05ml, from 25℃ to 30℃/min to 160℃ , Hold for 22 hours, the weight loss rate is obtained through analysis, weight If the amount reduction rate is 10 wt% or less, the Keken method determines that it is acceptable. The lower the weight reduction rate, the better the oxidation resistance.
通過Datacolor 650分光光度儀對染色後的筒編物進行L值測定。 The L value of the dyed tube knitted fabric was measured by Datacolor 650 spectrophotometer.
本發明實施例中涉及的抗氧化劑的的簡寫如下。 The abbreviations of antioxidants involved in the examples of the present invention are as follows.
組分a：(1)1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
組分b： (1)聚(二丙二醇)苯基亞磷酸酯(簡寫：抗氧化劑PDP)；(2)3,9-雙十八烷氧基-2,4,8,10-四氧-3,9-二磷螺環[5.5]十一烷(簡寫：抗氧化劑619)；(3)三(2,4-二第三丁基苯基)亞磷酸酯(簡寫：抗氧化劑168)；(4)三(1,2,2,6,6-五甲基哌啶醇)亞磷酸酯(簡寫：組分b1)；(5)雙(2,4,6-三第三丁基苯基)新戊四醇二亞磷酸酯(簡寫：抗氧化劑633)；(6)雙(2,4-二第三丁基苯基)苯基亞磷酸酯(簡寫：組分b2)。 Component b: (1) Poly(dipropylene glycol) phenyl phosphite (abbreviation: antioxidant PDP); (2) 3,9-bisoctadecyloxy-2,4,8,10-tetraoxy-3,9- Diphospho spiro[5.5]undecane (abbreviation: antioxidant 619); (3) tris(2,4-di-tert-butylphenyl) phosphite (abbreviation: antioxidant 168); (4) tri (1,2,2,6,6-pentamethylpiperidinol) phosphite (abbreviation: component b1); (5) bis(2,4,6-tri-tert-butylphenyl) neopentyl Tetraol diphosphite (abbreviation: antioxidant 633); (6) bis(2,4-di-t-butylphenyl)phenyl phosphite (abbreviation: component b2).
組分c：(1)聚{[6-[(1,1,3,3-四甲基丁基)胺基]]-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(四[β-(3,5-二第三丁基-4-羥基苯基)丙酸]新戊四醇酯)、組分b(3,9-雙十八烷氧基-2,4,8,10-四氧-3,9-二磷螺環[5.5]十一烷)和組分c(NI,NⅡ,NⅢ,NⅣ-四(2,4-二(N-1,2,2,6,6-五甲基-4-哌啶基)亞胺基-n)))-丁基胺基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三甲基-2,4,6-三(3,5-二第三丁基-4-羥基苄基)苯)、組分b(三(2,4-二第三丁基苯基)亞磷酸酯)和著色劑母粒(黑色)加入混煉機進行混煉並擠出造粒，其中組分a占聚丙烯混合物的1100ppm，組分b與組分a的重量比為3.0：1；最後將粒料經熔融紡絲製成有色聚丙烯纖維。 Polypropylene slices, component a (1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene), component b( Tri(2,4-di-tert-butylphenyl) phosphite) and colorant masterbatch (black) are added to the kneader to be kneaded and extruded and granulated, where component a accounts for 1100 ppm of the polypropylene mixture, The weight ratio of component b to component a is 3.0:1; finally, the pellets are melt-spun to make colored polypropylene fibers.
將聚丙烯切片、組分a(β-(3,5-二第三丁基-4-羥基苯基)丙酸甲酯)、組分c(聚丁二酸(4-羥乙基-2,2,6,6-四甲基-1-哌啶乙醇)酯)和著色劑母粒(黑色)加入混煉機進行混煉並擠出造粒，其中組分a占聚丙烯混合物的6000ppm，組分c占聚丙烯混合物的10000ppm；最後將粒料經熔融紡絲製成有色聚丙烯纖維。 Polypropylene slices, component a (β-(3,5-di-tert-butyl-4-hydroxyphenyl) methyl propionate), component c (polysuccinic acid (4-hydroxyethyl-2 , 2,6,6-tetramethyl-1-piperidineethanol) ester) and colorant masterbatch (black) are added to the kneader to be kneaded and extruded and granulated, where component a accounts for 6000 ppm of the polypropylene mixture , Component c accounts for 10000ppm of the polypropylene mixture; finally, the pellets are melt-spun into colored polypropylene fibers.
將聚丙烯切片、組分a(N,N'-1,6-亞己基-雙[3-(3,5-二第三丁基-4-羥基苯基)丙醯胺])和組分b(雙(2,4-二第三丁基苯基)苯基亞磷酸酯)加入混煉機進行混煉並擠出造粒，其中組分a占聚丙烯混合物的10000ppm，組分b與組分a的重量比為0.8：1；最後將粒料與著色劑母粒(黑色)混合後經熔融紡絲製成有色聚丙烯纖維。 Polypropylene slices, component a (N,N'-1,6-hexylene-bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionamide]) and components b (bis(2,4-di-tert-butylphenyl) phenyl phosphite) is added to the kneader to be kneaded and extruded and granulated, where component a occupies 10,000 ppm of the polypropylene mixture, component b and The weight ratio of component a is 0.8:1; finally, the pellets are mixed with the colorant masterbatch (black) and then melt-spun to make colored polypropylene fibers.
將聚丙烯切片、組分a(N,N'-雙[3-(3,5-二第三丁基-4-羥基苯基)丙醯]肼)和組分b(三(1,2,2,6,6-五甲基哌啶醇)亞磷酸酯)加入混煉機進行混煉並擠出造粒，其中組分a占聚丙烯混合物的 6000ppm，組分b與組分a的重量比為6.0：1；最後將粒料與著色劑母粒(黑色)混合後經熔融紡絲製成有色聚丙烯纖維。 Polypropylene slices, component a (N, N'-bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl) propyl hydrazine) and component b (tri (1,2 , 2,6,6-pentamethyl piperidinol) phosphite) added to the mixer for mixing and extrusion granulation, where component a accounts for the polypropylene mixture 6000ppm, the weight ratio of component b to component a is 6.0:1; finally, the pellets are mixed with the colorant masterbatch (black) and then melt-spun to make colored polypropylene fibers.
將聚丙烯切片、組分a(3-(3,5-二第三丁基-4-羥基)丙酸十八酯)和組分c(雙(1,2,2,6,6-五甲基-4-哌啶基)癸二酸酯)加入混煉機進行混煉並擠出造粒，其中組分a占聚丙烯混合物的1100ppm，組分c占聚丙烯混合物的5000ppm；最後將粒料與著色劑母粒(黑色)混合後經熔融紡絲製成有色聚丙烯纖維。 Polypropylene slices, component a (3-(3,5-di-tributyl-4-hydroxy)octadecyl propionate) and component c (bis(1,2,2,6,6-penta Methyl-4-piperidinyl) sebacate) is added to the kneading machine to be kneaded and extruded and granulated, where component a accounts for 1100 ppm of the polypropylene mixture and component c accounts for 5000 ppm of the polypropylene mixture; The pellets are mixed with colorant masterbatch (black) and then melt-spun to produce colored polypropylene fibers.
將聚丙烯切片、組分a(3-(3,5-二第三丁基-4-羥基)丙酸十八酯)和組分c(3-(2,2,6,6-四甲基哌啶-4-胺基)丙酸十二酯)加入混煉機進行混煉並擠出造粒，其中組分a占聚丙烯混合物的15000ppm，組分c占聚丙烯混合物的13000ppm；最後將粒料與著色劑母粒(黑色)混合後經熔融紡絲製成有色聚丙烯纖維。 Polypropylene slices, component a (3-(3,5-di-tert-butyl-4-hydroxy)octadecyl propionate) and component c (3-(2,2,6,6-tetramethyl (Piperidin-4-amino) dodecyl propionate) was added to the kneader for mixing and extrusion granulation, where component a accounted for 15000 ppm of the polypropylene mixture and component c accounted for 13000 ppm of the polypropylene mixture; finally The pellets are mixed with colorant masterbatch (black) and then melt-spun to produce colored polypropylene fibers.
將聚丙烯切片、組分a(2,2'-亞甲基雙(4-甲基-6-第三丁基酚))、組分b(雙(2,4,6-三第三丁基苯基)新戊四醇二亞磷酸酯)和組分c(2,4,6-三氯-1,3,5-三
將聚丙烯切片、組分a(2,6-二第三丁基-4-甲基苯酚)、組分b(雙(2,4,6-三第三丁基苯基)新戊四醇二亞磷酸酯)和組分c(N- 丁基-2,2,6,6-四甲基-4-哌啶胺)加入混煉機進行混煉並擠出造粒，其中組分a占聚丙烯混合物的1300ppm，組分b與組分a的重量比為4：1，組分c占聚丙烯混合物的15000ppm；最後將粒料與著色劑母粒(黑色)混合後經熔融紡絲製成有色聚丙烯纖維。 Polypropylene slices, component a (2,6-di-tert-butyl-4-methylphenol), component b (bis (2,4,6-tri-tert-butylphenyl) neopentyl alcohol Diphosphite) and component c (N- Butyl-2,2,6,6-tetramethyl-4-piperidinamine) was added to the kneader to be kneaded and extruded and granulated, where component a accounted for 1300 ppm of the polypropylene mixture, component b and group The weight ratio of sub-a is 4:1, and component c accounts for 15000 ppm of the polypropylene mixture; finally, the pellets are mixed with the colorant masterbatch (black) and then melt-spun to make colored polypropylene fibers.
將聚丙烯切片、組分a(1,3,5-三甲基-2,4,6-三(3,5-二第三丁基-4-羥基苄基)苯)、組分b(聚(二丙二醇)苯基亞磷酸酯)、組分c(1,3,5-三
將聚丙烯切片、組分a(四[β-(3,5-二第三丁基-4-羥基苯基)丙酸]新戊四醇酯)、組分b(3,9-雙十八烷氧基-2,4,8,10-四氧-3,9-二磷螺環[5.5]十一烷)和組分c(1,3,5-三
將聚丙烯切片、組分a(1,3,5-三甲基-2,4,6-三(3,5-二第三丁基-4-羥基苄基)苯)、組分b(三(2,4-二第三丁基苯基)亞磷酸酯)和著色劑母粒(黑色)加入混煉機進行混煉並擠出造粒，其中組分a占聚丙烯混合物的1200ppm，組分b與組分a的重量比為3.0：1；最後將粒料經熔融紡絲製成有色聚丙烯纖維。 Polypropylene slices, component a (1,3,5-trimethyl-2,4,6-tris(3,5-di-tert-butyl-4-hydroxybenzyl)benzene), component b( Tri(2,4-di-tert-butylphenyl) phosphite) and colorant masterbatch (black) are added to the kneading machine to be kneaded and extruded and granulated, where component a accounts for 1200 ppm of the polypropylene mixture, The weight ratio of component b to component a is 3.0:1; finally, the pellets are melt-spun to make colored polypropylene fibers.
將聚丙烯切片、組分a(β-(3,5-二第三丁基-4-羥基苯基)丙酸甲酯)、組分c(1,3,5-三
將聚丙烯切片、組分a(N,N'-1,6-亞己基-雙[3-(3,5-二第三丁基-4-羥基苯基)丙醯胺])和組分b(三(2,4-二第三丁基苯基)亞磷酸酯)加入混煉機進行混煉並擠出造粒，其中組分a占聚丙烯混合物的10000ppm，組分b與組分a的重量比為0.8：1；最後將粒料與著色劑母粒(黑色)混合後經熔融紡絲製成有色聚丙烯纖維。 Polypropylene slices, component a (N,N'-1,6-hexylene-bis[3-(3,5-di-tert-butyl-4-hydroxyphenyl)propionamide]) and components b (tris(2,4-di-tert-butylphenyl) phosphite) is added to the kneader to be kneaded and extruded and granulated, where component a occupies 10000ppm of polypropylene mixture, component b and component The weight ratio of a is 0.8:1; finally, the pellets and the colorant masterbatch (black) are mixed and melt-spun to make colored polypropylene fibers.
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基
-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、占最終纖維10wt%的聚酯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、占最終纖維10wt%的聚酯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、占最終纖維10wt%的聚酯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、占最終纖維10wt%的聚酯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、占最終纖維10wt%的聚酯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、占最終纖維10wt%的聚酯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
將聚丙烯切片、組分a(1,3,5-三(4-第三丁基-3-羥基-2,6-二甲基苄基)-1,3,5-三
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| CN109487365B (en) * | 2017-09-11 | 2021-09-28 | 东丽纤维研究所（中国）有限公司 | Dyeable polyolefin fiber |
| TW201930664A (en) * | 2018-01-12 | 2019-08-01 | 大陸商東麗纖維研究所（中國）有限公司 | Coloured polypropylene fibre and preparation method therefor |
| CN108300391A (en) * | 2018-02-02 | 2018-07-20 | 广州惠利电子材料有限公司 | A kind of double-component cold curing transparent epoxy glue of color inhibition and preparation method thereof |
| CN110218273A (en) * | 2019-04-04 | 2019-09-10 | 东华能源股份有限公司 | A kind of production method of the spun-bonded non-woven acrylic resin of the color inhibition of Narrow Molecular Weight Distribution |
| TWI754918B (en) * | 2020-04-20 | 2022-02-11 | 財團法人紡織產業綜合研究所 | Photochromic polypropylene fiber and preparation method thereof |
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