CN112981952A - 一种通过接枝聚合提升涤纶染色深度和色牢度的方法 - Google Patents
一种通过接枝聚合提升涤纶染色深度和色牢度的方法 Download PDFInfo
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Abstract
本发明公开了一种通过接枝聚合提升涤纶染色深度和色牢度的方法,属于纺织染整技术领域。具体是首先借助酯酶进行涤纶预处理,使纤维表面刻蚀产生羧基和羟基,再以分散染料进行染色;然后通过含乙烯基的三乙氧基硅烷醇解与涤纶反应,在涤纶表面引入乙烯基;最后借助硫酸亚铁和双氧水,引发涤纶与含氟丙烯酸酯和丙烯酸单体接枝共聚,在纤维表面形成低折射率聚合物,生成的铁离子与聚合物分子中羧基和涤纶上羧基络合,提升涤纶色牢度的方法。具体步骤包括:(1)涤纶酯酶预处理;(2)分散染料染色;(3)涤纶接枝乙烯基;(4)涤纶织物接枝共聚。与传统染色相比,涤纶染物色深和色牢度较高,处理条件缓和,织物拒水效果好。
Description
技术领域
本发明是一种提升涤纶染色深度和色牢度的方法,特别涉及一种通过接枝聚合提升涤纶染色深度和色牢度的方法,属于纺织染整技术领域。
背景技术
涤纶纤维是最常用的合成纤维原料,在家居服、运动服装和户外纺织品中得到广泛应用。与天然纤维相比,涤纶纤维制品具有较强的单纤维强度,不仅手感柔软,且具有优良的尺寸稳定性。实际染整生产中发现,涤纶织物深色产品(特别是黑色)加工中较难以达到所需的染色深度;即使部分涤纶产品能染得深色,其产品湿摩擦牢度和耐升华牢度较难达到满意的水平。因此,开发具有高色深、高色牢度的涤纶染色加工工艺成为研究人员的工作重点。
实现涤纶染色织物表观深度增深的方法主要有两大类,一类是通过增加纤维表面的粗糙度,减少镜面反射和增加漫发射的方法实现增深;另一种是采用低折射率树脂整理染色织物,减少表面反射光以达到提高织物表观深度的目的。碱减量是最简单的一种实现涤纶表面刻蚀的方法,经碱减量处理后的聚酯织物纤维表面出现凹坑和沟槽,增大了纤维比表面积,有利于染料在其表面吸附、扩散和沉积;另一方面,凹坑和沟槽增加了聚酯纤维表面粗糙程度,增加了漫反射,在同等染料用量条件下,而增加了视觉色深度。碱减量处理聚酯织物的缺点在于工艺过程不易控制,易产生较大的织物强力下降,减量加工中还会产生高COD的废水,不利于环境保护。
此外,选用低折射率树脂在涤纶纤维表面成膜,通过降低折射率,也可实现涤纶染色织物表观深度的增加。目前,市场上低折射率树脂薄膜主要有聚氨酯树脂、含氟树脂和有机硅树脂。其中,含氟类树脂除对染色织物色外观有明显的增深效果外,还能通过成膜一定程度上提升织物的染色牢度,并赋予织物表面疏水性,具有潜在的应用前景。
发明内容
本发明主要是解决现有技术中存在的不足,提供一种为解决上述问题,本发明提供了一种通过接枝聚合提升涤纶染色深度和色牢度的方法,旨在实现在较缓和条件下进行涤纶织物色深增加和色牢度提升,提高染料利用率,减少染色废水排放,减轻生产能耗低,达到生态染整加工的目的。的一种通过接枝聚合提升涤纶染色深度和色牢度的方法。
本发明的上述技术问题主要是通过下述技术方案得以解决的:
一种通过接枝聚合提升涤纶染色深度和色牢度的方法,按以下步骤进行:
首先,借助酯酶进行涤纶织物预处理,使纤维表面刻蚀产生羧基和羟基,再以分散染料进行染色;然后,通过含乙烯基的三乙氧基硅烷醇解与涤纶反应,在涤纶表面引入乙烯基;最后,借助硫酸亚铁和双氧水体系,引发涤纶与含氟丙烯酸酯和丙烯酸单体接枝共聚,在纤维表面形成低折射率聚合物,反应中生成的三价铁离子与聚合物分子中羧基和涤纶上羧基络合,提升涤纶色牢度的方法。
作为优选,具体工艺步骤如下:
(1)涤纶酯酶预处理:以酯酶进行涤纶织物预处理,处理后以去离子水净洗;
处理工艺处方及条件:酯酶1~2.5U/mL,渗透剂0.2~2g/L,pH范围7.0~9.0,温度30~50℃,处理时间1~2小时;
(2)分散染料染色:经步骤(1)处理的涤纶织物采用分散染料进行高温高压染色,染色后进行还原清洗;
处理工艺处方及条件:分散染料0.2~2.5%o.w.f,pH值的范围4~5.5,温度130℃,处理时间30~45分钟;还原清洗时保险粉2.5~5g/L,纯碱2~4g/L,温度为80℃,处理时间10~20分钟;
(3)涤纶接枝乙烯基:经步骤(2)处理的涤纶织物以含乙烯基的三乙氧基硅烷处理,处理后以去离子水净洗,得到含乙烯基的改性涤纶;
处理工艺处方及条件:含乙烯基的三乙氧基硅烷:水:乙醇=1:1:2~5;处理温度30~40℃,pH范围9~10,处理时间1~2小时;
(4)涤纶织物接枝共聚:经步骤(3)处理的改性涤纶织物浸渍在硫酸亚铁、双氧水、含氟丙烯酸酯和丙烯酸的混合乳液中,通过自由基反应实现涤纶表面接枝共聚,整理后织物在室温下水洗15分钟,在100℃烘干;
整理工艺处方及条件:硫酸亚铁2~6g/L,双氧水1~2.5g/L,含氟丙烯酸酯2.5~5g/L,丙烯酸1~2g/L,乳化剂十二烷基硫酸钠0.5~1g/L,处理温度30~40℃,pH范围4~6,处理时间0.5~2小时。
作为优选,所述酯酶包括来源于动物、植物或微生物且对酯键具有水解功效的酶;所述含氟丙烯酸酯的单体包括含氟丙烯酸乙酯、含氟丙烯酸丁酯和含氟甲基丙烯酸乙酯;所述涤纶织物包括以涤纶纤维为原料的针织物和机织物。
有益效果:
本发明先利用酯酶进行涤纶织物生物酶法预处理,经分散染料染色后,涤纶纤维表面接枝乙烯基单体,再与含乙烯基含氟的丙烯酸酯和丙烯酸单体接枝聚合,赋予涤纶染色织物增深效果,同时借助于三价铁离子与聚合物和涤纶形成络合结构,提升色牢度。与通过染色中增加染料用量进行增深、增加还原水洗次数提升色牢度的传统方法相比,本发明具有以下优点:
(1)反应条件缓和,在低温近中性条件下进行织物预处理,通过增加纤维表面粗糙度,促进后续分散染料在纤维表面的着色深度,同时避免了碱处理对纤维易造成的损伤的缺陷,该过程中酶法预处理后残液对环境影响较小;
(2)采用自由基聚合实现涤纶纤维表面含氟丙烯酸酯和丙烯酸共聚结合,不仅在涤纶表面沉积了低折射率聚合物分子层,提高了织物染色深度,通过铁离子与聚合物和涤纶纤维三者间络合,避免了热定型中分散染料从涤纶织物上升华,提高了织物染色牢度,起到一举二得的功效;
(3)采用本发明述及的方法不但实现了涤纶染色织物的表面增深和色牢度提升,而且赋予织物较好的拒水整理效果。
具体实施方式
下面通过实施例,对本发明的技术方案作进一步具体的说明。
采用酯酶进行涤纶织物预处理,增加纤维表面粗糙度,然后以分散染料进行染色;通过芬顿反应催化接枝聚合,在涤纶纤维表面形成低折射率含氟聚合物实现增深,生成的三价铁与聚合物分子中羧基和涤纶上羧基络合,提升涤纶色牢度。经上述处理后,分别测定涤纶织物试样染色深度K/S值(D65光源,10°视场)、参照GB/T 3920-2008测定湿摩擦牢度、参照GB/T 6152-1997测定耐熨烫升华牢度、测定10s时的涤纶染色织物表面接触角,具体实施例如下:
实施例1:
(1)涤纶酯酶预处理:以酯酶进行涤纶织物预处理,处理后以去离子水净洗;处理工艺处方及条件:酯酶1U/mL,渗透剂0.2g/L,pH 7.0,温度30℃,处理1小时;
(2)分散染料染色:经步骤(1)处理的涤纶织物采用分散染料进行高温高压染色,染色后进行还原清洗;处理工艺处方及条件:分散染料0.5%o.w.f,pH 4,130℃,染色30分钟;还原清洗时保险粉2.5g/L,纯碱2g/L,80℃处理10分钟;
(3)涤纶接枝乙烯基:经步骤(2)处理的涤纶织物以含乙烯基的三乙氧基硅烷处理,处理后以去离子水净洗,得到含乙烯基的改性涤纶;处理工艺处方及条件:含乙烯基的三乙氧基硅烷:水:乙醇=1:1:2;处理温度30℃,pH 9,处理时间1小时;
(4)涤纶织物接枝共聚:经步骤(3)处理的改性涤纶织物浸渍在硫酸亚铁、双氧水、含氟丙烯酸乙酯和丙烯酸的混合乳液中,通过自由基反应实现涤纶表面接枝共聚,整理后织物在室温下水洗15分钟,在100℃烘干;整理工艺处方及条件:硫酸亚铁2g/L,双氧水1g/L,含氟丙烯酸乙酯2.5g/L,丙烯酸1g/L,乳化剂十二烷基硫酸钠0.5g/L,处理温度30℃,pH4,处理0.5小时。
上述步骤(1)~(4)中所述涤纶织物类别为涤纶长丝为原料的机织物。
试样1:经步骤(2)染色处理;未经过步骤(1)、(3)和(4)处理;
试样2:经步骤(1)、(2)处理,未经过步骤(3)和(4)处理;
试样3:经步骤(1)、(2)和(4)处理样,未经过步骤(3)处理;
试样4:经步骤(1)、(2)、(3)和(4)处理;
经上述工艺处理后,分别测定试样1~4的染色深度K/S、湿摩擦牢度、耐熨烫升华牢度和表面润湿接触角。其中,试样1的表面深度为K/S为2.51,湿摩擦牢度3级、升华牢度3.5级、表面接触角0°;其中试样2的表面深度为K/S为2.65,湿摩擦牢度3级、升华牢度3.5级、表面接触角0°;其中试样3的表面深度为K/S为3.01,湿摩擦牢度3级、升华牢度4级、表面接触角90°其中试样4的表面深度为K/S为3.25,湿摩擦牢度4级、升华牢度4.5级、表面接触角112°。
实施例2:
(1)涤纶酯酶预处理:以酯酶进行涤纶织物预处理,处理后以去离子水净洗;处理工艺处方及条件:酯酶2.5U/mL,渗透剂2g/L,pH范围9.0,温度50℃处理2小时;
(2)分散染料染色:经步骤(1)处理的涤纶织物采用分散染料进行高温高压染色,染色后进行还原清洗;处理工艺处方及条件:分散染料2.5%o.w.f,pH 5.5,130℃,45分钟;还原清洗时保险粉5g/L,纯碱4g/L,80℃处理20分钟;
(3)涤纶接枝乙烯基:经步骤(2)处理的涤纶织物以含乙烯基的三乙氧基硅烷处理,处理后以去离子水净洗,得到含乙烯基的改性涤纶;处理工艺处方及条件:含乙烯基的三乙氧基硅烷:水:乙醇=1:1:5;处理温度40℃,pH 10,处理2小时;
(4)涤纶织物接枝共聚:经步骤(3)处理的改性涤纶织物浸渍在硫酸亚铁、双氧水、含氟甲基丙烯酸乙酯和丙烯酸的混合乳液中,通过自由基反应实现涤纶表面接枝共聚,整理后织物在室温下水洗15分钟,在100℃烘干;整理工艺处方及条件:硫酸亚铁6g/L,双氧水2.5g/L,含氟甲基丙烯酸乙酯5g/L,丙烯酸2g/L,乳化剂十二烷基硫酸钠1g/L,处理温度40℃,pH 6,处理2小时。
上述步骤(1)~(4)中所述涤纶织物类别为涤纶长丝为原料的针织物。
试样5:经步骤(2)染色处理;未经过步骤(1)、(3)和(4)处理;
试样6:经步骤(1)、(2)处理,未经过步骤(3)和(4)处理;
试样7:经步骤(1)、(2)和(4)处理样,未经过步骤(3)处理;
试样8:经步骤(1)、(2)、(3)和(4)处理;
经上述工艺处理后,分别测定试样5~8的染色深度K/S、湿摩擦牢度、耐熨烫升华牢度和表面润湿接触角;其中试样5的表面深度为K/S为9.21,湿摩擦牢度3级、升华牢度3级、表面接触角5°;其中试样6的表面深度为K/S为10.05,湿摩擦牢度3级、升华牢度3级、表面接触角0°其中试样7的表面深度为K/S为11.01,湿摩擦牢度3.5级、升华牢度3.5级、表面接触角97°其中试样8的表面深度为K/S为12.59,湿摩擦牢度4级、升华牢度4级、表面接触角132°。
结果表明,在实施例1和例2中,试样1、5采用传统高温高压染色后,获得染色深度K/S值较同组内的其他的涤纶染色样品低,摩擦牢度和升华牢度也略低,织物无拒水性;试样2、6经酯酶处理后再进行染色,试样染色深度较未经酯酶处理的试样染色深度增加,色牢度在同一水平,表明酯酶处理能增加纤维表面的粗糙度,产生增深效果;试样3、7经酯酶处理、染色和催化聚合(涤纶表面未接枝乙烯基),试样的染色深度分别较试样2和试样6增加,表明纤维表面有低折射率含氟聚合物沉积,获得一定增深效果,从接触角看织物表现出一定的疏水性;试样4、8经步骤(1)~(4)组合处理后,在同组中涤纶织物的染色深度最高,色牢度也最高,织物接触角也最大,表现出较好的拒水效果,表明在酶法增加纤维表面粗糙度基础上,结合涤纶上接枝乙烯基单体和与含氟丙烯酸酯接枝聚合,促进了纤维表面含氟聚合物分子层形成,使得染物湿摩擦牢度和升华牢度较高。由此可见,采用本发明述及的方法进行处理,不仅能提升涤纶织物的染色深度,且染物具有较高的染色牢度和拒水性,获得较好的染色和整理效果。
虽然本发明已以优选实施例公开如上,但其并非用以限定本发明,任何熟悉此技术的人,在不脱离本发明的精神和范围内,都可做各种的改动与修饰,因此本发明的保护范围应该以权利要求书所界定的为准。
Claims (3)
1.一种通过接枝聚合提升涤纶染色深度和色牢度的方法,其特征在于按以下步骤进行:
首先,借助酯酶进行涤纶织物预处理,使纤维表面刻蚀产生羧基和羟基,再以分散染料进行染色;然后,通过含乙烯基的三乙氧基硅烷醇解与涤纶反应,在涤纶表面引入乙烯基;最后,借助硫酸亚铁和双氧水体系,引发涤纶与含氟丙烯酸酯和丙烯酸单体接枝共聚,在纤维表面形成低折射率聚合物,反应中生成的三价铁离子与聚合物分子中羧基和涤纶上羧基络合,提升涤纶色牢度的方法。
2.根据权利要求1所述的种通过接枝聚合提升涤纶染色深度和色牢度的方法,其特征在于具体工艺步骤如下:
(1)涤纶酯酶预处理:以酯酶进行涤纶织物预处理,处理后以去离子水净洗;
处理工艺处方及条件:酯酶1~2.5U/mL,渗透剂0.2~2g/L,pH范围7.0~9.0,温度30~50℃,处理时间1~2小时;
(2)分散染料染色:经步骤(1)处理的涤纶织物采用分散染料进行高温高压染色,染色后进行还原清洗;
处理工艺处方及条件:分散染料0.2~2.5%o.w.f,pH值的范围4~5.5,温度130℃,处理时间30~45分钟;还原清洗时保险粉2.5~5g/L,纯碱2~4g/L,温度为80℃,处理时间10~20分钟;
(3)涤纶接枝乙烯基:经步骤(2)处理的涤纶织物以含乙烯基的三乙氧基硅烷处理,处理后以去离子水净洗,得到含乙烯基的改性涤纶;
处理工艺处方及条件:含乙烯基的三乙氧基硅烷:水:乙醇=1:1:2~5;处理温度30~40℃,pH范围9~10,处理时间1~2小时;
(4)涤纶织物接枝共聚:经步骤(3)处理的改性涤纶织物浸渍在硫酸亚铁、双氧水、含氟丙烯酸酯和丙烯酸的混合乳液中,通过自由基反应实现涤纶表面接枝共聚,整理后织物在室温下水洗15分钟,在100℃烘干;
整理工艺处方及条件:硫酸亚铁2~6g/L,双氧水1~2.5g/L,含氟丙烯酸酯2.5~5g/L,丙烯酸1~2g/L,乳化剂十二烷基硫酸钠0.5~1g/L,处理温度30~40℃,pH范围4~6,处理时间0.5~2小时。
3.根据权利要求1所述的一种通过接枝聚合提升涤纶染色深度和色牢度的方法,其特征在于:所述酯酶包括来源于动物、植物或微生物且对酯键具有水解功效的酶;所述含氟丙烯酸酯的单体包括含氟丙烯酸乙酯、含氟丙烯酸丁酯和含氟甲基丙烯酸乙酯;所述涤纶织物包括以涤纶纤维为原料的针织物和机织物。
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