CN114214843B - 一种阻燃涤纶的整理工艺 - Google Patents

一种阻燃涤纶的整理工艺 Download PDF

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CN114214843B
CN114214843B CN202111575964.5A CN202111575964A CN114214843B CN 114214843 B CN114214843 B CN 114214843B CN 202111575964 A CN202111575964 A CN 202111575964A CN 114214843 B CN114214843 B CN 114214843B
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卢森标
范苗星
董雅林
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Shaoxing Zhaofeng Velvet Fabric Co ltd
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Abstract

本申请涉及涤纶织物整理的技术领域,具体公开了一种阻燃涤纶的整理工艺。一种阻燃涤纶的整理工艺,包括以下工艺步骤:S1,将聚酯切片和阻燃剂进行干燥并混合,熔融、挤出;S2,纺丝,冷却成型,得到涤纶丝;S3,将涤纶丝编织形成涤纶面料;S4,对涤纶面料进行拒水拒油整理,得到阻燃拒水拒油涤纶面料;阻燃剂由以下重量份数的原料制成:3‑羟基苯基磷酰丙酸30‑40份;对氨基苯磺酰胺25‑30份;整理液由包含以下重量份数的原料配制而成:含氟拒水剂30‑40份;羟甲基类拒水剂20‑25份;交联剂25‑30份;渗透剂5‑7份;水200‑250份。本申请采用共混以及共聚改性的方式来对聚酯切片进行改性,并进一步通过对涤纶面料进行拒水拒油整理,最终获得阻燃和拒水拒油的性能的涤纶面料。

Description

一种阻燃涤纶的整理工艺
技术领域
本申请涉及涤纶织物整理的技术领域,更具体地说,它涉及一种阻燃涤纶的整理工艺。
背景技术
聚对苯二甲酸乙二醇酯,简称PET,是当今五大工程塑料之一。PET纤维俗称涤纶,是目前第一大合成纤维,然而涤纶的极限氧指数仅为21%,属于易燃材料,因此涤纶纤维的阻燃改性成为了研究热点。
目前,对于涤纶的阻燃改性通常采用后整理法,后整理法通常可分为物理整理和化学整理两类,后整理法是指通过物理或化学的方法对纤维或织物进行整理,以赋予材料一定的阻燃功能,如阻燃涂层整理。后整理法因其工艺简单、成本低、见效快和应用范围广等因素,被广泛应用于涤纶的阻燃改性工艺。
针对上述中的相关技术,发明人认为后整理法虽然能够赋予涤纶织物一定的阻燃性能,但是涤纶织物的阻燃性能会随着水洗次数逐渐减弱,而且为满足客户的需求,一般还会对阻燃后整理过的涤纶织物进行拒水拒油等三防处理,然而阻燃后整理工艺会对涤纶织物的表面产生影响,从而使得涤纶织物后续进行拒水拒油等处理的效果受到影响。
发明内容
为了改善涤纶织物经阻燃改性再进行拒水拒油整理后的阻燃性能和拒水拒油等性能可能会产生相互影响的问题,本申请提供一种阻燃涤纶的整理工艺。
本申请提供的一种阻燃涤纶的整理工艺采用如下的技术方案:
一种阻燃涤纶的整理工艺,包括以下工艺步骤:
S1,将聚酯切片和阻燃剂进行干燥并混合,熔融、挤出;
S2,纺丝,冷却成型,得到阻燃改性后的涤纶丝;
S3,将经过步骤S2的涤纶丝通过经纬编织形成涤纶面料;
S4,配置整理液,对涤纶面料进行拒水拒油整理,得到阻燃拒水拒油涤纶面料;
其中所述阻燃剂由包含以下重量份数的原料制成:3-羟基苯基磷酰丙酸30-40份;对氨基苯磺酰胺25-30份;
所述整理液由包含以下重量份数的原料配制而成:含氟拒水剂30-40份;羟甲基类拒水剂20-25份;交联剂25-30份;渗透剂5-7份;水200-250份。
通过采用上述技术方案,利用3-羟基苯基磷酰丙酸和对氨基苯磺酰胺之间的反应,制备获得含有P、N、S的无卤素阻燃剂,再利用聚酯切片和阻燃剂按照一定比例来进行共混并熔融、挤出,以此来对涤纶进行改性并获得具有阻燃性能的涤纶丝;最后对由阻燃改性后的涤纶丝编织而成的涤纶面料进行拒水拒油整理,含氟拒水剂和羟甲基类拒水剂在渗透剂和交联剂的作用下,交联接枝到涤纶面料上,降低了涤纶面料表面的表面张力,进而获得兼具阻燃和拒水拒油的性能的涤纶面料。
相较于阻燃后整理后再进行拒水拒油整理的方式而言,一方面,涤纶面料的阻燃性能容易受到水洗的影响,随着水洗次数的增加,涤纶面料的阻燃性能通常很会逐渐降低;另一方面,涤纶经阻燃后整理后通常会影响涤纶面料的表面结构,进而可能影响拒水拒油剂与涤纶面料间的结合牢度。通过聚酯切片与阻燃剂共混熔融挤出纺丝的设置,一定程度上增加了阻燃改性后涤纶面料的阻燃性能的耐水洗性,除此之外,较大程度上减小了对涤纶面料表面性能的影响,从而减小了阻燃改性后对涤纶织物拒水拒油性能的影响。
优选的,所述聚酯切片由以下摩尔份的原料制备得到:3-羟基苯基磷酰丙酸5-10份;阻燃剂DDP 10-15份;磷酸三苯酯3-5份;乙二醇50-75份;对苯二甲酸20-30份。
通过采用上述技术方案,利用3-羟基苯基磷酰丙酸和阻燃剂DDP来进行复配并对聚酯切片进行共聚改性,3-羟基苯基磷酰丙酸、阻燃剂DDP和对苯二甲酸均能够与乙二醇进行酯化反应,酯化反应的产物即聚酯单体在催化剂的作用下能够发生缩聚反应,从而获得共聚阻燃改性后的涤纶纤维。
相较于普通聚酯切片与阻燃剂共混熔融挤出纺丝的方式而言,将阻燃剂参与共聚反应并在涤纶纤维分子链上引入阻燃官能团,从而获取共聚阻燃改性后的涤纶纤维,一定程度上减少了阻燃纤维中阻燃剂的添加量,且所获得的阻燃纤维具有更好的阻燃耐久性。
优选的,所述含氟拒水剂由以下重量百分数的原料组成:Asahi Guard AG-71040-60%;Asahi Guard AG-480 40-60%。
优选的,所述羟甲基类拒水剂由以下摩尔份数的原料制成:异佛尔酮二异氰酸酯2-4份;聚酯二元醇2-4份;三羟甲基丙烷2-4份;N-甲基二乙醇胺4-6份;氨基封端二甲基聚硅氧烷3-5份。
通过采用上述技术方案,涤纶织物表面容易分布负电荷,选用上述羟甲基类拒水剂能够与负电荷结合,提高上述羟甲基类拒水剂在织物表面的黏附牢度,同时在焙烘的过程中上述羟甲基类拒水剂能够交联成膜,进一步提高含氟拒水剂和羟甲基类拒水剂的耐洗性能,从而提高了拒水拒油整理后的涤纶面料的拒水拒油性。
优选的,所述交联剂由以下重量百分比的原料组成:三羟甲基三聚氰胺40-60%;胺化环氧交联剂40-60%。
通过采用上述技术方案,选用三羟甲基三聚氰胺和胺化环氧交联剂,能够使得氟系防水剂与纤维间形成三维网状结构,进一步提高拒水拒油整理后涤纶面料的耐洗性,从而提高了涤纶面料拒水拒油性能的耐久性。
优选的,所述聚酯切片由以下工艺步骤制备得到:
Ⅰ、将乙二醇分为两份,第一份乙二醇以摩尔份计为25-40,第二份乙二醇以摩尔份计为25-35,按比例将3-羟基苯基磷酰丙酸、阻燃剂DDP和第一份乙二醇进行混合,通入氮气,加热后进行搅拌和恒温常压反应,得到产物A;
Ⅱ、按比例将对苯二甲酸和第二份乙二醇进行混合,加入催化剂后并通入氮气,加热后进行搅拌和恒温加压反应,得到产物B;
Ⅲ、将产物A加入到产物B中,通入氮气进行恒温常压反应,反应2h后,升温至260℃,抽真空至真空度低于100Pa,进行缩聚反应,得到终产物C,将终产物C进行出料、切粒和干燥工序,制备得到聚酯切片。
通过采用上述技术方案,将3-羟基苯基磷酰丙酸和阻燃剂DDP、对苯二甲酸分开与乙二醇反应,相较于将三者相混后与乙二醇反应的方式而言,申请人发现采用本申请的方式能够提高3-羟基苯基磷酰丙酸、阻燃剂DDP以及对苯二甲酸的收率,并且最终产品聚酯切片的三维空间网状结构和链长都得到提升,通过该聚酯切片来制备获得的涤纶面料的阻燃性能也相对更好些。
优选的,所述聚酯切片和阻燃剂按质量比为(17-18):(2-3)进行干燥并混合。
通过采用上述技术方案,选用上述比例制备获得的涤纶面料的阻燃性能较优且具有较好的可纺性能;进一步增加阻燃剂的比例制备获得的涤纶面料的阻燃性能,虽然一定程度上仍能够得到提升,但是其提升程度有限,且增加阻燃剂的比例后对于涤纶丝的可纺性能会产生影响;进一步降低阻燃剂的比例制备获得的涤纶面料的阻燃性能会随着阻燃剂的比例的下降而下降,因此综合考虑后选用聚酯切片:阻燃剂为(17-18):(2-3)来进行相混。
优选的,所述拒水拒油整理包括以下工艺步骤:
A,按比例将含氟拒水剂、羟甲基类拒水剂、交联剂、渗透剂和水混合,配制得到整理液;B,将经过步骤S3的涤纶面料浸入整理液中进行浸轧,控制轧余率为70-75%,将涤纶面料进行烘干;
C,将经过步骤C的涤纶面料进行焙烘,控制焙烘温度为150℃,得到阻燃拒水拒油涤纶面料。
优选的,所述步骤A具体包括:
将交联剂、渗透剂和水均分为两份,将含氟拒水剂与其中一份交联剂、渗透剂以及水混合并搅拌,得到第一次整理液,将羟甲基类拒水剂与另一份交联剂、渗透剂以及水混合并搅拌,得到第二次整理液;
所述步骤B具体包括:
将经过步骤S3的涤纶面料浸入第一次整理液中进行浸轧,控制轧余率为70-75%,将涤纶面料进行烘干;
将经过第一次整理液浸轧的涤纶面料浸入第二次整理液中进行浸轧,控制轧余率为70-75%,将涤纶面料烘干,得到阻燃拒水拒油涤纶面料。
通过采用上述技术方案,对涤纶面料先进行含氟拒水剂的整理再进行羟甲基类拒水剂的整理,相较于直接将涤纶面料浸入含氟拒水剂和羟甲基类拒水剂的整理液中的方式而言,能够进一步提高涤纶面料的拒水拒油性能,且一定程度上能够提高涤纶面料拒水拒油性能的耐水洗性。
综上所述,本申请具有以下有益效果:
1、本申请利用3-羟基苯基磷酰丙酸和对氨基苯磺酰胺之间的反应,制备获得含有P、N、S的无卤素阻燃剂,再利用聚酯切片和阻燃剂按照一定比例来进行共混并熔融、挤出,以此获得具有阻燃性能的涤纶丝;最后对由阻燃改性后的涤纶丝编织而成的涤纶面料进行拒水拒油整理,含氟拒水剂和羟甲基类拒水剂在渗透剂和交联剂的作用下,交联接枝到涤纶面料上,降低了涤纶面料表面的表面张力,进而获得兼具阻燃和拒水拒油的性能的涤纶面料;
2、本申请中优选采用羟甲基类拒水剂和含氟拒水剂复配的方式,使得整理液中的有效成分能够与织物表面的负电荷结合,提高羟甲基类拒水剂和含氟拒水剂在织物表面的黏附牢度,同时在焙烘的过程中上述羟甲基类拒水剂能够交联成膜,进一步提高含氟拒水剂和羟甲基类拒水剂的耐洗性能,从而提高了拒水拒油整理后的涤纶面料的拒水拒油性。
具体实施方式
以下结合实施例对本申请作进一步详细说明。
阻燃剂的制备例
制备例1
本制备例公开了一种阻燃剂,制备获得一份阻燃剂所需要的原料如下:3-羟基苯基磷酰丙酸345g;对氨基苯磺酰胺275g。
上述阻燃剂由以下工艺步骤制备得到:
按比例向3000ml三口烧瓶中加入345g 3-羟基苯基磷酰丙酸和275g对氨基苯磺酰胺,向三口烧瓶中通入氮气进行保护,对三口烧瓶内的物料进行搅拌,加热至190℃并进行恒温反应,控制反应时间为2h。反应2h后,待三口烧瓶内的温度自然冷却至室温,将反应生成的产物取出并进行粉碎工作,获得阻燃剂。
制备例2
制备例2与制备例1的区别在于:3-羟基苯基磷酰丙酸的添加量为300g,对氨基苯磺酰胺的添加量为250g。
制备例3
制备例3与制备例1的区别在于:3-羟基苯基磷酰丙酸的添加量为400g,对氨基苯磺酰胺的添加量为300g。
聚酯切片的制备例
制备例1
本制备例公开了一种聚酯切片,制备获得一份聚酯切片所需要的原料如下:3-羟基苯基磷酰丙酸107g(0.5mol);阻燃剂DDP 346.2g(1mol);磷酸三苯酯97.8g(0.3mol);乙二醇310g(5mol);对苯二甲酸332g(2mol)。
上述聚酯切片由以下工艺步骤制备得到:
将乙二醇分为两份,其中第一份乙二醇的质量为155g,第二份乙二醇的质量为155g。
按比例将107g 3-羟基苯基磷酰丙酸、346.2g阻燃剂DDP和155g第一份乙二醇加入到1000ml三口烧瓶中,向1000ml三口烧瓶中通入氮气进行保护,对三口烧瓶内的物料进行搅拌,加热至180℃进行常压恒温反应,控制反应时间为5h,反应5h后,待三口烧瓶内的温度冷却至室温后,得到产物A。
按比例将332g对苯二甲酸和155g乙二醇加入到1000ml三口烧瓶中,然后向1000ml三口烧瓶中加入14.6g乙二醇锑和三氧化二锑、97.8g磷酸三苯酯以及10g醋酸钠,充入氮气进行保护,对三口烧瓶内的物料进行搅拌,加热至230℃进行恒温加压反应,控制压强为0.2MPa,控制反应时间为3h,得到产物B;
将产物A加入到产物B中,通入氮气进行保护,进行常压恒温反应,控制反应温度为260℃,控制反应时间为2h,反应2h后,抽真空至真空度低于100Pa,进行缩聚反应,控制缩聚反应为275℃,控制缩聚反应时间为3h,得到终产物C。将终产物C进行出料、切粒和干燥工序,制备得到阻燃改性后的聚酯切片。
制备例2~4
制备例2~4与制备例1的区别如表1所示。
表1
制备例5
制备例5与制备例1的区别在于,上述聚酯切片由以下工艺步骤制备得到:
按比例将107g 3-羟基苯基磷酰丙酸、346.2g阻燃剂DDP、332g对苯二甲酸和310g乙二醇加入到2000ml三口烧瓶中,然后向2000ml三口烧瓶中加入14.6g乙二醇锑和三氧化二锑、97.8g磷酸三苯酯以及10g醋酸钠,向2000ml三口烧瓶中通入氮气进行保护,对三口烧瓶内的物料进行搅拌,加热至230℃进行恒温反应,控制反应时间为5h;升温至260℃进行常压恒温反映,控制反应时间为2h,反应2h后,抽真空至真空度低于100Pa,进行缩聚反应,控制缩聚反应为275℃,控制缩聚反应时间为3h,得到终产物C。将终产物C进行出料、切粒和干燥工序,制备得到阻燃改性后的聚酯切片。
羟甲基类拒水剂的制备例
制备例1
本申请制备例公开了一种羟甲基类拒水剂,制备获得一份羟甲基类拒水剂所需要的原料如下:异佛尔酮二异氰酸酯44.5g(0.2mol);聚酯二元醇200g(0.2mol);三羟甲基丙烷26.8g(0.2mol);N-甲基二乙醇胺47.7(0.4mol)g;氨基封端二甲基聚硅氧烷1500g(0.3mol)。
其中聚酯二元醇选用广州玖盈化工材料有限公司生产的型号为T1136的线性聚酯二元醇,平均分子量为1000;其中氨基封端二甲基聚硅氧烷选自北京灵宝科技有限公司,平均分子量为5000。
上述羟甲基类拒水剂由以下工艺步骤制备得到:
按比例将200g聚酯二元醇、26.8g三羟甲基丙烷加入到3000ml三口烧瓶中,再加入6.8g二月桂酸二丁基锡,向3000ml三口烧瓶中通入氮气进行保护,对三口烧瓶进行加热,加热至55℃后向三口烧瓶内滴加44.5g异佛尔酮二异氰酸酯,滴加完异佛尔酮二异氰酸酯后升温至75℃,进行恒温反应,恒温反应2h后,降温至60℃,然后向3000ml三口烧瓶内加入47.7g N-甲基二乙醇胺,进行恒温反应,恒温反应2h后加入17.4g封端剂甲基乙基酮肟,保温反应1h后降温至30℃,加入1500g氨基封端二甲基聚硅氧烷,搅拌并保温反应3h,得到羟甲基类拒水剂。
制备例2
制备例2与制备例1的区别计为表2,其中三口烧瓶的规格可根据物料总量进行选择。
表2
实施例
实施例1
本申请实施例公开了一种阻燃涤纶的整理工艺,包括以下工艺步骤:
S1,将8500g聚酯切片和1500g阻燃剂进行干燥并混合,熔融后通过挤出机进行挤出;
其中聚酯切片选用江苏微谷国际贸易有限公司;阻燃剂选用阻燃剂的制备例1;
S2,纺丝,冷却成型后,得到阻燃改性后的涤纶丝;
S3,将经过步骤S2的涤纶丝通过经纬编织形成涤纶面料;
S4,配置整理液,对涤纶面料进行拒水拒油整理,得到阻燃拒水拒油涤纶面料;
其中整理液由以下原料配制而成:300g含氟拒水剂;200g羟甲基类拒水剂;250g交联剂;50g渗透剂;2000g水;
含氟拒水剂选用常规市售的Asahiguard AG-710,羟甲基类拒水剂选用常规市售的防水剂703,交联剂选用广东德美化工有限公司的交联剂DM-3523,渗透剂选用常规市售的JFC渗透剂。
其中S4具体包括如下工艺步骤:
A,按比例将300g含氟拒水剂、200g羟甲基类拒水剂、250g交联剂、50g渗透剂以及2000g水进行混合并充分搅拌,配制得到整理液;
B,将涤纶面料进入整理液中进行二浸二轧工作,控制轧余率为70-75%,然后将涤纶面料进行烘干;
C,烘干后将涤纶面料置于150℃下进行焙烘热处理,控制焙烘热处理时间为3min,最后再对涤纶面料进行水洗烘干,得到阻燃拒水拒油涤纶面料。
实施例2
实施例2与实施例1的区别在于,聚酯切片的添加量为9000g,阻燃剂的添加量为1000g。
实施例3
实施例3与实施例1的区别在于,整理液由以下原料配制而成:400g含氟拒水剂;250g羟甲基类拒水剂;300g交联剂;70g渗透剂;2500g水。
实施例4
实施例4与实施例1的区别在于,聚酯切片选用聚酯切片的制备例1。
实施例5~8
实施例5~8与实施例4的区别记为表3。
表3
聚酯切片
实施例4 聚酯切片的制备例1
实施例5 聚酯切片的制备例2
实施例6 聚酯切片的制备例3
实施例7 聚酯切片的制备例4
实施例8 聚酯切片的制备例5
实施例9
实施例9与实施例4的区别在于,交联剂由以下原料组成:125g三羟甲基三聚氰胺;125g胺化环氧交联剂;
其中胺化环氧交联剂选自杭州永明树脂化学有限公司生产的YS-501-E胺化环氧树脂。
实施例10
实施例10与实施例9的区别在于,阻燃剂选用阻燃剂的制备例2。
实施例11
实施例11与实施例9的区别在于,阻燃剂选用阻燃剂的制备例3。
实施例12
实施例12与实施例9的区别在于,含氟拒水剂由以下原料组成:150g AsahiGuard-710;150g Asahi Guard-480。
实施例13
实施例13与实施例12的区别在于,羟甲基类拒水剂选用羟甲基类拒水剂的制备例1。
实施例14
实施例14与实施例12的区别在于,羟甲基类拒水剂选用羟甲基类拒水剂的制备例2。
实施例15
实施例15与实施例13的区别在于,步骤A具体包括:
将250g交联剂、50g渗透剂和2000g水均分为两份,将300g含氟拒水剂与一份交联剂、渗透剂以及水混合并搅拌,搅拌均匀后,得到第一次整理液;将200g羟甲基类拒水剂与另一份交联剂、渗透剂以及水混合并搅拌,得到的第二次整理液;
步骤B具体包括:
将经过步骤S3的涤纶面料浸入第一次整理液中进行二浸二轧工作,控制轧余率为70-75%,然后将涤纶面料进行烘干;
将经过的第一次整理液浸轧的涤纶面料浸入第二次整理液中进行二浸二轧工作,控制轧余率为70-75%,将涤纶面料烘干。
对比例
对比例1
对比例1与实施例1的区别在于:阻燃剂为红磷和氧化镁的混合物,红磷与氧化镁的质量比为8:1。
对比例2
对比例2与实施例1的区别在于,整理液由以下原料组成:84g甲基含氢硅烷乳液;196g羟基硅烷乳液;40g胺化环氧交联剂;30.2g结晶醋酸锌;15.1g氯氧化锆;12.6g一乙醇胺;1622.1g水。
性能检测试验
1.1阻燃性能测试
1.1.1燃烧测试法
根据GB/T 5455-2014《纺织品燃烧性能垂直方向损毁长度、阴燃和续燃时间的测定》来测试各实施例和对比例中涤纶的燃烧性能。
1.1.2极限氧指数
根据GB/T 5454-1997《纺织品燃烧性能试验氧指数法》来测试各实施例和对比例中涤纶的LOI值。
1.2拒水拒油性能测试
1.2.1拒水性能
根据GB/T 4745-2012《纺织品防水性能的检测和评价沾水法》来测试各实施例和对比例中涤纶的拒水性能。
1.2.2拒油性能
从各实施例和对比例中的涤纶织物上不同部位至少取三块试样,每块试样尺寸至少为180mm×180mm,试样应具有代表性,取样部位不应有折皱或折痕。
将调湿处理的试样置于光滑平台上,用滴管依次取各分值标准试剂,由低到高,小心地滴在试样上,每滴直径4~5mm,停留3min。从45°角斜上方观察,若试剂液滴底部织物反光发亮,则没有浸润,通过该分值测试;若发暗,则织物浸润,通不过该分值测试。以通过最大分值为准,评定拒油性能。
织物拒油性能测试采用评分法。各分值标准试剂是用白矿物油和正庚烷按不同比例配制的,其配比见表4。
表4标准试剂配比
燃烧测试结果如表5所示。
表5
极限氧指数测试结果如表6所示。
表6
拒水拒油性能测试结果如表7所示。
表7
结合实施例1~3和对比例1~2并结合表5~7可以看出,采用阻燃剂与聚酯切片共混的改性方式能够使得制备获得的涤纶面料具有良好的阻燃性能;选用本申请中的阻燃剂来对聚酯切片来进行共混改性,能够进一步提升改性后制备获得的涤纶面料的阻燃性能。
结合实施例1、4~8并结合表5~7可以看出,选用本申请中共聚改性后的聚酯切片与阻燃剂共混的改性方式,能够显著提高制备获得的涤纶面料的阻燃性能,同时也一定程度上提高了涤纶面料阻燃性能的耐水洗性。
另一方面,将3-羟基苯基磷酰丙酸和阻燃剂DDP、对苯二甲酸分开与乙二醇反应,相较于将三者相混后与乙二醇反应的方式而言,共聚改性后获得的涤纶面料的阻燃性能也能够得到一定程度上的提升。
结合实施例1、9~11和对比例1~2并结合表5~7可以看出,选用本申请中的三羟甲基三聚氰胺和胺化环氧交联剂,能够提高涤纶面料的拒水拒油性能的耐水洗能力,能够使得氟系防水剂与纤维间形成三维网状结构,进一步提高拒水拒油整理后涤纶面料的耐洗性,从而提高了涤纶面料拒水拒油性能的耐久性。
结合实施例1、9~15和对比例1~2并结合表5~7可以看出,选用本申请中的整理液和整理步骤,能够进一步提高涤纶面料的拒水拒油性能和耐水洗性,分析原因可能在于采用羟甲基类拒水剂和含氟拒水剂复配的方式,使得整理液中的有效成分能够与织物表面的负电荷结合,提高羟甲基类拒水剂和含氟拒水剂在织物表面的黏附牢度,同时在焙烘的过程中上述羟甲基类拒水剂能够交联成膜,进一步提高含氟拒水剂和羟甲基类拒水剂的耐洗性能,从而提高了拒水拒油整理后的涤纶面料的拒水拒油性。
本具体实施例仅仅是对本申请的解释,其并不是对本申请的限制,本领域技术人员在阅读完本说明书后可以根据需要对本实施例做出没有创造性贡献的修改,但只要在本申请的权利要求范围内都受到专利法的保护。

Claims (6)

1.一种阻燃涤纶的整理工艺,其特征在于,包括以下工艺步骤:
S1,将聚酯切片和阻燃剂进行干燥并混合,熔融、挤出;
S2,纺丝,冷却成型,得到阻燃改性后的涤纶丝;
S3,将经过步骤S2的涤纶丝通过经纬编织形成涤纶面料;
S4,配置整理液,对涤纶面料进行拒水拒油整理,得到阻燃拒水拒油涤纶面料;
其中所述阻燃剂由包含以下重量份数的原料制成:3-羟基苯基磷酰丙酸30-40份;对氨基苯磺酰胺25-30份;
所述整理液由包含以下重量份数的原料配制而成:含氟拒水剂30-40份;羟甲基类拒水剂20-25份;交联剂25-30份;渗透剂5-7份;水200-250份;
所述含氟拒水剂由以下重量百分数的原料组成:AsahiGuardAG-71040-60%;AsahiGuardAG-48040-60%;
所述羟甲基类拒水剂由以下摩尔份数的原料制成:异佛尔酮二异氰酸酯2-4份;聚酯二元醇2-4份;三羟甲基丙烷2-4份;N-甲基二乙醇胺4-6份;氨基封端二甲基聚硅氧烷3-5份;
所述交联剂由以下重量百分比的原料组成:三羟甲基三聚氰胺40-60%;胺化环氧交联剂40-60%。
2.根据权利要求1所述的一种阻燃涤纶的整理工艺,其特征在于,所述聚酯切片由以下摩尔份的原料制备得到:3-羟基苯基磷酰丙酸5-10份;阻燃剂DDP10-15份;磷酸三苯酯3-5份;乙二醇50-75份;对苯二甲酸20-30份。
3.根据权利要求1所述的一种阻燃涤纶的整理工艺,其特征在于,所述聚酯切片由以下工艺步骤制备得到:
Ⅰ、将乙二醇分为两份,第一份乙二醇以摩尔份计为25-40,第二份乙二醇以摩尔份计为25-35,按比例将3-羟基苯基磷酰丙酸、阻燃剂DDP和第一份乙二醇进行混合,通入氮气,加热后进行搅拌和恒温常压反应,得到产物A;
Ⅱ、按比例将对苯二甲酸和第二份乙二醇进行混合,加入催化剂后并通入氮气,加热后进行搅拌和恒温加压反应,得到产物B;
Ⅲ、将产物A加入到产物B中,通入氮气进行恒温常压反应,反应2h后,升温至260℃,抽真空至真空度低于100Pa,进行缩聚反应,得到终产物C,将终产物C进行出料、切粒和干燥工序,制备得到聚酯切片。
4.根据权利要求1所述的一种阻燃涤纶的整理工艺,其特征在于:所述聚酯切片和阻燃剂按质量比为(17-18):(2-3)进行干燥并混合。
5.根据权利要求1所述的一种阻燃涤纶的整理工艺,其特征在于,所述拒水拒油整理包括以下工艺步骤:
A,按比例将含氟拒水剂、羟甲基类拒水剂、交联剂、渗透剂和水混合,配制得到整理液;B,将经过步骤S3的涤纶面料浸入整理液中进行浸轧,控制轧余率为70-75%,将涤纶面料进行烘干;
C,将经过步骤C的涤纶面料进行焙烘,控制焙烘温度为150℃,得到阻燃拒水拒油涤纶面料。
6.根据权利要求5所述的一种阻燃涤纶的整理工艺,其特征在于,所述步骤A具体包括:将交联剂、渗透剂和水均分为两份,将含氟拒水剂与其中一份交联剂、渗透剂以及水混合并搅拌,得到第一次整理液,将羟甲基类拒水剂与另一份交联剂、渗透剂以及水混合并搅拌,得到第二次整理液;
所述步骤B具体包括:
将经过步骤S3的涤纶面料浸入第一次整理液中进行浸轧,控制轧余率为70-75%,将涤纶面料进行烘干;将经过第一次整理液浸轧的涤纶面料浸入第二次整理液中进行浸轧,控制轧余率为70-75%,将涤纶面料烘干,得到阻燃拒水拒油涤纶面料。
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