CN115450042A - 一种防水阻燃纺织品及其制备方法 - Google Patents
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Abstract
本发明公开了一种防水阻燃纺织品及其制备方法，其涉及纺织技术领域。本发明以棉纤维和涤纶纤维为原料，先在氢氧化钠溶液中预处理，得到预处理纤维；将预处理纤维与甲苯‑2,4‑二异氰酸酯改性，得到改性纤维组分一；将改性纤维组分一与1H,1H,2H,2H‑全氟‑1‑十二醇接枝，得到改性纤维组分二；将改性纤维组分二和二苯基磷酸反应，得到防水阻燃纺织纤维；将防水阻燃纺织纤维纺织，得到防水阻燃纺织品。本发明制备的防水阻燃纺织品具有优良的防水、阻燃性能，以及良好的耐水洗和耐用性能。
Description
技术领域
本发明涉及纺织技术领域，具体涉及一种防水阻燃纺织品及其制备方法。
背景技术
涤棉织物以其外观平整、易洗易干、透气舒适以及强度高等优点，长期占据劳动防护服、消防服以及军队作战服等织物市场的主要份额，然而，由于涤棉织物燃烧时的“支架现象”，涤纶纤维受热熔融后会依附在棉纤维的炭骨架上，同时棉纤维的炭骨架会以熔融的涤纶为燃料，导致更为剧烈的燃烧。涤棉织物的裂解产物相互诱导和阻燃性在不同纤维间的迁移等因素的影响，使其阻燃加工十分困难，涤纶纤维大分子链中极少活性基团，其光滑、整洁的纤维表面，不仅阻燃剂、交联剂无法与纤维大分子形成牢固的化学结合，而且阻燃剂、交联剂向纤维内部扩散、渗透和物理附着也很困难，所以耐水洗性能差、手感粗硬，限制了涤棉纤维在阻燃纺织品领域的应用。
而现有技术中常用的防水剂如有机硅类、硬脂酸衍生物等都是可燃材料，在与阻燃剂共用时，不仅使织物上阻燃剂粘附量减少。而且防水剂过多附着在纤维表面，导致织物的阻燃性下降，织物表面续燃性加大。因此，制备一种兼顾阻燃和防水的织物，是本领域技术人员亟需解决的技术问题。
发明内容
本发明的目的在于提供一种防水阻燃纺织品及其制备方法，解决以下技术问题：
现有的织物表面粘附的防水剂影响阻燃剂的附着，且防水剂的可燃性使织物表面续燃性加大，影响织物的阻燃性能。
本发明的目的可以通过以下技术方案实现：
一种防水阻燃纺织品的制备方法，包括如下步骤：
(1)将织物纤维置于1-1.5mol/L氢氧化钠溶液中，升温至60-80℃浸渍1-2h，水洗、乙醇洗，干燥，得到预处理纤维；
(2)将预处理纤维、无水甲苯加入反应瓶A中,在氮气氛围中,升温至55-65℃,加入甲苯-2,4-二异氰酸酯、二月桂酸二丁基锡组分一,保温反应6-12h，得到改性纤维组分一；
(3)将改性纤维组分一、乙酸乙酯加入反应釜中，在氮气氛围中，加入1H,1H,2H,2H-全氟-1-十二醇、二月桂酸二丁基锡组分二，升温至35-45℃，保温反应1-2h，得到改性纤维组分二；
(4)将二苯基磷酸、改性纤维组分二、叔丁基过氧化氢和碘化四丁基铵加入反应瓶B中，加入二氯甲烷，升温反应，纯化，得到防水阻燃纺织纤维；
(5)将防水阻燃纺织纤维纺织，得到防水阻燃纺织品。
作为本发明进一步的方案：所述织物纤维为棉纤维、涤纶纤维以任意比混合得到。
作为本发明进一步的方案：步骤(2)中预处理纤维：无水甲苯：甲苯-2,4-二异氰酸酯：二月桂酸二丁基锡组分一的添加量为10g：400-800mL：80-120g：1-1.5mL。
作为本发明进一步的方案：步骤(3)中改性纤维组分一：乙酸乙酯：1H,1H,2H,2H-全氟-1-十二醇、二月桂酸二丁基锡组分二的质量比为10：20-40：2-3：0.05-0.1。
作为本发明进一步的方案：步骤(4)中二苯基磷酸：改性纤维组分二：叔丁基过氧化氢：碘化四丁基铵：二氯甲烷的质量比为100-120：50：70-80：10-20：400-600。
作为本发明进一步的方案：步骤(4)中升温至70-90℃，搅拌反应9-12h。
一种防水阻燃纺织品，由上述制备方法制成。
本发明的有益效果：
本申请首先将织物纤维在氢氧化钠溶液中预处理，便于后续改性物质在纤维表面接枝；再将预处理纤维、甲苯-2,4-二异氰酸酯为原料，无水甲苯为溶剂、二月桂酸二丁基锡为催化剂,制备改性纤维组分一；在纤维表面接枝大量异氰酸酯基团。将改性纤维组分一、1H,1H,2H,2H-全氟-1-十二醇为原料，二月桂酸二丁基锡组分二为催化剂，将1H,1H,2H,2H-全氟-1-十二醇接枝在纤维表面，得到改性纤维组分二；将改性纤维组分二、二苯基磷酸为原料，得到防水阻燃纺织纤维；将防水阻燃纺织纤维纺织，得到防水阻燃纺织品。本发明在纤维表面进行一系列的反应，使纤维表面通过化学键接枝含有大量含氟烷烃、含磷有机物，而且附着于纤维表面的含氟烷烃与含磷有机物协同增效，提高涤棉纤维的阻燃效果，且赋予织物表面良好的防水性能。涤棉纤维上接枝的有机链段形成紧密堆积相，增加分子网络的紧密程度，水分子难以渗透，耐水压高，拒水性好。涤棉纤维在改性过程中，有机链段相互交联，还有效提升涤棉纤维的强力，达到保护纤维和提高强力的目的。有效避免现有技术中，在纺织面料表面印染或整理后，面料的强力受到损伤的缺点，对其本身的强力进行提升。本申请制备的纺织品不仅具有有优良的拒水、阻燃性能，而且具有良好的耐水洗以及耐用性能。
具体实施方式
下面将结合本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有作出创造性劳动前提下所获得的所有其它实施例，都属于本发明保护的范围。
实施例1
一种防水阻燃纺织品的制备方法，包括如下步骤：
(1)将涤纶纤维和棉纤维以质量比90:10混合，得到涤棉纤维
(2)将涤棉纤维置于1mol/L氢氧化钠溶液中，升温至60℃浸渍1h，水洗、乙醇洗，干燥，得到预处理纤维；
(3)将10g预处理纤维、400mL无水甲苯加入反应瓶A中,在氮气氛围中,升温至55℃,加入80g甲苯-2,4-二异氰酸酯、1mL二月桂酸二丁基锡组分一,保温反应6h，得到改性纤维组分一；
(4)将10g改性纤维组分一、23mL乙酸乙酯加入反应釜中，在氮气氛围中，加入2g1H,1H,2H,2H-全氟-1-十二醇、0.05g二月桂酸二丁基锡组分二，升温至35℃，保温反应1h，得到改性纤维组分二；
(5)将100g二苯基磷酸、50g改性纤维组分二、700g叔丁基过氧化氢和10g碘化四丁基铵加入反应瓶B中，加入305mL二氯甲烷，升温至70℃，搅拌反应9h，纯化，得到防水阻燃纺织纤维；
(6)将防水阻燃纺织纤维纺织，得到防水阻燃纺织品，纺织品80/20(205g/cm2),平纹组织。
实施例2
一种防水阻燃纺织品的制备方法，包括如下步骤：
(1)将涤纶纤维和棉纤维以质量比90:10混合，得到涤棉纤维
(2)将涤棉纤维置于1mol/L氢氧化钠溶液中，升温至60℃浸渍1h，水洗、乙醇洗，干燥，得到预处理纤维；
(3)将10g预处理纤维、600mL无水甲苯加入反应瓶A中,在氮气氛围中,升温至60℃,加入100g甲苯-2,4-二异氰酸酯、1.2mL二月桂酸二丁基锡组分一,保温反应9h，得到改性纤维组分一；
(4)将10g改性纤维组分一、35mL乙酸乙酯加入反应釜中，在氮气氛围中，加入2.5g1H,1H,2H,2H-全氟-1-十二醇、0.08g二月桂酸二丁基锡组分二，升温至40℃，保温反应1.5h，得到改性纤维组分二；
(5)将110g二苯基磷酸、50g改性纤维组分二、75g叔丁基过氧化氢和15g碘化四丁基铵加入反应瓶B中，加入400mL二氯甲烷，升温至80℃，搅拌反应10h，纯化，得到防水阻燃纺织纤维；
(6)将防水阻燃纺织纤维纺织，得到防水阻燃纺织品，纺织品80/20(205g/cm2),平纹组织。
实施例3
一种防水阻燃纺织品的制备方法，包括如下步骤：
(1)将涤纶纤维和棉纤维以质量比90:10混合，得到涤棉纤维
(2)将涤棉纤维置于1mol/L氢氧化钠溶液中，升温至60℃浸渍1h，水洗、乙醇洗，干燥，得到预处理纤维；
(3)将10g预处理纤维、800mL无水甲苯加入反应瓶A中,在氮气氛围中,升温至65℃,加入120g甲苯-2,4-二异氰酸酯、1.5mL二月桂酸二丁基锡组分一,保温反应12h，得到改性纤维组分一；
(4)将10g改性纤维组分一、44mL乙酸乙酯加入反应釜中，在氮气氛围中，加入3g1H,1H,2H,2H-全氟-1-十二醇、0.1g二月桂酸二丁基锡组分二，升温至45℃，保温反应2h，得到改性纤维组分二；
(5)将120g二苯基磷酸、50g改性纤维组分二、80g叔丁基过氧化氢和20g碘化四丁基铵加入反应瓶B中，加入450mL二氯甲烷，升温至90℃，搅拌反应12h，纯化，得到防水阻燃纺织纤维；
(6)将防水阻燃纺织纤维纺织，得到防水阻燃纺织品，纺织品80/20(205g/cm2),平纹组织。
对比例1
(1)将涤纶纤维和棉纤维以质量比90:10混合，得到涤棉纤维；
(2)将涤棉纤维纺织，得到纺织品，纺织品80/20(205g/cm2),平纹组织。
对比例2
一种防水阻燃纺织品的制备方法，包括如下步骤：
(1)将涤纶纤维和棉纤维以质量比90:10混合，得到涤棉纤维
(2)将涤棉纤维置于1mol/L氢氧化钠溶液中，升温至60℃浸渍1h，水洗、乙醇洗，干燥，得到预处理纤维；
(3)将10g预处理纤维、400mL无水甲苯加入反应瓶A中,在氮气氛围中,升温至55℃,加入80g甲苯-2,4-二异氰酸酯、1mL二月桂酸二丁基锡组分一,保温反应6h，得到改性纤维组分一；
(4)将10g改性纤维组分一、23mL乙酸乙酯加入反应釜中，在氮气氛围中，加入2g1H,1H,2H,2H-全氟-1-十二醇、0.05g二月桂酸二丁基锡组分二，升温至35℃，保温反应1h，得到改性纤维组分二；
(5)将改性纤维组分二纺织，得到防水阻燃纺织品，纺织品80/20(205g/cm2),平纹组织。
对比例3
一种防水阻燃纺织品的制备方法，包括如下步骤：
(1)将涤纶纤维和棉纤维以质量比90:10混合，得到涤棉纤维
(2)将涤棉纤维置于1mol/L氢氧化钠溶液中，升温至60℃浸渍1h，水洗、乙醇洗，干燥，得到预处理纤维；
(3)将10g预处理纤维、400mL无水甲苯加入反应瓶A中,在氮气氛围中,升温至55℃,加入80g甲苯-2,4-二异氰酸酯、1mL二月桂酸二丁基锡组分一,保温反应6h，得到改性纤维组分一；
(4)将10g改性纤维组分一、23mL乙酸乙酯加入反应釜中，在氮气氛围中，加入2g1H,1H,2H,2H-全氟-1-十二醇、0.05g二月桂酸二丁基锡组分二，升温至35℃，保温反应1h，得到改性纤维组分二；
(5)将100g二苯基磷酸、50g改性纤维组分二混合，得到防水阻燃纺织纤维；
(6)将防水阻燃纺织纤维纺织，得到防水阻燃纺织品，纺织品80/20(205g/cm2),平纹组织。
性能检测
(1)氧指数：按照GB/T 5454-1997纺织品氧指数性能试验，检测结果见表1。洗涤实验按照GB8965-88规定方法。
(2)断裂强力：按照GB/T 3923.1-1997断裂强力和断裂伸长的测定(条样法)，检测结果见表1。
(3)撕破强力：按照GB/T 3917.3-1997，梯形试样撕破强力的测定，检测结果见表1。
(4)静水压：按照GB/T 4744-1997纺织织物抗渗水性测试静水压测试；检测结果见表1。
表1：实施例1-3以及对比例1-3性能检测
由表1所示，实施例1-3制备的防水阻燃织物具有优异的拒水、阻燃性能以及良好的耐用性能，且耐水洗，经过多次水洗，依旧保持优良的防水阻燃性能。
以上对本发明的一个实施例进行了详细说明，但所述内容仅为本发明的较佳实施例，不能被认为用于限定本发明的实施范围。凡依本发明申请范围所作的均等变化与改进等，均应仍归属于本发明的专利涵盖范围之内。
Claims (7)
1.一种防水阻燃纺织品的制备方法，其特征在于，包括如下步骤：
(1)将织物纤维置于氢氧化钠溶液中，升温至60-80℃浸渍1-2h，水洗、乙醇洗，干燥，得到预处理纤维；
(2)将预处理纤维、无水甲苯加入反应瓶A中,在氮气氛围中,升温至55-65℃,加入甲苯-2,4-二异氰酸酯、二月桂酸二丁基锡组分一,保温反应6-12h，得到改性纤维组分一；
(3)将改性纤维组分一、乙酸乙酯加入反应釜中，在氮气氛围中，加入1H,1H,2H,2H-全氟-1-十二醇、二月桂酸二丁基锡组分二，升温至35-45℃，保温反应1-2h，得到改性纤维组分二；
(4)将二苯基磷酸、改性纤维组分二、叔丁基过氧化氢和碘化四丁基铵加入反应瓶B中，加入二氯甲烷，升温反应，纯化，得到防水阻燃纺织纤维；
(5)将防水阻燃纺织纤维纺织，得到防水阻燃纺织品。
2.根据权利要求1所述的一种防水阻燃纺织品的制备方法,其特征在于，所述织物纤维为棉纤维、涤纶纤维以任意比混合得到。
3.根据权利要求1所述的一种防水阻燃纺织品的制备方法,其特征在于，步骤(2)中预处理纤维：无水甲苯：甲苯-2,4-二异氰酸酯：二月桂酸二丁基锡组分一的添加量为10g：400-800mL：80-120g：1-1.5mL。
4.根据权利要求1所述的一种防水阻燃纺织品的制备方法,其特征在于，步骤(3)中改性纤维组分一：乙酸乙酯：1H,1H,2H,2H-全氟-1-十二醇、二月桂酸二丁基锡组分二的质量比为10：20-40：2-3：0.05-0.1。
5.根据权利要求1所述的一种防水阻燃纺织品的制备方法,其特征在于，步骤(4)中二苯基磷酸：改性纤维组分二：叔丁基过氧化氢：碘化四丁基铵：二氯甲烷的质量比为100-120：50：70-80：10-20：400-600。
6.根据权利要求1所述的一种防水阻燃纺织品的制备方法,其特征在于，步骤(4)中升温至70-90℃，搅拌反应9-12h。
7.一种防水阻燃纺织品，其特征在于，由权利要求1-6任一项所述制备方法制成。
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