CN111691197B - 一种耐水洗阻燃无纺布及其制备方法 - Google Patents

一种耐水洗阻燃无纺布及其制备方法 Download PDF

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CN111691197B
CN111691197B CN202010590286.9A CN202010590286A CN111691197B CN 111691197 B CN111691197 B CN 111691197B CN 202010590286 A CN202010590286 A CN 202010590286A CN 111691197 B CN111691197 B CN 111691197B
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woven fabric
flame
retardant
solution
needling
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CN111691197A (zh
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刘家浩
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Changzhou Jiasheng New Material Technology Co ltd
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Changzhou Jiasheng Non Woven Fabric Co ltd
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Priority to CN202110328277.7A priority patent/CN112918042A/zh
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    • B32B5/02—Layered products characterised by the non- homogeneity or physical structure, i.e. comprising a fibrous, filamentary, particulate or foam layer; Layered products characterised by having a layer differing constitutionally or physically in different parts characterised by structural features of a fibrous or filamentary layer
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Abstract

本发明公开了一种耐水洗阻燃无纺布及其制备方法，所述一种耐水洗阻燃无纺布由内到外依次包括，无纺布基层、耐水洗层、阻燃层；无纺布基层由改性粘胶纤维、丙纶纤维、涤纶纤维制得。其中改性粘胶纤维的制备方法中，由AlCl3改性的环糊精与氮‑磷系阻燃剂三聚氰胺磷酸酯协同形成高效阻燃剂，将高效阻燃剂与粘胶纤维原液共混，制得阻燃性的改性粘胶纤维；用其针刺加工成具有阻燃性的无纺布。将无纺布基层放入环氧丙烯酸酯、丙烯酸丁酯、β‑环糊精、甲基丙烯酸缩水甘油酯混合溶液中浸泡，经过系列反应形成耐水洗层，最外层再涂覆致密阻燃层，使无纺布拥有水洗不易变形，阻燃效果佳的特性。本发明设计合理，具有较高的实用性。

Description

一种耐水洗阻燃无纺布及其制备方法
技术领域
本发明涉及纺织领域，具体为一种耐水洗阻燃无纺布及其制备方法。
背景技术
无纺布由化学纤维如：丙纶、涤纶、锦纶、粘胶纤维、腈纶、乙纶、氯纶和天然植物纤维如：棉、丝、麻；进行定向或随机排列，形成纤网结构，然后采用机械、热粘或化学等方法加固而成，虽为布而不经纺织故称其为无纺布。无纺布以其良好的防潮、透气、柔韧、质轻、不助燃、容易分解、无毒无刺激性、色彩丰富、可循环再用及低廉的生产成本等优势迅速受到广大生产厂商和广大消费者的喜爱。广泛应用于医疗卫生、家庭装饰、服装、工业、母婴用品、农业、航天科技、包装材料、鞋包、汽车工业等领域。随着科技的发展，对于耐久性、隔热阻燃无纺布的需求越来越大，目前市场上存在的阻燃无纺布存在阻燃效果不理想，且耐久性较差。故研究一种耐久性、水洗不变形、阻燃性高的无纺布，是未来的发展趋势。
发明内容
本发明的目的在于提供一种耐水洗阻燃无纺布及其制备方法，具备阻燃性高，多次水洗不变形等优点，以解决现有技术中的问题。
为实现上述目的，本发明提供如下技术方案：
一种耐水洗阻燃无纺布，所述耐水洗阻燃无纺布包括，由内到外依次为无纺布基层、耐水洗层、阻燃层。其中无纺布基层包括，按重量份数计，改性粘胶纤维45-70份，涤纶纤维15-25份，丙纶纤维15-25份。
所述的耐水洗层依次经混合溶液A、包合物B浸泡形成，阻燃层由混合液C涂覆形成；混合溶液A和包合物B的质量比为1：2；
所述混合溶液A包括：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯，其质量比为5:1:1:0.1；所述包合物B由β-环糊精与甲基丙烯酸缩水甘油酯反应制得，其质量比为1:2；所述混合液C包括：三氧化二锑、氢氧化镁、氢氧化铝、UV胶，其质量比为3:1:1：0.1。
改性粘胶纤维包括：按重量份计，粘胶纤维70-90份、阻燃剂溶液15-25份；阻燃剂溶液为质量比为1：2的β-环糊精和三聚氰胺磷酸酯混配溶液。
一种耐水洗阻燃无纺布的制备方法，包括以下4个步骤；
(1)制备阻燃剂溶液，步骤如下：
取β-环糊精，加入蒸馏水制成饱和溶液，加入AlCl3混合，温度为60-70℃条件下，搅拌30-40min,静置，抽滤，乙醇溶液水洗，烘干，制得包合物A(包覆Al3+的β-环糊精)；三聚氰胺磷酸酯溶液与包合物A混合，超声分散10-20min,制得阻燃剂溶液；
三聚氰胺磷酸酯溶液是一种氮-磷系协同阻燃剂，是目前纺织工艺中常用的高效阻燃剂，具有烟气毒性低、不含卤族元素、持久性好、阻燃效果良好的特点；但三聚氰胺磷酸酯溶液与无纺布界面的相容性不够理想，易吸潮导致电性能较差；阻燃性能未能充分发挥，阻燃效果不理想，易产生熔融物滴落的现象。本技术方案中利用β-环糊精将AlCl3引入到系统中，β-环糊精分子内腔空间大且疏水，避免了吸潮现象，β-环糊精具有增溶性，与无纺布基层相容性良好。AlCl3中Al3+与三聚氰胺磷酸酯上P＝O键协同作用；使三聚氰胺磷酸酯热稳定性增强，燃烧时催化粘胶纤维裂解产生更多的焦炭，在无纺布基层形成碳化覆盖层，阻止外部氧气进入和热量的散出，同时抑制可燃气体的产生；提高了无纺布的阻燃性。
(2)制备改性粘胶纤维，步骤如下：
向阻燃剂溶液中加入粘胶纤维纺丝原液；磁力搅拌30min，搅拌速度为180-220r/min，得到共混液；共混液在温度为27-32℃条件下，真空脱泡40-45min，得到改性粘胶纺丝液；
将改性粘胶纺丝液与凝固浴中的凝固剂接触，经纺丝孔输出形成初生纤维；对初生纤维牵伸；中和、水洗；得到改性粘胶纤维。
(3)制备无纺布基层，步骤如下：
S1.将改性粘胶纤维、涤纶纤维、丙纶纤维开松，混条；
S2.梳理除杂，堆叠铺成纤维网，纤维网层数为8-10层；
S3.将纤维网自上而下针刺巩固；依次经一道预针刺、三道主针刺、高温热轧、卷绕；其中预针刺的针频为600刺/min，针深为12mm；第一主针刺的针频为750刺/min，针深为10mm；第二主针刺的针频为750刺/min，针深为8mm；第三主针刺的针频为750刺/min，针深为5mm；高温热轧，热轧温度为220-225℃；进入卷曲机卷绕；制得针刺无纺布；
S4.将针刺无纺布以7-9m/min匀速通过上述制备的阻燃剂溶液，使针刺无纺布在阻燃剂溶液中充分浸润；经阻燃剂溶液浸润后的针刺无纺布，以7-9m/min的速度，依次通过双辊压轧、轧干力度3-6kg；拉幅；温度为145-150℃条件下烘干，并将表面烫平压光得无纺布基层。
丙纶纤维、涤纶纤维属于本质阻燃型纤维；改性粘胶纤维经阻燃剂溶液处理后具有阻燃性能；将三种纤维共混，针刺制成的无纺布再经阻燃剂溶液浸泡处理，使得无纺布具有良好的阻燃效果。
(4)制备耐水洗层、阻燃层，步骤如下：
S1.耐水洗层：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯、以质量比5:1:0.1加入去离子水中，搅拌10-15min，制得混合液A；
将β-环糊精与甲基丙烯酸缩水甘油酯以质量比1：2的比例加入到二甲基乙酰胺溶剂中，加入对苯二酚，在温度为57-62℃条件下，反应6h；自然冷却；向其中加入丙酮溶液，反应产生白色成定；过滤白色沉淀，丙酮溶液洗涤；真空干燥，制得包合物B；
将无纺布基层放入混合液A中，浸泡40-60min；加入包合物B，包合物B与混合溶液A混合；在温度为37-40℃、在光引发的条件下，光引发剂选用自由基光引发剂1173(2-羟基-2-甲基-1-苯基丙酮)，浸泡6-8h；真空烘干，形成耐水洗层；
因环氧丙烯酸酯是一种优良的环氧树脂，具有优异的耐水性、耐热水性、耐药物性、粘结性、韧性，用其浸泡无纺布基层，可形成耐水性强的保护薄膜；但环氧丙烯酸酯极其粘稠，常温下无流动性，固加入丙烯酸丁酯作为活性稀释剂，稀释降低环氧丙烯酸酯的粘度，减小其薄膜的交联密度，进而降低环氧丙烯酸酯凝胶程度；使无纺布基层形成较优的环氧丙烯酸酯薄膜。将甲基丙烯酸缩水甘油酯引入到β-环糊精分子内，形成包合有乙烯基基团的β-环糊精超分子；β-环糊精超分子通过光引发剂，接枝到环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯的交联体系中，乙烯基与环氧丙烯酸酯共聚，增加薄膜的断裂伸长率，提高薄膜韧性；利于提高环氧丙烯酸酯薄膜的自我修复功能，在表层受到外力刮擦时，薄膜可完成自我修复，不产生裂纹。故环氧丙烯酸酯、丙烯酸丁酯、β-环糊精、甲基丙烯酸缩水甘油酯共同作用，可形成耐水洗层，同时耐水洗层还具良好的自我修复功能。
S2.三氧化二锑、氢氧化镁、氢氧化铝、UV胶混合熔融，制得混合液C；在S1中制备的无纺布基层正、反面涂覆涂混合液C，涂层厚度为15-30μm，静置，烘干，形成阻燃层。
三氧化二锑、氢氧化镁、氢氧化铝属于无机阻燃剂，在燃烧初期熔融，在无纺布基层表面形成致密保护膜来隔绝空气；分子内部吸热，可降低燃烧温度，起到阻燃作用；在高温时分子气化，降低空气中氧浓度，从而起到阻燃作用。
与现有技术相比，本发明的有益效果是：
利用三聚氰胺磷酸酯、β-环糊精、AlCl3复配阻燃剂，阻燃性对粘胶纤维进行改性处理，再对无纺布基层进行浸泡，得到阻燃无纺布。阻燃无纺布浸泡在环氧丙烯酸酯、丙烯酸丁酯、β-环糊精、甲基丙烯酸缩水甘油酯混合溶液中，经过系列反应，在无纺布基层形成了耐水洗且具有自我修复功能的耐水洗层。最后在无纺布最外层，涂覆三氧化二锑、氢氧化镁、氢氧化铝、UV胶混合熔融液，形成致密阻燃层。综上所述，本技术方案提供的耐水洗阻燃无纺布，具有良好的阻燃性和耐水洗性能。
具体实施方式：
下面将对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做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
实施例1
一种耐水洗阻燃无纺布，包括，由内到外依次为无纺布基层、耐水洗层、阻燃层。无纺布基层包括，按重量份数计，改性粘胶纤维45份，涤纶纤维15份，丙纶纤维15份。
耐水洗层为混合溶液A和包合物B浸泡形成，阻燃层由混合液C涂覆形成；混合溶液A和包合物B的质量比为1：2；混合溶液A包括：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯，其质量比为5:1:0.1；所述包合物B由β-环糊精与甲基丙烯酸缩水甘油酯反应制得，其质量比为1:2；
混合液C包括：三氧化二锑、氢氧化镁、氢氧化铝、UV胶，其质量比为3:1:1：0.1。
其中改性粘胶纤维包括：按重量份计，粘胶纤维70-90份、阻燃剂溶液15份。
阻燃剂溶液由质量比为1：2的β-环糊精和三聚氰胺磷酸酯混配制得。
一种耐水洗阻燃无纺布的制备方法，包括以下步骤；
(1)制备阻燃剂溶液，步骤如下：
取β-环糊精，加入蒸馏水制成饱和溶液，加入AlCl3混合，温度为60℃条件下，搅拌30min,静置，抽滤，乙醇溶液水洗，烘干，制得包合物A；三聚氰胺磷酸酯溶液与包合物A混合；超声分散10min,制得阻燃剂溶液。
(2)制备改性粘胶纤维，步骤如下：
向阻燃剂溶液中加入粘胶纤维纺丝原液；磁力搅拌30min，搅拌速度为180r/min，得到共混液；共混液在温度为27℃条件下，真空脱泡40min，得到改性粘胶纺丝液；
将改性粘胶纺丝液与凝固浴中的凝固剂接触，经纺丝孔输出形成初生纤维；对初生纤维牵伸；中和、水洗；得到改性粘胶纤维。
(3)制备无纺布基层，步骤如下：
S1.将改性粘胶纤维、涤纶纤维、丙纶纤维开松，混条；
S2.梳理除杂，堆叠铺成纤维网，纤维网层数为8层；
S3.将纤维网自上而下针刺巩固；依次经一道预针刺、三道主针刺、高温热轧、卷绕；其中预针刺的针频为600刺/min，针深为12mm；第一主针刺的针频为750刺/min，针深为10mm；第二主针刺的针频为750刺/min，针深为8mm；第三主针刺的针频为750刺/min，针深为5mm；高温热轧，热轧温度为220℃；进入卷曲机卷绕；制得针刺无纺布；
S4.将针刺无纺布以7m/min匀速通过步骤(1)制备的阻燃剂溶液，使针刺无纺布在阻燃剂溶液中充分浸润；经阻燃剂溶液浸润后的针刺无纺布，以7m/min的速度，依次通过双辊压轧、轧干力度3kg；拉幅；温度为145℃条件下烘干，并将表面烫平压光得无纺布基层。
(4)制备耐水洗层、阻燃层，步骤如下：
S1.耐水洗层：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯加入去离子水中，搅拌105min，制得混合液A；
将β-环糊精与甲基丙烯酸缩水甘油酯加入到二甲基乙酰胺溶剂中，加入对苯二酚，在温度为57℃条件下，反应6h；自然冷却；向其中加入丙酮溶液，反应产生白色沉淀；过滤白色沉淀，丙酮溶液洗涤；真空干燥，制得包合物B；
将无纺布基层放入混合液A中，浸泡40min；加入包合物B，在温度为37℃、在光引发条件下，浸泡6h；真空烘干，形成耐水洗层；
S2.三氧化二锑、氢氧化镁、氢氧化铝、UV胶混合熔融，制得混合液C；在S1中制备的无纺布基层正、反面涂覆涂混合液C，涂层厚度为15μm，静置，烘干，形成阻燃层。
实施例2
一种耐水洗阻燃无纺布，包括，由内到外依次为无纺布基层、耐水洗层、阻燃层。无纺布基层包括，按重量份数计，改性粘胶纤维69份，涤纶纤维23份，丙纶纤维18份。
耐水洗层为混合溶液A和包合物B浸泡形成，阻燃层由混合液C涂覆形成；混合溶液A和包合物B的质量比为1：2；混合溶液A包括：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯，其质量比为5:1:0.1；所述包合物B由β-环糊精与甲基丙烯酸缩水甘油酯反应制得，其质量比为1:2；
混合液C包括：三氧化二锑、氢氧化镁、氢氧化铝、UV胶，其质量比为3:1:1：0.1。
其中改性粘胶纤维包括：按重量份计，粘胶纤维82份、阻燃剂溶液23份。
阻燃剂溶液由质量比为1：2的β-环糊精和三聚氰胺磷酸酯混配制得。
一种耐水洗阻燃无纺布的制备方法，包括以下步骤；
(1)制备阻燃剂溶液，步骤如下：
取β-环糊精，加入蒸馏水制成饱和溶液，加入AlCl3混合，温度为65℃条件下，搅拌31min,静置，抽滤，乙醇溶液水洗，烘干，制得包合物A；三聚氰胺磷酸酯溶液与包合物A混合；超声分散16min,制得阻燃剂溶液。
(2)制备改性粘胶纤维，步骤如下：
向阻燃剂溶液中加入粘胶纤维纺丝原液；磁力搅拌30min，搅拌速度为185r/min，得到共混液；共混液在温度为32℃条件下，真空脱泡44min，得到改性粘胶纺丝液；
将改性粘胶纺丝液与凝固浴中的凝固剂接触，经纺丝孔输出形成初生纤维；对初生纤维牵伸；中和、水洗；得到改性粘胶纤维。
(3)制备无纺布基层，步骤如下：
S1.将改性粘胶纤维、涤纶纤维、丙纶纤维开松，混条；
S2.梳理除杂，堆叠铺成纤维网，纤维网层数为9层；
S3.将纤维网自上而下针刺巩固；依次经一道预针刺、三道主针刺、高温热轧、卷绕；其中预针刺的针频为600刺/min，针深为12mm；第一主针刺的针频为750刺/min，针深为10mm；第二主针刺的针频为750刺/min，针深为8mm；第三主针刺的针频为750刺/min，针深为5mm；高温热轧，热轧温度为221℃；进入卷曲机卷绕；制得针刺无纺布；
S4.将针刺无纺布以8m/min匀速通过步骤(1)制备的阻燃剂溶液，使针刺无纺布在阻燃剂溶液中充分浸润；经阻燃剂溶液浸润后的针刺无纺布，以8m/min的速度，依次通过双辊压轧、轧干力度4kg；拉幅；温度为147℃条件下烘干，并将表面烫平压光得无纺布基层。
(4)制备耐水洗层、阻燃层，步骤如下：
S1.耐水洗层：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯加入去离子水中，搅拌13min，制得混合液A；
将β-环糊精与甲基丙烯酸缩水甘油酯加入到二甲基乙酰胺溶剂中，加入对苯二酚，在温度为60℃条件下，反应6h；自然冷却；向其中加入丙酮溶液，反应产生白色沉淀；过滤白色沉淀，丙酮溶液洗涤；真空干燥，制得包合物B；
将无纺布基层放入混合液A中，浸泡52min；加入包合物B，在温度为39℃、在光引发条件下，浸泡7h；真空烘干，形成耐水洗层；
S2.三氧化二锑、氢氧化镁、氢氧化铝、UV胶混合熔融，制得混合液C；在S1中制备的无纺布基层正、反面涂覆涂混合液C，涂层厚度为23μm，静置，烘干，形成阻燃层。
实施例3
一种耐水洗阻燃无纺布，包括，由内到外依次为无纺布基层、耐水洗层、阻燃层。无纺布基层包括，按重量份数计，改性粘胶纤维70份，涤纶纤维25份，丙纶纤维25份。
耐水洗层为混合溶液A和包合物B浸泡形成，阻燃层由混合液C涂覆形成；混合溶液A和包合物B的质量比为1：2；混合溶液A包括：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯，其质量比为5:1:0.1；所述包合物B由β-环糊精与甲基丙烯酸缩水甘油酯反应制得，其质量比为1:2；
混合液C包括：三氧化二锑、氢氧化镁、氢氧化铝、UV胶，其质量比为3:1:1：0.1。
其中改性粘胶纤维包括：按重量份计，粘胶纤维90份、阻燃剂溶液25份。
阻燃剂溶液由质量比为1：2的β-环糊精和三聚氰胺磷酸酯混配制得。
一种耐水洗阻燃无纺布的制备方法，包括以下步骤；
(1)制备阻燃剂溶液，步骤如下：
取β-环糊精，加入蒸馏水制成饱和溶液，加入AlCl3混合，温度为70℃条件下，搅拌40min,静置，抽滤，乙醇溶液水洗，烘干，制得包合物A；三聚氰胺磷酸酯溶液与包合物A混合；超声分散10-20min,制得阻燃剂溶液。
(2)制备改性粘胶纤维，步骤如下：
向阻燃剂溶液中加入粘胶纤维纺丝原液；磁力搅拌30min，搅拌速度为220r/min，得到共混液；共混液在温度为32℃条件下，真空脱泡45min，得到改性粘胶纺丝液；
将改性粘胶纺丝液与凝固浴中的凝固剂接触，经纺丝孔输出形成初生纤维；对初生纤维牵伸；中和、水洗；得到改性粘胶纤维。
(3)制备无纺布基层，步骤如下：
S1.将改性粘胶纤维、涤纶纤维、丙纶纤维开松，混条；
S2.梳理除杂，堆叠铺成纤维网，纤维网层数为10层；
S3.将纤维网自上而下针刺巩固；依次经一道预针刺、三道主针刺、高温热轧、卷绕；其中预针刺的针频为600刺/min，针深为12mm；第一主针刺的针频为750刺/min，针深为10mm；第二主针刺的针频为750刺/min，针深为8mm；第三主针刺的针频为750刺/min，针深为5mm；高温热轧，热轧温度为225℃；进入卷曲机卷绕；制得针刺无纺布；
S4.将针刺无纺布以9m/min匀速通过步骤(1)制备的阻燃剂溶液，使针刺无纺布在阻燃剂溶液中充分浸润；经阻燃剂溶液浸润后的针刺无纺布，以9m/min的速度，依次通过双辊压轧、轧干力度6kg；拉幅；温度为150℃条件下烘干，并将表面烫平压光得无纺布基层。
(4)制备耐水洗层、阻燃层，步骤如下：
S1.耐水洗层：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯加入去离子水中，搅拌15min，制得混合液A；
将β-环糊精与甲基丙烯酸缩水甘油酯加入到二甲基乙酰胺溶剂中，加入对苯二酚，在温度为62℃条件下，反应6h；自然冷却；向其中加入丙酮溶液，反应产生白色沉淀；过滤白色沉淀，丙酮溶液洗涤；真空干燥，制得包合物B；
将无纺布基层放入混合液A中，浸泡60min；加入包合物B，在温度为40℃、在光引发条件下，浸泡8h；真空烘干，形成耐水洗层；
S2.三氧化二锑、氢氧化镁、氢氧化铝、UV胶混合熔融，制得混合液C；在S1中制备的无纺布基层正、反面涂覆涂混合液C，涂层厚度为30μm，静置，烘干，形成阻燃层。
对比例1
一种耐水洗阻燃无纺布，包括，由内到外依次为无纺布基层、耐水洗层、阻燃层。无纺布基层包括，按重量份数计，改性粘胶纤维70份，涤纶纤维25份，丙纶纤维25份。
耐水洗层为混合溶液A和包合物B浸泡形成，阻燃层由混合液C涂覆形成；混合溶液A和包合物B的质量比为1：2；混合溶液A包括：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯，其质量比为5:1:0.1；所述包合物B由β-环糊精与甲基丙烯酸缩水甘油酯反应制得，其质量比为1:2；
混合液C包括：三氧化二锑、氢氧化镁、氢氧化铝、UV胶，其质量比为3:1:1：0.1。
其中改性粘胶纤维包括：按重量份计，粘胶纤维90份、阻燃剂溶液25份，阻燃剂溶液为三聚氰胺磷酸酯。
一种耐水洗阻燃无纺布的制备方法，包括以下步骤；
(1)制备改性粘胶纤维，步骤如下：
向阻燃剂溶液中加入粘胶纤维纺丝原液；磁力搅拌30min，搅拌速度为220r/min，得到共混液；共混液在温度为32℃条件下，真空脱泡45min，得到改性粘胶纺丝液；
将改性粘胶纺丝液与凝固浴中的凝固剂接触，经纺丝孔输出形成初生纤维；对初生纤维牵伸；中和、水洗；得到改性粘胶纤维。
(2)制备无纺布基层，步骤如下：
S1.将改性粘胶纤维、涤纶纤维、丙纶纤维开松，混条；
S2.梳理除杂，堆叠铺成纤维网，纤维网层数为10层；
S3.将纤维网自上而下针刺巩固；依次经一道预针刺、三道主针刺、高温热轧、卷绕；其中预针刺的针频为600刺/min，针深为12mm；第一主针刺的针频为750刺/min，针深为10mm；第二主针刺的针频为750刺/min，针深为8mm；第三主针刺的针频为750刺/min，针深为5mm；高温热轧，热轧温度为225℃；进入卷曲机卷绕；制得针刺无纺布；
S4.将针刺无纺布以9m/min匀速通过步骤(1)制备的阻燃剂溶液，使针刺无纺布在阻燃剂溶液中充分浸润；经阻燃剂溶液浸润后的针刺无纺布，以9m/min的速度，依次通过双辊压轧、轧干力度6kg；拉幅；温度为150℃条件下烘干，并将表面烫平压光得无纺布基层。
(3)制备耐水洗层、阻燃层，步骤如下：
S1.耐水洗层：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯加入去离子水中，搅拌15min，制得混合液A；
将β-环糊精与甲基丙烯酸缩水甘油酯加入到二甲基乙酰胺溶剂中，加入对苯二酚，在温度为62℃条件下，反应6h；自然冷却；向其中加入丙酮溶液，反应产生白色沉淀；过滤白色沉淀，丙酮溶液洗涤；真空干燥，制得包合物B；
将无纺布基层放入混合液A中，浸泡60min；加入包合物B，在温度为40℃、在光引发条件下，浸泡8h；真空烘干，形成耐水洗层；
S2.三氧化二锑、氢氧化镁、氢氧化铝、UV胶混合熔融，制得混合液C；在S1中制备的无纺布基层正、反面涂覆涂混合液C，涂层厚度为30μm，静置，烘干，形成阻燃层。
对比例2
一种耐水洗阻燃无纺布，包括，由内到外依次为无纺布基层、耐水洗层、阻燃层。无纺布基层包括，按重量份数计，改性粘胶纤维70份，涤纶纤维25份，丙纶纤维25份。
耐水洗层为混合溶液A浸泡形成，阻燃层由混合液C涂覆形成；混合溶液A包括：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯，其质量比为5:1:0.1；
混合液C包括：三氧化二锑、氢氧化镁、氢氧化铝、UV胶，其质量比为3:1:1：0.1。
其中改性粘胶纤维包括：按重量份计，粘胶纤维90份、阻燃剂溶液25份。
阻燃剂溶液由质量比为1：2的β-环糊精和三聚氰胺磷酸酯混配制得。
一种耐水洗阻燃无纺布的制备方法，包括以下步骤；
步骤(1-3)与实施例3中步骤(1-3)相同；
(4)制备耐水洗层、阻燃层，步骤如下：
S1.耐水洗层：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯加入去离子水中，搅拌15min，制得混合液A；
将无纺布基层放入混合液A中，浸泡60min；真空烘干，形成耐水洗层；
S2.三氧化二锑、氢氧化镁、氢氧化铝、UV胶混合熔融，制得混合液C；在S1中制备的无纺布基层正、反面涂覆涂混合液C，涂层厚度为30μm，静置，烘干，形成阻燃层。
试验对比分析
为了更好的说明本发明技术方案的优势，将本发明技术方案与现有技术方案做对比实验；实施例1-3为本方明技术方案；
对比例1中阻燃剂仅使用三聚氰胺磷酸酯溶液，其他步骤与实施例3相同；
对比例2中制备耐水洗层时仅使用环氧丙烯酯、丙烯酸丁酯、十二碳醇酯，其他步骤与实施例3相同。
试验：取实施例1-3、对比例1-2制得的阻燃无纺布，测定极限氧指数；将5组阻燃无纺布同时置于水中，洗涤50次，每次水洗时间30min；真空烘干，采用极限氧指数测定仪检测水洗后无纺布的极限氧指数；测量水洗前后5组无纺布的横向尺寸，计算水洗后横向尺寸伸长量；检测数据见下表1：
Figure BDA0002555208240000171
表1
由表1可知，实施例1-3水洗前的极限氧指数比对比1高出9-10％，说明本技术方案中利用β-环糊精包合AlCl3形成的包合物与三聚氰胺磷酸酯协同阻燃效果比三聚氰胺磷酸酯的阻燃效果要好；
经水洗50次后，实施例1-3阻燃无纺布的横向尺寸伸长量比对比例2小，说明本技术方案提供的阻燃无纺布经环氧丙烯酸酯、β-环糊精、甲基丙烯酸缩水甘油酯混配溶液浸泡后的耐水洗性能比环氧丙烯酸酯溶液浸泡的阻燃无纺布的耐水洗性能优。
且实施例1-3阻燃无纺布水洗后的极限氧指数比对比例2要高，说明本技术方案提供的耐水洗层在保证耐水洗效果的情况下，还可以减少阻燃剂的流失。
对于本领域技术人员而言，显然本发明不限于上述示范性实施例的细节，而且在不背离本发明的精神或基本特征的情况下，能够以其他的具体形式实现本发明。因此，无论从哪一点来看，均应将实施例看作是示范性的，而且是非限制性的，本发明的范围由所附权利要求而不是上述说明限定，因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。

Claims (3)

1.一种耐水洗阻燃无纺布的制备方法，其特征在于：包括以下步骤；
（1）制备阻燃剂溶液：
取β-环糊精，加入蒸馏水制成饱和溶液，加入AlCl3混合，温度为60-70℃条件下，搅拌30-40min,静置，抽滤，乙醇溶液水洗，烘干，制得包合物A；三聚氰胺磷酸酯溶液与包合物A混合；超声分散10-20min,制得阻燃剂溶液；
（2）制备改性粘胶纤维：
向阻燃剂溶液中加入粘胶纤维纺丝原液；磁力搅拌30min，搅拌速度为180-220r/min，得到共混液；共混液在温度为27-32℃条件下，真空脱泡40-45min，得到改性粘胶纺丝液；
将改性粘胶纺丝液与凝固浴中的凝固剂接触，经纺丝孔输出形成初生纤维；对初生纤维牵伸；中和、水洗；得到改性粘胶纤维；
（3）制备无纺布基层：
S1.将改性粘胶纤维、涤纶纤维、丙纶纤维开松，混条；
S2.梳理除杂，堆叠铺成纤维网，纤维网层数为8-10层；
S3.将纤维网自上而下针刺巩固；依次经一道预针刺、三道主针刺、高温热轧、卷绕；其中预针刺的针频为600刺/min，针深为12mm；第一主针刺的针频为750刺/min，针深为10mm；第二主针刺的针频为750刺/min，针深为8mm；第三主针刺的针频为750刺/min，针深为5mm；高温热轧，热轧温度为220-225℃；进入卷曲机卷绕；制得针刺无纺布；
S4.将针刺无纺布以7-9m/min匀速通过步骤（1）制备的阻燃剂溶液，使针刺无纺布在阻燃剂溶液中浸泡；经阻燃剂溶液浸泡后的针刺无纺布，以7-9m/min的速度，依次通过双辊压轧、轧干力度3-6kg；拉幅；温度为145-150℃条件下烘干，并将表面烫平压光，制得无纺布基层；
（4）制备耐水洗层、阻燃层：
S1.耐水洗层：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯加入去离子水中，搅拌10-15min，制得混合液A；
将β-环糊精与甲基丙烯酸缩水甘油酯加入到二甲基乙酰胺溶剂中，加入对苯二酚，在温度为57-62℃条件下，反应6h；自然冷却；向其中加入丙酮溶液，反应产生白色沉淀；过滤白色沉淀，丙酮溶液洗涤；真空干燥，制得包合物B；
将无纺布基层放入混合液A中，浸泡40-60min；加入包合物B，在温度为37-40℃、光引发条件下，浸泡6-8h；真空烘干，形成耐水洗层；
S2.三氧化二锑、氢氧化镁、氢氧化铝、UV胶混合熔融，制得混合液C；在步骤（4）S1处理后的无纺布基层正、反面涂覆混合液C，涂层厚度为15-30μm，静置，烘干，形成阻燃层。
2.一种根据权利要求1所述的制备方法制备的耐水洗阻燃无纺布，其特征在于：所述耐水洗阻燃无纺布包括，由内到外依次为无纺布基层、耐水洗层、阻燃层；
其中无纺布基层包括，按重量份数计，改性粘胶纤维45-70份，涤纶纤维15-25份，丙纶纤维15-25份。
3.根据权利要求2所述的一种耐水洗阻燃无纺布，其特征在于：所述耐水洗层为混合溶液A和包合物B浸泡形成，阻燃层由混合液C涂覆形成；
所述混合溶液A和包合物B的质量比为1：2；
所述混合溶液A包括：环氧丙烯酸酯、丙烯酸丁酯、十二碳醇酯，其质量比为5:1:0.1；所述包合物B由β-环糊精与甲基丙烯酸缩水甘油酯反应制得，其质量比为1:2；
所述混合液C包括：三氧化二锑、氢氧化镁、氢氧化铝、UV胶，其质量比为3:1:1：0.1。
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