CN114481629B - 一种耐高温无纺布及其制备方法 - Google Patents

一种耐高温无纺布及其制备方法 Download PDF

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CN114481629B
CN114481629B CN202210119385.8A CN202210119385A CN114481629B CN 114481629 B CN114481629 B CN 114481629B CN 202210119385 A CN202210119385 A CN 202210119385A CN 114481629 B CN114481629 B CN 114481629B
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刘敬成
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Abstract

本发明公开了一种耐高温无纺布及其制备方法,耐高温无纺布由聚芳酰胺纤维经如下重量份的原料整理干燥后经水刺处理制得:改性氨基硅氧烷低聚物:6~10份;聚乙烯醇:10~20份;阳离子树脂:15~25份;耐温填料:3~8份;碱性调节剂:0.01~1份;水:60~80份。本申请的耐高温无纺布在高温环境下具有较好的吸水性能,且稳定性好,长效性好。

Description

一种耐高温无纺布及其制备方法
技术领域
本发明涉及无纺布领域,尤其是涉及一种耐高温无纺布及其制备方法。
背景技术
耐高温无纺布可用于高温环境下的防护服、滤材和装饰建材的制造,因其对高温的耐受性,被广泛应用于防护、电子机械、建筑等领域。目前,耐高温无纺布的纤维原料主要有芳香族聚酰胺纤维、聚酰亚胺纤维、聚四氟乙烯纤维以及玻璃纤维、陶瓷纤维等无机纤维。
当无纺布应用于防护服等防护材料时,其不仅需要具有耐高温性能,同时还需要有较好的亲水性,从而对高温环境下人体表面的汗水进行吸附,提高防护服的使用性能。
发明内容
为改善耐高温无纺布的亲水性,本申请提供一种耐高温无纺布及其制备方法。
第一方面,本申请提供一种耐高温无纺布,其由聚芳酰胺纤维经如下重量份的原料整理干燥后经水刺处理制得:
改性氨基硅氧烷低聚物:6~10份;
聚乙烯醇:10~20份;
阳离子树脂:15~25份;
耐温填料:3~8份;
碱性调节剂:0.01~1份;
水:60~80份。
通过采用上述技术方案,氨基硅氧烷低聚物与聚乙烯醇在纤维表面形成相互交联的具有聚合网络结构的亲水膜层,其表现为强亲水性,可增加聚芳酰胺纤维对汗水的吸附作用。同时,交联的网络结构保障了其粘接强度,使其不易脱落。阳离子树脂也具有一定的亲水性,同时,利用阳离子树脂将耐温填料粘接在亲水膜表面,保障纤维表面整理剂的整体的耐温性,提高其长效性。
优选的,所述改性氨基硅氧烷低聚物按照如下方法制备得到:
S101:将氨基硅氧烷充分溶解于醇类溶剂中,得到混合液,在加热条件下,将水和醇的混合溶液滴入混合液中,使硅烷充分水解,加入改性剂,充分混合,得到硅烷水解液;
S102:将硅烷水解液加热升温至95~110℃,聚合2~4h,减压蒸馏出溶剂,升温至120~140℃,继续进行聚合反应,聚合完成后降至室温,得到氨基硅氧烷低聚物。
上述技术方案中,使氨基硅氧烷在醇溶液中进行水解后进行缩聚,得到具有Si-O-Si主链和大量氨基的氨基硅氧烷低聚物。氨基具有较好的亲水性,且能够和纤维表面的活性基团以及聚乙烯醇的醇羟基通过氢键键合,在增强纤维亲水性的同时,保障了交联聚合物网络结构的形成,提高了亲水膜的粘接强度。
本申请对氨基硅氧烷的选择无特别要求,优选氨基官能度高的多氨基硅氧烷。可采用γ―氨丙基三甲氧基硅烷、γ―氨丙基三乙氧基硅烷、N-(2-氨乙基)-3-氨丙基甲基二甲氧基硅烷、N-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷、N-2-氨乙基-3-氨丙基三乙氧基硅烷、N-2-氨乙基-3-氨丙基三甲氧基硅烷中的至少一种;醇类溶剂可采用甲醇、乙醇;改性剂只需能够溶解即可,优选改性剂用量为氨基硅氧烷的5~10%。
优选的,所述氨基硅氧烷低聚物的聚合度为5~15。
上述技术方案中,在该聚合度下,氨基硅氧烷低聚物具有较好的亲水性,且在高温下的粘接性能稳定,不易脱落。
优选的,所述改性剂采用甲基纤维素和单宁酸中的一种或其组合物。
上述技术方案中,甲基纤维素具有较高的吸水性,采用甲基纤维素改性制得的氨基硅氧烷低聚物,有利于提高聚芳酰胺纤维的吸水率。聚芳酰胺纤维表面活性基团少,而单宁酸中含有大量的邻苯酚基团,具有强亲水性,采用单宁酸制得的氨基硅氧烷低聚物,有利于提高亲水膜层在聚芳酰胺纤维上的粘接强度和亲水性。
优选的,所述甲基纤维素采用羧甲基纤维素、羟丙基甲基纤维素与羟甲基纤维中的一种或多种。
上述的甲基纤维素均具有极好的吸水性能,有利于最终改善聚芳酰胺纤维的吸水率。
优选的,所述阳离子树脂按照如下方法制备得到:
S201:将有机胺、N-氨乙基哌嗪和3-氯-2羟丙基三甲基氯化铵在90~120℃下进行取代反应,得到季铵化有机胺;
S202:将季铵化有机胺溶解于有机溶剂中,加热升温至100~120℃,加入双氰胺,升温至150~170℃下进行缩聚反应,得到缩聚物;
S203:将缩聚物降温至110~130℃,加入二羟甲基二羟基乙烯脲树脂,得到阳离子树脂。
上述技术方案,步骤S201中,将有机胺与醚化剂3-氯-2羟丙基三甲基氯化铵反应,得到阳离子改性的有机胺;步骤S202中,通过加入具有大量氨基反应型基团的双氰胺,使得季铵化有机胺与双氰胺发生缩聚反应并经环构化,得到带正电性的缩聚物;步骤S203中,二羟甲基二羟基乙烯脲树脂与缩聚物分子链上的亚胺基反应,得到阳离子树脂。
利用该阳离子树脂,一方面,二羟甲基二羟基乙烯脲树脂中含有的羟甲基具有亲水性,另一方面,羟甲基能够与耐温填料通过氢键键合,还能够与亲水膜上的羟基或氨基等活性基团键合,起到架桥作用,从而形成牢固的连接。
优选的,所述有机胺采用二乙烯三胺、三乙烯四胺、四乙烯五胺与乙二胺中的一种或几种。
上述有机胺均能够有效参与醚化和缩聚反应,得到带正电性的阳离子树脂。
优选的,所述耐温填料采用空心玻璃微珠、氧化镁、氧化铝与二氧化硅中的一种或几种。
上述无机填料具有较好的隔热性能,有利于保障聚芳酰胺纤维表面亲水改性聚合物的粘接稳定性,提高其亲水性能的长效性。
第二方面,本申请提供一种耐高温无纺布的制备方法,包括如下步骤:
S301:取配方用水的30~50%,加入改性氨基硅氧烷低聚物与聚乙烯醇,充分混合,得到整理剂A,然后将聚芳酰胺纤维浸没于整理剂A中,充分混合,过滤静置,得到亲水改性聚芳酰胺纤维;
S302:取剩余配方用水,加入耐温填料与阳离子树脂,再加入碱性调节剂控制pH为9~10,得到整理剂B,将亲水改性聚芳酰胺纤维浸没于整理剂B中,充分混合,过滤取出后烘干,得到耐高温亲水聚芳酰胺纤维;
S303:将耐高温亲水聚芳酰胺纤维进行开松、梳理、铺网、牵伸和水刺处理,得到耐高温无纺布。
上述技术方案中,步骤S301中,改性氨基硅氧烷低聚物与聚乙烯醇在纤维表面形成相互交联的具有聚合网络结构的亲水膜,且具有较好的吸水率,可有效改善耐高温无纺布的亲水和吸水性能。步骤S302中,以阳离子树脂为粘接剂,由于其分子结构中含有的羟甲基能够与亲水膜的活性基团键合,也能够与耐温填料表面的活性基团键合,从而起到架桥作用,促使耐温填料被粘接在亲水膜表面,保障纤维表面改性聚合物整体的耐温性,提高其粘接性能的长效性。同时,通过碱性调节剂使得整理剂B呈碱性,使得整理剂B中的耐温填料表面的羟基与OH-反应而带负电,一方面通过同性电荷件的静电作用,促使耐温填料充分分散;另一方面,阳离子树脂能够对待负电的耐温填料形成更为牢固的连接,有利于保障聚芳酰胺纤维亲水性能的长效性。
综上所述,本申请具有如下有益效果:
1、首先,本申请中通过采用改性氨基硅烷低聚物、聚乙烯醇、阳离子树脂和耐温填料复配,并对聚芳酰胺纤维进行后整理,得到具有长效亲水性的耐高温无纺布。
2、其次,采用甲基纤维素与单宁酸对氨基硅烷低聚物进行改性,显著的提高了氨基硅烷低聚物的亲水性、吸水性及其与聚芳酰胺纤维的粘接性能。
3、最后,本申请通过采用有有机胺、3-氯-2羟丙基三甲基氯化铵和双氰胺制得带正电性的阳离子树脂,并通过使耐温填料带负电性,从而使得阳离子树脂和耐温填料间形成化学键合及静电吸附,有效保障所制得耐高温无纺布的长效亲水性。
具体实施方式
改性氨基硅氧烷低聚物的制备例
制备例1a,一种改性氨基硅烷低聚物,按照如下方法制备得到:
S101:将1000gN-(2-氨乙基)-3-氨丙基甲基二乙氧基硅烷加入200g甲醇溶剂中,搅拌混合,得到混合液,加热升温至50℃,在搅拌条件下,将100g水和200g甲醇的混合溶液滴入混合液中,使硅烷充分水解,加入30g羧甲基纤维素与30g单宁酸(改性剂),搅拌30min,得到硅烷水解液;
S102:将步骤S101所得硅烷水解液加热升温至95℃,进行缩聚反应,2h后减压蒸馏出溶剂甲醇,然后升温至130℃,继续进行缩聚反应,2h后降至室温,得平均聚合度为10的改性氨基硅氧烷低聚物。
制备例2a,一种改性氨基硅烷低聚物,按照如下方法制备得到:
S101:将1000gγ―氨丙基三甲氧基硅烷加入300g甲醇溶剂中,搅拌混合,得到混合液,加热升温至65℃,在搅拌条件下,将150g水和150g甲醇的混合溶液滴入混合液中,使硅烷充分水解,加入10g羧甲基纤维素与40g单宁酸(改性剂),搅拌30min,得到硅烷水解液;
S102:将步骤S101所得硅烷水解液加热升温至110℃,进行缩聚反应,3h后减压蒸馏出溶剂甲醇,然后升温至140℃,继续进行缩聚反应,2h后降至室温,得平均聚合度为13的改性氨基硅氧烷低聚物。
制备例3a,一种改性氨基硅烷低聚物,按照如下方法制备得到:
S101:将1000gγ―氨丙基三甲氧基硅烷加入250g乙醇溶剂中,搅拌混合,得到混合液,加热升温至60℃,在搅拌条件下,将80g水和300g乙醇的混合溶液滴入混合液中,使硅烷充分水解,加入60g羧甲基纤维素与10g单宁酸(改性剂),搅拌30min,得到硅烷水解液;
S102:将步骤S101所得硅烷水解液加热升温至100℃,进行缩聚反应,1h后减压蒸馏出溶剂乙醇,然后升温至120℃,继续进行缩聚反应,2h后降至室温,得平均聚合度为6的改性氨基硅氧烷低聚物。
制备例4a,一种改性氨基硅烷低聚物,与制备例1a的区别在于,改性剂中,采用等量的羟甲基纤维素替代羧甲基纤维素。
制备例5a,一种改性氨基硅烷低聚物,与制备例1a的区别在于,改性剂中,采用等量的羟丙基甲基纤维素替代羧甲基纤维素。
制备例6a,一种改性氨基硅烷低聚物,与制备例1a的区别在于,改性剂中,采用等量的单宁酸替代羧甲基纤维素。
制备例7a,一种改性氨基硅烷低聚物,与制备例1a的区别在于,改性剂中,采用等量的羧甲基纤维素替代单宁酸。
制备例8a,一种氨基硅烷低聚物,与制备例1a的区别在于,步骤S101中,未加入有改性剂。
阳离子树脂的制备例
制备例1b,一种阳离子树脂,按照如下步骤制备得到:
S201:将12㎏三乙烯四胺、6㎏N-氨乙基哌嗪和10㎏3-氯-2羟丙基三甲基氯化铵在110℃下进行取代反应,得到季铵化有机胺;
S202:将季铵化有机胺溶解于15㎏甲醇中,加热升温至120℃,加入10㎏双氰胺,在搅拌条件下,升温至160℃并保温,反应3h,得到缩聚物;
S203:将缩聚物降温至120℃,加入二羟甲基二羟基乙烯脲树脂,搅拌并反应2h,制得阳离子树脂。
其中,二羟甲基二羟基乙烯脲树脂获自南通润丰。
制备例2b,一种阳离子树脂,按照如下步骤制备得到:
S201:将10㎏二乙烯三胺、6.5㎏N-氨乙基哌嗪和8㎏3-氯-2羟丙基三甲基氯化铵在100℃下进行取代反应,得到季铵化有机胺;
S202:将季铵化有机胺溶解于15㎏甲醇中,加热升温至110℃,加入10㎏双氰胺,在搅拌条件下,升温至150℃并保温,反应2h,得到缩聚物;
S203:将缩聚物降温至110℃,加入二羟甲基二羟基乙烯脲树脂,搅拌并反应2h,制得阳离子树脂。
实施例
实施例1,一种耐高温无纺布,各原料配比如表1所示,且按照如下方法制备得到:S301:取配方用水的40%,加入改性氨基硅氧烷低聚物与聚乙烯醇,搅拌20min,得到整理剂A,然后将30㎏聚芳酰胺纤维浸没于整理剂A中,继续搅拌5min,过滤取出纤维,于室温下静置1h,得到亲水改性聚芳酰胺纤维;
S302:取剩余配方用水,加入空心玻璃微珠(耐温填料)与阳离子树脂,再加入10wt%氨水(碱性调节剂)控制pH为9~10,得到整理剂B,将亲水改性聚芳酰胺纤维浸没于整理剂B中,充分混合,过滤取出后烘干,得到耐高温亲水聚芳酰胺纤维;
S303:将耐高温亲水聚芳酰胺纤维进行开松、梳理、铺网、牵伸和水刺处理,得到耐高温无纺布。
实施例2~3,一种耐高温无纺布,与实施例1的区别在于,各原料配比不同且如表1所示。
表1、实施例1~3中整理用原料配比(㎏)
表1中,改性氨基硅氧烷低聚物为制备例1a制得改性氨基硅氧烷低聚物;聚乙烯醇的聚合度为500;阳离子树脂为制备例1b制得阳离子树脂;空心玻璃微珠D90≤100μm。
实施例4,一种耐高温无纺布,与实施例1的区别在于,改性氨基硅氧烷低聚物为制备例2a制得改性氨基硅氧烷低聚物。
实施例5,一种耐高温无纺布,与实施例1的区别在于,改性氨基硅氧烷低聚物为制备例3a制得改性氨基硅氧烷低聚物。
实施例6,一种耐高温无纺布,与实施例1的区别在于,改性氨基硅氧烷低聚物为制备例4a制得改性氨基硅氧烷低聚物。
实施例7,一种耐高温无纺布,与实施例1的区别在于,改性氨基硅氧烷低聚物为制备例5a制得改性氨基硅氧烷低聚物。
实施例8,一种耐高温无纺布,与实施例1的区别在于,改性氨基硅氧烷低聚物为制备例6a制得改性氨基硅氧烷低聚物。
实施例9,一种耐高温无纺布,与实施例1的区别在于,改性氨基硅氧烷低聚物为制备例7a制得改性氨基硅氧烷低聚物。
实施例10,一种耐高温无纺布,与实施例1的区别在于,阳离子树脂为制备例2b制得阳离子树脂。
实施例11,一种耐高温无纺布,与实施例1的区别在于,耐温填料采用平均粒径为30μm的氧化铝。
实施例12,一种耐高温无纺布,与实施例1的区别在于,步骤S302中,不添加碱性调节剂,且加入碳酸氢钠溶液,调节整理剂B的pH值为7。
对比例
对比例1,一种耐高温无纺布,与实施例1的区别在于,采用等量制备例8a制得氨基硅氧烷低聚物替代制备例1a制得改性氨基硅氧烷低聚物。
对比例2,一种耐高温无纺布,与实施例1的区别在于,原料中未添改性氨基硅氧烷低聚物。
对比例3,一种耐高温无纺布,与实施例1的区别在于,原料中未添加有聚乙烯醇。
对比例4,一种耐高温无纺布,与实施例1的区别在于,原料中未添加有聚乙烯醇和改性氨基硅氧烷低聚物。
对比例5,一种耐高温无纺布,与实施例1的区别在于,原料中采用等量的聚乙烯醇替代阳离子树脂。
对比例6,一种耐高温无纺布,与实施例1的区别在于,原料中未添加有耐温填料。
对比例7,市售芳纶无纺布。
性能检测试验
试验1:耐高温无纺布吸水性能测试试验方法:按照ASTM F726-12中的规定对无纺布的吸水性能进行测定。从上述实施例与对比例制得的无纺布中剪取尺寸为3cm*3cm的无纺布作为试样,取5块试样并测定其初始重量的平均值(M0);然后取一个1L的烧杯并向烧杯内注水,直至烧杯内水位高度达到8cm,将试样平铺于水面上;将烧杯放置于振动摇床上,设置振动频率为100r/min,振幅为3cm,10min后取出,悬空静置控水30s,称重,测得其平均值,记作M1。按照(M1-M0)/M0计算得到试样的吸水率S0(g.g-1),测试结果如表2所示。
试验2:耐高温无纺布长效性测试试验方法:(1)将上述实施例与对比例制得的耐高温无纺布于220℃的温度下静置24h,取出于室温环境(25±2℃,50±5%RH)下静置24h,然后按照试验1中的试验方法再次测量其吸水率S1,按照S0-S1测得吸水率下降值Sa,测试结果如表2所示。
(2)参照GB/T21196.1-2007的规定,采用马丁代尔耐磨试验仪进行1000次摩擦测试,测量1000次摩擦后试样的吸水率下降值St,测试结果如表2所示。
表2、耐高温无纺布吸水性能和长效性测试结果
试验结果分析:
结合实施例1~12和对比例1~7并结合表2可以看出,实施例1~12中采用由改性氨基硅烷低聚物、聚乙烯醇、阳离子树脂与耐温填料复配整理得到的耐高温无纺布,其具有较好的吸水率,能够在高温环境中有效吸附水分,且性能稳定,长效性好。
上述原因可能在于,改性氨基硅氧烷低聚物能够与聚乙烯醇在纤维表面形成相互交联的具有聚合网络结构的亲水膜,亲水膜层具有较好的吸水率,可有效改善耐高温无纺布的亲水和吸水性能。以阳离子树脂为粘接剂,并利用其架桥作用,将耐温填料粘接在亲水膜表面,以保障亲水膜的稳定,从而提高其粘接性能的长效性。另外,改性氨基硅氧烷低聚物能够与聚乙烯醇形成的交联网络结构也有助于提高吸水性能的长效性。
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 (5)

1.一种耐高温无纺布,其特征在于,由聚芳酰胺纤维经如下重量份的原料整理干燥后经水刺处理制得:
改性氨基硅氧烷低聚物:6~10份;
聚乙烯醇:10~20份;
阳离子树脂:15~25份;
耐温填料:3~8份;
碱性调节剂:0.01~1份;
水:60~80份;
所述改性氨基硅氧烷低聚物按照如下方法制备得到:
S101:将氨基硅氧烷充分溶解于醇类溶剂中,得到混合液,在加热条件下,将水和醇的混合溶液滴入混合液中,使硅烷充分水解,加入改性剂,充分混合,得到硅烷水解液;
S102:将硅烷水解液加热升温至95~110℃,聚合2~4h,减压蒸馏出溶剂,升温至120~140℃,继续进行聚合反应,聚合完成后降至室温,得到氨基硅氧烷低聚物;
所述改性剂采用羧甲基纤维素、羟丙基甲基纤维素、羟甲基纤维素和单宁酸中的一种或其组合物;
所述阳离子树脂按照如下方法制备得到:
S201:将有机胺、N-氨乙基哌嗪和3-氯-2-羟丙基三甲基氯化铵在90~120℃下进行取代反应,得到季铵化有机胺;
S202:将季铵化有机胺溶解于有机溶剂中,加热升温至100~120℃,加入双氰胺,升温至150~170℃下进行缩聚反应,得到缩聚物;
S203:将缩聚物降温至110~130℃,加入二羟甲基二羟基乙烯脲树脂,得到阳离子树脂。
2.根据权利要求1所述的一种耐高温无纺布,其特征在于,所述氨基硅氧烷低聚物的聚合度为5~15。
3.根据权利要求1所述的一种耐高温无纺布,其特征在于,所述有机胺采用二乙烯三胺、三乙烯四胺、四乙烯五胺与乙二胺中的一种或几种。
4.根据权利要求1所述的一种耐高温无纺布,其特征在于,所述耐温填料采用空心玻璃微珠、氧化镁、氧化铝与二氧化硅中的一种或几种。
5.根据权利要求1~4中任一项所述的一种耐高温无纺布的制备方法,其特征在于,包括如下步骤:
S301:取配方用水的30~50%,加入改性氨基硅氧烷低聚物与聚乙烯醇,充分混合,得到整理剂A,然后将聚芳酰胺纤维浸没于整理剂A中,充分混合,过滤静置,得到亲水改性聚芳酰胺纤维;
S302:取剩余配方用水,加入耐温填料与阳离子树脂,再加入碱性调节剂控制pH为9~10,得到整理剂B,将亲水改性聚芳酰胺纤维浸没于整理剂B中,充分混合,过滤取出后烘干,得到耐高温亲水聚芳酰胺纤维;
S303:将耐高温亲水聚芳酰胺纤维进行开松、梳理、铺网、牵伸和水刺处理,得到耐高温无纺布。
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