CN112553904A - 一种含磷氟硅超疏水阻燃棉织物及其制备方法 - Google Patents
一种含磷氟硅超疏水阻燃棉织物及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种含磷氟硅超疏水阻燃棉织物及其制备方法,通过光敏性含磷氟聚合物和八乙烯基‑POSS在紫外光下引发交联聚合,结合呼吸图法,在棉织物上构筑具有有序微纳结构的含磷氟硅交联涂层,交联后的涂层具有耐久性。棉织物上引入的涂层含有磷、氟、硅三种元素,三者通过协同作用有效提高棉织物的阻燃性能;同时,氟、硅元素与涂层表面微纳结构的结合,使棉织物具备超疏水的性能,从而赋予织物自清洁、抗污和油水分离等功能。
Description
技术领域
本发明属于超疏水阻燃棉织物领域,特别涉及一种含磷氟硅超疏水阻燃棉织物及其制备方法。
背景技术
当材料的表面接触角大于150°或滚动角小于10°时,就可被称为超疏水表面,超疏水材料是在仿生的基础上而发展起来的一种新型材料。超疏水表面优异的拒水能力,使其具备有抗污、自清洁、油水分离、防雾、防结冰或抗腐蚀等多种功能,因此自其发展起就收到了广泛的青睐与迅速的发展。虽然超疏水材料的制备方法层出不穷,然而超疏水表面的实现仍然需要结合低表面能化合物和微观形貌两种条件才可实现。
棉织物是以棉为原料纺织而生的面料,具有轻质、柔软和透气等优点,同时它也有缩水率大、吸湿性强、使用寿命短、容易发霉和抗污性差等缺点,限制了其在家居和服饰等领域的应用。同时,棉织物的主要组成成分是纤维素,阻燃性能差,其相应的棉制品在使用过程中存在着安全隐患。因此,要解决棉织物的这些缺点,对其进行超疏水与阻燃的改性,是十分必要的。对于棉织物的超疏水或阻燃整理,涂层的引入是一种直接、有效的手段。棉织物因其纺织特点,表面具有微细的纵横交错的纹路,是制备超疏水表面的理想材料,因此通过低表面能元素与阻燃元素的引入,即可同时实现棉织物的超疏水与阻燃改性。
发明内容
本发明目的在于提供一种含磷氟硅超疏水阻燃棉织物及其制备方法。
本发明解决其技术问题所采用的技术方案之一:
一种含磷氟硅超疏水阻燃棉织物,所述的棉织物经过了包括有以下结构式的光敏性含磷氟聚合物原料的处理:
其中,x:y:z=0.01~0.99:0.01~0.99:0.01~0.99,其分子量为100~100000。
本发明解决其技术问题所采用的技术方案之二:
一种含磷氟硅超疏水阻燃棉织物的制备方法,包括:
1)向单口瓶中依次加入甲基丙烯酸羟乙酯、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、三乙胺、第一溶剂,所述甲基丙烯酸羟乙酯、DOPO和三乙胺的摩尔比为0.1~50:0.1~50:0.1~50,所述第一溶剂和甲基丙烯酸羟乙酯的比例为20~100mL:0.001~10mol;反应液在-10~100℃下反应2~36h,反应结束后用水萃取3~5次,取有机层旋蒸、干燥后即得含磷单体MA-DOPO。
2)向反应容器中依次加入甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、MA-DOPO、偶氮二异丁腈和第二溶剂,用液氮反复冻融若干次,充入氩气,在35~85℃下反应12~72h,继续向反应液中加入三乙胺和甲基丙烯酰氯,反应6~36h后用第三溶剂进行沉淀,所述甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、MA-DOPO、偶氮二异丁腈、三乙胺和甲基丙烯酰氯的摩尔比为0.1~50:0.1~50:0.1~50:0.01~50:0.1~50:0.1~50;所述第二溶剂、第三溶剂、甲基丙烯酸羟乙酯的比例为:1~50mL:1~1000mL:0.001~10mol固液分离,固体部分用第三溶剂冲洗若干次后干燥,得到光敏性含磷氟聚合物。所述光敏性含磷氟聚合物如前述的结构式1所示:
3)向反应容器中加入光敏性含磷氟聚合物、八乙烯基-POSS(八乙烯基八硅倍半氧烷,化学式:C16H24O12Si8)、1-羟环己基苯酮和第四溶剂,将棉织物浸渍与上述溶液中,升温至35~90℃,用紫外灯照射0.1~36h后取出棉织物,置于湿度为35%~100%的密闭环境中,待干燥后即得所述含磷氟硅超疏水阻燃织物;所述光敏性含磷氟聚合物、八乙烯基-POSS和1-羟环己基苯酮的摩尔比例为0.001~10:0.001~10:0.001~10;所述的第四溶剂和光敏性含磷氟聚合物的比例为5~1000mL:0.001~10mol。
本发明的有益效果:
(1)本发明通过分子设计,制备了光敏性含磷氟聚合物,进一步通过紫外光引发含磷氟聚合物和八乙烯基-POSS聚合产生交联,结合呼吸图法在涂层表面构筑有序微纳结构,实现棉织物的超疏水与阻燃整理,制备方法简单。
(2)棉织物中引入了氟、硅元素,结合涂层表面微纳结构构筑,可赋予棉织物超疏水的性能,从而赋予棉织物抗污、自清洁和油水分离等功能;材料表面有序微纳结构的存在有助于实现油水乳液的分离。
(3)棉织物中引入了氟、硅、磷三种阻燃元素,三者之间协同配合可有效提高棉织物的阻燃性能。
(4)本发明设计了成膜性强的含磷氟聚合物,并通过接枝法引入光敏性基团,进一步与八乙烯基-POSS在紫外光引发下交联,交联后的涂层交联密度大,耐久性强;同时POSS的引入有效提高了涂层的热稳定性;八乙烯基-POSS的选择使得在提高涂层交联密度的同时,避免了POSS引入过多而引起的棉织物硬化。
附图说明
下面结合附图和实施例对本发明作进一步说明。
图1为实施例1中所得光敏性含磷氟聚合物的核磁氢谱。
图2为实施例1中所得含磷氟硅超疏水阻燃织物的表面微纳结构。
具体实施方式
下面通过实施例具体说明本发明的内容:
在本发明的各实施例中,所述第一溶剂优选为氯仿、二氯甲烷、三氯甲烷、四氯化碳中的至少一种。
在本发明的各实施例中,步骤2)所述第二溶剂优选为四氢呋喃、二氯甲烷、三氯甲烷、N,N-二甲基甲酰胺中的至少一种。
在本发明的各实施例中,所述第三溶剂优选为甲醇、乙醇、乙酸乙酯中的一种。
在本发明的各实施例中,步骤3)所述第四溶剂优选为四氢呋喃、二氯甲烷和三氯甲烷中的一种。
实施例1
(1)向单口瓶中依次加入7.23g(55.6mmol)甲基丙烯酸羟乙酯、10g(46.3mmol)9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、5.62g(55.6mmol)三乙胺和80mL二氯甲烷,在25℃下反应12h,反应结束后用水萃取3~5次,取有机层旋蒸、干燥后即得含磷单体MA-DOPO。
(2)向反应容器中依次加入1.3g(10mmol)甲基丙烯酸羟乙酯、4g(10mmol)甲基丙烯酸十二氟庚酯、4.59g(13.3mmol)MA-DOPO、0.037g(0.13mmol)偶氮二异丁腈和20mL四氢呋喃,用液氮反复冻融若干次,充入氩气,在65℃下反应24h,继续向反应液中加入1.0g(10mmol)三乙胺和1.0g(10mmol)甲基丙烯酰氯,反应后12h后用甲醇进行沉淀,固液分离,固体部分用甲醇冲洗若干次后干燥,得到带光敏性含磷氟聚合物。
(3)向反应容器中加入5g光敏性含磷氟聚合物、5g八乙烯基-POSS、0.5g1-羟环己基苯酮和100mL四氢呋喃,将棉织物浸渍与上述溶液中,升温至65℃,用紫外灯照射15min后取出棉织物,置于湿度为80%的密闭环境中,待干燥后即得所述含磷氟硅超疏水阻燃织物。
该含磷氟硅超疏水阻燃织物的接触角为151.2°,和未处理过的棉织物相比,燃烧速率下降了22.5%。
实施例2
(1)向单口瓶中依次加入7.23g(55.6mmol)甲基丙烯酸羟乙酯、10g(46.3mmol)9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、5.62g(55.6mmol)三乙胺和80mL二氯甲烷,在35℃下反应12h,反应结束后用水萃取3~5次,取有机层旋蒸、干燥后即得含磷单体MA-DOPO。
(2)向反应容器中依次加入1.3g(10mmol)甲基丙烯酸羟乙酯、4g(10mmol)甲基丙烯酸十二氟庚酯、4.59g(13.3mmol)MA-DOPO、0.037g(0.13mmol)偶氮二异丁腈和20mL四氢呋喃,用液氮反复冻融若干次,充入氩气,在75℃下反应12h,继续向反应液中加入1.0g(10mmol)三乙胺和1.0g(10mmol)甲基丙烯酰氯,反应后12h后用甲醇进行沉淀,固液分离,固体部分用甲醇冲洗若干次后干燥,得到光敏性含磷氟聚合物。
(3)向反应容器中加入5g光敏性含磷氟聚合物、5g八乙烯基-POSS、0.5g1-羟环己基苯酮和100mL四氢呋喃,将棉织物浸渍与上述溶液中,升温至65℃,用紫外灯照射15min后取出棉织物,置于湿度为80%的密闭环境中,待干燥后即得所述含磷氟硅超疏水阻燃织物。
该含磷氟硅超疏水阻燃织物的接触角为152.1°,和未处理过的棉织物相比,燃烧速率下降了21.3%。
实施例3
(1)向单口瓶中依次加入7.23g(55.6mmol)甲基丙烯酸羟乙酯、10g(46.3mmol)9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、5.62g(55.6mmol)三乙胺和80mL二氯甲烷,在35℃下反应12h,反应结束后用水萃取3~5次,取有机层旋蒸、干燥后即得含磷单体MA-DOPO。
(2)向反应容器中依次加入1.3g(10mmol)甲基丙烯酸羟乙酯、4g(10mmol)甲基丙烯酸十二氟庚酯、4.59g(13.3mmol)MA-DOPO、0.037g(0.13mmol)偶氮二异丁腈20mL四氢呋喃,用液氮反复冻融若干次,充入氩气,在65℃下反应24h,继续向反应液中加入1.0g(10mmol)三乙胺和1.0g(10mmol)甲基丙烯酰氯,反应后12h后用甲醇进行沉淀,固液分离,固体部分用甲醇冲洗若干次后干燥,得到光敏性含磷氟聚合物。
(3)向反应容器中加入2.5g光敏性含磷氟聚合物、2.5g八乙烯基-POSS、0.25g1-羟环己基苯酮和100mL四氢呋喃,将棉织物浸渍与上述溶液中,升温至65℃,用紫外灯照射15min后取出棉织物,置于湿度为80%的密闭环境中,待干燥后即得所述含磷氟硅超疏水阻燃织物。
该含磷氟硅超疏水阻燃织物的接触角为150.8°,和未处理过的棉织物相比,燃烧速率下降了15.5%。
实施例4
(1)向单口瓶中依次加入3.62g(27.8mmol)甲基丙烯酸羟乙酯、10g(46.3mmol)9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、5.62g(55.6mmol)三乙胺和80mL二氯甲烷,在35℃下反应12h,反应结束后用水萃取3~5次,取有机层旋蒸、干燥后即得含磷单体MA-DOPO。
(2)向反应容器中依次加入1.3g(10mmol)甲基丙烯酸羟乙酯、4g(10mmol)甲基丙烯酸十二氟庚酯、4.59g(13.3mmol)MA-DOPO、0.037g(0.13mmol)偶氮二异丁腈20mL四氢呋喃,用液氮反复冻融若干次,充入氩气,在65℃下反应24h,继续向反应液中加入1.0g(10mmol)三乙胺和1.0g(10mmol)甲基丙烯酰氯,反应后12h后用甲醇进行沉淀,固液分离,固体部分用甲醇冲洗若干次后干燥,得到光敏性含磷氟聚合物。
(3)向反应容器中加入5g光敏性含磷氟聚合物、5g八乙烯基-POSS、0.5g1-羟环己基苯酮和100mL四氢呋喃,将棉织物浸渍与上述溶液中,升温至65℃,用紫外灯照射15min后取出棉织物,置于湿度为80%的密闭环境中,待干燥后即得所述含磷氟硅超疏水阻燃织物。
该含磷氟硅超疏水阻燃织物的接触角为150.8°,和未处理过的棉织物相比,燃烧速率下降了15.5%。
实施例5
(1)向单口瓶中依次加入3.62g(27.8mmol)甲基丙烯酸羟乙酯、5g(23.2mmol)9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)、5.62g(55.6mmol)三乙胺和80mL二氯甲烷,在35℃下反应12h,反应结束后用水萃取3~5次,取有机层旋蒸、干燥后即得含磷单体MA-DOPO。
(2)向反应容器中依次加入1.3g(10mmol)甲基丙烯酸羟乙酯、4g(10mmol)甲基丙烯酸十二氟庚酯、4.59g(13.3mmol)MA-DOPO、0.037g(0.13mmol)偶氮二异丁腈20mL四氢呋喃,用液氮反复冻融若干次,充入氩气,在65℃下反应24h,继续向反应液中加入1.0g(10mmol)三乙胺和1.0g(10mmol)甲基丙烯酰氯,反应后12h后用甲醇进行沉淀,固液分离,固体部分用甲醇冲洗若干次后干燥,得到光敏性含磷氟聚合物。
(3)向反应容器中加入5g光敏性含磷氟聚合物、5g八乙烯基-POSS、0.5g1-羟环己基苯酮和100mL四氢呋喃,将棉织物浸渍与上述溶液中,升温至65℃,用紫外灯照射15min后取出棉织物,置于湿度为80%的密闭环境中,待干燥后即得所述含磷氟硅超疏水阻燃织物。
该含磷氟硅超疏水阻燃织物的接触角为150.8°,和未处理过的棉织物相比,燃烧速率下降了19.8%。
以上所述,仅为本发明较佳实施例而已,故不能依此限定本发明实施的范围,即依本发明专利范围及说明书内容所作的等效变化与修饰,皆应仍属本发明涵盖的范围内。
Claims (10)
2.根据权利要求1所述的一种含磷氟硅超疏水阻燃棉织物,其特征在于:所述的棉织物经过包括有权利要求1所述的光敏性含磷氟聚合物、八乙烯基-POSS、1-羟环己基苯酮和第四溶剂在内的溶液的处理。
3.根据权利要求2所述的一种含磷氟硅超疏水阻燃棉织物,其特征在于:光敏性含磷氟聚合物、八乙烯基-POSS、1-羟环己基苯酮的摩尔比例为0.001~10:0.001~10:0.001~10;所述的第四溶剂和光敏性含磷氟聚合物的比例为5~1000mL:0.001~10mol。
4.根据权利要求2或3所述的一种含磷氟硅超疏水阻燃棉织物,其特征在于:所述第四溶剂为四氢呋喃、二氯甲烷和三氯甲烷中的一种。
5.根据权利要求2所述的一种含磷氟硅超疏水阻燃棉织物,其特征在于:处理方法为将棉织物浸渍于溶液中,升温至35~90℃,用紫外灯照射0.1~36h后取出棉织物,置于湿度为35%~100%的密闭环境中,待干燥后即得所述含磷氟硅超疏水阻燃织物。
6.一种含磷氟硅超疏水阻燃棉织物的制备方法,包括如下步骤:
1)向单口瓶中依次加入甲基丙烯酸羟乙酯、9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物DOPO、三乙胺、第一溶剂,所述甲基丙烯酸羟乙酯、DOPO和三乙胺的摩尔比为0.1~50:0.1~50:0.1~50;所述第一溶剂和甲基丙烯酸羟乙酯的比例为5~100mL:0.001~10mol;反应液在-10~100℃下反应2~36h,反应结束后用水萃取3~5次,取有机层旋蒸、干燥后即得含磷单体MA-DOPO;
2)向反应容器中依次加入甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、MA-DOPO、偶氮二异丁腈和第二溶剂,用液氮反复冻融若干次,充入氩气,在35~85℃下反应12~72h,继续向反应液中加入三乙胺和甲基丙烯酰氯,反应6~36h后用第三溶剂进行沉淀,所述甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、MA-DOPO、偶氮二异丁腈、三乙胺和甲基丙烯酰氯的摩尔比为0.1~50:0.1~50:0.1~50:0.01~50:0.1~50:0.1~50;所述第二溶剂、第三溶剂、甲基丙烯酸羟乙酯的比例为:1~50mL:1~1000mL:0.001~10mol;固液分离,固体部分用第三溶剂冲洗若干次后干燥,得到光敏性含磷氟聚合物,所述光敏性含磷氟聚合物如下结构式所示:
其中,x:y:z=0.01~0.99:0.01~0.99:0.01~0.99,其分子量为100~100000;
3)向反应容器中加入光敏性含磷氟聚合物、八乙烯基-POSS、1-羟环己基苯酮和第四溶剂,将棉织物浸渍于上述溶液中,升温至35~90℃,用紫外灯照射0.1~36h后取出棉织物,置于湿度为35%~100%的密闭环境中,待干燥后即得所述含磷氟硅超疏水阻燃织物。
7.根据权利要求6所述的一种含磷氟硅超疏水阻燃棉织物的制备方法,其特征在于:步骤1)所述第一溶剂为氯仿、二氯甲烷、三氯甲烷、四氯化碳中的至少一种。
8.根据权利要求6所述的一种含磷氟硅超疏水阻燃棉织物的制备方法,其特征在于:步骤2)所述第二溶剂为四氢呋喃、二氯甲烷、三氯甲烷、N,N-二甲基甲酰胺中的至少一种。
9.根据权利要求6所述的一种含磷氟硅超疏水阻燃棉织物的制备方法,其特征在于:所述第三溶剂为甲醇、乙醇、乙酸乙酯中的一种。
10.根据权利要求6-9任一项所述的一种含磷氟硅超疏水阻燃棉织物的制备方法,其特征在于:步骤3)所述第四溶剂为四氢呋喃、二氯甲烷和三氯甲烷中的一种。
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