CN113978053B - 一种环保耐磨汽车地毯及其制备方法 - Google Patents
一种环保耐磨汽车地毯及其制备方法 Download PDFInfo
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- CN113978053B CN113978053B CN202111527517.2A CN202111527517A CN113978053B CN 113978053 B CN113978053 B CN 113978053B CN 202111527517 A CN202111527517 A CN 202111527517A CN 113978053 B CN113978053 B CN 113978053B
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Abstract
本发明公开了一种环保耐磨汽车地毯及其制备方法,在制备时方案以亚麻布为外侧布料,在中层加入聚氨酯海绵,形成外层亚麻布、聚氨酯海绵、内层亚麻布的夹心结构,以形成复合面料;由于本方案用于制备汽车地毯,因此需要其具有较优异的耐磨、防水性,因此外侧布料选择耐磨性能、力学性能较为优异的亚麻布,而在中层掺入聚氨酯海绵,提高其弹性和使用时的舒适性,三者通过粘合剂层压复合,以形成汽车地毯面料,发明工艺操作简单,组分配比适宜,制备得到的汽车地毯面料具有较优异的阻燃性能,防水性优异,且面料的表面耐磨性能好,多次洗涤后面料依旧能保持较优异的综合性能,可应用汽车内铺装,实用性较好。
Description
技术领域
本发明涉及地毯技术领域,具体为一种环保耐磨汽车地毯及其制备方法。
背景技术
随着汽车工业的快速发展,人们对汽车的质量要求也不断提高,而纺织材料在汽车上的应用也逐渐增加,汽车地毯作为其中较为常用的汽车内饰,其使用性能也逐渐被我们关注,也对其提出了更高的要求。
现有市面上的汽车地毯的种类多样,其中采用亚麻面料制备的汽车地毯具有较优异的抗菌除臭性能,应用逐渐广泛,但其阻燃、防水性能依旧无法满足我们的需求,实际使用时较为不便。
基于上述情况,我们公开了一种环保耐磨汽车地毯及其制备方法,以解决该技术问题。
发明内容
本发明的目的在于提供一种环保耐磨汽车地毯及其制备方法,以解决上述背景技术中提出的问题。
为了解决上述技术问题,本发明提供如下技术方案:
一种环保耐磨汽车地毯的制备方法,包括以下步骤:
(1)取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,80~90℃下回流反应5~6h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;
取三氯氧磷、催化剂,混合均匀,60~65℃下加入三氯氧磷、对苯二酚混合物,保温反应,减压蒸馏除去三氯氧磷,得到阻燃中间体;
取物料A、二氯甲烷和吡啶,搅拌溶解,缓慢加入富马酸单苯甲酯单酰氯、阻燃中间体、二氯甲烷混合溶液,30~40℃下反应2~3h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;
(2)取乳化剂、甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、阻燃剂、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷和去离子水,乳化反应得到有机硅乳液;
取有机硅乳液,加入填料和增稠剂,搅拌30~40min,得到整理剂;
(3)取亚麻布和聚氨酯海绵,以外层亚麻布、聚氨酯海绵、内层亚麻布的顺序堆叠,通过粘合剂层压复合,得到预处理面料;
取预处理面料,通过整理剂表面整理,二浸二轧,烘干,得到成品。
较优化的方案,包括以下步骤:
(1)取富马酸单苯甲酯和氯化亚砜,混合均匀,75~80℃下回流反应2~3h,蒸除氯化亚砜,得到富马酸单苯甲酯单酰氯;
取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,80~90℃下回流反应5~6h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;
取三氯氧磷、催化剂,混合均匀,60~65℃下加入三氯氧磷、对苯二酚混合物,保温反应5~6h,减压蒸馏除去三氯氧磷,得到阻燃中间体;
取物料A、二氯甲烷和吡啶,搅拌溶解10~20min,缓慢加入富马酸单苯甲酯单酰氯、阻燃中间体、二氯甲烷混合溶液,30~40℃下反应2~3h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;
(2)取乳化剂和去离子水,混合均匀后加入甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯和1/2量的引发剂,搅拌10~15min,加入阻燃剂、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷和1/2量的引发剂,继续搅拌20~30min,剪切乳化10min,得到预乳化液;
取1/2量的预乳化液,在70~75℃下保温反应10~20min,加入剩余1/2量的预乳化液,升温至80~85℃,保温50~60min,得到有机硅乳液;
取有机硅乳液,加入填料和增稠剂,1800~2000r/min转速下搅拌30~40min,得到整理剂;
(3)取亚麻布和聚氨酯海绵,以外层亚麻布、聚氨酯海绵、内层亚麻布的顺序堆叠,通过粘合剂层压复合,得到预处理面料;
取预处理面料,通过整理剂表面整理,二浸二轧,80~90℃下烘干,得到成品。
较优化的方案,步骤(1)中,物料A、富马酸单苯甲酯单酰氯、阻燃中间体的摩尔比为3:1:1。
较优化的方案,步骤(2)中,单体包括甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷,所述引发剂为单体总质量的0.5~1%,所述乳化剂为单体总质量的2~3%;所述阻燃剂为单体总质量的4~6%。
较优化的方案,步骤(2)中,填料包括硼化钛、氮化硼和二氧化硅,所述硼化钛、氮化硼和二氧化硅的质量比为1:1:2;所述乳化剂包括十二烷基硫酸钠和司盘60,质量比为1:1。
较优化的方案,步骤(2)中,所述填料为有机硅乳液量的3~5wt%;所述增稠剂为有机硅乳液量的0.5~1wt%。
较优化的方案,步骤(3)中,层压温度为140~150℃,层压时间为70~80s,压力为2N×cm-2。
较优化的方案,步骤(3)中,外层亚麻布、聚氨酯海绵、内层亚麻布之间的施胶量均为25~30g×m-2。
较优化的方案,根据以上所述的一种环保耐磨汽车地毯的制备方法制备的地毯。
与现有技术相比,本发明所达到的有益效果是:
本发明公开了一种环保耐磨汽车地毯及其制备方法,在制备时方案以亚麻布为外侧布料,在中层加入聚氨酯海绵,形成外层亚麻布、聚氨酯海绵、内层亚麻布的夹心结构,以形成复合面料;由于本方案用于制备汽车地毯,因此需要其具有较优异的耐磨、防水性,因此外侧布料选择耐磨性能、力学性能较为优异的亚麻布,而在中层掺入聚氨酯海绵,提高其弹性和使用时的舒适性,三者通过粘合剂层压复合,以形成汽车地毯面料,实际使用时粘合剂选择为聚氨酯粘合剂。
在该方案基础上,为进一步提高产品的耐磨、防水性能,本申请改进了其表面整理工艺,以甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯为单体共聚,反应得到有机硅乳液,再加入填料、增稠剂,以制得整理剂,由于其中引入了甲基丙烯酸十二氟庚酯和乙烯基三乙氧基硅烷,因此该整理剂能够大幅提高地毯的防水防油性;同时,本方案中还引入了填料硼化钛、氮化硼,这两种填料均具有极高的硬度和耐磨性能,能够保证地毯面料的表面耐磨性。
进一步的,为提高地毯的综合性能,本申请还在整理剂中引入了阻燃剂,该阻燃剂通过席夫碱双酚、阻燃中间体、富马酸单苯甲酯单酰氯共聚反应制得,本申请先通过2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛反应,以形成席夫碱双酚,该席夫碱双酚能够与阻燃中间体、富马酸单苯甲酯单酰氯反应,不仅能够提高地毯面料的阻燃性能,还能够提高地毯面料的抗菌性,使得面料综合使用效果更为优异。
在本方案中,由于本申请在整理剂中引入了阻燃剂,而阻燃剂是在丙烯酸酯单体、有机硅单体共聚时掺杂的,因此为保证阻燃剂能够参与共聚,本申请限定了“物料A、富马酸单苯甲酯单酰氯、阻燃中间体的摩尔比为3:1:1”,在该摩尔比下,物料A即双酚中的羟基远超过阻燃中间体、富马酸单苯甲酯单酰氯的反应位点,并能够很好的与整理剂中的其他单体反应,能够提高地毯面料的耐久性,阻燃长效,实用性更为优异。
本发明公开了一种环保耐磨汽车地毯及其制备方法,工艺操作简单,组分配比适宜,通过制备的地毯面料为主体,与其他常规配件配合加工制备得到的汽车地毯面料具有较优异的阻燃性能,防水性优异,且面料的表面耐磨性能好,多次洗涤后面料依旧能保持较优异的综合性能,可应用汽车内铺装,实用性较好。
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:
一种环保耐磨汽车地毯的制备方法,包括以下步骤:
(1)取富马酸单苯甲酯和氯化亚砜,混合均匀,75℃下回流反应3h,蒸除氯化亚砜,得到富马酸单苯甲酯单酰氯;所述富马酸单苯甲酯和氯化亚砜的摩尔比为1:4;
取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,80℃下回流反应6h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;所述2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛摩尔比为1:2;
取三氯氧磷、催化剂无水三氯化铝,混合均匀,60℃下加入三氯氧磷、对苯二酚混合物,保温反应6h,减压蒸馏除去三氯氧磷,得到阻燃中间体;所述三氯氧磷与对苯二酚含量为:30ml:7g,催化剂含量为对苯二酚含量的0.01wt%。
取物料A、二氯甲烷和吡啶,搅拌溶解10min,缓慢加入富马酸单苯甲酯单酰氯、阻燃中间体、二氯甲烷混合溶液,30℃下反应3h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;物料A、富马酸单苯甲酯单酰氯、阻燃中间体的摩尔比为3:1:1,所述吡啶含量为物料A的50wt%。
(2)取乳化剂和去离子水,混合均匀后加入甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯和1/2量的引发剂,搅拌10min,加入阻燃剂、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷和1/2量的引发剂,继续搅拌20min,剪切乳化10min,得到预乳化液;
取1/2量的预乳化液,在70℃下保温反应20min,加入剩余1/2量的预乳化液,升温至80℃,保温60min,得到有机硅乳液;
单体包括甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷,所述引发剂总质量为单体总质量的1%,所述乳化剂为单体总质量的3%;所述阻燃剂为单体总质量的6%,所述甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷的质量比为2:1:1:1:2:1;所述乳化剂包括十二烷基硫酸钠和司盘60,质量比为1:1。
取有机硅乳液,加入填料和增稠剂,2000r/min转速下搅拌30min,得到整理剂;所述填料为有机硅乳液量的5wt%;所述增稠剂为有机硅乳液量的0.5wt%;填料包括硼化钛、氮化硼和二氧化硅,所述硼化钛、氮化硼和二氧化硅的质量比为1:1:2。
(3)取亚麻布和聚氨酯海绵,以外层亚麻布、聚氨酯海绵、内层亚麻布的顺序堆叠,通过粘合剂层压复合,外层亚麻布、聚氨酯海绵、内层亚麻布之间的施胶量均为30g×m-2。层压温度为140℃,层压时间为80s,压力为2N×cm-2;得到预处理面料;
取预处理面料,通过质量浓度为50g/L的整理剂表面整理,二浸二轧,80℃下烘干,得到成品。
实施例2:
一种环保耐磨汽车地毯的制备方法,包括以下步骤:
(1)取富马酸单苯甲酯和氯化亚砜,混合均匀,78℃下回流反应2.5h,蒸除氯化亚砜,得到富马酸单苯甲酯单酰氯;所述富马酸单苯甲酯和氯化亚砜的摩尔比为1:4;
取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,85℃下回流反应5.5h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;所述2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛摩尔比为1:2;
取三氯氧磷、催化剂无水三氯化铝,混合均匀,62℃下加入三氯氧磷、对苯二酚混合物,保温反应5.5h,减压蒸馏除去三氯氧磷,得到阻燃中间体;所述三氯氧磷与对苯二酚含量为:30ml:7g,催化剂含量为对苯二酚含量的0.01wt%。
取物料A、二氯甲烷和吡啶,搅拌溶解15min,缓慢加入富马酸单苯甲酯单酰氯、阻燃中间体、二氯甲烷混合溶液,35℃下反应2.5h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;物料A、富马酸单苯甲酯单酰氯、阻燃中间体的摩尔比为3:1:1,所述吡啶含量为物料A的50wt%。
(2)取乳化剂和去离子水,混合均匀后加入甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯和1/2量的引发剂,搅拌12min,加入阻燃剂、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷和1/2量的引发剂,继续搅拌25min,剪切乳化10min,得到预乳化液;
取1/2量的预乳化液,在72℃下保温反应15min,加入剩余1/2量的预乳化液,升温至82℃,保温55min,得到有机硅乳液;
单体包括甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷,所述引发剂总质量为单体总质量的1%,所述乳化剂为单体总质量的3%;所述阻燃剂为单体总质量的6%,所述甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷的质量比为2:1:1:1:2:1;所述乳化剂包括十二烷基硫酸钠和司盘60,质量比为1:1。
取有机硅乳液,加入填料和增稠剂,2000r/min转速下搅拌35min,得到整理剂;所述填料为有机硅乳液量的5wt%;所述增稠剂为有机硅乳液量的0.5wt%;填料包括硼化钛、氮化硼和二氧化硅,所述硼化钛、氮化硼和二氧化硅的质量比为1:1:2。
(3)取亚麻布和聚氨酯海绵,以外层亚麻布、聚氨酯海绵、内层亚麻布的顺序堆叠,通过粘合剂层压复合,外层亚麻布、聚氨酯海绵、内层亚麻布之间的施胶量均为30g×m-2。层压温度为140℃,层压时间为80s,压力为2N×cm-2;得到预处理面料;
取预处理面料,通过质量浓度为50g/L的整理剂表面整理,二浸二轧,80℃下烘干,得到成品。
实施例3:
一种环保耐磨汽车地毯的制备方法,包括以下步骤:
(1)取富马酸单苯甲酯和氯化亚砜,混合均匀,80℃下回流反应2h,蒸除氯化亚砜,得到富马酸单苯甲酯单酰氯;所述富马酸单苯甲酯和氯化亚砜的摩尔比为1:4;
取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,90℃下回流反应5h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;所述2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛摩尔比为1:2;
取三氯氧磷、催化剂无水三氯化铝,混合均匀,65℃下加入三氯氧磷、对苯二酚混合物,保温反应5h,减压蒸馏除去三氯氧磷,得到阻燃中间体;所述三氯氧磷与对苯二酚含量为:30ml:7g,催化剂含量为对苯二酚含量的0.01wt%。
取物料A、二氯甲烷和吡啶,搅拌溶解20min,缓慢加入富马酸单苯甲酯单酰氯、阻燃中间体、二氯甲烷混合溶液,40℃下反应2h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;物料A、富马酸单苯甲酯单酰氯、阻燃中间体的摩尔比为3:1:1,所述吡啶含量为物料A的50wt%。
(2)取乳化剂和去离子水,混合均匀后加入甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯和1/2量的引发剂,搅拌15min,加入阻燃剂、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷和1/2量的引发剂,继续搅拌30min,剪切乳化10min,得到预乳化液;
取1/2量的预乳化液,在75℃下保温反应10min,加入剩余1/2量的预乳化液,升温至85℃,保温50min,得到有机硅乳液;
单体包括甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷,所述引发剂总质量为单体总质量的1%,所述乳化剂为单体总质量的3%;所述阻燃剂为单体总质量的6%,所述甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷的质量比为2:1:1:1:2:1;所述乳化剂包括十二烷基硫酸钠和司盘60,质量比为1:1。
取有机硅乳液,加入填料和增稠剂,2000r/min转速下搅拌40min,得到整理剂;所述填料为有机硅乳液量的5wt%;所述增稠剂为有机硅乳液量的0.5wt%;填料包括硼化钛、氮化硼和二氧化硅,所述硼化钛、氮化硼和二氧化硅的质量比为1:1:2。
(3)取亚麻布和聚氨酯海绵,以外层亚麻布、聚氨酯海绵、内层亚麻布的顺序堆叠,通过粘合剂层压复合,外层亚麻布、聚氨酯海绵、内层亚麻布之间的施胶量均为30g×m-2。层压温度为140℃,层压时间为80s,压力为2N×cm-2;得到预处理面料;
取预处理面料,通过质量浓度为50g/L的整理剂表面整理,二浸二轧,80℃下烘干,得到成品。
对比例1:对比例1以实施例2为基础,对比例1中并未引入阻燃中间体,其余组分含量和工艺参数一致。
一种环保耐磨汽车地毯的制备方法,包括以下步骤:
(1)取富马酸单苯甲酯和氯化亚砜,混合均匀,78℃下回流反应2.5h,蒸除氯化亚砜,得到富马酸单苯甲酯单酰氯;所述富马酸单苯甲酯和氯化亚砜的摩尔比为1:4;
取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,85℃下回流反应5.5h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;所述2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛摩尔比为1:2;
取物料A、二氯甲烷和吡啶,搅拌溶解15min,缓慢加入富马酸单苯甲酯单酰氯、二氯甲烷混合溶液,35℃下反应2.5h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;物料A、富马酸单苯甲酯单酰氯为3:1,所述吡啶含量为物料A的50wt%。
对比例2:对比例2以实施例2为基础,对比例2中并未引入富马酸单苯甲酯单酰氯,其余组分含量和工艺参数一致。
一种环保耐磨汽车地毯的制备方法,包括以下步骤:
(1)取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,85℃下回流反应5.5h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;所述2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛摩尔比为1:2;
取三氯氧磷、催化剂无水三氯化铝,混合均匀,62℃下加入三氯氧磷、对苯二酚混合物,保温反应5.5h,减压蒸馏除去三氯氧磷,得到阻燃中间体;所述三氯氧磷与对苯二酚含量为:30ml:7g,催化剂含量为对苯二酚含量的0.01wt%。
取物料A、二氯甲烷和吡啶,搅拌溶解15min,缓慢加入阻燃中间体、二氯甲烷混合溶液,35℃下反应2.5h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;物料A、阻燃中间体的摩尔比为3:1,所述吡啶含量为物料A的50wt%。
对比例3:对比例3以实施例2为基础,对比例3中物料A、富马酸单苯甲酯单酰氯、阻燃中间体的摩尔比为3:2:2,其余组分含量和工艺参数一致。
一种环保耐磨汽车地毯的制备方法,包括以下步骤:
(1)取富马酸单苯甲酯和氯化亚砜,混合均匀,78℃下回流反应2.5h,蒸除氯化亚砜,得到富马酸单苯甲酯单酰氯;所述富马酸单苯甲酯和氯化亚砜的摩尔比为1:4;
取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,85℃下回流反应5.5h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;所述2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛摩尔比为1:2;
取三氯氧磷、催化剂无水三氯化铝,混合均匀,62℃下加入三氯氧磷、对苯二酚混合物,保温反应5.5h,减压蒸馏除去三氯氧磷,得到阻燃中间体;所述三氯氧磷与对苯二酚含量为:30ml:7g,催化剂含量为对苯二酚含量的0.01wt%。
取物料A、二氯甲烷和吡啶,搅拌溶解15min,缓慢加入富马酸单苯甲酯单酰氯、阻燃中间体、二氯甲烷混合溶液,35℃下反应2.5h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;物料A、富马酸单苯甲酯单酰氯、阻燃中间体的摩尔比为3:2:2,所述吡啶含量为物料A的50wt%。
对比例4:对比例4以实施例2为基础,对比例4中未引入硼化钛、氮化硼,其余组分含量和工艺参数一致。
一种环保耐磨汽车地毯的制备方法,包括以下步骤:
(1)取富马酸单苯甲酯和氯化亚砜,混合均匀,78℃下回流反应2.5h,蒸除氯化亚砜,得到富马酸单苯甲酯单酰氯;所述富马酸单苯甲酯和氯化亚砜的摩尔比为1:4;
取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,85℃下回流反应5.5h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;所述2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛摩尔比为1:2;
取三氯氧磷、催化剂无水三氯化铝,混合均匀,62℃下加入三氯氧磷、对苯二酚混合物,保温反应5.5h,减压蒸馏除去三氯氧磷,得到阻燃中间体;所述三氯氧磷与对苯二酚含量为:30ml:7g,催化剂含量为对苯二酚含量的0.01wt%。
取物料A、二氯甲烷和吡啶,搅拌溶解15min,缓慢加入富马酸单苯甲酯单酰氯、阻燃中间体、二氯甲烷混合溶液,35℃下反应2.5h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;物料A、富马酸单苯甲酯单酰氯、阻燃中间体的摩尔比为3:1:1,所述吡啶含量为物料A的50wt%。
(2)取乳化剂和去离子水,混合均匀后加入甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯和1/2量的引发剂,搅拌12min,加入阻燃剂、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷和1/2量的引发剂,继续搅拌25min,剪切乳化10min,得到预乳化液;
取1/2量的预乳化液,在72℃下保温反应15min,加入剩余1/2量的预乳化液,升温至82℃,保温55min,得到有机硅乳液;
单体包括甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷,所述引发剂总质量为单体总质量的1%,所述乳化剂为单体总质量的3%;所述阻燃剂为单体总质量的6%,所述甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷的质量比为2:1:1:1:2:1;所述乳化剂包括十二烷基硫酸钠和司盘60,质量比为1:1。
取有机硅乳液,加入填料和增稠剂,2000r/min转速下搅拌35min,得到整理剂;所述填料为有机硅乳液量的5wt%;所述增稠剂为有机硅乳液量的0.5wt%;填料包括二氧化硅。
(3)取亚麻布和聚氨酯海绵,以外层亚麻布、聚氨酯海绵、内层亚麻布的顺序堆叠,通过粘合剂层压复合,外层亚麻布、聚氨酯海绵、内层亚麻布之间的施胶量均为30g×m-2。层压温度为140℃,层压时间为80s,压力为2N×cm-2;得到预处理面料;
取预处理面料,通过质量浓度为50g/L的整理剂表面整理,二浸二轧,80℃下烘干,得到成品。
检测实验:
(1)取实施例1-3、对比例1-4制备的地毯,进行以下性能测试:
耐磨性:取实施例1-3、对比例1-4制备的地毯,根据GB/T21196.2-2007《纺织品马丁代尔法织物耐磨性的测定第2部分:试样破损的测定》,测试时载荷为1600g。
防水性:取实施例1-3、对比例1-4制备的地毯,根据DB44/T1872-2016《纺织品表面润湿性能的测定接触角法》检测其表面静态水接触角,测试时共测试5次,取平均值并记录。
阻燃:取实施例1-3、对比例1-4制备的地毯,根据GB-T5454-1997《纺织品燃烧性能试验氧指数法》测试,记录地毯面料的极限氧指数。
抗菌:取实施例1-3、对比例1-4制备的地毯,根据GB/T20944.3-2008震荡法检测地毯的抗菌性能,并计算抑菌率,检测菌种为大肠杆菌。
(2)取实施例2、对比例1-4制备的地毯,根据GB/T12490—2014《纺织品色牢度试验耐家庭和商业洗涤色牢度》中规定的方法洗涤30次,洗涤时皂液浓度为3g/L,浴比为1:20,温度为28℃,洗涤时间为10min。
重新依据上述方法检测其性能。
结论:本发明公开了一种环保耐磨汽车地毯及其制备方法,工艺操作简单,组分配比适宜,制备得到的汽车地毯面料具有较优异的阻燃性能,防水性优异,且面料的表面耐磨性能好,多次洗涤后面料依旧能保持较优异的综合性能,可应用汽车内铺装,实用性较好。
最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种环保耐磨汽车地毯的制备方法,其特征在于:包括以下步骤:
(1)取富马酸单苯甲酯和氯化亚砜,混合均匀,75~80℃下回流反应2~3h,蒸除氯化亚砜,得到富马酸单苯甲酯单酰氯;
取2,2'-二氨基-4,4'-双噻唑和四羟基苯甲醛,乙醇溶解均匀,80~90℃下回流反应5~6h,反应结束后去离子水沉淀,过滤洗涤,真空干燥,得到物料A;
取三氯氧磷、催化剂,混合均匀,60~65℃下加入三氯氧磷、对苯二酚混合物,保温反应5~6h,减压蒸馏除去三氯氧磷,得到阻燃中间体;
取物料A、二氯甲烷和吡啶,搅拌溶解10~20min,缓慢加入富马酸单苯甲酯单酰氯、阻燃中间体、二氯甲烷混合溶液,30~40℃下反应2~3h,反应后水萃取除去吡啶盐酸盐,减压蒸馏除去二氯甲烷,得到阻燃剂;
(2)取乳化剂和去离子水,混合均匀后加入甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯和1/2量的引发剂,搅拌10~15min,加入阻燃剂、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷和1/2量的引发剂,继续搅拌20~30min,剪切乳化10min,得到预乳化液;
取1/2量的预乳化液,在70~75℃下保温反应10~20min,加入剩余1/2量的预乳化液,升温至80~85℃,保温50~60min,得到有机硅乳液;
取有机硅乳液,加入填料和增稠剂,1800~2000r/min转速下搅拌30~40min,得到整理剂;
(3)取亚麻布和聚氨酯海绵,以外层亚麻布、聚氨酯海绵、内层亚麻布的顺序堆叠,通过粘合剂层压复合,得到预处理面料;
取预处理面料,通过整理剂表面整理,二浸二轧,80~90℃下烘干,得到成品;
其中步骤(1)中,物料A、富马酸单苯甲酯单酰氯、阻燃中间体的摩尔比为3:1:1;步骤(2)中,填料包括硼化钛、氮化硼和二氧化硅,所述硼化钛、氮化硼和二氧化硅的质量比为1:1:2;所述乳化剂包括十二烷基硫酸钠和司盘60,质量比为1:1。
2.根据权利要求1所述的一种环保耐磨汽车地毯的制备方法,其特征在于:步骤(2)中,单体包括甲基丙烯酸甲酯、丙烯酸丁酯、甲基丙烯酸羟乙酯、甲基丙烯酸十二氟庚酯、乙烯基三乙氧基硅烷,所述引发剂为单体总质量的0.5~1%,所述乳化剂为单体总质量的2~3%;所述阻燃剂为单体总质量的4~6%。
3.根据权利要求1所述的一种环保耐磨汽车地毯的制备方法,其特征在于:步骤(2)中,所述填料为有机硅乳液量的3~5wt%;所述增稠剂为有机硅乳液量的0.5~1wt%。
4.根据权利要求1所述的一种环保耐磨汽车地毯的制备方法,其特征在于:步骤(3)中,层压温度为140~150℃,层压时间为70~80s。
5.根据权利要求1~4中任一项所述的一种环保耐磨汽车地毯的制备方法制备的地毯。
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