CN107236407B - 阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法 - Google Patents

阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法 Download PDF

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CN107236407B
CN107236407B CN201710423865.2A CN201710423865A CN107236407B CN 107236407 B CN107236407 B CN 107236407B CN 201710423865 A CN201710423865 A CN 201710423865A CN 107236407 B CN107236407 B CN 107236407B
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乐建军
姜慧
向宇
黄娇
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Fujian Zhongyu New Material Technology Co., Ltd
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Abstract

本发明公开了阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法,采用聚四氢呋喃醚二醇80g与二苯基甲烷二异氰酸酯45g混合,在催化剂0.12g存在的条件下,于85℃下反应2h,聚氨酯预聚体;向聚氨酯预聚体中加入4‑氨基‑5‑羟基‑2,7‑萘二磺酸3.5g、甘露醇3.5g和N‑羟甲基丙烯酰胺3.2g,在80℃下同时滴加10%的引发剂水溶液5.3g和鸡毛水解液6.6g,滴加时间1h,滴加完保温反应2h,反应结束,调节pH到7.5,得到阻燃性热塑性聚氨酯;将阻燃性聚氨酯树脂60份、丁酮15份、HDI三聚体固化剂、异辛酸铋促进剂按比例搅拌均匀配成无色高透明浆料,所得合成革浆料具有良好的阻燃、耐磨耗和真皮感。

Description

阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法
技术领域
本发明涉及到一种合成革的制备方法,尤其是一种阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法。
背景技术
聚氨酯合成革具有光泽柔和、自然,手感柔软,真皮感强,耐扰曲,抗老化等优异的特点,是天然皮革的最为理想的替代品,广泛用于服装,制鞋,箱包,家具等行业,但是目前市场上的聚氨酯合成革在透湿性,耐磨性能方面与天然皮革差距太大,透湿性能差的聚氨酯合成革制品会令人感觉闷热、湿冷,针对这些缺点,目前主要通过改变聚氨酯合成革浆料的性能进行改善,但目前市场上改变聚氨酯合成革浆料透湿性和耐磨性的工艺较复杂,成本较高,效果不明显。
传统聚氨酯合成中使用二月桂酸二丁基锡,但由于在合成过程中,难以将其取出,造成不必要的安全隐患,因此需要寻找合适的催化剂。
传统的阻燃聚氨酯的阻燃性经常用施加阻燃剂的方式,而阻燃剂分为添加型和反应型两种,添加型用量大,效率高,反应型的阻燃剂相对较少,如”201410470376.9一种无卤阻燃热塑性聚氨酯”将热塑性聚氨酯90克原料在80℃鼓风干燥2h,然后将10克的5-(4-羟基苯基)-2H-吡喃-2-酮在90℃下干燥3小时,混合在一起,并加入7克的1098、5克的EBS、2克的A3800和0 .3克的二甲基硅油,在高速混合机SHR-50A中在1500rpm的转速下高速搅拌5分钟,停止搅拌,转移到双螺杆挤出机TSAE-35A中,进行熔融共混,挤出机1-4段温度分别是140、150、160、165℃,挤出物切粒后80℃干燥4h备用。因此需要找到适合的提高阻燃效率的材料。
据统计,全世界每年产生的鸡毛等禽类羽毛废弃物达500万吨左右。这些废弃羽毛只有少量被制成枕芯、被垫、羽毛扇、羽毛球等,大部分被当作垃圾直接丢弃,不但造成环境污染,还会给人体健康造成危害。而且,废弃羽毛的主要成分为角蛋白,在土壤中不易自行降解,不能直接作为有机肥料使用。而如果能利用角蛋白对聚氨酯改性,提高聚氨酯的真皮感,是一种好的办法。
发明内容
传统的聚氨酯合成革浆料所成膜存在着耐磨性、阻燃性差,而且涂饰在合成革上,降低了合成革的真皮感,本发明采用4-氨基-5-羟基-2,7-萘二磺酸为扩链剂,以甘露醇提高扩链效果,以N-羟甲基丙烯酰胺为聚氨酯预聚体中引入双键,在自制的引发剂条件下与四氟乙烯、偏二氟乙烯反应,来提高聚氨酯合成革的耐磨性,采用三氟甲基苯胺、对硝基苄醇丙二酸单酯镁、四丁基溴化铵、四乙基溴化铵为催化剂,取代传统的二月桂酸二丁基锡,降低重金属的毒性,同时筛选成炭促进剂,提高聚氨酯的阻燃性,而自制鸡毛水解液,加入到聚氨酯合成革浆料中,提高聚氨酯的真皮革。
阻燃、耐磨耗、仿真皮感的合成革浆料的的制备方法,其特征在于:
(1)阻燃性热塑性聚氨酯制备:在装有搅拌浆、温度计、冷凝管 500ml 的四口烧瓶中,将聚四氢呋喃醚二醇 80g 与二苯基甲烷二异氰酸酯 45g 混合,在催化剂0.12g 存在的条件下,于85℃下反应 2h,聚氨酯预聚体;向聚氨酯预聚体中加入4-氨基-5-羟基-2,7-萘二磺酸3.5g、甘露醇3.5g和N-羟甲基丙烯酰胺3.2g,于85℃反应 3h,加入成炭促进剂2.4g,于70℃反应 1h,加入三乙胺 9g 进行中和反应 60min,在高速搅拌下加入去离子水100g进行乳化分散,并向体系中加入四氟乙烯3.1g、偏二氟乙烯1.6g和二乙酸碘苯1.5g,在80℃下同时滴加质量分数10%的引发剂水溶液5.3g、鸡毛水解液6.6g和六甲基环三硅氧烷2.3g,滴加时间1h,滴加完保温反应2h,反应结束,调节pH到7.5,,得到阻燃性热塑性聚氨酯。
(2)将阻燃性聚氨酯树脂60份、丁酮25份、HDI三聚体固化剂9g、异辛酸铋促进剂6g按比例搅拌均匀配成无色高透明浆料。
其催化剂为对三氟甲基苯胺、对硝基苄醇丙二酸单酯镁、四丁基溴化铵、四乙基溴化铵、异丙基三(焦磷酸二辛酯)钛酸酯、1,4-双(二苯基膦)丁烷、马来酸二苄酯、丙二酸二苄酯中的任意一种。
成炭促进剂为钛酸四异丙酯、乙酸锆、十二羰基三铁、苯基三乙氧基硅烷、甲基四氢苯酐、三羟甲基丙烷的任意一种。
鸡毛水解液的制备工艺为:称取经过十二烷基苯磺酸钠洗净、烘燥后的鸡毛10.3g于500ml反应器中,同时加入去离子水150ml及质量分数为37%的盐酸1.5ml,控制温度80℃,反应4h,使鸡毛充分溶胀;将反应器中的盐酸溶液过滤,用去离子水分三次冲洗溶胀后的鸡毛,将酸洗净;称取NaHSO3粉末2.6g,溶解于150ml的去离子水中,然后转移至反应器中,设定温度为80℃,反应4h;称取3.2g的氢氧化钠,加入反应器中,反应2h,十分钟内溶液变成褐黄色;将水解后的溶液离心、过滤,旋转蒸发浓缩至原溶液的一半,即为鸡毛水解液。
引发剂由下列步骤制备而成:在烧瓶中加入60g的 N-甲基咪唑、1,4-丁磺酸内酯30g、甲苯25g和环己基甲基二甲氧基硅烷5g,70 ℃恒温反应 3h,80℃烘干得到物质A粉末;冰浴条件下向物质A中缓慢加入质量分数37%的浓盐酸15g,,再加入2,4-二叔丁基苯酚0.29g,70 ℃下反应 12 h,得到粘稠状液体状的引发剂。
本发明的优势在于
(1)采用4-氨基-5-羟基-2,7-萘二磺酸为扩链剂,以甘露醇提高扩链效果,以N-羟甲基丙烯酰胺为聚氨酯预聚体中引入双键,在自制的引发剂条件下与四氟乙烯、偏二氟乙烯反应,来提高聚氨酯合成革的耐磨性;
(2)采用三氟甲基苯胺、对硝基苄醇丙二酸单酯镁、四丁基溴化铵、四乙基溴化铵为催化剂,取代传统的二月桂酸二丁基锡,降低重金属的毒性;
(3)自制鸡毛水解液,加入到聚氨酯合成革浆料中,提高聚氨酯的真皮革;
(4)筛选成炭促进剂,提高聚氨酯的阻燃性;
(5)六甲基环三硅氧烷适当增加鸡毛水解液在膜中的柔软性;
(6)异辛酸铋促进剂购买于淄博新正环境科技有限公司。
(7)本发明所用的其他原料只要是主要成份相同即可。
实施方式
实例1
(1)阻燃性热塑性聚氨酯制备:在装有搅拌浆、温度计、冷凝管 500ml 的四口烧瓶中,将聚四氢呋喃醚二醇 80g 与二苯基甲烷二异氰酸酯 45g 混合,在三氟甲基苯胺0.12g存在的条件下,于85℃下反应 2h,聚氨酯预聚体;向聚氨酯预聚体中加入4-氨基-5-羟基-2,7-萘二磺酸3.5g、甘露醇3.5g和N-羟甲基丙烯酰胺3.2g,于85℃反应 3h,加入钛酸四异丙酯2.4g,于70℃反应 1h,加入三乙胺 9g 进行中和反应 60min,在高速搅拌下加入去离子水100g进行乳化分散,并向体系中加入四氟乙烯3.1g、偏二氟乙烯1.6g二乙酸碘苯1.5g,在80℃下同时滴加10%的引发剂水溶液5.3g(将下述引发剂作为单一物质计算)和鸡毛水解液6.6g和六甲基环三硅氧烷2.3g,滴加时间1h,滴加完保温反应2h,反应结束,调节pH到7.5,得到阻燃性热塑性聚氨酯。
(2)将阻燃性聚氨酯树脂60kg、丁酮25份、HDI三聚体固化剂9g(德国拜耳bayerN3390)、异辛酸铋促进剂6g按比例搅拌均匀配成无色高透明浆料;
鸡毛水解液的制备工艺为:称取经过十二烷基苯磺酸钠洗净、烘燥后的鸡毛10.3g于500ml反应器中,同时加入去离子水150ml及质量分数为37%的盐酸1.5ml,控制温度80℃,反应4h,使鸡毛充分溶胀;将反应器中的盐酸溶液过滤,用去离子水分三次冲洗溶胀后的鸡毛,将酸洗净;称取NaHSO3粉末2.6g,溶解于150ml的去离子水中,然后转移至反应器中,反应温度为80℃,反应4h;称取3.2g的氢氧化钠,加入反应器中,反应2h,十分钟内溶液变成褐黄色;将水解后的溶液离心、过滤,旋转蒸发浓缩至原溶液的一半,即为所需鸡毛水解液;
引发剂由下列步骤制备而成:在烧瓶中加入60g的 N-甲基咪唑、1,4-丁磺酸内酯30g、甲苯25g和环己基甲基二甲氧基硅烷5g,70 ℃恒温反应 3h,80℃烘干得到物质A粉末;冰浴条件下向物质A中缓慢加入质量分数37%的浓盐酸15g,滴加完毕,再加入2,4-二叔丁基苯酚0.29g,70 ℃下反应 12 h,得到粘稠状液体状的引发剂。
实例2
(1)阻燃性热塑性聚氨酯制备:在装有搅拌浆、温度计、冷凝管 500ml 的四口烧瓶中,将聚四氢呋喃醚二醇 80g 与二苯基甲烷二异氰酸酯 45g 混合,在对硝基苄醇丙二酸单酯镁0.12g 存在的条件下,于85℃下反应 2h,聚氨酯预聚体;向聚氨酯预聚体中加入4-氨基-5-羟基-2,7-萘二磺酸3.5g、甘露醇3.5g和N-羟甲基丙烯酰胺3.2g,于85℃反应 3h,加入乙酸锆2.4g,于70℃反应 1h,加入三乙胺 9g 进行中和反应 60min,在高速搅拌下加入去离子水100g进行乳化分散,并向体系中加入四氟乙烯3.1g、偏二氟乙烯1.6g二乙酸碘苯1.5g,在80℃下同时滴加10%的引发剂水溶液5.3g和鸡毛水解液6.6g和六甲基环三硅氧烷2.3g,滴加时间1h,滴加完保温反应2h,反应结束,调节pH到7.5,得到阻燃性热塑性聚氨酯;
(2)将阻燃性聚氨酯树脂60kg、丁酮25份、HDI三聚体固化剂9g(德国拜耳bayerN3390)、异辛酸铋促进剂6g按比例搅拌均匀配成无色高透明浆料;
鸡毛水解液的制备工艺为:称取经过十二烷基苯磺酸钠洗净、烘燥后的鸡毛10.3g于500ml反应器中,同时加入去离子水150ml及质量分数为37%的盐酸1.5ml,控制温度80℃,反应4h,使鸡毛充分溶胀;将反应器中的盐酸溶液过滤,用去离子水分三次冲洗溶胀后的鸡毛,将酸洗净;称取NaHSO3粉末2.6g,溶解于150ml的去离子水中,然后转移至反应器中,反应温度为80℃,反应4h;称取3.2g的氢氧化钠,加入反应器中,反应2h,十分钟内溶液变成褐黄色;将水解后的溶液离心、过滤,旋转蒸发浓缩至原溶液的一半,即为所需鸡毛水解液;
引发剂由下列步骤制备而成:在烧瓶中加入60g的 N-甲基咪唑、1,4-丁磺酸内酯30g、甲苯25g和环己基甲基二甲氧基硅烷5g,70 ℃恒温反应 3h,80℃烘干得到物质A粉末;冰浴条件下向物质A中缓慢加入质量分数37%的浓盐酸15g,滴加完毕,再加入2,4-二叔丁基苯酚0.29g,70 ℃下反应 12 h,得到粘稠状液体状的引发剂。
实例3
(1)阻燃性热塑性聚氨酯制备:在装有搅拌浆、温度计、冷凝管 500ml 的四口烧瓶中,将聚四氢呋喃醚二醇 80g 与二苯基甲烷二异氰酸酯 45g 混合,在马来酸二苄酯0.12g存在的条件下,于85℃下反应 2h,聚氨酯预聚体;向聚氨酯预聚体中加入4-氨基-5-羟基-2,7-萘二磺酸3.5g、甘露醇3.5g和N-羟甲基丙烯酰胺3.2g,于85℃反应 3h,加入苯基三乙氧基硅烷2.4g,于70℃反应 1h,加入三乙胺 9g 进行中和反应 60min,在高速搅拌下加入去离子水100g进行乳化分散,并向体系中加入四氟乙烯3.1g、偏二氟乙烯1.6g二乙酸碘苯1.5g,在80℃下同时滴加10%的引发剂水溶液5.3g和鸡毛水解液6.6g和六甲基环三硅氧烷2.3g,滴加时间1h,滴加完保温反应2h,反应结束,调节pH到7.5,得到阻燃性热塑性聚氨酯。
(2)将阻燃性聚氨酯树脂60kg、丁酮25份、HDI三聚体固化剂9g(德国拜耳bayerN3390)、异辛酸铋促进剂6g按比例搅拌均匀配成无色高透明浆料。
鸡毛水解液的制备工艺为:称取经过十二烷基苯磺酸钠洗净、烘燥后的鸡毛10.3g于500ml反应器中,同时加入去离子水150ml及质量分数为37%的盐酸1.5ml,控制温度80℃,反应4h,使鸡毛充分溶胀;将反应器中的盐酸溶液过滤,用去离子水分三次冲洗溶胀后的鸡毛,将酸洗净;称取NaHSO3粉末2.6g,溶解于150ml的去离子水中,然后转移至反应器中,反应温度为80℃,反应4h;称取3.2g的氢氧化钠,加入反应器中,反应2h,十分钟内溶液变成褐黄色;将水解后的溶液离心、过滤,旋转蒸发浓缩至原溶液的一半,即为所需鸡毛水解液;
引发剂由下列步骤制备而成:在烧瓶中加入60g的 N-甲基咪唑、1,4-丁磺酸内酯30g、甲苯25g和环己基甲基二甲氧基硅烷5g,70 ℃恒温反应 3h,80℃烘干得到物质A粉末;冰浴条件下向物质A中缓慢加入质量分数37%的浓盐酸15g,滴加完毕,再加入2,4-二叔丁基苯酚0.29g,70 ℃下反应 12 h,得到粘稠状液体状的引发剂。
实例4
(1)阻燃性热塑性聚氨酯制备:在装有搅拌浆、温度计、冷凝管 500ml 的四口烧瓶中,将聚四氢呋喃醚二醇 80g 与二苯基甲烷二异氰酸酯 45g 混合,在丙二酸二苄酯0.12g存在的条件下,于85℃下反应 2h,聚氨酯预聚体;向聚氨酯预聚体中加入4-氨基-5-羟基-2,7-萘二磺酸3.5g、甘露醇3.5g和N-羟甲基丙烯酰胺3.2g,于85℃反应 3h,加入十二羰基三铁2.4g,于70℃反应 1h,加入三乙胺 9g 进行中和反应 60min,在高速搅拌下加入去离子水100g进行乳化分散,并向体系中加入四氟乙烯3.1g、偏二氟乙烯1.6g二乙酸碘苯1.5g,在80℃下同时滴加10%的引发剂水溶液5.3g和鸡毛水解液6.6g和六甲基环三硅氧烷2.3g,滴加时间1h,滴加完保温反应2h,反应结束,调节pH到7.5,得到阻燃性热塑性聚氨酯;
(2)将阻燃性聚氨酯树脂60kg、丁酮25份、HDI三聚体固化剂9g(德国拜耳bayerN3390)、异辛酸铋促进剂6g按比例搅拌均匀配成无色高透明浆料。
鸡毛水解液的制备工艺为:称取经过十二烷基苯磺酸钠洗净、烘燥后的鸡毛10.3g于500ml反应器中,同时加入去离子水150ml及质量分数为37%的盐酸1.5ml,控制温度80℃,反应4h,使鸡毛充分溶胀;将反应器中的盐酸溶液过滤,用去离子水分三次冲洗溶胀后的鸡毛,将酸洗净;称取NaHSO3粉末2.6g,溶解于150ml的去离子水中,然后转移至反应器中,反应温度为80℃,反应4h;称取3.2g的氢氧化钠,加入反应器中,反应2h,十分钟内溶液变成褐黄色;将水解后的溶液离心、过滤,旋转蒸发浓缩至原溶液的一半,即为所需鸡毛水解液;
引发剂由下列步骤制备而成:在烧瓶中加入60g的 N-甲基咪唑、1,4-丁磺酸内酯30g、甲苯25g和环己基甲基二甲氧基硅烷5g,70 ℃恒温反应 3h,80℃烘干得到物质A粉末;冰浴条件下向物质A中缓慢加入质量分数37%的浓盐酸15g,滴加完毕,再加入2,4-二叔丁基苯酚0.29g,70 ℃下反应 12 h,得到粘稠状液体状的引发剂。
为了更准确的说明所得浆料的性质,将所得浆料成膜,测定其性质,真皮感采用的是将浆料喷在合成革表面,找五名富有经验的工程师手摸进行现场评估。
表1 真皮感数据
实例1 实例2 实例3 实例4 普通的聚氨酯浆料
真皮感 有真皮感 有真皮感 有真皮感 有真皮感 塑感强
柔软性
普通的聚氨酯浆料(采用东莞米人占化工有限公司的柔软皮革用高光水性聚氨酯树脂)
表2 未加鸡毛水解液的性质
实例1 实例2 实例3 实例4 普通的聚氨酯浆料
真皮感 塑感强 塑感强 塑感强 塑感强 塑感强
柔软性
表3 未加入六甲基环三硅氧烷所成膜的性质
实例1 实例2 实例3 实例4
真皮感 有真皮感 有真皮感 有真皮感 有真皮感
柔软性 表面发硬 表面发硬 表面发硬 表面稍微发硬
表4 膜的阻燃性能
实例1 实例2 实例3 实例4 普通的聚氨酯浆料
氧指数/% 27.8 28.6 28.9 29.2 23.1
最大烟密度/% 12 15 8 7 89
有焰燃烧时间/s 3.8 5.3 2.1 4.5 15.7.
无焰燃烧时间/s 0 0 0 0 0
表5未加成炭促进剂所成膜的阻燃性能
实例1 实例2 实例3 实例4
氧指数/% 24.2 25.2 24.6 23.8
最大烟密度/% 35 45 21 23
有焰燃烧时间/s 5.2 12.3 5.1 4.2
无焰燃烧时间/s 2.3 5.3 4.2 2.6
各项指标的检测分别依据如下标准:烟密度依据 GB8323-2008 来测定,氧指数采用 GB/T5454-1997《纺织品燃烧性能试验 - 氧指数法》测定;有焰燃烧时间和无焰燃烧时间是由 GB/T 5455-1997《纺织品燃烧能试验 - 垂直法》来测定。
表6未加催化剂所成膜的阻燃性能
实例1 实例2 实例3 实例4
氧指数/% 22.2 23.5 22.8 23.3
最大烟密度/% 62 56 57 46
有焰燃烧时间/s 6.2 12.2 6.1 7.8
无焰燃烧时间/s 1.0 1.3 0.8 3.2
表7聚氨酯所成膜的耐磨耗性
实例1 实例2 实例3 实例4
耐磨耗性/mg 18 12 14 16
未加引发剂的耐磨性/mg 25 31 26 28
未加四氟乙烯和偏二氟乙烯耐磨性/mg 35 38 39 41
未加二乙酸碘苯的耐磨性/mg 34 33 37 45
普通聚氨酯的耐磨性为27mg。
参考QB/T 2780-2006标准测定鞋面用聚氨酯人造革的耐磨耗性的标准进行测试。未加那个只是表明实例在未加上述物质,其他原料都存在下进行测试,本领域技术人员都会理解。
本发明应用了具体个例对本发明的原理及实施方式进行了阐述,以上实施例的说明只是用于帮助理解本发明的方法及其核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求的保护范围内。

Claims (5)

1.阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法,其特征在于:
(1)阻燃性热塑性聚氨酯制备:在装有搅拌浆、温度计、冷凝管 500ml的四口烧瓶中,将聚四氢呋喃醚二醇 80g 与二苯基甲烷二异氰酸酯 45g 混合,在催化剂0.12g 存在的条件下,于85℃下反应 2h,聚氨酯预聚体;向聚氨酯预聚体中加入4-氨基-5-羟基-2,7-萘二磺酸3.5g、甘露醇3.5g和N-羟甲基丙烯酰胺3.2g,于85℃反应 3h,加入成炭促进剂2.4g,于70℃反应 1h,加入三乙胺 9g 进行中和反应 60min,在高速搅拌下加入去离子水100g进行乳化分散,并向体系中加入四氟乙烯3.1g、偏二氟乙烯1.6g和二乙酸碘苯1.5g,在80℃下同时滴加质量分数10%的引发剂水溶液5.3g、鸡毛水解液6.6g和六甲基环三硅氧烷2.3g,滴加时间1h,滴加完保温反应2h,反应结束,调节pH到7.5,得到阻燃性热塑性聚氨酯;
(2)将阻燃性聚氨酯树脂60kg、丁酮25kg、HDI三聚体固化剂9g、异辛酸铋促进剂6g按比例搅拌均匀配成无色高透明浆料。
2.如权利要求1所述的阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法,其催化剂为对三氟甲基苯胺、对硝基苄醇丙二酸单酯镁、四丁基溴化铵、四乙基溴化铵、异丙基三(焦磷酸二辛酯)钛酸酯、1,4-双(二苯基膦)丁烷、马来酸二苄酯、丙二酸二苄酯中的任意一种。
3.如权利要求1所述的阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法,其成炭促进剂为钛酸四异丙酯、乙酸锆、十二羰基三铁、苯基三乙氧基硅烷、甲基四氢苯酐、三羟甲基丙烷的任意一种。
4.如权利要求1所述的阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法,鸡毛水解液的制备工艺为:称取经过十二烷基苯磺酸钠洗净、烘燥后的鸡毛10.3g于500ml反应器中,同时加入去离子水150ml及质量分数为37%的盐酸1.5ml,控制温度80℃,反应4h,使鸡毛充分溶胀;将反应器中的盐酸溶液过滤,用去离子水分三次冲洗溶胀后的鸡毛,将酸洗净;称取NaHSO3粉末2.6g,溶解于150ml的去离子水中,然后转移至反应器中,设定温度为80℃,反应4h;称取3.2g的氢氧化钠,加入反应器中,反应2h,十分钟内溶液变成褐黄色;将水解后的溶液离心、过滤,旋转蒸发浓缩至原溶液的一半,即为鸡毛水解液。
5.如权利要求1所述的阻燃、耐磨耗、仿真皮感的合成革浆料的制备方法,其引发剂由下列步骤制备而成:在烧瓶中加入60g的 N-甲基咪唑、1,4-丁磺酸内酯30g、甲苯25g和环己基甲基二甲氧基硅烷5g,70 ℃恒温反应 3h,80℃烘干得到物质A粉末;冰浴条件下向物质A中缓慢加入质量分数37%的浓盐酸15g,再加入2,4-二叔丁基苯酚0.29g,70 ℃下反应 12h,得到粘稠状液体状的引发剂。
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