CN108951164A - 一种纯棉织物用阻燃整理剂及其制备方法 - Google Patents
一种纯棉织物用阻燃整理剂及其制备方法 Download PDFInfo
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- CN108951164A CN108951164A CN201810572276.5A CN201810572276A CN108951164A CN 108951164 A CN108951164 A CN 108951164A CN 201810572276 A CN201810572276 A CN 201810572276A CN 108951164 A CN108951164 A CN 108951164A
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Abstract
本发明公开了一种纯棉织物用阻燃整理剂及其制备方法,包括以下步骤:将制备的聚氨酯乳液加水稀释后,加入阻燃增效剂,表面活性剂以及羟甲基纤维素,控制温度为50‑60℃,搅拌1‑2h后,去除气泡后制得所述纯棉织物用阻燃整理剂。纯棉织物经本申请的环保阻燃整理剂整理过后,具有良好的防燃性,并且织物的手感不会变的僵硬,长时间使用和洗涤后仍能保持良好的防燃性能。
Description
技术领域
本发明涉及纺织助剂领域,特别是一种纯棉织物用阻燃整理剂及其制备方法。
背景技术
近年来由纺织品引起的火灾以及死亡率日渐增多,已经远远超过了其他原因引起的火灾,约占世界总火灾量的50%,因此纺织品的阻燃引起了人们的广泛关注。棉织物具有优良的吸湿透气性,手感柔软,良好的染色性以及可完全生物降解等特点,已经被广泛应用于人们的日常生活中,成为了不可替代的纺织品。棉纤维主要成分是纤维素,纤维素是一种天然的有机化合物,有许多脱水的β-葡萄糖组成,一般和木质素、天然树脂、半纤维素等混合在一起。但是棉纤维为可燃性纤维,其极限氧指数仅为18.0,为易燃纤维,因此对棉织物进行阻燃整理具有重要的意义。
棉纤维的燃烧与引燃源和氧气有关,当纤维素受热分解时会产生左旋葡萄糖,左旋葡萄糖继续脱水生成焦油、可燃气体等。随着上一步生成的易燃性气体的燃烧,促使焦油等分解成为更多的易燃性产物,后者继续燃烧,形成碳渣。尽管经过阻燃剂整理后棉纤维的残碳与未阻燃整理的棉纤维相同,但是经过阻燃剂整理后的棉纤维燃烧后的石墨化炭明显多于未经阻燃的,说明阻燃剂经过促进称叹,阻碍继续燃烧,最终可以起到阻燃的作用。
目前使用较广泛的阻燃整理剂主要有含卤阻燃剂、含磷阻燃剂、含氮阻燃剂、含硼阻燃剂、含硅阻燃剂、过渡金属络合物阻燃剂以及磷腈阻燃剂。其中,含卤阻燃剂会释放有毒气体,含氮阻燃剂阻燃性不佳,含硼阻燃剂水解不稳定这些均制约这几类阻燃剂的发展。因此,研发一种阻燃效果好,耐洗涤,且不影响织物手感的阻燃整理剂十分有必要。
中国专利CN201310622317.4公开了一种织物阻燃整理剂的制备方法,包括如下步骤:(1)取2-3质量份磷酸氢二铵、15-17质量份硼砂、8-9质量份三羟甲基三聚酰胺、2-3质量份四羟乙基氯化磷、6-7质量份硅酸钠研细,混合均匀;(2)然后同时加入2-3质量份十二烷基三甲基硫酸铵、5-6质量份氯化镁、150-180质量份去离子水、10-15质量份磷酸三甲苯酯,15-20分钟内投料完毕,在60-65℃搅拌混合均匀;(3)冷却至室温,依次加入2-3质量份羟丙基甲基纤维素、12-14质量份三乙醇胺、8-9质量份尿素,搅拌混合均匀,即得织物阻燃整理剂。该织物阻燃整理剂整理后的织物具有良好的防燃性和隐燃性,可以防止熔滴,耐水洗和干洗。
发明内容
本发明涉及一种纯棉织物用阻燃整理剂及其制备方法,纯棉织物经该环保阻燃整理剂整理过后,具有良好的防燃性,并且织物的手感不会变的僵硬,长时间使用和洗涤后仍能保持良好的防燃性能。
为实现上述目的,本发明采用以下技术方案:
一种纯棉织物用阻燃整理剂的制备方法,包括以下步骤:
(1)将壳聚糖溶于水中,加入Na2CO3调节pH为9-11,之后控制温度为0-4℃,加入三氯氧磷,进行超声处理反应30-60min后,减压蒸馏去除水后,向其中加入二氯甲烷,加热至60-80℃,搅拌混合均匀后,加入双氰胺,进行反应6-7h,降至室温,蒸除二氯甲烷,制得阻燃剂;
(2)将聚己二酸-1,4-丁二醇酯二醇,聚氧化丙烯四醇,聚四氢呋喃二醇和甲基环己基二异氰酸酯,催化剂加入反应釜中,加热,使温度维持在110-120℃,以40-60转/min的速度搅拌,加入丙酮和扩链剂,阻燃剂以及丙三醇,并降低温度至40-55℃,持续搅拌90-120min,之后加入水,以200-300转/min的速度搅拌,减压蒸馏去除丙酮,制得聚氨酯乳液;
(3)将制备的聚氨酯乳液加水稀释后,加入阻燃增效剂,表面活性剂以及羟甲基纤维素,控制温度为50-60℃,搅拌1-2h后,去除气泡后制得所述纯棉织物用阻燃整理剂。
优选的,所述壳聚糖和三氯氧磷的使用量摩尔比为5:2;壳聚糖和二氯甲烷的使用量摩尔比为2:1。
优选的,所述步骤(2)中原料的使用量为,以质量份数计:
聚己二酸-1,4-丁二醇酯二醇50-60份,聚氧化丙烯四醇20-30份,聚四氢呋喃二醇35-45份,扩链剂10-17份,阻燃剂9-17份,丙三醇7-12份。
优选的,所述步骤(2)中甲基环己基二异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1-1.5。
优选的,所述催化剂为三乙醇胺和三乙胺的混合物。
优选的,所述扩链剂为1,2-二羟基-3-丙磺酸钠。
优选的,所述阻燃增效剂为三氧化二锑,所述表面活性剂为鲸蜡硬质基葡糖苷。
优选的,所述步骤(3)中原料的使用量为,以质量份数计:聚氨酯乳液100份,阻燃增效剂10-17份,表面活性剂7-9份,羟甲基纤维素12-17份。
优选的,所述纯棉织物用阻燃整理剂的固含量为45%。
本发明具有以下有益效果:
本申请以壳聚糖、三氯氧磷和双氰胺为原料将三氯氧磷与壳聚糖表面的羟基进行反应后,再连接到双氰胺上,以壳聚糖为碳源制得膨胀型阻燃剂。并以其为原料,连接到聚氨酯中,制备得到具有阻燃效果的聚氨酯乳液。本申请合成的聚氨酯乳液,以聚己二酸-1,4-丁二醇酯二醇,聚氧化丙烯四醇,聚四氢呋喃二醇和甲基环己基二异氰酸酯为原料,该聚氨酯乳液具有良好的交联性能,能够在棉织物上牢固的附着,成膜后具有较为柔软的特性,不会影响织物的手感。本申请制得的纯棉织物用阻燃整理剂具有良好的阻燃效果,并且具有良好的成膜性能,可以稳定的附着于纯棉织物上,耐水洗性能较强,使用寿命长。
具体实施方式
为了更好的理解本发明,下面通过实施例对本发明进一步说明,实施例只用于解释本发明,不会对本发明构成任何的限定。
实施例1
一种纯棉织物用阻燃整理剂的制备方法,包括以下步骤:
(1)将壳聚糖溶于水中,加入Na2CO3调节pH为9,之后控制温度为0℃,加入三氯氧磷,进行超声处理反应30min后,减压蒸馏去除水后,向其中加入二氯甲烷,加热至60℃,搅拌混合均匀后,加入双氰胺,进行反应6h,降至室温,蒸除二氯甲烷,制得阻燃剂,所述壳聚糖和三氯氧磷的使用量摩尔比为5:2;壳聚糖和二氯甲烷的使用量摩尔比为2:1;
(2)将聚己二酸-1,4-丁二醇酯二醇,聚氧化丙烯四醇,聚四氢呋喃二醇和甲基环己基二异氰酸酯,三乙醇胺和三乙胺的混合物加入反应釜中,加热,使温度维持在110℃,以40转/min的速度搅拌,加入丙酮和1,2-二羟基-3-丙磺酸钠,阻燃剂以及丙三醇,并降低温度至40℃,持续搅拌90min,之后加入水,以200转/min的速度搅拌,减压蒸馏去除丙酮,制得聚氨酯乳液;
(3)将制备的聚氨酯乳液加水稀释后,加入三氧化二锑,鲸蜡硬质基葡糖苷以及羟甲基纤维素,控制温度为50℃,搅拌1h后,去除气泡后制得所述纯棉织物用阻燃整理剂,固含量为45%。
步骤(2)中原料的使用量为,以质量份数计:
聚己二酸-1,4-丁二醇酯二醇50份,聚氧化丙烯四醇20份,聚四氢呋喃二醇35份,扩链剂10份,阻燃剂9份,丙三醇7份;甲基环己基二异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1。
步骤(3)中原料的使用量为,以质量份数计:聚氨酯乳液100份,三氧化二锑10份,鲸蜡硬质基葡糖苷7份,羟甲基纤维素12份。
纯棉织物经该阻燃剂整理后,具有良好的阻燃性能。
实施例2
一种纯棉织物用阻燃整理剂的制备方法,包括以下步骤:
(1)将壳聚糖溶于水中,加入Na2CO3调节pH为11,之后控制温度为4℃,加入三氯氧磷,进行超声处理反应60min后,减压蒸馏去除水后,向其中加入二氯甲烷,加热至80℃,搅拌混合均匀后,加入双氰胺,进行反应7h,降至室温,蒸除二氯甲烷,制得阻燃剂,所述壳聚糖和三氯氧磷的使用量摩尔比为5:2;壳聚糖和二氯甲烷的使用量摩尔比为2:1;
(2)将聚己二酸-1,4-丁二醇酯二醇,聚氧化丙烯四醇,聚四氢呋喃二醇和甲基环己基二异氰酸酯,三乙醇胺和三乙胺的混合物加入反应釜中,加热,使温度维持在120℃,以60转/min的速度搅拌,加入丙酮和1,2-二羟基-3-丙磺酸钠,阻燃剂以及丙三醇,并降低温度至55℃,持续搅拌120min,之后加入水,以300转/min的速度搅拌,减压蒸馏去除丙酮,制得聚氨酯乳液;
(3)将制备的聚氨酯乳液加水稀释后,加入三氧化二锑,鲸蜡硬质基葡糖苷以及羟甲基纤维素,控制温度为60℃,搅拌2h后,去除气泡后制得所述纯棉织物用阻燃整理剂,固含量为45%。
步骤(2)中原料的使用量为,以质量份数计:
聚己二酸-1,4-丁二醇酯二醇60份,聚氧化丙烯四醇30份,聚四氢呋喃二醇45份,扩链剂17份,阻燃剂17份,丙三醇12份;甲基环己基二异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1.5。
步骤(3)中原料的使用量为,以质量份数计:聚氨酯乳液100份,三氧化二锑17份,鲸蜡硬质基葡糖苷9份,羟甲基纤维素17份。
纯棉织物经该阻燃剂整理后,具有良好的阻燃性能。
实施例3
一种纯棉织物用阻燃整理剂的制备方法,包括以下步骤:
(1)将壳聚糖溶于水中,加入Na2CO3调节pH为9,之后控制温度为4℃,加入三氯氧磷,进行超声处理反应30min后,减压蒸馏去除水后,向其中加入二氯甲烷,加热至80℃,搅拌混合均匀后,加入双氰胺,进行反应6h,降至室温,蒸除二氯甲烷,制得阻燃剂,所述壳聚糖和三氯氧磷的使用量摩尔比为5:2;壳聚糖和二氯甲烷的使用量摩尔比为2:1;
(2)将聚己二酸-1,4-丁二醇酯二醇,聚氧化丙烯四醇,聚四氢呋喃二醇和甲基环己基二异氰酸酯,三乙醇胺和三乙胺的混合物加入反应釜中,加热,使温度维持在120℃,以40转/min的速度搅拌,加入丙酮和1,2-二羟基-3-丙磺酸钠,阻燃剂以及丙三醇,并降低温度至55℃,持续搅拌90min,之后加入水,以300转/min的速度搅拌,减压蒸馏去除丙酮,制得聚氨酯乳液;
(3)将制备的聚氨酯乳液加水稀释后,加入三氧化二锑,鲸蜡硬质基葡糖苷以及羟甲基纤维素,控制温度为50℃,搅拌2h后,去除气泡后制得所述纯棉织物用阻燃整理剂,固含量为45%。
步骤(2)中原料的使用量为,以质量份数计:
聚己二酸-1,4-丁二醇酯二醇50份,聚氧化丙烯四醇30份,聚四氢呋喃二醇35份,扩链剂17份,阻燃剂9份,丙三醇12份;甲基环己基二异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1。
步骤(3)中原料的使用量为,以质量份数计:聚氨酯乳液100份,三氧化二锑17份,鲸蜡硬质基葡糖苷7份,羟甲基纤维素17份。
纯棉织物经该阻燃剂整理后,具有良好的阻燃性能。
实施例4
一种纯棉织物用阻燃整理剂的制备方法,包括以下步骤:
(1)将壳聚糖溶于水中,加入Na2CO3调节pH为11,之后控制温度为0℃,加入三氯氧磷,进行超声处理反应60min后,减压蒸馏去除水后,向其中加入二氯甲烷,加热至60℃,搅拌混合均匀后,加入双氰胺,进行反应7h,降至室温,蒸除二氯甲烷,制得阻燃剂,所述壳聚糖和三氯氧磷的使用量摩尔比为5:2;壳聚糖和二氯甲烷的使用量摩尔比为2:1;
(2)将聚己二酸-1,4-丁二醇酯二醇,聚氧化丙烯四醇,聚四氢呋喃二醇和甲基环己基二异氰酸酯,三乙醇胺和三乙胺的混合物加入反应釜中,加热,使温度维持在110℃,以60转/min的速度搅拌,加入丙酮和1,2-二羟基-3-丙磺酸钠,阻燃剂以及丙三醇,并降低温度至40℃,持续搅拌120min,之后加入水,以200转/min的速度搅拌,减压蒸馏去除丙酮,制得聚氨酯乳液;
(3)将制备的聚氨酯乳液加水稀释后,加入三氧化二锑,鲸蜡硬质基葡糖苷以及羟甲基纤维素,控制温度为60℃,搅拌1h后,去除气泡后制得所述纯棉织物用阻燃整理剂,固含量为45%。
步骤(2)中原料的使用量为,以质量份数计:
聚己二酸-1,4-丁二醇酯二醇60份,聚氧化丙烯四醇20份,聚四氢呋喃二醇45份,扩链剂10份,阻燃剂17份,丙三醇7份;甲基环己基二异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1.5。
步骤(3)中原料的使用量为,以质量份数计:聚氨酯乳液100份,三氧化二锑10份,鲸蜡硬质基葡糖苷9份,羟甲基纤维素12份。
纯棉织物经该阻燃剂整理后,具有良好的阻燃性能。
实施例5
一种纯棉织物用阻燃整理剂的制备方法,包括以下步骤:
(1)将壳聚糖溶于水中,加入Na2CO3调节pH为10,之后控制温度为2℃,加入三氯氧磷,进行超声处理反应45min后,减压蒸馏去除水后,向其中加入二氯甲烷,加热至70℃,搅拌混合均匀后,加入双氰胺,进行反应7h,降至室温,蒸除二氯甲烷,制得阻燃剂,所述壳聚糖和三氯氧磷的使用量摩尔比为5:2;壳聚糖和二氯甲烷的使用量摩尔比为2:1;
(2)将聚己二酸-1,4-丁二醇酯二醇,聚氧化丙烯四醇,聚四氢呋喃二醇和甲基环己基二异氰酸酯,三乙醇胺和三乙胺的混合物加入反应釜中,加热,使温度维持在110℃,以50转/min的速度搅拌,加入丙酮和1,2-二羟基-3-丙磺酸钠,阻燃剂以及丙三醇,并降低温度至50℃,持续搅拌100min,之后加入水,以300转/min的速度搅拌,减压蒸馏去除丙酮,制得聚氨酯乳液;
(3)将制备的聚氨酯乳液加水稀释后,加入三氧化二锑,鲸蜡硬质基葡糖苷以及羟甲基纤维素,控制温度为55℃,搅拌2h后,去除气泡后制得所述纯棉织物用阻燃整理剂,固含量为45%。
步骤(2)中原料的使用量为,以质量份数计:
聚己二酸-1,4-丁二醇酯二醇55份,聚氧化丙烯四醇25份,聚四氢呋喃二醇40份,扩链剂13份,阻燃剂14份,丙三醇9份;甲基环己基二异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1.3。
步骤(3)中原料的使用量为,以质量份数计:聚氨酯乳液100份,三氧化二锑15份,鲸蜡硬质基葡糖苷8份,羟甲基纤维素15份。
纯棉织物经该阻燃剂整理后,具有良好的阻燃性能。
Claims (10)
1.一种纯棉织物用阻燃整理剂的制备方法,其特征在于,包括以下步骤:
(1)将壳聚糖溶于水中,加入Na2CO3调节pH为9-11,之后控制温度为0-4℃,加入三氯氧磷,进行超声处理反应30-60min后,减压蒸馏去除水后,向其中加入二氯甲烷,加热至60-80℃,搅拌混合均匀后,加入双氰胺,进行反应6-7h,降至室温,蒸除二氯甲烷,制得阻燃剂;
(2)将聚己二酸-1,4-丁二醇酯二醇,聚氧化丙烯四醇,聚四氢呋喃二醇和甲基环己基二异氰酸酯,催化剂加入反应釜中,加热,使温度维持在110-120℃,以40-60转/min的速度搅拌,加入丙酮和扩链剂,阻燃剂以及丙三醇,并降低温度至40-55℃,持续搅拌90-120min,之后加入水,以200-300转/min的速度搅拌,减压蒸馏去除丙酮,制得聚氨酯乳液;
(3)将制备的聚氨酯乳液加水稀释后,加入阻燃增效剂,表面活性剂以及羟甲基纤维素,控制温度为50-60℃,搅拌1-2h后,去除气泡后制得所述纯棉织物用阻燃整理剂。
2.根据权利要求1所述的纯棉织物用阻燃整理剂的制备方法,其特征在于:所述壳聚糖和三氯氧磷的使用量摩尔比为5:2;壳聚糖和二氯甲烷的使用量摩尔比为2:1。
3.根据权利要求1所述的纯棉织物用阻燃整理剂的制备方法,其特征在于:所述步骤(2)中原料的使用量为,以质量份数计:
聚己二酸-1,4-丁二醇酯二醇50-60份,聚氧化丙烯四醇20-30份,聚四氢呋喃二醇35-45份,扩链剂10-17份,阻燃剂9-17份,丙三醇7-12份。
4.根据权利要求1所述的纯棉织物用阻燃整理剂的制备方法,其特征在于:所述步骤(2)中甲基环己基二异氰酸酯的使用量与多元醇化合物的使用量摩尔比满足-NCO:-OH=1:1-1.5。
5.根据权利要求1所述的纯棉织物用阻燃整理剂的制备方法,其特征在于:所述催化剂为三乙醇胺和三乙胺的混合物。
6.根据权利要求1所述的纯棉织物用阻燃整理剂的制备方法,其特征在于:所述扩链剂为1,2-二羟基-3-丙磺酸钠。
7.根据权利要求1所述的纯棉织物用阻燃整理剂的制备方法,其特征在于:所述阻燃增效剂为三氧化二锑,所述表面活性剂为鲸蜡硬质基葡糖苷。
8.根据权利要求1所述的纯棉织物用阻燃整理剂的制备方法,其特征在于:所述步骤(3)中原料的使用量为,以质量份数计:聚氨酯乳液100份,阻燃增效剂10-17份,表面活性剂7-9份,羟甲基纤维素12-17份。
9.根据权利要求1所述的纯棉织物用阻燃整理剂的制备方法,其特征在于:所述纯棉织物用阻燃整理剂的固含量为45%。
10.一种纯棉织物用阻燃整理剂,其特征在于:由权利要求1-9任一项所述的方法制备而成。
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