CN105949427A - 一种低模量慢回弹性能的水性聚氨酯 - Google Patents

一种低模量慢回弹性能的水性聚氨酯 Download PDF

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CN105949427A
CN105949427A CN201610470677.0A CN201610470677A CN105949427A CN 105949427 A CN105949427 A CN 105949427A CN 201610470677 A CN201610470677 A CN 201610470677A CN 105949427 A CN105949427 A CN 105949427A
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华明扬
华伽杰
蔡爱文
项高朋
沈群
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Jiangyin Ruco Technology Co Ltd
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Abstract

本发明涉及一种低模量慢回弹性能的水性聚氨酯，以聚酯、二异氰酸酯和聚醚为主要原料，聚酯为具有侧甲基的聚酯，以己二酸和新戊二醇为聚酯反应单体，聚酯的数均分子量为4500～5000；二异氰酸酯为具有对称结构的脂肪族二异氰酸酯，二异氰酸酯的添加量满足其所含硬段与原料软段的摩尔比为2.5～4.5；聚醚是由环氧乙烷、环氧丙烷的共聚物和分子量1000以下的三官能团聚醚组成的混合物，聚醚的添加量满足其所含羟基量占原料总羟基量的摩尔百分比为5～20%。本申请所制得的水性聚氨酯具有低模量和慢回弹性能，模量指数为1～10，回弹性能满足：1cm宽的试样，拉伸6倍，释放后30s内缓慢回弹恢复至原样。

Description

一种低模量慢回弹性能的水性聚氨酯
技术领域
本发明涉及水性聚氨酯涂层技术领域，具体涉及一种低模量、慢回弹性能的水性聚氨酯。
背景技术
聚氨酯树脂的水性化已逐步取代溶剂型，成为聚氨酯工业发展的重要方向。水性聚氨酯是以水代替有机溶剂作为分散介质的新型聚氨酯体系，也称水分散聚氨酯、水系聚氨酯或水基聚氨酯。水性聚氨酯以水为溶剂，无污染、安全可靠、机械性能优良、相容性好、易于改性等优点。
水性聚氨酯可广泛应用于涂料、胶粘剂、织物涂层与整理剂、皮革涂饰剂、纸张表面处理剂和纤维表面处理剂。依合成单体不同水性聚氨酯可分为聚醚型、聚酯型和聚醚、聚酯混合型。依照选用的二异氰酸酯的不同，水性聚氨酯又可分为芳香族和脂肪族。
水性聚氨酯整个合成过程可分为两个阶段。第一阶段为预逐步聚合，即由低聚物二醇、扩链剂、水性单体、二异氰酸酯通过溶液逐步聚合生成相对分子质量为l000量级的水性聚氨酯预聚体；第二阶段为中和后预聚体在水中的分散。
发明内容
本发明的目的是提供一种低模量、慢回弹性能的水性聚氨酯，作为织物涂层，能够增加物料的柔软度以及更慢的回弹性能。
本发明解决上述问题所采用的技术方案为：一种低模量慢回弹性能的水性聚氨酯，以聚酯、二异氰酸酯和聚醚为主要原料，其中，聚酯为具有侧甲基的聚酯，以己二酸和新戊二醇为聚酯反应单体，聚酯的数均分子量为4500～5000；二异氰酸酯为具有对称结构的脂肪族二异氰酸酯，二异氰酸酯的添加量满足其所含硬段与原料软段的摩尔比为2.5～4.5；聚醚是由环氧乙烷、环氧丙烷的共聚物和分子量1000以下的三官能团聚醚组成的混合物，聚醚的添加量满足其所含羟基量占原料总羟基量的摩尔百分比为5～20%。
优选地，所述分子量1000以下的三官能团聚醚为长华（江苏长华聚氨酯科技有限公司）慢回弹307聚醚。
上述低模量慢回弹性能的水性聚氨酯的制备方法，包括如下步骤：
1）于反应釜内加入聚酯和聚醚，温度设置为95～120℃，脱水；
2）体系降温至60～70℃，加入二异氰酸酯，再升温至75～90℃，保温2小时及以上，反应至异氰酸根***理论值；
3）向熔融体系中加入溶剂，降低体系粘度，溶剂为N-乙基吡咯、烷酮；同时加入亲水扩链剂，该亲水扩链剂包括二羟甲基丙酸、分子量500以内的小分子量二醇和蓖麻油，二羟甲基丙酸占体系内总反应原料的质量百分比为3～10%；温度升至60～70℃，保温反应4小时及以上；
4）体系降温至40～50℃，加中和剂如三乙胺，搅拌2-3min，中和度50～80%；
5）加水乳化：乳化温度30～40℃，加入胺类扩链剂封闭异氰酸根，胺类扩链剂优选二乙烯三胺常温条件下反应10min及以上，胺类扩链剂的添加量满足成品中异氰酸根与羟基的摩尔比为1.1～1.3；
6）出料。
所述步骤3的小分子量二醇为丁二醇、二甘醇、十二醇。
与现有技术相比，本发明的优点在于：通过进一步设计原料来获得一种具有低模量、慢回弹性能的水性聚氨酯，优选具有侧甲基的聚酯降低回弹速度，同时优化聚酯的分子量有助于降低模量。聚醚中包含长华慢回弹307聚醚，进一步地让产品具有较慢的回弹性能。在乳化过程中，优化亲水扩链剂，以蓖麻油替代部分小分子量二醇，因蓖麻油具有长链烷烃结构，能够降低最终产品的模量并减小回弹速度。本申请产品模量指数1～10，低于现有市场上的10～15，本发明的水性聚氨酯具有更好的柔软性，1cm宽试样拉伸6倍后能够在释放后30s内缓慢恢复。
具体实施方式
以下结合实施例对本发明作进一步详细描述。
实施例1
水性聚氨酯以聚酯、二异氰酸酯和聚醚为主要原料，其中，聚酯为具有侧甲基的聚酯，以己二酸和新戊二醇为聚酯反应单体，聚酯的数均分子量为4500～5000；二异氰酸酯为具有对称结构的脂肪族二异氰酸酯如HDI，二异氰酸酯的添加量满足其所含硬段与原料软段的摩尔比为2.5～4.5；聚醚是由环氧乙烷、环氧丙烷的共聚物和长华慢回弹307聚醚组成的混合物，聚醚的添加量满足其所含羟基量占原料总羟基量的摩尔百分比为5%。
上述水性聚氨酯的制备方法，包括如下步骤：
1）于反应釜内加入聚酯和聚醚，温度设置为95～120℃，脱水；
2）体系降温至60～70℃，加入二异氰酸酯，再升温至75～90℃，保温2小时，反应至异氰酸根***理论值；
3）向熔融体系中加入溶剂，降低体系粘度，溶剂为N-乙基吡咯、丙酮；同时加入亲水扩链剂，该亲水扩链剂包括二羟甲基丙酸、十二醇和蓖麻油，二羟甲基丙酸占体系内总反应原料的质量百分比为3～10%；温度升至60～70℃，保温反应4小时；
4）体系降温至40～50℃，加中和剂三乙胺，搅拌3min，中和度50%；
5）加水乳化：乳化温度30～40℃，加入胺类扩链剂封闭异氰酸根，胺类扩链剂优选二乙烯三胺常温条件下反应10min及以上，胺类扩链剂的添加量满足成品中异氰酸根与羟基的摩尔比为1.1；
6）出料。
实施例2
水性聚氨酯以聚酯、二异氰酸酯和聚醚为主要原料，其中，聚酯为具有侧甲基的聚酯，以己二酸和新戊二醇为聚酯反应单体，聚酯的数均分子量为4500～5000；二异氰酸酯为具有对称结构的脂肪族二异氰酸酯如HMDI，二异氰酸酯的添加量满足其所含硬段与原料软段的摩尔比为2.5～4.5；聚醚是由环氧乙烷、环氧丙烷的共聚物和长华慢回弹307聚醚组成的混合物，聚醚的添加量满足其所含羟基量占原料总羟基量的摩尔百分比为5%。
上述水性聚氨酯的制备方法，包括如下步骤：
1）于反应釜内加入聚酯和聚醚，温度设置为95～120℃，脱水；
2）体系降温至60～70℃，加入二异氰酸酯，再升温至75～90℃，保温2小时，反应至异氰酸根***理论值；
3）向熔融体系中加入溶剂，降低体系粘度，溶剂为N-乙基吡咯、丁酮；同时加入亲水扩链剂，该亲水扩链剂包括二羟甲基丙酸、二甘醇和蓖麻油，二羟甲基丙酸占体系内总反应原料的质量百分比为3～10%；温度升至60～70℃，保温反应6小时；
4）体系降温至40～50℃，加中和剂三乙胺，搅拌3min，中和度80%；
5）加水乳化：乳化温度30～40℃，加入胺类扩链剂封闭异氰酸根，胺类扩链剂优选二乙烯三胺常温条件下反应10min及以上，胺类扩链剂的添加量满足成品中异氰酸根与羟基的摩尔比为1.1；
6）出料。
实施例3
水性聚氨酯以聚酯、二异氰酸酯和聚醚为主要原料，其中，聚酯为具有侧甲基的聚酯，以己二酸和新戊二醇为聚酯反应单体，聚酯的数均分子量为4500～5000；二异氰酸酯为具有对称结构的脂肪族二异氰酸酯如HDI，二异氰酸酯的添加量满足其所含硬段与原料软段的摩尔比为2.5～4.5；聚醚是由环氧乙烷、环氧丙烷的共聚物和长华慢回弹307聚醚组成的混合物，聚醚的添加量满足其所含羟基量占原料总羟基量的摩尔百分比为5%。
上述水性聚氨酯的制备方法，包括如下步骤：
1）于反应釜内加入聚酯和聚醚，温度设置为95～120℃，脱水；
2）体系降温至60～70℃，加入二异氰酸酯，再升温至75～90℃，保温4小时，反应至异氰酸根***理论值；
3）向熔融体系中加入溶剂，降低体系粘度，溶剂为N-乙基吡咯、丁酮；同时加入亲水扩链剂，该亲水扩链剂包括二羟甲基丙酸、丁二醇和蓖麻油，二羟甲基丙酸占体系内总反应原料的质量百分比为3～10%；温度升至60～70℃，保温反应4小时；
4）体系降温至40～50℃，加中和剂三乙胺，搅拌3min，中和度60%；
5）加水乳化：乳化温度30～40℃，加入胺类扩链剂封闭异氰酸根，胺类扩链剂优选二乙烯三胺常温条件下反应20min，胺类扩链剂的添加量满足成品中异氰酸根与羟基的摩尔比为1.1；
6）出料。
上述各实施例所制得的水性聚氨酯，具有低模量和慢回弹性能，模量指数为1～10，回弹性能满足：1cm宽的试样，拉伸6倍，释放后30s内缓慢回弹恢复至原样。或者取圆片材为检测试样，半悬于工作台，观察其自由下垂变化，越慢越好。

Claims (6)

1.一种低模量慢回弹性能的水性聚氨酯，其特征在于：以聚酯、二异氰酸酯和聚醚为主要原料，其中，聚酯为具有侧甲基的聚酯，以己二酸和新戊二醇为聚酯反应单体，聚酯的数均分子量为4500～5000；二异氰酸酯为具有对称结构的脂肪族二异氰酸酯，二异氰酸酯的添加量满足其所含硬段与原料软段的摩尔比为2.5～4.5；聚醚是由环氧乙烷、环氧丙烷的共聚物和分子量1000以下的三官能团聚醚组成的混合物，聚醚的添加量满足其所含羟基量占原料总羟基量的摩尔百分比为5～20%。
2.根据权利要求1所述的低模量慢回弹性能的水性聚氨酯，其特征在于：所述分子量1000以下的三官能团聚醚为长华慢回弹307聚醚。
3.一种制备权利要求1所述低模量慢回弹性能的水性聚氨酯的方法，其特征在于：包括如下步骤：
1）于反应釜内加入聚酯和聚醚，温度设置为95～120℃，脱水；
2）体系降温至60～70℃，加入二异氰酸酯，再升温至75～90℃，保温2小时及以上，反应至异氰酸根***理论值；
3）向熔融体系中加入溶剂，降低体系粘度，溶剂为N-乙基吡咯、烷酮；同时加入亲水扩链剂，该亲水扩链剂包括二羟甲基丙酸、分子量500以内的小分子量二醇和蓖麻油，二羟甲基丙酸占体系内总反应原料的质量百分比为3～10%；温度升至60～70℃，保温反应4小时及以上；
4）体系降温至40～50℃，加中和剂，搅拌2-3min，中和度50～80%；
5）加水乳化：乳化温度30～40℃，加入胺类扩链剂封闭异氰酸根，常温条件下反应10min及以上，胺类扩链剂的添加量满足成品中异氰酸根与羟基的摩尔比为1.1～1.3；
6）出料。
4.根据权利要求3所述的低模量慢回弹性能的水性聚氨酯的方法，其特征在于：所述步骤3的小分子量二醇为丁二醇、二甘醇、十二醇。
5.根据权利要求3所述的低模量慢回弹性能的水性聚氨酯的方法，其特征在于：所述步骤4的中和剂为三乙胺。
6.根据权利要求3所述的低模量慢回弹性能的水性聚氨酯的方法，其特征在于：所述步骤5的胺类扩链剂为二乙烯三胺。
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