CN105566608B - 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂 - Google Patents

用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂 Download PDF

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CN105566608B
CN105566608B CN201610151504.2A CN201610151504A CN105566608B CN 105566608 B CN105566608 B CN 105566608B CN 201610151504 A CN201610151504 A CN 201610151504A CN 105566608 B CN105566608 B CN 105566608B
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aqueous polyurethane
artificial leather
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CN105566608A (zh
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花亮亮
李维虎
戴家兵
朱有奎
汪飞
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Lnzhou Ketian Aqueous Polymer Material Co Ltd
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Abstract

本发明涉及一种用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇70~200份；多异氰酸酯15~50份；亲水化合物1~20份；扩链剂1~18份；成盐剂1~8份；硅烷偶联剂2~9份。本发明无毒、环保，采用其制备的沙发革贝斯产品性能良好。

Description

用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂
技术领域
本发明涉及水性聚氨酯树脂技术领域，尤其涉及用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂。
背景技术
目前大规模生产的沙发革贝斯主要由溶剂型树脂制成。而制作溶剂型树脂的有机溶剂，具有有毒、易挥发、对环境和人体有危害的特性，特别用于制作沙发革、服装革类产品时，对人体的危害体现的更为明显。
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。水性聚氨酯制成的产品具有溶剂型湿法合成革贝斯的基本结构，手感与物性接近溶剂型合成革贝斯，适合大规模生产。
用于制作水性聚氨酯沙发革贝斯的产品具有传统溶剂型聚氨酯沙发革贝斯的手感及物性性能，同时具备传统溶剂型聚氨酯沙发革贝斯所不具有的环保性能以及满足人们逐渐增长的家居环保要求。
发明内容
本发明所要解决的技术问题是提供一种无毒、性能良好的用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂。
为解决上述问题，本发明所述的用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，其特征在于：该水性聚氨酯树脂包括以下重量份的原料：多元醇70~200份；多异氰酸酯15~50份；亲水化合物1~20份；扩链剂1~18份；成盐剂1~8份；硅烷偶联剂2~9份。
所述多元醇是指分子量为1000~3000的聚四氢呋喃醚多元醇、聚环氧乙烷多元醇、聚环氧丙烷多元醇、端羟基聚丁二烯、聚硅氧烷多元醇、聚丙二醇多元醇中的一种或几种。
所述多异氰酸酯是指甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、1,6-己二异氰酸酯、苯二亚甲基二异氰酸酯、萘-1,5-二异氰酸酯、多亚甲基多苯基异氰酸酯、四甲基苯二亚甲基二异氰酸酯、甲基环己基二异氰酸酯、二环己基甲烷二异氰酸酯、4,4'-二环己基甲烷二异氰酸酯中的一种或几种。
所述亲水化合物是指2,2-二羟甲基丙酸、2,2-二羟甲基丁酸的一种或两种。
所述扩链剂是指异佛尔酮二胺、间苯二甲胺、乙二胺中的一种或几种。
所述成盐剂是指三乙胺或浓度为0.5mol/L的氨水。
所述硅烷偶联剂是指N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷、γ―氨丙基三乙氧基硅烷、γ―(2,3-环氧丙氧) 丙基三甲氧基硅烷、硅烷偶联剂G-570中的一种或几种。
如上所述的用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法，包括以下步骤：
⑴按配比称重；
⑵将多元醇加热至100℃~110℃脱水0.5~1.5h，然后降温至45~55℃，再加入多异氰酸酯，升温至85~95℃，并在该温度下保温反应1.5~2.5 h；之后降温至45~55℃，加入亲水化合物，并加入容器内固体质量分数4%的丙酮；其次升温至75~85℃反应1.5~3.5 h，之后降温至45~55℃，此时加入0.2~0.4g的有机铋催化剂和固体质量分数6%的丙酮，升温至65~75℃反应2.5~4h；反应结束测定NCO含量，直至NCO达到理论值，最后加入容器内固体质量分数55%的丙酮，降温至40~50℃加入硅烷偶联剂反应10~30分钟，得到水性聚氨酯预聚体；
⑶将成盐剂加入所述水性聚氨酯预聚体中，在800~1000r/min情况下进行中和反应，以1500~3000r/min的速率搅拌加入所述水性聚氨酯预聚体中固体份质量的1.5~3.5倍的去离子水，并加入扩链剂，再以800~1000r/min的速率搅拌5~30分钟，得到含丙酮的阴离子水性聚氨酯半成品；
⑷所述含丙酮的阴离子水性聚氨酯半成品经减压蒸馏出丙酮，即得用于服装革湿法浸渍贝斯的阴离子水性聚氨酯树脂。
所述步骤⑷中减压蒸馏的条件是指压力为-0.09MPa~-0.1MPa。
本发明与现有技术相比具有以下优点：
1、本发明水性聚氨酯原料组分及产品中均不含有甲醛、甲苯、二甲苯、丙酮、丁酮（MEK）、乙酸、乙酯和二甲基甲酰胺等有机物，因此，无毒环保，减轻对环境的污染和保持生产车间的健康。
2、本发明采用硅烷偶联剂后扩链加入方式。通过化学结合理论，硅烷偶联剂可以和异氰酸酯形成稳定的化学键，可以显著提高分子链段的机械性能；硅烷偶联剂能与织物表面作用形成共价键，起着无机相与有机相之间连接的桥梁作用。通过可变层理论，偶联剂在聚合物和填料之间形成一层比分子层厚的多的挠性树脂层，该层能松弛界面应力，阻止界面裂缝的扩展，因而改善了界面的结合强度，提高了材料的机械性能。因此，本发明中的硅烷偶联剂对于树脂所制成的贝斯材料的剥离和耐屈挠有着很好的提高作用。
3、采用本发明产品按照下述方法制备的沙发革贝斯产品在耐黄变、触感、耐屈挠、剥离、贝斯外观、耐水解等方面均有良好的性能体现（参见表1）。制备方法如下：
①将实施例中的1-3号样品加入发泡剂 K12 ( 济南硕昌化工)、泡沫稳定剂207( 青岛中宝化工)、增稠剂3220( 深圳海川化工)、pH调节稳定剂AMP–95（广东顺德世邦佳明化工）、固化剂3099( 德国拜耳)、水性色浆（吴江金峰化工）和填料木质纤维素（郑州银鹤糊精），机械发泡混合制成水性浆料；
②将基布分别浸渍于稀释15倍数的实施例中的1-3号样品，后经5%氯化钠水溶液凝固，置于120℃的烘箱中烘干；
③将水性浆料直接涂覆在步骤②经过处理的基布上，通过凝聚、水洗、烘干的方式，制得沙发革贝斯。
表1 本发明所得产品制得的沙发革贝斯的检测技术指标
4、本发明制备工艺简单，容易控制，生产安全性大大提高，适合大规模工业化生产。
具体实施方式
实施例1 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇190g；多异氰酸酯39g；亲水化合物5 g；扩链剂5 g；成盐剂4g；硅烷偶联剂8 g。
其中：多元醇是指分子量为1000~3000的聚丙二醇多元醇。多异氰酸酯是指异佛尔酮二异氰酸酯、1,6-己二异氰酸酯、4,4'-二环己基甲烷二异氰酸酯，其质量比为1.8：1：2。亲水化合物是指2,2-二羟甲基丙酸。扩链剂是指乙二胺。成盐剂是指三乙胺。硅烷偶联剂是指N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷、γ―氨丙基三乙氧基硅烷，其质量比为1：1.2。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法，包括以下步骤：
⑴按配比称重；
⑵将多元醇加热至100℃~110℃脱水0.5~1.5h，然后降温至45~55℃，再加入多异氰酸酯，升温至85~95℃，并在该温度下保温反应1.5~2.5 h；之后降温至45~55℃，加入亲水化合物，并加入容器内固体质量分数4%的丙酮；其次升温至75~85℃反应1.5~3.5 h，之后降温至45~55℃，此时加入0.2~0.4g的有机铋催化剂和固体质量分数6%的丙酮，升温至65~75℃反应2.5~4h；反应结束测定NCO含量，直至NCO达到理论值，最后加入容器内固体质量分数55%的丙酮，降温至40~50℃加入硅烷偶联剂反应10~30分钟，得到水性聚氨酯预聚体；
⑶将成盐剂加入水性聚氨酯预聚体中，在800~1000r/min情况下进行中和反应，以1500~3000r/min的速率搅拌加入水性聚氨酯预聚体中固体份质量的1.5~3.5倍的去离子水，并加入扩链剂，再以800~1000r/min的速率搅拌5~30分钟，得到含丙酮的阴离子水性聚氨酯半成品；
⑷含丙酮的阴离子水性聚氨酯半成品在压力为-0.09MPa~-0.1MPa的条件下经减压蒸馏出丙酮，即得用于服装革湿法浸渍贝斯的阴离子水性聚氨酯树脂。
实施例2 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇200g；多异氰酸酯50g；亲水化合物4g；扩链剂6 g；成盐剂5g；硅烷偶联剂6 g。
其中：多元醇是指分子量为1000~3000的聚四氢呋喃醚多元醇。多异氰酸酯是指异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯，其质量比为1：1.2。亲水化合物是指2,2-二羟甲基丁酸。扩链剂是指异佛尔酮二胺。成盐剂是指三乙胺。硅烷偶联剂是指N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷、γ―氨丙基三乙氧基硅烷，其质量比为1：1.2。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例3 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇185g；多异氰酸酯45g；亲水化合物4g；扩链剂6 g；成盐剂5g；硅烷偶联剂6 g。
其中：多元醇是指分子量为1000~3000的聚环氧丙烷多元醇。多异氰酸酯是指四甲基苯二亚甲基二异氰酸酯。亲水化合物是指2,2-二羟甲基丁酸。扩链剂是指间苯二甲胺。成盐剂是指三乙胺。硅烷偶联剂是指N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例4 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇70 g；多异氰酸酯15 g；亲水化合物1 g；扩链剂1 g；成盐剂1 g；硅烷偶联剂2 g。
其中：多元醇是指分子量为1000~3000的聚环氧乙烷多元醇。多异氰酸酯是指甲苯二异氰酸酯。亲水化合物是指2,2-二羟甲基丙酸。扩链剂是指异佛尔酮二胺。成盐剂是指浓度为0.5mol/L的氨水。硅烷偶联剂是指γ―氨丙基三乙氧基硅烷。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例5 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇100 g；多异氰酸酯40 g；亲水化合物20 g；扩链剂18 g；成盐剂8 g；硅烷偶联剂9 g。
其中：多元醇是指分子量为1000~3000的端羟基聚丁二烯。多异氰酸酯是指异佛尔酮二异氰酸酯。亲水化合物是指2,2-二羟甲基丁酸。扩链剂是指间苯二甲胺。成盐剂是指浓度为0.5mol/L的氨水。硅烷偶联剂是指γ―(2,3-环氧丙氧) 丙基三甲氧基硅烷。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例6 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇80 g；多异氰酸酯20 g；亲水化合物6 g；扩链剂8 g；成盐剂2 g；硅烷偶联剂3 g。
其中：多元醇是指分子量为1000~3000的聚硅氧烷多元醇。多异氰酸酯是指二苯基甲烷二异氰酸酯。亲水化合物是指2,2-二羟甲基丙酸。扩链剂是指异佛尔酮二胺。成盐剂是指三乙胺。硅烷偶联剂是指硅烷偶联剂G-570。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例7 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇90 g；多异氰酸酯25 g；亲水化合物8 g；扩链剂10 g；成盐剂3 g；硅烷偶联剂4g。
其中：多元醇是指分子量为1000~3000的聚四氢呋喃醚多元醇。多异氰酸酯是指1,6-己二异氰酸酯。亲水化合物是指2,2-二羟甲基丁酸。扩链剂是指乙二胺。成盐剂是指浓度为0.5mol/L的氨水。硅烷偶联剂是指N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例8 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇110 g；多异氰酸酯30 g；亲水化合物10 g；扩链剂12g；成盐剂6 g；硅烷偶联剂5g。
其中：多元醇是指分子量为1000~3000的聚环氧乙烷多元醇。多异氰酸酯是指苯二亚甲基二异氰酸酯。亲水化合物是指2,2-二羟甲基丙酸。扩链剂是指间苯二甲胺。成盐剂是指浓度为0.5mol/L的氨水。硅烷偶联剂是指N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例9 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇120 g；多异氰酸酯35 g；亲水化合物12 g；扩链剂14 g；成盐剂7 g；硅烷偶联剂7 g。
其中：多元醇是指分子量为1000~3000的聚环氧乙烷多元醇。多异氰酸酯是指萘-1,5-二异氰酸酯。亲水化合物是指2,2-二羟甲基丙酸。扩链剂是指异佛尔酮二胺。成盐剂是指三乙胺。硅烷偶联剂是指γ―氨丙基三乙氧基硅烷。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例10 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇130 g；多异氰酸酯18 g；亲水化合物14 g；扩链剂16 g；成盐剂4.5 g；硅烷偶联剂4.5 g。
其中：多元醇是指分子量为1000~3000的聚环氧丙烷多元醇。多异氰酸酯是指多亚甲基多苯基异氰酸酯。亲水化合物是指2,2-二羟甲基丁酸。扩链剂是指异佛尔酮二胺。成盐剂是指三乙胺。硅烷偶联剂是指γ―(2,3-环氧丙氧) 丙基三甲氧基硅烷。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例11 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇140 g；多异氰酸酯22 g；亲水化合物16 g；扩链剂15 g；成盐剂5.5 g；硅烷偶联剂5.5 g。
其中：多元醇是指分子量为1000~3000的端羟基聚丁二烯。多异氰酸酯是指甲基环己基二异氰酸酯。亲水化合物是指、2,2-二羟甲基丁酸。扩链剂是指乙二胺。成盐剂是指三乙胺。硅烷偶联剂是指硅烷偶联剂G-570。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例12 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇150 g；多异氰酸酯28 g；亲水化合物18 g；扩链剂17 g；成盐剂6.5g；硅烷偶联剂6.5 g。
其中：多元醇是指分子量为1000~3000的聚硅氧烷多元醇。多异氰酸酯是指二环己基甲烷二异氰酸酯。亲水化合物是指2,2-二羟甲基丁酸。扩链剂是指异佛尔酮二胺。成盐剂是指浓度为0.5mol/L的氨水。硅烷偶联剂是指N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
实施例13 用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，该水性聚氨酯树脂包括以下重量份的原料：多元醇160 g；多异氰酸酯32 g；亲水化合物17 g；扩链剂18 g；成盐剂8 g；硅烷偶联剂8 g。
其中：多元醇是指分子量为1000~3000的聚丙二醇多元醇。多异氰酸酯是指4,4'-二环己基甲烷二异氰酸酯。亲水化合物是指2,2-二羟甲基丙酸。扩链剂是指异佛尔酮二胺。成盐剂是指三乙胺。硅烷偶联剂是指N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷。
该用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂的制备方法同实施例1。
上述实施例1~11中，多元醇是指分子量为1000~3000的聚四氢呋喃醚多元醇、聚环氧乙烷多元醇、聚环氧丙烷多元醇、端羟基聚丁二烯、聚硅氧烷多元醇、聚丙二醇多元醇中的几种组合。
多异氰酸酯是指甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、1,6-己二异氰酸酯、苯二亚甲基二异氰酸酯、萘-1,5-二异氰酸酯、多亚甲基多苯基异氰酸酯、四甲基苯二亚甲基二异氰酸酯、甲基环己基二异氰酸酯、二环己基甲烷二异氰酸酯、4,4'-二环己基甲烷二异氰酸酯中的几种组合。
亲水化合物是指2,2-二羟甲基丙酸、2,2-二羟甲基丁酸的两种组合。
扩链剂是指异佛尔酮二胺、间苯二甲胺、乙二胺中的几种组合。
硅烷偶联剂是指N-(β-氨乙基)-γ-氨丙基甲基二甲氧基硅烷、γ―氨丙基三乙氧基硅烷、γ―(2,3-环氧丙氧) 丙基三甲氧基硅烷、硅烷偶联剂G-570中的几种组合。
应该理解，这里讨论的实施例和实施方案只是为了说明，对熟悉该领域的人可以提出各种改进和变化，这些改进和变化将包括在本申请的精神实质和范围以及所附的权利要求范围内。

Claims (5)

1.用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，其特征在于：该水性聚氨酯树脂包括以下重量份的原料：多元醇70~200份；多异氰酸酯15~50份；亲水化合物1~20份；扩链剂1~18份；成盐剂1~8份；硅烷偶联剂2~9份；所述亲水化合物是指2,2-二羟甲基丙酸、2,2-二羟甲基丁酸的一种或两种；所述硅烷偶联剂是指硅烷偶联剂G-570；
其制备方法，包括以下步骤：
⑴按配比称重；
⑵将多元醇加热至100℃~110℃脱水0.5~1.5h，然后降温至45~55℃，再加入多异氰酸酯，升温至85~95℃，并在该温度下保温反应1.5~2.5 h；之后降温至45~55℃，加入亲水化合物，并加入容器内固体质量分数4%的丙酮；其次升温至75~85℃反应1.5~3.5 h，之后降温至45~55℃，此时加入0.2~0.4g的有机铋催化剂和容器内固体质量分数6%的丙酮，升温至65~75℃反应2.5~4h；反应结束测定NCO含量，直至NCO达到理论值，最后加入容器内固体质量分数55%的丙酮，降温至40~50℃加入硅烷偶联剂反应10~30分钟，得到水性聚氨酯预聚体；
⑶将成盐剂加入所述水性聚氨酯预聚体中，在800~1000r/min情况下进行中和反应，以1500~3000r/min的速率搅拌加入所述水性聚氨酯预聚体中固体份质量的1.5~3.5倍的去离子水，并加入扩链剂，再以800~1000r/min的速率搅拌5~30分钟，得到含丙酮的阴离子水性聚氨酯半成品；
⑷所述含丙酮的阴离子水性聚氨酯半成品经减压蒸馏出丙酮，即得用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂；所述减压蒸馏的条件是指压力为-0.09MPa~-0.1MPa。
2.如权利要求1所述的用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，其特征在于：所述多元醇是指分子量为1000~3000的聚四氢呋喃醚多元醇、聚环氧乙烷多元醇、聚环氧丙烷多元醇、端羟基聚丁二烯、聚硅氧烷多元醇中的一种或几种。
3.如权利要求1所述的用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，其特征在于：所述多异氰酸酯是指甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、1,6-己二异氰酸酯、苯二亚甲基二异氰酸酯、萘-1,5-二异氰酸酯、多亚甲基多苯基异氰酸酯、甲基环己基二异氰酸酯、二环己基甲烷二异氰酸酯中的一种或几种。
4.如权利要求1所述的用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，其特征在于：所述扩链剂是指异佛尔酮二胺、间苯二甲胺、乙二胺中的一种或几种。
5.如权利要求1所述的用于沙发革湿法浸渍贝斯的阴离子水性聚氨酯树脂，其特征在于：所述成盐剂是指三乙胺或浓度为0.5mol/L的氨水。
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