CN110938185A - 一种水性聚氨酯树脂的制备方法 - Google Patents

一种水性聚氨酯树脂的制备方法 Download PDF

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CN110938185A
CN110938185A CN201811118473.6A CN201811118473A CN110938185A CN 110938185 A CN110938185 A CN 110938185A CN 201811118473 A CN201811118473 A CN 201811118473A CN 110938185 A CN110938185 A CN 110938185A
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姜涛
何子健
金玥
徐广宇
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Shanghai Hongye Coatings Technology Development Co ltd
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Abstract

本发明公开了一种水性聚氨酯树脂的制备方法，包括步骤：S1、向反应釜内加入聚酯多元醇或/和聚醚多元醇，真空脱水，降温，得到物料A；S2、向物料A中加入多异氰酸，保温反应，降温，得到B物料；S3、向B物料中加入二羟甲基丙酸，然后将1,4‑丁二醇和三乙胺溶液滴加至反应釜中，保温反应，加入有机金属催化剂、光稳定剂，保温反应，得到C物料；S4、C物料降温至室温后，加入三乙胺进行中和，加入后扩链剂，搅拌反应，加入去离子水乳化分散，减压蒸馏，得到水性聚氨酯树脂。本发明所得水性聚氨酯树脂具有优异的粘结强度、光泽度、耐磨性及耐黄变性，其中二羟甲基丙酸作为亲水扩链剂，能够构成阴离子型自乳化性聚氨酯并提高聚氨酯分子量。

Description

一种水性聚氨酯树脂的制备方法
技术领域
本发明涉及水性聚氨酯树脂制备技术领域，尤其涉及一种水性聚氨酯树脂的制备方法。
背景技术
聚氨酯树脂作为一种具有高强度、抗撕裂、耐磨等特性的高分子材料，在日常生活、工农业生产、医学等领域广泛应用。然而随着各国环境安全法律法规的出台，许多国家已限制了溶剂型聚氨酯的应用。目前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。市场上现有水性聚氨酯树脂粘结强度、光泽度、耐热性、耐黄变及耐水性不够理想，难以达到实际需要。
发明内容
本发明的目的就是针对现有技术的不足，提出一种水性聚氨酯树脂的制备方法，所得水性聚氨酯树脂具有优异的光泽度、粘结强度、耐水性、耐热性、耐磨性及耐黄变性。
为了实现上述目的，本发明采用如下技术方案：
一种水性聚氨酯树脂的制备方法，包括如下步骤：
S1、向反应釜内加入50～75份聚酯多元醇或/和聚醚多元醇，在90℃～110℃下真空脱水1～2小时，降温至50～63℃，得到物料A；
S2、向物料A中加入15～37份多异氰酸，在50～120℃条件下保温反应2～4小时，降温至70～80℃，得到B物料；
S3、向B物料中加入1～9份二羟甲基丙酸，然后将丙酮溶液溶解的1～5份1,4-丁二醇和5～12份三乙胺溶液滴加至反应釜中，40～60℃条件下保温反应1～3小时，加入有机金属催化剂0.01～0.5份、光稳定剂0.2～2份，40～60℃条件下保温反应1～3小时，得到C物料；
S4、C物料降温至室温后，加入18.5～26份三乙胺进行中和，加入1.2～5.3份后扩链剂，搅拌反应1～3小时，加入24～45份去离子水乳化分散，减压蒸馏，得到水性聚氨酯树脂。
优选的，所述步骤S1中所述聚酯多元醇或/和聚醚多元醇的分子量为500～10000g/mol。
优选的，所述步骤S2中所述多异氰酸为异佛尔酮异氰酸酯。
优选的，所述步骤S3中所述有机金属催化剂选自辛酸亚锡、有机铋催化剂、有机锆催化剂中的一种。
优选的，所述有机金属催化剂为有机铋催化剂。
优选的，所述步骤S3中所述光稳定剂为受阻胺光稳定剂。
优选的，所述步骤S4中后扩链剂选自三乙烯二胺、四乙烯五胺、乙二胺中的一种或多种。
优选的，所述步骤S4中加入后扩链剂后搅拌转速为800～1200r/min。
优选的，所述步骤S4中乳化转速为1200～1450r/min，乳化时间为30～45min。乳化时间越长，预聚体中-NCO基团与水反应的量越多，但乳化时间若过短，则乳胶，粒子不能充分均匀的分散，会导致乳液例子大小分布不均，因此乳化时间优选为30～45min。
与现有技术相比，本发明实现的有益效果：本发明所得水性聚氨酯树脂具有优异的粘结强度、光泽度、耐水性、耐热性、耐磨性及耐黄变性，其中二羟甲基丙酸作为亲水扩链剂，能够构成阴离子型自乳化性聚氨酯并提高聚氨酯分子量，选用高效、环保的有机铋催化剂，毒性小，同时可提高乳液的成膜效果。
具体实施方式
下面，用实施例来进一步说明本发明内容，但本发明的保护范围并不仅限于实施例。对本领域的技术人员在不背离本发明精神和保护范围的情况下做出的其它的变化和修改，仍包括在本发明保护范围之内。
实施例1
S1、向反应釜内加入50g分子量在500～10000g/mol的聚酯多元醇，在95℃下真空脱水1小时，降温至50℃，得到物料A；
S2、向物料A中加入15g异佛尔酮异氰酸酯，在60℃条件下保温反应2小时，降温至75℃，得到B物料；
S3、向B物料中加入1g二羟甲基丙酸，然后将丙酮溶液溶解的1g1,4-丁二醇和2g三乙胺溶液滴加至反应釜中，45℃条件下保温反应1小时，加入铋催化剂0.02g、光稳定剂0.2g，45℃条件下保温反应1小时，得到C物料；
S4、C物料降温至室温后，加入18.5g三乙胺进行中和，加入1.2g乙二胺，在800r/min的转速下搅拌反应1小时，加入24g去离子水乳化分散，其中，乳化转速为1200r/min，乳化时间为30min，最后减压蒸馏，得到水性聚氨酯树脂。
实施例2
S1、向反应釜内加入75g分子量在500～10000g/mol的聚醚多元醇，在95℃下真空脱水2小时，降温至50℃，得到物料A；
S2、向物料A中加入37g异佛尔酮异氰酸酯，在80℃条件下保温反应4小时，降温至75℃，得到B物料；
S3、向B物料中加入9g二羟甲基丙酸，然后将丙酮溶液溶解的5g1,4-丁二醇和12g三乙胺溶液滴加至反应釜中，55℃条件下保温反应3小时，加入有机铋催化剂0.5g、光稳定剂2g，55℃条件下保温反应3小时，得到C物料；
S4、C物料降温至室温后，加入26g三乙胺进行中和，加入5.3g三乙烯二胺，搅拌反应3小时，加入45g去离子水乳化分散，其中，乳化转速为1200r/min，乳化时间为30min，减压蒸馏，得到水性聚氨酯树脂。
实施例3
S1、向反应釜内加入60g分子量在500～10000g/mol的聚醚多元醇，在100℃下真空脱水1.5小时，降温至50℃，得到物料A；
S2、向物料A中加入25g异佛尔酮异氰酸酯，在100℃条件下保温反应3小时，降温至79℃，得到B物料；
S3、向B物料中加入6g二羟甲基丙酸，然后将丙酮溶液溶解的3g1,4-丁二醇和8g三乙胺溶液滴加至反应釜中，50℃条件下保温反应1小时，加入有机铋催化剂0.3g、光稳定剂1g，50℃条件下保温反应1小时，得到C物料；
S4、C物料降温至室温后，加入21g三乙胺进行中和，加入3.1g四乙烯五胺，搅拌反应2小时，加入32g去离子水乳化分散，其中，乳化转速为1200r/min，乳化时间为30min，减压蒸馏，得到水性聚氨酯树脂。
上述的具体实施方式只是示例性的，是为了更好地使本领域技术人员能够理解本专利，不能理解为是对本专利包括范围的限制；只要是根据本专利所揭示精神的所作的任何等同变更或修饰，均落入本专利包括的范围。

Claims (9)

1.一种水性聚氨酯树脂的制备方法，其特征在于，包括如下步骤：
S1、向反应釜内加入50～75份聚酯多元醇或/和聚醚多元醇，在90℃～110℃下真空脱水1～2小时，降温至50～63℃，得到物料A；
S2、向物料A中加入15～37份多异氰酸，在50～120℃条件下保温反应2～4小时，降温至70～80℃，得到B物料；
S3、向B物料中加入1～9份二羟甲基丙酸，然后将丙酮溶液溶解的1～5份1,4-丁二醇和5～12份三乙胺溶液滴加至反应釜中，40～60℃条件下保温反应1～3小时，加入有机金属催化剂0.01～0.5份、光稳定剂0.2～2份，40～60℃条件下保温反应1～3小时，得到C物料；
S4、C物料降温至室温后，加入18.5～26份三乙胺进行中和，加入1.2～5.3份后扩链剂，搅拌反应1～3小时，加入24～45份去离子水乳化分散，减压蒸馏，得到水性聚氨酯树脂。
2.如权利要求1所述的一种水性聚氨酯树脂的制备方法，其特征在于，所述步骤S1中所述聚酯多元醇或/和聚醚多元醇的分子量为500～10000g/mol。
3.如权利要求1所述的一种水性聚氨酯树脂的制备方法，其特征在于，所述步骤S2中所述多异氰酸为异佛尔酮异氰酸酯。
4.如权利要求1所述的一种水性聚氨酯树脂的制备方法，其特征在于，所述步骤S3中所述有机金属催化剂选自辛酸亚锡、有机铋催化剂、有机锆催化剂中的一种。
5.如权利要求1所述的一种水性聚氨酯树脂的制备方法，其特征在于，所述有机金属催化剂为有机铋催化剂。
6.如权利要求1所述的一种水性聚氨酯树脂的制备方法，其特征在于，所述步骤S3中所述光稳定剂为受阻胺光稳定剂。
7.如权利要求1所述的一种水性聚氨酯树脂的制备方法，其特征在于，所述步骤S4中后扩链剂选自三乙烯二胺、四乙烯五胺、乙二胺中的一种或多种。
8.如权利要求1所述的一种水性聚氨酯树脂的制备方法，其特征在于，所述步骤S4中加入后扩链剂后搅拌转速为800～1200r/min。
9.如权利要求1所述的一种水性聚氨酯树脂的制备方法，其特征在于，所述步骤S4中乳化转速为1200～1450r/min，乳化时间为30～45min。
CN201811118473.6A 2018-09-25 2018-09-25 一种水性聚氨酯树脂的制备方法 Pending CN110938185A (zh)

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Publication number Priority date Publication date Assignee Title
CN112694593A (zh) * 2021-01-14 2021-04-23 浙江大邦聚氨酯有限公司 一种聚氨酯树脂的生产方法
CN114133504A (zh) * 2022-01-07 2022-03-04 天津华映蔚蓝科技有限公司 一种水性油墨通用水性树脂及制备方法

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CN106432665A (zh) * 2016-10-08 2017-02-22 合肥科天水性科技有限责任公司 一种高性能水性聚氨酯树脂及其制备方法

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CN106432665A (zh) * 2016-10-08 2017-02-22 合肥科天水性科技有限责任公司 一种高性能水性聚氨酯树脂及其制备方法

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112694593A (zh) * 2021-01-14 2021-04-23 浙江大邦聚氨酯有限公司 一种聚氨酯树脂的生产方法
CN114133504A (zh) * 2022-01-07 2022-03-04 天津华映蔚蓝科技有限公司 一种水性油墨通用水性树脂及制备方法

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