CN105237721A - 一种高附着力水性聚氨酯树脂的制备方法 - Google Patents
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Abstract
本发明公开了一种高附着力水性聚氨酯树脂的制备方法,包括以下步骤:将对苯二甲酸酐聚酯二元醇和聚己二酸乙二醇酯二醇升温熔融,保温,接着真空脱水得到第一物料;将环己烷二亚甲基二异氰酸酯加入第一物料中,升温,保温,降温后加入乙二醇、1,4-丁二醇-2-磺酸钠、蓖麻油和N,N-二甲基甲酰胺,再加入邻苯基苯酚钠,升温,保温,得到第二物料;将第二物料降温后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,升温,保温得到第三物料;向第三物料中加入乙酸进行中和后,真空蒸馏得到高附着力水性聚氨酯树脂。本发明方法简单,所得水性聚氨酯树脂具有高附着力,而且硬度高,能满足市场的需要。
Description
技术领域
本发明涉及聚氨酯技术领域,尤其涉及一种高附着力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。但是目前聚氨酯制品绝大部分还是采用溶剂型聚氨酯树脂,大规模频繁发生的持续性雾霾天气不禁让人们认识到VOC排放的严重性,2015年2月1日起,国家开始对VOC含量高于420g/L的涂料企业征收4%涂料消费税以限制VOC的排放。水性聚氨酯树脂由于其无毒、低污染等优点越来越受到市场的认可和青睐。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。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。
为了提高水性聚氨酯的综合性能,国内外做了大量研究进行改性和采用不同活性的异氰酸酯改变合成进度,以提高水性聚氨酯的断裂伸长率、拉伸强度、粘结强度等。但目前常用的水性聚氨酯树脂硬度不高、附着力一般,因此急需要研发一种高附着力高硬度的产品来满足市场的需要。
发明内容
基于背景技术存在的技术问题,本发明提出了一种高附着力水性聚氨酯树脂的制备方法,方法简单,所得水性聚氨酯树脂具有高附着力,而且硬度高,能满足市场的需要。
本发明提出的一种高附着力水性聚氨酯树脂的制备方法,包括以下步骤:
S1、将对苯二甲酸酐聚酯二元醇和聚己二酸乙二醇酯二醇升温熔融,保温,接着真空脱水得到第一物料;
S2、将环己烷二亚甲基二异氰酸酯加入第一物料中,升温,保温,降温后加入乙二醇、1,4-丁二醇-2-磺酸钠、蓖麻油和N,N-二甲基甲酰胺,再加入邻苯基苯酚钠,升温,保温,得到第二物料;
S3、将第二物料降温后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,升温,保温得到第三物料;
S4、向第三物料中加入乙酸进行中和后,真空蒸馏得到高附着力水性聚氨酯树脂。
优选地,S1中,对苯二甲酸酐聚酯二元醇与聚己二酸乙二醇酯二醇的重量比为30~60:10~30。
优选地,S1中,将对苯二甲酸酐聚酯二元醇和聚己二酸乙二醇酯二醇升温至100~120℃,保温2~5h,接着真空脱水得到第一物料。
优选地,S2中,将环己烷二亚甲基二异氰酸酯加入第一物料中,升温至80~90℃,保温3~4h,降温至45~55℃后,加入乙二醇、1,4-丁二醇-2-磺酸钠、蓖麻油和N,N-二甲基甲酰胺,再加入邻苯基苯酚钠,升温至78~82℃,保温2~5h,得到第二物料。
优选地,对苯二甲酸酐聚酯二元醇、环己烷二亚甲基二异氰酸酯、乙二醇、1,4-丁二醇-2-磺酸钠、蓖麻油、N,N-二甲基甲酰胺和邻苯基苯酚钠的重量比为30~60:35~50:7~10:0.3~0.6:4~5:25~35:0.2~0.4。
优选地,S3中,含二乙醇胺和双(2-羟乙基)苯胺的混合溶液包括:二乙醇胺、双(2-羟乙基)苯胺和N,N-二甲基甲酰胺。
优选地,二乙醇胺、双(2-羟乙基)苯胺、N,N-二甲基甲酰胺和邻苯基苯酚钠的重量比为2~5:3~4:12~15:0.2~0.4。
优选地,S3中,将第二物料降温至35~45℃后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,滴加时间为0.4~0.8h,升温至60~70℃,保温0.4~0.6h得到第三物料。
优选地,二乙醇胺、乙酸和水的重量比为2~5:5~6:300~350。
由于同等条件下对苯二甲酸酐聚酯二元醇合成的水性聚氨酯胶膜硬度较高,本发明采用高硬度的对苯二甲酸酐聚酯二元醇为软段,二乙醇胺和双(2-羟乙基)苯胺配合作为阳离子型亲水扩链剂,1,4-丁二醇-2-磺酸钠作为磺酸盐型阴离子亲水扩链剂,分段逐步聚合的方式合成了硬度高、附着力强、封闭性好、抗渗油和抗色素渗出性能优越、耐水性好的聚氨酯树脂,而且阴阳离子联用并控制反应速度,提高乳液的稳定性和固含量,克服阳离子水性聚氨酯生产过程中容易暴聚凝胶的缺陷,降低生产凝胶风险。本发明所得水性聚氨酯具有批次稳定性好,生产风险小。
与现有技术相比,本发明具有以下优点:
1)本发明硬度高,附着力强,封闭性好,抗渗油和抗色素渗出性能优越,耐水性好;
2)本发明润湿性好,防止润湿剂对渗油性的影响;
3)本发明成膜速度快,漆膜透明,铅笔硬度达H~2H,耐水48h无异常,附着力为0级;
4)本发明渗透性强,抗渗油性好,漆膜表面与其他树脂相容性好;
5)本发明制备方法工艺稳定,反应易于控制,生产风险小。
附图说明
图1为本发明提出的一种高附着力水性聚氨酯树脂的制备方法的流程示意图。
具体实施方式
如图1所示,图1为本发明提出的一种高附着力水性聚氨酯树脂的制备方法的流程示意图。
参照图1,本发明提出的一种高附着力水性聚氨酯树脂的制备方法,包括以下步骤:
S1、将对苯二甲酸酐聚酯二元醇和聚己二酸乙二醇酯二醇升温熔融,保温,接着真空脱水得到第一物料;
S2、将环己烷二亚甲基二异氰酸酯加入第一物料中,升温,保温,降温后加入乙二醇、1,4-丁二醇-2-磺酸钠、蓖麻油和N,N-二甲基甲酰胺,再加入邻苯基苯酚钠,升温,保温,得到第二物料;
S3、将第二物料降温后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,升温,保温得到第三物料;
S4、向第三物料中加入乙酸进行中和后,真空蒸馏得到高附着力水性聚氨酯树脂。
下面,通过具体实施例对本发明的技术方案进行详细说明。
实施例1
本发明提出的一种高附着力水性聚氨酯树脂的制备方法,包括以下步骤:
S1、按重量份将30份对苯二甲酸酐聚酯二元醇和30份聚己二酸乙二醇酯二醇升温至100℃,保温5h,接着真空脱水得到第一物料;
S2、将35份环己烷二亚甲基二异氰酸酯加入第一物料中,升温至90℃,保温3h,降温至55℃后,加入7份乙二醇、0.6份1,4-丁二醇-2-磺酸钠、4份蓖麻油和35份N,N-二甲基甲酰胺,再加入0.2份邻苯基苯酚钠,升温至82℃,保温2h,得到第二物料;
S3、将第二物料降温至45℃后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,其中混合溶液包括:2份二乙醇胺、4份双(2-羟乙基)苯胺、12份N,N-二甲基甲酰胺,滴加时间为0.8h,升温至60℃,保温0.6h得到第三物料。
S4、向第三物料中加入5份乙酸进行中和后,真空蒸馏得到高附着力水性聚氨酯树脂。
实施例2
本发明提出的一种高附着力水性聚氨酯树脂的制备方法,包括以下步骤:
S1、按重量份将60份对苯二甲酸酐聚酯二元醇和10份聚己二酸乙二醇酯二醇升温至120℃,保温2h,接着真空脱水得到第一物料;
S2、将50份环己烷二亚甲基二异氰酸酯加入第一物料中,升温至80℃,保温4h,降温至45℃后,加入10份乙二醇、0.3份1,4-丁二醇-2-磺酸钠、5份蓖麻油和25份N,N-二甲基甲酰胺,再加入0.4份邻苯基苯酚钠,升温至78℃,保温5h,得到第二物料;
S3、将第二物料降温至35℃后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,其中混合溶液包括:5份二乙醇胺、3份双(2-羟乙基)苯胺、15份N,N-二甲基甲酰胺,滴加时间为0.4h,升温至70℃,保温0.4h得到第三物料。
S4、向第三物料中加入6份乙酸进行中和后,真空蒸馏得到高附着力水性聚氨酯树脂。
实施例3
本发明提出的一种高附着力水性聚氨酯树脂的制备方法,包括以下步骤:
S1、按重量份将40份对苯二甲酸酐聚酯二元醇和25份聚己二酸乙二醇酯二醇升温至105℃,保温4h,接着真空脱水得到第一物料;
S2、将40份环己烷二亚甲基二异氰酸酯加入第一物料中,升温至88℃,保温3.3h,降温至52℃后,加入8份乙二醇、0.5份1,4-丁二醇-2-磺酸钠、4.6份蓖麻油和32份N,N-二甲基甲酰胺,再加入0.25份邻苯基苯酚钠,升温至80℃,保温3h,得到第二物料;
S3、将第二物料降温至42℃后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,其中混合溶液包括:3份二乙醇胺、3.8份双(2-羟乙基)苯胺、13份N,N-二甲基甲酰胺,滴加时间为0.7h,升温至63℃,保温0.56h得到第三物料。
S4、向第三物料中加入5.5份乙酸进行中和后,真空蒸馏得到高附着力水性聚氨酯树脂。
实施例4
本发明提出的一种高附着力水性聚氨酯树脂的制备方法,包括以下步骤:
S1、按重量份将50份对苯二甲酸酐聚酯二元醇和15份聚己二酸乙二醇酯二醇升温至115℃,保温3h,接着真空脱水得到第一物料;
S2、将45份环己烷二亚甲基二异氰酸酯加入第一物料中,升温至82℃,保温3.6h,降温至48℃后,加入9份乙二醇、0.4份1,4-丁二醇-2-磺酸钠、4.8份蓖麻油和30份N,N-二甲基甲酰胺,再加入0.35份邻苯基苯酚钠,升温至79℃,保温4h,得到第二物料;
S3、将第二物料降温至38℃后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,其中混合溶液包括:4份二乙醇胺、3.5份双(2-羟乙基)苯胺、14份N,N-二甲基甲酰胺,滴加时间为0.5h,升温至67℃,保温0.48h得到第三物料。
S4、向第三物料中加入5.8份乙酸进行中和后,真空蒸馏得到高附着力水性聚氨酯树脂。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (9)
1.一种高附着力水性聚氨酯树脂的制备方法,其特征在于,包括以下步骤:
S1、将对苯二甲酸酐聚酯二元醇和聚己二酸乙二醇酯二醇升温熔融,保温,接着真空脱水得到第一物料;
S2、将环己烷二亚甲基二异氰酸酯加入第一物料中,升温,保温,降温后加入乙二醇、1,4-丁二醇-2-磺酸钠、蓖麻油和N,N-二甲基甲酰胺,再加入邻苯基苯酚钠,升温,保温,得到第二物料;
S3、将第二物料降温后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,升温,保温得到第三物料;
S4、向第三物料中加入乙酸进行中和后,真空蒸馏得到高附着力水性聚氨酯树脂。
2.根据权利要求1所述高附着力水性聚氨酯树脂的制备方法,其特征在于,S1中,对苯二甲酸酐聚酯二元醇与聚己二酸乙二醇酯二醇的重量比为30~60:10~30。
3.根据权利要求1或2所述高附着力水性聚氨酯树脂的制备方法,其特征在于,S1中,将对苯二甲酸酐聚酯二元醇和聚己二酸乙二醇酯二醇升温至100~120℃,保温2~5h,接着真空脱水得到第一物料。
4.根据权利要求1-3任一项所述高附着力水性聚氨酯树脂的制备方法,其特征在于,S2中,将环己烷二亚甲基二异氰酸酯加入第一物料中,升温至80~90℃,保温3~4h,降温至45~55℃后,加入乙二醇、1,4-丁二醇-2-磺酸钠、蓖麻油和N,N-二甲基甲酰胺,再加入邻苯基苯酚钠,升温至78~82℃,保温2~5h,得到第二物料。
5.根据权利要求1-4任一项所述高附着力水性聚氨酯树脂的制备方法,其特征在于,对苯二甲酸酐聚酯二元醇、环己烷二亚甲基二异氰酸酯、乙二醇、1,4-丁二醇-2-磺酸钠、蓖麻油、N,N-二甲基甲酰胺和邻苯基苯酚钠的重量比为30~60:35~50:7~10:0.3~0.6:4~5:25~35:0.2~0.4。
6.根据权利要求1-5任一项所述高附着力水性聚氨酯树脂的制备方法,其特征在于,S3中,含二乙醇胺和双(2-羟乙基)苯胺的混合溶液包括:二乙醇胺、双(2-羟乙基)苯胺和N,N-二甲基甲酰胺。
7.根据权利要求6所述高附着力水性聚氨酯树脂的制备方法,其特征在于,二乙醇胺、双(2-羟乙基)苯胺、N,N-二甲基甲酰胺和邻苯基苯酚钠的重量比为2~5:3~4:12~15:0.2~0.4。
8.根据权利要求1-7任一项所述高附着力水性聚氨酯树脂的制备方法,其特征在于,S3中,将第二物料降温至35~45℃后,再滴加含二乙醇胺和双(2-羟乙基)苯胺的混合溶液,滴加时间为0.4~0.8h,升温至60~70℃,保温0.4~0.6h得到第三物料。
9.根据权利要求1-8任一项所述高附着力水性聚氨酯树脂的制备方法,其特征在于,二乙醇胺、乙酸和水的重量比为2~5:5~6:300~350。
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