CN115073914B - 一种蓝色水性聚氨酯色浆及其制备方法 - Google Patents
一种蓝色水性聚氨酯色浆及其制备方法 Download PDFInfo
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- CN115073914B CN115073914B CN202210725986.3A CN202210725986A CN115073914B CN 115073914 B CN115073914 B CN 115073914B CN 202210725986 A CN202210725986 A CN 202210725986A CN 115073914 B CN115073914 B CN 115073914B
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- aqueous polyurethane
- diisocyanate
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- Processes Of Treating Macromolecular Substances (AREA)
Abstract
本发明公开了一种蓝色水性聚氨酯色浆及其制备方法,涉及水性聚氨酯技术领域,本发明利用小分子染料反应活性特点和通过反应条件的控制,将含有发色基团的染料与二异氰酸酯反应合成出具有发色基团结构的二异氰酸酯,这种蓝色的二异氰酸酯可代替普通二异氰酸酯参与合成蓝色水性聚氨酯,实现小分子染料的高分子化和水性化。本发明还提供了可与之配合使用的无色水性聚氨酯,调配不同蓝色深度的色浆。本发明克服了低分子染料在迁移、安全性等方面的不足;与无色水性聚氨酯混合使用,无需加入分散剂;同时还具有环保、无污染、性能可调以及可加工性。
Description
技术领域:
本发明涉及水性聚氨酯技术领域,具体涉及一种蓝色水性聚氨酯色浆及其制备方法。
背景技术:
水性聚氨酯以水为分散介质,避免了传统有机溶剂污染环境、对人体有害等缺点,是绿色环保、安全可靠的新型聚氨酯材料。水性聚氨酯材料已广泛应用于轻纺、色浆、印染、皮革加工、涂料、胶粘剂、造纸等行业。安全性是未来的主要趋势,在各行业中对绿色产品的要求越来越多。随着科技的进步,人们对具有特殊功能的水性聚氨酯材料需求日益增加。
在染料领域,蒽醌系染料是含有蒽醌结构的各种染料,蒽醌型染料有良好的耐光牢度和耐热性能,色彩艳丽,应用范围广,已发展成为色谱全、性能好的染料类别,在合成染料工业中占有重要地位。
对于色浆的使用,传统色浆染料通常是将聚氨酯与小分子颜料或染料直接混合而成,这种办法虽然简单,但由于颜料或染料与聚合物之间的相容性不好,产品的乳化性和功能性缺乏稳定性和耐久性,出现沉降、胶化等现象。另外在成膜过程中,颜料或染料有迁移现象,产品分散不均匀时,颜色浮于漆膜表面,导致漆膜表面浮色发花,且迁移到表面的颜料或染料对人体和环境也有极大的危害。
逐步加聚法在合成以聚氨酯、聚脲为主链的高分子染料反应中较为常见。将染料母体接枝到聚氨酯分子链中,既保留了染料对光的吸收性和发色性等特点,又具有高分子材料的耐迁移和可加工等特性。目前新型色浆材料的研究已经展开,但应用于实际的新型色不多,由于它性能优异,其应用具有广阔的前景,越来越受到国内外人士的关注。
发明内容:
本发明所要解决的技术问题在于提供一种蓝色水性聚氨酯色浆及其制备方法,利用小分子染料反应活性特点和通过反应条件的控制,将含有发色基团的染料与二异氰酸酯反应合成出具有发色基团结构的二异氰酸酯,这种蓝色的二异氰酸酯可代替普通二异氰酸酯参与合成高固含量阴-非离子型蓝色水性聚氨酯,实现小分子染料的高分子化和水性化。本发明还提供了可与之配合使用的无色水性聚氨酯,用于调配不同蓝色深度的色浆。
本发明所要解决的技术问题采用以下的技术方案来实现:
本发明的第一个目的是提供一种蓝色水性聚氨酯色浆,由以下重量份的原料混合而成:蓝色水性聚氨酯1~10份、无色水性聚氨酯10~100份、卡松防腐剂0.01~1份。
本发明将蓝色水性聚氨酯和无色水性聚氨酯复配得到色浆,根据需要配制不同蓝色深度的色浆。
所述蓝色水性聚氨酯由以下重量份的原料制成:二异氰酸酯15~50份、小分子染料0.1~20份、大分子二元醇20~70份、二元醇扩链剂1~10份、非离子扩链剂1~7份、阴离子扩链剂2~15份、催化剂0.01~0.1份、后扩链剂0.5~5份、中和剂1~10份、N-甲基吡咯烷酮1~10份、丁酮50~200份、去离子水100~300份。
小分子染料与二异氰酸酯反应得到含有发色基团的二异氰酸酯,含有发色基团的二异氰酸酯与大分子二元醇、二元醇扩链剂、非离子扩链剂、阴离子扩链剂、后扩链剂反应得到蓝色水性聚氨酯。
优选地,所述二异氰酸酯选自甲苯二异氰酸酯(TDI)、异佛尔酮二异氰酸酯(IPDI)、二苯基甲烷二异氰酸酯(MDI)、六次亚甲基二异氰酸酯(HDI)中的至少一种。
优选地,所述大分子二元醇选自聚乙二醇(PEG)、聚氧化丙烯二醇(PPG)、聚醚二元醇、聚四氢呋喃醚二醇(PTMG)、聚碳酸脂二醇(PCDL)、聚己二酸-1,4-丁二醇酯二元醇(PBA)、聚己内酯二元醇(PCL)中的至少一种。
优选地,所述二元醇扩链剂选自乙二醇(EG)、1,2-丙二醇(MPD)、1,4-丁二醇(BDO)、新戊二醇(NPG)、1,6-己二醇(HDO)、一缩二乙二醇(DEG)中的至少一种。
优选地,所述非离子扩链剂选自双[2-(2-羟基乙氧基)乙基]醚、聚乙烯乙二醇甲醚、三羟甲基丙烷聚乙二醇单甲醚(TMPEG)、非离子二元醇Ymer N120、聚四亚甲基醚二醇双对氨基苯甲酸酯中的至少一种。
优选地,所述阴离子扩链剂选自二羟甲基丙酸(DMPA)、二羟甲基丁酸(DMBA)、1,2-丙二醇-3-磺酸钠、1,4-丁二醇-2-磺酸钠中的至少一种。
优选地,所述小分子染料选自以下结构式中的至少一种:
优选地,所述催化剂选自有机锡类催化剂和胺类催化剂中的至少一种。
优选地,所述后扩链剂选自乙二胺基乙磺酸钠、乙二胺、丁二胺、二乙烯三胺、异佛尔酮二胺、N,N-二甲基乙二胺中的至少一种。
优选地,所述中和剂为三乙胺、氢氧化钠、氢氧化钾、氨水、碳酸氢钠中的至少一种。
本发明的第二个目的是提供一种蓝色水性聚氨酯的制备方法,包括如下步骤:
(1)向反应器中加入二异氰酸酯和催化剂,加热,然后缓慢加入采用丁酮和N-甲基吡咯烷酮溶解的小分子染料溶液,在惰性气体保护下进行反应;
(2)加入经真空脱水的大分子二元醇,在惰性气体保护下进行反应;
(3)加入二元醇扩链剂、非离子扩链剂、阴离子扩链剂和催化剂,用丁酮调节粘度,在惰性气体保护下进行反应;
(4)加入中和剂反应,加入含后扩链剂的去离子水乳化,得到蓝色水性聚氨酯。
本发明的有益效果是:
1、本发明将发色基团以共价键的方式引入到聚氨酯材料中,可长久保持聚氨酯材料的显色性能,兼具发色体的色彩性、光吸收性及高分子材料的成膜性、耐迁移性、耐热性特点,有效克服低分子染料在受热迁移方面的不足。
2、本发明在聚氨酯的合成工艺中将小分子染料作为一种扩链剂,由于小分子染料本身基团反应活性的原因,使得小分子染料的接入量受到大大限制,本发明合成出了含有发色基团的二异氰酸酯,克服了小分子染料本身反应活性基团的影响,提高了小分子染料的接入量,使得反应易于控制。
3、常规聚氨酯材料在户外使用过程中会逐渐发生颜色发黄的现象,影响材料外观。将小分子染料接入到水性聚氨酯材料可以消除聚氨酯材料黄变而对外观造成的影响,且制备的蓝色水性聚氨酯色浆显色效果好、性能稳定,适宜工业化生产,且不污染环境。
4、将小分子染料引入到聚氨酯分子中,相比传统色浆将染料物理分散在聚氨酯中,本发明中染料的分散达到了分子级别,且无需再加入分散剂,染料的使用效率大大提高;在相同条件下也减少了染料的使用,节省了染料的使用成本;且合成的蓝色水性聚氨酯固含量高,可与其它水性树脂混合,使用操作简单方便且显色均匀。
5、本发明合成的高固含量蓝色水性聚氨酯为阴-非离子型,其乳液稳定性远远好于传统阴离子型水性聚氨酯,因此可以与其它阴离子型水性聚氨酯相互混合而不会导致乳液破乳,解决其与不同阴离子水性聚氨酯混合而使乳液不稳定的问题,扩展了蓝色水性聚氨酯的使用范围。
具体实施方式:
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解,下面结合具体实施例,进一步阐述本发明。
实施例1
无色水性聚氨酯的制备:加入50g TDI和100g PTMG(Mn=2000)到反应体系中,在氮气氛围下90℃反应2h;然后降温至50℃以下,加入8.5g 1,4-丁二醇、9.0g DMBA和0.2g二月桂酸二丁基锡(T12),再加入60g丁酮调节粘度,于70℃反应3h;降温至30℃以下,加入6g三乙胺成盐0.5h,加入390g去离子水乳化,得到水性聚氨酯乳液,保存备用。
蓝色水性聚氨酯的制备:在三口烧瓶中加入12g IPDI和1滴T12加热至70℃,加入已溶解在10mL丁酮和2mLN-甲基吡咯烷酮中的0.18g DYE2于烧瓶中,在氮气氛围下70℃反应2h;将20g PTMG(Mn=2000)加入到体系中,在90℃反应2h;然后降温至50℃以下,加入2.1g 1,4-丁二醇、双[2-(2-羟基乙氧基)乙基]醚0.5g、1.4g DMBA和1滴T12,再加入6mL丁酮调节粘度,于70℃反应3h;降温至30℃以下,加入0.95g三乙胺成盐0.5h,加入45g去离子水(乙二胺基乙磺酸钠0.85g)溶液,高速剪切乳化1h,减压蒸馏去除有机溶剂,得到蓝色水性聚氨酯,保存备用。
蓝色水性聚氨酯色浆:取上述制备的蓝色水性聚氨酯2份、水性聚氨酯10份、卡松防腐剂0.01份,混合均匀,制得蓝色水性聚氨酯色浆。
实施例2
蓝色水性聚氨酯的制备:在三口烧瓶中加入9.4g TDI和1滴T12加热至70℃,加入已溶解在10mL丁酮和3mLN-甲基吡咯烷酮中的0.36g DYE1于烧瓶中,在氮气氛围下70℃反应2h;将20g PTMG(Mn=2000)加入到体系中,在90℃反应2h;然后降温至50℃以下,加入2.06g 1,4-丁二醇、双[2-(2-羟基乙氧基)乙基]醚0.5g、1.6g DMPA和1滴T12,再加入5mL丁酮调节粘度,于70℃反应3h;降温至30℃以下,加入1.09g三乙胺成盐0.5h,加入35g去离子水(乙二胺基乙磺酸钠0.70g)溶液,高速剪切乳化1h,减压蒸馏去除有机溶剂,得到蓝色水性聚氨酯,保存备用。
蓝色水性聚氨酯色浆:取上述制备的蓝色水性聚氨酯2份、实施例1制备的水性聚氨酯10份、卡松防腐剂0.01份,混合均匀,制得蓝色水性聚氨酯色浆。
实施例3
蓝色水性聚氨酯的制备:在三口烧瓶中加入12g IPDI和1滴T12加热至70℃,加入已溶解在15mL丁酮和4mLN-甲基吡咯烷酮中的1.54g DYE2于烧瓶中,在氮气氛围下70℃反应2h;将20g PCDL(Mn=2000)加入到反应体系中,90℃反应2h;然后降温至50℃以下,加入1.6g 1,4-丁二醇、双[2-(2-羟基乙氧基)乙基]醚0.7g、1.4g DMPA和1滴T12,再加入8mL丁酮调节粘度,于70℃反应3h;将体系降温至30℃以下,加入三乙胺1.15g,成盐0.5h,加入40g去离子水(乙二胺基乙磺酸钠0.80g)溶液,高速剪切乳化1h,减压蒸馏去除有机溶剂,得到蓝色水性聚氨酯,保存备用。
蓝色水性聚氨酯色浆:取上述制备的蓝色水性聚氨酯2份、实施例1制备的水性聚氨酯10份、卡松防腐剂0.01份,混合均匀,制得蓝色水性聚氨酯色浆。
实施例4
蓝色水性聚氨酯的制备:在三口烧瓶中加入10g TDI和1滴T12加热至70℃,加入已溶解在25mL丁酮和8mLN-甲基吡咯烷酮中的3.08g DYE2于烧瓶中,在氮气氛围下70℃反应2h;将20g PTMG(Mn=2000)加入到反应体系中,在90℃下反应2h;然后降温至50℃以下,加入1.44g 1,4-丁二醇、双[2-(2-羟基乙氧基)乙基]醚0.65g、1.5g DMBA和1滴T12,再加入5mL丁酮调节粘度,于70℃反应3h;将体系降温至30℃以下,加入1.09g三乙胺成盐0.5h,加入35g去离子水(乙二胺基乙磺酸钠0.85g)溶液,高速剪切乳化1h,减压蒸馏去除有机溶剂,得到蓝色水性聚氨酯,保存备用。
蓝色水性聚氨酯色浆:取上述制备的蓝色水性聚氨酯2份、实施例1制备的水性聚氨酯10份、卡松防腐剂0.01份,混合均匀,制得蓝色水性聚氨酯色浆。
对比例1
取上述实施例1制备的无色水性聚氨酯50g、染料DYE10.1 g、TEGO Dispers 745W分散剂0.018g、卡松防腐剂0.05g,混合均匀,制得蓝色水性聚氨酯色浆。
对比例2
取上述实施例1制备的无色水性聚氨酯50g、染料DYE20.45 g、TEGO Dispers 745W分散剂0.081g、卡松防腐剂0.05g,混合均匀,制得蓝色水性聚氨酯色浆。
对上述实施例1~4和对比例1~2制备的蓝色水性聚氨酯色浆进行性能测试,根据GB/T 3920-2008《纺织品色牢度试验耐摩擦色牢度》和GB/T 3921-2008《纺织品色牢度试验耐皂洗色牢度》测试由蓝色水性聚氨酯色浆所形成涂层织物的干、湿摩擦牢度和耐洗牢度,并通过标准灰色样卡评级。
表1中的蓝色水性聚氨酯色浆颜色按照RAL-K7国际标准色卡对比,色卡每页有5个颜色块:5×2cm,共215种颜色,其外形尺寸:15×5×1.6cm。
表1
检测项目 | 实施例1 | 实施例2 | 实施例3 | 实施例4 | 对比例1 | 对比例2 |
蓝色水性聚氨酯外观 | 亮蓝色 | 龙胆蓝 | 钢蓝色 | 钴蓝色 | 淡蓝色 | 夜蓝色 |
耐干摩色牢度/级 | 4~5 | 5 | 5 | 4~5 | 3 | 3 |
耐湿摩色牢度/级 | 4 | 4~5 | 4~5 | 4 | 3 | 3 |
水洗牢度褪色/级 | 4~5 | 5 | 5 | 4~5 | 3~4 | 3 |
水洗牢度沾色/级 | 4~5 | 4~5 | 4~5 | 4~5 | 3~4 | 3 |
由表1可以看出,本发明提供的蓝色水性聚氨酯色浆既兼具聚氨酯材料良好的粘接性、柔韧性、耐迁移等优点,又保留了染料对光的吸收性和发色性等特点,在使用过程中无需加入分散剂,同时满足人们对于涂料环保无害的要求。
以上显示和描述了本发明的基本原理和主要特征和本发明的优点。本行业的技术人员应该了解,本发明不受上述实施例的限制,上述实施例和说明书中描述的只是说明本发明的原理,在不脱离本发明精神和范围的前提下,本发明还会有各种变化和改进,这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。
Claims (6)
1.一种蓝色水性聚氨酯色浆,其特征在于,所述蓝色水性聚氨酯色浆由以下重量份的原料混合而成:蓝色水性聚氨酯1~10份、无色水性聚氨酯10~100份、卡松防腐剂0.01~1份;
所述蓝色水性聚氨酯由以下重量份的原料制成:二异氰酸酯15~50份、小分子染料0.1~20份、大分子二元醇20~70份、二元醇扩链剂1~10份、非离子扩链剂1~7份、阴离子扩链剂2~15份、催化剂0.01~0.1份、后扩链剂0.5~5份、中和剂1~10份、N-甲基吡咯烷酮1~10份、丁酮50~200份、去离子水100~300份;
所述蓝色水性聚氨酯的制备方法包括如下步骤:
(1)向反应器中加入二异氰酸酯和催化剂,加热,然后缓慢加入采用丁酮和N-甲基吡咯烷酮溶解的小分子染料溶液,在惰性气体保护下进行反应;
(2)加入经真空脱水的大分子二元醇,在惰性气体保护下进行反应;
(3)加入二元醇扩链剂、非离子扩链剂、阴离子扩链剂和催化剂,用丁酮调节粘度,在惰性气体保护下进行反应;
(4)加入中和剂反应,加入含后扩链剂的去离子水乳化,得到蓝色水性聚氨酯;
所述非离子扩链剂选自双[2-(2-羟基乙氧基)乙基]醚、三羟甲基丙烷聚乙二醇单甲醚中的至少一种;
所述小分子染料选自以下结构式中的至少一种:
所述二元醇扩链剂选自乙二醇、1,2-丙二醇、1,4-丁二醇、新戊二醇、1,6-己二醇、一缩二乙二醇中的至少一种。
2.根据权利要求1所述的蓝色水性聚氨酯色浆,其特征在于:所述二异氰酸酯选自甲苯二异氰酸酯、异佛尔酮二异氰酸酯、二苯基甲烷二异氰酸酯、六亚甲基二异氰酸酯中的至少一种。
3.根据权利要求1所述的蓝色水性聚氨酯色浆,其特征在于:所述大分子二元醇选自聚乙二醇、聚氧化丙烯二醇、聚四氢呋喃醚二醇、聚碳酸酯二醇、聚己二酸-1,4-丁二醇酯二元醇、聚己内酯二元醇中的至少一种。
4.根据权利要求1所述的蓝色水性聚氨酯色浆,其特征在于:所述阴离子扩链剂选自二羟甲基丙酸、二羟甲基丁酸、1,2-丙二醇-3-磺酸钠、1,4-丁二醇-2-磺酸钠中的至少一种。
5.根据权利要求1所述的蓝色水性聚氨酯色浆,其特征在于:所述催化剂选自有机锡类催化剂和胺类催化剂中的至少一种;所述中和剂为三乙胺、氢氧化钠、氢氧化钾、氨水、碳酸氢钠中的至少一种。
6.根据权利要求1所述的蓝色水性聚氨酯色浆,其特征在于:所述后扩链剂选自乙二胺基乙磺酸钠、乙二胺、丁二胺、二乙烯三胺、异佛尔酮二胺、N,N-二甲基乙二胺中的至少一种。
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