CN111138963A - 一种高性能自交联水性聚氨酯自消光树脂的合成工艺 - Google Patents

一种高性能自交联水性聚氨酯自消光树脂的合成工艺 Download PDF

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CN111138963A
CN111138963A CN201911225316.XA CN201911225316A CN111138963A CN 111138963 A CN111138963 A CN 111138963A CN 201911225316 A CN201911225316 A CN 201911225316A CN 111138963 A CN111138963 A CN 111138963A
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刘斌
许修棋
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Anhui Shengda Biopharmaceutical Co Ltd
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Abstract

本发明公开了一种高性能自交联水性聚氨酯自消光树脂的合成工艺,包括以下步骤:取WPU1与WPU2,按照质量比为1:0.1~0.3加至分散设备,再加入WPU1和WPU2总质量的0.5~2%的有机硅流平剂、0.05‑0.1%的消泡剂、0.5~2%的聚氨酯缔合型增稠剂,调整25℃时的粘度为800~2000mPa.s,制得高性能自交联水性聚氨酯自消光树脂。本发明通过乳液在成膜过程中实现常温交联,形成高分子-高分子的分子间的较粘,增加了粒子和粒子之间有效的粘合,提高了涂层的成膜性、通透性,对基材的附着力,耐刮擦,耐化学品性能较好;在工艺上大幅度的提高了生产效率,极大的增加了经济效益。

Description

一种高性能自交联水性聚氨酯自消光树脂的合成工艺
技术领域
本发明涉及一种高性能自交联水性聚氨酯自消光树脂的合成工艺,属于水性聚氨酯涂料领域。
背景技术
皮革涂饰剂是对合成革进行后处理,赋予合成革特殊的光泽和手感的一种产品。消光性涂饰剂具有更柔和、自然、优雅的外观,广泛应用于皮革涂饰、纸张涂饰涂层、印花胶浆、纺织品涂层、特种涂料等。
传统的消光水性聚氨酯树脂是在聚氨酯分散体中加人填充料、微蜡粉、无机二氧化硅等消光剂,涂膜干燥后消光剂浮于涂膜表面产生微观的不平整,从而达到消光效果。然而消光粉的外添加导致体系的不稳定,同时涂饰的表面出现泛白、灰暗、挂霜等现象,严重影响表面涂饰产品的外观。
目前使用较多的是自消光水性聚氨酯树脂,通过合成大粒径且不易变形的分散体粒子,在成膜过程中,粒子之间相互融合组装形成连续的粗糙表面,依靠增加胶膜的漫反射获得消光性能,进而获得消光效果较好的涂层。然而涂层的乳胶粒子比较大,成膜过程中乳胶粒子不能较好的融合,使得成膜不完善,造成涂膜物化性能下降,强度低,对基材的附着力差,通透性差,不能展现涂膜基材的色彩,出现雾蒙的现象,为了避免这种情况,需要加入大量的交联剂,如氮丙啶、异氰酸酯或封闭型交联剂等,来增强聚氨酯颗粒与颗粒间的粘结性,提高涂层成膜物性,如耐刮擦、耐磨性、耐候性等。
氮丙啶、异氰酸酯交联剂属于双组份,一般在12小时内必须用完,过期失效,客户使用极为不便,若碰到特殊情况未及时用完,会造成一定的经济损失;封闭型交联剂需要110℃以上的高温,20分钟左右解封后达到交联效果,能耗较高,因此经济效益下降。
发明内容
针对上述现有技术存在的问题,本发明提供一种高性能自交联水性聚氨酯自消光树脂的合成工艺。
为了实现上述目的,一种有机硅改性含羧基交联基团的水性聚氨酯自消光树脂WPU1的制备方法,包括以下步骤:
称取多异氰酸酯、分子量为1000-10000的聚合物多元醇、乙二醇封端有机硅聚醚硅油OFX-3667、亲水扩链剂二羟甲基丙酸、三羟甲基丙烷、异佛尔酮二胺、水合肼、磺酸盐亲水扩链剂VESTAMIN A95、聚氨酯缔合型增稠剂,分步混合反应,得粒径为1500-3000nm的自消光树脂WPU1。
作为优选,WPU1的制备方法,具体包括以下步骤:
取1mol多异氰酸酯、0.16-0.35mol分子量为1000-10000的聚合物多元醇、0.046mol乙二醇封端有机硅聚醚硅油OFX-3667,加热至85-95℃聚合反应2小时,然后加入0.014mol三羟甲基丙烷,0.08-0.09mol二羟甲基丙酸,0.74mol N-甲基吡咯烷酮溶液,加热至70-85℃聚合反应3-5小时,待-NCO的残留量为5.8-6.8%,得预产物;
将预产物加至分散设备,高速分散状态下加入0.08mol三乙胺搅拌1-3分钟,加入0.058mol的VESTAMIN A95保温在50-60℃反应5-15min,加水制备分散体乳液,再把0.46mol水合肼和0.018-0.025异佛尔酮二胺混合,用2.4mol水稀释后加入,搅拌20-30min,加水乳化,获得水性聚氨酯树脂,再加入水性聚氨酯树脂质量0.5-3%的聚氨酯缔合型增稠剂,调整25℃粘度为500-2000mPa.s,制备得到固含量为35±1%的水性聚氨酯自消光树脂WPU1。
另外,本发明还提供了一种含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2的制备方法,包括以下步骤:
取多异氰酸酯、分子量为1000-10000的聚合物多元醇、非离子亲水扩链剂TegomerD3403、羟基环氧扩链剂甘油二缩水甘油基醚、三羟甲基丙烷、1.4丁二醇、异佛尔酮二胺、乙二胺,分步混合反应,制备粒径为300-600nm的非离子水性聚氨酯粘结树脂WPU2,成膜性能较好,具有优异的基材附着力,作为粘结性树脂。
作为优选,WPU2的制备方法,具体包括以下步骤:
取1mol多异氰酸酯、0.18-0.38mol分子量为1000-10000的聚合物多元醇,加热至85-95℃聚合反应2h,然后加入0.059mol非离子亲水扩链剂Tegomer D3403、0.181mol羟基环氧扩链剂甘油二缩水甘油基醚、0.055mol三羟甲基丙烷、0.123mol 1.4丁二醇、0.99molN-甲基吡咯烷酮溶液,加热至70-80℃聚合反应3-4h,至-NCO的残留量为3.1-5.2%,得预产物;
将预产物加至分散设备,搅拌冷却到40℃,将分散设备调为高速,加水乳化,制备分散体乳液,把0.152mol异佛尔酮二胺和0.173mol乙二胺混合,用6mol水稀释后加入乳液中,继续搅拌10min,获得固含量为35±1%的含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2。
另外,本发明还提供了一种高性能自交联水性聚氨酯自消光树脂的合成工艺,包括以下步骤:
取所述WPU1与所述WPU2,按照质量比为1:0.1~0.3加至分散设备,再加入WPU1和WPU2总质量的0.5~2%的有机硅流平剂、0.05-0.1%的消泡剂、0.5~2%的聚氨酯缔合型增稠剂,调整25℃时的粘度为800~2000mPa.s,制得高性能自交联水性聚氨酯自消光树脂。
作为优选,所述WPU1中的多异氰酸酯采用六次甲基二异氰酸酯、异佛尔酮二异氰酸酯或二环己基甲烷二异氰酸酯中的至少一种;
所述WPU2中的多异氰酸酯为甲苯二异氰酸酯、六次甲基二异氰酸酯、异佛尔酮二异氰酸酯或二环己基甲烷二异氰酸酯中的至少一种。
作为优选,所述WPU1和WPU2中的聚合物多元醇采用聚醚多元醇或聚酯多元醇中的至少一种。
作为优选,所述聚醚多元醇采用聚四氢呋喃多元醇、聚氧化丙烯多元醇中的至少一种。
作为优选,所述聚酯多元醇采用聚己二酸己二醇酯二元醇、聚己二酸丁二醇酯二元醇、聚己二酸新戊二醇酯二醇、聚己二酸乙二醇酯二元醇或聚己內酯二醇中的至少一种。
与现有技术相比,本发明先制备有机硅改性含羧基交联基团的水性聚氨酯自消光树脂WPU1(粒径1500-3000nm)、含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2(粒径300-600nm),然后将WPU1、WPU2以不同的比例混合,由于羧基的官能团与环氧官能团分别存在于不同的分散体WPU1和WPU2中,被连续的水相分隔,不会发生反应,因此可以制备常温稳定存放的高性能自交联水性聚氨酯自消光树脂,使用成膜时,随着水分、三乙胺的挥发,体系的pH由8-9变为酸性,体系中WPU1和WPU2粒子融合,羧基基团与环氧基团接触,常温产生交联反应,形成高分子-高分子之间的交联,增加了粒子和粒子之间有效的粘合,提高了涂层的成膜性、通透性,对基材的附着力,耐刮擦,耐化学品性能较好。本发明实现了常温交联反应,解决了双组份交联剂存在的使用时间限制问题(一般12小时以内必须使用完),封闭型交联剂存在的热能消耗问题(120℃以上的高温,10分钟以上的固化时间),在工艺上大幅度的提高了生产效率,极大的增加了经济效益。
本发明将WPU1、WPU2以不同的比例混合,合成了不同光泽度的水性聚氨酯自消光树脂,如45度角反射光(%)≤5,成膜有很好的通透性感和绒毛油滑手感,主要用于真皮、PU革、PVC革、PET等表面消光处理;45度角反射光(%)≤10,成膜性优异,通透性好,手感舒适,应用于纸张,包装材料等表面消光处理,具有淡雅高档的视觉效果。
具体实施方式
下述实施例是对于本发明内容的进一步说明以作为对本发明技术内容的阐释,但本发明的实质内容并不仅限于下述实施例所述,本领域的普通技术人员可以且应当知晓任何基于本发明实质精神的简单变化或替换均应属于本发明所要求的保护范围。
实施例1
一种有机硅改性含羧基交联基团的水性聚氨酯自消光树脂WPU1的制备方法,具体包括以下步骤:
在装有搅拌器、温度计、回流冷凝器的反应瓶中,加入222g(1mol)异佛尔酮二异氰酸酯(多异氰酸酯)、481g(0.331mol)分子量为2000的聚氧化丙烯二元醇、111g(0.046mol)乙二醇封端有机硅聚醚硅油OFX-3667,加热至85℃聚合反应2小时,降温至60℃,然后加入1.85g(0.014mol)三羟甲基丙烷,11.1g(0.082mol)二羟甲基丙酸,72.5g(0.74mol)N-甲基吡咯烷酮溶液,加热至80℃聚合反应4小时,待-NCO的残留量为6.1%,得预产物;
将预产物加至分散设备,高速分散状态下加入0.08mol三乙胺搅拌2分钟,加入24.4g(0.058mol,有效成分的摩尔数)的VESTAMIN A95,保温在50℃反应15min,加水制备分散体乳液,把18.4g(0.46mol)水合肼和3.7g(0.020mol)异氟尔酮二胺混合,用2.4mol水稀释后加入,搅拌20min,加水乳化,获得水性聚氨酯自消光树脂,再加入24.4g聚氨酯缔合型增稠剂HEUR-A,调整至25℃粘度为1800mPa.s,制备得到粒径为2120nm、固含量为34.9%的水性聚氨酯自消光树脂WPU1
实施例2
一种有机硅改性含羧基交联基团的水性聚氨酯自消光树脂WPU1,包括以下步骤:
在装有搅拌器、温度计、回流冷凝器的反应瓶中,加入222g(1mol)异佛尔酮二异氰酸酯(多异氰酸酯)、481g(0.331mol)分子量为2000的聚四氢呋喃二元醇、111g(0.046mol)乙二醇封端有机硅聚醚硅油OFX-3667,加热至85℃聚合反应2小时,降温至60℃,然后加入1.85g(0.014mol)三羟甲基丙烷,11.1g(0.082mol)二羟甲基丙酸,72.5g(0.74mol)N-甲基吡咯烷酮溶液,加热至80℃聚合反应4小时,待-NCO的残留量为6.3%,得预产物;
将预产物加至分散设备,高速分散状态下加入0.08mol三乙胺搅拌2分钟,加入24.4g(0.058mol,有效成分的摩尔数)的VESTAMIN A95,保温在50℃反应15min,加水制备分散体乳液,把18.4g(0.46mol)水合肼和3.7g(0.020mol)异氟尔酮二胺混合,用2.4mol水稀释后加入,搅拌20min,加水乳化,获得水性聚氨酯自消光树脂WPU1,再加入19.5g聚氨酯缔合型增稠剂HEUR-A,调整至25℃粘度为1600mPa.s,制备得到粒径为1870nm、固含量为35.2%的水性聚氨酯自消光树脂WPU1。
实施例3
一种有机硅改性含羧基交联基团的水性聚氨酯自消光树脂WPU1,包括以下步骤:
在装有搅拌器、温度计、回流冷凝器的反应瓶中,加入222g(1mol)异佛尔酮二异氰酸酯(多异氰酸酯)、481g(0.331mol)分子量为2000的聚氧化丙烯二元醇、111g(0.046mol)乙二醇封端有机硅聚醚硅油OFX-3667,加热至85℃聚合反应2小时,降温至60℃,然后加入1.85g(0.014mol)三羟甲基丙烷,11.1g(0.082mol)二羟甲基丙酸,72.5g(0.74mol)N-甲基吡咯烷酮溶液,加热至80℃聚合反应4小时,待-NCO的残留量为5.9%,得预产物;
将预产物加至分散设备,高速分散状态下加入0.08mol三乙胺搅拌2分钟,加入24.4g(0.058mol,有效成分的摩尔数)的VESTAMIN A95,保温在55℃反应10min,加水制备分散体乳液,把18.4g(0.46mol)水合肼和3.7g(0.020mol)异佛尔酮二胺混合,用2.4mol水稀释后加入,搅拌20min,加水乳化,获得的水性聚氨酯自消光树脂WPU1,再加入20g聚氨酯缔合型增稠剂HEUR-A,调整至25℃粘度为1700mPa.s,制备得到粒径为1730nm、固含量为34.8%的水性聚氨酯自消光树脂WPU1。
实施例4
将实施例1中采用的222g异佛尔酮二异氰酸酯替换为262g(1mol)二环己基甲烷二异氰酸酯;其余工艺步骤、参数与实施例1相同。
实施例5
将实施例2中采用的222g异佛尔酮二异氰酸酯替换为262g(1mol)二环己基甲烷二异氰酸酯;其余工艺步骤、参数与实施例2相同。
实施例6
将实施例3中采用的222g异佛尔酮二异氰酸酯替换为262g(1mol)二环己基甲烷二异氰酸酯;其余工艺步骤、参数与实施例3相同。
实施例7
一种含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2的制备方法,具体包括以下步骤:
在装有搅拌器、温度计、回流冷凝器的反应瓶中,取222g(1mol)异佛尔酮二异氰酸酯(多异氰酸酯),592g(0.197mol)分子量为3000的聚己二酸新戊二醇二元醇,加热至85℃聚合反应2h,加入74g(0.059mol)非离子亲水扩链剂Tegomer D3403、37g(0.181mol)羟基环氧扩链剂甘油二缩水甘油基醚、7.4g(0.055mol)三羟甲基丙烷、11.1g(0.123mol)1.4丁二醇、100g(0.99mol)N-甲基吡咯烷酮溶剂,加热至70℃聚合反应4h,至-NCO的残留量为3.9%,得预产物;
将预产物加至分散设备,搅拌冷却到40℃,将分散设备调为高速,加水乳化,制备分散体乳液,把25.9g(0.152mol)异佛尔酮二胺和11g(0.173mol)乙二胺混合,用108g(6mol)水稀释后加入乳液中,继续搅拌10min,加水乳化,获得固含量为35.3%的非离子水性聚氨酯粘结树脂WPU2,粒径为430nm。
实施例8
一种含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2的制备方法,具体包括以下步骤:
取222g(1mol)异佛尔酮二异氰酸酯(多异氰酸酯),592g(0.197mol)分子量为3000的聚四氢呋喃二元醇,加热至85℃聚合反应2h,加入74g(0.059mol)非离子亲水扩链剂Tegomer D3403、37g(0.181mol)羟基环氧扩链剂甘油二缩水甘油基醚,7.4g(0.055mol)三羟甲基丙烷,11.1g(0.123mol)1.4丁二醇,100g(0.99mol)N-甲基吡咯烷酮溶液,加热至75℃聚合反应3.5h,至-NCO的残留量为4.1%,得预产物;
将预产物加至分散设备,搅拌冷却到40℃,将分散设备调为高速,加水乳化,制备分散体乳液,把25.9g(0.152mol)异佛尔酮二胺和11g(0.173mol)乙二胺混合,用108g(6mol)水稀释后加入乳液中,继续搅拌10min,加水乳化,获得固含量为35%的含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2。
实施例9
一种含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2的制备方法,具体包括以下步骤:
取222g(1mol)异佛尔酮二异氰酸酯(多异氰酸酯),592g(0.197mol)分子量为3000的聚碳酸酯二元醇,加热至85℃聚合反应2h,加入74g(0.059mol)非离子亲水扩链剂Tegomer D3403、37g(0.181mol)羟基环氧扩链剂甘油二缩水甘油基醚,7.4g(0.055mol)三羟甲基丙烷,11.1g(0.123mol)1.4丁二醇,100g(0.99mol)N-甲基吡咯烷酮溶液,加热至80℃聚合反应3h,至-NCO的残留量为4.3%,得预产物;
将预产物加至分散设备,搅拌冷却到40℃,将分散设备调为高速,加水乳化,制备分散体乳液,把25.9g(0.152mol)异佛尔酮二胺和11g(0.173mol)乙二胺混合,用108g(6mol)水稀释后加入乳液中,继续搅拌10min,加水乳化,获得粒径480nm、固含量为34.6%的含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2。
实施例10
将222g异佛尔酮二异氰酸酯替换为262g(1mol)二环己基甲烷二异氰酸酯,其余工艺步骤、参数与实施例7相同。
实施例11
将222g异佛尔酮二异氰酸酯替换为164g(1mol)六亚甲基二异氰酸酯,其余工艺步骤、参数与实施例7相同。
实施例12
将222g异佛尔酮二异氰酸酯替换为250g(1mol)二苯基甲烷二异氰酸酯,其余工艺步骤、参数与实施例8相同。
实施例13
将222g异佛尔酮二异氰酸酯替换为262g(1mol)二环己基甲烷二异氰酸酯,其余工艺步骤、参数与实施例9相同。
实施例14
将222g异佛尔酮二异氰酸酯替换为164g(1mol)六亚甲基二异氰酸酯,其余工艺步骤、参数与实施例8相同。
实施例19
一种高性能自交联水性聚氨酯自消光树脂的合成工艺,包括以下步骤:取WPU1与WPU2,按照质量比为1:0.15加至分散设备,再加入WPU1和WPU2总质量的2%的有机硅流平剂BYK333、0.05%消泡剂104(陶氏DF104消泡剂)、0.8%的聚氨酯缔合型增稠剂HEUR-A,调整25℃时的粘度为1900mPa.s,制得高性能自交联水性聚氨酯自消光树脂。
实施例20
一种高性能自交联水性聚氨酯自消光树脂的合成工艺,包括以下步骤:取WPU1与WPU2,按照质量比为1:0.2加至分散设备,再加入WPU1和WPU2总质量的2%的有机硅流平剂BYK333、0.05%消泡剂104、0.6%的聚氨酯缔合型增稠剂HEUR-A,调整25℃时的粘度为1500mPa.s,制得高性能自交联水性聚氨酯自消光树脂。
实施例21
一种高性能自交联水性聚氨酯自消光树脂的合成工艺,包括以下步骤:取WPU1与WPU2,按照质量比为1:0.30加至分散设备,再加入WPU1和WPU2总质量的0.1%机硅流平剂BYK333、0.08%消泡剂104、0.5%的聚氨酯缔合型增稠剂HEUR-A,调整25℃时的粘度为1400mPa.s,制得高性能自交联水性聚氨酯自消光树脂。
对上述实施例19-21制得高性能自交联水性聚氨酯自消光树脂的性能,进行测试:
附着力测试:将树脂涂膜在皮革上,干燥后,在测试样表面划10*40个1mm*1mm小网格,用毛刷将测试区的碎片刷干净,用3M610胶带牢牢黏住被测试小网格,并用橡皮檫用力擦拭胶带,已加大胶带与被测区域的接触面积及力度,用手抓住胶带一端,在垂直方向(90°)迅速扯下胶带,观测脱落情况,附着力大于等于4B为合格。5B:无胶膜脱落;4B:划线交叉点有小块脱落,总脱落面积小于5%;3B:划线交叉点有小块脱落,脱落面积在5%-15%;2B:划线交叉点有成块脱落,脱落面积在15%-35%;1B:划线交叉点有成块脱落,脱落面积在35%-65%。
耐刮擦性测试:在树脂中加入1%红色颜料,涂膜在皮革上,干燥后,将其固定在测试机上,磨棒上包上白布,对样品干摩擦20次(来回为一次),测试后白布上的颜色进行色卡对比,级别越高,耐磨性越好。具体分级为:一级:掉色严重,二级:掉色,三级:轻微掉色,四级:不掉色
具体测试结果如下表1所示。
表1本发明制得自消光树脂的性能
附着力 耐刮擦
实施例19 5B 4级
实施例20 5B 4级
实施例21 5B 4级
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换或改进等,均应包含在本发明的保护范围之内。

Claims (9)

1.一种有机硅改性含羧基交联基团的水性聚氨酯自消光树脂WPU1的制备方法,其特征在于,包括以下步骤:
称取多异氰酸酯、分子量为1000-10000的聚合物多元醇、乙二醇封端有机硅聚醚硅油OFX-3667、亲水扩链剂二羟甲基丙酸、三羟甲基丙烷、异佛尔酮二胺、水合肼、磺酸盐亲水扩链剂VESTAMIN A95、聚氨酯缔合型增稠剂,分步混合反应,得粒径为1500-3000nm的自消光树脂WPU1。
2.根据权利要求1所述的一种有机硅改性含羧基交联基团的水性聚氨酯自消光树脂WPU1的制备方法,其特征在于,具体包括以下步骤:
取1mol多异氰酸酯、0.16-0.35mol分子量为1000-10000的聚合物多元醇、0.046mol乙二醇封端有机硅聚醚硅油OFX-3667,加热至85-95℃聚合反应2小时,然后加入0.014mol三羟甲基丙烷,0.08-0.09mol二羟甲基丙酸,0.74mol N-甲基吡咯烷酮溶液,加热至70-85℃聚合反应3-5小时,待-NCO的残留量为5.8-6.8%,得预产物;
将预产物加至分散设备,高速分散状态下加入0.08mol三乙胺搅拌1-3分钟,加入0.058mol的VESTAMIN A95保温在50-60℃反应5-15min,加水制备分散体乳液,再把0.46mol水合肼和0.018-0.025mol异佛尔酮二胺混合,用2.4mol水稀释后加入,搅拌20-30min,加水乳化,获得水性聚氨酯树脂,再加入水性聚氨酯树脂质量0.5-3%的聚氨酯缔合型增稠剂,调整25℃粘度为500-2000mPa.s,制备得到固含量为35±1%的水性聚氨酯自消光树脂WPU1。
3.一种含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2的制备方法,其特征在于,包括以下步骤:取多异氰酸酯、分子量为1000-10000的聚合物多元醇、非离子亲水扩链剂Tegomer D3403、羟基环氧扩链剂甘油二缩水甘油基醚、三羟甲基丙烷、1.4丁二醇、异佛尔酮二胺、乙二胺,分步混合反应,制备粒径为300-600nm的非离子水性聚氨酯粘结树脂WPU2。
4.根据权利要求3所述的一种含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2的制备方法,其特征在于,具体包括以下步骤:
取1mol多异氰酸酯、0.18-0.38mol分子量为1000-10000的聚合物多元醇,加热至85-95℃聚合反应2h,然后加入0.059mol非离子亲水扩链剂Tegomer D3403、0.181mol羟基环氧扩链剂甘油二缩水甘油基醚、0.055mol三羟甲基丙烷、0.123mol 1.4丁二醇、0.99mol N-甲基吡咯烷酮溶液,加热至70-80℃聚合反应3-4h,至-NCO的残留量为3.1-5.2%,得预产物;
将预产物加至分散设备,搅拌冷却到40℃,将分散设备调为高速,加水乳化,制备分散体乳液,把0.152mol异佛尔酮二胺和0.173mol乙二胺混合,用6mol水稀释后加入乳液中,继续搅拌10min,加水乳化,获得固含量为35±1%的含环氧交联基团的非离子水性聚氨酯粘结树脂WPU2。
5.一种高性能自交联水性聚氨酯自消光树脂的合成工艺,其特征在于,包括以下步骤:
取权利要求1-2任一项所述WPU1与权利要求3-4任一项所述WPU2,按照质量比为1:0.1~0.3加至分散设备,再加入WPU1和WPU2总质量的0.5~2%的有机硅流平剂、0.05-0.1%的消泡剂、0.5~2%的聚氨酯缔合型增稠剂,调整25℃时的粘度为800~2000mPa.s,制得高性能自交联水性聚氨酯自消光树脂。
6.根据权利要求5所述的一种高性能自交联水性聚氨酯自消光树脂的合成工艺,其特征在于,所述WPU1中的多异氰酸酯采用六次甲基二异氰酸酯、异佛尔酮二异氰酸酯或二环己基甲烷二异氰酸酯中的至少一种;
所述WPU2中的多异氰酸酯为甲苯二异氰酸酯、六次甲基二异氰酸酯、异佛尔酮二异氰酸酯或二环己基甲烷二异氰酸酯中的至少一种。
7.根据权利要求5所述的一种高性能自交联水性聚氨酯自消光树脂的合成工艺,其特征在于,所述WPU1和WPU2中的聚合物多元醇采用聚醚多元醇或聚酯多元醇中的至少一种。
8.根据权利要求7所述的一种高性能自交联水性聚氨酯自消光树脂的合成工艺,其特征在于,所述聚醚多元醇采用聚四氢呋喃多元醇、聚氧化丙烯多元醇中的至少一种。
9.根据权利要求7所述的一种高性能自交联水性聚氨酯自消光树脂的合成工艺,其特征在于,所述聚酯多元醇采用聚己二酸己二醇酯二元醇、聚己二酸丁二醇酯二元醇、聚己二酸新戊二醇酯二醇、聚己二酸乙二醇酯二元醇或聚己內酯二醇中的至少一种。
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