CN112940215A - 一种单组分水性聚氨酯乳液及其制备方法 - Google Patents
一种单组分水性聚氨酯乳液及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种单组分水性聚氨酯乳液及其制备方法和应用,属于水型乳液技术领域。本发明提供了一种单组分水性聚氨酯乳液,由包括以下质量百分含量的组分制得:水55~63%、聚四氢呋喃10~20%、4,4'‑二苯甲撑基异氰酸酯10~12%、第一扩链剂2.5~3%、亲水扩链剂4~4.7%、有机硅树脂1~4.5%、中和剂2.8~3%和消泡剂0.5~0.6%,所述第一扩链剂为多元醇类扩链剂或多元胺类扩链剂。本发明通过使用亲水扩链剂以及控制亲水扩链剂的用量,使水性聚氨酯乳液的分散稳定性更好,耐水性更佳;通过添加一定比例的有机硅树脂,使单组分水性聚氨酯乳液的附着力明显提升,达到划格实验一级以上。
Description
技术领域
本发明涉及水型乳液技术领域,尤其涉及一种单组分水性聚氨酯乳液及其制备方法。
背景技术
随着社会经济活动的持续进行对空气,土壤带来的污染,而导致的人与环境的关系带来一定的影响,以往的含有溶剂型乳液、涂料、胶黏剂等材料对环境的迫害已不言而喻。环境污染治理得到了关注。为了保证人们所呼吸的空气、食入的食品安全健康的基本需求,减少溶剂对环境的迫害,提高空气及环境的质量,水型乳液能够满足以上社会要求。
聚醚型单组分水性聚氨酯(WPU)弹性优良,成膜性好,具有非常优异的耐低温性,质地柔软,应用领域广。聚醚型单组分水性聚氨酯是由聚四氢呋喃(PTMEG)为软段、4,4'-二苯甲撑基异氰酸酯(MDI)、常规扩链剂、亲水扩链剂、中和剂等单体通过乳液聚合而成的一种聚醚型聚氨酯,有着长亚甲基链的柔顺性,又有芳环的韧性。
现有技术中的单组分聚氨酯的固含量均在32~35%,附着力(测试方法为划格实验)都未达到1级,基本处于2~3级,存在着固含量和附着力等级低的问题。
发明内容
有鉴于此,本发明的目的在于提供一种单组分水性聚氨酯乳液及其制备方法。本发明提供的单组分水性聚氨酯乳液具有较高的固含量和附着力等级。
为了实现上述发明目的,本发明提供以下技术方案:
本发明提供了一种单组分水性聚氨酯乳液,由包括以下质量百分含量的组分制得:
水55~63%、聚四氢呋喃10~20%、4,4'-二苯甲撑基异氰酸酯10~12%、第一扩链剂2.5~3%、亲水扩链剂4~4.7%、有机硅树脂1~4.5%、中和剂2.8~3%和消泡剂0.5~0.6%,所述第一扩链剂为多元醇类扩链剂或多元胺类扩链剂。
优选地,所述亲水扩链剂为磺酸类扩链剂或羧酸类扩链剂。
优选地,所述羧酸类扩链剂为2,2-二羟甲基丙酸和/或2,2-二羟甲基丁酸。
优选地,所述多元醇类扩链剂包括1,4丁二醇、乙二醇、聚乙二醇、三羟甲基丙烷、甘油和季戊四醇中的一种或多种。
优选地,所述多元胺类扩链剂包括3,3'-二氯-4,4'-二氨基二苯基甲烷、乙二胺和N,N-二羟基(二异丙基)苯胺中的一种或多种。
优选地,所述有机硅树脂为乙烯基MQ硅树脂或三甲基硅烷氧基硅酸酯。
本发明还提供了上述技术方案所述的单组分水性聚氨酯乳液的制备方法,包括以下步骤:
将聚四氢呋喃醚二醇、4,4'-二苯甲撑基异氰酸酯和亲水扩链剂混合,进行加成反应,得到加成产物;
将所述加成产物、第一扩链剂和有机硅树脂混合,进行扩链反应,得到扩链产物;
将所述扩链产物、中和剂和消泡剂混合,加入水进行乳化,得到所述单组分水性聚氨酯乳液。
优选地,所述加成反应的温度为60~80℃,时间为3~5h。
优选地,所述乳化的温度为4~10℃。
优选地,其特征在于,所述乳化的搅拌速率为1500~2500r/min。
本发明提供了一种单组分水性聚氨酯乳液,由包括以下质量百分含量的组分制得:水55~63%、聚四氢呋喃10~20%、4,4'-二苯甲撑基异氰酸酯10~12%、第一扩链剂2.5~3%、亲水扩链剂4~4.7%、有机硅树脂1~4.5%、中和剂2.8~3%和消泡剂0.5~0.6%,所述第一扩链剂为多元醇类扩链剂或多元胺类扩链剂。本发明通过使用亲水扩链剂以及控制亲水扩链剂的用量,使水性聚氨酯乳液的分散稳定性更好,耐水性更佳;通过添加一定比例的有机硅树脂,使单组分水性聚氨酯乳液的附着力明显提升,达到划格实验一级以上。
与现有技术相比,本发明具有如下有益的技术效果:
本发明在尽量不改变粘度的前提下,利用有机硅树脂降低乳液聚合物的亲水性,同时控制原料的用量得到合适的交联密度来进一步降低乳液聚合物的亲水性,确保乳液干燥后形成的涂覆层致密、稳定、疏水,以此来提高水性聚氨酯乳液的固含量和附着力等级,增加水性聚氨酯在涂料、胶黏剂、油墨等的应用宽度。实施例的数据表明,本发明提供的单组分水性聚氨酯乳液不经额外与市售固化剂混配即可单独使用,固含量为37~42%,附着力达到1级,且经60℃水浴24h,附着力依旧达到1级。
具体实施方式
本发明提供了一种单组分水性聚氨酯乳液,由包括以下质量百分含量的组分制得:
水55~63%、聚四氢呋喃(PTMEG)10~20%、4,4'-二苯甲撑基异氰酸酯(MDI)10~12%、第一扩链剂2.5~3%、亲水扩链剂4~4.7%、有机硅树脂1~4%、中和剂2.8~3%和消泡剂0.5~0.6%,所述第一扩链剂为多元醇类扩链剂或多元胺类扩链剂。
在本发明中,若无特殊说明,本发明使用的原料均为本领域市售商品。
在本发明中,所述聚四氢呋喃的数均分子量优选为650~3000。
在本发明中,所述4,4'-二苯甲撑基异氰酸酯优选为聚合异氰酸酯MDI-50或异氰酸酯MDI-100。
在本发明中,所述亲水扩链剂优选为磺酸类扩链剂或羧酸类扩链剂。
在本发明中,所述羧酸类扩链剂优选为2,2-双羟甲基丙酸(DMPA)和/或2,2-双羟甲基丁酸(DMBA)。
在本发明中,所述磺酸类扩链剂优选为乙二胺基乙磺酸钠,所述乙二胺基乙磺酸钠优选以乙二胺基乙磺酸钠水溶液(质量浓度为50%的AAS水溶液)的形式加入。
在本发明中,所述多元醇类扩链剂优选包括1,4丁二醇(BDO)、乙二醇(EG)、聚乙二醇(PEG)、三羟甲基丙烷(TMP)、甘油和季戊四醇中的一种或多种,所述多元醇类扩链剂占水性聚氨酯乳液固体份的重量比优选为0.5%~4%。在本发明中,所述聚乙二醇更优选为PEG100。
在本发明中,所述多元胺类扩链剂优选包括3,3'-二氯-4,4'-二氨基二苯基甲烷(MOCA)、乙二胺(EDA)和N,N-二羟基(二异丙基)苯胺(HPA)中的一种或多种,所述多元胺类扩链剂占水性聚氨酯乳液固体份的重量比优选为0.01%~1%。
在本发明中,所述有机硅树脂优选为乙烯基MQ硅树脂或三甲基硅烷氧基硅酸酯。
在本发明中,所述中和剂优选为TEA、氢氧化钠或氢氧化钾。
在本发明中,所述消泡剂优选为聚氧乙烯聚氧丙烯季戊四醇醚、聚氧丙烯甘油醚或聚二甲基硅氧烷。
在本发明中,所述水优选为蒸馏水。
本发明还提供了上述技术方案所述的单组分水性聚氨酯乳液的制备方法,包括以下步骤:
将聚四氢呋喃、4,4'-二苯甲撑基异氰酸酯和亲水扩链剂混合,进行加成反应,得到加成产物;
将所述加成产物、第一扩链剂和有机硅树脂混合,进行扩链反应,得到扩链产物;
将所述扩链产物、中和剂和消泡剂混合,加入水进行乳化,得到所述单组分水性聚氨酯乳液。
本发明将聚四氢呋喃、4,4'-二苯甲撑基异氰酸酯和亲水扩链剂混合,进行加成反应,得到加成产物。
在本发明中,所述混合优选为先将所述聚四氢呋喃和亲水扩链剂混合进行脱水后,再加入所述4,4'-二苯甲撑基异氰酸酯。在本发明中,所述脱水的温度优选为110~130℃,更优选为120℃,真空压力优选为0.1~0.4MPa,更优选为0.25MPa,时间优选为1~4h,更优选为3h。在本发明中,所述脱水优选在搅拌的条件下进行,所述搅拌的转速优选为50~150r/min,更优选为100r/min。
脱水后,本发明优选还包括降温至70℃恒温1h的步骤。
在本发明中,所述加成反应的温度优选为60~80℃,更优选为65~75℃,最优选为70℃,时间优选为3~5h。在本发明的具体实施例中,所述加成反应的终点优选为至反应NCO含量稳定不变。在本发明中,所述加成反应的过程中,所述MDI中的异氰酸酯基和羟基发生加成反应,生成氨基甲酸酯,使产物数均分子量增大。
得到加成产物后,本发明将所述加成产物、第一扩链剂和有机硅树脂混合,进行扩链反应,得到扩链产物。
在本发明中,所述扩链反应的过程中优选加入有机溶剂,所述有机溶剂优选为丙酮、丁酮或甲乙酮,所述有机溶剂的重量优选为反应物总重量的40~120%,更优选为70%。
在本发明中,所述扩链反应的时间优选为2~3h。
得到扩链产物后,本发明将所述扩链产物、中和剂和消泡剂混合,加入水进行乳化,得到所述单组分水性聚氨酯乳液。
得到扩链产物后,本发明优选将所述扩链产物降温至10℃以下保温1h,再与中和剂和消泡剂混合。
在本发明中,所述进行乳化的反应体系的酸碱度通过中和剂调节,所述进行乳化的反应体系的pH值优选为6.5~8。
在本发明中,所述乳化的温度优选为4~10℃,所述乳化的时间优选为3~5h。
在本发明中,所述乳化的搅拌速率优选为1500~2500r/min,更优选为2000r/min。
在本发明中,所述水的加入速度优选为100~200mL/min。
所述乳化完成后,本发明优选将所得乳化产物进行抽真空脱溶剂,回收溶剂,得到所述单组分水性聚氨酯乳液。本发明对所述抽真空脱溶剂的具体方式没有特殊的限定。
为了进一步说明本发明,下面结合实例对本发明提供的单组分水性聚氨酯乳液及其制备方法进行详细地描述,但不能将它们理解为对本发明保护范围的限定。
实施例1
一种单组分水性聚氨酯乳液由包括以下质量百分含量的组分制得:蒸馏水63%,聚四氢呋喃10%、MDI-5012%、第一扩链剂2.5%、亲水扩链剂(DMPA)4.7%、有机硅树脂乙烯基MQ硅树脂4.3%、中和剂TEA3%和消泡剂聚氧乙烯聚氧丙烯季戊四醇醚0.5%,所述第一扩链剂为1,4丁二醇。
PTMEG和亲水扩链剂在120℃,转速100r/min,真空0.25MPa下混合3h,再降温至70℃恒温1h,然后加入MDI保持70℃反应5h测试NCO含量稳定不变,再加入第一扩链剂进行扩链反应,同时加入有机硅树脂,增加溶剂丙酮,丙酮的质量为反应物总重量的70%,反应时间为2h,然后降温至10℃保温1h,加入中和剂,调节体系pH值至6.5,提高转速至2000r/min,以加水速度100mL/min加入蒸馏水直至发生相转变,水的量为反应物总重量的1.5倍,扭矩明显变小,乳化3h,加入消泡剂,抽真空脱溶剂,回收溶剂,得到单组分水性聚氨酯乳液。
对制得的单组分水性聚氨酯乳液性能进行测试,测试结果如表1所示。
表1实施例1制得的单组分水性聚氨酯乳液的性能
项目 | 固含量 | 附着力(划格实验) | 粒径/μm | 存储稳定性 |
数据 | 37% | 2 | 50 | 7~8个月 |
实施例2
一种单组分水性聚氨酯乳液由包括以下质量百分含量的组分制得:蒸馏水60%、聚四氢呋喃18%、MDI-5011%、第一扩链剂2.6%、亲水扩链剂(DMBA)4%、有机硅树脂三甲基硅烷氧基硅酸酯1%、中和剂TEA2.8%和消泡剂聚二甲基硅氧烷0.6%,所述第一扩链剂为乙二醇。
PTMEG和亲水扩链剂在110℃,转速150r/min,真空0.4MPa下混合3h,再降温至80℃恒温1h,然后加入MDI保持80℃反应5h测试NCO含量稳定不变,再加入第一扩链剂进行扩链反应,同时加入有机硅树脂,增加溶剂丙酮,丙酮的质量为反应物总重量的40%,反应时间为2h,然后降温至10℃保温1h,加入中和剂,调节体系pH值至8,提高转速至2000r/min,以加水速度200mL/min加入蒸馏水直至发生相转变,扭矩明显变小,乳化3h,加入消泡剂,抽真空脱溶剂,回收溶剂,得到单组分水性聚氨酯乳液。
对制得的单组分水性聚氨酯乳液性能进行测试,测试结果如表2所示。
表2实施例2制得的单组分水性聚氨酯乳液的性能
项目 | 固含量 | 附着力(划格实验) | 粒径/μm | 存储稳定性 |
数据 | 39% | 1 | 45 | 6~8个月 |
实施例3
一种单组分水性聚氨酯乳液由包括以下质量百分含量的组分制得:蒸馏水58%、聚四氢呋喃16%、MDI-5011%、第一扩链剂3%、亲水扩链剂(DMBA)4.5%、有机硅树脂有机硅树脂乙烯基MQ硅树脂4%、中和剂TEA3%和消泡剂聚二甲基硅氧0.5%,所述第一扩链剂为BDO。
PTMEG和亲水扩链剂在130℃,转速150r/min,真空0.4MPa下混合3h,再降温至70℃恒温1h,然后加入MDI保持80℃反应5h测试NCO含量稳定不变,再加入第一扩链剂进行扩链反应,同时加入有机硅树脂,增加溶剂丙酮,丙酮的质量为反应物总重量的120%,反应时间为2h,然后降温至10℃保温1h,加入中和剂,调节体系pH值至8,提高转速至2000r/min,以加水速度200mL/min加入蒸馏水直至发生相转变,扭矩明显变小,乳化3h,抽真空脱溶剂5h,回收溶剂,得到单组分水性聚氨酯乳液。
对制得的单组分水性聚氨酯乳液性能进行测试,测试结果如表3所示。可知,固含量升高至42%,且附着力稳定达到1级,60℃下水浴24h,附着力无下降。
表3实施例3制得的单组分水性聚氨酯乳液的性能
项目 | 固含量 | 附着力(划格实验) | 粒径/μm | 存储稳定性 |
数据 | 42% | 1 | 60 | 6~7个月 |
以上所述仅是本发明的优选实施方式,并非对本发明作任何形式上的限制。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (10)
1.一种单组分水性聚氨酯乳液,其特征在于,由包括以下质量百分含量的组分制得:
水55~63%、聚四氢呋喃10~20%、4,4'-二苯甲撑基异氰酸酯10~12%、第一扩链剂2.5~3%、亲水扩链剂4~4.7%、有机硅树脂1~4.5%、中和剂2.8~3%和消泡剂0.5~0.6%,所述第一扩链剂为多元醇类扩链剂或多元胺类扩链剂。
2.根据权利要求1所述的单组分水性聚氨酯乳液,其特征在于,所述亲水扩链剂为磺酸类扩链剂或羧酸类扩链剂。
3.根据权利要求2所述的单组分水性聚氨酯乳液,其特征在于,所述羧酸类扩链剂为2,2-二羟甲基丙酸和/或2,2-二羟甲基丁酸。
4.根据权利要求1所述的单组分水性聚氨酯乳液,其特征在于,所述多元醇类扩链剂包括1,4丁二醇、乙二醇、聚乙二醇、三羟甲基丙烷、甘油和季戊四醇中的一种或多种。
5.根据权利要求1所述的单组分水性聚氨酯乳液,其特征在于,所述多元胺类扩链剂包括3,3'-二氯-4,4'-二氨基二苯基甲烷、乙二胺和N,N-二羟基(二异丙基)苯胺中的一种或多种。
6.根据权利要求1所述的单组分水性聚氨酯乳液,其特征在于,所述有机硅树脂为乙烯基MQ硅树脂或三甲基硅烷氧基硅酸酯。
7.权利要求1~6任一项所述的单组分水性聚氨酯乳液的制备方法,其特征在于,包括以下步骤:
将聚四氢呋喃醚二醇、4,4'-二苯甲撑基异氰酸酯和亲水扩链剂混合,进行加成反应,得到加成产物;
将所述加成产物、第一扩链剂和有机硅树脂混合,进行扩链反应,得到扩链产物;
将所述扩链产物、中和剂和消泡剂混合,加入水进行乳化,得到所述单组分水性聚氨酯乳液。
8.根据权利要求7所述的制备方法,其特征在于,所述加成反应的温度为60~80℃,时间为3~5h。
9.根据权利要求7所述的制备方法,其特征在于,所述乳化的温度为4~10℃。
10.根据权利要求7或9所述的制备方法,其特征在于,所述乳化的搅拌速率为1500~2500r/min。
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