CN109553752A - 一种低吸水率的织物涂层用水性聚氨酯乳液及其制备方法 - Google Patents

一种低吸水率的织物涂层用水性聚氨酯乳液及其制备方法 Download PDF

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CN109553752A
CN109553752A CN201811487700.2A CN201811487700A CN109553752A CN 109553752 A CN109553752 A CN 109553752A CN 201811487700 A CN201811487700 A CN 201811487700A CN 109553752 A CN109553752 A CN 109553752A
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chain extender
added
aqueous polyurethane
water absorption
low water
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武小康
赫长生
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NANTONG GAOMENG NEW MATERIAL CO Ltd
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Abstract

本发明涉及一种低吸水率的织物涂层用水性聚氨酯乳液及其制备方法，包括：步骤一、先制得多元醇混合物；步骤二、将多元醇混合物和亲水扩链剂完全溶解后，加入二异氰酸酯制得溶液A；步骤三、向溶液A中加入二元扩链剂和三元扩链剂，制成预聚体B；步骤四、将制得的预聚体B中加入三乙胺中和，加入胺基类后扩链剂得到乳液C；步骤五、将制得的乳液C脱酮减压制得乳液，即为低吸水率的织物涂层用水性聚氨酯乳液。通过引入含不同活性胺基类后扩链剂，活性高的伯胺基和异氰酸酯反应，接入到分子链中，活性低的胺基留在分子侧链中，配合异氰酸酯类外添加固化剂制备了一种低吸水率水性聚氨酯。

Description

一种低吸水率的织物涂层用水性聚氨酯乳液及其制备方法
技术领域
本发明涉及纺织化工的聚氨酯制备领域，尤其涉及一种低吸水率的织物涂层用水性聚氨酯乳液及其制备方法。
背景技术
水性聚氨酯是一种水为分散介质的聚氨酯体系，相对于溶剂型聚氨酯，水性聚氨酯具有低VOC、生产成本低、树脂可设计性强、环保无污染等特点，在大力倡导环保的当今社会水性聚氨酯受到广泛的关注和研究。由于水性聚氨酯的特殊性，其在性能方面有一定的限制和缺陷。制备水性聚氨酯需加入亲水单体以使聚氨酯树脂分散于水中，这使水性聚氨酯在耐水方面有一定的缺陷，很难媲美溶剂型产品。
织物涂层是指织物表面均匀涂覆的一层或多层可成膜物质，以赋予织物表面一定的特殊性能。其中一些织物，如帐篷、衣物等需要表层有一定防水性，且手感柔软不发粘。这就要求涂层对织物有良好的附着力，并且涂层成膜要柔软，为了保证遇水后织物没有明显增重要求涂层有较低的吸水率，而且从环保角度出发要求成膜物质有较低的VOC，以免在施工过程中有大量溶剂挥发，污染环境。因此低吸水率的织物涂层用水性聚氨酯的研究有重要意义。
目前，针对水性聚氨酯吸水率的研究较少，现有研究中，吸水率低于10％(7d)的产品较少，一般为了改善水性聚氨酯胶膜的吸水率，常采用加入三官能团的扩链剂或大分子醇，如果加入量过少，则吸水率的改善效果并不明显；如果加入量过大则导致预聚体分子量过大粘度过高，后期的乳化分散困难，无法得到稳定的乳液。除此之外，为了改善吸水率，通常加入异氰酸酯型固化剂对乳液中剩余的少量羟基和氨基甲酸酯基进行交联。大多数乳液为了使水性聚氨酯成膜后具有一定的力学性能，分子量会略高，相对应的羟基剩余较少，加入固化剂后起到的交联作用并不明显；而含量较高的氨基甲酸酯基与异氰酸酯基的反应较为困难，并且需要较高的温度，而且其两者反应生成的双二脲提高了胶膜的硬度，整体改善效果不理想。
发明内容
基于现有技术所存在的问题，本发明的目的是提供一种低吸水率的织物涂层用水性聚氨酯乳液及其制备方法，能改善现有水性聚氨酯吸水率偏高的问题。
本发明的目的是通过以下技术方案实现的：
本发明实施方式提供一种低吸水率的织物涂层用水性聚氨酯乳液，该乳液以多元醇、亲水扩链剂、溶剂、二异氰酸酯、二元扩链剂、三元扩链剂、三乙胺、胺基类后扩链剂为原料制成的水性聚氨酯乳液。
本发明实施方式还提供一种低吸水率的织物涂层用水性聚氨酯乳液的制备方法，用于制备本发明所述的低吸水率的织物涂层用水性聚氨酯乳液，包括以下步骤：
按本发明所述的水性聚氨酯乳液的配方取各原料；
步骤一、对多元醇进行脱水处理；
步骤二、在氮气保护、82～88℃温度下，向反应釜中加入所述步骤一脱水后的多元醇和亲水扩链剂，待所有原料完全溶解后，加入二异氰酸酯，待完全反应后得到溶液A；
步骤三、向所述步骤二制得的溶液A中加入二元扩链剂和三元扩链剂，所有反应单体的R值为1.2～2.0，所述R值为异氰酸酯基与羟基的比值，并加入溶剂溶解降粘，待完全反应后得到预聚体B；
步骤四、将所述步骤三制得的预聚体B置于分散缸内，降至0～10℃，向其中加入三乙胺中和，三乙胺和亲水扩链剂的摩尔比例为0.9～1.1；反应完全后，加入冰水在高剪切下进行乳化，然后加入胺基类后扩链剂，10min后得到乳液C；
步骤五、将所述步骤四制得的乳液C进行减压脱酮处理，得到的乳液即为低吸水率的织物涂层用水性聚氨酯乳液。
由上述本发明提供的技术方案可以看出，本发明实施例提供的低吸水率的织物涂层用水性聚氨酯乳液及其制备方法，其有益效果为：
通过在制备过程的后扩链步骤中，加入特定的胺基类后扩链剂，使制成的耐水水性聚氨酯分子侧链上带有羟基或胺基，使后续的固化更容易进行，达到了吸水率低于8％(7d)的效果，与现有的耐水水性聚氨酯产品相比，很好的改善了现有水性聚氨酯吸水率偏高的现状，本发明水性聚氨酯配合固化剂用于涤纶表面涂层时，成膜柔软不粘手，具有良好的附着力。
具体实施方式
下面结合本发明的具体内容，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明的保护范围。本发明实施例中未作详细描述的内容属于本领域专业技术人员公知的现有技术。
本发明实施例提供一种低吸水率的织物涂层用水性聚氨酯乳液，该乳液以多元醇、亲水扩链剂、溶剂、二异氰酸酯、二元扩链剂、三元扩链剂、三乙胺、胺基类后扩链剂为原料制成的水性聚氨酯乳液。
上述水性聚氨酯乳液中，各原料用量按质量份为：
多元醇15～25份、亲水扩链剂0.5～1.5份、溶剂8～15份、二异氰酸酯5～10份、三元扩链剂0.01～0.2份、三乙胺0.5～1份、胺基类后扩链剂0.2～1份。
上述水性聚氨酯乳液中，所述多元醇采用聚醚二元醇和聚酯二元醇的混合物。优选的，聚醚二元醇采用：聚四氢呋喃二醇和聚丙二醇的混合物；聚酯二元醇采用：聚己二酸二乙二醇酯和聚己二酸异丙二醇酯的混合物。
上述水性聚氨酯乳液中，溶剂采用：丙酮或丁酮；
所述亲水扩链剂采用：二羟甲基丙酸或二羟甲基丁酸；
所述二异氰酸酯采用异佛尔酮二异氰酸酯或六亚甲基二异氰酸酯；
所述三元扩链剂采用：三羟甲基丙烷；
所述胺基类后扩链剂采用乙二胺、1,3-二胺基-2-丙醇、二乙烯三胺、三乙烯四胺、四乙烯五胺中的任一种或几种，胺基后扩链中胺基和异氰酸基的比例为20～90％。
上述乳液的原料中还包括：二元扩链剂。该二元扩链剂的用量按质量份计为：0.1～1份；优选的，该二元扩链剂采用：乙二醇、1,4丁二醇、1,6-己二醇、二乙二醇中的任一种。
上述水性聚氨酯乳液按下述方式制得：
步骤一、对多元醇进行脱水处理；
步骤二、在氮气保护、82～88℃温度下，向反应釜中加入所述步骤一脱水后的多元醇和亲水扩链剂，待所有原料完全溶解后，加入二异氰酸酯，待完全反应后得到溶液A；
步骤三、向所述步骤二制得的溶液A中加入三元扩链剂，所有反应单体的R值为1.2～2.0，所述R值为异氰酸酯基与羟基的比值，并加入溶剂溶解降粘，待完全反应后得到预聚体B；
步骤四、将所述步骤三制得的预聚体B置于分散缸内，降至0～10℃，向其中加入三乙胺中和，三乙胺和亲水扩链剂的摩尔比例为0.9～1.1；反应完全后，加入冰水在高剪切下进行乳化，然后加入胺基类后扩链剂，10min后得到乳液C；
步骤五、将所述步骤四制得的乳液C进行减压脱酮处理，得到的乳液即为低吸水率的织物涂层用水性聚氨酯乳液。
上述步骤一的对多元醇进行脱水处理为：将聚醚二元醇和聚酯二元醇在100～120℃下脱水后混合形成脱水后的多元醇。
上述步骤二中，将所述多元醇和亲水扩链剂同时加入反应釜中，不使用催化剂。
上述方法步骤二中，向反应釜中加入所述步骤一脱水后的多元醇和亲水扩链剂中，若亲水扩链剂采用二羟甲基丙酸，还同时加入占溶剂总质量5～20％的溶剂；而步骤三中加入溶剂溶解降粘为加入剩余的溶剂。
上述步骤三中，向所述步骤二制得的溶液A中加入三元扩链剂时，还同时加入二元扩链剂。
上述步骤五中的脱酮压力为-0.085～0.095MPa，温度为45～65℃，直至溶剂含量低于1000ppm完成减压脱酮处理。
本发明实施例还提供一种低吸水率的织物涂层用水性聚氨酯乳液的制备方法，用于制备上述的低吸水率的织物涂层用水性聚氨酯乳液，包括以下步骤：
按上述的水性聚氨酯乳液的配方取各原料；
步骤一、将聚醚二元醇和聚酯二元醇在100～120℃下脱水后形成多元醇；
步骤二、在氮气保护、82～88℃温度下，向反应釜中加入所述步骤一脱水后的多元醇和亲水扩链剂，待所有原料完全溶解后，加入二异氰酸酯，待完全反应后得到溶液A；
步骤三、向所述步骤二制得的溶液A中加入三元扩链剂，所有反应单体的R值为1.2～2.0，所述R值为异氰酸酯基与羟基的比值，并加入溶剂溶解降粘，待完全反应后得到预聚体B；
步骤四、将所述步骤三制得的预聚体B置于分散缸内，降至0～10℃，向其中加入三乙胺中和，三乙胺和亲水扩链剂的摩尔比例为0.9～1.1；反应完全后，加入冰水在高剪切下进行乳化，然后加入胺基类后扩链剂，10min后得到乳液C；
步骤五、将所述步骤四制得的乳液C进行减压脱酮处理，得到的乳液即为低吸水率的织物涂层用水性聚氨酯乳液。
上述方法步骤一的对多元醇进行脱水处理为：将聚醚二元醇和聚酯二元醇在100～120℃下脱水后混合形成脱水后的多元醇。
上述方法的步骤二中，所述多元醇和亲水扩链剂同时加入反应釜中，不使用催化剂。
上述方法步骤二中，向反应釜中加入所述步骤一脱水后的多元醇和亲水扩链剂中，若亲水扩链剂采用二羟甲基丙酸，还同时加入占溶剂总质量5～20％的溶剂；而步骤三中加入溶剂溶解降粘为加入剩余的溶剂。
上述步骤三中，向所述步骤二制得的溶液A中加入三元扩链剂时，还同时加入二元扩链剂。
上述方法步骤五中，脱酮压力为-0.085～0.095MPa，温度为45～65℃，直至溶剂含量低于1000ppm完成减压脱酮处理。
上述方法制得的水性聚氨酯乳液配合异氰酸酯型固化剂使用，可作为织物涂层胶使用。
本发明通过引入含不同活性的胺基类后扩链剂，活性高的伯胺基和异氰酸酯反应，接入到分子链中，活性低的羟基或胺基留在分子侧链中，配合异氰酸酯类外添加固化剂形成一种低吸水率水性聚氨酯；制备的水性聚氨酯应用于涤纶表面时，具有良好附着、表面光滑不粘手、无毒环保。乳液具有良好的储存稳定性，7天吸水率为7.0％～8.0％，断裂伸长率大于1700％。
下面对本发明实施例具体作进一步地详细描述。
实施例一
本实施例提供一种低吸水率的织物涂层用水性聚氨酯乳液，其制备方法包括以下步骤：
取聚四氢呋喃二醇PTMG2000(60g)，聚己二酸二乙二醇酯(Mn1300)39g于120℃下脱水1h，降温至85℃，加入5.37g二羟甲基丙酸DMPA，通氮气，接入冷凝回流装置，加入10g丙酮，待固体完全溶解后加入31.1g异佛尔酮二异氰酸酯IPDI，反应2h后加入0.67g三羟甲基丙烷TMP，反应1h，加入58.1g丙酮降粘，体系溶解均匀后降至室温，将预聚体置于分散机中，500r/min下加入4.04g三乙胺中和10～15min，提高转速至1500r/min，加入347g去离子水分散，然后加入2.35g二乙烯三胺进行后扩链，搅拌10min后形成含酮乳液，对乳液在55℃，-0.09MPa下进行脱酮处理2h后得到水性聚氨酯乳液。
实施例二
本实施例提供一种低吸水率的织物涂层用水性聚氨酯乳液，其制备方法包括以下步骤：
取聚丙二醇PPG2000(60g)，聚四氢呋喃二醇PTMG2000(60g)于120℃下脱水1h，降温至85℃，加入5.93g二羟甲基丁酸DMBA，通氮气，待固体完全溶解后加入31.1g异佛尔酮二异氰酸酯IPDI，反应2h后加入0.67g三羟甲基丙烷TMP，反应1h，加入47.3g丙酮降粘，体系溶解均匀后降至室温，将预聚体置于分散机中，500r/min下加入4.04g三乙胺中和10～15min，提高转速至1800r/min，加入347g去离子水分散，然后加入2.35g二乙烯三胺进行后扩链，搅拌10min后形成含酮乳液，对乳液在55℃，-0.09MPa下进行脱酮处理2h后得到水性聚氨酯乳液。
实施例三
本实施例提供一种低吸水率的织物涂层用水性聚氨酯乳液，其制备方法包括以下步骤：
取聚丙二醇PTMG2000(60g)，聚己二酸异丙二醇酯(Mn2000)60g于120℃下脱水1h，降温至85℃，加入7.41g二羟甲基丁酸DMBA，通氮气，待固体完全溶解后加入44.46g异佛尔酮二异氰酸酯IPDI，反应2h后加入0.67g三羟甲基丙烷TMP，3.60g1，4-丁二醇BDO，反应1h，加入88g丙酮降粘，体系溶解均匀后降至室温，将预聚体置于分散机中，500r/min下加入5.05g三乙胺中和10～15min，提高转速至1500r/min，加入392g去离子水分散，然后加入5.58g三乙烯四胺进行后扩链，搅拌10min后形成含酮乳液，对乳液在55℃，-0.09MPa下进行脱酮处理2h后得到水性聚氨酯乳液。
实施例四
本实施例提供一种低吸水率的织物涂层用水性聚氨酯乳液，其制备方法包括以下步骤：
取PTMG2000(60g)，聚己二酸异丙二醇酯(Mn2000)60g于120℃下脱水1h，降温至85℃，加入7.41g二羟甲基丁酸DMBA，通氮气，待固体完全溶解后加入44.46g异佛尔酮二异氰酸酯IPDI，反应2h后加入0.67g三羟甲基丙烷TMP，3.60g1，4-丁二醇BDO，反应1h，加入88g丙酮降粘，体系溶解均匀后降至室温，将预聚体置于分散机中，500r/min下加入5.05g三乙胺中和10～15min，提高转速至1500r/min，加入392g去离子水分散，然后加入2.79g三乙烯四胺和1.15g乙二胺进行后扩链，搅拌10min后形成含酮乳液，对乳液在55℃，-0.09MPa下进行脱酮处理2h后得到水性聚氨酯乳液。
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披露的技术范围内，可轻易想到的变化或替换，都应涵盖在本发明的保护范围之内。因此，本发明的保护范围应该以权利要求书的保护范围为准。

Claims (10)

1.一种低吸水率的织物涂层用水性聚氨酯乳液，其特征在于，该乳液以多元醇、亲水扩链剂、溶剂、二异氰酸酯、三元扩链剂、三乙胺、胺基类后扩链剂为原料制成的水性聚氨酯乳液。
2.根据权利要求1所述的低吸水率的织物涂层用水性聚氨酯乳液，其特征在于，所述乳液中，各原料用量按质量份为：
多元醇15～25份、亲水扩链剂0.5～1.5份、溶剂8～15份、二异氰酸酯5～10份、三元扩链剂0.01～0.2份、三乙胺0.5～1份、胺基类后扩链剂0.2～1份。
3.根据权利要求1或2所述的低吸水率的织物涂层用水性聚氨酯乳液，其特征在于，所述多元醇采用聚醚二元醇和聚酯二元醇的混合物。
4.根据权利要求3所述的低吸水率的织物涂层用水性聚氨酯乳液，其特征在于，
所述聚醚二元醇采用：聚四氢呋喃二醇和聚丙二醇的混合物；
所述聚酯二元醇采用：聚己二酸二乙二醇酯和聚己二酸异丙二醇酯的混合物。
5.根据权利要求1或2所述的低吸水率的织物涂层用水性聚氨酯乳液，其特征在于，所述溶剂采用：丙酮或丁酮；
所述亲水扩链剂采用：二羟甲基丙酸或二羟甲基丁酸；
所述二异氰酸酯采用异佛尔酮二异氰酸酯或六亚甲基二异氰酸酯；
所述三元扩链剂采用：三羟甲基丙烷；
所述胺基类后扩链剂采用乙二胺、1,3-二胺基-2-丙醇、二乙烯三胺、三乙烯四胺、四乙烯五胺中的任一种或几种，胺基后扩链中胺基和异氰酸基的比例为20～90％。
6.根据权利要求1或2所述的低吸水率的织物涂层用水性聚氨酯乳液，其特征在于，所述乳液的原料中还包括：二元扩链剂。
7.根据权利要求6所述的低吸水率的织物涂层用水性聚氨酯乳液，其特征在于，所述二元扩链剂的用量按质量份计为：0.1～1份；
所述二元扩链剂采用：乙二醇、1,4丁二醇、1,6-己二醇、二乙二醇中的任一种。
8.一种低吸水率的织物涂层用水性聚氨酯乳液的制备方法，其特征在于，用于制备权利要求1至7任一项所述的低吸水率的织物涂层用水性聚氨酯乳液，包括以下步骤：
按权利要求1至7任一项所述的水性聚氨酯乳液的配方取各原料；
步骤一、对多元醇进行脱水处理；
步骤二、在氮气保护、82～88℃温度下，向反应釜中加入所述步骤一脱水后的多元醇和亲水扩链剂，待所有原料完全溶解后，加入二异氰酸酯，待完全反应后得到溶液A；
步骤三、向所述步骤二制得的溶液A中加入三元扩链剂，所有反应单体的R值为1.2～2.0，所述R值为异氰酸酯基与羟基的比值，并加入溶剂溶解降粘，待完全反应后得到预聚体B；
步骤四、将所述步骤三制得的预聚体B置于分散缸内，降至0～10℃，向其中加入三乙胺中和，三乙胺和亲水扩链剂的摩尔比例为0.9～1.1；反应完全后，加入冰水在高剪切下进行乳化，然后加入胺基类后扩链剂，10min后得到乳液C；
步骤五、将所述步骤四制得的乳液C进行减压脱酮处理，得到的乳液即为低吸水率的织物涂层用水性聚氨酯乳液。
9.根据权利要求8所述的低吸水率的织物涂层用水性聚氨酯乳液的制备方法，其特征在于，所述方法的步骤三中，向所述步骤二制得的溶液A中加入三元扩链剂时，还同时加入二元扩链剂。
10.根据权利要求8或9所述的低吸水率的织物涂层用水性聚氨酯乳液的制备方法，其特征在于，
所述方法步骤一中的对多元醇进行脱水处理为：将聚醚二元醇和聚酯二元醇在100～120℃下脱水后混合形成脱水后的多元醇；
所述方法的步骤二中，所述多元醇和亲水扩链剂同时加入反应釜中；
所述方法步骤二中，向反应釜中加入所述步骤一脱水后的多元醇和亲水扩链剂中，若亲水扩链剂采用二羟甲基丙酸，还同时向反应釜中加入占溶剂总质量5～20％的溶剂；而步骤三中加入溶剂溶解降粘为加入剩余的溶剂；
所述方法步骤五中，脱酮压力为-0.085～0.095MPa，温度为45～65℃，直至溶剂含量低于1000ppm完成减压脱酮处理。
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