CN107936212B - 指甲油用水性聚氨酯树脂及其制备方法 - Google Patents

指甲油用水性聚氨酯树脂及其制备方法 Download PDF

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CN107936212B
CN107936212B CN201711229292.6A CN201711229292A CN107936212B CN 107936212 B CN107936212 B CN 107936212B CN 201711229292 A CN201711229292 A CN 201711229292A CN 107936212 B CN107936212 B CN 107936212B
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polyurethane resin
nail polish
chain extender
waterborne polyurethane
diisocyanate
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CN107936212A (zh
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龙志云
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YINGDE GUOCAI FINE CHEMICAL Co.,Ltd.
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Guangzhou Guanzhi New Material Technology Co ltd
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Abstract

本发明公开了一种指甲油用水性聚氨酯树脂及其制备方法，其包括低聚物二元醇、二异氰酸酯、小分子扩链剂、亲水扩链剂、胺基磺酸盐扩链剂、后扩链剂、水等原料制备而得，本发明的指甲油用水性聚氨酯树脂具有环保、稳定性好、持久、强度高、耐水性极佳、良好的油脂性以及耐温性能、产品成本低等优点，为环保型指甲油化妆品提供了高性价比的基础树脂，可广泛的用于指甲、皮肤防护领域中，特别适用指甲表面保护中；合成工艺简单，可控性强，对设备的要求明显降低，同时避免了多重改性产品在合成过程中所带来的诸多影响因素。

Description

指甲油用水性聚氨酯树脂及其制备方法
技术领域
本发明属于水性聚氨酯技术领域，特别涉及一种环保型无溶剂指甲油用水性聚氨酯树脂及其制备方法和应用。
背景技术
随着生活水平的不断提高，人们对产品的外观、环保性及其使用性能等要求也在日益增加。化妆品在人的手和脸等皮肤表面附加一层保护以其美观度，甚至起到保护性能。
目前市场上大部分基础树脂仍是低毒溶剂型的，其在生产、施工及使用过程中均会对环境及人体造成伤害，有悖于绿色环保的发展理念。虽有小部分水性产品在使用，但是也暴露出不少的问题：(1)在使用过程中，涂层对指甲及皮肤有轻微腐蚀；(2)涂层不够，易脱离；(3)亲水扩链剂作为内乳化剂，对乳液的稳定性起着至关重要的作用，但是涂膜干燥后，其极易吸水，使得涂层耐水性较差，吸水后易泛白，大大降低了涂膜对指甲的保护效果；(4)涂层耐油脂以及耐温性能差等。
发明内容
基于此，为了克服上述现有技术的缺陷，本发明提供了一种环保型无溶剂指甲油用水性聚氨酯树脂及其制备方法。
为了实现上述发明目的，本发明采取了以下技术方案：
一种指甲油用水性聚氨酯树脂，包括以下重量份的原料制备而得：
Figure BDA0001487880790000021
在其中一个实施例中，所述胺基磺酸盐扩链剂为磺酸盐A95。
在其中一个实施例中，所述胺基磺酸盐扩链剂与低聚物二元醇的质量比为0.5～4.5：60。
在其中一个实施例中，所述小分子扩链剂和亲水扩链剂的总重量份为2.5～9.5份。
在其中一个实施例中，所述低聚物二元醇为聚酯型二元醇或者聚醚型二元醇，为聚己二酸丁二醇酯二醇、聚己内酯二醇、聚碳酸酯二醇、聚四氢呋喃醚二醇和聚丙二醇中的一种或几种，其分子量为400～4000。
在其中一个实施例中，所述二异氰酸酯并无特别限制，已知使用的二异氰酸酯均可，可为异佛尔酮二异氰酸酯(IPDI)、六次甲基二异氰酸酯(HDI)、甲苯二异氰酸酯(TDI)和4,4-二环己基甲烷二异氰酸酯(H12-MDI)中的一种或几种。
在其中一个实施例中，所述小分子扩链剂并无特别限制，已知使用的小分子扩链剂均可，为了更好地实现本发明，所述的小分子扩链剂优选为1,4-丁二醇(BDO)、新戊二醇(NPG)、1,6-己二醇(HEG)和一缩二乙二醇中一种或几种。
在其中一个实施例中，所述亲水扩链剂并无特别限制，已知使用的亲水扩链剂均可，为了更好地实现本发明，所述的亲水扩链剂优选为二羟甲基丙酸、二羟甲基丁酸和双羟基磺酸盐中的一种或几种。
在其中一些实施例中，所述后扩链剂并无特别限制，已知使用的后扩链剂均可，为了更好地实现本发明，所述后扩链剂优选为乙二胺、丙二胺、1,6-己二胺、二亚-2-乙基三胺、异氟尔酮二胺和三亚乙基四胺中的一种或几种。
本发明还提供了上述环保型无溶剂指甲油用水性聚氨酯树脂的制备方法，包括以下步骤：
(1)在惰性气体保护下，将低聚物二元醇与二异氰酸酯混合，在60～90℃下，搅拌反应1.5～2.5h；
(2)降低反应体系的温度至40～60℃，加入小分子扩链剂和亲水扩链剂，70～85℃，反应2.5～4.5h；
(3)降低反应体系的温度至50℃以下，加入中和剂、胺基磺酸盐扩链剂后分别搅拌1～5min，加入水、后扩链剂后分别高速搅拌10～30min，即得。
在其中一些实施例中，步骤(1)中所述低聚物二元醇于80～140℃下脱水2h后再用于反应。
在其中一些实施例中，步骤(3)中所述中和剂为本领域任意常用的碱液，如三甲胺、三乙胺、氨水等，用于调节反应体系的pH值至弱碱性。
本发明还提供了上述环保型无溶剂指甲油用水性聚氨酯树脂在指甲及皮肤防护中的应用。
本发明的环保型指甲油水性聚氨酯树脂选材独具匠心，体系中加入了胺基磺酸盐扩链剂，提高了树脂的抗絮凝稳定性，可与其他阴离子或者非离子分散剂达到好的相容性，也提高了树脂的牢度和水解稳定性。同时，本发明优选使用聚醚多元醇和聚酯多元醇进行混合制备树脂，从而获得优异的各项性能。
与现有技术相比，本发明具有以下有益效果：
(1)本发明的环保型指甲油性聚氨酯树脂中加入了胺基磺酸盐扩链剂，提高了树脂的抗絮凝稳定性，可与其他阴离子或者非离子分散剂达到好的相容性，也提高了树脂的牢度和水解稳定性。且分散介质为水，成本较低，具有环保、稳定性好、持久、强度高、耐水性极佳、良好的油脂性以及耐温性能、产品成本低等优点，为环保型指甲油化妆品提供了高性价比的基础树脂，可广泛的用于指甲、皮肤防护领域中，特别适用指甲表面保护中；
(2)本发明的环保型指甲油水性聚氨酯树脂合成工艺简单，可控性强，对设备的要求明显降低，同时避免了多重改性产品在合成过程中所带来的诸多影响因素。
具体实施方式
下面结合具体实施例进一步叙述本发明，本发明未述及之处适用于现有技术。下面给出本发明的具体实施例，但实施例仅是为了进一步详细叙述本说明，并不限制本发明的权利要求。以下实施例中所使用的试剂或原料，均可从商业渠道获得。
实施例1环保型指甲油用水性聚氨酯树脂
本实施例的环保型指甲油用水性聚氨酯树脂包括以下重量份的原料制备而得：
Figure BDA0001487880790000041
Figure BDA0001487880790000051
上述环保型无溶剂指甲油用水性聚氨酯树脂的制备方法，包括以下步骤：
(1)在干燥氮气保护下，将120℃下真空脱水2h后的聚四氢呋喃醚二醇80克，异佛尔酮二异氰酸酯26.7克，加入反应器中，在机械搅拌下控制温度在70～90℃进行反应2小时；
(2)降低反应体系的温度至40～60℃，加入1,6-己二醇5.6克，二羟甲基丙酸3.5克，在70～85℃反应3小时；
(3)降低反应体系的温度至50℃以下，加入计量三乙胺2.45克调节体系pH为弱碱性，继续搅拌5分钟；加入磺酸盐A950.7克，继续搅拌5分钟；加入水200克，高速(转速优选≥1200r/min)分散10分钟；加入丙二胺1.5克，继续高速分散30分钟，即可得到环保型指甲油水性聚氨酯树脂。
实施例2环保型指甲油用水性聚氨酯树脂
本实施例的环保型指甲油用水性聚氨酯树脂包括以下重量份的原料制备而得：
Figure BDA0001487880790000052
Figure BDA0001487880790000061
上述环保型无溶剂指甲油用水性聚氨酯树脂的制备方法，包括以下步骤：
(1)在干燥氮气保护下，将120℃下真空脱水2h后的聚四氢呋喃醚二醇40克，聚丙二醇40克，异佛尔酮二异氰酸酯44.4克，加入反应器中，在机械搅拌下控制温度在70～90℃进行反应2小时；
(2)降低反应体系的温度至40～60℃，加入一缩二乙二醇4.0克，二羟甲基丁酸5.0克，在70～85℃反应3小时；
(3)降低反应体系的温度至50℃以下，加入计量三乙胺2.45克调节体系pH为弱碱性，继续搅拌5分钟；加入磺酸盐A954.5克，继续搅拌5分钟；加入水200克，高速(转速优选≥1200r/min)分散10分钟；加入乙二胺1.5克，继续高速分散30分钟，即可得到环保型指甲油水性聚氨酯树脂。
实施例3环保型指甲油用水性聚氨酯树脂
本实施例的环保型指甲油用水性聚氨酯树脂包括以下重量份的原料制备而得：
Figure BDA0001487880790000062
Figure BDA0001487880790000071
上述环保型无溶剂指甲油用水性聚氨酯树脂的制备方法，包括以下步骤：
(1)在干燥氮气保护下，将120℃下真空脱水2h后的聚己内酯二醇40克，聚己二酸丁二醇酯二醇40克，甲苯二异氰酸酯34.8克，加入反应器中，在机械搅拌下控制温度在70～90℃进行反应2小时；
(2)降低反应体系的温度至40～60℃，加入一缩二乙二醇5.6克，双羟基磺酸盐3.5克，在70～85℃反应3小时；
(3)降低反应体系的温度至50℃以下，加入计量三乙胺2.45克调节体系pH为弱碱性，继续搅拌5分钟；加入磺酸盐A954.5克，继续搅拌5分钟；加入水200克，高速(转速优选≥1200r/min)分散10分钟；加入1,6-己二胺1.5克，继续高速分散30分钟，即可得到环保型指甲油水性聚氨酯树脂。
实施例4环保型指甲油用水性聚氨酯树脂
本实施例的环保型指甲油用水性聚氨酯树脂包括以下重量份的原料制备而得：
Figure BDA0001487880790000072
Figure BDA0001487880790000081
上述环保型无溶剂指甲油用水性聚氨酯树脂的制备方法，包括以下步骤：
(1)在干燥氮气保护下，将120℃下真空脱水2h后的聚碳酸酯二元醇40克，聚四氢呋喃醚二醇40克，异佛尔酮二异氰酸酯22.2克，六次甲基二异氰酸酯16.8克，加入反应器中，在机械搅拌下控制温度在70～90℃进行反应2小时；
(2)降低反应体系的温度至40～60℃，加入1,4-丁二醇4.75克，二羟甲基丙酸3.5克，在70～85℃反应3小时；
(3)降低反应体系的温度至50℃以下，加入计量三乙胺2.45克调节体系pH为弱碱性，继续搅拌5分钟；加入磺酸盐A956.0克，继续搅拌5分钟；加入水200克，高速(转速优选≥1200r/min)分散10分钟；加入二亚-2-乙基三胺1.5克，继续高速分散30分钟，即可得到环保型指甲油水性聚氨酯树脂。
实施例5环保型指甲油用水性聚氨酯树脂
本实施例的环保型指甲油用水性聚氨酯树脂包括以下重量份的原料制备而得：
Figure BDA0001487880790000082
Figure BDA0001487880790000091
上述环保型无溶剂指甲油用水性聚氨酯树脂的制备方法，包括以下步骤：
(1)在干燥氮气保护下，将120℃下真空脱水2h后的聚碳酸酯二元醇40克，聚四氢呋喃醚二醇40克，4,4-二环己基甲烷二异氰酸酯14.8克，六次甲基二异氰酸酯16.8克，加入反应器中，在机械搅拌下控制温度在70～90℃进行反应2小时；
(2)降低反应体系的温度至40～60℃，加入1,4-丁二醇1.75克，二羟甲基丙酸1.0克，在70～85℃反应3小时；
(3)降低反应体系的温度至50℃以下，加入计量三乙胺2.45克调节体系pH为弱碱性，继续搅拌5分钟；加入磺酸盐A951.8克，继续搅拌5分钟；加入水200克，高速(转速优选≥1200r/min)分散10分钟；加入三亚乙基四胺1.5克，继续高速分散30分钟，即可得到环保型指甲油水性聚氨酯树脂。
试验例实施例1～5的水性聚氨酯树脂制成的指甲油的综合性能评价
将实施例1～5及不含胺基磺酸盐扩链剂的水性聚氨酯树脂(对比例，其他原料及制备方法均与实施例1相同)制成指甲油，对其综合性能进行了评价，其中：
指甲油的耐摩擦性测试：取5g指甲油涂覆在聚四氟乙烯上(模拟人体指甲)，5小时后在型号为Taber710五指刮擦磨耗仪上测试指甲油的耐摩擦性。
指甲油的防水性测试：取5g指甲油涂覆在聚四氟乙烯上(模拟人体指甲)，浸没于50ml水中，7天后观察聚四氟乙烯上指甲油的脱落程度，测量指甲油的防水性能(1～100级，其中100级为指甲油完整，未从聚四氟乙烯上掉落)。
具体结果如下表所示。
性能 实施例1 实施例2 实施例3 实施例4 实施例5 对比例
耐摩擦性均值 68 79 88 92 99 5.65
耐摩擦性标准差 2.6 1.5 1.1 0.6 0.2 7.8
防水性均值 83 88 0.6 93 99 38
防水性标准差 1.2 0.8 0.2 0.3 0.1 5.8
从上表可知，本发明的水性聚氨酯树脂制成的指甲油具有良好的耐摩擦性和防水性能，同时其性能的均匀性较好。
以上所述实施例的各技术特征可以进行任意的组合，为使描述简洁，未对上述实施例中的各个技术特征所有可能的组合都进行描述，然而，只要这些技术特征的组合不存在矛盾，都应当认为是本说明书记载的范围。
以上所述实施例仅表达了本发明的几种实施方式，其描述较为具体和详细，但并不能因此而理解为对发明专利范围的限制。应当指出的是，对于本领域的普通技术人员来说，在不脱离本发明构思的前提下，还可以做出若干变形和改进，这些都属于本发明的保护范围。因此，本发明专利的保护范围应以所附权利要求为准。

Claims (10)

1.一种指甲油用水性聚氨酯树脂，其特征在于，包括以下重量份的原料制备而得：
Figure FDA0002457196650000011
其中，低聚物二元醇和二异氰酸酯之间的重量比例为(1.8～3)：1；
所述指甲油用水性聚氨酯树脂由包括如下步骤的制备方法制备得到：
(1)在惰性气体保护下，将低聚物二元醇与二异氰酸酯混合，在60～90℃下，搅拌反应1.5～2.5h；
(2)降低反应体系的温度至40～60℃，加入小分子扩链剂和亲水扩链剂，70～85℃，反应2.5～4.5h；
(3)降低反应体系的温度至50℃以下，加入中和剂、磺酸盐A95后分别搅拌1～5min，加入水、后扩链剂后分别高速搅拌10～30min；
所述指甲油用水性聚氨酯树脂为非有机溶剂型指甲油用水性聚氨酯树脂，制备所述指甲油用水性聚氨酯树脂的原料和过程中均不使用除了所述指甲油用水性聚氨酯树脂的各原料组分和所述中和剂之外的有机溶剂。
2.根据权利要求1所述的指甲油用水性聚氨酯树脂，其特征在于，所述磺酸盐A95与所述低聚物二元醇的质量比为0.5～4.5：60。
3.根据权利要求1所述的指甲油用水性聚氨酯树脂，其特征在于，所述小分子扩链剂和所述亲水扩链剂的总重量份为2.75～9.5份。
4.根据权利要求1～3任一项所述的指甲油用水性聚氨酯树脂，其特征在于，所述低聚物二元醇为聚己二酸丁二醇酯二醇、聚己内酯二醇、聚碳酸酯二醇、聚四氢呋喃醚二醇和聚丙二醇中的一种或几种，其分子量为400～4000。
5.根据权利要求1～3任一项所述的指甲油用水性聚氨酯树脂，其特征在于，所述二异氰酸酯为异佛尔酮二异氰酸酯、六次甲基二异氰酸酯、甲苯二异氰酸酯和4,4-二环己基甲烷二异氰酸酯中的一种或几种。
6.根据权利要求1～3任一项所述的指甲油用水性聚氨酯树脂，其特征在于，所述小分子扩链剂为1,4-丁二醇、新戊二醇、1,6-己二醇和一缩二乙二醇中的一种或几种；所述亲水扩链剂为二羟甲基丙酸、二羟甲基丁酸和双羟基磺酸盐中的一种或几种；所述后扩链剂为乙二胺、丙二胺、1,6-己二胺、二亚-2-乙基三胺、异氟尔酮二胺和三亚乙基四胺中的一种或几种。
7.一种根据权利要求1～6任一项所述的指甲油用水性聚氨酯树脂的制备方法，其特征在于，由以下步骤制备得到：
(1)在惰性气体保护下，将低聚物二元醇与二异氰酸酯混合，在60～90℃下，搅拌反应1.5～2.5h；
(2)降低反应体系的温度至40～60℃，加入小分子扩链剂和亲水扩链剂，70～85℃，反应2.5～4.5h；
(3)降低反应体系的温度至50℃以下，加入中和剂、磺酸盐A95后分别搅拌1～5min，加入水、后扩链剂后分别高速搅拌10～30min，即得。
8.根据权利要求7所述的指甲油用水性聚氨酯树脂的制备方法，其特征在于，步骤(1)中所述低聚物二元醇于80～140℃下脱水2h后再用于反应。
9.根据权利要求7所述的指甲油用水性聚氨酯树脂的制备方法，其特征在于，步骤(3)中所述中和剂为三甲胺、三乙胺或氨水。
10.一种指甲油或皮肤防护产品，其特征在于，包括权利要求1～6任一项所述的指甲油用水性聚氨酯树脂，或是包括由权利要求7～9任一项所述的指甲油用水性聚氨酯树脂的制备方法制备所得的指甲油用水性聚氨酯树脂。
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