CN117924643A - 一种有机硅改性水性聚氨酯防水剂的制备方法 - Google Patents
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Abstract
本发明公开了一种有机硅改性水性聚氨酯防水剂的制备方法,它涉及防水剂技术领域;由以下质量百分比的原料制成:多异氰酸酯类单体15~18%;多元醇类单体15~30%;羟基硅油2~7%;小分子扩链剂2~6%;引发剂0.01~1%;交联剂0.01~1%;溶剂8~15%;余量为去离子水。本申请还提供一种无氟防水剂的制备方法。本申请提供的无氟防水剂配方及制备方法所制得的无氟防水剂,具有防水效果优良、耐洗性好、操作简单的优点。
Description
技术领域
本发明涉及防水剂技术领域,具体涉及一种有机硅改性水性聚氨酯防水剂的制备方法。
背景技术
市场上使用最多的防水剂为含氟防水剂,其降解性难和生物累积毒性高使其在纺织品上的应用受到严格限制。有相当一部分经含氟防水剂整理的织物,如运动服、家用纺织品、户外服装和休闲服等,实际工作中只要求有拒水效果,并不需要拒油性能,因而只需采用具有耐久拒水功能的整理剂处理。水性聚氨酯是以水代替有机溶剂作为分散介质的新型聚氨酯体系也称水分散聚氨酯、水系聚氨酯或水基聚氨酯。水性聚氨酯以水为溶剂,具有无污染、安全可靠、机械性能优良、相容性好、易于改性等优点。随着环保法律法规的健全和人们环保意识的加强,无氟防水剂日益受到重视。但由于亲水单体的加入以及氨基甲酸酯、脲键等的亲水性,使得其耐水性较差,具体表现为吸水率较大,水接触角较小。为了更好地提高水性聚氨酯的耐水性,扩大应用范围,有机硅改性无氟聚氨酯的研究成为研究热点之一。
发明内容
本发明的目的提供一种有机硅改性无氟聚氨酯防水剂的制备方法,具有工艺简单,制备的防水剂薄膜耐水性好的特点。
本发明所采用的技术方案是一种有机硅改性阳离子水性聚氨酯防水剂的制备方法,具体按照以下步骤实施:
步骤1、按照质量百分比分别称取如下原料:
多异氰酸酯类单体15~18%;多元醇类单体15~30%;羟基硅油2~7%;小分子扩链剂2~6%;引发剂0.01~1%;交联剂0.01~1%;溶剂8~15%;余量为去离子水。以上各组分的含量总和为100%。
步骤2、将步骤1中称取的所述多元醇类单体和羟基硅油进行混合,在油浴中搅拌均匀后,真空下抽干水分,得到羟基硅油的醇类混合物,;
步骤3、将步骤1中称取的所述多异氰酸酯添加到所述羟基硅油的醇类混合物中,在油浴中搅拌均匀后,得到含有端异氰酸酯基团的预聚体;
步骤4、将步骤1中称取的所述扩链剂添加到所述含有端异氰酸酯基团的预聚体中,在油浴中搅拌均匀后,得到扩链混合物料;
步骤5、步骤5、将步骤1中称取的所述引发剂和交联剂添加到所述扩链混合物料中,在油浴中搅拌均匀后,加入溶剂降黏,得到混合物料;
步骤6、将所述混合物料添加到步骤1中称取的所述去离子水中,搅拌均匀后,得到硅改性无氟聚氨酯防水剂。
本发明的特点还在于:
所述多异氰酸酯为甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、二环己基甲烷二异氰酸酯、六次亚甲基二异氰酸酯或异佛尔酮二异氰酸酯等中的一种或多种。
所述多元醇为聚酯多元醇、聚酰胺多元醇、聚缩醛多元醇、聚烯烃多元醇或聚醚多元醇等中的一种或多种。
所述扩链剂为二羟甲基丙酸、二羟甲基丁酸、1,4-丁二醇等中的一种或多种。
所述交联剂为三羟甲基丙烷、蓖麻油、季戊四醇、乙二醇等中的一种或多种。
步骤2中,所述油浴温度控制在100-120℃,所述搅拌时间为0.5h~2.5h。
步骤3中,所述油浴温度控制在90-110℃,所述搅拌时间为2h~3h。
步骤4中,所述油浴温度控制在50℃~70℃,所述搅拌时间为0.5h~2.5h。
步骤5中,所述油浴温度控制在40℃~70℃,所述搅拌时间为1h~3h。
步骤6中,所述搅拌时间为0.5h~1.5h。
本发明的有益效果是:
(1)羟基硅油具有极性,且表面能低,用于聚氨酯的改性可解决由于亲水基团的引入导致成品耐水性能下降的问题;此外有机硅氧烷链段具有柔软、润滑作用,不需要借助大量的树脂来提高粘合性,并且具有一定的可成膜性;可以赋予其良好的柔软性和耐水性;避免了含氟物质的使用,对环境友好,具有很高的商业价值。
具体实施方式
下面结合具体实施方式对本发明进行详细说明。描述的实施例是示例性的,仅用于解释本发明,而不能理解为对本发明的限制。
为了验证经本发明所述无氟防水剂处理后纺织品的防水效果,可通过标准方法进行考察,以便比较。所述标准方法是采用国标GB/T 4745-2012考察防水效果,下面是方法简介。
国家标准GB/T 4745-2012试验方法。截取18×18cm整理后织物绷于夹持器上并倾斜45°放置,其上方150mm处设置喷嘴在25-30s内迅速将250ml水迅速淋于倾斜织物上,淋洒完毕后取出夹持器正面向下水平敲击两次,观察实验润湿程度,然后用文字描述及与标准图片对比评定其等级,取2次平均值。
评级标准文字如表1。
表1
耐洗涤性能将整理好的纺织品进行10次标准洗涤,然后考察防水性能。
本发明所采用的技术方案是一种有机硅改性水性聚氨酯防水剂的制备方法,具体按照以下步骤实施:
步骤1、按照质量百分比分别称取如下原料:
多异氰酸酯类单体15~18%;多元醇类单体15~30%;羟基硅油2~7%;小分子扩链剂2~6%;引发剂0.01~1%;交联剂0.01~1%;溶剂8~15%;余量为去离子水。以上各组分的含量总和为100%。
步骤2、将步骤1中称取的所述多元醇类单体和羟基硅油进行混合,在油浴中搅拌均匀后,真空下抽干水分,得到羟基硅油的醇类混合物;
步骤3、将步骤1中称取的所述多异氰酸酯添加到所述羟基硅油的醇类混合物中,在油浴中搅拌均匀后,得到含有端异氰酸酯基团的预聚体;
步骤4、将步骤1中称取的所述扩链剂添加到所述含有端异氰酸酯基团的预聚体中,在油浴中搅拌均匀后,得到扩链混合物料;
步骤5、将步骤1中称取的所述引发剂和交联剂添加到所述扩链混合物料中,在油浴中搅拌均匀后,加入溶剂降黏,得到混合物料;
步骤6、将所述混合物料添加到步骤1中称取的所述去离子水中,搅拌均匀后,得到有机硅改性水性聚氨酯防水剂。
实施例1
一种有机硅改性水性聚氨酯防水剂的制备方法:
S1.按照质量百分比分别称取如下原料:二苯基甲烷二异氰酸酯15%;聚酯多元醇15%;羟基硅油2%;二羟甲基丙酸2%;引发剂0.05%;三羟甲基丙烷0.05%;溶剂8%;余量为去离子水。以上各组分的含量总和为100%;
S2.将上述称取的聚酯多元醇和羟基硅油进行混合,油浴搅拌均匀,真空下抽干水分,得到羟基硅油的醇类混合物;其中,搅拌时间为0.5h;
S3.将上述称取的二苯基甲烷二异氰酸酯添加到羟基硅油的醇类混合物中,在油浴中搅拌均匀后,得到含有端异氰酸酯基团的预聚体;其中,油浴温度控制在100℃,搅拌时间为1h;
S4.将上述称取的二羟甲基丙酸添加到含有端异氰酸酯基团的预聚体中,在油浴中搅拌均匀后,得到扩链混合物料;其中,油浴温度控制在55℃,搅拌时间为2.5h;
S5.将上述称取的引发剂和三羟甲基丙烷添加到扩链混合物料中,在油浴中搅拌均匀后,加入溶剂降黏,得到混合物料;其中,油浴温度控制在50℃,搅拌时间为3h;
S6.将混合物料添加到步骤1中称取的水中,搅拌均匀后,得到有机硅改性水性聚氨酯;其中,搅拌时间为0.5h。
实施例2
一种有机硅改性水性聚氨酯防水剂的制备方法:
S1.按照质量百分比分别称取如下原料:二苯基甲烷二异氰酸酯16%;聚酯多元醇15%;羟基硅油3%;二羟甲基丙酸2%;引发剂0.08%;三羟甲基丙烷0.06%;溶剂9%;余量为去离子水。以上各组分的含量总和为100%;
S2.将上述称取的聚酯多元醇和羟基硅油进行混合,油浴搅拌均匀,真空下抽干水分,得到羟基硅油的醇类混合物;其中,搅拌时间为1h;
S3.将上述称取的二苯基甲烷二异氰酸酯添加到羟基硅油的醇类混合物中,在油浴中搅拌均匀后,得到含有端异氰酸酯基团的预聚体;其中,油浴温度控制在105℃,搅拌时间为1h;
S4.将上述称取的二羟甲基丙酸添加到含有端异氰酸酯基团的预聚体中,在油浴中搅拌均匀后,得到扩链混合物料;其中,油浴温度控制在60℃,搅拌时间为2.5h;
S5.将上述称取的引发剂和三羟甲基丙烷添加到扩链混合物料中,在油浴中搅拌均匀后,加入溶剂降黏,得到混合物料;其中,油浴温度控制在40℃,搅拌时间为2.5h;
S6.将混合物料添加到步骤1中称取的水中,搅拌均匀后,得到有机硅改性水性聚氨酯;其中,搅拌时间为1.5h。
实施例3
一种有机硅改性水性聚氨酯防水剂的制备方法:
S1.按照质量百分比分别称取如下原料:异佛尔酮二异氰酸酯16%;聚醚多元醇15%;羟基硅油3%;二羟甲基丁酸2%;引发剂0.05%;三羟甲基丙烷0.05%;溶剂9%;余量为去离子水。以上各组分的含量总和为100%;
S2.将上述称取的聚醚多元醇和羟基硅油进行混合,油浴搅拌均匀,真空下抽干水分,得到羟基硅油的醇类混合物;其中,搅拌时间为1h;
S3.将上述称取的异佛尔酮二异氰酸酯添加到羟基硅油的醇类混合物中,在油浴中搅拌均匀后,得到含有端异氰酸酯基团的预聚体;其中,油浴温度控制在105℃,搅拌时间为1h;
S4.将上述称取的二羟甲基丁酸添加到含有端异氰酸酯基团的预聚体中,在油浴中搅拌均匀后,得到扩链混合物料;其中,油浴温度控制在60℃,搅拌时间为2.5h;
S5.将上述称取的引发剂和三羟甲基丙烷添加到扩链混合物料中,在油浴中搅拌均匀后,加入溶剂降黏,得到混合物料;其中,油浴温度控制在50℃,搅拌时间为2h;
S6.将混合物料添加到步骤1中称取的水中,搅拌均匀后,得到有机硅改性水性聚氨酯;其中,搅拌时间为1h。
实施例4
一种有机硅改性水性聚氨酯防水剂的制备方法:
S1.按照质量百分比分别称取如下原料:甲苯二异氰酸酯18%;聚醚多元醇15%;羟基硅油3%;1,4-丁二醇3%;引发剂0.05%;三羟甲基丙烷和乙二醇0.1%;溶剂10%;余量为去离子水。以上各组分的含量总和为100%;
S2.将上述称取的聚醚多元醇和羟基硅油进行混合,油浴搅拌均匀,真空下抽干水分,得到羟基硅油的醇类混合物;其中,搅拌时间为1h;
S3.将上述称取的甲苯二异氰酸酯添加到羟基硅油的醇类混合物中,在油浴中搅拌均匀后,得到含有端异氰酸酯基团的预聚体;其中,油浴温度控制在110℃,搅拌时间为2h;
S4.将上述称取的1,4-丁二醇添加到含有端异氰酸酯基团的预聚体中,在油浴中搅拌均匀后,得到扩链混合物料;其中,油浴温度控制在90℃,搅拌时间为2.5h;
S5.将上述称取的引发剂和三羟甲基丙烷和乙二醇添加到扩链混合物料中,在油浴中搅拌均匀后,加入溶剂降黏,得到混合物料;其中,油浴温度控制在70℃,搅拌时间为1.5h。
试验例1
将实施例1制得的有机硅改性水性聚氨酯防水剂与丙酮、乙二胺、二乙烯三胺混合,缓慢加去离子水乳化1.5小时得到25%含固量、外观透明的防水剂乳液,有机硅改性水性聚氨酯防水剂;丙酮、乙二胺、二乙烯三胺和水的重量比为60:5:3:240。分别在50℃、60℃、70℃和80℃下保温半小时,观测是否出现漂油漂絮现象。测试结果如表2所示:
温度(℃) | |
50 | 未出现漂油漂絮现象 |
60 | 未出现漂油漂絮现象 |
70 | 未出现漂油漂絮现象 |
80 | 未出现漂油漂絮现象 |
表2
由表2可看出,在持续升温过程中防水剂乳液均未出现漂油漂絮现象,表明本发明制得的有机硅改性水性聚氨酯防水剂具有较好的稳定性。
试验例2
有机硅改性水性聚氨酯防水剂整理后纺织物的防水性能测试:
将实施例的防水剂,加水配制成100g/L的整理液;然后将纯棉织物、涤纶织物、尼龙织物进行二浸二轧,轧余率70%;在100℃下烘干2min,170℃下定型2min。将整理后的纺织物参照AATCC 22—2010《纺织品拒水性测试:喷淋法》测试防水性;参照AATCC 135—2015《织物经家庭洗涤后的尺寸稳定性》进行洗涤20次,洗涤后的织物在60℃干燥箱中干燥。试整理纺织物的耐水洗性。测试结果如表3所示
表3不同防水剂整理纺织物的性能
初始防水性能 | 洗涤后的防水性能 | |
棉织物 | 90 | 80 |
涤纶织物 | 85 | 70 |
尼龙织物 | 85 | 70 |
上述实施例仅例示性说明本发明的原理及其功效,而非用于限制本发明。任何熟悉此技术的人士皆可在不违背本发明的精神及范畴下,对上述实施例进行修饰或改变。因此,举凡所属技术领域中具有通常知识者在未脱离本发明所揭示的精神与技术思想下所完成的一切等效修饰或改变,仍应由本发明的权利要求所涵盖。
Claims (10)
1.一种有机硅改性水性聚氨酯防水剂的制备方法,其特征在于:按质量百分比计包括以下组分。具体按照以下步骤实施,其特征在于:
步骤1、按照质量百分比分别称取如下原料:
多异氰酸酯类单体15~18%;
多元醇类单体15~30%;
羟基硅油2~7%;
小分子扩链剂2~6%;
引发剂0.01~1%;
交联剂0.01~1%;
溶剂8~15%;
余量为去离子水。以上各组分的含量总和为100%。
步骤2、将步骤1中称取的所述多元醇类单体和羟基硅油进行混合,在油浴中搅拌均匀后,真空下抽干水分,得到羟基硅油的醇类混合物;
步骤3、将步骤1中称取的所述多异氰酸酯添加到所述羟基硅油的醇类混合物中,在油浴中搅拌均匀后,得到含有端异氰酸酯基团的预聚体;
步骤4、将步骤1中称取的所述扩链剂添加到所述含有端异氰酸酯基团的预聚体中,在油浴中搅拌均匀后,得到扩链混合物料;
步骤5、将步骤1中称取的所述引发剂和交联剂添加到所述扩链混合物料中,在油浴中搅拌均匀后,加入溶剂降黏,得到混合物料;
步骤6、将所述混合物料添加到步骤1中称取的所述去离子水中,搅拌均匀后,得到有机硅改性水性聚氨酯防水剂防水剂。
2.根据权利要求1所述的一种有机硅改性水性聚氨酯防水剂的制备方法,其特征在于:所述多异氰酸酯为甲苯二异氰酸酯、二苯基甲烷二异氰酸酯、二环己基甲烷二异氰酸酯、六次亚甲基二异氰酸酯或异佛尔酮二异氰酸酯等中的一种或多种。
3.根据权利要求1所述的一种有机硅改性水性聚氨酯防水剂的制备方法,其特征在于:所述多元醇为聚酯多元醇、聚酰胺多元醇、聚缩醛多元醇、聚烯烃多元醇或聚醚多元醇等中的一种或多种。
4.根据权利要求1所述的一种有机硅改性水性聚氨酯防水剂的制备方法,其特征在于:所述扩链剂为二羟甲基丙酸、二羟甲基丁酸、1,4-丁二醇等中的一种或多种。
5.根据权利要求1所述的一种有机硅改性水性聚氨酯防水剂,其特征在于:所述交联剂为三羟甲基丙烷、蓖麻油、季戊四醇、乙二醇等中的一种或多种。
6.根据权利要求1所述的一种有机硅改性水性聚氨酯防水剂的制备方法,其特征在于,步骤2中,所述油浴温度控制在100-120℃,所述搅拌时间为0.5h~2.5h。
7.根据权利要求1所述的一种有机硅改性水性聚氨酯防水剂的制备方法,其特征在于,步骤3中,所述油浴温度控制在90-110℃,所述搅拌时间为2h~3h。
8.根据权利要求1所述的一种有机硅改性水性聚氨酯防水剂的制备方法,其特征在于,步骤4中,所述油浴温度控制在50℃~70℃,所述搅拌时间为0.5h~2.5h。
9.根据权利要求1所述的一种有机硅改性水性聚氨酯防水剂的制备方法,其特征在于,步骤5中,所述油浴温度控制在40℃~70℃,所述搅拌时间为1h~3h。
10.根据权利要求1所述的一种有机硅改性水性聚氨酯防水剂的制备方法,其特征在于,步骤6中,所述搅拌时间为0.5h~1.5h。
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