CN111040105B - 一种柔软型无氟防水剂及其制备方法 - Google Patents
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Abstract
本发明属于印染助剂技术领域,具体涉及一种柔软型无氟防水剂及其制备方法。本发明提供的无氟防水剂,以二聚酸和多元醇及脂肪族异氰酸酯、交联单体嵌段共聚形成纳米无氟防水剂乳液。同时合成一种以己二异氰酸酯三聚体为原料,以N‑甲基二乙醇胺为水溶性单体,以丁酮肟为封端剂,合成的水分散性异氰酸酯乳液作为交联剂。并与前述纳米无氟防水剂乳液复配改性,在一定温度条件下,封端异氰酸酯解封,与防水剂中的交联单体反应,交联成膜后,形成低表面张力状态,有效防止水滴的润湿和渗透,最终形成一种新的无氟防水整理剂。本发明提供的无氟防水剂可以提高防腐剂的耐洗性及防水性,手感柔软,弹性好。
Description
技术领域
本发明属于印染助剂技术领域,具体涉及一种柔软型无氟防水剂及其制备方法。
背景技术
防水剂是一种功能性整理剂,经防水剂整理过的织物具有拒水性能,广泛用于服装、雨伞、帐篷等领域。传统的防水剂一般为全氟烷基丙烯酸酯聚合物乳液(俗称C8防水剂),这类防水剂防水防油性能优异,耐洗性优良,而且成本较低。但含氟防水剂存在PFOS、PFOA等对环境有严重污染的物质,已被限制使用。无氟防水剂具有防水性能好,环境污染少的优点,是相关领域的研究热点。目前无氟防水剂存在手感硬,容易出现手抓痕、耐洗性不足的问题,拟开发具有高耐洗性、手感柔软的新型环保型无氟防水剂产品,在防水性能方面达到或接近传统C8防水剂的水平、手感柔软、耐洗性达到或超过含氟防水剂的水平。
目前含氟防水防油剂已明确在2020年全面禁止使用,因此开发高性能的无氟防水剂迫在眉睫,特别是手感柔软的高耐洗性无氟防水剂更是各种功能性纺织品的整理,必不可少的功能性整理剂,因此开发低环境危害的无氟防水剂很有必要。
中国专利申请CN109988264A公开了一种无氟防水剂及其制备方法和应用,所述无氟防水剂主要由无氟共聚物,表面活性剂,助溶剂,石蜡及水混合而成,具有优异的防水效果,可以赋予织物良好的手感,提高织物的耐洗性能。但是,这种防水剂不耐洗,且手感硬。
综上可知,现有技术的无氟防水剂普遍存在手感硬,容易出现抓痕,耐洗性不足,防水性能不佳等缺点。
发明内容
本发明的目的在于针对现有技术中存在的缺点,提供一种柔软型无氟防水剂及其制备方法。本发明提供的无氟防水剂,手感舒服,对皮肤温和,且具有足够的耐洗性能。
为了达到上述目的,本发明采用的技术方案为:
一种聚氨酯乳液,制备方法如下:
将蓖麻油酸二聚体和脂肪族异氰酸酯,按58-70:30-42比例混合,以丙酮为溶剂,在60-80℃条件下进行聚合反应,反应2-4小时后,加入2-8%二羟甲基丁酸进行扩链,保温1-2小时,降温至45℃,于12000rpm的转速下加入纯水乳化15~20min,即得粒径在80-120nm,且易溶于水的聚氨酯乳液。
本发明还提供了一种柔软型无氟防水剂专用交联剂,包括如下组分及其重量百分数:己二异氰酸酯三聚体15~25%,N-甲基二乙醇胺5~8%,丁酮肟1~3%,助溶剂0.5~1%,纯化水63~78.5%。
优选地,所述柔软型无氟防水专用交联剂,由如下组分及其重量百分数组成:己二异氰酸酯三聚体20%,N-甲基二乙醇胺7%,丁酮肟2%,助溶剂0.8%,纯化水70.2%。
优选地,所述助溶剂由异辛醇、乙酰胺及乳酸钙按质量比1~3:2~4:7~9组成。
优选地,所述助溶剂由异辛醇、乙酰胺及乳酸钙按质量比2:3:8组成。
本发明还提供了所述柔软型无氟防水剂专用交联剂的制备方法,制备过程如下:将己二异氰酸酯三聚体,N-甲基二乙醇胺,丁酮肟及助溶剂在50-60℃条件下反应45-90min,降温至35~40℃,于12000rpm的转速下搅拌,加入纯化水,继续搅拌20~30min,混合均匀,即得。
本发明还提供了一种柔软型无氟防水剂,由如下组分及其重量百分数组成:聚氨酯乳液75-90%,专用交联剂10-25%。
本发明还提供了所述柔软型无氟防水剂的制备方法,制备过程如下:于25℃的温度下,将聚氨酯乳液与专用交联剂混合,于800rpm的转速下搅拌30min,即得。
本发明中,创造性的以二聚酸和多元醇、交联单体及脂肪族异氰酸酯嵌段共聚形成纳米无氟防水剂乳液,且乳液粒径在100-150nm之间,具有极好的水分散性。而且,发明意外的发现,用丁酮肟对交联剂进行封端处理,制得水分散性封端型异氰酸酯,与聚氨酯乳液复配使用,使得聚合物在一定的温度条件下,发生交联反应,即在焙烘过程中迅速交联成膜,可以获得良好的耐洗防水性能。
进一步地,本申请的聚氨酯结构是通过筛选特殊结构的二聚酸和脂肪族异氰酸酯,在特定的水分散性扩链剂用量的情况下,得到特定粒径,并且粒径分布集中在100nm左右的水分散性聚氨酯乳液;将利用该方法制得的聚氨酯乳液加入交联剂,可以提高无氟防水剂的弹性及柔软度。
与现有技术相比,本申请提供的柔软型无氟防水剂具有如下优点:
(1)本发明提供的柔软型无氟防水剂,将水分散性封端型异氰酸酯与聚氨酯乳液复配使用,最终制得的防水剂具有良好的耐洗防水性能;
(2)本申请提供的柔软型无氟防水剂,采用特殊结构的二聚酸和脂肪族异氰酸酯制成聚氨酯乳液,大大提高了防水剂的弹性及柔软度;
(3)本申请提供的柔软型无氟防水剂,制备方法简单,成本低,形成时表面张力低,可以有效防止水滴的润湿和渗透。
具体实施方式
下面结合具体实施例对本发明作进一步解释,但是应当注意的是,以下实施例仅用以解释本发明,而不能用来限制本发明,所有与本发明相同或相近的技术方案均在本发明的保护范围之内。若未特别指明,实施例中所用的技术手段为本领域技术人员所熟知的常规手段,所用原料为市售商品。
实施例1一种柔软型无氟防水剂专用交联剂
所述柔软型无氟防水剂专用交联剂,由如下组分及其重量百分数组成:己二异氰酸酯三聚体15%,N-甲基二乙醇胺5%,丁酮肟1%,助溶剂0.5%,纯化水78.5%;所述助溶剂由异辛醇、乙酰胺及乳酸钙按质量比1:2:7组成。
所述柔软型无氟防水剂专用交联剂的制备过程为:将己二异氰酸酯三聚体,N-甲基二乙醇胺,丁酮肟及助溶剂在50℃条件下反应45min,降温至35℃,于12000rpm的转速下搅拌,加入纯化水,继续搅拌20min,混合均匀,即得。
实施例2一种柔软型无氟防水剂专用交联剂
所述柔软型无氟防水剂专用交联剂,由如下组分及其重量百分数组成:己二异氰酸酯三聚体20%,N-甲基二乙醇胺7%,丁酮肟2%,助溶剂0.8%,纯化水70.2%;所述助溶剂由异辛醇、乙酰胺及乳酸钙按质量比2:3:8组成。
所述柔软型无氟防水剂专用交联剂的制备过程为:将己二异氰酸酯三聚体,N-甲基二乙醇胺,丁酮肟及助溶剂在55℃条件下反应60min,降温至38℃,于12000rpm的转速下搅拌,加入纯化水,继续搅拌25min,混合均匀,即得。
实施例3一种柔软型无氟防水剂专用交联剂
所述柔软型无氟防水剂专用交联剂,由如下组分及其重量百分数组成:己二异氰酸酯三聚体25%,N-甲基二乙醇胺8%,丁酮肟3%,助溶剂1%,纯化水63%。所述助溶剂由异辛醇、乙酰胺及乳酸钙按质量比3:4:9组成。
所述柔软型无氟防水剂专用交联剂的制备过程为:将己二异氰酸酯三聚体,N-甲基二乙醇胺,丁酮肟及助溶剂在60℃条件下反应90min,降温至40℃,于12000rpm的转速下搅拌,加入纯化水,继续搅拌30min,混合均匀,即得。
实施例4一种柔软型无氟防水剂
所述柔软型无氟防水剂,包括如下组分及其重量百分数:聚氨酯乳液75%,实施例1所述方法制备的专用交联剂25%。
所述柔软型无氟防水剂的制备方法为:
S1、将蓖麻油酸二聚体和脂肪族异氰酸酯,按58:30比例混合,以丙酮为溶剂,在60℃条件下进行聚合反应,反应2小时后,加入2%的二羟甲基丁酸进行扩链,保温1小时,降温至45℃,于12000rpm的转速下加入纯水乳化15min,即得粒径在80nm,且易溶于水的聚氨酯乳液;
S2、于25℃的温度下,将步骤S1所得聚氨酯乳液与实施例1制得的专用交联剂混合,于800rpm的转速下搅拌30min,即得。
实施例5一种柔软型无氟防水剂
所述柔软型无氟防水剂,包括如下组分及其重量百分数:聚氨酯乳液82%,实施例2所述方法制备的专用交联剂18%。
所述柔软型无氟防水剂的制备方法为:
S1、将蓖麻油酸二聚体和脂肪族异氰酸酯,按65:37比例混合,以丙酮为溶剂,在70℃条件下进行聚合反应,反应3小时后,加入5%二羟甲基丁酸进行扩链,保温1.5小时,降温至45℃,于12000rpm的转速下加入纯水乳化18min,即得粒径在100nm,且易溶于水的聚氨酯乳液;
S2、于25℃的温度下,将步骤S1所得聚氨酯乳液与实施例2制得的专用交联剂混合,于800rpm的转速下搅拌30min,即得。
实施例6一种柔软型无氟防水剂
所述柔软型无氟防水剂,包括如下组分及其重量百分数:聚氨酯乳液90%,实施例3所述方法制备的专用交联剂10%。
所述柔软型无氟防水剂的制备方法为:
S1、将蓖麻油酸二聚体和脂肪族异氰酸酯,按70:42比例混合,以丙酮为溶剂,在80℃条件下进行聚合反应,反应4小时后,加入8%二羟甲基丁酸进行扩链,保温2小时,降温至45℃,于12000rpm的转速下加入纯水乳化20min,即得粒径在120nm,且易溶于水的聚氨酯乳液;
S2、于25℃的温度下,将步骤S1所得聚氨酯乳液与实施例2制得的专用交联剂混合,于800rpm的转速下搅拌30min,即得。
对比例1一种柔软型无氟防水剂
所述柔软型无氟防水剂,包括如下组分及其重量百分数组成:聚氨酯乳液82%,专用交联剂18%;
所述专用交联剂与实施例2类似;与实施例2的区别在于,对比例1中的助溶剂由异辛醇、乙酰胺及乳酸钙按质量比1:1:1组成。
所述柔软型无氟防水剂的制备过程与实施例5相同。
对比例2一种柔软型无氟防水剂
所述柔软型无氟防水剂,包括如下组分及其重量百分数组成:聚氨酯乳液82%,专用交联剂18%;
所述专用交联剂与实施例2类似;与实施例2的区别在于,对比例2中不包含丁酮肟。
所述柔软型无氟防水剂的制备过程与实施例5相同。
试验例1性能测试
1.试验样品:实施例4-6制得的柔软型无氟防水剂
2.试验方法:将实施例4-6制得的无氟防水剂进行平均粒径,机械稳定性和储藏稳定性测试。
其中,机械稳定性是在l0mL离心管中加入无氟防水剂,在离心机中以3000r/min离心30分钟,观察无氟防水剂有无漂浮、分层和沉淀等不稳定现象。
储藏稳定性:将水性分散液在40℃保存1个月,观察沉降的发生。
储藏稳定性评价标准:Ο:完全没有产生凝聚物
△:产生很少凝聚物
×:产生很多凝聚物
3.试验结果:具体试验结果见表1。
表1无氟防水剂性能测试结果
试验样品 | 平均粒径/nm | 机械稳定性 | 储藏稳定性 |
实施例4 | 80 | 稳定 | Ο |
实施例5 | 120 | 稳定 | Ο |
实施例6 | 100 | 稳定 | Ο |
由表1可知,本发明制得的无氟防水剂具有良好的机械稳定性和储藏稳定性。
试验例2防水性能测试
1.试验样品:实施例4-6及对比例1-2制得的无氟防水剂;国外产品防水剂R3;纯棉白色纱卡布;宝兰色65、35涤棉纱卡布。
2.试验方法:
将试验样品用去离子水分别稀释成浓度为80g/L,100g/L,120g/L,将纯棉白色纱卡布浸泡于稀释液中15分钟,用轧车轧一次,带液率100%,经过一浸一轧工艺后,将棉布于180℃下定型1min,得到无氟防水剂处理过的棉布。
将棉布用13g WOB洗衣粉,西门子滚筒洗衣机40℃洗20分钟为一次,洗后抛干。分别记录洗之前,洗5次,10次,20次后面料的防水性能。
宝兰色65、35涤棉纱卡布的试验过程与纯棉白色纱卡布的试验操作相同。
3.试验结果:具体试验结果见表2、表3、表4、表5。
表2纯棉白色纱卡布的初始防水性能
表3不同试验样品处理时纯棉白色纱卡布的防水性能
表4宝兰色65、35涤棉纱卡布初始防水性能
表5不同试验样品处理时宝兰色65、35涤棉纱卡布的防水性能
由表2、表3、表4及表5可知,本申请实施例4-6制得的无氟防水剂与国外产品R3防水剂相比,具有良好的防水性能,尤其是实施例4的无氟防水剂,洗20次后仍然具有极佳的防水性,故实施例4为本发明的最佳实施例;而对比例1制得的防水剂,由于改变了助溶剂比例,降低了物质的可溶性,对比例2中去掉了封端剂,使防水性能大大降低。
最后应当说明的是,以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (5)
1.一种柔软型无氟防水剂,其特征在于,由如下组分及其重量百分数组成:聚氨酯乳液75-90%,专用交联剂10-25%;所述聚氨酯乳液的制备方法如下:
将蓖麻油酸二聚体和脂肪族异氰酸酯,按58-70:30-42比例混合,以丙酮为溶剂,在60-80℃条件下进行聚合反应,反应2-4小时后,加入2-8%二羟甲基丁酸进行扩链,保温1-2小时,降温至45℃,于12000rpm的转速下加入纯水乳化15~20min,即得粒径在80-120nm,且易溶于水的聚氨酯乳液;
所述专用交联剂包括如下组分及其重量百分数:己二异氰酸酯三聚体15~25%,N-甲基二乙醇胺5~8%,丁酮肟1~3%,助溶剂0.5~1%,纯化水63~78.5%;所述助溶剂由异辛醇、乙酰胺及乳酸钙按质量比1~3:2~4:7~9组成。
2.如权利要求1所述的柔软型无氟防水剂,其特征在于,所述专用交联剂由如下组分及其重量百分数组成:己二异氰酸酯三聚体20%,N-甲基二乙醇胺7%,丁酮肟2%,助溶剂0.8%,纯化水70.2%。
3.如权利要求1所述的柔软型无氟防水剂,其特征在于,所述助溶剂由异辛醇、乙酰胺及乳酸钙按质量比2:3:8组成。
4.如权利要求1所述柔软型无氟防水剂,其特征在于,所述专用交联剂的制备过程如下:将己二异氰酸酯三聚体,N-甲基二乙醇胺,丁酮肟及助溶剂在50-60℃条件下反应45-90min,降温至35~40℃,于12000rpm的转速下搅拌,加入纯化水,继续搅拌20~30min,混合均匀,即得。
5.一种如权利要求1-4任一项所述柔软型无氟防水剂的制备方法,其特征在于,制备过程如下:于25℃的温度下,将聚氨酯乳液与专用交联剂混合,于800rpm的转速下搅拌30min,即得。
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