CN109609074A - 一种单组份湿固化聚氨酯热熔胶的制备方法 - Google Patents
一种单组份湿固化聚氨酯热熔胶的制备方法 Download PDFInfo
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Abstract
本发明涉及一种单组份湿固化聚氨酯热熔胶的制备方法,其步骤如下:(1)按预设比例,将聚醚多元醇、聚酯多元醇、增粘剂和抗氧剂,加入到反应釜中搅拌混合均匀,加热升温至120℃~140℃,在真空度<200Pa条件下脱水2h~3h;(2)降温至60℃~80℃,加入异氰酸酯和催化剂,搅拌,在85℃~100℃、真空度<200Pa条件下反应60min~90min;(3)加入扩链继续反应40min~60min;(4)加入填料,在100℃~120℃条件下搅拌0.5h~1h;(5)反应结束,保持出料温度在100℃~120℃,氮气保护下快速出料,密封包装即得。
Description
技术领域
本发明涉及一种单组份湿固化聚氨酯热熔胶的制备方法,特别是一种对尼龙织物具有良好粘接效果的单组份湿固化聚氨酯热熔胶的制备方法。
技术背景
单组份湿固化聚氨酯热熔胶是一类含端-NCO基团的聚氨酯胶黏剂,使用时,将其加热熔融施胶,待胶层冷却物理固化产生初步的粘结力后,胶层中的端-NCO再与空气中湿气或被黏物表面的活泼氢反应,产生化学交联固化。与传统的热塑性热熔胶相比,单组份湿固化聚氨酯热熔胶的主要优点在于固化后粘接强度要远大于前者。但是也存在一些缺点,比如初粘强度较低,用于粘接基材时,容易变形错位,影响后期加工过程,固化时间较长等,不能满足更高要求的使用需求。
为了解决这一问题,有些厂家开始对单组份湿固化聚氨酯热熔胶进行改性,比如加入增粘剂,提高粘度,从而达到提高初粘的目的。传统单组份湿固化聚氨酯热熔胶的增粘剂大都为松香树脂、碳五加氢石油树脂、萜烯树脂、丙烯酸树脂中的一种、两种或者两种以上的混合物。但是通过上胶试验发现,添加这类增粘树脂,虽然热熔胶粘度有所上升,但是由于现有的单组份湿固化聚氨酯热熔胶在配方组成和配比上不具有针对性,故其用于粘接尼龙织物时,初始和最终粘结效果仍不理想。专利CN1261519虽有公开一种用于尼龙膜复合的聚氨酯胶粘剂,其本质是一种溶剂型双组分聚氨酯胶粘剂,主要是利用溶剂和常规的聚酰胺树脂对双组分聚氨酯胶粘剂的主剂进行改性;但如何将其应用到单组份湿固化聚氨酯热熔胶体系并获得相应效果,本领域技术人员并不可知。且本发明人于实际验证中发现,常规的聚酰胺树脂与传统单组份湿固化聚氨酯热熔胶体系,存在着严重的相容性问题,影响施胶操作。
因此,如何提供一种对尼龙织物具有良好粘接效果的单组份湿固化聚氨酯热熔胶,成为待解决的问题。
发明内容
本发明的目的在于,针对上述技术问题,提供一种单组份湿固化聚氨酯热熔胶的制备方法。使得通过本发明制备所得的单组份湿固化聚氨酯热熔胶,对尼龙织物的粘接效果有明显的提升。
本发明所采用的技术方案为:一种单组份湿固化聚氨酯热熔胶的制备方法,其步骤如下:
(1)以质量份数计,将聚醚多元醇30~40份、聚酯多元醇15~25份、增粘剂15~20份和抗氧剂1份,加入到反应釜中搅拌混合均匀,加热升温至120℃~140℃,在真空度<200Pa条件下脱水2h~3h;
(2)降温至60℃~80℃,加入异氰酸酯20~25份和催化剂0.1份,搅拌,在85℃~100℃、真空度<200Pa条件下反应60min~90min;
(3)加入扩链1~1.5份,继续反应40min~60min;
(4)加入填料1~1.5份,在100℃~120℃条件下搅拌0.5h~1h;
(5)反应结束,保持出料温度在100℃~120℃,氮气保护下快速出料,密封包装即得。
上述聚醚多元醇为非晶聚醚二元醇,具体为聚氧化丙烯二醇,且其数据分子量为1000;
上述聚酯多元醇为高晶聚酯二元醇,可选自聚己二酸丁二醇酯、聚己二酸己二醇酯、聚己二酸新戊二醇酯中的一种,且其数均分子量为3000;
上述增粘剂为共聚酰胺热熔胶树脂,且其数均分子量为10000~2000,其熔点为100℃~120℃,其160℃下熔指为20~30g/10min;该共聚酰胺热熔胶树脂的型态优选为粒子或粉末。
上述抗氧剂的牌号选自1010或168;异氰酸酯为二苯基甲烷异氰酸酯;催化剂为辛酸亚锡;扩链剂为1,4-丁二醇;填料为有机蒙脱土,轻质碳酸钙,或气象二氧化硅中的一种,其规格为400 ~800目。
本发明的创新之处及有益效果在于:设计了具有针对性的配方组成和配比,特别是选用了特定的共聚酰胺热熔胶树脂作为增粘剂,对传统的单组份湿固化聚氨酯热熔胶体系进行特殊改性,有效解决了相容性问题,并使得产物对尼龙织物的粘接具有针对性,改善了复合面料织物在后期储存和加工过程中出现的错位滑移问题,有效提升了单组份湿固化聚氨酯热熔胶对尼龙织物的粘接性能和使用效率。
具体实施方式
下面通过具体实施例对本发明做进一步的具体说明,但并不以此为限。
实施例1:
一种单组份湿固化聚氨酯热熔胶的制备方法,步骤如下:
(1)按质量份数计,将聚氧化丙烯二醇40份、聚己二酸新戊二醇酯15份、共聚酰胺热熔胶树脂20份(数均分子量10000、熔点120℃、熔指30g/10min)、及抗氧剂(牌号1010)1份,加入到反应釜中搅拌混合均匀,加热升温至120℃~140℃,在真空度<200Pa条件下脱水2h~3h;
(2)降温至60℃~80℃,加入二苯基甲烷异氰酸酯21.5份和辛酸亚锡0.1份,搅拌,在85℃~100℃、真空度<200Pa条件下反应60min~90min;
(3)加入1,4-丁二醇1.4份,继续反应40min~60min;
(4)加入气相二氧化硅1份(规格400目),在100℃~120℃条件下搅拌0.5h~1h;
(5)反应结束,保持出料温度在100℃~120℃,氮气保护下快速出料,密封包装即得。
通过实施例1所得产物样品标记为A1。
对比例1:
除选用常规的丙烯酸树脂为增粘剂外,其他物料、用量及制备步骤同实施例1,通过对比例1所得产物样品标记为D1。
实施例2:
一种单组份湿固化聚氨酯热熔胶的制备方法,步骤如下:
(1)按质量份数计,将聚氧化丙烯二醇30份、聚己二酸己二醇酯25份、共聚酰胺热熔胶树脂16.4份(数均分子量15000、熔点110℃、熔指25g/10min)、及抗氧剂(牌号168)1份,加入到反应釜中搅拌混合均匀,加热升温至120℃~140℃,在真空度<200Pa条件下脱水2h~3h;
(2)降温至60℃~80℃,加入二苯基甲烷异氰酸酯25份和辛酸亚锡0.1份,搅拌,在85℃~100℃、真空度<200Pa条件下反应60min~90min;
(3)加入1,4-丁二醇1.5份,继续反应40min~60min;
(4)加入轻质碳酸钙1份(规格800目),在100℃~120℃条件下搅拌0.5h~1h;
(5)反应结束,保持出料温度在100℃~120℃,氮气保护下快速出料,密封包装即得。
通过实施例2所得产物样品标记为A2。
对比例2:
除选用常规的聚酰胺树脂(尼龙6)为增粘剂外,其他物料、用量及制备步骤同实施例2,通过对比例2所得产物样品标记为D2。
实施例3:
一种单组份湿固化聚氨酯热熔胶的制备方法,步骤如下:
(1)按质量份数计,将聚氧化丙烯二醇38份、聚己二酸丁二醇酯23.4份、共聚酰胺热熔胶树脂15份(数均分子量20000、熔点115℃、熔指20g/10min)、及抗氧剂(牌号168)1份,加入到反应釜中搅拌混合均匀,加热升温至120℃~140℃,在真空度<200Pa条件下脱水2h~3h;
(2)降温至60℃~80℃,加入二苯基甲烷异氰酸酯20份和辛酸亚锡0.1份,搅拌,在85℃~100℃、真空度<200Pa条件下反应60min~90min;
(3)加入1,4-丁二醇1份,继续反应40min~60min;
(4)加入有机蒙脱土1.5份(规格600目),在100℃~120℃条件下搅拌0.5h~1h;
(5)反应结束,保持出料温度在100℃~120℃,氮气保护下快速出料,密封包装即得。
通过实施例3所得产物样品标记为A3。
对比例3:
除选用常规的聚酰胺树脂(尼龙66)为增粘剂外,其他物料、用量及制备步骤同实施例3,通过对比例3所得产物样品标记为D3。
性能测试:
将上述各实施例及对比例所得样品用于尼龙织物粘接并进行性能测试,其中黏度测试参考GB/T 2794;初始剥离强度及固话24h后剥离强度测试参考GB/T 2791;产物的相容性采用目测方式。
具体结果如下表1所示:
表1:性能测试结果。
Claims (5)
1.一种单组份湿固化聚氨酯热熔胶的制备方法,其特征在于,包括如下步骤:
(1)以质量份数计,将聚醚多元醇30~40份、聚酯多元醇15~25份、增粘剂15~20份和抗氧剂1份,加入到反应釜中搅拌混合均匀,加热升温至120℃~140℃,在真空度<200Pa条件下脱水2h~3h;
(2)降温至60℃~80℃,加入异氰酸酯20~25份和催化剂0.1份,搅拌,在85℃~100℃、真空度<200Pa条件下反应60min~90min;
(3)加入扩链1~1.5份,继续反应40min~60min;
(4)加入填料1~1.5份,在100℃~120℃条件下搅拌0.5h~1h;
(5)反应结束,保持出料温度在100℃~120℃,氮气保护下快速出料,密封包装即得;
所述步骤(1)中,聚醚多元醇为非晶聚醚二元醇;聚酯多元醇为高晶聚酯二元醇;增粘剂为共聚酰胺热熔胶树脂,且其数均分子量为10000~2000,熔点为100℃~120℃,160℃下熔指为20~30g/10min;抗氧剂的牌号选自1010或168;
所述步骤(2)中,异氰酸酯为二苯基甲烷异氰酸酯;催化剂为辛酸亚锡;
所述步骤(3)中,扩链剂为1,4-丁二醇;
所述步骤(4)中,填料为有机蒙脱土、轻质碳酸钙、或气象二氧化硅中的一种。
2.如权利要求1所述的单组份湿固化聚氨酯热熔胶的制备方法,其特征在于:所述非晶非晶聚醚二元醇为聚氧化丙烯二醇,且其数均分子量为1000。
3.如权利要求1所述的单组份湿固化聚氨酯热熔胶的制备方法,其特征在于:所述高晶聚酯二元醇自聚己二酸丁二醇酯、聚己二酸己二醇酯、聚己二酸新戊二醇酯中的一种,且其数均分子量为3000。
4.如权利要求1所述的单组份湿固化聚氨酯热熔胶的制备方法,其特征在于:所述共聚酰胺热熔胶树脂的型态为粒子或粉末。
5.如权利要求1所述的单组份湿固化聚氨酯热熔胶的制备方法,其特征在于:所述填料规格为400 ~800目。
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