CN107779170A - 一种环保型粘合密封剂的制备方法 - Google Patents
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Abstract
本发明涉及一种环保型粘合密封剂的制备方法,包括:将30~50份硅烷封端聚合物、5~20份增塑剂、25~45份填料、1~10份颜料、1~2份紫外光吸收剂、1~2份光稳定剂依次加入双行星搅拌釜内,在100~110℃条件下搅拌分散并真空脱水2小时,真空度不小于‑0.098MPa,冷却至50℃以下,将1~5份除水剂加入双行星搅拌釜内,在真空状态下混合10分钟,然后将1~5份增粘剂加入双行星搅拌釜内,在真空状态下混合10分钟,最后将0.5~5份催化剂加入搅拌釜内,N2封存包装即可;本发明密封剂单组分包装,易于施胶,固化后胶层对基材具有较高的粘接力,耐冷热冲击性能好。
Description
技术领域
本发明涉及一种环保型粘合密封剂的制备方法,尤其涉及一种不含有机锡催化剂和邻苯二甲酸酯(或盐)类增塑剂的粘合密封剂的制备方法。
背景技术
胶粘剂工业突飞猛进的发展,为社会提供了许多新胶种,胶粘剂的功能和应用已受到广泛重视,其在日常生活、工业制造、电子电器、医疗卫生等领域有着越来越广阔的应用,而胶粘剂的环保问题却往往被人所忽视,化学物质污染引起的环境和生态危机,已成为影响国民经济和社会发展的重要因素。在环境意识和健康意识日益提高的今天,对胶粘剂的环保问题的要求将愈加严格,保护环境显得更为重要,生产单位应制造出环保型绿色胶粘剂,使用者则渴望能用上无毒无害的胶粘剂。有机锡化合物在胶黏剂中的主要用途有:用作催化剂(二丁基锡、辛酸亚锡)、稳定剂(如二甲基锡、二辛基锡、四苯基锡)、农用杀虫剂、杀菌剂(如二丁基锡、三丁基锡、三苯基锡)、防霉剂等。有机锡化合物对生物体的主要损害为:中枢神经系统会造成脑白质水肿、细胞能量利用中氧化磷酸化过程受障、胸腺和淋巴系统的抑制作用、细胞免疫性受妨害、激素分泌抑制引起糖尿病和高血脂病等。对人的毒性,局部对皮肤、呼吸道、角膜的刺激作用,通过皮肤或脑水肿会引起全身中毒,甚至死亡。因此,欧盟出台指令于2015年1月1日开始对日用消费品或专业用产品中释放出来的有机锡化合物(含二、三取代有机锡化合物)限制使用,其限量要求为商品中锡含量的质量百分比浓度小于0.1%,有些更严格的客户要求产品中二、三取代有机锡化合物的含量为零。
另一方面,邻苯二甲酸酯(或盐)类增塑剂在塑料、粘合剂、涂料、密封材料等领域有着广泛的应用,这类物质与高分子聚合物之间是物理结合,随着时间的推移,它们会慢慢从材料中迁移出来,污染空气、土壤、水源乃至食物,邻苯二甲酸酯可在人体内逐渐累积并可分解成相应的代谢产物进而危害人体健康。因此,欧盟对邻苯二甲酸酯类增塑剂限制使用的产品越来越多。
发明内容
本发明的技术方案如下:一种不含有机锡催化剂和邻苯二甲酸酯(或盐)类增塑剂的粘合密封剂的制备方法包括:将30~50份硅烷封端聚合物、5~20份增塑剂、25~45份填料、1~10份颜料、1~2份紫外光吸收剂、1~2份光稳定剂依次加入双行星搅拌釜内,在100~110℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa ,冷却至50℃以下,将1~5份除水剂加入双行星搅拌釜内,在真空状态下混合10分钟,然后将1~5份增粘剂加入双行星搅拌釜内,在真空状态下混合10分钟,最后将0.5~5份催化剂加入搅拌釜内,在真空状态下混合15分钟,真空度不小于-0.098MPa , N2封存包装即可。
在上述技术方案的基础上,本发明还可以做如下改进。
进一步,所述硅烷封端聚合物为日本KANEKA的产品,如SAX580、SAX510、MA451、MAX602、MA440中的一种或几种的混合物。
SAX580、SAX510、MA440、MAX602这四种硅烷封端聚合物属于日本KANEKA的常规产品,在国内有备货并且性价比高,较其他一些公司的端硅烷基聚醚或端硅烷基聚氨酯具有贮存稳定性好,力学性能优异,工艺操作性好等特点。
进一步,所述增塑剂为SAT010、SAX015、聚醚多元醇DP-2000或 DP-3000。
本发明所用的增塑剂 SAT010、SAX015具有活性基团的一类物质,能参与到反应中去,不会降低固化后胶的强度,并且在使用过程中不会析出。聚醚多元醇DP-2000或 DP-3000是属于环保类增塑剂,不在欧盟限制使用范围内,并且它与体系的相容性比较好,不容易析出。
进一步,所述填料为纳米活性碳酸钙、氧化铝、氢氧化铝、气相二氧化硅中的一种或几种的混合物。
进一步,所述颜料为钛白粉、炭黑中的一种。
进一步,所述光稳定剂为双(2, 2, 6, 6-四甲基-4-哌啶基)癸二酸酯。
进一步,所述紫外光吸收剂为UV-329。
进一步,所述除水剂为乙烯基三甲氧基硅烷。
进一步,所述增粘剂为N-β-氨乙基-γ-氨丙基三甲氧基硅烷、γ―(2,3-环氧丙氧)丙基三甲氧基硅烷、氨丙基三甲氧基硅烷、氨丙基三乙氧基硅烷中的一种或几种的混合物。
进一步,所述催化剂为1,8-二氮杂二环十一碳-7-烯(DBU)。
众所周知,锡类化合物在硅胶、聚氨酯、硅烷封端聚合物等密封胶中是应用最多,也是最有效的催化剂,随着环保意识的不断增强,很多场合都限制或禁止使用锡化合物做催化剂。本发明的催化剂是一种特殊的物质,其在聚氨酯、环氧胶粘剂领域有些应用,但在硅烷封端聚合物粘合密封剂中作为催化剂使用尚未见报道,用它做催化剂的粘合密封剂与锡催化的粘合密封剂相比,表干时间和性能差别不大,更重要的是它不是欧盟限制或禁用物质。
本发明的有益效果是:本发明提供的一种环保型粘合密封剂,不含有机锡催化剂和邻苯二甲酸酯(或盐)类增塑剂,符合欧盟出口标准,通过ROHS、REACH等认证,单组分包装,易于施胶,固化后胶层对基材具有较高的粘接力,耐冷热冲击性能好。
具体实施方式
以下对本发明的原理和特征进行描述,所举实例只用于解释本发明,并非用于限定本发明的范围。
实施例1
将20份硅烷封端聚合物SAX580,10份MA440,5份DP-3000,25份纳米活性碳酸钙,1份钛白粉,1份双(2, 2, 6, 6-四甲基-4 - 哌啶基)癸二酸酯,1份UV-329,依次加入双行星搅拌釜内,在100~110℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa , 冷却至50℃以下,将1份乙烯基三甲氧基硅烷加入双行星搅拌釜内,在氮气保护下混合10分钟,之后将1份N-β-氨乙基-γ-氨丙基三甲氧基硅烷加入双行星搅拌釜内在氮气保护下混合10分钟,最后将0.5份DBU加入搅拌釜内在真空状态下混合10分钟,真空度不小于-0.098MPa , N2封存包装即可。
实施例2
将50份硅烷封端聚合物MAX620,20份SAT010,25份纳米活性碳酸钙,20份氧化铝,10份钛白粉,2份双(2, 2, 6, 6-四甲基-4 - 哌啶基)癸二酸酯,2份UV-329,依次加入双行星搅拌釜内,在100~110℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa ,冷却至50℃以下,将5份乙烯基三甲氧基硅烷加入双行星搅拌釜内,在氮气保护下混合10分钟,之后将5份氨丙基三甲氧基硅烷加入双行星搅拌釜内在氮气保护下混合10分钟,最后将5份DBU加入搅拌釜内在真空状态下混合10分钟,真空度不小于-0.098MPa , N2封存包装即可。
实施例3
将20份硅烷封端聚合物MA451,20份SAX510,10份SAX015,15份纳米活性碳酸钙,20份氢氧化铝,1份炭黑,1.5份双(2, 2, 6, 6-四甲基-4 - 哌啶基)癸二酸酯,1.5份UV-329,依次加入双行星搅拌釜内,在100~110℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa , 冷却至50℃以下,将3份乙烯基三甲氧基硅烷加入双行星搅拌釜内,在氮气保护下混合10分钟,之后将1.5份N-β-氨乙基-γ-氨丙基三甲氧基硅烷和1.5份γ―(2,3-环氧丙氧)丙基三甲氧基硅烷加入双行星搅拌釜内在氮气保护下混合10分钟,最后将3份DBU加入搅拌釜内在真空状态下混合10分钟,真空度不小于-0.098MPa , N2封存包装即可。
实施例4
将20份硅烷封端聚合物MAX620,15份SAX580,15份DP-2000,30份氧化铝,5份气相二氧化硅,5份炭黑,1.5份双(2, 2, 6, 6-四甲基-4 - 哌啶基)癸二酸酯,1.5份UV-329,依次加入双行星搅拌釜内,在100~110℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa , 冷却至50℃以下,将2份乙烯基三甲氧基硅烷加入双行星搅拌釜内,在氮气保护下混合10分钟,之后将5份氨丙基三乙氧基硅烷加入双行星搅拌釜内在氮气保护下混合10分钟,最后将4份DBU加入搅拌釜内在真空状态下混合10分钟,真空度不小于-0.098MPa ,N2封存包装即可。
将实施例1至4和通用型端硅烷基聚合物密封胶做性能对比测试,力学性能数据均在23±2℃,相对湿度50±5%的条件下固化7天后测试所得,具体测试结果见下表1。
试验实施例
通过下面的试验测试本发明的一种不含有机锡催化剂和邻苯二甲酸酯(或盐)类增塑剂的粘合密封剂的性能。
试验实施例1
表干时间依据GB/T13477.5-2002进行测试。
试验实施例2
拉伸强度和断裂伸长率依据GB/T 528-2009进行测试。
试验实施例3
剪切强度依据GB/T 7124-2008进行测试。
将通用型含锡类催化剂的端硅烷基聚合物密封胶与实施例1、2、3、4进行性能对比测试,测试结果见下表。
从上表的测试结果可以看出本发明制备的一种不含有机锡催化剂和邻苯二甲酸酯(或盐)类增塑剂的粘合密封剂,虽然未使用常用的有机锡化合物做催化剂,但通过配方调整后,其各方面性能与含锡配方相当,可以满足客户的需要,更重要的是配方体系中不含有机锡催化剂和邻苯二甲酸酯类增塑剂,更加环保和安全,符合RoHS和REACH的严格要求。
以上所述仅为本发明的较佳实施例,并不是用于限制本发明范围,凡是在本发明的精神和原则之内,所做的任何修改、等同替换、改进等,均已该包含在本发明的保护范围之内。
Claims (4)
1.一种环保型粘合密封剂的制备方法,其特征在于,包括:将30~50份硅烷封端聚合物、5~20份增塑剂、25~45份填料、1~10份颜料、1~2份紫外光吸收剂、1~2份光稳定剂依次加入双行星搅拌釜内,在100~110℃条件下搅拌分散并真空脱水2小时,真空度不小于-0.098MPa ,冷却至50℃以下,将1~5份除水剂加入双行星搅拌釜内,在真空状态下混合10分钟,然后将1~5份增粘剂加入双行星搅拌釜内,在真空状态下混合10分钟,最后将0.5~5份催化剂加入搅拌釜内,在真空状态下混合15分钟,真空度不小于-0.098MPa , N2封存包装即可;
所述硅烷封端聚合物为日本KANEKA的SAX580、SAX510、MA451、MAX602、MA440中的一种或几种的混合物。
2.根据权利要求1所述的制备方法,其特征在于,所述增塑剂为SAT010、SAX015、聚醚多元醇DP-2000或 DP-3000中的一种。
3.根据权利要求1所述的制备方法,其特征在于,所述填料为纳米活性碳酸钙、氧化铝、氢氧化铝、气相二氧化硅中的一种或几种的混合物;所述光稳定剂为双(2, 2, 6, 6-四甲基-4-哌啶基)癸二酸酯;所述紫外光吸收剂为UV-329;所述除水剂为乙烯基三甲氧基硅烷;所述增粘剂为N-β-氨乙基-γ-氨丙基三甲氧基硅烷、γ―(2,3-环氧丙氧)丙基三甲氧基硅烷、氨丙基三甲氧基硅烷、氨丙基三乙氧基硅烷中的一种或几种的混合物。
4.根据权利要求1所述的制备方法,其特征在于,所述催化剂为1,8-二氮杂二环十一碳-7-烯。
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