CN109181616A - 一种鞋用胶粘剂的合成方法 - Google Patents
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Abstract
本发明公开了一种鞋用胶粘剂的合成方法,所述鞋用胶粘剂为pH敏感型水性鞋用胶粘剂,所述pH敏感型水性鞋用胶粘剂由一种pH敏感型水性聚氨酯分散体添加一定量助剂而成,所述pH敏感型水性聚氨酯分散体由多异氰酸酯、多元醇、2,2‑二羟甲基丙酸、扩链剂、酚酞和有机胺等化合物聚合而成,所述胶粘剂在湿态下呈浅红色,适用于成品鞋生产时刷胶的均匀度检验,干燥后则呈无色透明状态,不影响成品鞋的美观度。所述胶粘剂为环保的水性胶粘剂,粘接强度高,耐热性好;使用工艺与现有工艺相同,无需添置新设备。
Description
技术领域
本发明涉及一种鞋用胶粘剂的合成方法。
背景技术
我国是世界上最大的成品鞋生产国。据统计,2017年,我国成品鞋产量达126亿双,约占全世界总产量的55%左右。成品鞋从原料到成品需经几十道工序,其中鞋面和鞋底的贴合成型最为关键。鞋面和鞋底贴合成型中,首先使用清洗剂、处理剂等将鞋面和鞋底的待贴合部位进行处理,通过烘道烘干后,在待贴合部位刷鞋用胶粘剂,然后进入烘道将胶粘剂中的挥发物烘干。待胶层变为无色透明后趁热进行贴合,并加压以增强贴合效果。
在此过程中,鞋用胶粘剂的刷胶显得极为重要。若部分部位刷胶不够或没有刷到位,可能造成粘接强度不足,甚至开胶。若刷胶过厚,容易积胶,胶层干燥速度慢,贴合时可能发生胶层拉丝现象,无法贴合;这时需重新进行烘烤,造成生产效率偏低,甚至部分胶层由于烘烤时间过长,出现“死胶”现象,无法贴合。
工人刷胶时,常常会查看胶层的均匀度。但由于多数鞋材,尤其是鞋底颜色较浅,而鞋用胶粘剂颜色为无色透明(溶剂型鞋胶)或乳白色(水性鞋胶),工人在查看时胶层的颜色和鞋材颜色差异不大,有时难以观察到胶层的均匀程度。因此, 应进行改革创新。
发明内容
本发明的目的在提供一种鞋用胶粘剂的合成方法,为实现上述目的,本发明采用如下技术方案:
本发明的鞋用胶粘剂是一种pH敏感型水性鞋用胶粘剂,所述的pH敏感型水性鞋用胶粘剂的合成方法包括如下步骤:
a.将1mol多元醇和0.1~0.5mol 2,2-二羟甲基丙酸,升温至100~150 oC,并通过抽真空方式去除水分,至水分的重量比小于0.1%;降温至40~50 oC,将2.1~2.5mol多异氰酸酯缓慢加入体系,并升温至60~100 oC,反应1~8小时后降温至40~50 oC,得异氰酸酯预聚体;
b.将0.001~0.002mol酚酞溶于适量丙酮中,加入0.001~0.002mol有机胺至溶液颜色恰好变为浅红色,并缓慢加入步骤(1)得到的异氰酸酯预聚体中,升温至50~70℃,反应0.5~2小时;将0.3~0.8mol扩链剂缓慢加入,并升温至50~100 oC,反应2~16小时,降温至40~50 oC;
c.将0.1~0.5mol有机胺缓慢加入体系中,调节体系pH=8~9,或体系呈浅红色。在一定的搅拌速度下,通过减压蒸馏的方式回收体系中的丙酮,同时滴加适量水,保持蒸馏温度不高于55 oC。待体系中丙酮含量降至0.1%以下时,停止蒸馏,并补充适量水至体系中聚氨酯分散体有效含量约为50%,搅拌均匀,即得浅红色pH敏感型水性聚氨酯分散体;
d.以重量份数计,取步骤(3)得到的水性聚氨酯分散体980~998份,依次加入1~2份消泡剂,1~5份润湿剂,0~10份增稠剂,分散0.5~1小时,即得pH敏感型水性鞋用胶粘剂。
所述多异氰酸酯为六亚甲基二异氰酸酯(HDI),异佛尔酮二异氰酸酯(IPDI)和二环己基甲烷二异氰酸酯(HMDI)中的一种或几种的组合物;
所述多元醇为聚乙二醇-2000(PEG-2000),聚丙二醇-1000(PPG-1000)和聚己二酸-1,4-丁二醇酯-1000(PBA-1000)中的一种或几种的组合物;
所述有机胺为三乙胺;
所述扩链剂为乙二胺(EA),二乙烯三胺(DETA),三乙烯四胺(TETA)中的一种或几种的组合物;
所述润湿剂为普为化学CoaddTM W110,CoaddTM W138和CoaddTM W130中的一种或几种的组合物;
所述消泡剂为普为化学CoaddTM DF-420和普为化学CoaddTM DF-860中的一种或两种的组合物;
所述增稠剂为万华化学Vesmody® U605,Vesmody® U905和Vesmody® U505中的一种或几种的组合物。
本发明的有益效果在于:
1.本发明所述pH敏感型水性鞋用胶粘剂为环保的水性胶粘剂,粘接强度高,耐热性好;
2.使用工艺与现有工艺基本相同,无需添置新设备;
3.本发明所述pH敏感型水性鞋用胶粘剂pH保持在8.2~10.0之间,因此液态下为浅红色液体,有利于成品鞋生产时刷胶均匀度检验;但酚酞与有机胺的结合不够稳定,在使用过程中,随着胶粘剂的干燥,将发生可逆反应,即单羟基化合物中的有机胺将脱离酚酞结构,逸出胶层,pH降低,胶层变为无色透明状,不影响成品鞋的美观度。
具体实施方式
下面将结合本发明实施例,对本发明实施例中的技术方案进行清楚、完整地描述。显然,所描述的实施例仅是本发明的一部分,基于本发明中的实施例,本领域技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
据研究发现,酚酞在pH=0~8.2时,分子中含有两个羟基,在等摩尔有机胺的作用下一个酚羟基脱氢生成一种无色的单羟基化合物,此单羟基化合物容易部分转变为浅红色的醌式结构,两种互变异构体同时存在于体系中(童沈阳,金霞. 酚酞的变色机理.《化学通报》,1988(8),52-55.)。两种互变异构体均含有一个羟基,此羟基能与异氰酸酯反应,并且不影响互变异构体由于pH变化带来的颜色转化。本发明所述胶黏剂在湿态下呈浅红色,适用于生产时刷胶的均匀度检验,干燥后则呈无色透明状态,不影响成品鞋的美观度。
本发明所述pH敏感型水性鞋用胶粘剂由一种pH敏感型水性聚氨酯分散体添加一定量助剂而成,所述pH敏感型水性聚氨酯分散体由多异氰酸酯、多元醇、2,2-二羟甲基丙酸、扩链剂、酚酞和有机胺等化合物聚合而成,以摩尔比计,所述酚酞和有机胺为1:1。
实施例 1
一种pH敏感型水性鞋用胶粘剂, 其合成方法如下:
1.将1mol PEG-2000和0.1mol 2,2-二羟甲基丙酸,升温至110 oC,并通过抽真空方式去除水分,至水分的重量比小于0.1%;降温至50 oC,将2.1mol HDI缓慢加入体系,并升温至70 oC,反应1小时后降温至50 oC,得异氰酸酯预聚体;
2.将0.002mol酚酞溶于500ml丙酮中,加入0.002mol三乙胺至溶液颜色恰好变为浅红色,并缓慢加入步骤(1)得到的异氰酸酯预聚体中,升温至60℃,反应2小时;将0.8mol二乙烯三胺缓慢加入,并升温至70 oC,反应8小时,降温至50 oC;
3.将0.1mol三乙胺缓慢加入体系中,调节体系恰好呈浅红色。在一定的搅拌速度下,通过减压蒸馏的方式回收体系中的丙酮,同时滴加2000ml水,保持蒸馏温度不高于55 oC。待体系中丙酮含量降至0.1%以下时,停止蒸馏,并补充480ml水至体系中聚氨酯分散体有效含量约为50%,搅拌均匀,即得浅红色pH敏感型水性聚氨酯分散体;
4.以重量份数计,取步骤(3)得到的水性聚氨酯分散体990份,依次加入2份CoaddTMDF-420,4份CoaddTM W110,4份Vesmody® U605,分散0.5小时,即得pH敏感型水性鞋用胶粘剂A。
实施例 2
一种pH敏感型水性鞋用胶粘剂, 其合成方法如下:
1.将1mol PPG-1000和0.3mol 2,2-二羟甲基丙酸,升温至110 oC,并通过抽真空方式去除水分,至水分的重量比小于0.1%;降温至50 oC,将2.3mol IPDI缓慢加入体系,并升温至80 oC,反应6小时后降温至40 oC,得异氰酸酯预聚体;
2.将0.0015mol酚酞溶于500ml丙酮中,加入0.0015mol三乙胺至溶液颜色恰好变为浅红色,并缓慢加入步骤(1)得到的异氰酸酯预聚体中,升温至60℃,反应2小时;将0.6mol三乙烯四胺缓慢加入,并升温至70 oC,反应10小时,降温至50 oC;
3.将0.3mol三乙胺缓慢加入体系中,调节体系恰好呈浅红色。在一定的搅拌速度下,通过减压蒸馏的方式回收体系中的丙酮,同时滴加1500ml水,保持蒸馏温度不高于55 oC。待体系中丙酮含量降至0.1%以下时,停止蒸馏,并补充150ml水至体系中聚氨酯分散体有效含量约为50%,搅拌均匀,即得浅红色pH敏感型水性聚氨酯分散体;
4.以重量份数计,取步骤(3)得到的水性聚氨酯分散体993份,依次加入1份CoaddTMDF-860,3份CoaddTM W138,3份Vesmody® U905,分散0.5小时,即得pH敏感型水性鞋用胶粘剂B。
实施例 3
一种pH敏感型水性鞋用胶粘剂, 其合成方法如下:
1.将1mol PBA-1000和0.5mol 2,2-二羟甲基丙酸,升温至110 oC,并通过抽真空方式去除水分,至水分的重量比小于0.1%;降温至50 oC,将2.5mol IPDI缓慢加入体系,并升温至65 oC,反应3小时后降温至40 oC,得异氰酸酯预聚体;
2.将0.0018mol酚酞溶于500ml丙酮中,加入0.0018mol三乙胺至溶液颜色恰好变为浅红色,并缓慢加入步骤(1)得到的异氰酸酯预聚体中,升温至60℃,反应2小时;将0.7mol乙二胺缓慢加入,并升温至70 oC,反应10小时,降温至50 oC;
3.将0.5mol三乙胺缓慢加入体系中,调节体系恰好呈浅红色。在一定的搅拌速度下,通过减压蒸馏的方式回收体系中的丙酮,同时滴加1500ml水,保持蒸馏温度不高于55 oC。待体系中丙酮含量降至0.1%以下时,停止蒸馏,并补充150ml水至体系中聚氨酯分散体有效含量约为50%,搅拌均匀,即得浅红色pH敏感型水性聚氨酯分散体;
4.以重量份数计,取步骤(3)得到的水性聚氨酯分散体994份,依次加入1份CoaddTMDF-860,2份CoaddTM W130,3份Vesmody® U505,分散0.5小时,即得pH敏感型水性鞋用胶粘剂C。
Claims (4)
1.一种鞋用胶粘剂的合成方法,其特征在于,所述鞋用胶粘剂为pH敏感型水性鞋用胶粘剂, 其合成方法如下:
a.将1mol多元醇和0.1~0.5mol 2,2-二羟甲基丙酸,升温至100~150 oC,并通过抽真空方式去除水分,至水分的重量比小于0.1%;降温至40~50 oC,将2.1~2.5mol多异氰酸酯缓慢加入体系,并升温至60~100 oC,反应1~8小时后降温至40~50 oC,得异氰酸酯预聚体;
b.将0.001~0.002mol酚酞溶于适量丙酮中,加入0.001~0.002mol有机胺至溶液颜色恰好变为浅红色,并缓慢加入步骤(1)得到的异氰酸酯预聚体中,升温至50~70℃,反应0.5~2小时;将0.3~0.8mol扩链剂缓慢加入,并升温至50~100 oC,反应2~16小时,降温至40~50 oC;
c.将0.1~0.5mol有机胺缓慢加入体系中,调节体系pH=8~9,或体系呈浅红色;
在一定的搅拌速度下,通过减压蒸馏的方式回收体系中的丙酮,同时滴加适量水,保持蒸馏温度不高于55 oC;待体系中丙酮含量降至0.1%以下时,停止蒸馏,并补充适量水至体系中聚氨酯分散体有效含量约为50%,搅拌均匀,即得浅红色pH敏感型水性聚氨酯分散体;
d.以重量份数计,取步骤(3)得到的水性聚氨酯分散体980~998份,依次加入1~2份消泡剂,1~5份润湿剂,0~10份增稠剂,分散0.5~1小时,即得pH敏感型水性鞋用胶粘剂;
所述多异氰酸酯为六亚甲基二异氰酸酯(HDI),异佛尔酮二异氰酸酯(IPDI)和二环己基甲烷二异氰酸酯(HMDI)中的一种或几种的组合物;
所述多元醇为聚乙二醇-2000(PEG-2000),聚丙二醇-1000(PPG-1000)和聚己二酸-1,4-丁二醇酯-1000(PBA-1000)中的一种或几种的组合物;
所述有机胺为三乙胺;
所述扩链剂为乙二胺(EA),二乙烯三胺(DETA),三乙烯四胺(TETA)中的一种或几种的组合物;
所述润湿剂为普为化学CoaddTM W110,CoaddTM W138和CoaddTM W130中的一种或几种的组合物;
所述消泡剂为普为化学CoaddTM DF-420和普为化学CoaddTM DF-860中的一种或两种的组合物;
所述增稠剂为万华化学Vesmody® U605,Vesmody® U905和Vesmody® U505中的一种或几种的组合物。
2.根据权利要求1所述鞋用胶粘剂,其特征在于,所述pH敏感型水性鞋用胶粘剂其合成方法如下:
1).将1mol PEG-2000和0.1mol 2,2-二羟甲基丙酸,升温至110 oC,并通过抽真空方式去除水分,至水分的重量比小于0.1%;降温至50 oC,将2.1mol HDI缓慢加入体系,并升温至70 oC,反应1小时后降温至50 oC,得异氰酸酯预聚体;
2).将0.002mol酚酞溶于500ml丙酮中,加入0.002mol三乙胺至溶液颜色恰好变为浅红色,并缓慢加入步骤(1)得到的异氰酸酯预聚体中,升温至60℃,反应2小时;将0.8mol二乙烯三胺缓慢加入,并升温至70 oC,反应8小时,降温至50 oC;
3). 将0.1mol三乙胺缓慢加入体系中,调节体系恰好呈浅红色;
在一定的搅拌速度下,通过减压蒸馏的方式回收体系中的丙酮,同时滴加2000ml水,保持蒸馏温度不高于55 oC;
待体系中丙酮含量降至0.1%以下时,停止蒸馏,并补充480ml水至体系中聚氨酯分散体有效含量约为50%,搅拌均匀,即得浅红色pH敏感型水性聚氨酯分散体;
4).以重量份数计,取步骤(3)得到的水性聚氨酯分散体990份,依次加入2份CoaddTMDF-420,4份CoaddTM W110,4份Vesmody® U605,分散0.5小时,即得pH敏感型水性鞋用胶粘剂A。
3.根据权利要求1所述鞋用胶粘剂,其特征在于,所述pH敏感型水性鞋用胶粘剂其合成方法如下:
1).将1mol PPG-1000和0.3mol 2,2-二羟甲基丙酸,升温至110 oC,并通过抽真空方式去除水分,至水分的重量比小于0.1%;降温至50 oC,将2.3mol IPDI缓慢加入体系,并升温至80 oC,反应6小时后降温至40 oC,得异氰酸酯预聚体;
2).将0.0015mol酚酞溶于500ml丙酮中,加入0.0015mol三乙胺至溶液颜色恰好变为浅红色,并缓慢加入步骤(1)得到的异氰酸酯预聚体中,升温至60℃,反应2小时;将0.6mol三乙烯四胺缓慢加入,并升温至70 oC,反应10小时,降温至50 oC;
3).将0.3mol三乙胺缓慢加入体系中,调节体系恰好呈浅红色;
在一定的搅拌速度下,通过减压蒸馏的方式回收体系中的丙酮,同时滴加1500ml水,保持蒸馏温度不高于55 oC;
待体系中丙酮含量降至0.1%以下时,停止蒸馏,并补充150ml水至体系中聚氨酯分散体有效含量约为50%,搅拌均匀,即得浅红色pH敏感型水性聚氨酯分散体;
4).以重量份数计,取步骤(3)得到的水性聚氨酯分散体993份,依次加入1份CoaddTMDF-860,3份CoaddTM W138,3份Vesmody® U905,分散0.5小时,即得pH敏感型水性鞋用胶粘剂B。
4.根据权利要求1所述鞋用胶粘剂,其特征在于,所述pH敏感型水性鞋用胶粘剂其合成方法如下:
将1mol PBA-1000和0.5mol 2,2-二羟甲基丙酸,升温至110 oC,并通过抽真空方式去除水分,至水分的重量比小于0.1%;降温至50 oC,将2.5mol IPDI缓慢加入体系,并升温至65oC,反应3小时后降温至40 oC,得异氰酸酯预聚体;
1). 将0.0018mol酚酞溶于500ml丙酮中,加入0.0018mol三乙胺至溶液颜色恰好变为浅红色,并缓慢加入步骤(1)得到的异氰酸酯预聚体中,升温至60℃,反应2小时;将0.7mol乙二胺缓慢加入,并升温至70 oC,反应10小时,降温至50 oC;
2).将0.5mol三乙胺缓慢加入体系中,调节体系恰好呈浅红色;
在一定的搅拌速度下,通过减压蒸馏的方式回收体系中的丙酮,同时滴加1500ml水,保持蒸馏温度不高于55 oC;
待体系中丙酮含量降至0.1%以下时,停止蒸馏,并补充150ml水至体系中聚氨酯分散体有效含量约为50%,搅拌均匀,即得浅红色pH敏感型水性聚氨酯分散体;
以重量份数计,取步骤(3)得到的水性聚氨酯分散体994份,依次加入1份CoaddTM DF-860,2份CoaddTM W130,3份Vesmody® U505,分散0.5小时,即得pH敏感型水性鞋用胶粘剂C。
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