CN112126397B - 一种环氧辣木油基水性聚氨酯胶黏剂及其制备方法 - Google Patents
一种环氧辣木油基水性聚氨酯胶黏剂及其制备方法 Download PDFInfo
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Abstract
本发明提供了一种环氧辣木油基水性聚氨酯胶黏剂及其制备方法。步骤如下:制备环氧辣木油多元醇;将上述环氧辣木油多元醇和甲苯二异氰酸酯混合均匀,加入1,4‑丁二醇、二羟甲基丙酸进行扩链反应,得到聚氨酯预聚体;降温,加入丙酮和三乙胺中和反应;降温至室温,在转速1000‑2000r/min下缓慢加入蒸馏水进行分散,相转变后滴加三乙胺至乳液pH至6‑8,保持高速乳化;压蒸馏脱除丙酮后即得环氧辣木油基水性聚氨酯胶黏剂。本发明的环氧辣木油基水性聚氨酯胶黏剂具有粘度高,成模性好,胶膜的物理机械性能佳。
Description
技术领域
本发明涉及新材料领域,具体涉及一种环氧辣木油基水性聚氨酯胶黏剂及其制备方法。
背景技术
水性聚氨酯胶粘剂以水为溶剂,采用自乳化技术制备分散体,相比传统聚氨酯胶粘剂,在合成树脂时减少或者不使用有机溶剂,这一方面降低了原料成本,另一方面也降低了可挥发性有机污染物的排放,改善了人居环境,降低了化工事故的风险。因此,水性聚氨酯胶粘剂的应用领域十分广泛,在汽车、医药行业中作为粘接层,在满足优异粘接力的同时,赋予了材料良好的手感和防水透气等功能;在汽车行业中,根除了由于暴晒造成的残留溶剂挥发,保证了驾乘人员的身体健康。
辣木油是一种可再生资源,价格低廉,分子中含有大量羟基,将其进行环氧化后,其光稳定性、挥发性、耐候性、耐热性都得到了很大的提高,将其制备水性胶黏剂还未见报道。
发明内容
要解决的技术问题:本发明的目的是提供一种环氧辣木油基水性聚氨酯胶黏剂,具有粘度高,成模性好,胶膜的物理机械性能佳。
技术方案:一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,包括以下步骤:
(1)将无水甲醇、蒸馏水和氟硼酸加入三口烧瓶里,将环氧辣木油加入滴液漏斗中,在转速200-300rpm下边搅拌边在70-75℃下滴加环氧辣木油,反应60-90min;
(2)加入碳酸氢钠中和氟硼酸,结束反应;
(3)将反应液转入分液漏斗中,加入蒸馏水和三氯甲烷进行萃取,静置分层;
(4)将有机相转入分液漏斗中,加入蒸馏水洗涤,静置分层,取下层有机相,加入无水硫酸钠,搅拌15min后放置至干燥完全;
(5)过滤,滤液减压蒸馏除掉三氯甲烷即得环氧辣木油多元醇;
(6)将上述环氧辣木油多元醇和甲苯二异氰酸酯混合均匀,加入1,4-丁二醇、二羟甲基丙酸进行扩链反应,80-85℃下反应2-2.5h,得到聚氨酯预聚体;
(7)降温至45℃,加入丙酮和三乙胺中和反应10min;
(8)降温至室温,在转速1000-2000r/min下缓慢加入-5℃的蒸馏水进行分散,相转变后滴加三乙胺至乳液pH至6-8,保持高速乳化20-30min;
(9)压蒸馏脱除丙酮后即得环氧辣木油基水性聚氨酯胶黏剂。
进一步的,所述环氧辣木油的制备步骤如下:
(1)将100g辣木油和0.8-1g过氧磷钨酸盐混合,在温度60-65℃下搅拌均匀,并缓慢匀速滴加130-150mL双氧水;
(2)滴加完毕后,以搅拌速度100-200rpm下反应7-8h,反应结束后用分液漏斗静置分层,弃去下层,并对上层液体进行水洗至中性;
(3)在上层液体中加入无水硫酸钠除去其中的水,即得环氧辣木油。
进一步的,所述环氧辣木油的环氧值为7.18-7.35%。
进一步的,所述步骤(1)中无水甲醇与蒸馏水的摩尔比为4-5:1;无水甲醇与环氧辣木油的摩尔比为12-13:1;氟硼酸的添加量为0.3-0.4%。
进一步的,所述步骤(6)中环氧辣木油多元醇和甲苯二异氰酸酯的摩尔比为1:3。
进一步的,所述1,4-丁二醇的含量为环氧辣木油多元醇的2-2.5wt%、二羟甲基丙酸的含量为环氧辣木油多元醇的1-2wt%。
上述的一种环氧辣木油基水性聚氨酯胶黏剂的制备方法制备的环氧辣木油基水性聚氨酯胶黏剂。
有益效果:
1、环氧辣木油中的三官能度部分可以用作内交联剂,大幅度增加聚氨酯分子链的网状交联程度,提高水性聚氨酯的耐热性能和粘接性能;二官能度的部分可用于代替部分聚醚或小分子扩链剂,降低配方成本。
2、本发明的环氧辣木油分子中的非极性长链脂肪酸结构能有效提高胶膜耐水性。
3、本发明的环氧辣木油基水性聚氨酯胶黏剂,具有粘度高,成模性好,胶膜的物理机械性能佳。
具体实施方式
实施例1
一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,包括以下步骤:
(1)将无水甲醇、蒸馏水和氟硼酸加入三口烧瓶里,将环氧辣木油加入滴液漏斗中,在转速200rpm下边搅拌边在70℃下滴加环氧辣木油,反应60min,其中,无水甲醇与蒸馏水的摩尔比为4:1;无水甲醇与环氧辣木油的摩尔比为12:1;氟硼酸的添加量为0.3%;
(2)加入碳酸氢钠中和氟硼酸,结束反应;
(3)将反应液转入分液漏斗中,加入蒸馏水和三氯甲烷进行萃取,静置分层;
(4)将有机相转入分液漏斗中,加入蒸馏水洗涤,静置分层,取下层有机相,加入无水硫酸钠,搅拌15min后放置至干燥完全;
(5)过滤,滤液减压蒸馏除掉三氯甲烷即得环氧辣木油多元醇;
(6)将上述环氧辣木油多元醇和甲苯二异氰酸酯混合均匀,加入1,4-丁二醇、二羟甲基丙酸进行扩链反应,80℃下反应2h,得到聚氨酯预聚体,其中,环氧辣木油多元醇和甲苯二异氰酸酯的摩尔比为1:3,1,4-丁二醇的含量为环氧辣木油多元醇的2wt%、二羟甲基丙酸的含量为环氧辣木油多元醇的1wt%;
(7)降温至45℃,加入丙酮和三乙胺中和反应10min;
(8)降温至室温,在转速1000r/min下缓慢加入-5℃的蒸馏水进行分散,相转变后滴加三乙胺至乳液pH至6,保持高速乳化20min;
(9)压蒸馏脱除丙酮后即得环氧辣木油基水性聚氨酯胶黏剂。
环氧辣木油的制备步骤如下:
(1)将100g辣木油和0.8g过氧磷钨酸盐混合,在温度60℃下搅拌均匀,并缓慢匀速滴加130mL双氧水;
(2)滴加完毕后,以搅拌速度100rpm下反应7h,反应结束后用分液漏斗静置分层,弃去下层,并对上层液体进行水洗至中性;
(3)在上层液体中加入无水硫酸钠除去其中的水,即得环氧值为7.18%的环氧辣木油。本实施例所制备的胶黏剂的粘度在25℃下为9.33MPa·s;成模性很好,胶膜的物理机械性能如下:
硬度(邵尔A) | 68 |
拉伸强度(MPa) | 17.3 |
断裂伸长率(%) | 926 |
实施例2
一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,包括以下步骤:
(1)将无水甲醇、蒸馏水和氟硼酸加入三口烧瓶里,将环氧辣木油加入滴液漏斗中,在转速250rpm下边搅拌边在72℃下滴加环氧辣木油,反应70min,其中,无水甲醇与蒸馏水的摩尔比为4.5:1;无水甲醇与环氧辣木油的摩尔比为12.5:1;氟硼酸的添加量为0.35%;
(2)加入碳酸氢钠中和氟硼酸,结束反应;
(3)将反应液转入分液漏斗中,加入蒸馏水和三氯甲烷进行萃取,静置分层;
(4)将有机相转入分液漏斗中,加入蒸馏水洗涤,静置分层,取下层有机相,加入无水硫酸钠,搅拌15min后放置至干燥完全;
(5)过滤,滤液减压蒸馏除掉三氯甲烷即得环氧辣木油多元醇;
(6)将上述环氧辣木油多元醇和甲苯二异氰酸酯混合均匀,加入1,4-丁二醇、二羟甲基丙酸进行扩链反应,83℃下反应2.5h,得到聚氨酯预聚体,其中,环氧辣木油多元醇和甲苯二异氰酸酯的摩尔比为1:3,1,4-丁二醇的含量为环氧辣木油多元醇的2.3wt%、二羟甲基丙酸的含量为环氧辣木油多元醇的1.5wt%;
(7)降温至45℃,加入丙酮和三乙胺中和反应10min;
(8)降温至室温,在转速1500r/min下缓慢加入-5℃的蒸馏水进行分散,相转变后滴加三乙胺至乳液pH至7,保持高速乳化25min;
(9)压蒸馏脱除丙酮后即得环氧辣木油基水性聚氨酯胶黏剂。
环氧辣木油的制备步骤如下:
(1)将100g辣木油和0.9g过氧磷钨酸盐混合,在温度63℃下搅拌均匀,并缓慢匀速滴加140mL双氧水;
(2)滴加完毕后,以搅拌速度150rpm下反应7.5h,反应结束后用分液漏斗静置分层,弃去下层,并对上层液体进行水洗至中性;
(3)在上层液体中加入无水硫酸钠除去其中的水,即得环氧值为7.25%的环氧辣木油。本实施例所制备的胶黏剂的粘度在25℃下为9.33MPa·s;成模性很好,胶膜的物理机械性能如下:
硬度(邵尔A) | 70 |
拉伸强度(MPa) | 17.6 |
断裂伸长率(%) | 933 |
实施例3
一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,包括以下步骤:
(1)将无水甲醇、蒸馏水和氟硼酸加入三口烧瓶里,将环氧辣木油加入滴液漏斗中,在转速300rpm下边搅拌边在75℃下滴加环氧辣木油,反应90min,其中,无水甲醇与蒸馏水的摩尔比为5:1;无水甲醇与环氧辣木油的摩尔比为13:1;氟硼酸的添加量为0.4%;
(2)加入碳酸氢钠中和氟硼酸,结束反应;
(3)将反应液转入分液漏斗中,加入蒸馏水和三氯甲烷进行萃取,静置分层;
(4)将有机相转入分液漏斗中,加入蒸馏水洗涤,静置分层,取下层有机相,加入无水硫酸钠,搅拌15min后放置至干燥完全;
(5)过滤,滤液减压蒸馏除掉三氯甲烷即得环氧辣木油多元醇;
(6)将上述环氧辣木油多元醇和甲苯二异氰酸酯混合均匀,加入1,4-丁二醇、二羟甲基丙酸进行扩链反应,85℃下反应2.5h,得到聚氨酯预聚体,其中,环氧辣木油多元醇和甲苯二异氰酸酯的摩尔比为1:3,1,4-丁二醇的含量为环氧辣木油多元醇的2.5wt%、二羟甲基丙酸的含量为环氧辣木油多元醇的2wt%;
(7)降温至45℃,加入丙酮和三乙胺中和反应10min;
(8)降温至室温,在转速2000r/min下缓慢加入-5℃的蒸馏水进行分散,相转变后滴加三乙胺至乳液pH至8,保持高速乳化30min;
(9)压蒸馏脱除丙酮后即得环氧辣木油基水性聚氨酯胶黏剂。
环氧辣木油的制备步骤如下:
(1)将100g辣木油和1g过氧磷钨酸盐混合,在温度65℃下搅拌均匀,并缓慢匀速滴加150mL双氧水;
(2)滴加完毕后,以搅拌速度200rpm下反应8h,反应结束后用分液漏斗静置分层,弃去下层,并对上层液体进行水洗至中性;
(3)在上层液体中加入无水硫酸钠除去其中的水,即得环氧值为7.35%的环氧辣木油。本实施例所制备的胶黏剂的粘度在25℃下为9.33MPa·s;成模性很好,胶膜的物理机械性能如下:
硬度(邵尔A) | 71 |
拉伸强度(MPa) | 17.7 |
断裂伸长率(%) | 942 |
Claims (7)
1.一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,其特征在于,包括以下步骤:
(1)将无水甲醇、蒸馏水和氟硼酸加入三口烧瓶里,将环氧辣木油加入滴液漏斗中,在转速200-300rpm下边搅拌边在70-75℃下滴加环氧辣木油,反应60-90 min;
(2)加入碳酸氢钠中和氟硼酸,结束反应;
(3)将反应液转入分液漏斗中,加入蒸馏水和三氯甲烷进行萃取,静置分层;
(4)将有机相转入分液漏斗中,加入蒸馏水洗涤,静置分层,取下层有机相,加入无水硫酸钠,搅拌15 min 后放置至干燥完全;
(5)过滤,滤液减压蒸馏除掉三氯甲烷即得环氧辣木油多元醇;
(6)将上述环氧辣木油多元醇和甲苯二异氰酸酯混合均匀,加入1,4-丁二醇、二羟甲基丙酸进行扩链反应,80-85℃下反应2-2.5 h,得到聚氨酯预聚体;
(7)降温至45℃,加入丙酮和三乙胺中和反应10 min;
(8)降温至室温,在转速1000-2000 r/min下缓慢加入-5℃的蒸馏水进行分散,相转变后滴加三乙胺至乳液pH至6-8,保持高速乳化20-30 min;
(9)压蒸馏脱除丙酮后即得环氧辣木油基水性聚氨酯胶黏剂。
2.根据权利要求1所述的一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,其特征在于,所述环氧辣木油的制备步骤如下:
(1)将100g辣木油和0.8-1g过氧磷钨酸盐混合,在温度60-65℃下搅拌均匀,并缓慢匀速滴加130-150mL双氧水;
(2)滴加完毕后,以搅拌速度100-200rpm下反应7-8h,反应结束后用分液漏斗静置分层,弃去下层,并对上层液体进行水洗至中性;
(3)在上层液体中加入无水硫酸钠除去其中的水,即得环氧辣木油。
3.根据权利要求1所述的一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,其特征在于,所述环氧辣木油的环氧值为7.18-7.35%。
4.根据权利要求1所述的一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,其特征在于,所述步骤(1)中无水甲醇与蒸馏水的摩尔比为4-5:1;无水甲醇与环氧辣木油的摩尔比为12-13:1;氟硼酸的添加量为0.3-0.4%。
5.根据权利要求1所述的一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,其特征在于,所述步骤(6)中环氧辣木油多元醇和甲苯二异氰酸酯的摩尔比为1:3。
6.根据权利要求1所述的一种环氧辣木油基水性聚氨酯胶黏剂的制备方法,其特征在于,所述1,4-丁二醇的含量为环氧辣木油多元醇的2-2.5wt%、二羟甲基丙酸的含量为环氧辣木油多元醇的1-2wt%。
7.权利要求1-6任一项所述的一种环氧辣木油基水性聚氨酯胶黏剂的制备方法所制备的环氧辣木油基水性聚氨酯胶黏剂。
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