CN107267107A - 一种环保型水性聚氨酯胶黏剂的制备方法 - Google Patents

一种环保型水性聚氨酯胶黏剂的制备方法 Download PDF

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CN107267107A
CN107267107A CN201710394663.XA CN201710394663A CN107267107A CN 107267107 A CN107267107 A CN 107267107A CN 201710394663 A CN201710394663 A CN 201710394663A CN 107267107 A CN107267107 A CN 107267107A
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吴俊华
牛笑
牛笑一
孙玮鸿
齐华春
庞久寅
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Beihua University
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Abstract

本发明是一种环保型水性聚氨酯胶黏剂的制备方法,其特点是,包括:预聚体、乳化水溶液和水性聚氨酯胶黏剂成品的制备过程。其优点是,制备得到的胶黏剂的耐水性好,粘接强度高,大大地降低了其中未反应基团的含量,提高了使用时间;由于使用以水为分散剂实现了无VOC释放,对环境无污染,便于工业化生产;由于制备得到的胶黏剂是低黏度液体,使用方便,贮存期长、耐药品和耐大气老化性能高;制备得到的胶黏剂适用范围广,在木材加工、包装、纺织、造纸、建筑、机械等多领域,可作胶黏剂、密封胶和涂料的原材料。

Description

一种环保型水性聚氨酯胶黏剂的制备方法
技术领域
本发明涉及一种水性聚氨酯胶黏剂的制备方法,是一种环保型水性聚氨酯胶黏剂的制备方法。
背景技术
水性聚氨酯首次实现工业化生产是在1967年,其特点是原料丰富、无甲醛释放、无颜色污染,特别是胶合强度高,适合制造各类人造板材;缺点是干燥速度慢,初始粘性低,并且耐水性不佳,耐水性不佳的原因是由于水性聚氨酯本身含有亲水基团,所以要提高耐水性就要在保证乳液稳定的情况下,减少亲水基团的含量。
传统方法制备水性聚氨酯胶黏剂,没有考虑反应所残留的亲水基团,采用传统方法制备的水性聚氨酯胶黏剂,耐水性能欠佳,且贮存期短。在使用过程中因为其耐水性差限制了水性聚氨酯胶黏剂的发展。
发明内容
本发明的目的是克服现有技术的不足,提供一种粘接强度高,耐水性能好,无游离甲醛释放的环保型水性聚氨酯胶黏剂的制备方法。
实现本发明采用的技术方案是:一种环保型水性聚氨酯胶黏剂的制备方法,其特征是,它包括以下步骤,原料用量以质量份计,
1)将100份的聚醚多元醇加入到三口瓶中,在200~400r/min的速度下搅拌均匀,滴入20~25份的异氰酸酯,搅匀,升温至75℃,恒温反应1-2h;
2)取2~3份的扩链剂和0.1~0.6份的催化剂加入到步骤1)所述的三口瓶中充分搅拌,恒温反应3h,降温,将其倒入烧杯中,降至常温,加入1~2份的中和剂,搅拌10min,制成预聚体;
3)制备乳化水溶液:取乳化剂原液10份,加入100份水中加热溶解,待其水溶液呈透明且温度为常温,即制成乳化水溶液;
4)将乳化剂水溶液缓慢加入到步骤2)的预聚体溶液中,并在1500~2000r/min的速度下高速搅拌,搅拌时间10min,得到固含量在40%—50%的水性聚氨酯胶黏剂成品。
所述的聚醚多元醇为聚醚多元醇N220、聚丙二醇(PPG)和聚乙二醇(PEG)中的一种。
所述的异氰酸酯为甲苯二异氰酸酯(TDI)或二苯基甲烷二异氰酸酯(MDI)。
所述的扩链剂为二羟甲基丙酸(DMPA)、1,4-丁二醇(BDO)和三羟甲基丙烷中的一种;
所述的催化剂为二乙烯三胺、三乙烯二胺和二月桂酸二丁基锡中的一种。
所述的中和剂为三乙胺。
所述的乳化剂原液为丁二酸改性聚氧乙烯烷基酚醚(OS)或聚氧乙烯壬基酚醚(OP)中的一种。
本发明的一种环保型水性聚氨酯胶黏剂的制备方法与传统水性聚氨酯胶黏剂制备方法相比,具有以下优点:
①耐水性好;原因是对异氰酸酯基团的端部,进行封闭,不暴露其中的亲水基团,故其胶黏剂的耐水性较好;
②对多种材料有良好的粘接强度,异氰酸酯胶黏剂含有大量的极性基团和活性反应基团,能满足不同基材粘接和使用条件要求;
③大大地降低了其中未反应基团的含量,提高了使用时间;
④由于使用以水为分散剂,实现了无VOC释放,对环境的无污染,便于工业化生产;
⑤由于制备得到的产品是低黏度液体,使用方便,贮存期长、耐药品和耐大气老化性能高;
⑥适用范围广,在木材加工、包装、纺织、造纸、建筑、机械等多领域,可作胶黏剂、密封胶和涂料的原材料。
具体实施方式
下面利用实施例对本发明的一种环保型水性聚氨酯胶黏剂的制备方法作详细说明。
实施例1:实施例1的环保型水性聚氨酯胶黏剂的制备方法,包括以下步骤:
1、称取原料
2、预聚体的制备:
在三口烧瓶中加入100g聚醚多元醇N220,并在400r/min的速度下搅拌均匀,再采用25g甲苯二异氰酸酯(TDI)滴加方式滴加,在75℃下恒温反应1h,加入2g二羟甲基丙酸作为扩链剂,加入0.1g二乙烯三胺作为催化剂,恒温反应3h降温,将其倒入烧杯中,待降至常温后加入1g三乙胺作为中合剂,搅拌10min,即获得预聚体。
3、制备乳化水溶液:
取乳化剂丁二酸改性聚氧乙烯烷基酚醚(OS)10g,加入100g水中加热溶解,待其水溶液呈透明且温度为常温,即制成乳化水溶液;
4、制备水性聚氨酯胶黏剂
将乳化剂水溶液缓慢加入到盛有预聚体杯子中,并在1500r/min的速度下高速搅拌,搅拌时间10min,待溶液由透明变成乳白色、溶液均一稳定时,得到固含量在40%—50%的水性聚氨酯胶黏剂成品。
实施例2:实施例2的环保型水性聚氨酯胶黏剂的制备方法,包括以下步骤:
1、称取原料
2、预聚体的制备:
在三口烧瓶中加入100g聚丙二醇,滴加加入23g的二苯基甲烷二异氰酸酯,并在温度为75℃、200r/min的速度下搅拌均匀,恒温搅拌2h,加入扩链剂1,4-丁二醇2.5g和催化剂三乙烯二胺0.2g并搅拌均匀,搅拌时间为3h,然后降温倒入烧杯中备用,待温度降至常温,用胶头滴管滴加1g的中和剂三乙胺,边滴加边搅拌,搅拌10min,待有大量气泡后,即获得预聚体备用。
3、乳化水溶液的制备
取10g聚氧乙烯壬基酚醚加入100g的水中加热溶解,待聚氧乙烯壬基酚醚完全溶解于水中并降到室温后,制得乳化水溶液。
4、制备水性聚氨酯胶黏剂
将乳化水溶液缓慢加入盛有预聚体的杯子中,并高速搅拌,转速在1800r/min,待溶液由透明变成乳白色、溶液均一稳定时,出料即获得固含40%—50%的水性聚氨酯胶黏剂。
实施例3:实施例3的环保型水性聚氨酯胶黏剂的制备方法,包括以下步骤:
1、称取原料
2、预聚体的制备:
在三口烧瓶中加入100g的聚乙二醇,并用滴液漏斗滴加甲苯二异氰酸酯20g,滴加完后开始计时,温度为75℃,在转速为300r/min下搅拌均匀,恒温反应2h,之后加入3g的扩链剂三羟甲基丙烷和0.6g的催化剂二月桂酸二丁基锡,搅拌均匀,恒温反应3h。然后降温,将其转到烧杯中,加入中和剂三乙胺2g,搅拌10min后有大量气泡现象产生,即可停止搅拌,制得预聚体。
3、制备水性聚氨酯胶黏剂
取10g乳化剂丁二酸改性聚氧乙烯烷基酚醚加入100g的水加热充分搅拌,当乳化剂溶解后,降温将搅拌均匀的溶液慢慢地加入到预聚体中,2000r/min高速搅拌,当溶液变为乳白色且溶液稳定后出料,获得固含40%—50%的环保型水性聚氨酯胶黏剂。
胶合强度的测定
1、胶合板制作:
找出表板紧面,将紧面朝外,按对称原则配坯;制胶;确定涂胶量,将制备的水性聚氨酯胶黏剂放入烧杯中,加入一定量面粉调整粘度,用毛刷搅拌均匀;涂胶时,毛刷方向一致,均匀地涂在芯板的两个面上;确定热压工艺条件,进行操作;卸压取板;按标准将胶合板裁成100mm×25mm的标准试件,给胶合板编号并进行性能检测。
2、实验材料:
①试件的制作:按国家GB/T9846-2004标准制作胶合板试件1、2、3、4。
②按国家GB/T9846-2004标准规定进行胶合强度测试,将试件进行浸泡处理。国家Ⅱ类胶合板处理条件:将试件浸泡在63±3℃热水中3h,取出后在室温下冷却10min,再进行胶合强度测试。
③调整好木材万能实验机,进行胶合强度检测。
3、要求:
①试件的装置应其纵轴与试验机的活动夹头的轴线一致,并保持上下夹持位置的正常。
②夹持部位与试件锯口的距离在5mm范围内。
③对试件的加荷速度均匀,最大破坏荷重的读数应精确到5N。
4、结果与讨论
试件的胶合强度计算与分析:
其中:P-最大破坏荷重,N;
A-试件剪断的实际宽度,mm;
B-试件剪断面的实际长度,mm;
S-试件的胶合强度,N/mm2
检测结果见下表。
表1胶合强度的检测结果
压制胶合板的热压工艺参数为:单位压力为0.8MPa,热压温度为90℃,热压时间是6min(1.5min/mm)。从上表可看出:以本发明的环保型水性聚氨酯胶黏剂压制的胶合板,其胶合强度均大于0.7MPa,达到了国家标准GB/T9846—2004Ⅱ类胶合板要求。
以上实施方式仅用以说明本发明的技术方案,而非对其限制,所属领域的普通技术人员应该理解,参照上述实施例所作的任何形式的修改、等同变化均在本发明权利要求保护范围之内。

Claims (7)

1.一种环保型水性聚氨酯胶黏剂的制备方法,其特征是,它包括以下步骤,原料用量以质量份计,
1)将100份的聚醚多元醇加入到三口瓶中,在200~400r/min的速度下搅拌均匀,滴入20~25份的异氰酸酯,搅匀,升温至75℃,恒温反应1-2h;
2)取2~3份的扩链剂和0.1~0.6份的催化剂加入到步骤1)所述的三口瓶中充分搅拌,恒温反应3h,降温,将其倒入烧杯中,降至常温,加入1~2份的中和剂,搅拌10min,制成预聚体;
3)制备乳化水溶液:取乳化剂原液10份,加入100份水中加热溶解,待其水溶液呈透明且温度为常温,即制成乳化水溶液;
4)将乳化剂水溶液缓慢加入到步骤2)的预聚体溶液中,并在1500~2000r/min的速度下高速搅拌,搅拌时间为10min,得到固含量在40%—50%的水性聚氨酯胶黏剂成品。
2.根据权利要求1所述的一种环保型水性聚氨酯胶黏剂的制备方法,其特征是,所述的聚醚多元醇为聚醚多元醇N220、聚丙二醇(PPG)和聚乙二醇(PEG)中的一种。
3.根据权利要求1所述的一种环保型水性聚氨酯胶黏剂的制备方法,其特征是,所述的异氰酸酯为甲苯二异氰酸酯(TDI)或二苯基甲烷二异氰酸酯(MDI)。
4.根据权利要求1所述的一种环保型水性聚氨酯胶黏剂的制备方法,其特征是,所述的扩链剂为二羟甲基丙酸(DMPA)、1,4-丁二醇(BDO)和三羟甲基丙烷中的一种。
5.根据权利要求1所述的一种环保型水性聚氨酯胶黏剂的制备方法,其特征是,所述的催化剂为二乙烯三胺、三乙烯二胺和二月桂酸二丁基锡中的一种。
6.根据权利要求1所述的一种环保型水性聚氨酯胶黏剂的制备方法,其特征是,所述的中和剂为三乙胺。
7.根据权利要求1所述的一种环保型水性聚氨酯胶黏剂的制备方法,其特征是,所述的乳化剂原液为丁二酸改性聚氧乙烯烷基酚醚(OS)或聚氧乙烯壬基酚醚(OP)中的一种。
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Application publication date: 20171020