CN115537153A - 单组分聚醋酸乙烯酯乳液木材胶粘剂及其制备方法 - Google Patents
单组分聚醋酸乙烯酯乳液木材胶粘剂及其制备方法 Download PDFInfo
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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Abstract
本发明涉及一种聚醋酸乙烯酯乳液木材胶粘剂及其制备方法。本发明方法包括:在烧瓶中加入水,然后缓慢投入4‑5份聚乙烯醇,升温到90‑95℃保温1‑1.5h,接着降温到65‑70℃,加入0.03‑0.05份PH调节剂、0.05‑0.07份消泡剂、0.05‑0.1份乳化剂,升温到75‑85℃并搅拌均匀,滴加40‑43份的混合单体,并同时缓慢滴加包含0.1‑0.12份引发剂的引发剂水溶液,升温到85‑90℃并保温1‑1.5h,接着降温到40‑45℃,然后加入2‑3份增塑剂、3‑5份金属盐、水4.5‑9份和0.1‑0.2份防腐剂,搅拌均匀即得。发明胶粘剂满足防水等级满足欧洲EN204‑D3标准的特点。
Description
技术领域
本发明涉及水基胶粘剂制备技术,特别涉及一种单组分聚醋酸乙烯酯乳液木材胶粘剂及其制备方法,一种具有单组份、环保、防水等级满足欧洲EN204-D3标准的聚醋酸乙烯酯(PVAc)乳液木工胶粘剂制备方法。
背景技术
聚醋酸乙烯酯白乳胶因其健康环保、施工方便、价格低廉、力学强度较高等特点被广泛应用于木材加工行业,特别在木材胶合、板材组装拼接等领域展现出突出的应用效果。聚醋酸乙烯酯白乳胶通常是以聚乙烯醇为保护胶体,以水为分散介质,在引发剂、乳化剂、PH调节剂、消泡剂、增塑剂等常规助剂的辅助作用下,以醋酸乙烯酯为主单体,通过乳液聚合技术制备得到。普通的PVAc白乳胶耐水性很差,因此限制了其在高端防水木工胶领域的应用。欧洲EN204标准定义的D3级木工胶是一类具有比普通木工胶具有更好耐水性、更高湿粘接强度的水基胶粘剂,综合性能更佳,具有更好的应用价值,故常被用于对环境湿度、湿粘接强度要求更高的高档家具、地板、以及船舶制造等产品领域。开展高性能D3级木工胶的制备研究对于完善水基木材胶粘剂产品品类,满足人们对美好产品的需要具有积极意义。
目前,国内外对于D3级木工胶的制备方法取得了一定的研究进展。主要有基于多异氰酸酯的双组份固化技术;对保护胶体聚乙烯醇进行改性(如缩醛化,乙酰乙酰化等)或对淀粉进行氧化改性来提高耐水性;采用种子乳液聚合技术进行核壳结构设计,制备具有特殊嵌段组成的高分子聚合物,从而提高所成胶膜的耐水性;采用氧化还原低温引发体系,并引入内交联单体如N-羟甲基丙烯酰胺或外交联单体双丙酮丙烯酰胺等,通过胶膜干燥后的交联固化反应来提高其粘接强度和耐水性;或者将耐水性好的树脂胶如酚醛树脂类胶粘剂与普通白胶复配改性提高耐水性等。其中,缩醛化改性、引入交联单体N-羟甲基丙烯酰胺以及与“三醛胶”复配等方法有向产品中引入甲醛的缺陷,环保性较差。
在常规乳液聚合中,大量使用乳化剂可以寻求聚合过程以及后聚合样品较好的稳定性,但也会使得胶膜的耐水性下降。无皂乳液聚合是一种新型的乳液聚合方法,由于乳化剂添加量极少,胶膜的耐水性相比于常规乳液聚合要好;且制备得到的聚合物乳胶粒粒径比较均匀,最终所成膜的综合性能也较好,是常被用来提高乳液涂膜性能的有效方法。另外,离子配位交联策略也常被用来提高水基胶粘剂的耐水性。
发明内容
本发明提供一种聚醋酸乙烯酯乳液木材胶粘剂及其制备方法。本发明通过无皂乳液聚合技术并结合配位交联策略制备的聚醋酸乙烯酯乳液木材胶粘剂兼具单组份、环保、防水等级满足欧洲EN204-D3标准的特点。
本发明通过以下技术方案实现:
本发明的单组份聚醋酸乙烯酯乳液木工胶的制备方法,由以下质量份数比的组分按照以下步骤制备而成:
在烧瓶中加入40-45份水,在搅拌速率为130-170rmp下缓慢投入4-5份聚乙烯醇,然后升温到90-95℃保温1-1.5h,接着降温到65-70℃,然后加入0.03-0.05份PH调节剂、0.05-0.07份消泡剂、0.05-0.1份乳化剂,接着逐渐升温到75-85℃并继续搅拌混合均匀,然后滴加40-43份的混合单体,并同时缓慢滴加包含0.1-0.12份引发剂的引发剂水溶液,滴加完成用时为4-5小时,然后升温到85-90℃并保温1-1.5h,接着降温到40-45℃,然后加入2-3份增塑剂、3-5份金属盐、水4.5-9份和0.1-0.2份防腐剂,搅拌均匀即得所述的单组份聚醋酸乙烯酯乳液木工胶。
进一步地,所述的聚乙烯醇为改性聚乙烯醇。
进一步地,所述的PH调节剂为醋酸钠、碳酸氢钠等PH调节剂。
进一步地,所述的消泡剂为矿物油类消泡剂。
进一步地,所述的乳化剂为非离子烷基聚氧乙烯醚类乳化剂。
进一步地,所述引发剂为过硫酸铵引发剂。
进一步地,所述的引发剂水溶液中引发剂的质量分数比为3.5-4.7%。
进一步地,所述的混合单体为由醋酸乙烯酯、丙烯酸酯类单体和叔碳酸乙烯酯按照质量比为34-36份:1-5份:0-5份混合而成的混合单体。
进一步地,所述增塑剂为二丙二醇二苯甲酸酯增塑剂。
进一步地,所述防腐剂为异噻唑啉酮类防腐剂。
进一步地,所述的金属盐中的金属离子为能与氧原子产生类似配位效果的多价金属离子,所述的金属盐具体可以为硝酸铝、氯化铝、硫酸铝、氯化锌或者硝酸锌,如果不考虑最后得到胶黏剂的颜色,也可以为铁盐或者铬盐。
进一步地,所述的烧瓶为四口烧瓶。
原理说明:
本发明的关键之处在于利用了无皂乳液聚合技术以及金属离子配位交联策略使制备得到的聚醋酸乙烯酯乳胶满足欧洲EN204中D3防水等级要求。
首先,本发明在制备聚醋酸乙烯酯乳胶过程中添加极少量小分子乳化剂,依靠高分子量聚乙烯醇的乳化和保护作用可以成功制备得到稳定乳胶。
此外,在聚合反应末期加入高价金属离子化合物,利用高价金属离子价电层提供的空轨道(Al3+可以提供3d空轨道)与聚乙烯醇、醋酸乙烯-丙烯酸及酯类共聚高分子的分子链上氧原子提供的孤对电子形成多重配位键作用(如附图1所示意),可以使失水固化后的胶膜耐水性、力学强度大大提高。当共聚过程中引入丙烯酸单体时,乳胶失水固化成膜后,聚合物分子链上的羧基基团会与Al3+结合形成离子键,使胶膜的亲水性下降,耐水性提升;同时,多重离子键的形成也增大了体系的交联密度,胶膜的内聚强度也被提高。
本发明的有益之处:本发明制备的聚醋酸乙烯酯乳液木材胶粘剂兼具单组份、环保、防水等级满足欧洲EN204-D3标准的特点。该乳胶整个制备过程无醛添加,环保性好;湿粘接强度高;生产工艺操作简单。
附图说明
图1是本发明离子配位交联的示意图。
具体实施方式
下面结合实施例进行具体说明。
实施例1
500ml四口烧瓶中加入40g水,在搅拌速率为130rmp下缓慢投入4g聚乙烯醇,升温到90℃保温1h后降温到65℃,依次加入0.04gPH调节剂、0.05g消泡剂、0.1g乳化剂,搅拌混合均匀,并逐渐升温到75℃,开始滴加40g的混合单体,并同步开始缓慢滴加0.1g引发剂(引发剂被溶解成3.5%的水溶液),控制同步滴加完成用时4.5小时,升温到85℃继续保温1h后降温到40℃左右,加入2.2g增塑剂、4.5g金属盐(硝酸铝)、9g水、0.1g防腐剂后搅拌均匀出料,得到粘稠均匀白色乳胶,即得所述的胶粘剂。所述的40g混合单体中包含醋酸乙烯酯35g、丙烯酸1g,丙烯酸丁酯2g,叔碳酸乙烯酯2g。
实施例2
500ml四口烧瓶中加入43g水,在搅拌速率为140rmp下缓慢投入5g聚乙烯醇,升温到91℃保温1h后降温到66℃。依次加入0.03gPH调节剂、0.07g消泡剂、0.08g乳化剂,搅拌混合均匀,并逐渐升温到85℃,开始滴加40g的混合单体,并同步开始缓慢滴加0.11g引发剂(引发剂被溶解成4.7%的水溶液),控制同步滴加完成用时4.8小时,升温到86℃继续保温1.2h后降温到42℃左右,加入2g增塑剂、3g金属盐(氯化铝)、6.72g水、0.1g防腐剂后出料,得到粘稠均匀白色乳胶,即得所述的胶粘剂。所述40g混合单体中包含醋酸乙烯酯36g、丙烯酸-2乙基己酯2g,丙烯酸1g,丙烯酸羟乙酯1g。
实施例3
500ml四口烧瓶中加入45g水,在搅拌速率为150rmp下缓慢投入5g聚乙烯醇,升温到92℃保温1h后降温到67℃,依次加入0.05gPH调节剂、0.06g消泡剂、0.05g乳化剂,搅拌混合均匀,并逐渐升温到80℃,开始滴加40g的混合单体,并同步开始缓慢滴加0.12g引发剂(引发剂被溶解成3.6%的水溶液),控制同步滴加完成用时5小时,升温到90℃继续保温1.5h后降温到45℃左右,加入2g增塑剂、3.2g金属盐(硫酸铝)、4.5g水、0.1g防腐剂后出料,得到粘稠均匀白色乳胶,即得所述的胶粘剂。所述40g混合单体中包含醋酸乙烯酯36g、丙烯酸1g,丙烯酸-2乙基己酯3g。
本实施例的混合单体也可以是40-43g,由醋酸乙烯酯与其它丙烯酸酯类单体按照质量比为36:4混合而成的的混合物。
实施例4
500ml四口烧瓶中加入41g水,在搅拌速率为160rmp下缓慢投入5g聚乙烯醇,升温到93℃保温1.2h后降温到68℃,依次加入0.04gPH调节剂、0.06g消泡剂、0.1g乳化剂,搅拌混合均匀,并逐渐升温到75℃,开始滴加40g的混合单体,并同步开始缓慢滴加0.12g引发剂(引发剂被溶解成3.6%的水溶液),控制同步滴加完成用时4.7小时,升温到85℃继续保温1h后降温到40℃左右,加入2g增塑剂、5g金属盐(氯化锌)、6.7g水、0.15g防腐剂后出料,得到粘稠均匀白色乳胶,即得所述的胶粘剂。所述40g混合单体中包含醋酸乙烯酯34g、丙烯酸羟乙酯1g,叔碳酸乙烯酯5g。
本实施例的混合单体也可以是40-43g,由醋酸乙烯酯、其它丙烯酸酯类单体和叔碳酸乙烯酯按照质量比为34:1:5混合而成的的混合物。
实施例5
500ml四口烧瓶中加入40g水,在搅拌速率为170rmp下缓慢投入4.5g聚乙烯醇,升温到95℃保温1.5h后降温到70℃,依次加入0.04gPH调节剂、0.06g消泡剂、0.08g乳化剂,搅拌混合均匀,并逐渐升温到75℃,开始滴加40g的混合单体,并同步开始缓慢滴加0.12g引发剂(引发剂被溶解成3.6%的水溶液),控制同步滴加完成用时4小时。升温到85℃继续保温1h后降温到40℃左右,加入3g增塑剂、3.94g金属盐(硝酸锌)、8.78g水、0.2g防腐剂后出料,得到粘稠均匀白色乳胶,即得所述的胶粘剂,所述40g混合单体中包含醋酸乙烯酯35g、丙烯酸乙酯3g,丙烯酸羟乙酯1g,丙烯酸1g。
本实施例的混合单体也可以是40-43g,由醋酸乙烯酯与其它丙烯酸酯类单体按照质量比为35:5混合而成的的混合物。
以上实施例中所述的聚乙烯醇为可乐丽的改性聚乙烯醇RS-2117,也可以采用国产聚乙烯醇1799、2099或者2499。
所述的PH调节剂为醋酸钠或碳酸氢钠。
所述的消泡剂为矿物油类消泡剂。
所述的乳化剂为非离子烷基聚氧乙烯醚类乳化剂。
所述引发剂为过硫酸铵引发剂。
所述增塑剂为二丙二醇二苯甲酸酯增塑剂。
所述防腐剂为异噻唑啉酮类防腐剂。
以上实施例1-5的实验结果如表1所示,表1测试结果为实施例1-5制备的聚醋酸乙烯酯乳胶按照EN204 D3的制样要求,将胶合后的木块(尺寸为25mm×25mm)放在室温标准条件下养护7天,然后放入冷水中浸泡4天后拿出,立即进行压缩剪切强度测试的数据结果,为了保证制样及评价时的可靠性,每一个实施例平行制备了10个样品进行测试,取10个样品的平均结果作为最终的实验数据。
表1实施例1-5的外观、固含、pH及湿强度等试验结果
本发明不仅限于上述实施例,凡是依据本发明原理的简单替换和改进均在本发明保护范围之内。
Claims (9)
1.一种单组份聚醋酸乙烯酯乳液木工胶的制备方法,其特征在于:由以下质量份数比的组分按照以下步骤制备而成:
在烧瓶中加入40-45份水,在搅拌速率为130-170rmp下缓慢投入4-5份聚乙烯醇,然后升温到90-95℃保温1-1.5h,接着降温到65-70℃,然后加入0.03-0.05份PH调节剂、0.05-0.07份消泡剂及0.05-0.1份乳化剂,接着逐渐升温到75-85℃并继续搅拌混合均匀,然后滴加40-43份的混合单体,并同时缓慢滴加由0.1-0.12份引发剂制成的引发剂水溶液,滴加完成用时为4-5小时,然后升温到85-90℃并保温1-1.5h,接着降温到40-45℃,然后加入2-3份增塑剂、3-5份金属盐、4.5-9份水和0.1-0.2份防腐剂,搅拌均匀即得所述的单组份聚醋酸乙烯酯乳液木工胶;
所述的混合单体为由醋酸乙烯酯、丙烯酸酯类单体和叔碳酸乙烯酯按照质量比为34-36份:1-5份:0-5份混合而成的混合单体。
2.根据权利要求1所述的单组份聚醋酸乙烯酯乳液木工胶的制备方法,其特征在于:所述的聚乙烯醇为改性聚乙烯醇。
3.根据权利要求1所述的单组份聚醋酸乙烯酯乳液木工胶的制备方法,其特征在于:所述的PH调节剂为醋酸钠或碳酸氢钠。
4.根据权利要求1所述的单组份聚醋酸乙烯酯乳液木工胶的制备方法,其特征在于:所述的消泡剂为矿物油类消泡剂。
5.根据权利要求1所述的单组份聚醋酸乙烯酯乳液木工胶的制备方法,其特征在于:所述的乳化剂为非离子烷基聚氧乙烯醚类乳化剂。
6.根据权利要求1所述的单组份聚醋酸乙烯酯乳液木工胶的制备方法,其特征在于:所述引发剂为过硫酸铵引发剂。
7.根据权利要求1所述的单组份聚醋酸乙烯酯乳液木工胶的制备方法,其特征在于:所述的引发剂水溶液中引发剂的质量分数比为3.5-4.7%。
8.根据权利要求1所述的单组份聚醋酸乙烯酯乳液木工胶的制备方法,其特征在于:所述的混合单体为由醋酸乙烯酯、丙烯酸酯类单体和叔碳酸乙烯酯按照质量比为34-36份:1-5份:0-5份混合而成的混合单体。
9.一种单组份聚醋酸乙烯酯乳液木工胶,其特征在于:由权利要求1-8中任一项所述的方法制备而成。
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