CN114437285A - 一种超低voc乳液聚合高分子及其制备方法 - Google Patents
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Abstract
本发明公开了一种超低VOC乳液聚合高分子,主要由单体、乳化剂及引发剂聚合反应而成,所述单体包括但不限于:丙烯酸丁酯、丙烯酸异辛酯、丙烯酸、甲基丙烯酸、甲基丙烯酸甲酯、苯乙烯、醋酸乙烯酯、丙烯酰胺、丙烯酸羟乙酯、丙烯酸羟丙酯的一种或多种,所述乳化剂包括但不限于:烷基聚氧乙烯醚、烷基磺酸盐、烷基醚硫酸盐、烷基醚琥铂磺酸盐的一种或多种,所述引发剂包括但不限于:过硫酸盐。本发明降低VOC效果明显,根据实际检测结果,采用YC/T207‑2016的标准进行检测,溶剂残留总量结果为0.81mg/㎡,而常规方法做出来结果一般为13.96mg/㎡,实际有效。
Description
技术领域
本发明涉及高分子材料技术领域,尤其是一种超低VOC乳液聚合高分子及其制备方法。
背景技术
现在胶粘剂和涂料中使用的丙烯酸高分子树脂越来越向着水性化、无有机溶剂排放的方向发展,而全水性化的最成熟方案是连成膜助剂都不加的乳液聚合高分子。在一些特殊应用场景,不仅需要纯水性的乳液聚合高分子,还对乳液聚合高分子产品中的残存VOC提出了近乎苛刻的要求。比如一般的做的比较好的聚合高分子乳液,理论投料58%的固含量,实际收到57.4%,未反应率是(58-57.4)/58*100=1%,反应率是约99%。未反应的残单会带入杂质气味并对理化性能产生影响,并对产品的应用领域和品质产生影响。
为此,我们提出一种超低VOC乳液聚合高分子及其制备方法解决上述问题。
发明内容
本发明的目的在于提供一种超低VOC乳液聚合高分子及其制备方法,选用合适的单体,以及配套的乳化剂和引发剂,增加反应性,尽可能减少单体的残留,减少VOC,以解决上述背景技术中提出的问题。
为实现上述目的,本发明提供如下技术方案:
一种超低VOC乳液聚合高分子,主要由单体、乳化剂及引发剂聚合反应而成,
所述单体包括但不限于:丙烯酸丁酯、丙烯酸异辛酯、丙烯酸、甲基丙烯酸、甲基丙烯酸甲酯、苯乙烯、醋酸乙烯酯、丙烯酰胺、丙烯酸羟乙酯、丙烯酸羟丙酯的一种或多种。
所述乳化剂包括但不限于:烷基聚氧乙烯醚、烷基磺酸盐、烷基醚硫酸盐、烷基醚琥铂磺酸盐的一种或多种。
所述引发剂包括但不限于:过硫酸盐。
一种超低VOC乳液聚合高分子的制备方法,包括备料、加热溶解、合成反应、冷却、调整、检测、过滤、包装等过程。生产过程约需8h。
在进一步的实施例中,所述A.备料:将液体原料自动化称量投料,固体原料人工投料。包括三部分:一是将单体物料和乳化剂以及预乳需要的工艺水泵入到预乳化釜,开动搅拌进行预乳化,得到预乳液,二是将引发剂和工艺水加入到引发剂釜,搅拌均匀,得到引发剂溶液,三是将打底乳化剂和工艺水等投入到聚合釜,搅拌混匀。
在进一步的实施例中,所述B. 加热升温:将聚合釜加热升温到80~86℃,搅拌混匀。
在进一步的实施例中,所述C.合成反应:将打底的预乳液从预乳釜中加入到聚合釜中,持续加热,待温度升到78~84℃加入打底引发剂,进行打底反应。打底反应完成后,开始滴加预乳液,进行合成反应,温度控制在80~86℃,时间约需4~6h,随着反应的进行,期间会在反应釜夹套中加入冷却水控制反应温度80~86℃。
在进一步的实施例中,所述D.冷却:聚合反应完成后,经保温过程,再降温冷却后,使釜内温度降到50℃以下,加入后处理剂等进行后处理调整。
与现有技术相比,本发明的有益效果是:
本发明降低VOC效果明显,根据实际检测结果,采用YC/T207-2016的标准进行检测,溶剂残留总量结果为0.81mg/㎡,而常规方法做出来结果一般为13.96mg/㎡,实际有效,生产出超低VOC的乳液聚合高分子来满足无气味、完全无害化的更高要求的乳液聚合高分子,实际重复做到了投料理论固份58%,实际收率固份57.9-57.95%,反应完全率99.83-99.99%,密闭闻人体感官几乎没有气味,产品在客户车间实际使用1.5小时没有闻到任何气味,产品经专用高精仪器检测,溶剂杂质总量控制要求2.5mg/㎡,而实际测出是0.77mg/㎡。
附图说明
图1为乳乳液聚合高分子具体反应方程式示意图;
图2为乳液聚合高分子工艺流程图;
图3为本发明方法做出的产品的检测结果示意图;
图4为常规方法做出的产品的检测结果示意图。
具体实施方式
下面将结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域普通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。
一种超低VOC乳液聚合高分子,主要由单体、乳化剂及引发剂聚合反应而成,
所述单体包括但不限于:丙烯酸丁酯、丙烯酸异辛酯、丙烯酸、甲基丙烯酸、甲基丙烯酸甲酯、苯乙烯、醋酸乙烯酯、丙烯酰胺、丙烯酸羟乙酯、丙烯酸羟丙酯的一种或多种;
所述乳化剂包括但不限于:烷基聚氧乙烯醚、烷基磺酸盐、烷基醚硫酸盐、烷基醚琥铂磺酸盐的一种或多种;
所述引发剂包括但不限于:过硫酸盐。
选用合适的单体,以及配套的乳化剂和引发剂,增加反应性,尽可能减少单体的残留,减少VOC;合适的工艺,包括且不限于聚合工艺、后处理工艺等。
乳液胶粘剂是通过乳液聚合的方法,把合适的单体用适当的乳化剂和引发剂在一定条件下在水中进行聚合反应而制成的胶粘剂。选用合适的单体,包括但不限于丙烯酸丁酯、丙烯酸异辛酯、丙烯酸、甲基丙烯酸、甲基丙烯酸甲酯、苯乙烯、醋酸乙烯酯、丙烯酰胺、丙烯酸羟乙酯、丙烯酸羟丙酯等,适当的乳化剂包括但不限于烷基聚氧乙烯醚、烷基磺酸盐、烷基醚硫酸盐、烷基醚琥铂磺酸盐等,适当的引发剂包括但不限于过硫酸盐。
反应方程式示意如图1所示。
工艺过程是半连续工艺,工艺过程包括备料、加热溶解、合成反应、冷却、调整、检测、过滤、包装等过程。生产过程约需8h。
具体工艺操作步骤如下:
A.备料:将液体原料自动化称量投料,固体原料人工投料。包括三部分:一是将单体物料和乳化剂以及预乳需要的工艺水泵入到预乳化釜,开动搅拌进行预乳化,得到预乳液,二是将引发剂和工艺水加入到引发剂釜,搅拌均匀,得到引发剂溶液,三是将打底乳化剂和工艺水等投入到聚合釜,搅拌混匀;
B.加热升温:将聚合釜加热升温到80~86℃,搅拌混匀;
C.合成反应:将打底的预乳液从预乳釜中加入到聚合釜中,持续加热,待温度升到78~84℃加入打底引发剂,进行打底反应。打底反应完成后,开始滴加预乳液,进行合成反应,温度控制在80~86℃,时间约需4~6h,随着反应的进行,期间会在反应釜夹套中加入冷却水控制反应温度80~86℃;
D.冷却:聚合反应完成后,经保温过程,再降温冷却后,使釜内温度降到50℃以下,加入后处理剂等进行后处理调整;
E.包装出料:调整完后,检验合格,过滤包装出料。
工艺流程如图2所示。
采用本方法,降低VOC效果明显,根据实际检测结果,采用YC/T207-2016的标准进行检测,溶剂残留总量结果为0.81mg/㎡,而常规方法做出来结果一般为13.96mg/㎡。实际有效。
对于本方法做出的产品的检测结果如图3所示。
对于常规方法做出的产品的检测结果如图4所示。
对于本领域技术人员而言,显然本发明不限于上述示范性实施例的细节,而且在不背离本发明的精神或基本特征的情况下,能够以其他的具体形式实现本发明。因此,无论从哪一点来看,均应将实施例看作是示范性的,而且是非限制性的,本发明的范围由所附权利要求而不是上述说明限定,因此旨在将落在权利要求的等同要件的含义和范围内的所有变化囊括在本发明内。不应将权利要求中的任何附图标记视为限制所涉及的权利要求。
此外,应当理解,虽然本说明书按照实施方式加以描述,但并非每个实施方式仅包含一个独立的技术方案,说明书的这种叙述方式仅仅是为清楚起见,本领域技术人员应当将说明书作为一个整体,各实施例中的技术方案也可以经适当组合,形成本领域技术人员可以理解的其他实施方式。
Claims (6)
1.一种超低VOC乳液聚合高分子,其特征在于:主要由单体、乳化剂及引发剂聚合反应而成,所述单体包括但不限于:丙烯酸丁酯、丙烯酸异辛酯、丙烯酸、甲基丙烯酸、甲基丙烯酸甲酯、苯乙烯、醋酸乙烯酯、丙烯酰胺、丙烯酸羟乙酯、丙烯酸羟丙酯的一种或多种;所述乳化剂包括但不限于:烷基聚氧乙烯醚、烷基磺酸盐、烷基醚硫酸盐、烷基醚琥铂磺酸盐的一种或多种;所述引发剂包括但不限于:过硫酸盐。
2.根据权利要求1所述的一种超低VOC乳液聚合高分子的制备方法,其特征在于:包括备料、加热溶解、合成反应、冷却、调整、检测、过滤、包装等过程;生产过程约需8h。
3.根据权利要求2所述的一种超低VOC乳液聚合高分子及其制备方法,其特征在于:所述,
A.备料:将液体原料自动化称量投料,固体原料人工投料;包括三部分:一是将单体物料和乳化剂以及预乳需要的工艺水泵入到预乳化釜,开动搅拌进行预乳化,得到预乳液,二是将引发剂和工艺水加入到引发剂釜,搅拌均匀,得到引发剂溶液,三是将打底乳化剂和工艺水等投入到聚合釜,搅拌混匀。
4.根据权利要求2所述的一种超低VOC乳液聚合高分子及其制备方法的制备工艺,其特征在于:所述,
B.加热溶解:将聚合釜加热升温到80~86℃,搅拌混匀。
5.根据权利要求2所述的一种超低VOC乳液聚合高分子及其制备方法,其特征在于:所述,
C.合成反应:将打底的预乳液从预乳釜中加入到聚合釜中,持续加热,待温度升到78~84℃加入打底引发剂,进行打底反应;打底反应完成后,开始滴加预乳液,进行合成反应,温度控制在80~86℃,时间约需4~6h,随着反应的进行,期间会在反应釜夹套中加入冷却水控制反应温度80~86℃。
6.根据权利要求2所述的一种超低VOC乳液聚合高分子及其制备方法,其特征在于:所述,
D.冷却:聚合反应完成后,经保温过程,再降温冷却后,使釜内温度降到50℃以下,加入后处理剂等进行后处理调整。
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