CN114478898A - 一种锂电池负极代sbr用乳液聚合粘合剂及其制备方法 - Google Patents
一种锂电池负极代sbr用乳液聚合粘合剂及其制备方法 Download PDFInfo
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Abstract
本发明公开了一种锂电池负极代SBR用乳液聚合粘合剂，所述乳液聚合是不饱和单体和水在乳化剂的作用下配制成的乳状液中进行的聚合，体系主要由不饱和单体、水、乳化剂（复合几种乳化剂）及水溶性引发剂四大类成分组成，所述单体包括但不限于：丙烯酸、甲基丙烯酸、甲基丙烯酸甲酯、苯乙烯、醋酸乙烯酯、丙烯酸丁酯、丙烯酸异辛酯、丙烯酰胺、N‑甲基丙烯酰胺的一种或多种。本发明用一种简单、又环保的方法，得到一种比SBR丁苯橡胶乳液更优秀的更适合锂电池使用，可以提高现有锂电池性能的高分子粘合剂来代替现今广泛使用进口的SRB粘合剂，选用单体是聚合后非常稳定可靠的，耐老化耐高低温都很好，交联和吸电解液适度，保持负极层收纳释放锂离子的框架稳定。
Description
技术领域
本发明涉及高分子材料技术领域，尤其是一种锂电池负极代SBR用乳液聚合粘合剂及其制备方法。
背景技术
现今绝大部分锂电池制造企业使用的负极粘结剂仍然是SBR，中文解释大至是改性羧基丁苯橡胶乳液。为什么改性我们分析是：一是普通的SBR本身不耐电解液溶剂，二是SBR乳液主要由丁二烯-苯乙烯-丙烯酸经低温乳液聚合而成，高分子主链上还剩余一个丁二烯自由聚合后-C=C-不饱和双键，具有不耐老化和耐氧化性。综上二个原因，所以要进行硫化交联去双键和提高耐电解液性。经交联改性大致就是可用的锂电池负极粘结剂SBR乳液了。但是这种改性是差不多完全交联了其中的剩余-C=C-不饱和双键的情况下达到的。交联少了-C=C-没有完全去除，耐老化性，耐久性不够，交联完全了，又交联度度太高，太硬粘结性不太好了。另外由于常温下丁二烯是气体，苯乙烯和丙烯酸是液体，为了使它能很好共聚现行大多数采用低温乳液聚合方法生产丁苯乳液。低温乳液聚合方法，要采用特殊歧化松香乳化剂，过氧化物、硫酸亚铁、吊白块氧化-还原引发体系引发聚合，后期还有脱未反应丁二烯和苯乙烯分离，过程复杂，加入物料品种太多，所以SBR的膜通常通常不透明、颜色深，杂质含量高一些，导电性和低温性差（交联太密集），低温反应可加入改善共聚单体不多，性能改善难度大，具有以下缺点：a.为了消除不饱和双键，提高耐老化性能，交联度很大，损失了柔韧性，使的耐低温性比较差，从而影响锂电池低温性。b.SBR生产工艺复杂，连续法生产改性不容易。c.所使用的乳化剂是惰性乳化剂，没有参与高分子链上去，将来容易浮霜出高分子，影响性能。d.SBR低温合成时添加剂太多对电池的性能可能有影响。
为此，我们提出一种锂电池负极代SBR用乳液聚合粘合剂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锂电池负极代SBR用乳液聚合粘合剂及其制备方法，首先选用单体是聚合后非常稳定可靠的，耐老化耐高低温都很好，交联和吸电解液适度，保持负极层收纳释放锂离子的框架稳定，另外选择了价键连入高分子的乳化剂，使得所有的高分子粘合剂是一个完整体，没有多余的杂质，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：
一种锂电池负极代SBR用乳液聚合粘合剂，所述乳液聚合是不饱和单体和水在乳化剂的作用下配制成的乳状液中进行的聚合，体系主要由不饱和单体、水、乳化剂（复合几种乳化剂）及水溶性引发剂四大类成分组成；
所述单体包括但不限于：丙烯酸、甲基丙烯酸、甲基丙烯酸甲酯、苯乙烯、醋酸乙烯酯、丙烯酸丁酯、丙烯酸异辛酯、丙烯酰胺、N-甲基丙烯酰胺的一种或多种。
一种锂电池负极代SBR用乳液聚合粘合剂的制备方法，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：一是将单体醋酸乙烯酯、丙烯酸丁酯、丙烯酸异辛酯和其它单体物料泵入到预乳化釜，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，三是将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℃、保温10～30分钟，搅拌混匀。
在进一步的实施例中，所述C．合成反应：将少量的预乳液从预乳釜中滴加到聚合釜中，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调整。
在进一步的实施例中，所述E．包装出料：调整完后，检验合格，过滤包装出料。
与现有技术相比，本发明的有益效果是：
本发明用一种简单、又环保的方法，得到一种比SBR丁苯橡胶乳液更优秀的更适合锂电池使用，可以提高现有锂电池性能的高分子粘合剂来代替现今广泛使用进口的SRB粘合剂，选用单体是聚合后非常稳定可靠的，耐老化耐高低温都很好，交联和吸电解液适度，保持负极层收纳释放锂离子的框架稳定，另外选择价键连入高分子的乳化剂，使得所有的高分子粘合剂是一个完整体，没有多余的杂质，则本发明的锂电池负极用乳液聚合高分子粘合剂比SBR更优秀。
附图说明
图1为锂电池负极代SBR用乳液聚合粘合剂具体反应方程式示意图；
图2为锂电池负极代SBR用乳液聚合粘合剂工艺流程图。
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。
一种锂电池负极代SBR用乳液聚合粘合剂，所述乳液聚合是不饱和单体和水在乳化剂的作用下配制成的乳状液中进行的聚合，体系主要由不饱和单体、水、乳化剂（复合几种乳化剂）及水溶性引发剂四大类成分组成，
所述单体包括但不限于：丙烯酸、甲基丙烯酸、甲基丙烯酸甲酯、苯乙烯、醋酸乙烯酯、丙烯酸丁酯、丙烯酸异辛酯、丙烯酰胺、N-甲基丙烯酰胺的一种或多种。
具体反应方程式示意如图1（四种不饱和单体只是示意其实包含上述多种）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。生产过程需8-10h。
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：一是将单体醋酸乙烯酯、丙烯酸丁酯、丙烯酸异辛酯和其它单体物料泵入到预乳化釜，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，三是将乳化剂和工艺水等投入到聚合釜，搅拌混匀；
B．加热溶解：将聚合釜加热升温到80～86℃、保温10～30分钟，搅拌混匀；
C．合成反应：将少量的预乳液从预乳釜中滴加到聚合釜中，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调整；
E．包装出料：调整完后，检验合格，过滤包装出料。
其工艺流程如图2所示（该图为乳液聚合50L中试设备）。
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)
1.一种锂电池负极代SBR用乳液聚合粘合剂，其特征在于：所述乳液聚合是不饱和单体和水在乳化剂的作用下配制成的乳状液中进行的聚合，体系主要由不饱和单体、水、乳化剂（复合几种乳化剂）及水溶性引发剂四大类成分组成；所述单体包括但不限于：丙烯酸、甲基丙烯酸、甲基丙烯酸甲酯、苯乙烯、醋酸乙烯酯、丙烯酸丁酯、丙烯酸异辛酯、丙烯酰胺、N-甲基丙烯酰胺的一种或多种。
2.根据权利要求1所述的一种锂电池负极代SBR用乳液聚合粘合剂的制备方法，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8-10h。
3.根据权利要求2所述的一种锂电池负极代SBR用乳液聚合粘合剂的制备方法，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：一是将单体醋酸乙烯酯、丙烯酸丁酯、丙烯酸异辛酯和其它单体物料泵入到预乳化釜，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，三是将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所述的一种锂电池负极代SBR用乳液聚合粘合剂的制备方法，其特征在于：所述，
B．加热溶解：将聚合釜加热升温到80～86℃、保温10～30分钟，搅拌混匀。
5.根据权利要求2所述的一种锂电池负极代SBR用乳液聚合粘合剂的制备方法，其特征在于：所述，
C．合成反应：将少量的预乳液从预乳釜中滴加到聚合釜中，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所述的一种锂电池负极代SBR用乳液聚合粘合剂的制备方法，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调整。
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