CN107779133A - 一种水性压敏胶制备工艺 - Google Patents

一种水性压敏胶制备工艺 Download PDF

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CN107779133A
CN107779133A CN201610735303.7A CN201610735303A CN107779133A CN 107779133 A CN107779133 A CN 107779133A CN 201610735303 A CN201610735303 A CN 201610735303A CN 107779133 A CN107779133 A CN 107779133A
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张孝俤
王翠冈
马海建
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Jiangsu Guojiao Chemical Technology Co Ltd
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Abstract

本发明涉及一种水性压敏胶制备工艺，包括如下步骤：乳化釜配制：反应釜配制：加入过硫酸铵滴加引发，再依次加入碳酸氢铵和乳化剂，搅拌均匀后，开始打开蒸汽阀升温，当温度升到78℃时，关闭蒸汽阀，待釜内温度升至80‑81℃时，开始滴加预乳化液，作为初引种子，整个滴加时间控制在3.5‑4h，反应温度控制在80‑84℃：预乳化液为取自乳化釜内的预乳液；后处理：酸碱度调整及消泡处理：出料：待检测合格后，用滤布过滤、出料。本发明的优点在于：划分多个温度段，有利于提高反应转化效率，达到指定固化量和粘度要求；分次加入乳化剂和过硫酸铵引发剂，保证反应平稳进行；预乳化液滴加缓慢有序，在最佳反应时长内，最大化提高反应转化效率。

Description

一种水性压敏胶制备工艺
技术领域
本发明涉及一种领域，特别涉及一种水性压敏胶制备工艺。
背景技术
水性聚氨酯压敏胶是一类具有对压力有敏感性的胶粘剂。具有较高剥离力、较高剥离强度，适用于泡棉、纸等材料之间的粘接。但是传统的水性压敏胶制备存在固含量不达标，粘度不高，转化率低的问题。
发明内容
本发明要解决的技术问题是提供一种固含量和粘度符合要求且转化率较高的水性压敏胶制备工艺。
为解决上述技术问题，本发明的技术方案为：一种水性压敏胶制备工艺，其创新点在于：包括如下步骤：
（1）乳化釜配制：上好釜底水，开动搅拌，按顺序加入丙烯酸、丙烯酸羟乙酯、丙烯酸丁酯、甲基丙烯酸甲酯、硫醇及乳化剂，继续搅拌15-20min，形成预乳液；
（2）反应釜配制：上好釜底水，开动搅拌，加入过硫酸铵滴加引发，再依次加入碳酸氢铵和乳化剂，搅拌均匀后，开始打开蒸汽阀升温，当温度升到78℃时，关闭蒸汽阀，待釜内温度升至80-81℃时，开始滴加预乳化液，作为初引种子，整个滴加时间控制在3.5-4h，正常反应温度控制在80-95℃：预乳化液为取自乳化釜内的预乳液；
（3）后处理：预乳化液滴加完后，保温1h，保温结束后，开始降温至75℃以下，开始滴加过硫酸铵，滴加完后，继续保温0.5h；
（4）酸碱度调整及消泡处理：第二次保温结束后，开始降温至55℃以下，缓慢加入氨水、消泡剂，10min后加入防腐剂，加完后继续搅拌20-30min，取样测试pH、固含量等指标，补加适量的水，调整固含量至合适的范围；
（5）出料：待检测合格后，用滤布过滤、出料。
进一步的，所述乳化剂为十二烷基苯磺酸钠和OP-8。
进一步的所述步骤（1）中还加入松香酯类增黏树脂。
本发明的优点在于：
（1）更为严格地控制各步骤的反应时间及反应温度，划分多个温度段，有利于提高反应转化效率，达到指定固化量和粘度要求；分次加入乳化剂和过硫酸铵引发剂，保证反应平稳进行；预乳化液滴加缓慢有序，在最佳反应时长内，最大化提高反应转化效率。
（2）为十二烷基苯磺酸钠和OP-8两者混合的乳化效果好。
（3）将松香酯类增粘树脂加入到压敏胶中，可以提高其粘结强度。
具体实施方式
实施例1
本发明公开了一种水性压敏胶制备工艺，包括如下步骤：
（1）乳化釜配制：上好釜底水，开动搅拌，按顺序加入丙烯酸、丙烯酸羟乙酯、丙烯酸丁酯、甲基丙烯酸甲酯、硫醇及乳化剂，乳化剂为十二烷基苯磺酸钠和OP-8，搅拌15-20min，使各原料完全溶解混合，形成预乳液；
（2）反应釜配制：上好釜底水，开动搅拌，加入过硫酸铵滴加引发，再依次加入碳酸氢铵和乳化剂，搅拌均匀后，开始打开蒸汽阀升温，当温度升到78℃时，关闭蒸汽阀，待釜内温度升至80-81℃时，开始滴加预乳化液，作为初引种子，整个滴加时间控制在3.5-4h，反应温度控制在80-84℃：预乳化液为取自乳化釜内的预乳液；
（3）后处理：预乳化液滴加完后，保温1h，保温结束后，开始降温至75℃以下，开始滴加过硫酸铵，滴加完后，继续保温0.5h；
（4）酸碱度调整及消泡处理：第二次保温结束后，开始降温至55℃以下，缓慢加入氨水、消泡剂，10min后加入防腐剂，加完后继续搅拌20-30min，取样测试pH、固含量等指标，补加适量的水，调整固含量至合适的范围；
（5）出料：待检测合格后，用滤布过滤、出料。
经检测，粘度值为103mm2·s-1。
实施例2
在实施例1的基础上，步骤（2）中的反应温度控制在84-90℃，出料后检测粘度值为195.0mm2·s-1，原料转化率为95%。
实施例3
在实施例1或2的基础上，步骤（2）中的反应温度控制在90-95℃，反应过程中出现爆聚现象，出料后产品出现结块，无法使用。
实施例4
在实施例2的基础上，步骤（3）中，预乳化液滴加完后，未经保温直接将反应溶液降温至75℃，测得反应转化率为80%。
由实施例1、2、3可得在其他条件皆相同的情况下产品粘度值对比表，如下：
序号 1 2 3
粘度值（mm2·s-1） 103 195 —
可知，当步骤（2）中的反应温度控制在80-84℃为最佳控制温度。
由实施例2、4可知，在其他条件都相同的情况下，减少反应的保温时间，将影响原料的转化率。
以上显示和描述了本发明的基本原理和主要特征。本行业的技术人员应该了解，本发明不受上述实施例的限制，上述实施例和说明书中描述的只是说明本发明的原理，在不脱离本发明精神和范围的前提下，本发明还会有各种变化和改进，这些变化和改进都落入要求保护的本发明范围内。本发明要求保护范围由所附的权利要求书及其等效物界定。

Claims (3)

1.一种水性压敏胶制备工艺，其特征在于：包括如下步骤：
乳化釜配制：上好釜底水，开动搅拌，按顺序加入丙烯酸、丙烯酸羟乙酯、丙烯酸丁酯、甲基丙烯酸甲酯、硫醇及乳化剂，继续搅拌15-20min，形成预乳液；
反应釜配制：上好釜底水，开动搅拌，加入过硫酸铵滴加引发，再依次加入碳酸氢铵和乳化剂，搅拌均匀后，开始打开蒸汽阀升温，当温度升到78℃时，关闭蒸汽阀，待釜内温度升至80-81℃时，开始滴加预乳化液，作为初引种子，整个滴加时间控制在3.5-4h，正常反应温度控制在80-95℃：预乳化液为取自乳化釜内的预乳液；
后处理：预乳化液滴加完后，保温1h，保温结束后，开始降温至75℃以下，开始滴加过硫酸铵，滴加完后，继续保温0.5h；
酸碱度调整及消泡处理：第二次保温结束后，开始降温至55℃以下，缓慢加入氨水、消泡剂，10min后加入防腐剂，加完后继续搅拌20-30min，取样测试pH、固含量等指标，补加适量的水，调整固含量至合适的范围；
出料：待检测合格后，用滤布过滤、出料。
2.根据权利要求1所述的一种水性压敏胶制备工艺，其特征在于：所述乳化剂为十二烷基苯磺酸钠和OP-8。
3.根据权利要求1所述的一种水性压敏胶制备工艺，其特征在于：所述步骤（1）中还加入松香酯类增黏树脂。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109266260A (zh) * 2018-09-20 2019-01-25 浙江逸雅新材料有限公司 一种乳液型压敏胶的制备方法
CN114341306A (zh) * 2019-09-10 2022-04-12 株式会社Lg化学 丙烯酸酯类压敏粘合剂组合物的制备方法
CN114437262A (zh) * 2021-12-21 2022-05-06 沈其林 一种用于催化剂生产乳液连续净化的新工艺

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109266260A (zh) * 2018-09-20 2019-01-25 浙江逸雅新材料有限公司 一种乳液型压敏胶的制备方法
CN114341306A (zh) * 2019-09-10 2022-04-12 株式会社Lg化学 丙烯酸酯类压敏粘合剂组合物的制备方法
EP3998318A4 (en) * 2019-09-10 2022-10-19 LG Chem, Ltd. PROCESS FOR THE MANUFACTURE OF AN ACRYLATE-BASED ADHESIVE
CN114341306B (zh) * 2019-09-10 2023-11-14 株式会社Lg化学 丙烯酸酯类压敏粘合剂组合物的制备方法
CN114437262A (zh) * 2021-12-21 2022-05-06 沈其林 一种用于催化剂生产乳液连续净化的新工艺

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