CN107366186B - 一种抗返潮表面施胶剂的制备方法 - Google Patents
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Abstract
本发明提供一种抗返潮表面施胶剂的制备方法，其组成部分包括聚胺树脂600‑700份、苯丙树脂195‑215份、135‑160份乙二醛、70‑90份硫酸铝、7‑12份氧氯化锆、烷基悕酮二聚体180‑195份和650‑750份水。这几种物资复配组成的抗返潮聚胺树脂乳化剂将烷基悕酮二聚体乳化后能形成非常稳定的乳液，通过表面施胶后，在纸张表面快速形成性能优异的抗水涂层，这种涂层几乎不需要熟化，纸张下机即产生100%的抗水能力，不会因为熟化期长导致纸张返潮而影响强度和抗水能力。
Description
技术领域
本发明涉及一种表面施胶剂，尤其涉及一种抗返潮表面施胶剂的制备方法。
背景技术
AKD(烷基烯酮二聚体)是一种不饱和内酯，产品是不溶于水的蜡状固体，熔点为51~52℃左右。AKD蜡必须制成乳液才能用于造纸施胶，其产品的颗粒粒径约为0.5~2μm，乳液呈白色，易水解，所以一般贮存期较短，仅3个月。由于合成和乳化技术的发展，AKD乳液除用于浆内施胶外，现在也越来越多的用于纸张表面施胶了。目前AKD乳液的生产主要是通过淀粉乳化再均质的工艺，虽然技术成熟，抗水能力强，但AKD乳液熟化期长，纸张易返潮等缺陷一直未有明显改善。
发明内容
本发明的目的在于提供一种抗返潮表面施胶剂的制备方法，解决现有技术中淀粉乳化烷基悕酮二聚体，乳液易水解，保存期短，施胶效率低且纸张易返潮等技术问题。
本发明为解决上述技术问题，所采用的技术方案为：
一、聚胺树脂的制备
将二甲基二烯丙基氯化铵300-460份加入到500-700份水中，升温到65-75℃加EDTA1份，次磷酸钠2-5份，通氮气，在70-88℃时，加8%浓度的过硫酸铵水溶液8-13份和已二酸铵6-9份，反应放热温度会逐步升到88-91℃左右，继续反应一小时后，再次加入过硫酸铵4-6份和已二酸铵水溶液8-10份，温度会逐步上升到95-97℃左右，在此温度下反应28-35分钟，间隔15分钟检测一下粘度，当粘度达到1200-1300时（90℃测），立即加亚硫酸氢钠0.35-0.43份并快速降温到45℃，此产品即为聚胺树脂；
二、苯丙树脂的制备
将淀粉80-120份加入到580-660份水中，升温到89-91℃糊化28-33分钟，然后加入0.8-1.3份硫酸亚铁和8-12份双氧水；往上述溶液中滴加苯乙烯80-90份、丙烯酸丁酯98-108份、改性松香18-23份, 甲基丙烯酰氧乙基三甲基氯化铵30-50份，反应时间7-9小时；降温到45℃时过滤放料即为苯丙树脂；
三、抗返潮聚胺树脂乳化剂的制备
将上述聚胺树脂600-700份升温到65度，加入苯丙树脂195-215份搅拌均匀后加135-160份乙二醛，搅拌30分钟，再加70-90份硫酸铝搅拌30分钟，降温到40℃以下即为抗返潮聚胺树脂乳化剂；
四、抗返潮表面施胶剂的制备
将上述乳化剂80-90份加入到650-750份水中，升温到90℃，加入7-12份氧氯化锆，再加入烷基悕酮二聚体180-195份，待片状的烷基悕酮二聚体全部融化后，调高搅拌机速度，在1000转/分钟下高速搅拌30分钟，当乳液完全发白后，再通过高压均质机乳化二遍，快速冷却后得到本产品：抗返潮表面施胶剂。
抗返潮乳化剂中，苯丙树脂本身就是一种抗水剂但同时也是一种乳化剂，聚胺树脂是一种性能优良的高分子乳化剂，可促进乳液的均一稳定，提高施胶效率，乙二醛在纸张表面的的成膜性能良好。这几种物资复配组成的抗返潮聚胺树脂乳化剂将烷基悕酮二聚体乳化后能形成非常稳定的乳液，通过表面施胶后，在纸张表面快速形成性能优异的抗水涂层，这种涂层几乎不需要熟化，纸张下机即产生100%的抗水能力，不会因为熟化期长导致纸张返潮而影响强度和抗水能力。
具体实施方式
下面结合具体实施例，对本发明的实施方法做进一步详细说明。
实施例1：
A）将二甲基二烯丙基氯化铵390份（Kg，下同）加入到600份水中，升温到70℃加EDTA1份，次磷酸钠3份，通氮气，在79℃时，加8%浓度的过硫酸铵水溶液10份和已二酸铵8份，反应放热温度会逐步升到90℃左右，继续反应一小时后，再次加入过硫酸铵5份和已二酸铵水溶液9份，温度会逐步上升到96℃左右，在此温度下反应31分钟，间隔15分钟检测一下粘度，当粘度达到1200-1300时（90℃测），立即加亚硫酸氢钠0.4份并快速降温到45℃，此产品即为聚胺树脂；
B）将淀粉100份加入到620份水中，升温到90℃糊化30分钟，然后加入1份硫酸亚铁和10份双氧水；往上述溶液中滴加苯乙烯85份、丙烯酸丁酯103份、改性松香20份, 甲基丙烯酰氧乙基三甲基氯化铵40份，反应时间8小时；降温到45℃时过滤放料即为苯丙树脂；
C）将上述聚胺树脂650份升温到65度，加入苯丙树脂205份搅拌均匀后加147份乙二醛，搅拌30分钟，再加80份硫酸铝搅拌30分钟，降温到40℃以下即为抗返潮聚胺树脂乳化剂；
D）将上述乳化剂85份加入到700份水中，升温到90℃，加入9份氧氯化锆，再加入烷基悕酮二聚体188份，待片状的烷基悕酮二聚体全部融化后，调高搅拌机速度，在1000转/分钟下高速搅拌30分钟，当乳液完全发白后，再通过高压均质机乳化二遍，快速冷却后得到本产品：抗返潮表面施胶剂。
实施例2：
A）将二甲基二烯丙基氯化铵460份（Kg，下同）加入到500份水中，升温到65℃加EDTA1份，次磷酸钠5份，通氮气，在88℃时，加8%浓度的过硫酸铵水溶液13份和已二酸铵6份，反应放热温度会逐步升到91℃左右，继续反应一小时后，再次加入过硫酸铵6份和已二酸铵水溶液10份，温度会逐步上升到95℃左右，在此温度下反应35分钟，间隔15分钟检测一下粘度，当粘度达到1200-1300时（90℃测），立即加亚硫酸氢钠0.43份并快速降温到45℃，此产品即为聚胺树脂；
B）将淀粉120份加入到580份水中，升温到91℃糊化28分钟，然后加入1.3份硫酸亚铁和12份双氧水；往上述溶液中滴加苯乙烯90份、丙烯酸丁酯108份、改性松香23份, 甲基丙烯酰氧乙基三甲基氯化铵30份，反应时间9小时；降温到45℃时过滤放料即为苯丙树脂；
C）将上述聚胺树脂700份升温到65度，加入苯丙树脂195份搅拌均匀后加160份乙二醛，搅拌30分钟，再加70份硫酸铝搅拌30分钟，降温到40℃以下即为抗返潮聚胺树脂乳化剂；
D）将上述乳化剂90份加入到650份水中，升温到90℃，加入12份氧氯化锆，再加入烷基悕酮二聚体180份，待片状的烷基悕酮二聚体全部融化后，调高搅拌机速度，在1000转/分钟下高速搅拌30分钟，当乳液完全发白后，再通过高压均质机乳化二遍，快速冷却后得到本产品：抗返潮表面施胶剂。
实施例3：
A）将二甲基二烯丙基氯化铵300份（Kg，下同）加入到700份水中，升温到75℃加EDTA1份，次磷酸钠2份，通氮气，在70℃时，加8%浓度的过硫酸铵水溶液8份和已二酸铵9份，反应放热温度会逐步升到88℃左右，继续反应一小时后，再次加入过硫酸铵4份和已二酸铵水溶液8份，温度会逐步上升到95℃左右，在此温度下反应28分钟，间隔15分钟检测一下粘度，当粘度达到1200-1300时（90℃测），立即加亚硫酸氢钠0.35份并快速降温到45℃，此产品即为聚胺树脂；
B）将淀粉80份加入到580份水中，升温到89℃糊化28分钟，然后加入0.8份硫酸亚铁和8份双氧水；往上述溶液中滴加苯乙烯80份、丙烯酸丁酯98份、改性松香18份, 甲基丙烯酰氧乙基三甲基氯化铵30份，反应时间7小时；降温到45℃时过滤放料即为苯丙树脂；
C）将上述聚胺树脂600份升温到65度，加入苯丙树脂215份搅拌均匀后加135份乙二醛，搅拌30分钟，再加90份硫酸铝搅拌30分钟，降温到40℃以下即为抗返潮聚胺树脂乳化剂；
D）将上述乳化剂80份加入到750份水中，升温到90℃，加入7份氧氯化锆，再加入烷基悕酮二聚体195份，待片状的烷基悕酮二聚体全部融化后，调高搅拌机速度，在1000转/分钟下高速搅拌30分钟，当乳液完全发白后，再通过高压均质机乳化二遍，快速冷却后得到本产品：抗返潮表面施胶剂。
对上述三种方案所得的成品分别进行抗水试验和抗返潮试验检测，检测结果如下表中：
表一，取广东亚太森博纸业有限公司未施胶的纸样，定量70g/m2经表面涂布后，做抗水实验，吸水值越低，抗水性能越好。
表二，用上述已涂布施胶后的纸张与市售70g/m2双胶纸在90%的相同湿度环境下，放置48小时，吸水值越低表明抗返潮能力越强。
由上表可以看出：经过抗返潮表面施胶剂处理过的纸张，经过48小时的高湿度环境存放后，纸张吸水值涨幅较小，而市售纸张涨幅较大，证明抗返潮效果明显；上述三种方案中，以实验方案一的抗水抗返潮效果最优。
Claims (1)
1.一种抗返潮表面施胶剂的制备方法，其特征在于所采用的技术方案为：
聚胺树脂的制备：
将二甲基二烯丙基氯化铵300-460份加入到500-700份水中，升温到65-75℃加EDTA1份，次磷酸钠2-5份，通氮气，在70-88℃时，加8%浓度的过硫酸铵水溶液8-13份和己二酸铵6-9份，反应放热温度会逐步升到88-91℃，继续反应一小时后，再次加入过硫酸铵4-6份和己二酸铵水溶液8-10份，温度会逐步上升到95-97℃，在此温度下反应28-35分钟，间隔15分钟检测一下粘度，当粘度达到1200-1300时（90℃测），立即加亚硫酸氢钠0.35-0.43份并快速降温到45℃，此产品即为聚胺树脂；
苯丙树脂的制备：
将淀粉80-120份加入到580-660份水中，升温到89-91℃糊化28-33分钟，然后加入0.8-1.3份硫酸亚铁和8-12份双氧水；往上述溶液中滴加苯乙烯80-90份、丙烯酸丁酯98-108份、改性松香18-23份, 甲基丙烯酰氧乙基三甲基氯化铵30-50份，反应时间7-9小时；降温到45℃时过滤放料即为苯丙树脂；
抗返潮聚胺树脂乳化剂的制备：
将上述聚胺树脂600-700份升温到65度，加入苯丙树脂195-215份搅拌均匀后加135-160份乙二醛，搅拌30分钟，再加70-90份硫酸铝搅拌30分钟，降温到40℃以下即为抗返潮聚胺树脂乳化剂；
抗返潮表面施胶剂的制备：
将上述乳化剂80-90份加入到650-750份水中，升温到90℃，加入7-12份氧氯化锆，再加入烷基烯酮二聚体180-195份，待片状的烷基烯酮二聚体全部融化后，调高搅拌机速度，在1000转/分钟下高速搅拌30分钟，当乳液完全发白后，再通过高压均质机乳化二遍，快速冷却后得到本产品：抗返潮表面施胶剂。
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