CN112695565B - 一种天然环保湿强剂的制备方法 - Google Patents
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Abstract
本发明公开了一种天然环保湿强剂的制备方法,包括如下步骤:步骤一、将壳聚糖溶解于醋酸水溶液,升温至100‑150℃后加入异氰酸酯和二月桂酸二丁基锡充分反应,经提纯后得到壳聚糖聚合物浓缩液;步骤二、将瓜尔胶粉溶解于水中,加入适量表面活性剂充分混匀后得到瓜尔胶溶液;步骤三、将所述瓜尔胶溶液加入所述壳聚糖聚合物浓缩液中充分混合,然后向其中缓慢加入氯化锌溶液,再加醇类溶剂使产物析出,经洗涤、过滤、干燥、粉碎后即得所述天然环保湿强剂。本发明通过将壳聚糖聚合物与瓜尔胶复配后固化制成固体粉剂,一方面解决了传统湿强剂储存稳定性差的问题,一方面可显著提高湿强度和抗撕裂性能。
Description
技术领域
本发明涉及造纸湿强剂制备领域,尤其涉及天然环保湿强剂的制备方法。
背景技术
湿强性是指纸张被润湿后,其纤维网络结构仍具有机械强度的性能。纸张的湿强性不仅取决于纤维自身特性,还取决于纤维与纤维的节点数量及结合强度。作为造纸的原料,纤维素具有亲水的特点,在纸张上沾水后,纤维素会失去其对应的强度,在工业造纸过程中,如果添加湿强剂后,可以显著的提高纸张的湿强抗张强度。在造纸配方中添加各种化学助剂,可促进湿纤维网的形成,并最终提高纸张的强度性能。加入少量的湿强剂可使纸张湿强性提高几个数量级。
近年来,聚酰胺环氧氯丙烷(PAE)树脂是目前应用较多的一种纸张湿强剂。它能够在中性、碱性条件下使用,是一种由环氧氯丙烷交联长链聚酰胺多胺所得的具有热固性、水溶性的阳离子型高分子树脂。该类湿强剂储存稳定性差,室温长期储存容易产生pH、粘度升高、交联和凝胶化,在环境温度高时或者pH偏高时短时间内就会出现pH、粘度迅速升高和凝胶化问题。此外,PAE型湿强剂在生产过程中,由于环氧氯丙烷发生水解副反应,产生有机氯1,3-二氯-2-丙醇(DCP)和3-氯-1,2-丙二醇(MCPD),该类物质有毒,会危及人体健康。因此开发储存稳定性好的无氯湿强剂是重要的研究发展方向。
发明内容
本发明旨在提供一种天然环保湿强剂的制备方法,以解决背景技术存在的上述缺陷。
本发明是通过如下的技术方案实现的:
一种天然环保湿强剂的制备方法,包括如下步骤:
步骤一、将壳聚糖溶解于醋酸水溶液,升温至100-150℃后加入异氰酸酯和二月桂酸二丁基锡充分反应,经提纯后得到壳聚糖聚合物浓缩液;
步骤二、将瓜尔胶粉溶解于水中,加入适量表面活性剂充分混匀后得到瓜尔胶溶液;
步骤三、将所述瓜尔胶溶液加入所述壳聚糖聚合物浓缩液中充分混合,然后向其中缓慢加入氯化锌溶液,再加醇类溶剂使产物析出,经洗涤、过滤、干燥、粉碎后即得所述天然环保湿强剂。
作为优选的技术方案,各组分的重量份数如下:壳聚糖10-50份、醋酸水溶液50-200份、异氰酸酯2-5份、二月桂酸二丁基锡0.3-0.5份、瓜尔胶粉2-10份、表面活性剂1-2份、氯化锌1-10份、醇类溶剂50-500份。
进一步的,所述醋酸水溶液的质量百分比浓度为0.5-2%;所述瓜尔胶溶液的质量百分比浓度为0.2-1.5%。
所述壳聚糖是脱乙酰度不同的壳聚糖或其衍生物,优选胺基含量75-80%的壳聚糖。
优选的,所述瓜尔胶选自瓜尔胶原粉、非离子瓜尔胶、阴离子瓜尔胶及阳离子瓜尔胶,更优选瓜尔胶原粉,最好是分子量为120-150万、甘露糖和半乳糖之比为1.7-1.8:1的瓜尔胶原粉。发明人发现,采用经改性的瓜尔胶,例如非离子瓜尔胶、阴离子瓜尔胶或阳离子瓜尔胶,最终得到的湿强剂湿强效果较瓜尔胶原粉差。
所述表面活性剂可采用本领域常规的表面活性剂,例如可选自吐温60、吐温80、阴离子表面活性剂SDS、LAS、两性甜菜碱型表面活性剂、非离子型表面活性剂APG、Gemini表面活性剂等。
所述醇类溶剂为C1-C3的一元或二元脂肪醇,例如可选自甲醇、乙醇、异丙醇、乙二醇。
步骤一中所述提纯步骤是将反应产物置于蒸馏装置中加热至85-90℃,蒸馏40-50min。
本发明通过将壳聚糖聚合物与瓜尔胶复配后固化制成固体粉剂,一方面解决了传统湿强剂储存稳定性差的问题,一方面可显著提高湿强度和抗撕裂性能。
具体实施方式
下面通过具体实施例对本发明进行阐述,但并不限制本发明。所用各原料如无特别说明均为常规市售产品。实施例中所用的壳聚糖为胺基含量75-80%的壳聚糖,瓜尔胶原粉采用分子量为120-150万、甘露糖和半乳糖之比为1.7-1.8:1的瓜尔胶原粉。
实施例1
首先称取10份壳聚糖加入到烧瓶中,将烧瓶置于水浴锅中,升温至80℃,加入1%的醋酸溶液50份,溶解后得到改性壳聚糖;将上述改性壳聚糖加入到烧瓶中,并将烧瓶置于油浴锅中,升温至120℃,搅拌3min后,再加入2份异氰酸酯和0.3份二月桂酸二丁基锡,搅拌反应2h后,收集反应物,并置于蒸馏装置中,对装置进行加热至85℃,蒸馏40min,将蒸馏后的液体转移至旋转蒸发仪中,旋转蒸发得到浓度为60%壳聚糖聚合物浓缩液,备用;
将2份瓜尔胶原粉溶解在800份去离子水中,溶解完全后,加入1份表面活性剂吐温80,搅拌均匀后,缓慢加入上述60%壳聚糖聚合物浓缩液中,混合均匀后,向其中缓慢滴加2份氯化锌(配成5%的氯化锌水溶液)中进行固化,加入50份的乙醇,产品析出,过滤、烘干后粉碎,得天然环保湿强剂。
实施例2
首先称取50份壳聚糖加入到烧瓶中,将烧瓶置于水浴锅中,升温至90℃,加入1%的醋酸溶液200份,溶解后得到改性壳聚糖;将上述改性壳聚糖加入到烧瓶中,并将烧瓶置于油浴锅中,升温至130℃,搅拌5min后,再加入5份异氰酸酯和0.5份二月桂酸二丁基锡,搅拌反应3h后,收集反应物,并置于蒸馏装置中,对装置进行加热至90℃,蒸馏50min,将蒸馏后的液体转移至旋转蒸发仪中,旋转蒸发得到浓度为65%壳聚糖聚合物浓缩液,备用;
准确称取10份瓜尔胶原粉溶解在1000份的去离子水中,溶解完全后,加入2份表面活性剂吐温60,搅拌均匀后,加入65%壳聚糖聚合物浓缩液,混合均匀后,向其中缓慢滴加5份氯化锌(配成7%的氯化锌水溶液)中进行固化,最后加入500份的异丙醇中,产品析出,抽滤烘干后粉碎,得天然环保湿强剂。
实施例3
首先称取75份壳聚糖加入到烧瓶中,将烧瓶置于水浴锅中,升温至85℃,加入1%的醋酸溶液150份,溶解后得到改性壳聚糖;将上述改性壳聚糖加入到烧瓶中,并将烧瓶置于油浴锅中,升温至125℃,搅拌4min后,再加入3份异氰酸酯和0.4份二月桂酸二丁基锡,搅拌反应2.5h后,收集反应物,并置于蒸馏装置中,对装置进行加热至90℃,蒸馏50min,将蒸馏后的液体转移至旋转蒸发仪中,旋转蒸发得到浓度为70%壳聚糖聚合物浓缩液,备用;
准确称取5份瓜尔胶原粉分散在900份离子水中,完全溶胀后,加入非离子表面活性剂APG中,搅拌均匀后,加入70%的壳聚糖聚合物浓缩液,混合均匀后,向其中缓慢滴加8份氯化锌(配成6%的氯化锌水溶液)中进行固化,而后加入350份的乙二醇中,过滤烘干后粉碎既得天然环保湿强剂。
对比例1
常规PAE型湿强剂,制备方法如下:将102.3克己二酸与82.5克二乙烯三胺混合,升温到135℃,保温30分钟后,升温至175℃,保温4小时后降温,再加入220克去离子水,得到聚酰胺多胺预聚体水溶液。向上述聚酰胺预聚体水溶液加入1000克去离子水,搅拌均匀,室温下缓慢滴加环氧氯丙烷92.52克,搅拌10分钟后,升温至50℃,保温2小时,然后升温至60℃,保温3.5小时,加入15克硫酸作为终止剂,并加入后期水850克,于40℃保温30min,反应结束后降温,所得产物即为PAE型湿强剂,剪切粘度为35厘泊。
对比例2
CN106638144A实施例1的方法制备的造纸湿强剂。
对比例3
用CN106638144A实施例1制备的改性瓜尔胶替换瓜尔胶原粉,其他同实施例1。
对比例4
首先称取10份壳聚糖加入到烧瓶中,将烧瓶置于水浴锅中,升温至80℃,加入1%的醋酸溶液50份,溶解后得到改性壳聚糖;将上述改性壳聚糖加入到烧瓶中,并将烧瓶置于油浴锅中,升温至120℃,搅拌3min后,再加入2份异氰酸酯和0.3份二月桂酸二丁基锡,搅拌反应2h后,得收集反应物,并置于蒸馏装置中,对装置进行加热至85℃,蒸馏40min,将蒸馏后的液体转移至旋转蒸发仪中,旋转蒸发得到浓度为60%壳聚糖聚合物浓缩液,备用;
将2份的瓜尔胶原粉溶解在800份去离子水中,溶解完全后,加入1份表面活性剂吐温80,搅拌均匀后,缓慢加入60%壳聚糖聚合物浓缩液10份,混合均匀后,将混合液加入到5%的氯化锌溶液中,无法进行固化,然后加入50份的乙醇,产品难以析出,无法得到固体湿强剂。
应用实施例
将400SR针叶木浆和350SR阔叶木浆按照质量比为1:1混合后,打浆至370SR。加入湿强剂量为120Kg/t纸,成纸抄造定量为50g/m2。在LABTECH73-62半自动纸页成型器抄片后,LABTECH 73-50标准纸页压榨机压榨,在纸页快速干燥器上烘干后,在105℃烘箱熟化15分钟平衡水份后,检测纸样的干、湿强度。结果如表1:
表1、纸样物理指标(温/湿度25℃/40%)
由以上检测数据可见,实施例样品的湿抗张强度及湿强保留率均明显高于常规PAE型湿强剂(对比例1),也优于专利CN106638144A公开的方法制备的湿强剂(对比例2)。并且由于本发明为固体粉剂,在使用便捷性、计量准确性、储存稳定性等方面较现有技术制备的液态湿强剂有明显优势。从对比例3的检测数据可以看出,用改性瓜尔胶替代瓜尔胶原粉,湿强保留率略有提高,但湿抗张强度有所下降。从对比例4的检测数据可以看出,氯化锌的添加方式对产物性能影响比较大,将瓜尔胶原粉和壳聚糖聚合物浓缩液混合后直接加入到氯化锌溶液中,湿抗张强度和湿强保留率均明显下降。
以上显示和描述了本发明的基本原理、主要特征及本发明的优点。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。本发明要求保护的范围由所附的权利要求书及其等效物界定。
Claims (9)
1.一种天然环保湿强剂的制备方法,其特征在于,包括如下步骤:
步骤一、将壳聚糖溶解于醋酸水溶液,升温至100-150℃后加入异氰酸酯和二月桂酸二丁基锡充分反应,经提纯后得到壳聚糖聚合物浓缩液;
步骤二、将瓜尔胶粉溶解于水中,加入适量表面活性剂充分混匀后得到瓜尔胶溶液;
步骤三、将所述瓜尔胶溶液加入所述壳聚糖聚合物浓缩液中充分混合,然后向其中缓慢加入氯化锌溶液,再加醇类溶剂使产物析出,经洗涤、过滤、干燥、粉碎后即得所述天然环保湿强剂;
各组分的重量份数如下:壳聚糖10-50份、醋酸水溶液50-200份、异氰酸酯2-5份、二月桂酸二丁基锡0.3-0.5份、瓜尔胶粉2-10份、表面活性剂1-2份、氯化锌1-10份、醇类溶剂50-500份。
2.如权利要求1所述的方法,其特征在于,所述醋酸水溶液的质量百分比浓度为0.5-2%;所述瓜尔胶溶液的质量百分比浓度为0.2-1.5%。
3.如权利要求1所述的方法,其特征在于,所述壳聚糖选自胺基含量75-80%的壳聚糖。
4.如权利要求1所述的方法,其特征在于,所述瓜尔胶为瓜尔胶原粉。
5.如权利要求4所述的方法,其特征在于,所述瓜尔胶为分子量为120-150万、甘露糖和半乳糖之比为1.7-1.8:1的瓜尔胶原粉。
6.如权利要求1所述的方法,其特征在于,所述表面活性剂选自吐温60、吐温80、阴离子表面活性剂SDS、LAS、两性甜菜碱型表面活性剂、非离子型表面活性剂APG、Gemini表面活性剂。
7.如权利要求1所述的方法,其特征在于,所述醇类溶剂为C1-C3的一元或二元脂肪醇。
8.如权利要求7所述的方法,其特征在于,所述醇类溶剂选自甲醇、乙醇、异丙醇、乙二醇。
9.如权利要求1所述的方法,其特征在于,步骤一中所述提纯步骤是将反应产物置于蒸馏装置中加热至85-90℃,蒸馏40-50min。
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