CN110885403B - 一种改性淀粉乳化剂及采用该乳化剂制备的akd乳液 - Google Patents
一种改性淀粉乳化剂及采用该乳化剂制备的akd乳液 Download PDFInfo
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Abstract
本发明公开了一种改性淀粉乳化剂,其制备方法包括如下步骤:将淀粉、适量催化剂、占淀粉重量5‑12%的辛烯基琥珀酸酐和适量水混合,将混合液送入挤压膨化机内进行挤压反应,将挤压产物与一定量的苯乙烯、甲基丙烯酸甲酯、丙烯酸丁酯、引发剂和适量水混合,高速剪切乳化,得到所述改性淀粉乳化剂。本发明还提供一种AKD乳液,是采用上述改性淀粉乳化剂对AKD蜡进行乳化而成。本发明采用辛烯基琥珀酸酐对淀粉进行干法改性,降低分子间力,同时降低表面能,成功制备出一种改性淀粉乳化剂,并进而获得一种性能优异的新型AKD乳液。本发明AKD乳液具有熟化速率快,施胶度高的特点,在造纸领域具有广泛应用价值。
Description
技术领域
本发明涉及AKD施胶剂制备技术领域,具体涉及改性淀粉乳化剂,以及采用该乳化剂制备的AKD乳液。
背景技术
施胶的目的是使纸或纸板具有抗拒液体扩散和渗透的能力,以适于书写和防潮抗湿。在这一过程中,中性施胶剂AKD由于其良好的性能受到广泛的关注。
AKD为蜡状固体,本身不具有电荷,因此无法在纤维上留着,需要使用阳离子乳化剂使其带有正电荷,吸附在纤维上与其发生反应,产生施胶作用。早期,一般采用阳离子淀粉作为乳化剂。由于淀粉电荷量较低,在纤维上的留着率低,且易发生霉变,对乳液的稳定性及后期施胶效果会产生影响。
发明内容
本发明旨在提供一种改性淀粉乳化剂,以及采用该乳化剂制备的AKD乳液,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:
一种改性淀粉乳化剂,其制备方法包括如下步骤:
步骤一,将淀粉、适量催化剂、占淀粉重量5-12%的辛烯基琥珀酸酐和适量水混合,得到混合液;
步骤二,将所述混合液送入挤压膨化机内进行挤压反应;
步骤三,将步骤二获得的挤压产物与一定量的苯乙烯、甲基丙烯酸甲酯、丙烯酸丁酯、引发剂和适量水混合,高速剪切乳化,得到所述改性淀粉乳化剂。
所述淀粉没有特别限定,可以选用各类淀粉,包括但不限于玉米淀粉、木薯淀粉、马铃薯淀粉、小麦淀粉、土豆淀粉、绿豆淀粉。所述淀粉的粒径不大于100目。
优选的,步骤一所用催化剂选自碳酸氢钠、碳酸钠、碳酸氢钾、碳酸钾、氢氧化钠、氢氧化钾、磷酸氢二钠、醋酸钠和氢氧化钙中的至少一种。其用量为淀粉重量的3-5%。
步骤一中,加入水主要是使各组分分散混合更均匀且具有一定流动性,有利于后续的挤压反应。优选加水至混合液的水含量达到18-25wt%。
优选的,步骤二的挤压反应是在套筒温度140-185℃、转速100-200r/min下进行的,产物通过直径0.01m的孔被挤出。
优选的,步骤三中,按淀粉100重量份计,各组分的用量如下:苯乙烯8-10份、甲基丙烯酸甲酯16-22份、丙烯酸丁酯18-25份。
步骤三中所述引发剂可以选用本领域的常用引发剂,包括但不限于:过硫酸钠、过硫酸铵、过硫酸钾、过氧化氢、叔丁基过氧化氢、过氧化二苯甲酰、偶氮二异丁腈、偶氮二异丁基脒盐酸盐、N,N-二甲基苯胺、N,N-二甲基—对甲苯胺、偶氮二异庚腈和偶氮二异丁酸二甲酯中的至少一种。其用量也是本领域技术人员根据反应需要容易进行调整的,优选的用量为苯乙烯用量的0.5-3wt%。水的用量是可以根据反应需要以及最终乳化剂产物的固含量和分散性能进行调整的,优选的用量为150-220份。
优选的,步骤三是在8000-12000r/min的转速下高速剪切乳化。
本发明还进一步提供一种AKD乳液,是采用上述改性淀粉乳化剂对AKD蜡进行乳化而成。
作为进一步优选的技术方案,所述AKD乳液包括如下重量份的组分:
优选的,所述稳定助剂选自高纯聚合氯化铝、聚酰胺多胺环氧氯丙烷树脂、十二烷基硫酸钠、十六烷醇中的至少一种。
所述AKD乳液,可以采用本领域的常规方法制备,例如采用如下方法制备:
将AKD蜡加热熔融,缓慢加入所述改性淀粉乳化剂,5000-8000r/min剪切乳化2-3分钟,然后加入稳定助剂、水,继续高速剪切搅拌5-10分钟后快速冷却、出料。其中加入的水的用量根据AKD乳液产品的实际使用需要调节,优选的水的用量为200-500重量份。
本发明采用辛烯基琥珀酸酐对淀粉进行干法改性,利用酸酐的高表面活性,在挤压膨化机中与淀粉上的羟基发生酯化反应,从而引入疏水基,同时在淀粉分子链间引入长链烃基,降低分子间力,同时降低表面能,成功制备出一种改性淀粉乳化剂,并进而获得一种性能优异的新型AKD乳液。本发明AKD乳液具有熟化速率快,施胶度高的特点,在造纸领域具有广泛应用价值。
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。
实施例1
本实施例技术方案如下:
1.按质量计,将100份玉米淀粉,5份的碳酸钠,10份的辛烯基琥珀酸酐,在高速混合机中混合均匀,补水至水分含量为20%。
2.加入到挤压膨化机中,在套筒温度150℃和转速150r/min下挤压反应,样品通过直径0.01m孔被挤出。然后将10份苯乙烯,20份甲基丙烯酸甲酯,10份丙烯酸丁酯,0.1份过硫酸钠,180份水,加入到上述体系,然后混合均匀,在12000r/min转速下高速剪切乳化,得到一种辛烯基琥珀酸酐改性淀粉乳化剂。
3.将300份AKD蜡加热熔融,将100份上述辛烯基琥珀酸酐改性淀粉乳化剂溶液缓慢加入,6000r/min剪切乳化3分钟,加入4份高纯聚合氯化铝,400份的水,继续高速剪切搅拌10分钟后快速冷却、出料。
实施例2
本实施例技术方案如下:
1.按质量计,将100份玉米淀粉,4份的碳酸氢钠,10份的辛烯基琥珀酸酐,在高速混合机中混合均匀,补水至水分含量为18%。
2.加入到挤压膨化机中,在套筒温度175℃和转速200r/min下挤压反应,样品通过直径0.01m孔被挤出。然后将10份苯乙烯,20份甲基丙烯酸甲酯,10份丙烯酸丁酯,0.1份过硫酸铵,220份水,加入到上述体系,然后混合均匀,在8000r/min转速下高速剪切乳化,得到一种辛烯基琥珀酸酐改性淀粉乳化剂。
3.将400份AKD蜡加热熔融,将100份上述辛烯基琥珀酸酐改性淀粉乳化剂溶液缓慢加入,6000r/min剪切乳化3分钟,加入5份聚酰胺多胺环氧氯丙烷树脂,300份的水,继续高速剪切搅拌10分钟后快速冷却、出料。
实施例3
本实施例技术方案如下:
1.按质量计,将100份玉米淀粉,4份的磷酸氢二钠,7份的辛烯基琥珀酸酐,在高速混合机中混合均匀,补水至水分含量为22%。
2.加入到挤压膨化机中,在套筒温度155℃和转速300r/min下挤压反应,样品通过直径0.01m孔被挤出。然后将10份苯乙烯,20份甲基丙烯酸甲酯,10份丙烯酸丁酯,0.1份过氧化二苯甲酰,190份水,加入到上述体系,然后混合均匀,在10000r/min转速下高速剪切乳化,得到一种辛烯基琥珀酸酐改性淀粉乳化剂。
3.将300份AKD蜡水浴熔融,将100份上述辛烯基琥珀酸酐改性淀粉乳化剂溶液缓慢加入,6000r/min剪切乳化3分钟,加入3份聚酰胺多胺环氧氯丙烷树脂,200份的水,继续高速剪切搅拌5分钟后快速冷却、出料。
实施例4
本实施例技术方案如下:
1.按质量计,将100份玉米淀粉,4份的醋酸钠,9份的辛烯基琥珀酸酐,在高速混合机中混合均匀,补水至水分含量为25%。
2.加入到挤压膨化机中,在套筒温度165℃和转速150r/min下挤压反应,样品通过直径0.01m孔被挤出。然后将10份苯乙烯,20份甲基丙烯酸甲酯,10份丙烯酸丁酯,0.1份偶氮二异丁腈,180份水,加入到上述体系,然后混合均匀,在9000r/min转速下高速剪切乳化,得到一种辛烯基琥珀酸酐改性淀粉乳化剂。
3.将350份AKD蜡加热熔融,将100份上述辛烯基琥珀酸酐改性淀粉乳化剂溶液缓慢加入,6000r/min剪切乳化3分钟,加入4份十六烷醇,300份的水,继续高速剪切搅拌10分钟后快速冷却、出料。
应用实施例
以糊化淀粉AKD乳液为对比例,抄纸:
选用质量分数为0.5%的针叶木浆,顺序加入绝干浆质量0.2%的AKD和0.02%的阳离子聚丙烯酰胺,搅拌1min,最后加入20%GCC(研磨碳酸钙)搅拌均匀后抄纸,抄造定量为60g·m-2左右,再用油压机在0.4MPa压力下压榨1min后,用真空干燥机干燥(92℃左右)4min。下机即测施胶度。施胶度按GB/T5405-1985测定。
此外,熟化率按照下列公式计算:
测定结果如表1所示:
表1
施胶度(%) | 熟化率(%) | |
对比例 | 51 | 59 |
实施例一 | 73 | 82 |
实施例二 | 73 | 81 |
实施例三 | 68 | 75 |
实施例四 | 69 | 78 |
结果表明,本发明所制备的AKD乳液具有更高的施胶度和熟化率,产生了出乎意料的技术效果。
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)
1.一种改性淀粉乳化剂的制备方法,其特征在于,包括如下步骤:
步骤一,将淀粉、适量催化剂、占淀粉重量5-12%的辛烯基琥珀酸酐和适量水混合,得到混合液;
步骤二,将所述混合液送入挤压膨化机内进行挤压反应;
步骤三,将步骤二获得的挤压产物与一定量的苯乙烯、甲基丙烯酸甲酯、丙烯酸丁酯、引发剂和适量水混合,高速剪切乳化,得到所述改性淀粉乳化剂,按淀粉100重量份计,各组分的用量如下:苯乙烯8-10份、甲基丙烯酸甲酯16-22份、丙烯酸丁酯18-25份。
2.如权利要求1所述的方法,其特征在于,所述淀粉的粒径不大于100目。
3.如权利要求1所述的方法,其特征在于,所述催化剂选自碳酸氢钠、碳酸钠、碳酸氢钾、碳酸钾、氢氧化钠、氢氧化钾、磷酸氢二钠、醋酸钠和氢氧化钙中的至少一种。
4.如权利要求3所述的方法,其特征在于,所述催化剂的用量为淀粉重量的3-5%。
5.如权利要求1所述的方法,其特征在于,步骤一中,加水至所述混合液的水含量达到18-25wt%。
6.如权利要求1所述的方法,其特征在于,步骤二的挤压反应是在套筒温度140-185℃、转速100-200r/min下进行的,产物通过直径0.01 m的孔被挤出。
7.一种AKD乳液,其特征在于,是采用权利要求1-6任一项所述方法制备的改性淀粉乳化剂对AKD蜡进行乳化而成。
8.如权利要求7所述的AKD乳液,其特征在于,包括如下重量份的组分:AKD蜡200-500份、改性淀粉乳化剂100份、稳定助剂3-5份、水适量。
9.如权利要求8所述的AKD乳液,其特征在于,所述稳定助剂选自高纯聚合氯化铝、聚酰胺多胺环氧氯丙烷树脂、十二烷基硫酸钠、十六烷醇中的至少一种。
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