CN103435708B - 一种纳米两性淀粉的制备方法 - Google Patents
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Abstract
本发明公开了一种纳米两性淀粉的制备方法。该方法以原淀粉为原料，加入增塑剂，阳离子醚化剂，碱化剂，在高速搅拌机混合均匀，通过八节筒体的双螺杆挤压机挤压，在第五节筒体处以液体喷枪注入阴离子化试剂和碱化剂，在第七节筒体处以液体喷枪注入交联剂，物料挤压后通过挤压机出料口，再经干燥、冷却、粉碎后得到纳米两性淀粉。本发明制得的纳米两性淀粉，阳离子取代度为0.01-0.15，阴离子取代度0.01-0.1，平均粒径100-400nm；在国内首次用双螺杆挤压机生产了纳米两性淀粉，且为纳米两性淀粉在造纸工业中的应用提供了基础。
Description
技术领域
本发明属于淀粉变性技术领域，特别涉及一种纳米两性淀粉的制备方法。
背景技术
淀粉是一种重要的可再生和可生物降解的天然资源，淀粉分子上有很多羟基，在一定温度条件下，能吸水膨胀而糊化，具有一定的粘性和粘着力，在工业上有较广泛的应用。随着造纸工业的发展，对淀粉产品的功能性要求更高，如要求有更好的成膜性，粘度稳定性高、渗透性强、粘结力好、抗老化、耐剪切等性能。两性淀粉是变性淀粉的主要品种之一，系指在淀粉链中既接有阳离子基团，又接上阴离子基团的变性淀粉，具有阳离子淀粉、阴离子淀粉、天然高分子聚合物等多重结构和特性，使用性能比单一变性淀粉衍生物更为优越。
将阴、阳离子引入淀粉骨架上制备两性淀粉的方法主要有湿法和干法。湿法生产用水量大，污染环境，生产成本高；干法存在淀粉与化学试剂混合不均匀，产品粒径大，溶解性差等问题，应用上受到限制。一般制备纳米淀粉的途径主要有：物理法，如机械球磨、气流粉碎、超声波处理等；化学法，如酸、碱降解；生物法，如生物酶水解，以及反相微乳液法。由于淀粉固有的分子结构特性，采用以上方法制备纳米淀粉都存在一定的局限性。
采用双螺杆挤压技术生产纳米两性淀粉，工艺简单，无污水产生，反应效率高，生产成本低。挤压法生产纳米两性淀粉，在对淀粉进行阳离子化、阴离子化的同时，还可使得淀粉糊化，并通过挤压后期添加交联剂，对析出的淀粉分子进行干交联，从而形成稳定的纳米级两性淀粉。
本发明为实现采用双螺杆挤压技术大规模生产纳米两性淀粉奠定了很好的基础。
发明内容
本发明的目的是提供一种纳米两性淀粉的挤压制备方法。
本发明的技术方案为：一种纳米两性淀粉的制备方法，以原淀粉为原料，加入增塑剂，阳离子醚化剂，碱化剂，在高速搅拌机混合均匀，通过八节筒体的双螺杆挤压机挤压，在第五节筒体处以液体喷枪注入阴离子化试剂和碱化剂，在第七节筒体处以液体喷枪注入交联剂，物料挤压后通过挤压机出料口，再经干燥、冷却、粉碎后得到纳米两性淀粉；
1)制备混合料
按比例称取原淀粉，加入塑化剂，阳离子醚化剂，碱化剂，加蒸馏水调节体系水分含量至20-25％，在高速搅拌机混合均匀；
2)双螺杆挤压机挤压条件控制
螺杆转速250-350rpm，挤压机八段温度分别设定为50-60℃，70-90℃，100-110℃，110-120℃，120-125℃，125-130℃，130-135℃，130-135℃，挤压机出料口的模头孔径为5-10mm；
3)挤压
将混合料放入双螺杆挤压机，经由喂料器进入挤压机内挤压，开始进行淀粉的阳离子化，并在挤压机第五节筒体出以液体喷枪注入阴离子化试剂和氢氧化钠，进行淀粉的阴离子化，最后在挤压机的第七节筒体处以液体喷枪注入交联剂，使已塑化的两性淀粉分子的碳六原子通过交联剂的官能团互相连接，进行干交联，形成稳定的纳米两性淀粉微粒；
4)干燥、粉碎
将通过双螺杆挤压机挤压反应后所得产物放入烘箱，烘箱温度30-45℃，对挤出物进行烘干，在室温下冷却，用粉碎机粉碎，得纳米两性淀粉产品。
本发明所用的原淀粉为木薯淀粉、玉米淀粉中的一种。
所述的增塑剂是甲酰胺、水、甘油、尿素中的一种或两种混合物，用量为原淀粉绝干量的5％-10％。
所述的阳离子醚化剂为2，3-环氧丙基三甲基氯化铵，用量为原淀粉绝干量的1％-20％。
所述的碱化剂为氢氧化钠、氢氧化钾中的一种或两种混合物，用量为原淀粉绝干量的0.5％-10％。
所述的阴离子化试剂为氯乙酸钠或氯乙酸，用量为原淀粉绝干量的1％-20％。喷入的阴离子化试剂和氢氧化钠的溶液浓度为40％-60％，其中氢氧化钠用量为原淀粉绝干量的1％-10％。
所述的交联剂为环氧氯丙烷、乙二醛、甲醛中的一种或两种混合物，用量为原淀粉绝干量的0.1％-5％。
本发明的有益效果：本发明采用双螺杆挤压技术生产纳米两性淀粉，原料易得，生产工艺简单，生产成本降低，绿色无污染，可生物降解。挤压法生产的纳米两性淀粉，淀粉的糊化同时发生，且为纳米级粒子，产品溶于水，改善了湿法生产出的产品使用前要经过蒸煮后才能溶解在水中的缺点。
本发明制得的产品纳米两性淀粉，阳离子取代度为0.01-0.15，阴离子取代度0.01-0.1，平均粒径100-400nm，在国内首次用双螺杆挤压机生产了纳米两性淀粉，且为纳米两性淀粉在造纸工业中的应用提供了基础。
具体实施方式
实施例1：
称取10kg玉米淀粉，加入甘油600g，2，3-环氧丙基三甲基氯化铵600g，氢氧化钠200g，加蒸馏水调节体系水分含量至20％，在高速搅拌机混合均匀。调节双螺杆挤压机螺杆转速280rpm，挤压机八段温度分别设定为60℃，80℃，100℃，110℃，120℃，125℃，130℃，135℃，挤压机出料口的模头孔径为5mm。将混合料经由喂料器进入双螺杆挤压机内挤压，并在挤压机第五节筒体以液体喷枪注入60％的氯乙酸钠和氢氧化钠的混合液(其中氯乙酸钠400g，氢氧化钠100g)，第七节筒体处以液体喷枪注入交联剂乙二醛80g。将挤出物放入烘箱，烘箱温度35℃，对挤出物进行烘干，在室温下冷却，用粉碎机粉碎，得纳米两性淀粉产品。
实施例2：
称取10kg玉米淀粉，加入甘油700g，2，3-环氧丙基三甲基氯化铵800g，氢氧化钠220g，加蒸馏水调节体系水分含量至25％，在高速搅拌机混合均匀。调节双螺杆挤压机螺杆转速300rpm，挤压机八段温度分别设定为60℃，85℃，105℃，115℃，120℃，125℃，130℃，135℃，挤压机出料口的模头孔径为5mm。将混合料经由喂料器进入双螺杆挤压机内挤压，并在挤压机第五节筒体以液体喷枪注入60％的氯乙酸钠和氢氧化钠的混合液(其中氯乙酸钠600g，氢氧化钠120g)，第七节筒体处以液体喷枪注入交联剂乙二醛100g。将挤出物放入烘箱，烘箱温度35℃，对挤出物进行烘干，在室温下冷却，用粉碎机粉碎，得纳米两性淀粉产品。
实施例3：
称取15kg玉米淀粉，加入甘油1200g，2，3-环氧丙基三甲基氯化铵900g，氢氧化钠375g，加蒸馏水调节体系水分含量至25％，在高速搅拌机混合均匀。调节双螺杆挤压机螺杆转速300rpm，挤压机八段温度分别设定为50℃，75℃，105℃，115℃，120℃，125℃，130℃，135℃，挤压机出料口的模头孔径为6mm。将混合料经由喂料器进入双螺杆挤压机内挤压，并在挤压机第五节筒体以液体喷枪注入60％的氯乙酸钠和氢氧化钠的混合液(其中氯乙酸钠750g，氢氧化钠195g)，第七节筒体处以液体喷枪注入交联剂乙二醛135g。将挤出物放入烘箱，烘箱温度35℃，对挤出物进行烘干，在室温下冷却，用粉碎机粉碎，得纳米两性淀粉产品。
Claims (1)
1.一种纳米两性淀粉的制备方法，其特征在于：以玉米淀粉为原料，加入增塑剂甘油，阳离子醚化剂2，3-环氧丙基三甲基氯化铵，碱化剂氢氧化钠，在高速搅拌机混合均匀，通过八节筒体的双螺杆挤压机挤压，在第五节筒体处以液体喷枪注入阴离子化试剂氯乙酸钠和氢氧化钠混合溶液，在第七节筒体处以液体喷枪注入交联剂乙二醛，物料挤压后通过挤压机出料口，再经干燥、冷却、粉碎后得到纳米两性淀粉；主要步骤为：
1)制备混合料：按比例称取玉米淀粉，加入玉米淀粉绝干量5％-10％的塑化剂甘油，玉米淀粉绝干量的1％-20％的阳离子醚化剂2，3-环氧丙基三甲基氯化铵，玉米淀粉绝干量的0.5％-10％的碱化剂氢氧化钠，加蒸馏水调节体系水分含量至20-25％，在高速搅拌机混合均匀；
2)八节筒体的双螺杆挤压机挤压条件控制：螺杆转速250-350rpm，挤压机八段温度分别设定为50-60℃，70-90℃，100-110℃，110-120℃，120-125℃，125-130℃，130-135℃，130-135℃，挤压机出料口的模头孔径为5-10mm；
3)挤压：将混合料放入双螺杆挤压机，经由喂料器进入挤压机内挤压，开始进行淀粉的阳离子化，并在挤压机第五节筒体处以液体喷枪注入浓度为40％-60％的阴离子化试剂氯乙酸钠和氢氧化钠的混合液，进行淀粉的阴离子化，其中氯乙酸钠用量为玉米淀粉绝干量的1％-20％，氢氧化钠用量为玉米淀粉绝干量的1％-10％；最后在挤压机的第七节筒体处以液体喷枪注入玉米淀粉绝干量的0.1％-5％的交联剂乙二醛，使己塑化的两性淀粉分子的碳六原子通过交联剂的官能团互相连接，进行干交联，形成稳定的纳米两性淀粉微粒；
4)干燥、粉碎：将通过双螺杆挤压机挤压反应后所得产物放入烘箱，烘箱温度30-45℃，对挤出物进行烘干，在室温下冷却，用粉碎机粉碎，得纳米两性淀粉产品。
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| CN110407947A (zh) * | 2018-04-27 | 2019-11-05 | 上海东升新材料有限公司 | 一种采用双螺杆挤压法制备阳离子淀粉的方法 |
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