CN108841015A - 一种纳晶纤维素乳液的制备方法 - Google Patents
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Abstract
本发明公开了一种纳晶纤维素乳液的制备方法。该包括如下步骤:(1)制备纳晶纤维素水溶液,用酸性溶液调节所述水溶液的pH为4.8‑5.2,得到混合溶液I;(2)在上述步骤(1)得到的混合溶液I中加入油溶性溶剂,得到混合溶液Ⅱ;(3)利用高速剪切机将步骤(2)得到的混合溶液Ⅱ搅拌均匀,即得到纳晶纤维素乳液。本发明具有工艺简单、原料易得、体系无毒、制得的纳晶纤维素乳液稳定性高等优点。
Description
技术领域
本发明属于胶体材料技术领域,特别是涉及一种纳晶纤维素乳液的制备方法。
背景技术
天然纤维素微纤丝含有在长度方向上随机分布的结晶区和无定形区。结晶区纤维素链堆积紧密,性质稳定;而无定形区结构松散,容易受到化学试剂或酶的攻击。因此,在合适的酸或酶解处理条件下,去除天然纤维素中的无定形区而保留结晶区,可得到粉末、液体或凝胶态的纳晶纤维素(Nanocrystalline Cellulose,简称NCC)。
纳晶纤维素是直径小于100nm的超微细纤维,也是纤维素的最小物理结构单元。NCC的来源非常广泛,主要有针叶木、阔叶木、棉花、棉短绒、苎麻、剑麻、甜菜、棕榈、被囊动物、微晶纤维素和细菌纤维素等,不同原料制备的NCC在尺寸和形态上有所差异。
NCC具有许多优良特性,如高结晶度、高纯度、高杨氏模量、高强度、高亲水性、超精细结构、高透明性和液晶性等,加之还具有天然纤维素的轻质、可生物降解、生物相容及可再生等特性,因此,NCC在增强材料、光电、催化和生物医学等领域有良好的应用前景。
NCC具有纳米材料的表面效应和小尺寸效应,可以作为乳化剂和稳定剂。传统的纳米乳液是一种热力学不稳定体系,长时间静置易发生破乳现象,为了提高纳晶纤维素的相容性,本发明开发了一种纳晶纤维素乳液的制备方法,通过本发明可以形成纳晶纤维素稳定存在的胶体体系,具有潜在的应用价值。
发明内容
本发明的目的在于提供一种纳晶纤维素乳液的制备方法。本发明具有工艺简单、原料易得、体系无毒稳定性高等优点。
为了达到上述的目的,本发明采取以下技术方案:
一种纳晶纤维素乳液的制备方法,包括如下步骤:
(1)制备纳晶纤维素水溶液,用酸性溶液调节所述水溶液的pH为4.8-5.2,得到混合溶液I;
(2)在上述步骤(1)得到的混合溶液I中加入油溶性溶剂,得到混合溶液Ⅱ;
(3)利用高速剪切机将步骤(2)得到的混合溶液Ⅱ搅拌均匀,即得到纳晶纤维素乳液。
本发明通过控制步骤(1)混合溶液I的pH,能够有效保证后续添加油溶性溶剂后体系的稳定性。其原理为:NCC比表面积大,表面有大量的羟基,通过调节pH值,能使表面的羟基形成氢键的作用力减弱,减少颗粒间的静电吸引,避免了颗粒的聚集破乳现象。
进一步地,所述纳晶纤维素乳液的制备方法中的纳晶纤维素直径为为50nm到100nm,长度100nm到400nm。
进一步地,所述纳晶纤维素乳液的制备方法步骤(1)中的纳晶纤维素水溶液的质量浓度为0.5%-2.5%。
进一步地,所述纳晶纤维素乳液的制备方法步骤(1)中的酸性溶液优选为乙酸溶液。
进一步地,所述乙酸溶液的浓度为0.01M。
进一步地,所述纳晶纤维素乳液的制备方法步骤(2)中的油溶性溶剂优选为油酸甲酯或环氧大豆油。
油酸甲酯(Methyl oleate),又名顺式-9-十八烯酸甲酯(CIS-9-Octadecenoicacid,methyl ester),9-十八烯酸甲酯(9-Octadecenoic acid methyl ester),无色至淡黄色油状液体,可燃,不溶于水,与乙醇,乙醚等有机溶剂互溶。是一种不饱和高级脂肪酸酯,重要的化工原料,广泛用于制备表面活性剂、皮革添加剂、纺织助剂等,还用作杀虫剂助剂等。
环氧大豆油是用大豆油经过氧化处理后制得的一种化工产品,常温下为浅黄色粘稠油状液体,是一种使用广泛的聚氯乙烯无毒增塑剂兼稳定剂:与PVC树脂相容性好,挥发性低、迁移性小。具有优良的热稳定性和光稳定性,耐水性和耐油性亦佳,可赋予制品良好的机械强度、耐候性及电性能,且无毒性,是国际认可的用于食品包装材料的化学工艺助剂。
油酸甲酯或环氧大豆油都是工业用油溶性溶剂,通过加入油酸甲酯或环氧大豆油能够阻碍纳晶纤维素在空间上的直接接触和聚集,保持良好的分散性,使纳晶纤维素乳液不易沉淀和分层。
进一步地,所述纳晶纤维素乳液的制备方法步骤(2)中混合溶液I与油溶性溶剂的质量比为2:8-5:5。
进一步地,所述纳晶纤维素乳液的制备方法步骤(3)中高速剪切的转速为18000r/min-26000r/min,剪切时间为5-10min。
本发明具有以下技术特点:
1)本发明原料简单,油酸甲酯和环氧大豆油在工业上容易得到,且纳晶纤维素、油酸甲酯和环氧大豆油对环境友好,无污染。
2)本发明制备方法简单,通过调节体系pH,简单混合即可得到稳定的纳米纤维素乳液体系,该体系不易沉淀和分层。
具体实施方式
以下具体实施例是对本发明提供的方法与技术方案的进一步说明,但不应理解成对本发明的限制。
实施例1:
将直径50nm,长度160nm的纳晶纤维素,制成质量浓度为0.5%的水溶液溶液,用浓度为0.01M的乙酸调pH值为5.0,然后将上述混合物与环氧大豆油按质量比5:5的比例混合,在高速剪切机23000r/min转速下剪切5min,形成稳定的乳液。
经检测,该纳晶纤维素乳液在常温储存48h不分层;低温(4℃)储存48h不分层;用蒸馏水稀释10倍,搅拌均匀,不分层。
实施例2:
将直径100nm,长度230nm的纳晶纤维素,制成质量浓度为1%的水溶液溶液,用浓度为0.01M的乙酸调pH值为4.9,然后将上述混合物与环氧大豆油按质量比5:5的比例混合,在高速剪切机23000r/min转速下剪切5min,形成稳定的乳液。
经检测,该纳晶纤维素乳液在常温储存48h不分层;低温(4℃)储存48h不分层;用蒸馏水稀释10倍,搅拌均匀,不分层。
实施例3:
将直径100nm,长度320nm的纳晶纤维素,制成质量浓度为1%的水溶液溶液,用浓度为0.01M的乙酸调pH值为4.8,然后将上述混合物与油酸甲酯按质量比5:5的比例混合,在高速剪切机26000r/min转速下剪切5min,形成稳定的乳液。
经检测,该纳晶纤维素乳液在常温储存48h不分层;低温(4℃)储存48h不分层;用蒸馏水稀释10倍,搅拌均匀,不分层。
实施例4:
将直径100nm,长度400nm的纳晶纤维素,制成质量浓度为1%的水溶液溶液,用浓度为0.01M的乙酸调pH值为5.2,然后将上述混合物与油酸甲酯按质量比5:5的比例混合,在高速剪切机26000r/min转速下剪切5min,形成稳定的乳液。
经检测,该纳晶纤维素乳液在常温储存48h不分层;低温(4℃)储存48h不分层;用蒸馏水稀释10倍,搅拌均匀,不分层。
实施例5:
将直径100nm,长度320nm的纳晶纤维素,制成质量浓度为2.5%的水溶液溶液,用浓度为0.01M的乙酸调pH值为5.2,然后将上述混合物与环氧大豆油按质量比2:8的比例混合,在高速剪切机26000r/min转速下剪切5min,形成稳定的乳液。
经检测,该纳晶纤维素乳液在常温储存48h不分层;低温(4℃)储存48h不分层;用蒸馏水稀释10倍,搅拌均匀,不分层。
对比例1:
将直径100nm,长度320nm的纳晶纤维素,制成质量浓度为1%的水溶液溶液,用浓度为0.01M的乙酸调pH值为5.5,然后将上述混合物与环氧大豆油按质量比2:8的比例混合,在高速剪切机26000r/min转速下剪切5min,形成均一的乳液。
经检测,该纳晶纤维素乳液在常温储存12h分层;低温(4℃)储存24h分层;用蒸馏水稀释10倍,搅拌均匀,常温放置1h分层。
对比例2
将直径100nm,长度320nm的纳晶纤维素,制成质量浓度为1%的水溶液溶液,用浓度为0.01M的乙酸调pH值为4.5,然后将上述混合物与油酸甲酯按质量比2:8的比例混合,在高速剪切机26000r/min转速下剪切5min,形成均一的乳液。
经检测,该纳晶纤维素乳液在常温储存24h分层;低温(4℃)储存24h分层;用蒸馏水稀释10倍,搅拌均匀,常温放置1h分层。
对比例3
将直径100nm,长度320nm的纳晶纤维素,制成质量浓度为0.2%的水溶液溶液,用浓度为0.01M的乙酸调pH值为4.5,然后将上述混合物与环氧大豆油按质量比5:5的比例混合,在高速剪切机26000r/min转速下剪切5min,形成均一的乳液。
经检测,该纳晶纤维素乳液在常温储存6h分层;低温(4℃)储存12h分层;用蒸馏水稀释10倍,搅拌均匀,常温放置30min分层。
以上实施例的说明只是用于帮助理解本发明方法及其核心思想。应当指出,对于本技术领域的普通技术人员来说,在不脱离本发明原理的前提下,还可以对本发明进行若干改进和修饰,这些改进和修饰也落入本发明权利要求保护范围内。
Claims (8)
1.一种纳晶纤维素乳液的制备方法,其特征在于,包括如下步骤:
(1)制备纳晶纤维素水溶液,用酸性溶液调节所述水溶液的pH为4.8-5.2,得到混合溶液I;
(2)在上述步骤(1)得到的混合溶液I中加入油溶性溶剂,得到混合溶液Ⅱ;
(3)利用高速剪切机将步骤(2)得到的混合溶液Ⅱ搅拌均匀,即得到纳晶纤维素乳液。
2.根据权利要求1所述的一种纳晶纤维素乳液的制备方法,其特征在于,所述纳晶纤维素直径为为50nm-100nm,长度100nm-400nm。
3.根据权利要求1所述的一种纳晶纤维素乳液的制备方法,其特征在于,所述步骤(1)中的纳晶纤维素水溶液的质量浓度为0.5%-2.5%。
4.根据权利要求1所述的一种纳晶纤维素乳液的制备方法,其特征在于,所述步骤(1)中的酸性溶液为乙酸溶液。
5.根据权利要求1所述的一种纳晶纤维素乳液的制备方法,其特征在于,所述乙酸溶液的浓度为0.01M。
6.根据权利要求1所述的一种纳晶纤维素乳液的制备方法,其特征在于,所述步骤(2)中的油溶性溶剂为油酸甲酯或环氧大豆油。
7.根据权利要求1所述的一种纳晶纤维素乳液的制备方法,其特征在于,所述步骤(2)中混合溶液I与油溶性溶剂的质量比为2:8-5:5。
8.根据权利要求1所述的一种纳晶纤维素乳液的制备方法,其特征在于,所述纳晶纤维素乳液的制备方法步骤(3)中高速剪切的转速18000r/min-26000r/min,剪切时间为5-10min。
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