CN117285989A - 一种含油茶饼粕提取物的洗洁精及其制备方法 - Google Patents
一种含油茶饼粕提取物的洗洁精及其制备方法 Download PDFInfo
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Abstract
本申请为2022100554882的分案申请,本发明提供的一种含油茶饼粕提取物的洗洁精,通过采用本发明方法制备得到的油茶饼粕提取物,由于其自带的表面活性剂,可直接用作洗护用品的生产,节约资源,且所得的成品泡沫丰富且绵密,清洁去污能力强,增加了消费者的体验需求。
Description
本申请为分案申请,原申请的申请号为2022100554882,申请日为2022年01月18日,发明专利名称为:一种油茶饼粕提取物、制备方法及其应用。
技术领域
本发明洗护用品技术领域,具体涉及一种含油茶饼粕提取物的洗洁精及其制备方法。
背景技术
茶皂素,一种天然的表面活性剂,是从山茶科植物油茶种子中提取得到的。但是,目前油茶饼粕资源基本作为废弃物,充分利用油茶饼粕资源开发茶皂素和更新茶皂素的应用途径是我国当前合理利用油茶饼粕资源的重要任务之一。
茶皂素作为一种源于自然的非离子表面活性剂,其表面临界交束浓度(CMC)为0.5%,HLB值为16,表面张力极小,具有亲水和亲油两部分,在分散、发泡、去污等方面均有较好的性能,茶皂素还具有抗氧化、杀菌、消炎止痒、可降解、无污染、无毒害等优点。
然而,目前茶皂素的研究与应用中还是存在着一些问题,比如:工业化提取的茶皂素成品不论是得率或是纯度都不高,特别是油茶饼粕中的油脂脱离需要多步工艺,纯化技术尚需改进,提取成本有待合理降低。
因此,亟需一种得率高、工艺步骤少且纯化程度高的从油茶饼粕中提取茶皂素用于洗洁精的方法。
发明内容
本发明为了解决现有技术提取茶皂素的效果不高,且提取成本较大,油茶饼粕中的油脂分离效果差等技术问题,提供一种含油茶饼粕提取物的洗洁精。
本发明的第二个目的是提供一种含油茶饼粕提取物的洗洁精的制备方法。
为实现上述第一个目的,本发明采用的技术方案是:
一种含油茶饼粕提取物的洗洁精,按重量份数计,包括以下组分:油茶饼粕提取物20-50份、十二烷基苯磺酸钠8-11份、脂肪醇聚氧乙烯醚硫酸钠(AES)2-5份、椰油酸单乙醇酰胺10-15份、苯甲酸钠1-2份、乙二胺四乙酸二钠(EDTA-Na2)0.1-0.3份、柠檬酸0.5-1.5份、氯化钠饱和溶液20-30份、去离子水40-50份;
所述油茶饼粕提取物的制备方法,包括如下步骤:
步骤1:油茶饼、粕的预处理,得茶饼、粕粉;
步骤2:制备反胶束萃取溶液;
步骤3:将预处理后的油茶饼、粕粉置于步骤2中的反胶束溶液中,进行超声波提取,离心分离,得上清液,所述上清液为反胶束的前萃液;
步骤4:在上清液中加入缓冲溶液,进行反萃取、离心分离后得到有机相和水相;
步骤5:将上述有机相进行柱层析分离,即得油茶饼粕提取物。
优选的,所述步骤2中的反胶束萃取溶液,按重量份数计,包括以下组分:表面活性剂1-5份、非极性有机溶剂10-25份、去离子水70-90份。
优选的,所述表面活性剂为二(2-乙基己基)丁二酸酯磺酸钠(AOT)、十六烷基三甲基溴化铵(CTAB)、三辛基甲基氯化铵(TOMAC)的任意一种。
优选的,所述非极性有机溶剂为异辛烷、环己烷、四氯化碳、三氯甲烷的任意一种。
优选的,所述步骤4中缓冲溶液为含有KI的磷酸缓冲溶液,所述磷酸缓冲溶液的pH值为7.2-9.8。
优选的,所述反胶束溶液的制备方法包括以下步骤,将非极性有机溶剂加入含有表面活性剂的水溶液中,在30-50℃的条件下超声混合溶解,所述反胶束溶液的W0为20-40。
优选的,所述步骤1中的预处理包括,粉碎、过筛、干燥,所述干燥温度为60-80℃,所述过筛的目数为30-60目。
优选的,所述步骤3中的超声波功率为500-700W。
为实现上述第二个目的,本发明采用的技术方案是:
一种如上任一项所述的含油茶饼粕提取物的洗洁精的制备方法,包括以下步骤:取去离子水,将EDTA-Na2溶于水后,缓慢加入十二烷基苯磺酸钠,缓慢搅拌,待十二烷基苯磺酸钠溶解完全后,加入AES和椰油酸单乙醇酰胺,搅拌溶解,用柠檬酸调节pH=7,加入氯化钠饱和溶液、苯甲酸钠,调节黏度,静置除泡,待泡沫去除后,加入油茶饼粕提取物,溶解完全后,即得。
本发明相对于现有技术,有以下优点:
1、本发明提供的一种含油茶饼粕提取物的洗洁精,通过采用本发明方法制备得到的油茶饼粕提取物,由于其自带的表面活性剂,可直接用作洗护用品的生产,节约资源,且所得的成品泡沫丰富且绵密,清洁去污能力强,增加了消费者的体验需求。
2、本发明提供一种油茶饼粕提取物的制备方法,通过含有表面活性剂和非极性有机溶剂的水溶液形成的反胶束体系,结合超声波的方法提取油茶饼粕中的茶皂素,经过前萃、离心和反萃取,所得的油茶饼粕提取物中的茶皂素含量大幅度提高,缩短了工艺流程,相比传统的需要先对油茶饼粕进行脱油除脂的复杂冗长流程,改进为直接用反胶束体系分离茶皂素、油脂及蛋白质,通过将表面活性剂溶于非极性的有机溶剂中并使其浓度超过临界胶束浓度形成的反胶束,以及表面活性剂和蛋白质之间的静电作用,使得茶皂素与油脂和蛋白质更好的分离,从而达到纯化的效果。
3、通过缓冲溶液调节pH,将表面活性剂上极性基团所带的表面电荷进行增大,使得油茶饼粕中的其余杂质产生更大的静引力,蛋白质等杂质进入反胶束基团中,得以分离茶皂素;通过反胶束体系溶液作为提取液,对于油茶饼粕中的油脂及蛋白质有很好的脱除效果,大大提高的生产效率。
具体实施方式
下面结合实施例1-4对本发明的技术方案进行说明。
实施例1
步骤1:将100g的油茶饼粕进行粉碎,得到油茶饼粕粉末,将所得粉末在筛网目数为30目的条件下过筛,并将过筛后的粉末在60℃的条件下进行干燥,得到油茶饼粕粉粗品;
步骤2:将异辛烷加入含有AOT的水溶液中,在30℃的条件下超声混合溶解,所得到的溶液澄清,即为反胶束萃取溶液;
步骤3:将油茶饼粕粉粗品置于步骤2中的反胶束溶液中,在超声波功率为500W的条件下,进行超声波辅助提取,将超声波提取后溶液进行离心分离,得上清液,所述上清液为反胶束的前萃液;
步骤4:在上清液中加入pH值为7.2的含有KI的缓冲溶液,进行反萃取、离心分离后得到有机相和水相;
步骤5:将上述有机相进行柱层析分离,即得油茶饼粕提取物23.2g。
实施例2
步骤1:将100g的油茶饼粕进行粉碎,得到油茶饼粕粉末,将所得粉末在筛网目数为40目的条件下过筛,并将过筛后的粉末在70℃的条件下进行干燥,得到油茶饼粕粉粗品;
步骤2:将异辛烷加入含有AOT的水溶液中,在40℃的条件下超声混合溶解,所得到的溶液澄清,即为反胶束萃取溶液;
步骤3:将油茶饼粕粉粗品置于步骤2中的反胶束溶液中,在超声波功率为600W的条件下,进行超声波辅助提取,将超声波提取后溶液进行离心分离,得上清液,所述上清液为反胶束的前萃液;
步骤4:在上清液中加入pH值为8.0的含有KI的缓冲溶液,进行反萃取、离心分离后得到有机相和水相;
步骤5:将上述有机相进行柱层析分离,即得油茶饼粕提取物25.1g。
实施例3
步骤1:将100g的油茶饼粕进行粉碎,得到油茶饼粕粉末,将所得粉末在筛网目数为50目的条件下过筛,并将过筛后的粉末在70℃的条件下进行干燥,得到油茶饼粕粉粗品;
步骤2:将异辛烷加入含有AOT的水溶液中,在45℃的条件下超声混合溶解,所得到的溶液澄清,即为反胶束萃取溶液;
步骤3:将油茶饼粕粉粗品置于步骤2中的反胶束溶液中,在超声波功率为650W的条件下,进行超声波辅助提取,将超声波提取后溶液进行离心分离,得上清液,所述上清液为反胶束的前萃液;
步骤4:在上清液中加入pH值为8.7的含有KI的缓冲溶液,进行反萃取、离心分离后得到有机相和水相;
步骤5:将上述有机相进行柱层析分离,即得油茶饼粕提取物26.8g。
实施例4
步骤1:将100g的油茶饼粕进行粉碎,得到油茶饼粕粉末,将所得粉末在筛网目数为60目的条件下过筛,并将过筛后的粉末在80℃的条件下进行干燥,得到油茶饼粕粉粗品;
步骤2:将异辛烷加入含有AOT的水溶液中,在50℃的条件下超声混合溶解,所得到的溶液澄清,即为反胶束萃取溶液;
步骤3:将油茶饼粕粉粗品置于步骤2中的反胶束溶液中,在超声波功率为700W的条件下,进行超声波辅助提取,将超声波提取后溶液进行离心分离,得上清液,所述上清液为反胶束的前萃液;
步骤4:在上清液中加入pH值为9.8的含有KI的缓冲溶液,进行反萃取、离心分离后得到有机相和水相;
步骤5:将上述有机相进行柱层析分离,即得油茶饼粕提取物28.5g。
表1:实施例1-4的反胶束溶液制备配方(单位:重量份)
计算实施例1-4中油茶饼粕提取物中茶皂素的含量和纯度如表2所示。
表2:实施例1-4中油茶饼粕提取物以及其中茶皂素的含量和纯度
产物有效成分 | 实施例1 | 实施例2 | 实施例3 | 实施例4 |
提取物含量(g) | 23.2 | 25.1 | 26.8 | 28.5 |
茶皂素含量(%) | 22.8 | 24.3 | 25.7 | 27.6 |
茶皂素纯度(%) | 98.27 | 96.81 | 95.89 | 96.84 |
从表2可以看出,通过反胶束体系结合超声波的方法提取油茶饼粕中的茶皂素,经过前萃、离心和反萃取,所得的油茶饼粕提取物中的茶皂素含量大幅度提高,缩短了工艺流程,相比传统的需要先对油茶饼粕进行脱油除脂的复杂冗长流程,改进为直接用反胶束体系分离茶皂素、油脂及蛋白质,通过将表面活性剂溶于非极性的有机溶剂中并使其浓度超过临界胶束浓度形成的反胶束,以及表面活性剂和蛋白质之间的静电作用,使得茶皂素与油脂和蛋白质更好的分离,从而达到纯化的效果其得率均高于22%,纯度均能高于95.1%。
实施例5茶皂素在洗护产品中应用
分别取5个相同规格的烧杯量取40份的去离子水,将0.2份的EDTA-Na2溶于水缓慢加入8份的十二烷基苯磺酸钠,缓慢搅拌,待十二烷基苯磺酸钠溶解完全后,加入4份的AES和10份的6502,搅拌溶解,用柠檬酸调节pH=7左右,加入氯化钠饱和溶液20份、苯甲酸钠1份,调节黏度至所需的黏度,静置除泡,待泡沫去除后,分别加入上述实施例1中的油茶饼粕提取物0、20、30、40、50份至溶解完全后,记作1、2、3、4、5号,并测试其发泡情况根据国家标准GB/T 13173-2021和去污能力,如表3所示。
表3:不同油茶饼粕提取物的添加量对发泡能力和去污能力的影响
由表3的测试结果可知,通过采用本发明方法制备得到的油茶饼粕提取物,由于其自带的表面活性剂,可直接用作洗护用品且气泡能力强,泡沫绵密度高去污效果好,特别是加入30份的油茶饼粕提取物所制得的洗洁精效果最好。
以上所述仅为本申请的较佳实施例而已,并不用以限制本申请,凡在本申请的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本申请的保护范围之内。
Claims (9)
1.一种含油茶饼粕提取物的洗洁精,其特征在于,按重量份数计,包括以下组分:油茶饼粕提取物20-50份、十二烷基苯磺酸钠8-11份、脂肪醇聚氧乙烯醚硫酸钠(AES)2-5份、椰油酸单乙醇酰胺10-15份、苯甲酸钠1-2份、乙二胺四乙酸二钠(EDTA-Na2)0.1-0.3份、柠檬酸0.5-1.5份、氯化钠饱和溶液20-30份、去离子水40-50份;
所述油茶饼粕提取物的制备方法,包括如下步骤:
步骤1:油茶饼、粕的预处理,得茶饼、粕粉;
步骤2:制备反胶束萃取溶液;
步骤3:将预处理后的油茶饼、粕粉置于步骤2中的反胶束溶液中,进行超声波提取,离心分离,得上清液,所述上清液为反胶束的前萃液;
步骤4:在上清液中加入缓冲溶液,进行反萃取、离心分离后得到有机相和水相;
步骤5:将上述有机相进行柱层析分离,即得油茶饼粕提取物。
2.根据权利要求1所述的含油茶饼粕提取物的洗洁精,其特征在于:所述步骤2中的反胶束萃取溶液,按重量份数计,包括以下组分:表面活性剂1-5份、非极性有机溶剂10-25份、去离子水70-90份。
3.根据权利要求2所述的含油茶饼粕提取物的洗洁精,其特征在于:所述表面活性剂为二(2-乙基己基)丁二酸酯磺酸钠(AOT)、十六烷基三甲基溴化铵(CTAB)、三辛基甲基氯化铵(TOMAC)的任意一种。
4.根据权利要求2所述的含油茶饼粕提取物的洗洁精,其特征在于:所述非极性有机溶剂为异辛烷、环己烷、四氯化碳、三氯甲烷的任意一种。
5.根据权利要求1所述的含油茶饼粕提取物的洗洁精,其特征在于:所述步骤4中缓冲溶液为含有KI的磷酸缓冲溶液,所述磷酸缓冲溶液的pH值为7.2-9.8。
6.根据权利要求1所述的含油茶饼粕提取物的洗洁精,其特征在于:所述反胶束溶液的制备方法包括以下步骤,将非极性有机溶剂加入含有表面活性剂的水溶液中,在30-50℃的条件下超声混合溶解,所述反胶束溶液的W0为20-40。
7.根据权利要求1所述的含油茶饼粕提取物的洗洁精,其特征在于:所述步骤1中的预处理包括,粉碎、过筛、干燥,所述干燥温度为60-80℃,所述过筛的目数为30-60目。
8.根据权利要求1所述的含油茶饼粕提取物的洗洁精,其特征在于:所述步骤3中的超声波功率为500-700W。
9.一种如权利要求1-8任一项所述的含油茶饼粕提取物的洗洁精的制备方法,其特征在于,包括以下步骤:取去离子水,将EDTA-Na2溶于水后,缓慢加入十二烷基苯磺酸钠,缓慢搅拌,待十二烷基苯磺酸钠溶解完全后,加入AES和椰油酸单乙醇酰胺,搅拌溶解,用柠檬酸调节pH=7,加入氯化钠饱和溶液、苯甲酸钠,调节黏度,静置除泡,待泡沫去除后,加入油茶饼粕提取物,溶解完全后,即得。
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