CN113100440B - 一种纳米有机硒及其制备方法 - Google Patents

一种纳米有机硒及其制备方法 Download PDF

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CN113100440B
CN113100440B CN202110222372.9A CN202110222372A CN113100440B CN 113100440 B CN113100440 B CN 113100440B CN 202110222372 A CN202110222372 A CN 202110222372A CN 113100440 B CN113100440 B CN 113100440B
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selenium
selenite
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deionized water
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韩长平
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Han Changping
Han Ziyi
Yin Xiangping
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Abstract

本发明提供了一种纳米有机硒及其制备方法，涉及纳米材料制备领域；所本发明提供的纳米有机硒的制备方法包括以下步骤：将***盐加入到去离子水中，再加入稳定剂A，搅拌使其充分溶解，得到混合液1；取还原剂加入到去离子水中，再加入稳定剂B，搅拌使其充分溶解，得到混合液2；将混合液1和混合液2混匀，加热反应，得到纳米硒粉；取纳米硒粉，加入山梨糖醇和氨基酸溶液进行螯合，并超声处理，冷冻干燥，得到纳米有机硒粉。本发明提供的制备方法操作简单，安全稳定，将化学和物理方法相结合，得到不同粒径均匀的纳米有机硒粉，且本发明中间产物得到的纳米硒回收率高，纳米硒也可被广泛使用。

Description

一种纳米有机硒及其制备方法
技术领域：
本发明涉及纳米材料制备领域，具体涉及一种纳米有机硒及其制备方法。
背景技术：
硒是人和动物必需的微量元素之一，与机体的抗氧化能力、免疫功能、抗病毒、抗癌作用等有着重要关系。硒在自然界的存在方式分为两种：无机硒和植物活性硒；硒能直接作用于病毒，抑制病毒在体内的复制，并能参与细胞的修复，预防多种病毒性疾病(如乙肝、心炎等)。硒能中和或转化自由基的物质，抗氧化，从而祛除自由基对人体的损害，有延缓衰老的作用。硒具有和胰岛素相同的作用，可以不依赖胰岛素来调节体内糖份，可以延缓、减轻、防止糖尿病并发症的产生。硒是癌细胞的杀伤剂，能减轻放、化疗的毒副作用，降低抗癌药物对肾、骨髓和肠胃的毒性，缓解患者的病痛。硒与污染食物、蓄积体内的铅、汞、镉等重金属有很强的亲和力，与其结合形成硒-金属-蛋白质复合物，直接排出体外，起到解毒排毒的作用。另外，硒还被广泛应用于半导体光电、医药生物和陶瓷工业等领域，同时纳米硒还被用作食品添加剂和荧光染料等。
目前的国内外研究表明，人体通过从食物中获取天然有机硒进行补硒是最安全可靠的补硒可靠的补硒方式，而作物通过根际吸收转化形成的有机硒是最安全的。有机硒，如硒酵母、甲壳素硒、氨基酸硒、葡苷聚糖硒等较***钠的安全性高，有机硒是以主动运输机制通过肠壁被机体吸收利用，其吸收率高于***钠，有效改善人体内血硒状况。但有机硒仍存在生产工艺复杂，生产成本高，生物活性较低等问题。
目前，纳米硒的生物活性比无机硒、有机硒高，安全性好，是作为保健品和饲料添加剂的理想硒源。此外，纳米硒与蛋白的NH，C＝O，COO和C-N键结合时表现出很好的生物活性和吸附能力，作为一种抗氧化剂在防治癌症方面具有很好的应用潜力。但其生产成本较高，回收率低。利用纳米硒为人体或者植物补硒时，不能像有机硒一样，同时补充其他重要物质。
本发明将纳米硒和有机物相结合，制备成纳米有机硒，其制备方法将化学和物理方法相结合，得到了不同粒径均匀的纳米有机硒粉，且纳米有机硒粉的回收率较高。
发明内容：
本发明的目的在于提供一种纳米有机硒及其制备方法。本发明提供的纳米有机硒的制备方法操作简单，安全稳定，将化学和物理方法相结合，得到不同粒径均匀的纳米有机硒粉。
本发明一方面提供了一种纳米有机硒的制备方法，包括以下步骤：
(1)称取***盐加入到去离子水中，再加入稳定剂A，搅拌使其充分溶解，得到混合液1；
(2)称取还原剂加入到去离子水中，再加入稳定剂B，搅拌使其充分溶解，得到混合液2；
(3)将混合液1和混合液2混合均匀，加热至40-60℃，反应15-25min，离心，弃上清，加入去离子水，超声处理10-30min，冷冻干燥，得到纳米硒粉；
(4)取步骤(3)得到的纳米硒粉，加入山梨糖醇和氨基酸溶液进行螯合，并超声处理10-30min，冷冻干燥，得到纳米有机硒粉；
按体积比计，氨基酸溶液包括3％的甘氨酸，2％的天冬氨酸和2％的丙氨酸，其余为去离子水；
所述步骤(4)中山梨糖醇、纳米硒粉和氨基酸溶液的质量比为1.5-3:1:10。
优选地，所述的***盐为***钠、***锌或***氢钠中的一种。
优选地，所述的还原剂为抗坏血酸或者葡萄糖中的一种。
优选地，所述的稳定剂A是聚乙烯醇和聚乙二醇按照质量比为2:1的比例混合得到的。
优选地，所述的稳定剂B是十六烷基三甲基溴化铵和正丁醇按照质量比为1:5的比例混合得到的。
优选地，步骤(3)中所述的离心的条件为转速10000-12000rpm，离心时间10-15min。
具体地，一种纳米有机硒的制备方法，包括以下步骤：
(1)称取0.1-1.2g的***盐加入到1-5ml去离子水中，再加入15-40ml稳定剂A，搅拌使其充分溶解，得到混合液1；
(2)称取0.5-6g还原剂加入到1-5ml去离子水中，再加入1-5ml稳定剂B，搅拌使其充分溶解，得到混合液2；
(3)将混合液1和混合液2混合均匀，加热至40-60℃，反应15-25min，在转速10000-12000rpm下离心10-15min，弃上清，加入去离子水，超声处理10-30min，冷冻干燥，得到纳米硒粉；
(4)取步骤(3)得到的纳米硒粉，加入山梨糖醇和氨基酸溶液进行螯合，并超声处理10-30min，冷冻干燥，得到纳米有机硒粉；
按体积比计，氨基酸溶液包括3％的甘氨酸，2％的天冬氨酸和2％的丙氨酸，其余为去离子水；
所述步骤(4)中山梨糖醇、纳米硒粉和氨基酸溶液的质量比为1.5-3:1:10。
本发明的有益效果：
本发明提供了一种纳米有机硒及其制备方法。本发明提供的纳米有机硒的制备方法操作简单，反应时间短，安全稳定，将化学和物理方法相结合，通过控制超声处理的时间得到不同粒径均匀的纳米有机硒粉，且本发明中间产物得到的纳米硒回收率高，纳米硒也可被广泛使用。
具体实施方式
为了使本发明实现的技术手段、创作特征、达成目的与功效易于明白了解，下面结合具体实施例进一步阐明本发明，但下述实施例仅为本发明的优选实施例，并非全部。基于实施方式中的实施例，本领域技术人员在没有做出创造性劳动的前提下所获得其它实施例，都属于本发明的保护范围。
下述实施例中的实验方法，如无特殊说明，均为常规方法，下述实施例中所用的材料、试剂等，如无特殊说明，均可从商业途径得到。
实施例1
一种纳米有机硒的制备方法，包括以下步骤：
(1)称取0.1g的***锌加入到1ml去离子水中，再加入15ml稳定剂A，搅拌使其充分溶解，得到混合液1；
(2)称取0.5g葡萄糖加入到1ml去离子水中，再加入1ml稳定剂B，搅拌使其充分溶解，得到混合液2；
(3)将混合液1和混合液2混合均匀，加热至40℃，反应25min，在转速10000rpm下离心15min，弃上清，加入去离子水，超声处理20min，冷冻干燥，得到纳米硒粉；
(4)取步骤(3)得到的纳米硒粉称重，按照山梨糖醇、纳米硒粉和氨基酸溶液的质量比为1.5:1:10的比例加入山梨糖醇和氨基酸溶液进行螯合，并超声处理20min，冷冻干燥，得到纳米有机硒粉；
按体积比计，氨基酸溶液包括3％的甘氨酸，2％的天冬氨酸和2％的丙氨酸，其余为去离子水。
稳定剂A是聚乙烯醇和聚乙二醇按照质量比为2:1的比例混合得到的。
稳定剂B是十六烷基三甲基溴化铵和正丁醇按照质量比为1:5的比例混合得到的。
用透射电子显微镜观察步骤(3)得到的纳米硒的粒径和步骤(4)得到的纳米有机硒的粒径，平均粒径分别为平均粒径为32nm和35nm。同时计算纳米硒中硒原料的回收率，回收率＝纳米硒的重量/***盐的重量*100％，本实施例纳米硒中硒原料的回收率为38％。
实施例2
一种纳米有机硒的制备方法，包括以下步骤：
(1)称取0.5g的***钠加入到3ml去离子水中，再加入25ml稳定剂A，搅拌使其充分溶解，得到混合液1；
(2)称取2g抗坏血酸加入到3ml去离子水中，再加入2ml稳定剂B，搅拌使其充分溶解，得到混合液2；
(3)将混合液1和混合液2混合均匀，加热至50℃，反应20min，在转速12000rpm下离心10min，弃上清，加入去离子水，超声处理20min，冷冻干燥，得到纳米硒粉；
(4)取步骤(3)得到的纳米硒粉称重，按照山梨糖醇、纳米硒粉和氨基酸溶液的质量比为2:1:10的比例加入山梨糖醇和氨基酸溶液进行螯合，并超声处理20min，冷冻干燥，得到纳米有机硒粉；
按体积比计，氨基酸溶液包括3％的甘氨酸，2％的天冬氨酸和2％的丙氨酸，其余为去离子水。
稳定剂A是聚乙烯醇和聚乙二醇按照质量比为2:1的比例混合得到的。
稳定剂B是十六烷基三甲基溴化铵和正丁醇按照质量比为1:5的比例混合得到的。
用透射电子显微镜观察步骤(3)得到的纳米硒的粒径和步骤(4)得到的纳米有机硒的粒径，平均粒径分别为30nm和32nm。同时计算纳米硒中硒原料的回收率，回收率＝纳米硒的重量/***盐的重量*100％，本实施例纳米硒中硒原料的回收率为45％。
实施例3
一种纳米有机硒的制备方法，包括以下步骤：
(1)称取1.2g的***氢钠加入到5ml去离子水中，再加入40ml稳定剂A，搅拌使其充分溶解，得到混合液1；
(2)称取6g抗坏血酸加入到5ml去离子水中，再加入5ml稳定剂B，搅拌使其充分溶解，得到混合液2；
(3)将混合液1和混合液2混合均匀，加热至60℃，反应15min，在转速11000rpm下离心12min，弃上清，加入去离子水，超声处理20min，冷冻干燥，得到纳米硒粉；
(4)取步骤(3)得到的纳米硒粉称重，按照山梨糖醇、纳米硒粉和氨基酸溶液的质量比为3:1:10的比例加入山梨糖醇和氨基酸溶液进行螯合，并超声处理20min，冷冻干燥，得到纳米有机硒粉；
按体积比计，氨基酸溶液包括3％的甘氨酸，2％的天冬氨酸和2％的丙氨酸，其余为去离子水。
稳定剂A是聚乙烯醇和聚乙二醇按照质量比为2:1的比例混合得到的。
稳定剂B是十六烷基三甲基溴化铵和正丁醇按照质量比为1:5的比例混合得到的。
用透射电子显微镜观察步骤(3)得到的纳米硒的粒径和步骤(4)得到的纳米有机硒的粒径，平均粒径分别为31nm和33nm。同时计算纳米硒中硒原料的回收率，回收率＝纳米硒的重量/***盐的重量*100％，本实施例纳米硒中硒原料的回收率为41％。
实施例4
一种纳米有机硒的制备方法，与实施例2的区别仅在于，步骤(3)和(4)中所述的超声处理的时间为10min。
用透射电子显微镜观察步骤(3)得到的纳米硒的粒径和步骤(4)得到的纳米有机硒的粒径，平均粒径分别为54nm和57nm。同时计算纳米硒中硒原料的回收率，回收率＝纳米硒的重量/***盐的重量*100％，本实施例纳米硒中硒原料的回收率为38％。
实施例5
一种纳米有机硒的制备方法，与实施例2的区别仅在于，步骤(3)和(4)中所述的超声处理的时间为15min。
用透射电子显微镜观察步骤(3)得到的纳米硒的粒径和步骤(4)得到的纳米有机硒的粒径，平均粒径分别为42nm和45nm。同时计算纳米硒中硒原料的回收率，回收率＝纳米硒的重量/***盐的重量*100％，本实施例纳米硒中硒原料的回收率为40％。
实施例6
一种纳米有机硒的制备方法，与实施例2的区别仅在于，步骤(3)和(4)中所述的超声处理的时间为25min。
用透射电子显微镜观察步骤(3)得到的纳米硒的粒径和步骤(4)得到的纳米有机硒的粒径，平均粒径分别为27nm和29nm。同时计算纳米硒中硒原料的回收率，回收率＝纳米硒的重量/***盐的重量*100％，本实施例纳米硒中硒原料的回收率为43％。
实施例6
一种纳米有机硒的制备方法，与实施例2的区别仅在于，步骤(3)和(4)中所述的超声处理的时间为30min。
用透射电子显微镜观察步骤(3)得到的纳米硒的粒径和步骤(4)得到的纳米有机硒的粒径，平均粒径分别为25nm和27nm。同时计算纳米硒中硒原料的回收率，回收率＝纳米硒的重量/***盐的重量*100％，本实施例纳米硒中硒原料的回收率为42％。
综上，本发明提供的一种纳米有机硒的制备方法反应操作简单，安全稳定，时间更短，可通过控制超声处理的时间得到不同粒径均匀的纳米硒和纳米有机硒，且本发明中间产物得到的纳米硒回收率高，也为扩宽纳米硒的应用领域，提高纳米硒的应用价值提供良好的材料基础。
以上所述，仅是本发明的较佳实施例而已，并非对本发明做任何形式上的限制，故凡未脱离本发明技术方案的内容，依据本发明的技术实质对以上实施例所做的任何简单修改、等同变化。

Claims (4)

1.一种纳米有机硒的制备方法，其特征在于，包括以下步骤：
(1）称取***盐加入到去离子水中，再加入稳定剂A，搅拌使其充分溶解，得到混合液1；
(2）称取还原剂加入到去离子水中，再加入稳定剂B，搅拌使其充分溶解，得到混合液2；
(3）将混合液1和混合液2混合均匀，加热至40-60℃，反应15-25min，离心，弃上清，加入去离子水，超声处理10-30min，冷冻干燥，得到纳米硒粉：
(4）取步骤（3）得到的纳米硒粉，加入山梨糖醇和氨基酸溶液进行整合，并超声处理10-30min，冷冻干燥，得到纳米有机硒粉：
按体积比计，氨基酸溶液包括3%的甘氨酸，2%的天冬氨酸和2%的丙氨酸，其余为去离子水：
所述步骤（4）中山梨糖醇、纳米硒粉和氨基酸溶液的质量比为1.5-3:1:10；
其中，所述的稳定剂A是聚乙烯醇和聚乙二醇按照质量比为2:1的比例混合得到的；
所述的稳定剂B是十六烷基三甲基溴化铵和正丁醇按照质量比为1:5的比例混合得到的。
2.根据权利要求1所述的制备方法，其特征在于，所述的***盐为***钠、***锌或***氢钠中的一种。
3.根据权利要求1所述的制备方法，其特征在于，所述的还原剂为抗坏血酸或者葡萄糖中的一种。
4.根据权利要求1所述的制备方法，其特征在于，步骤（3）中所述的离心的条件为转速10000-12000rpm，离心时间10-15min。
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