| Publication number | CN103192091 B |
| Publication type | Grant |
| Application number | CN 201310141406 |
| Publication date | 8 Apr 2015 |
| Filing date | 23 Apr 2013 |
| Priority date | 23 Apr 2013 |
| Also published as | CN103192091A |
| Publication number | 201310141406.7, CN 103192091 B, CN 103192091B, CN 201310141406, CN-B-103192091, CN103192091 B, CN103192091B, CN201310141406, CN201310141406.7 |
| Inventors | 彭亮, 杨万鑫, 熊勇超, 曾清如, 邵继海 |
| Applicant | 湖南农业大学 |
| Export Citation | BiBTeX, EndNote, RefMan |
| Patent Citations (6), Classifications (1), Legal Events (3) | |
| External Links: SIPO, Espacenet | |
技术领域 TECHNICAL FIELD
[0001] 本发明涉及水溶性纳米铁的制备方法，特别是一种利用猴欢喜树叶绿色合成水溶性纳米铁的方法。 [0001] The present invention relates to a method for preparing a water-soluble nano iron, especially an Sloanea leaves green synthetic water-soluble nano-iron approach.
背景技术 Background technique
[0002] 纳米铁由于其强还原性、优异的催化性在废水处理、土壤修复、催化降解等领域发挥着重要的作用，所以，纳米铁的制备方法备受人们的关注。 [0002] The nano-iron because of its strong reduction, excellent catalytic wastewater treatment, soil remediation, catalytic degradation plays an important role in the field, so nano iron preparation much attention. 现在常用制备纳米铁的方法是利用强还原剂还原法。 Now commonly used method is the use of nano iron strong reducing agent reduction.
[0003] 强还原剂还原法常用NaBH4、N2H4等还原铁盐制备成纳米铁。 [0003] The method is commonly used strong reducing agent NaBH4, N2H4 and other prepared nanometer ferric iron reduction. NaBH4、N2H4具有易燃易爆性质，其运输及制备过程对环境影响很大，并且成本较高。 NaBH4, N2H4 has explosive properties, the transport and preparation process a great impact on the environment, and high cost. 户田工业株式会社(TodaKogyo Ltd.)开始使用氢气作为还原剂，在350。 Toda Kogyo Co., Ltd. (TodaKogyo Ltd.) started using hydrogen as a reducing agent, at 350. C -600。 C -600. C范围内还原氧化铁纳米颗粒。 Reduction of iron oxide nanoparticles within the C range. 这个过程虽然比NaBH4还原法进了一步，但是此方法制备氧化铁纳米颗粒需要步骤很繁琐。 Although this process a step further than the NaBH4 reduction method, but this method requires the preparation of iron oxide nanoparticles steps are cumbersome. Laurab.Hoch采用了将碳黑和铁盐混合后在Ar气保护下于600-800° C热解，从而制备出碳负载的纳米铁。 Laurab.Hoch used to heat the solution at 600-800 ° C under Ar protection of carbon black and iron salts mixed, thereby preparing a carbon nano-iron load. 但是这种制备方法需要保护气体和高温，且无法制备出水溶性、高分散的纳米铁。 However, this method requires the preparation of protective gas and heat, and can not prepare a water-soluble, highly dispersed nano-iron.
[0004] 为了发展一项绿色环保的还原技术，替代常规的强还原剂还原法，一系列的生物可再生资源如废弃生物质、维生素、果渣、油酸、咖啡，用于还原制备纳米金属颗粒如金、银及铜等。 [0004] In order to develop a green reduction technology, a strong reducing agent instead of the conventional method, a series of bio-renewable resources such as waste biomass, vitamins, Marc, oleic acid, coffee, used to restore the nano metal particles such as gold, silver and copper. 现在，只发现茶叶、葡萄中的多酚类物质能够将铁盐还原制备出纳米铁。 Now, only found in tea, grape polyphenols can be prepared by reduction of ferric iron nano. 然而，这些物质都是食品，其广泛的工业应用必将引起相关食品的短缺。 However, these substances are food, it will cause a wide range of industrial applications related to food shortages. 因此，开发新的非食品性生物质作为制备纳米铁的还原剂具有重要的意义。 Therefore, the development of new non-food biomass has an important significance as nano iron reductant.
发明内容 SUMMARY OF THE INVENTION
[0005] 本发明所要解决的问题是，针对纳米铁制备成本太高而且难度大的状况，提供一种制备方法简单，成本低廉，绿色环保的利用植物质绿色合成水溶性纳米铁的方法。 [0005] The present invention is to solve the problem is for the preparation of nano-iron high cost and difficulty of the situation, there is provided a preparation method is simple, low cost and the use of green vegetable green synthetic water-soluble nano-iron approach.
[0006] 为解决上述技术问题，本发明所采用的技术方案是:一种利用猴欢喜树叶绿色合成水溶性纳米铁的方法，其包括:首先按100.0 mL除氧水中加入1.00g-5.00g猴欢喜树叶粉末的标准制得猴欢喜树叶溶液，在50° C -70° C热水中水浴30-120分钟；然后将加热后的猴欢喜树叶溶液经转速为3000r/min-6000r/min的离心机离心5min_10min，得到的上清液即为猴欢喜树叶提取液；接着按40.0 mL猴欢喜树叶提取液加入摩尔浓度为0.10mol/L且已除氧的铁盐水溶液2mL-10.0 mL的标准，摇勾，即得到水溶性纳米铁。 [0006] In order to solve the above problems, the technical aspect of the present invention is used is: a monkey joy leaf green synthetic water-soluble nano-iron method uses, which include: first by 100.0 mL of water was added 1.00g-5.00g oxygen monkey joy leaf powder standard solution prepared Sloanea leaves, water bath at 50 ° C -70 ° C hot water for 30 to 120 minutes; then the joy leaf monkey heated solution through speed of 3000r / min-6000r / min centrifugal Centrifugal 5min_10min, supernatant was joy leaf extract is a monkey; followed by 40.0 mL Sloanea leaf extract was added to the molar concentration of iron salt solution 0.10mol / L and has oxygen in 2mL-10.0 mL of standard, shake hook, to obtain a water soluble nano-iron.
[0007] 该铁盐水溶液优选为硝酸铁水溶液或硫酸亚铁水溶液或氯化铁水溶液。 [0007] The aqueous ferrous salt solution is preferably an aqueous solution of ferric nitrate or ferrous sulfate or ferric chloride aqueous solution.
[0008] 猴欢喜树叶粉末是将新鲜干净的猴欢喜树叶于60°C-80°C干燥36h-144h后经粉碎得到的。 [0008] Sloanea leaves powder is fresh clean leaves monkey joy at 60 ° C-80 ° C after drying 36h-144h pulverized get.
[0009] 经研宄发现，猴欢喜树叶中含有大量的强还原性生物质，而且含有多糖类物质，所以猴欢喜树叶中的强还原性物质能够将硝酸铁水溶液中的铁离子还原制备成纳米铁，而新制备的纳米铁表面立即被多糖类物质包覆，从而形成在水中分散性良好的纳米铁，即水溶性纳米铁。 [0009] traitor discovered through research, Sloanea leaves contain a lot of strong reduction of the biomass, but also contains polysaccharides, so Sloanea leaves a strong reducing substances can be iron nitrate solution of iron ions to prepare a Nano-iron, nano-iron surface of freshly prepared immediately polysaccharide coating, thereby forming water-dispersible nano-iron well, that water soluble nano-iron. 所制备的水溶性纳米铁呈黑色，与淡黄色铁离子、黄色的植物提取液颜色完全不同，表明铁离子被还原成为黑色的零价铁。 Water-soluble nano-iron produced was black, with a pale yellow iron, yellow color completely different plant extracts, showed black iron ions are reduced to the zero-valent iron.
[0010] 与现有制备纳米铁的方法相比，本发明具有以下优点: [0010] Compared with the existing method of preparation of nano-iron, the present invention has the following advantages:
[0011] 1、本发明采用了一种新的植物质，即猴欢喜树叶提取液可以将铁盐还原制备成水溶性纳米铁，开发了植物功能，并为水溶性纳米铁的合成提供了新的技术。 [0011] 1, the present invention utilizes a new plant material, namely Sloanea leaves extract can be prepared as a water-soluble nano ferric iron reduction, the development of plant functions, and provides a new synthetic water soluble nano-iron technology.
[0012] 2、本发明方法，不仅制备方法简单，成本低廉，而且从原料、生产过程、产品都是绿色环保的，有效地促进环境的可持续发展，具有重要的环保，经济，生态意义。 [0012] 2. The method of the present invention, not only the preparation method is simple, low cost, but also from raw materials, production processes, products are green, effective in promoting environmentally sustainable development, with important environmental, economic and ecological significance.
[0013] 3、所制备的水溶性纳米铁具有优秀的催化作用，对降解溴百里酚蓝等物质具有很强催化效果。 [0013] 3, water soluble nano-iron produced has excellent catalytic degradation of bromothymol blue and other substances with a strong catalytic effect.
附图说明 Brief Description
[0014]图1为利用猴欢喜树叶制备出的水溶性纳米铁的透射电镜照片。 [0014] FIG. 1 is prepared utilizing Sloanea leaves soluble nano-iron TEM photographs.
[0015]图2为所制得的水溶性纳米铁催化降解溴百里酚蓝动力学情况。 Water-soluble nano-iron catalysis [0015] FIG. 2 is prepared bromothymol blue degradation kinetics. 其中，空白对照的是没有加入水溶性纳米铁时溴百里酚蓝随时间变化的情况。 Wherein, when the control is not a member of the water-soluble nano bromine thymol blue iron over time to changing circumstances.
具体实施方式 DETAILED DESCRIPTION
[0016] 实施例1: [0016] Example 1:
[0017] 1.将采集的猴欢喜树叶在60°C干燥144h，粉碎后得到猴欢喜树叶粉末。 [0017] 1. The collection of monkey rejoice at 60 ° C and dried leaves 144h, after grinding to obtain a powder monkey joy leaves.
[0018] 2.称取1.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在70° C热水中水浴30分钟。 [0018] 2. Weigh 1.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 70 ° C water bath for 30 minutes.
[0019] 3.将加热后的猴欢喜树叶溶液以转速为4000 r/min离心5min，得到的上清液即为猴欢喜树叶提取液。 [0019] 3. The joy leaf monkey heated solution at a rotational speed of 4000 r / min centrifugal 5min, supernatant was joy leaf extract is a monkey.
[0020] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.lOmol/L的硝酸铁溶液2.0 mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0020] 4. Take 40ml Sloanea leaf extract iron nitrate solution was added to remove oxygen 0.lOmol / L of 2.0 mL, mixing, to obtain a black gel, to obtain a water soluble nano-iron.
[0021] 实施例2: [0021] Example 2:
[0022] 1.将采集的猴欢喜树叶在60°C干燥144h，粉碎后得到猴欢喜树叶粉末。 [0022] 1. The collection of monkey rejoice at 60 ° C and dried leaves 144h, after grinding to obtain a powder monkey joy leaves.
[0023] 2.称取2.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在70° C热水中水浴30分钟。 [0023] 2. Weigh 2.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 70 ° C water bath for 30 minutes.
[0024] 3.将加热后的猴欢喜树叶溶液以转速为6000 r/min离心5min，得到的上清液即为猴欢喜树叶提取液。 [0024] 3. The joy leaf monkey heated solution at a rotational speed of 6000 r / min centrifugal 5min, supernatant was joy leaf extract is a monkey.
[0025] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.1OmoI/L的硫酸亚铁水溶液4.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0025] 4. Take 40ml Sloanea leaf extract was added to remove oxygen 0.1OmoI / L of ferrous sulfate solution 4.0mL, mixing, to obtain a black gel, to obtain a water soluble nano-iron.
[0026] 实施例3: [0026] Example 3:
[0027] 1.将采集的猴欢喜树叶在60°C干燥144h，粉碎后得到猴欢喜树叶粉末。 [0027] 1. The collection of monkey rejoice at 60 ° C and dried leaves 144h, after grinding to obtain a powder monkey joy leaves.
[0028] 2.称取4.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在70° C热水中水浴30分钟。 [0028] 2. Weigh 4.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 70 ° C water bath for 30 minutes.
[0029] 3.将加热后的猴欢喜树叶溶液以转速为4000 r/min离心7min，得到的上清液即为猴欢喜树叶提取液。 [0029] 3. The joy leaf monkey heated solution at a rotational speed of 4000 r / min centrifugation 7min, the supernatant obtained is Sloanea leaves extract.
[0030] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.1OmoI/L的硝酸铁水溶液8.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0030] 4. Take 40ml Sloanea leaf extract was added to remove oxygen 0.1OmoI / 8.0mL L iron nitrate solution, and mixed to obtain a black gel, to obtain a water soluble nano-iron.
[0031] 实施例4: [0031] Example 4:
[0032] 1.将采集的猴欢喜树叶在60°C干燥144h，粉碎后得到猴欢喜树叶粉末。 [0032] 1. The collection of monkey rejoice at 60 ° C and dried leaves 144h, after grinding to obtain a powder monkey joy leaves.
[0033] 2.称取5.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在70° C热水中水浴30分钟。 [0033] 2. Weigh 5.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 70 ° C water bath for 30 minutes.
[0034] 3.将加热后的猴欢喜树叶溶液以转速为4000 r/min离心5min，得到的上清液即为猴欢喜树叶提取液。 [0034] 3. The joy leaf monkey heated solution at a rotational speed of 4000 r / min centrifugal 5min, supernatant was joy leaf extract is a monkey.
[0035] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.10mol/L的硝酸铁溶液10.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0035] 4. Take 40ml Sloanea leaf extract iron nitrate solution was added to remove oxygen 10.0mL 0.10mol / L, and mixed to obtain a black gel, to obtain a water soluble nano-iron.
[0036] 实施例5: [0036] Example 5:
[0037] 1.将采集的猴欢喜树叶在60°C干燥144h，粉碎后得到猴欢喜树叶粉末。 [0037] 1. The collection of monkey rejoice at 60 ° C and dried leaves 144h, after grinding to obtain a powder monkey joy leaves.
[0038] 2.称取3.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在70° C热水中水浴30分钟。 [0038] 2. Weigh 3.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 70 ° C water bath for 30 minutes.
[0039] 3.将加热后的猴欢喜树叶溶液以转速为4000 r/min离心5min，得到的上清液即为猴欢喜树叶提取液。 [0039] 3. The joy leaf monkey heated solution at a rotational speed of 4000 r / min centrifugal 5min, supernatant was joy leaf extract is a monkey.
[0040] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.10mol/L的硝酸铁水溶液6.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0040] 4. Take 40ml Sloanea leaf extract, adding iron nitrate solution 6.0mL remove oxygen 0.10mol / L, and mixed to obtain a black gel, to obtain a water soluble nano-iron.
[0041] 实施例6: [0041] Example 6:
[0042] 1.将采集的猴欢喜树叶在70°C干燥72h，粉碎后得到猴欢喜树叶粉末。 [0042] 1. The collection of monkey rejoice dried leaves in 70 ° C 72h, after grinding to obtain a powder monkey joy leaves.
[0043] 2.称取5.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在70° C热水中水浴30分钟。 [0043] 2. Weigh 5.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 70 ° C water bath for 30 minutes.
[0044] 3.将加热后的猴欢喜树叶溶液以转速为3000 r/min离心10 min，得到的上清液即为猴欢喜树叶提取液。 [0044] 3. The joy leaf monkey heated solution at a rotational speed of 3000 r / min centrifugation 10 min, the supernatant obtained is Sloanea leaf extract.
[0045] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.10mol/L的硝酸铁溶液10.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0045] 4. Take 40ml Sloanea leaf extract iron nitrate solution was added to remove oxygen 10.0mL 0.10mol / L, and mixed to obtain a black gel, to obtain a water soluble nano-iron.
[0046] 实施例7: [0046] Example 7:
[0047] 1.将采集的猴欢喜树叶在80°C干燥36h，粉碎后得到猴欢喜树叶粉末。 [0047] 1. The collection of monkey rejoice dried leaves in 80 ° C 36h, after grinding to obtain a powder monkey joy leaves.
[0048] 2.称取5.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在50° C热水中水浴120分钟。 [0048] 2. Weigh 5.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 50 ° C water bath for 120 minutes.
[0049] 3.将加热后的猴欢喜树叶溶液以转速为4000 r/min离心5 min，得到的上清液即为猴欢喜树叶提取液。 [0049] 3. The joy leaf monkey heated solution at a rotational speed of 4000 r / min centrifugation 5 min, the supernatant obtained is Sloanea leaf extract.
[0050] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.10mol/L的硝酸铁水溶液10.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0050] 4. Take 40ml Sloanea leaf extract iron nitrate solution was added to remove oxygen 10.0mL 0.10mol / L, and mixed to obtain a black gel, to obtain a water soluble nano-iron.
[0051] 实施例8: [0051] Example 8:
[0052] 1.将采集的猴欢喜树叶在70°C干燥72h，粉碎后得到猴欢喜树叶粉末。 [0052] 1. The collection of monkey rejoice dried leaves in 70 ° C 72h, after grinding to obtain a powder monkey joy leaves.
[0053] 2.称取5.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在50° C热水中水浴75分钟。 [0053] 2. Weigh 5.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 50 ° C water bath for 75 minutes.
[0054] 3.将加热后的猴欢喜树叶溶液以转速为4000 r/min离心5 min，得到的上清液即为猴欢喜树叶提取液。 [0054] 3. The joy leaf monkey heated solution at a rotational speed of 4000 r / min centrifugation 5 min, the supernatant obtained is Sloanea leaf extract.
[0055] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.1OmoI/L的硝酸铁水溶液10.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0055] 4. Take 40ml Sloanea leaf extract was added to remove oxygen 0.1OmoI / iron nitrate solution 10.0mL L, and mixed to obtain a black gel, to obtain a water soluble nano-iron.
[0056] 实施例9: [0056] Example 9:
[0057] 1.将采集的猴欢喜树叶在70°C干燥72h，粉碎后得到猴欢喜树叶粉末。 [0057] 1. The collection of monkey rejoice dried leaves in 70 ° C 72h, after grinding to obtain a powder monkey joy leaves.
[0058] 2.称取5.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在60° C热水中水浴30分钟。 [0058] 2. Weigh 5.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 60 ° C water bath for 30 minutes.
[0059] 3.将加热后的猴欢喜树叶溶液以转速为4000 r/min离心5 min，得到的上清液即为猴欢喜树叶提取液。 [0059] 3. The joy leaf monkey heated solution at a rotational speed of 4000 r / min centrifugation 5 min, the supernatant obtained is Sloanea leaf extract.
[0060] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.1OmoI/L的硝酸铁水溶液10.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0060] 4. Take 40ml Sloanea leaf extract was added to remove oxygen 0.1OmoI / iron nitrate solution 10.0mL L, and mixed to obtain a black gel, to obtain a water soluble nano-iron.
[0061] 实施例10: [0061] Example 10:
[0062] 1.将采集的猴欢喜树叶在80°C干燥36h，粉碎后得到猴欢喜树叶粉末。 [0062] 1. The collection of monkey rejoice dried leaves in 80 ° C 36h, after grinding to obtain a powder monkey joy leaves.
[0063] 2.称取5.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在60° C热水中水浴30分钟。 [0063] 2. Weigh 5.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 60 ° C water bath for 30 minutes.
[0064] 3.将加热后的猴欢喜树叶溶液以转速为4000 r/min离心5 min，得到的上清液即为猴欢喜树叶提取液。 [0064] 3. The joy leaf monkey heated solution at a rotational speed of 4000 r / min centrifugation 5 min, the supernatant obtained is Sloanea leaf extract.
[0065] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.1OmoI/L的硝酸铁水溶液10.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0065] 4. Take 40ml Sloanea leaf extract was added to remove oxygen 0.1OmoI / iron nitrate solution 10.0mL L, and mixed to obtain a black gel, to obtain a water soluble nano-iron.
[0066] 实施例11: [0066] Example 11:
[0067] 1.将采集的猴欢喜树叶在70°C干燥72h，粉碎后得到猴欢喜树叶粉末。 [0067] 1. The collection of monkey rejoice dried leaves in 70 ° C 72h, after grinding to obtain a powder monkey joy leaves.
[0068] 2.称取5.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在70° C热水中水浴30分钟。 [0068] 2. Weigh 5.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 70 ° C water bath for 30 minutes.
[0069] 3.将加热后的猴欢喜树叶溶液以转速为3000 r/min离心10 min，得到的上清液即为猴欢喜树叶提取液。 [0069] 3. The joy leaf monkey heated solution at a rotational speed of 3000 r / min centrifugation 10 min, the supernatant obtained is Sloanea leaf extract.
[0070] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.1OmoI/L的硫酸亚铁水溶液10.0 mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0070] 4. Take 40ml Sloanea leaf extract was added to remove oxygen 0.1OmoI / L aqueous solution of ferrous sulfate 10.0 mL, mixing, to obtain a black gel, to obtain a water soluble nano-iron.
[0071] 实施例12: [0071] Example 12:
[0072] 1.将采集的猴欢喜树叶在70°C干燥72h，粉碎后得到猴欢喜树叶粉末。 [0072] 1. The collection of monkey rejoice dried leaves in 70 ° C 72h, after grinding to obtain a powder monkey joy leaves.
[0073] 2.称取5.00 g猴欢喜树叶粉末，加入锥形瓶中，加入100.0mL除氧的超纯水得到猴欢喜树叶溶液，瓶口密封，在70° C热水中水浴30分钟。 [0073] 2. Weigh 5.00 g Sloanea leaves powder, add conical flask, 100.0mL oxygen in ultrapure water to obtain a solution Sloanea leaves, bottle sealed, hot water at 70 ° C water bath for 30 minutes.
[0074] 3.将加热后的猴欢喜树叶溶液以转速为3000 r/min离心10 min，得到的上清液即为猴欢喜树叶提取液。 [0074] 3. The joy leaf monkey heated solution at a rotational speed of 3000 r / min centrifugation 10 min, the supernatant obtained is Sloanea leaf extract.
[0075] 4.取40ml猴欢喜树叶提取液，加入除去氧气的0.1OmoI/L的氯化铁水溶液10.0mL，混合均匀，得到黑色的凝胶，即得到水溶性纳米铁。 [0075] 4. Take 40ml Sloanea leaf extract was added to remove oxygen 0.1OmoI / 10.0mL L of ferric chloride aqueous solution, mixed to obtain a black gel, to obtain a water soluble nano-iron.
[0076] 实施例1-12所制得的水溶性纳米铁的透射电镜照片如图1所示，由此电镜照片说明实施例1-12确实制得了纳米铁。 1-12 prepared water soluble nano-iron TEM photograph [0076] Example 1, whereby the electron micrographs illustrate Example 1-12 really prepared nanoscale iron implement. 另外，取实施例1-12所制备的水溶性纳米铁1.6 mL加Λ 100.0 mL含500.0 mg/L溴百里酚蓝水溶液中，并加入H2O2 2.0 mL (30%)混匀后在震荡器上进行震荡，降解时间为2、5、8、10、13、15、18、20 min后取出样品对溴百里酚蓝浓度进行测量，得到随着降解时间的变化溴百里酚蓝浓度的变化情况如图2所示。 Also, take Example 1-12 prepared water-soluble nano iron plus Λ 100.0 mL 1.6 mL containing 500.0 mg / L bromothymol blue solution and added after the shaker on H2O2 2.0 mL (30%) and mix conduct shocks, degradation time 2,5,8,10,13,15,18,20 min after the sample was taken to bromothymol blue concentration was measured to obtain a change with bromothymol blue concentration variation degradation time the case shown in Figure 2. 同时取100.0 mL含500.0 mg/L溴百里酚蓝水溶液，并加入H202 2.0 mL(30%)混匀后形成空白对照组(不加入水溶性纳米铁溶液)，混匀后在震荡器上震荡，降解时间为2、5、8、10、13、15、18、20 min后取出样品对溴百里酚蓝浓度进行测量，同样得到随着降解时间的变化溴百里酚蓝浓度的变化情况如图2所示。 While taking 100.0 mL containing 500.0 mg / L bromothymol blue solution and add H202 2.0 mL (30%) formed the control group (without the addition of a water soluble nano-iron solution) after mixing, after mixing the shock on the shaker The degradation time of 2,5,8,10,13,15,18,20 min after samples were removed for bromothymol blue concentration was measured to obtain the same time changes with the change of degradation bromothymol blue concentration of cases As shown in Figure 2. 由图2可知，加入水溶性纳米铁的溴百里酚蓝水溶液中溴百里酚蓝浓度随着降解时间的加长，而大幅度降低；而在未加入水溶性纳米铁的空白对照组中，溴百里酚蓝水溶液中溴百里酚蓝浓度随着降解时间的加长，变化不大。 Figure 2 shows, a water soluble nano-iron aqueous bromothymol blue bromothymol blue concentration with longer degradation time, and significantly reduced; and if not, a water soluble nano-iron blank control group, bromothymol blue bromothymol blue solution in concentration with longer degradation time, little change. 由此说明，实施例1-12所制备的水溶性纳米铁具有优秀的催化作用，对降解溴百里酚蓝具有很强催化效果。 Which shows that the water-soluble nano iron prepared in Example 1 to 12 have excellent catalytic degradation of bromothymol blue has a strong catalytic effect.
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