一种西柚皮提取液微波合成银纳米粒子的方法 One kind of liquid grapefruit Bark microwave synthesis method of silver nanoparticles

技术领域 FIELD

[0001] 本发明涉及银纳米粒子的制备方法，尤其是一种西柚皮提取液微波合成银纳米粒子的方法。 [0001] The present invention relates to the preparation of silver nanoparticles, especially a grapefruit skin extract liquid silver nanoparticles synthesized by microwave method.

背景技术 BACKGROUND

[0002] 近年来，贵金属纳米粒子因具有大的比表面积、良好的界面效应及小尺寸效应等独特的性能，在催化，光学，信息存储，表面增强拉曼散射，生物标记，影像和传感等方面具有潜在的应用前景；在所有的金属中，贵金属银有最好的电导率和热导率，而且银纳米颗粒具有很稳定的物理化学性能，在电学、光学和催化等众多方面具有十分优异的性能，现已广泛应用于陶瓷材料、环保材料、涂料、催化和表面增强拉曼散射技术等许多领域，应用前景广阔，因此引起研究者的广泛关注。 [0002] In recent years, because of the noble metal nanoparticles have unique properties larger than the surface area, good interface effect and the small size effect in catalysis, optics, information storage, surface-enhanced Raman scattering, biomarkers, imaging and sensing so has potential applications; in all metals, precious metals silver has the best electrical and thermal conductivity, and silver nanoparticles have a very stable physical and chemical properties, have in many respects very electrical, optical and catalytic excellent performance, is now widely used in ceramic materials, environmentally friendly materials, coatings, catalysis and surface-enhanced Raman scattering technique in many areas such as application prospects, thus causing much attention.

[0003] 化学法是目前最常用的银纳米粒子的制备方法，使用较多的还原剂有硼氢化钠、水合肼、二甲基甲酰胺等，然而这些化合物毒性强、污染严重，对人体以及环境都存在严重的危害，因此，纳米材料制备过程的“绿色化”就显得尤为重要，而用安全、环保的绿色溶剂、无毒无害的还原剂及高分子稳定剂代替传统的、有毒的有机化合物，就成为绿色化学的重要研究方向；同时，绿色合成的贵金属纳米材料具有很好的生物相容性，可以更方便、更容易地在制药和生物医学方面得到应用；Raveendran等用无毒可再生的化物质β-D-葡萄糖还原AgNO3溶液，可溶性淀粉作为保护剂，在氛气保护下40°C反应20h后可以得到银纳米溶胶(J.Am.Chem.Soc., 2003, 125, 13940) ;Sastry小组研究了天竺蔡叶子、印度楝树叶子的提取液对对氯金酸、银离子的还原作用，制备了金、银纳米粒子，并对其潜在应用进行了探究(J.Colloid Interface Sc1., 2004, 275, 496)。 [0003] Chemical methods are the most commonly used method for preparing silver nanoparticles, using more reducing agents include sodium borohydride, hydrazine hydrate, dimethylformamide, etc., these compounds are highly toxic, however, pollution, and on the human body there are serious environmental hazards, so the "green" manufacturing process of nano-materials is particularly important, with safe, environmentally friendly green solvents, non-toxic polymer reductant and stabilizer instead of the traditional, toxic organic compounds, has become an important research direction of green chemistry; at the same time, the green synthesis of noble metal nano-materials with good biocompatibility, can be more convenient and easier to get applications in the pharmaceutical and biomedical; Raveendran and other non-toxic substance β-D- glucose reduction and renewable AgNO3 solution, soluble starch as a protective agent, under the protection of 40 ° C reactive gas atmosphere can get silver nano sol (J.Am.Chem.Soc after 20h., 2003, 125, 13940); Sastry team studied Tianzhu Cai leaves, neem leaves to extract gold chloride reduction of silver ions, the preparation of gold, silver nanoparticles, and the inquiry (J.Colloid their potential applications Interface Sc1., 2004, 275, 496). Phlilip 等用可食用的蘑燕、蜂蜜合成了金、银纳米粒子(Molecular and Biomolecidar Spectroscopy., 2009.73,374);迄今为止，尚未见在西柚皮提取液存在下，微波法合成银纳米粒子的的报道。 Phlilip and other edible mushroom with Yan, honey synthesized gold, silver nanoparticles (Molecular and Biomolecidar Spectroscopy, 2009.73,374.); So far, has not been in the presence of grapefruit skin extract liquid, the microwave synthesis of silver nanoparticles reported.

发明内容 SUMMARY

[0004] 本发明涉及一种微波合成银纳米粒子的方法，尤其是一种西柚皮提取液微波合成银纳米粒子的方法。 [0004] The present invention relates to a microwave method for the synthesis of silver nanoparticles, especially a grapefruit skin extract liquid silver nanoparticles synthesized by microwave method.

[0005] 本发明通过以下步骤实现: [0005] The present invention is accomplished by the following:

(1)西柚皮提取液:西柚皮提取液是参照Sun课题组报道(Anal.Chem.2012, 84，5351 5357)的方法得到的，用水溶解定容至浓度为0.lg/L，即每升溶液中含有西柚皮提取物0.1g ; (1) liquid grapefruit Bark: Bark grapefruit Task Force report was a reference to the Sun (Anal.Chem.2012, 84,5351 5357) method was dissolved water to the concentration of 0.lg / L, That liter of solution containing grapefruit skin extract 0.1g;

(2)配制AgNO3水溶液(浓度为1.7〜8.5g/L)，再量取一定体积的西柚皮提取液与AgNO3溶液一起加入烧杯中(其中柚子皮提取液与AgNO3溶液的体积比为0.5〜1.2:1)，混合搅拌均匀后，转移至微波反应器中，在400〜700W功率下，反应3〜30 min。 (2) the preparation of AgNO3 solution (concentration 1.7~8.5g / L), and then take a certain amount of volume of grapefruit skin extract fluid and join beaker AgNO3 solution (which grapefruit skin extract liquid with AgNO3 solution volume ratio 0.5~ 1.2: 1), after uniform mixing, was transferred to a microwave reactor, at 400~700W power, reaction 3~30 min.

[0006] (3)反应结束后冷却至室温，用蒸馏水、乙醇分别离心、清洗产物多次后，得到银纳米粒子。 After cooling [0006] (3) The reaction to room temperature, centrifuged separately with distilled water, ethanol, after washing the product several times to obtain silver nanoparticles. [0007] (4 )利用X射线衍射仪(XRD )、透射电子显微镜(TEM)、紫外可见分光光度计(UV)对产物进行形貌结构分析。 [0007] (4) the use of X-ray diffraction (XRD), transmission electron microscopy (TEM), UV-visible spectrophotometer (UV) products were analyzed morphologies.

[0008] 与现有技术相比，本发明具有以下特点:采用天然绿色的柚子皮提取液作为银纳米粒子的还原剂和稳定剂，采用微波辅助的合成方法，简单快速，并且整个制备过程中无需添加任何化学试剂，制备过程具有绿色环保、便捷高效等优点，所制备的银纳米粒子的粒径为8-15nm，颗粒形貌均一，分散性良好；本方法合成的银纳米颗粒在生物、制药、催化等领域有良好应用前景。 [0008] Compared with the prior art, the present invention has the following characteristics: the use of natural grapefruit green bark was used as a reducing agent and stabilizer silver nanoparticles using microwave-assisted synthesis method, simple and fast, and the entire preparation process without adding any chemicals, the preparation process with green, convenient and efficient, etc., the particle size of the prepared silver nanoparticles 8-15nm, uniform particle morphology, good dispersion; this method for the synthesis of silver nanoparticles in biology, pharmaceutical, catalysis, etc. have a good prospect.

附图说明 Brief Description

[0009] 图1为制备的银纳米粒子的XRD衍射谱图，可以看出，通过本方法制备的银纳米粒子为纯相。 [0009] Figure 1 is a XRD diffraction pattern of the silver nanoparticles prepared, it can be seen, the silver nanoparticles prepared by the present method is a pure phase.

[0010] 图2为制备的银纳米粒子的TEM照片。 [0010] Figure 2 is a TEM photograph of the preparation of silver nanoparticles. 由照片中可以看出所制备的银纳米粒子的大小为8-15nm,粒径分布均勻,颗粒形貌均一，分散性良好。 As can be seen from the photograph the size of the silver nanoparticles prepared as 8-15nm, uniform particle size distribution, particle morphology uniformity, good dispersibility.

[0011] 图3为制备的银纳米粒子的紫外可见光谱图，由谱图中可以观察到在450cm—1出现了一个较宽的吸收峰，进一步证实了银纳米颗粒的成功制备。 [0011] Figure 3 is prepared by UV-Vis spectra of silver nanoparticles, the spectra can be observed in the 450cm-1 absorption peak appeared in a wider, further confirmed the success of the preparation of silver nanoparticles.

[0012] 实施例1 [0012] Example 1

量取30mL制备好的西柚皮提取液(0.lg/L)倒入至250mL烧杯中，再量取30mLAgN03溶液(3.4g/L)加入烧杯中，持续搅拌混合液20min后，将烧杯转移至微波反应器中，功率400W下反应30min ;反应完成后，将所得产物离心分离，并分别用蒸馏水、乙醇分别清洗3次后，得到银纳米粒子。 Measure 30mL prepared grapefruit skin extract solution (0.lg / L) was poured into 250mL beaker, and then weighed 30mLAgN03 solution (3.4g / L) added to the beaker, stirring was continued for 20min after the mixed solution, the beaker was transferred to a microwave reactor, 400W power under the reaction 30min; After completion of the reaction, the product obtained was centrifuged, and separately with distilled water, ethanol were washed three times, to obtain silver nanoparticles.

[0013] 实施例2 [0013] Example 2

量取36mL制备好的西柚皮提取液(0.lg/L)倒入至250mL烧杯中，再量取30mLAgN03溶液(1.7g/L)加入烧杯中，持续搅拌混合液20min后，将烧杯转移至微波反应器中，功率500W下反应20min ;反应完成后，将所得产物离心分离，并分别用蒸馏水、乙醇分别清洗3次后，得到银纳米粒子。 Measure 36mL prepared grapefruit skin extract solution (0.lg / L) was poured into 250mL beaker, and then weighed 30mLAgN03 solution (1.7g / L) added to the beaker, stirring was continued for 20min after the mixed solution, the beaker was transferred to a microwave reactor, at power 500W reaction 20min; After completion of the reaction, the product obtained was centrifuged, and distilled water, respectively, were washed three times in ethanol to give the silver nanoparticles.

[0014] 实施例3 [0014] Example 3

量取40mL制备好的西柚皮提取液(0.lg/L)倒入至250mL烧杯中，再量取50mLAgN03溶液(6.8g/L)加入烧杯中，持续搅拌混合液20min后，将烧杯转移至微波反应器中，功率700W下反应3min ;反应完成后，将所得产物离心分离，并分别用蒸馏水、乙醇分别清洗3次后，得到银纳米粒子。 Measure 40mL prepared grapefruit skin extract solution (0.lg / L) was poured into 250mL beaker, and then weighed 50mLAgN03 solution (6.8g / L) added to the beaker, stirring was continued for 20min after the mixed solution, the beaker was transferred to a microwave reactor, 700W power under reaction 3min; After completion of the reaction, the product obtained was centrifuged, and separately with distilled water, ethanol were washed three times, to obtain silver nanoparticles.

[0015] 实施例4 [0015] Example 4

量取20mL制备好的西柚皮提取液(0.lg/L)倒入至250mL烧杯中，再量取40mLAgN03溶液(8.5g/L)加入烧杯中，持续搅拌混合液20min后，将烧杯转移至微波反应器中，功率600W下反应12min ;反应完成后，将所得产物离心分离，并分别用蒸馏水、乙醇分别清洗3次后，得到银纳米粒子。 Measure 20mL prepared grapefruit skin extract solution (0.lg / L) was poured into 250mL beaker, and then weighed 40mLAgN03 solution (8.5g / L) added to the beaker, stirring was continued for 20min after the mixed solution, the beaker was transferred to a microwave reactor, at power 600W reaction 12min; After completion of the reaction, the product obtained was centrifuged, and separately with distilled water, ethanol were washed three times, to obtain silver nanoparticles.