CN110182790A - The method of glucan synthesizing graphite alkene quantum dot - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 21
- 230000002194 synthesizing effect Effects 0.000 title claims abstract description 9
- 229920001503 Glucan Polymers 0.000 title claims 2
- 239000002096 quantum dot Substances 0.000 title description 10
- 229910002804 graphite Inorganic materials 0.000 title 1
- 239000010439 graphite Substances 0.000 title 1
- -1 graphite alkene Chemical class 0.000 title 1
- 229920002307 Dextran Polymers 0.000 claims abstract description 30
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims abstract description 25
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 239000007864 aqueous solution Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 229910021389 graphene Inorganic materials 0.000 claims description 14
- 239000000243 solution Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 238000005119 centrifugation Methods 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 6
- 239000002253 acid Substances 0.000 abstract description 4
- 238000001035 drying Methods 0.000 abstract description 4
- 239000007800 oxidant agent Substances 0.000 abstract description 4
- 239000000047 product Substances 0.000 abstract description 4
- 239000006228 supernatant Substances 0.000 abstract description 4
- 238000001308 synthesis method Methods 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 2
- 230000001590 oxidative effect Effects 0.000 abstract description 2
- 241000233866 Fungi Species 0.000 abstract 1
- 238000009776 industrial production Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 7
- 239000002086 nanomaterial Substances 0.000 description 5
- 239000011521 glass Substances 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 239000008103 glucose Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000012805 post-processing Methods 0.000 description 2
- 239000002243 precursor Substances 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 239000002028 Biomass Substances 0.000 description 1
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 description 1
- 238000001241 arc-discharge method Methods 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 238000005906 dihydroxylation reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000012377 drug delivery Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000000383 hazardous chemical Substances 0.000 description 1
- 238000000608 laser ablation Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000012286 potassium permanganate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000011540 sensing material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
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- C01B2204/00—Structure or properties of graphene
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Abstract
本发明提供了一种采用葡聚糖合成石墨烯量子点的绿色方法，合成方法仅以葡聚糖和去离子水为原料，不添加任何其它强酸、强氧化剂，在高压水热釜中按一定比例混合葡聚糖和去离子水后，调节鼓风干燥箱到适宜温度进行水热反应，所得产物用高速离心机离心分离得到上层清液，即石墨烯量子点水溶液。本发明所使用的原料葡聚糖广泛存在于真菌及植物中，是一种自然可持续资源，合成石墨烯量子点的过程简单，绿色环保，有利于工业化生产。同时，所制备的石墨烯量子点具有良好的水溶性、荧光稳定性和生物相容性，有望应用于生物领域。
The invention provides a green method for synthesizing graphene quantum dots using dextran. The synthesis method only uses dextran and deionized water as raw materials without adding any other strong acid or strong oxidant. After mixing dextran and deionized water in proportion, adjust the blast drying oven to a suitable temperature for hydrothermal reaction, and centrifuge the obtained product with a high-speed centrifuge to obtain a supernatant, that is, an aqueous solution of graphene quantum dots. The raw material dextran used in the present invention widely exists in fungi and plants, and is a natural and sustainable resource. The process of synthesizing graphene quantum dots is simple, green and environmentally friendly, and is conducive to industrial production. At the same time, the prepared graphene quantum dots have good water solubility, fluorescence stability and biocompatibility, and are expected to be applied in the biological field.
Description
技术领域technical field
本发明涉及采用葡聚糖合成石墨烯量子点的绿色方法，属于纳米材料领域。更具体指仅以葡聚糖与去离子水为原料，不添加其他强酸、强氧化剂，采用水热法制备石墨烯量子点的方法。制备的石墨烯量子点具有良好的荧光性能、水溶性和生物相容性，有望应用于生物领域。The invention relates to a green method for synthesizing graphene quantum dots with dextran, and belongs to the field of nanometer materials. More specifically, it refers to a method for preparing graphene quantum dots by a hydrothermal method using only dextran and deionized water as raw materials without adding other strong acids and strong oxidants. The prepared graphene quantum dots have good fluorescence properties, water solubility and biocompatibility, and are expected to be applied in the biological field.
背景技术Background technique
碳纳米材料，包括碳纳米管、富勒烯、石墨烯，在纳米技术、生物传感和药物传递等领域有着广泛的应用前景。近年来，石墨烯量子点（GQDs）作为一种新型的碳纳米材料在生物成像和生物传感领域得到了广泛的研究和应用。与半导体量子点形成鲜明对比的是，石墨烯量子点是一种低毒、高化学稳定性、低环境危害的荧光纳米材料。目前，合成GQDs的方法主要有电弧放电法、激光烧蚀法、电化学合成法、微波合成法、水热合成法等，其中，水热路线被认为是一种直接、有效的方法。另外，大自然提供了几乎无限的资源，而利用天然生物质制备纳米材料的路线在较多领域均取得了一定的进展，在能源材料、传感材料、功能材料等领域均展示了潜在的应用前景。因此，葡聚糖作为一种自然的多糖，有望为合成性能良好的纳米材料提供一种新的前驱体。在此，我们开发了一种过程简单、后处理方便、绿色环保的水热处理葡聚糖制备石墨烯量子点的工艺路线。Carbon nanomaterials, including carbon nanotubes, fullerenes, and graphene, have broad application prospects in nanotechnology, biosensing, and drug delivery. In recent years, graphene quantum dots (GQDs), as a new type of carbon nanomaterial, have been widely studied and applied in the fields of bioimaging and biosensing. In stark contrast to semiconductor quantum dots, graphene quantum dots are fluorescent nanomaterials with low toxicity, high chemical stability, and low environmental hazards. At present, the methods for synthesizing GQDs mainly include arc discharge method, laser ablation method, electrochemical synthesis method, microwave synthesis method, hydrothermal synthesis method, etc. Among them, the hydrothermal route is considered to be a direct and effective method. In addition, nature provides almost unlimited resources, and the route of using natural biomass to prepare nanomaterials has made some progress in many fields, showing potential applications in energy materials, sensing materials, functional materials and other fields prospect. Therefore, dextran, as a natural polysaccharide, is expected to provide a new precursor for the synthesis of nanomaterials with good properties. Here, we developed a process route for preparing graphene quantum dots by hydrothermally treating dextran with simple process, convenient post-processing, and environmental protection.
发明内容Contents of the invention
以葡聚糖和去离子水为原料，在高压反应釜中进行混合后，在高温高压下进行水热反应，然后产物用高速离心机分离，即可得到石墨烯量子水溶液。本发明所述的采用葡聚糖合成石墨烯量子点的绿色方法，得到的石墨烯量子点平均粒径2.74nm，紫外吸收在225nm与283nm有特征峰。Using dextran and deionized water as raw materials, after mixing in a high-pressure reactor, a hydrothermal reaction is carried out under high temperature and high pressure, and then the product is separated by a high-speed centrifuge to obtain a graphene quantum water solution. According to the green method of using dextran to synthesize graphene quantum dots in the present invention, the obtained graphene quantum dots have an average particle size of 2.74nm, and ultraviolet absorption has characteristic peaks at 225nm and 283nm.
所述的采用葡聚糖合成石墨烯量子点的绿色方法，包括以下制备步骤：The described green method adopting dextran to synthesize graphene quantum dots comprises the following preparation steps:
（1）将葡聚糖溶于去离子水中，搅拌分散至完全溶解，得到葡聚糖水溶液；(1) Dissolve dextran in deionized water, stir and disperse until completely dissolved to obtain an aqueous solution of dextran;
（2）将步骤（1）中得到的葡聚糖水溶液加入高压反应釜，加压条件下进行水热反应得到棕黄色溶液；(2) adding the dextran aqueous solution obtained in step (1) into a high-pressure reactor, and performing a hydrothermal reaction under pressure to obtain a brown-yellow solution;
（3）将步骤（2）中得到的棕黄色溶液经离心分离出上层棕黄色透明液体，即为石墨烯量子点的水溶液。(3) The brown-yellow solution obtained in step (2) is centrifuged to separate the upper layer of brown-yellow transparent liquid, which is the aqueous solution of graphene quantum dots.
所述的步骤（1）中去离子水与葡聚糖的质量比范围为10 ~ 250：10 ~ 25。In the step (1), the mass ratio of deionized water to dextran ranges from 10 to 250:10 to 25.
所述的步骤（2）中高压反应釜内压力为6-12Mpa，稳定为160-220℃，进行水热反应2-15h后出料。In the step (2), the internal pressure of the high-pressure reactor is 6-12Mpa, and the temperature is stable at 160-220°C, and the hydrothermal reaction is carried out for 2-15h before discharging.
所述的步骤（3）中离心分离转速为3000-15000r/min。In the step (3), the centrifugal separation speed is 3000-15000r/min.
所述的采用葡聚糖合成石墨烯量子点的绿色方法，仅以葡聚糖与去离子水为原料，不添加其他强酸、强氧化剂。合成石墨烯量子点的工艺流程简单、绿色无污染，可大规模生产，制备的石墨烯量子点具有良好的水溶性、荧光稳定性和生物相容性，可应用于生物领域。The green method of using dextran to synthesize graphene quantum dots only uses dextran and deionized water as raw materials, without adding other strong acids and strong oxidants. The process of synthesizing graphene quantum dots is simple, green and pollution-free, and can be produced on a large scale. The prepared graphene quantum dots have good water solubility, fluorescence stability and biocompatibility, and can be applied in the biological field.
本发明与其它方法的优势在于，创造性地将自然可持续资源-葡聚糖用作合成石墨烯量子点的前驱体。整个制备过程仅使用葡聚糖和去离子水做为反应原料，在高温高压下通过水热反应有效地制备出石墨烯量子点。反应无需添加强酸和氧化剂，也无需使用任何含金属离子的试剂（如高锰酸钾等）。所得产物除石墨烯量子点之外，只含有水和碳化物沉淀，因此后处理极为方便。该反应的机理主要是葡聚糖在水热条件下水解，生成小分子的葡萄糖，然后葡萄糖分子互相发生脱羟基缩环化的反应，生成石墨烯量子点。该反应条件简单可控，适合大规模的制备出工业化的石墨烯量子点产品。The advantage of the present invention and other methods lies in the creative use of natural sustainable resource - dextran as a precursor for the synthesis of graphene quantum dots. The whole preparation process only uses dextran and deionized water as reaction raw materials, and graphene quantum dots are effectively prepared by hydrothermal reaction under high temperature and pressure. The reaction does not need to add strong acid and oxidant, and does not need to use any reagents containing metal ions (such as potassium permanganate, etc.). The obtained product only contains water and carbide precipitation except graphene quantum dots, so post-processing is extremely convenient. The mechanism of this reaction is mainly that dextran is hydrolyzed under hydrothermal conditions to generate small molecule glucose, and then the glucose molecules undergo dehydroxylation and condensation reaction with each other to generate graphene quantum dots. The reaction conditions are simple and controllable, and are suitable for large-scale preparation of industrialized graphene quantum dot products.
附图说明Description of drawings
图1为实施例1所制备的石墨烯量子点的XRD谱图。Fig. 1 is the XRD spectrogram of the graphene quantum dot prepared in embodiment 1.
图2为实施例1所制备的石墨烯量子点的TEM照片。Fig. 2 is the TEM picture of the graphene quantum dot prepared in embodiment 1.
图3为实施例1所制备的石墨烯量子点的紫外吸收光谱图。Fig. 3 is the ultraviolet absorption spectrogram of the graphene quantum dot prepared in embodiment 1.
图4为实施例1所制备的石墨烯量子点的荧光光谱图。Fig. 4 is the fluorescence spectrogram of the graphene quantum dot prepared in embodiment 1.
具体实施方式Detailed ways
实施例1Example 1
取25mg的葡聚糖，于50mL烧杯中，加入25mL去离子水，用玻璃棒搅拌至充分溶解；将该溶液转移至50mL高压水热釜中，放置鼓风干燥箱，调节温度为180℃，反应8h；将反应得到的棕黄色溶液离心，速度为10000r/min，用吸管分离上清液，即可得到石墨烯量子点溶液，产率可达61%。Take 25mg of dextran, add 25mL of deionized water to a 50mL beaker, and stir with a glass rod until fully dissolved; transfer the solution to a 50mL high-pressure hydrothermal kettle, place in a blast drying oven, and adjust the temperature to 180°C. React for 8 hours; centrifuge the brown-yellow solution obtained from the reaction at a speed of 10,000 r/min, and separate the supernatant with a pipette to obtain a graphene quantum dot solution with a yield of up to 61%.
实施例2Example 2
取30mg的葡聚糖，于50mL烧杯中，加入50mL去离子水，用玻璃棒搅拌至充分溶解；将该溶液转移至100mL高压水热釜中，放置鼓风干燥箱，调节温度为170℃，反应11h；将反应得到的棕黄色溶液离心，速度为8000r/min，用吸管分离上清液，即可得到石墨烯量子点溶液，产率可达55%。Take 30mg of dextran, add 50mL of deionized water to a 50mL beaker, and stir with a glass rod until fully dissolved; transfer the solution to a 100mL high-pressure hydrothermal kettle, place in a blast drying oven, and adjust the temperature to 170°C. React for 11 hours; centrifuge the brown-yellow solution obtained from the reaction at a speed of 8000 r/min, and separate the supernatant with a pipette to obtain a graphene quantum dot solution with a yield of up to 55%.
实施例3Example 3
取50mg的葡聚糖，于50mL烧杯中，加入40mL去离子水，用玻璃棒搅拌至充分溶解；将该溶液转移至100mL高压水热釜中，放置鼓风干燥箱，调节温度为190℃，反应6h；将反应得到的棕黄色溶液离心，速度为12000r/min，用吸管分离上清液，即可得到石墨烯量子点溶液，产率可达57%。Take 50mg of dextran, add 40mL of deionized water to a 50mL beaker, and stir with a glass rod until fully dissolved; transfer the solution to a 100mL high-pressure hydrothermal kettle, place in a blast drying oven, and adjust the temperature to 190°C. React for 6 hours; centrifuge the brown-yellow solution obtained from the reaction at a speed of 12000 r/min, and separate the supernatant with a pipette to obtain a graphene quantum dot solution with a yield of up to 57%.
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| CN113277499A (en) * | 2021-05-07 | 2021-08-20 | 优彩科技(湖北)有限公司 | Preparation method and application of silicon-nitrogen co-doped graphene quantum dot |
| CN113277499B (en) * | 2021-05-07 | 2022-11-08 | 优彩科技(湖北)有限公司 | Preparation method and application of silicon-nitrogen co-doped graphene quantum dots |
| CN114836760A (en) * | 2022-05-16 | 2022-08-02 | 大连民族大学 | A kind of preparation method of rust remover containing graphene quantum dot corrosion inhibitor |
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Application publication date: 20190830 |