Synthesis method and application of molybdenum trioxide quantum dots

文档序号:1281823 发布日期:2020-08-28 浏览:32次 中文

阅读说明:本技术 一种三氧化钼量子点的合成方法及其应用 (Synthesis method and application of molybdenum trioxide quantum dots ) 是由 陈晓勇 张泽宇 洪应平 梁庭 贾平岗 雷程 李晨 于 2020-04-29 设计创作,主要内容包括:本发明涉及一种三氧化钼量子点的合成方法及其应用,其合成方法为S1、将高锰酸钾,溶于水中,调节pH值到酸性;S2、向步骤S1中获得的溶液加入二硫化钼,水浴加热至反应完全;S3、将步骤S2中获得的溶液,离心,取上清液加入无水乙醇、过氧化氢溶液,于反应釜中进行水热反应,得到三氧化钼量子点。三氧化钼量子点的应用为用于Cr<Sub>2</Sub>O<Sub>7</Sub><Sup>2-</Sup>的检测。本发明的合成方法不用表面活性剂,合成的量子点中钼的价态高,导致制备的量子产率高,合成的MoO<Sub>3</Sub>量子点可以用于Cr<Sub>2</Sub>O<Sub>7</Sub><Sup>2-</Sup>的快速和高灵敏度的检测,其对Cr<Sub>2</Sub>O<Sub>7</Sub><Sup>2-</Sup>的检测限宽为0~3μmol/L,检出限可达59nmol/L。(The invention relates to a synthesis method and application of molybdenum trioxide quantum dots, wherein the synthesis method comprises the steps of S1, dissolving potassium permanganate in water, and adjusting the pH value to acidity; s2, adding molybdenum disulfide into the solution obtained in the step S1, and heating in a water bath until the reaction is completed; s3, centrifuging the solution obtained in the step S2, taking supernate, adding absolute ethyl alcohol and hydrogen peroxide solution into the supernate, and carrying out hydrothermal reaction in a reaction kettle to obtain the molybdenum trioxide quantum dots. Application of molybdenum trioxide quantum dots to Cr 2 O 7 2‑ Detection of (3). The synthesis method of the invention does not use a surfactant, andthe valence of molybdenum in the prepared quantum dots is high, so that the prepared quantum yield is high, and the synthesized MoO 3 Quantum dots can be used for Cr 2 O 7 2‑ Rapid and highly sensitive detection of Cr 2 O 7 2‑ The detection limit width of the probe is 0-3 mu mol/L, and the detection limit can reach 59 nmol/L.)

1. A method for synthesizing molybdenum trioxide quantum dots is characterized by comprising the following steps:

s1, dissolving potassium permanganate in water, and adjusting the pH value to acidity by using acid;

s2, adding molybdenum disulfide into the solution obtained in the step S1, and heating in a water bath until the reaction is completed;

s3, centrifuging the solution obtained in the step S2, taking supernate, adding absolute ethyl alcohol and hydrogen peroxide solution into the supernate, and carrying out hydrothermal reaction in a reaction kettle to obtain the molybdenum trioxide quantum dots.

2. The method of claim 1, wherein in step S1, sulfuric acid is used for the adjustment, and the pH value is 1-2.

3. The synthesis method according to claim 1, wherein in step S1, the concentration of potassium permanganate is 1-9 g/L.

4. The synthesis method according to claim 1, wherein in step S2, the added amount of molybdenum disulfide is 50-100% of the mass of potassium permanganate.

5. The method of synthesis of claim 1, wherein in step S2, the water bath heating is at 25 ℃ or room temperature.

6. The method of synthesis according to claim 1, wherein in step S3, the centrifugation is performed at 8000 xg for 10-30 min.

7. The method of synthesis of claim 1, wherein in step S3, the supernatant is mixed with a solution of anhydrous ethanol and hydrogen peroxide in a ratio of ethanol: hydrogen peroxide: adding the supernatant at a ratio of 5:3:2, wherein the concentration of the hydrogen peroxide is 30%; the constant temperature of the reaction kettle is 180-200 ℃, and the hydrothermal reaction time is 8-10 h.

8. Application of molybdenum trioxide quantum dots or molybdenum trioxide quantum dots synthesized by adopting method of any one of claims 1 to 7 in Cr2O7 2-Application in concentration or content detection.

9. The use of claim 9, wherein the molybdenum trioxide quantum dots are used in Cr2O7 2-The concentration detection method comprises the following steps: dissolving molybdenum trioxide quantum dots by adopting absolute ethyl alcohol, and respectively adding Cr with different known concentrations2O7 2-As a standard solution, wherein the fluorescence intensity emitted by the standard solution at 440nm is measured when the excitation wavelength of the standard solution is 370nm and the concentration of Cr is 0-3 mu mol/L2O7 2-The fluorescence intensity measured at a concentration of 0 is recorded as I0,Cr2O7 2-For recording fluorescence intensity measured at different concentrationsFor I, calculate (I)0-I)/I0A value of (d); known Cr2O7 2-Is the abscissa, and is calculated corresponding to I (I)0-I)/I0The value of (d) is taken as the ordinate, and a standard curve is drawn; for the measured fluorescence intensity of the sample to be measured, finding out the point corresponding to the fluorescence intensity corresponding to the standard curve to obtain the Cr of the sample2O7 2-The concentration of (c).

10. The method of claim 9 for Cr2O7 2-The application of the molybdenum trioxide quantum dots in concentration or content detection is characterized in that the concentration of the molybdenum trioxide quantum dots is 0.0002-0.4 mol/L, and Cr with different known concentrations is2O7 2-The standard solution is a standard solution with concentration increased by 2-4 times based on 0.0005-0.15 mu mol/L.

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