IODINE DOPED BISMUTHYL CARBONATE NANOSHEET AND MOLYBDENUM DISULFIDE MODIFIED CARBON NANOFIBER COMPOSITES, PREPARATION METHOD AND APPLICATION THEREOF

20190127883 ยท 2019-05-02

    Inventors

    Cpc classification

    International classification

    Abstract

    Iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites, preparation method and its application in wastewater treatment are disclosed. Bismuth citrate and sodium carbonate as precursors, sodium carbonate as a precipitating agent, dispersed in a mixed solution of water and ethylene glycol, sodium iodide as a iodine source, nano carbon fiber membrane act as the carrier, to synthesis carbon fiber membrane that modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets; then sodium molybdate and thioacetamide as precursors, dispersed in water to react to obtain iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites. The composite material synthesized through a series of steps exhibit excellent photocatalytic activity for the degradation of Rhodamine B and can be recycled for many times. And this invention has the advantages of simple preparation process, easy recovery and multiple use, etc., and has industrial application prospect in water pollution treatment.

    Claims

    1. A preparation method of iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites, characterized in comprising the following steps: (1) dispersing nano carbon fiber membrane, bismuth citrate, sodium iodide and sodium carbonate in a mixed solution of water and ethylene glycol to obtain a kind of nano carbon fiber material modified by iodine doped bismuthyl carbonate; (2) dispersing sodium molybdate and thioacetamide in water, then adding said nano carbon fiber material modified by iodine doped bismuthyl carbonate, reacting to obtain iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites.

    2. The preparation method of iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites according to claim 1, wherein in step (1), using an N,N-dimethylformamide solution of polyacrylonitrile as raw material, obtaining polyacrylonitrile fiber membrane by electrospinning method, then calcining to obtain nano carbon fiber membrane; the diameter of said nano carbon fiber membrane is 0.5 m.

    3. The preparation method of iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites according to claim 2, wherein in step (1), the calcination conditions are calcination for 3 to 6 hours under argon, the calcination temperature is 400 to 600 C., the heating rate is 2 to 15 C. per minute.

    4. The preparation method of iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites according to claim 1, wherein in step (1), the mass ratio of said bismuth citrate, sodium carbonate, sodium iodide and said nanocarbon fiber membrane is (132 to 134):(38 to 40):100:(8 to 10), after dispersing nano carbon fiber membrane, bismuth citrate, sodium iodide and sodium carbonate in a mixed solution of water and ethylene glycol, waiting 2 to 4 hours to start the reaction, the reaction temperature is 150 to 180 C., and reaction time is 24 to 36 hours.

    5. The preparation method of iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites according to claim 1, wherein in step (2), the mass ratio of said sodium molybdate and thioacetamide is 1.2:1, dispersing said sodium molybdate and thioacetamide in water, after ultrasonic treatment for half an hour, adding said nano carbon fiber material modified by iodine doped bismuthyl carbonate, the reaction temperature is 180 to 250 C., reaction time is 6 to 8 hours.

    6. The preparation method of iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites according to claim 1, wherein in step (1), after the reaction is finished, the product is washed with water and ethanol respectively, and then vacuum-dried to obtain nano carbon fiber material modified by iodine doped bismuthyl carbonate; in step (2), the product is washed with water and ethanol respectively, and then vacuum-dried to obtain iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites.

    7. A preparation method of nano carbon fiber material modified by iodine doped bismuthyl carbonate, characterized in comprising the following steps: dispersing nano carbon fiber membrane, bismuth citrate, sodium iodide and sodium carbonate in a mixed solution of water and ethylene glycol to obtain a kind of nano carbon fiber material modified by iodine doped bismuthyl carbonate.

    8. The preparation method of nano carbon fiber material modified by iodine doped bismuthyl carbonate according to claim 7, wherein using an N,N-dimethylformamide solution of polyacrylonitrile as raw material, obtaining polyacrylonitrile fiber membrane by electrospinning method, then calcining to obtain nano carbon fiber membrane; the diameter of said nano carbon fiber membrane is 0.5 m, the mass ratio of said bismuth citrate, sodium carbonate, sodium iodide and said nanocarbon fiber membrane is (132 to 134):(38 to 40):100:(8 to 10), after dispersing nano carbon fiber membrane, bismuth citrate, sodium iodide and sodium carbonate in a mixed solution of water and ethylene glycol, waiting 2 to 4 hours to start the reaction, the reaction temperature is 150 to 180 C., and reaction time is 24 to 36 hours.

    9. A product prepared by the preparation method according to claim 1.

    10. (canceled)

    11. A product prepared by the preparation method according to claim 7.

    Description

    BRIEF DESCRIPTION OF THE DRAWINGS

    [0020] FIG. 1 is the SEM image of carbon nanofibers;

    [0021] FIG. 2 is the SEM image of carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets;

    [0022] FIG. 3 is the SEM image of carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets and MoS.sub.2 nanoflakes;

    [0023] FIG. 4 is the TEM image of carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets and MoS.sub.2 nanoflakes;

    [0024] FIG. 5 is the UV-vis DRS spectra of RhB solution photodegraded by carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets and MoS.sub.2 nanoflakes;

    [0025] FIG. 6 is cycling effect of the composites.

    [0026] FIG. 7 is comparison chart of the effect of photocatalytic degradation of Rhodamine B by several composites.

    DETAILED DESCRIPTION OF THE INVENTION

    Example 1

    [0027] Preparation of carbon nanofiber membrane. Specific steps are as follows:

    [0028] 1 g of polyacrylonitrile and 9 g of N, N-dimethylformamide are placed in a 20 ml glass bottle and stirred at room temperature for 5 hours until the polyacrylonitrile is completely dissolved and mixed well. Then the solution is added to the syringe and spun by electrospinning method, get a white polyacrylonitrile fiber membrane. The polyacrylonitrile fiber membrane is calcined for 5 hours at 500 C. with a heating rate of 10 C. per minute under argon protection, finally obtained a carbon nanofiber membrane having a diameter of 0.5 m; FIG. 1 is the SEM image of carbon nanofibers, it can be seen that the nanofibers with diameter of 0.5 m distributed evenly and the surface of them are smooth.

    [0029] Preparation of carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets. Specific steps are as follows:

    [0030] 0.8 g of bismuth citrate and 0.23 g of sodium carbonate are added to a mixed solution of 30 ml of water and 6 ml of ethylene glycol, sonicated for 5 minutes, stirred for half an hour, and further added 0.6 g of sodium iodide and stirred at room temperature for 2 hours hour. Then, the mixed precursor is transferred to a 50 mL Teflon-lined stainless reaction vessel together with 50 mg of carbon nanofibers. The reaction is carried out for 30 hours at 160 C. After the reaction is completed, the product is naturally cooled to room temperature and the product is taken out with tweezers. Washed with water and ethanol twice, respectively, and dried in vacuo; FIG. 2 the SEM image of carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets, the iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets are coated on the surface of carbon nanofibers evenly.

    Preparation of carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets and MoS.sub.2 nanoflakes. Specific steps are as follows:

    [0031] 24 mg of sodium molybdate and 20 mg of thioacetamide are dispersed in 30 ml of water, sonicated for half an hour and stirred at room temperature for half an hour, then the precursor is transferred to a 50 mL Teflon-lined stainless reaction vessel together with 50 mg of carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets to carry out the second reaction at 200 C. for 7 hours. After the reaction is over, the mixture is naturally cooled to room temperature, and the product is removed by tweezers and washed twice with water and ethanol, respectively, and dried in vacuo. FIG. 3 and FIG. 4 showed the SEM and TEM images of carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets and MoS.sub.2 nanoflakes, the structure of which can be seen that MoS.sub.2 nanoflakes modified to its surface uniformly.

    Example 2

    [0032] Photocatalytic degradation of Rhodamine B. Specific steps are as follows:

    [0033] 50 mg of a carbon nanofiber membranes modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets and MoS.sub.2 nanoflakes are added to a beaker containing a 50 ml (5 ppm) Rhodamine B solution, kept in a water bath at 25 C., stirred for 30 minutes in the dark, the photocatalyst composite and dye reached adsorption equilibrium, and then open the 300 W xenon lamp irradiation sampling every one minute for UV detection, the Rhodamine B solution could be degraded completely within 5 min. Photocatalyst composite material can be recycled many times, with good stability, the catalytic effect is still good the catalytic effect is still good recycling after 5 times; FIG. 5 is the UV-vis DRS spectra of RhB solution photodegraded by carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets and MoS.sub.2 nanoflakes; FIG. 6 is cycling of carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets and MoS.sub.2 nanoflakes photocatalyst for RhB degradation; FIG. 7 is comparison chart of the effect of photocatalytic degradation of Rhodamine B by several composites.

    [0034] The above analysis shows that the carbon nanofibers modified by iodine-doped Bi.sub.2O.sub.2CO.sub.3 nanosheets and MoS.sub.2 nanoflakes synthesized by the two-step hydrothermal reaction have good photocatalytic activity on the dye Rhodamine B; and can be recycled for many times and has the advantages that the preparation process is relatively simple, and the raw materials are easy to obtained, etc., has a prospect in the application of wastewater treatment.