1. Reagents and Instruments
Cyanuric Acid, nitric acid and methanol were purchased from Beijing Chemical Plant, and the purity of the reagents were all analytical grade.
T-1200 temperature-programmed tube furnace (Hefei Kejing); HR-200 high-pressure hydrothermal reactor (Shanghai Huotong Experimental Instrument Co., Ltd.); AV400 (400 MHz) superconducting nuclear magnetic resonance instrument (NMR, Bruker, Switzerland) Company); NEXUS870 Fourier Transform Infrared Spectrometer (FTIR, Thermoelectric Nicolis, USA); Vario EL-III Elemental Analyzer (Elementar, Germany); Bruker Smart APEXIICCD Single Crystal Diffractometer (Bruker, Switzerland); JNOECXP-201 Polarizing Microscope (Shanghai Precision Instrument Co., Ltd.).
2. Experimental method
Preparation of gt-C3N4: gt-C3N4 was prepared according to the method reported in the literature. Weigh 10.0 g of Cyanuric Acid and put it in a quartz boat, then place the quartz boat in a temperature-programmed tube furnace, replace the air in the tube with N2 gas, set the heating rate at 5 °C/min under N2 gas atmosphere, and heat up To 500 °C, keep the temperature at 500 °C, and calcined for 1 h. After the calcination was completed, it was cooled to room temperature to obtain 6.2 g of yellow powder gt-C3N4 with a mass yield of 62%.
Preparation of Cyanuric Acid: Add the prepared gt-C3N4 and 1 mol/L dilute nitric acid into a hydrothermal reaction kettle at a mass ratio of 1:10, and conduct a hydrothermal reaction at 140 °C for 2 h, and wait for the reaction kettle to cool to room temperature , and the reaction solution was evaporated to dryness to obtain a white crystal product.
3. Single crystal cultivation
Take a small amount of white crystals, dissolve them in aqueous methanol (V (methanol): V (water) = 1:1), then pour the solution into a 10 mL glass bottle, seal the bottle with a small-hole sealing film, and then Place the glass bottle in a cool place to allow the solvent to evaporate slowly to obtain massive colorless transparent crystals, and select crystals of appropriate size on the stage of a polarizing microscope for single crystal diffraction testing.