Solvent thermal constant-pressure synthesis method for controlling phase of carbon nitride material
A synthesis method and carbon nitride technology, applied in the directions of nitrogen and non-metallic compounds, nitrogen purification/separation, etc., can solve the problems of difficult preparation conditions, reduce the application value of products, damage the selectivity of the reaction process, etc., and achieve high application value. , to achieve the effect of low-cost mass synthesis and scale-up of preparation
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Embodiment 1
[0038] Example 1: First, metal sodium flakes were added to benzene, and after standing for 24 hours, it was distilled to remove water and oxygen. Then under the protection of nitrogen, weigh out the stoichiometric ratio of sodium azide (NaN 3 ) And trichloroazine (C 3 N 3 Cl 3 ) Put it into the autoclave, add 8ml of dried benzene and seal it. A pressure of 40 MPa was applied to the autoclave, and the temperature of the autoclave was controlled to rise to 220° C. at a rate of 0.01° C. / min, and the temperature and pressure was reacted for 8 hours and then naturally cooled to room temperature.
[0039] After the reaction, the benzene is firstly filtered off with suction, and then the product is washed successively with acetone, ethanol, and dilute hydrochloric acid to remove organic by-products and other impurities, and then the product is washed repeatedly with deionized water until the filtrate is neutral. Heating the product in vacuum to 60°C for drying, then graphite carbon nitr...
Embodiment 2
[0040] Example 2: As described in Example 1, the difference is that the reaction temperature is increased to 260°C.
Embodiment 3
[0041] Example 3: As described in Example 1, the difference is that the reaction temperature of the autoclave is increased to 300° C., trichloroazine is replaced by trimethylamine, and sodium azide is replaced by nitrogen trichloride.
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