Polyacid Schiff base compound and its synthesis method and use
A technology of Schiff bases and compounds, applied in the field of polyacid Schiff base compounds and their synthesis, can solve the problems of lack of expansion and the like
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[0022] The preparation method of polyacid Schiff base compound of the present invention is characterized in that comprising the following steps:
[0023] A. Put the ammonium heptamolybdate solution in a container, add 3mol / L hydrochloric acid with a volume ratio of 15:1 to the ammonium heptamolybdate solution dropwise and stir at a speed of 800~1000 rpm 40~80min to obtain solution a;
[0024] B. Then the ammonium heptamolybdate solution with a volume ratio of 10:1 contains the newly prepared [Mn(salpn)(H 2 O)] 2 (ClO 4 ) 2 (0.1mol) methanol solution was added dropwise to solution a, and stirred at 800-1000 rpm for 20-40 minutes at 50-70°C to obtain solution b;
[0025] C. Put the solution b under 150~250W microwave radiation and heat it to 50°C to continue the reaction for 5~7 minutes, filter after cooling, and seal the filtrate with a thin film with small holes for slow volatilization for 7~10 days to obtain massive crystals. Rinse and dry naturally in the air to obtain ...
Embodiment 1
[0033] Add 0.17 g of ammonium heptamolybdate into 15 ml of deionized water and stir at 1000 rpm, then add 1 ml of 3 mol / L hydrochloric acid dropwise into the above solution and stir vigorously for 1 hour. Then, the newly prepared [Mn(salpn)(H 2 O)] 2 (ClO 4 ) 2 (0.90g, 1 mmol) (salpn) methanol solution 5ml was added dropwise to the above solution. After stirring in the Erlenmeyer flask at 60°C for 30 minutes, the resulting brown solution was subjected to 200W microwave irradiation for 6 minutes. After filtration, seal the filtrate with a membrane with small holes for slow evaporation. Blocky crystals were obtained after one week. Rinse with methanol and air dry.
Embodiment 2
[0035] The difference between this embodiment and embodiment 1 is that in step 1, 0.17 g of ammonium heptamolybdate is added to 10 ml of deionized water and stirred at a speed of 800 rpm, and other steps and parameters are the same as in embodiment 1 。
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