Preparation method of penta-member plane square chalcogenide metal cluster compound functional molecular crystal
A technology of planar square and functional molecules, which is applied in the field of preparation of pentanuclear planar square chalcogenide metal cluster functional molecular crystals, can solve the problems of restricting development and practical application, low synthesis yield, harsh reaction conditions, etc., and achieve super The effect of strong light limitation performance, mild process conditions, and simple raw materials
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[0014] In conjunction with the accompanying drawings, the preparation method of the pentanuclear planar square chalcogenide metal cluster functional molecular crystal of the present invention comprises the following steps:
[0015] 1.1 Put hydrogen sulfide into the ammonia solution of sodium molybdate or tungstic acid to react, and the product is filtered and vacuum-dried to obtain ammonium tetrathiomolybdate or ammonium tetrathiotungstate;
[0016] 1.2 Add the cuprous halide to the pyridine solvent, stir until the cuprous halide is completely dissolved, and prepare a solution of the cuprous halide pyridine adduct;
[0017] 1.3 Add the ammonium tetrathiotungstate or ammonium tetrathiomolybdate obtained in step 1.1 to the solution of cuprous halide pyridine adduct obtained in step 1.2, stir until completely dissolved and then filter; among them, The molar ratio of ammonium tungstate or ammonium tetrathiomolybdate to cuprous halide is 1:3.5-4.5;
[0018] 1.4 Add methanol, ethan...
Embodiment 1
[0020] Embodiment 1: The preparation method of the pentanuclear planar square chalcogenide metal cluster functional molecular crystal of the present invention comprises the following steps:
[0021] In the first step, hydrochloric acid aqueous solution is added to ferrous sulfide to react, and the generated gas passes through a safety bottle equipped with deionized water, and then passes through a drying tower equipped with molecular sieves to obtain hydrogen sulfide gas;
[0022] The second step is to add tungstic acid into the ammonia solution and stir to obtain the ammonia solution of tungstic acid;
[0023] The third step is to pass the hydrogen sulfide prepared in the first step into the ammonium tungstate solution prepared in the second step to react, filter and dry to obtain the compound tetrathioammonium tungstate, and the reaction condition is 60°C 8 hours;
[0024] In the fourth step, add 7.6 grams of cuprous iodide to 200 milliliters of pyridine after dehydration a...
Embodiment 2
[0033] The preparation method of the pentanuclear planar square chalcogenide metal cluster functional molecular crystal of the present invention comprises the following steps:
[0034] In the first step, hydrochloric acid aqueous solution is added to ferrous sulfide to react, and the generated gas passes through a safety bottle equipped with deionized water, and then passes through a drying tower equipped with molecular sieves to obtain hydrogen sulfide gas;
[0035] In the second step, sodium molybdate is added to the ammonia solution and stirred to obtain the ammonia solution of sodium molybdate;
[0036] In the third step, the hydrogen sulfide obtained in the first step is passed to the sodium molybdate ammonia solution prepared in the second step to react through suction filtration and drying to obtain the compound ammonium tetrathiomolybdate, and the reaction conditions are room temperature 0.5 hours;
[0037] In the fourth step, add 7.6 grams of cuprous iodide to 200 mi...
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