Preparation method of anhydrous (Ba (tmhd)2)
A technology of diketone barium and diketone, which is applied in the field of preparation of anhydrous β-diketone barium precursor salt, can solve the problems of accelerated reaction speed, slow reaction speed and low efficiency of the contact area, and achieve shortened reaction time and short reaction time , the effect of high reaction efficiency
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Embodiment 1
[0012] Add 6.85 grams of powdered metal barium and 700 milliliters of dry n-hexane successively in a 1000 milliliter three-necked flask equipped with a condenser tube, a drying tube and a nitrogen gas inlet conduit. The purity of the metal barium is 99.99%, and the particle size is 2200 mesh. After passing nitrogen for 20 minutes, mix 18.4 grams of 2,2,6,6-tetramethyl-3,5-heptanedione (β-diketone, tmhd) and 184 milliliters of n-hexane evenly, and pass through the normal pressure dropping funnel Slowly add it dropwise into a three-necked flask, and stir vigorously at 50°C under an anhydrous and oxygen-free airtight condition. After 15 hours, the metal barium powder completely disappears and the reaction ends; The solvent was distilled off, vacuum dried in a vacuum oven at 60°C to obtain a white powdery anhydrous β-diketone barium precursor salt (Ba(tmhd) 2 ), the yield is 98%.
[0013] Such as figure 1 Shown, by infrared spectroscopic analysis (IR, cm -1 ) to characterize th...
Embodiment 2
[0015] Add 1.37 grams of powdered metal barium and 150 milliliters of dry n-hexane successively in a 250 milliliter three-neck flask equipped with a condenser tube, a drying tube and a nitrogen inlet conduit. The purity of the metal barium is 99.5%, and the particle size is 100 mesh. After passing nitrogen for 20 minutes, mix 3.68 grams of 2,2,6,6-tetramethyl-3,5-heptanedione (β-diketone, tmhd) and 40 milliliters of n-hexane evenly, and pass through the normal pressure dropping funnel Slowly add it dropwise into a three-neck flask, and stir vigorously at 60°C under an anhydrous and oxygen-free airtight condition. After 48 hours, the metal barium powder completely disappears, and the reaction ends; The solvent was distilled off, vacuum dried in a vacuum oven at 60°C to obtain a white powdery anhydrous β-diketone barium precursor salt (Ba(tmhd) 2 ), the yield is 96%.
[0016] The resulting Ba(tmhd) 2 The infrared spectrum analysis result is the same as embodiment 1.
Embodiment 3
[0018] Add 3.425 grams of powdered metal barium and 350 milliliters of dry n-hexane successively in a 500 milliliter three-neck flask equipped with a condenser tube, a drying tube and a nitrogen inlet conduit. The purity of the metal barium is 99.99%, and the particle size is 1000 mesh. After passing nitrogen for 20 minutes, mix 3.68 grams of 2,2,6,6-tetramethyl-3,5-heptanedione (β-diketone, tmhd) and 40 milliliters of n-hexane evenly, and pass through the normal pressure dropping funnel Slowly add it dropwise into a three-neck flask, and stir vigorously at 40°C under an anhydrous and oxygen-free airtight condition. After 20 hours, the metal barium powder completely disappears, and the reaction ends; The solvent was distilled off, vacuum dried in a vacuum oven at 60°C to obtain a white powdery anhydrous β-diketone barium precursor salt (Ba(tmhd) 2 ), the yield is 96%. The resulting Ba(tmhd) 2 The infrared spectrum analysis result is the same as embodiment 1.
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