China is rich in rare earth resources and has the largest reserves in the world. Acetylacetone rare earth complexes have wide application prospects in new luminescent materials, extraction chemistry, displacement reagents, especially stabilizers for plastic processing.
In the past, the production process of lanthanum acetyl acetonate adopts solution precipitation method and solution extraction method. These two methods not only consume solvent, but also affect the yield and the performance of the functional complex. In the actual production process, it is complicated and difficult to control, the product is unstable, and the consumption is high cost. And the by-products and waste water caused serious environmental pollution, not in line with today’s environmental trend.
Step 1 Add an appropriate amount of water to the reactor, heat and stir the water, and keep the water temperature at 20°-35°;
Step 2, stop stirring, and then add lanthanum oxide and catalyst in the water in turn, and then continue to stir evenly and keep the temperature of water at 30°-35°, when water, lanthanum oxide and catalyst violent reaction stop stirring, violent reaction after the completion of continuous stirring into hydration reactants;
Step 3, the hydration reactants were added to the reaction kettle of hydration reactants at the speed of 1 L/min, 2 L/min, 10 L/min, slowly stirring continuous drops of acetyl acetone, keep the temperature in the reaction kettle of hydration reactants at 40°-80°, until the end of dripping, heat preservation reaction 2-5 hours after the lanthanum acetyl acetone material;
Step 4, the lanthanum acetyl acetone material is cooled to room temperature, and then feeding filtration;
Step 5, put the filtered material into the oven, keep the oven temperature at 100°-150°, and dry for 136 hours. The dried material is crushed to obtain the finished product lanthanum acetyl acetone.
The mole ratio of water to lanthanum oxide in step 2 is 3.0:4.5 ~ 5.5:9.9.
Wherein, the stirring method in step 2 is clockwise stirring.
Wherein, the stirring method in step 3 is: when the hydration reactant is added at a speed of 1 L/min, the stirring method is clockwise stirring; When the hydration reactant is added at a speed of 2 L/min, the stirring method is counterclockwise stirring.
When the hydration reactant was added at a speed of 10 L/min, the stirring method was clockwise stirring for 3 min, then counterclockwise stirring for 3 min, alternating stirring.
The lanthanum acetyl acetone material in step 4 is cooled to room temperature 25°-30° and filtered by centrifuge.
The preparation method of lanthanum acetonate proposed in the invention takes lanthanum oxide and acetacetone as raw materials and adds catalyst to synthesize lanthanum acetonate. The reaction process is simple, the production cost is low, the production cost can be greatly reduced, and the product quality is stable. At the same time, the filtrate can be recycled for many times, no waste water discharge, in line with the national environmental protection requirements, but also save energy.