Preparation method of magnetically supported titanium-silicon molecular sieve catalyst and special impact ultrasonic micro-mixing reactor
A titanium-silicon molecular sieve and catalyst technology, which is applied in the field of preparation of magnetically supported titanium-silicon molecular sieve catalyst, can solve the problems of reducing the catalytic activity and selectivity of the titanium-silicon molecular sieve catalyst, losing the specific surface area and effective active site of the catalyst, and achieving easy solid-liquid The effect of separation, good catalytic performance, and efficient recovery and reuse
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[0034] The impingement ultrasonic micro-mixing reactor used in the preparation method of the magnetic-supported titanium-silicon molecular sieve catalyst of the present invention includes a reactor 1, the upper part of the inner cavity of the reactor 1 is provided with two nozzles 2, and the lower part is equipped with an ultrasonic oscillator 3. The shell of the reactor 1 is higher than the ultrasonic oscillator 3 and lower than the nozzle 2. There is an overflow port 4. The nozzle 2 is connected to the two liquid storage tanks 5 through the pipeline. The pipeline is equipped with a delivery pump 6 and the overflow port 4 communicates with the liquid storage tank 7 through pipelines. A flow meter 8 and a control valve 9 are installed on the pipeline. The ultrasonic oscillator 3 is connected to the control board 10 .
[0035] In step (1), the mixed solution of soluble ferrous salt and soluble nickel salt is placed in one of the liquid storage tanks 5, and the ammonia solution...
Embodiment 1
[0038] Prepare a mixed solution with a concentration of 2.0 mol / L ferric nitrate and 1.0 mol / L nickel nitrate, and then prepare a solution with a concentration of 4.0 mol / L ammonia solution, put the two liquids in the liquid storage tank respectively, and pump them into the In reactor 1, the impact velocity of the liquid is 10m / s, and the pH of the reaction liquid is controlled to be 10 by adjusting the flow rate. Then move the reaction solution into a closed kettle for hydrothermal reaction. The hydrothermal temperature is 180°C and the hydrothermal time is 6 hours. After the reaction is completed, it is filtered, washed, and vacuum-dried at 120°C to obtain nickel ferrite powder.
[0039] Mix 208g (1.0mol) tetraethyl ammonium hydroxide (TAPOH) (20%wt) and 180g (10mol) deionized water, and stir at 18°C After 60 minutes, a silicon ester hydrolyzate was obtained. Then 3.4g (0.01mol) tetrabutyl titanate (TBOT), without adding isopropanol (IPA) solvent, 101.5g (0.05mol) tetraprop...
Embodiment 2
[0044] Prepare a mixed solution with a concentration of 1.0 mol / L ferric chloride and 0.5 mol / L nickel chloride, and then prepare a solution with a concentration of 2.0 mol / L ammonia solution, place the two liquids in the liquid storage tank respectively, and transport them by the delivery pump 6 Entering reactor 1, the impact velocity of the liquid is 3m / s, and the pH of the reaction liquid is controlled to be 12 by adjusting the flow rate. Then move the reaction liquid into a closed kettle for hydrothermal reaction. The hydrothermal temperature is 120°C and the hydrothermal time is 12 hours. After the reaction is completed, it is filtered, washed, and vacuum-dried at 150°C to obtain nickel ferrite powder.
[0045] Mix 208g (1.0mol) Tetraethyl Tetrasilicate (TEOS), 304.5g (0.3mol) Tetrapropylammonium Hydroxide (TAPOH) (20%wt) and 720g (40mol) deionized water, stir at 5°C After 30 minutes, a silicon ester hydrolyzate was obtained. Then 13.6g (0.04mol) tetrabutyl titanate (TBO...
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