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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

Inactive Publication Date: 2011-12-07
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned patents load titanium-silicon molecular sieves on large particle carriers, which is easy to filter and recover catalyst particles, but the specific surface area and effective active sites of the catalysts are lost to varying degrees, which reduces the catalytic activity and selectivity of titanium-silicon molecular sieve catalysts.

Method used

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  • Preparation method of magnetically supported titanium-silicon molecular sieve catalyst and special impact ultrasonic micro-mixing reactor
  • Preparation method of magnetically supported titanium-silicon molecular sieve catalyst and special impact ultrasonic micro-mixing reactor
  • Preparation method of magnetically supported titanium-silicon molecular sieve catalyst and special impact ultrasonic micro-mixing reactor

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preparation example Construction

[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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Abstract

The invention relates to a method for producing a magnetic-loaded titanium silicon molecular sieve catalyst and special equipment of the method. The method for producing the magnetic-loaded titanium silicon molecular sieve catalyst comprises the following steps: colliding a mixture solution of soluble ferric salt and soluble nickel salt with ammonia spirit and then completely mixing under condition of sonic oscillation; obtaining ferrous acid nickel powder through a hydro-thermal reaction, and then mixing titanate hydrolysate with estersil hydrolystate to produce tianium silicon sol, and thenadding ferrous acid nickel powder into the tianium silicon sol, finally producing the magnetic-loaded titanium silicon molecular sieve catalyst through steps of hydro-thermal reaction, filtering, washing, drying and annealing. The colliding ultrasonic micro hybrid reactor used by the method is to install two nuzzles capable of colliding and mixing mixture solution mixed by soluble ferric salt andsoluble nickel salt with ammonia spirit in the reactor. in the invention, the magnetic is used nanoparticle as carrier; surface of the magnetic nanoparticle is cladded with a titanium silicon compound; high catalytic activity of the titanium silicon molecular sieve catalyst is maintained relatively, and solid-liquid separation is preformed under additional condition of magnetic field and a purpose of efficiently reclaiming the catalyst is achieved.

Description

[0001] technical field [0002] The invention relates to a method for preparing a magnetically separable magnetic-loaded titanium-silicon molecular sieve catalyst and special equipment for the preparation. Background technique [0003] Titanium silicate molecular sieve is a new type of catalyst material, which can be used in organic oxidation reactions involving hydrogen peroxide as a green oxidant, such as ammoxidation of cyclohexanone to cyclohexanone oxime, epoxidation of olefins, partial oxidation of alkanes, oxidation of alcohols And the hydroxylation of aromatic rings, etc. The environmental pollution problem of the traditional organic oxidation process is avoided. As a catalyst, titanium silicate molecular sieve has the advantages of high product selectivity, mild reaction conditions, economy, energy saving and environmental friendliness. [0004] The particle size range of the titanium-silicon molecular sieve catalyst is about 0.1-15 μm, and the smaller the particl...

Claims

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Application Information

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IPC IPC(8): B01J29/89B01J37/34C07C39/08C07C37/60
Inventor 李裕李俊华李军平王东琴
Owner ZHONGBEI UNIV
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