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A kind of magnetic heteropolyacid catalyst and preparation method thereof

A technology of heteropolyacid and catalyst, which is applied in the field of magnetic heteropolyacid catalyst and its preparation, can solve the problems of unstable product performance, long reaction time, unfavorable scale-up production, etc., achieve good reusable effect, simple preparation process, improve The effect of utilization

Active Publication Date: 2020-03-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The above-mentioned methods for preparing heteropolyacid catalysts are all batch reaction synthesis methods, which have disadvantages such as long reaction time and unstable product performance during the preparation process, which is not conducive to large-scale industrial scale-up production of products

Method used

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  • A kind of magnetic heteropolyacid catalyst and preparation method thereof
  • A kind of magnetic heteropolyacid catalyst and preparation method thereof
  • A kind of magnetic heteropolyacid catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Dissolve 13.52g ferric chloride in 500ml water to form solution A, dissolve 10.51g trimesic acid in 500ml isopropanol to form solution B, dissolve 71.2g phosphotungstic acid in 500ml water to form solution C, and dissolve 5.8g Ferroferric oxide and 500ml of water were stirred and mixed to form solution D. Both solution A and solution B are sent to the microchannel reactor module I at a flow rate of 5 μl / min to generate MOFs seeds in situ. The reaction temperature of module I is 50°C, the pressure is 0.1MPa, and the residence time is 30s. The feed liquid containing MOFs seed crystals is generated in the microchannel reactor module II, and the flow rate is 10 μl / min; the solution C is sent into the microchannel reactor module II at a flow rate of 5 μl / min, and the solution D is sent at a flow rate of The reaction temperature is 70°C, the pressure is 0.1MPa, and the residence time is 60s. The product feed liquid is sent to the module III at a flow rate of 20 μl / min. Soluti...

Embodiment 2

[0045] Dissolve 135.29g of ferric chloride in 500ml of water to form solution A, dissolve 210.24g of trimesic acid in 500ml of isopropanol to form solution B, dissolve 712g of phosphotungstic acid in 500ml of water to form solution C, and dissolve 11.57g of tetra Ferric oxide was stirred and mixed with 500ml of water to form solution D. Both solution A and solution B are sent to the microchannel reactor module I at a flow rate of 200 μl / min to generate MOFs seeds in situ. The reaction temperature of module I is 70°C, the pressure is 1.0MPa, and the residence time is 180s. The feed liquid containing MOFs seed crystals is generated in the microchannel reactor module II, and the flow rate is 400 μl / min; the solution C is sent into the microchannel reactor module II at a flow rate of 100 μl / min, and the solution D is sent at a flow rate of The reaction temperature is 110°C, the pressure is 1.0MPa, and the residence time is 240s. The product feed liquid is sent to the module III at...

Embodiment 3

[0048] Dissolve 48.13g ferric chloride in 500ml water to form solution A, dissolve 100.34g trimesic acid in 500ml isopropanol to form solution B, dissolve 189.5g phosphotungstic acid in 500ml water to form solution C, and dissolve 8.9g Ferroferric oxide and 500ml of water were stirred and mixed to form solution D. Both solution A and solution B are sent to the microchannel reactor module I at a flow rate of 100 μl / min to generate MOFs seeds in situ. The reaction temperature of module I is 60°C, the pressure is 0.5MPa, and the residence time is 120s. The feed liquid containing MOFs seed crystals is generated in the microchannel reactor module II, and the flow rate is 200 μl / min; the solution C is sent into the microchannel reactor module II at a flow rate of 50 μl / min, and the solution D is sent at a flow rate of The reaction temperature is 100°C, the pressure is 0.5MPa, and the residence time is 120s. The product material liquid is sent to the module III at a flow rate of 300 ...

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Abstract

The invention relates to a magnetic heteropoly acid catalyst and a preparation method thereof. The preparation method comprises the following steps: (1) adding a metal precursor into an organic solvent to prepare a solution A; (2) adding an organic ligand into an organic solvent to prepare a solution B; (3) conveying the solution A and the solution B into a module I of a microchannel reactor at acertain flow velocity for in-situ production of MOFs seed crystals; (4) adding heteropoly acid into water, carrying out stirring to obtain a solution C, adding magnetic oxides into water, carrying outstirring to obtain a solution D and when feed liquid obtained in the step (3) is entering a module II, feeding the solution C and the solution D into the module II at a certain flow rate; and (5) when feed liquid obtained in the step (4) is entering a module III, feeding the solution B into the module III at a certain flow rate, and carrying out seed crystal-induced crystallization under ultrasonic conditions so as to produce the magnetic heteropoly acid catalyst. The method provided by the invention prepares the magnetic heteropoly acid catalyst by using the microchannel reactor under ultrasonic conditions, and is good in dispersibility of the heteropoly acid and magnetic substances, short in preparation time and high in production efficiency.

Description

technical field [0001] The invention relates to a heteropolyacid catalyst, in particular to a magnetic heteropolyacid catalyst and a preparation method thereof. Background technique [0002] Heteropolyacids are a class of polymetallic oxygen cluster compounds composed of pre-transition metals, whose structure can be regulated at the molecular or atomic level, and have a wide range of applications in the fields of catalysis, electrochemistry, biological science, and material science. Heteropolyacids are a class of excellent homogeneous catalytic materials, but they are difficult to separate from the liquid reaction medium. Therefore, scholars have been paying attention to the heterogeneous work of heteropolyacids. Due to the low specific surface area of ​​heteropolyacids, the study of heteropolyacid encapsulation carriers has important practical significance. At present, the more commonly used heteropolyacid encapsulation carriers include silica, activated carbon, silica ge...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07D307/46
CPCB01J27/188B01J31/2213B01J2531/0213B01J2531/0238B01J2531/842C07D307/46
Inventor 王海洋马蕊英张英王刚
Owner CHINA PETROLEUM & CHEM CORP