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Continuous flow microreactor, manufacturing method and application

A micro-reactor and catalytic reaction technology, which is applied in chemical instruments and methods, chemical/physical/physical-chemical reactors, carboxylic acid nitrile preparation, etc., can solve problems such as poor temperature uniformity, many by-products, and slow heating rate

Active Publication Date: 2020-12-11
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The continuous flow microreactor can not only realize the accurate control of the reaction temperature, but also solve the problems of slow heating rate, high energy consumption, poor heat transfer efficiency, etc. of the traditional electric heating reactor, as well as the poor temperature uniformity of the reaction system. Causes many by-products and other problems, and can improve the activity of the catalyst

Method used

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  • Continuous flow microreactor, manufacturing method and application
  • Continuous flow microreactor, manufacturing method and application
  • Continuous flow microreactor, manufacturing method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] Example 1: Preparation of 3D printed microreactor unit

[0054] According to the set formula (vol.%): nickel zinc ferrite (46.0%), polyacrylate (2.3%), polyvinyl alcohol (2.0%), polyethylene glycol and glycerin are both (3.5%) , the rest is deionized water, add polyacrylate, polyethylene glycol, polyvinyl alcohol and glycerin to deionized water, stir well and get a premixed solution, add nickel zinc ferrite powder to the beaker and stir, After all the powder is added, put it on the mixer and stir for 8 hours, then add hydrochloric acid to adjust the pH value of the mud to 7, and put it in a tank for standby; the air pump pressure of the printing equipment is 5bar, the diameter of the extrusion needle is 0.6mm, and the printing speed is 20 mm s -1 , When the slice layer thickness is 0.54mm, the printed samples of nano-ferrite microreactors with different apertures can be obtained, and after 24 h drying, 900 o C above sintering to obtain the microreactor unit.

[0055]...

Embodiment 2

[0056] Embodiment 2: ZIF-8 grows in microreactor unit channel

[0057] APTES was used to assist the growth of ZIF-8 in the microreactor unit channel. After adding 0.05mmol APTES to 20ml of toluene solution, put 2g of washed and dried microreactor unit into it, 110 o C was refluxed for 24h, the cooled sample was thoroughly washed with methanol, and o C vacuum dried for 24 h for later use; Zn(NO 3 ) 2 ·6H 2 O (3mmol) and 2-methylimidazole (12mmol) were dissolved in 30ml and 20ml of anhydrous methanol respectively, until the solid was completely dissolved, the modified microreactor unit was put into the methanol solution of imidazole, and the Zn salt solution Quickly add in the imidazole solution under stirring, transfer the mixture to a 100mL polytetrafluoro reactor after stirring for 5min, seal it, and o C for 24 h. After cooling to room temperature, the mother liquor was removed from the mixture, and the microreactor was soaked and washed 4 times with anhydrous methanol....

Embodiment 3

[0058] Embodiment 3: the making and usage of microreactor unit

[0059] In the first step, the catalytic reaction unit obtained in Example 2 is superimposed on the lower end of the quartz tube as a catalytic reaction zone, and a microreactor unit with a certain height unloaded catalyst is superimposed on it as a preheating section, and a temperature sensor is implanted in the two-section contact surface. Lay glass beads with an outer diameter of 2.5mm on the quartz tube, and connect a double-hole rubber stopper at the end, one of which is connected to nitrogen, and the other is connected to a Y-shaped mixer through a hose, and the two inlets of the mixer are connected to the constant flow pump , the storage tank, and the hose are connected, and the outlet port of the quartz tube is connected to the product collection pool for the collection of reaction products;

[0060] In the second step, the quartz tube assembled with the microchannel reactor unit is placed in the magnetic ...

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Abstract

The invention relates to a continuous flow microreactor, a manufacturing method and an application. The continuous flow microreactor comprises a pipe body, one end of the pipe body communicates with afeeding pipe and an air inlet pipe, the other end of the pipe body is open, a microreactor unit is arranged in the pipe body, and a plurality of micron-sized pore channels are distributed in the microreactor unit; the microreactor unit is made of a nano ferrite magnetic material, the microreactor unit comprises a preheating section and a catalytic reaction section which are distributed in the length direction of the pipe body, and the catalytic reaction section is close to the open end of the pipe body; and an induction coil sleeves the pipe body, two ends of the induction coil are electrically connected with a high-frequency power supply, and the magnetic heating effect of nano magnetic particles in an external alternating magnetic field has the advantages of high efficiency, easiness incontrol, targeting and the like, and has the advantages of good temperature uniformity, low energy consumption, high efficiency, simple structure, convenience in use, easiness in system integration and scale amplification and the like. High-purity and high-yield synthesis of a target product in a fine chemical product process can be realized.

Description

technical field [0001] The invention relates to a continuous flow microreactor, a manufacturing method and its application, in particular to a continuous flow microreactor, a manufacturing method and its application in the production process of medicines and fine chemicals, and belongs to the technical field of microreactors and their preparation and application. Background technique [0002] In the past decade, continuous catalytic reactions have become one of the most active research areas in the fields of pharmaceuticals and fine chemicals. During the continuous reaction process, only one operation step and one purification step are required, which can greatly improve the synthesis efficiency. However, the traditional stirred tank reactor has problems such as low reaction efficiency, serious waste of resources, lack of environmental protection, and difficulty in scaling up due to mass transfer limitations, making it difficult to transform into industrial scale production. ...

Claims

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Application Information

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IPC IPC(8): B01J19/00C07C253/30C07C255/41C07C45/45C07C49/84
CPCB01J19/0093C07C253/30C07C45/45C07C255/41C07C49/84Y02P20/141
Inventor 高朋召吴迪刘小磐吴登明
Owner HUNAN UNIV
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