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A production method of a fiber-loaded catalyst prepared by a microfluidic one-step method and its application in p-aminophenol

A production method and microfluidic technology, applied in catalytic reactions, chemical instruments and methods, catalyst activation/preparation, etc., can solve problems such as short mixing time, achieve catalytic activity, increase utilization rate, and more catalytic active points Effect

Active Publication Date: 2021-04-06
苏州艾博特化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The morphology and particle size of the catalyst have a great influence on the catalytic activity of the catalyst. The preparation methods of commonly used supported catalysts include impregnation method, ion exchange method, chemical reduction method, chemical vapor deposition method, precipitation method, etc., but microfluidic control Compared with conventional synthesis methods, the technology has the advantages of higher mass transfer and heat transfer speed, shorter mixing time, continuous reaction and less reagent consumption, etc., and has great advantages in realizing the controllable shape and size of material particles , but there are not many reports on the preparation and application of supported fiber catalysts synthesized by microfluidic one-step synthesis for p-aminophenol

Method used

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  • A production method of a fiber-loaded catalyst prepared by a microfluidic one-step method and its application in p-aminophenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] (1) Slowly add the three-dimensional chitosan sol with a particle size of 40-80nm into the graphene oxide solution of 3 mg / L, stir ultrasonically, evaporate the solvent and concentrate to obtain a carrier sol with a solid content of 50%, wherein the shell in the carrier sol The mass ratio of polysaccharide to graphene oxide is 50:3.

[0029] (2) the SO4 of the nickel nitrate loading of 1wt% 2- / MXOY solid superacid powder and bronsted acidic ionic liquid are mixed uniformly to obtain a loaded suspension with a solid content of 10%.

[0030] (3) Using the coaxial microfluidic channel network as a device, the carrier solution is loaded into the innermost syringe, the load solution is loaded into the outermost syringe, and the hydrazine hydrate reducing agent is added to the middle syringe, and the injection pumps are used to separate Control the flow rate of the carrier solution to be 0.1ml / min, the flow rate of the outermost injector to be 0.4ml / min, and the flow rate o...

Embodiment 2

[0032] (1) Slowly add the three-dimensional chitosan sol with a particle size of 40-80nm into the graphene oxide solution of 5mg / L, stir ultrasonically, evaporate the solvent and concentrate to obtain a carrier sol with a solid content of 70%, wherein the shell in the carrier sol The mass ratio of polysaccharide to graphene oxide is 80:10.

[0033] (2) the SO4 of the nickel nitrate loading of 2wt% 2- / MXOY solid superacid powder and bronsted acidic ionic liquid are mixed uniformly to obtain a loaded suspension with a solid content of 20%.

[0034](3) Using the coaxial microfluidic channel network as a device, the carrier solution is loaded into the innermost syringe, the load solution is loaded into the outermost syringe, and the hydrazine hydrate reducing agent is added to the middle syringe, and the injection pumps are used to separate Control the flow rate of the carrier solution to be 0.2ml / min, the flow rate of the outermost injector to be 0.5ml / min, and the flow rate of...

Embodiment 3

[0036] (1) Slowly add the three-dimensional chitosan sol with a particle size of 40-80nm into the graphene oxide solution of 4 mg / L, stir ultrasonically, evaporate the solvent and concentrate to obtain a carrier sol with a solid content of 55%, wherein the shell in the carrier sol The mass ratio of polysaccharide to graphene oxide is 60:5.

[0037] (2) the SO4 of the nickel nitrate load of 1.5wt% 2- / MXOY solid superacid powder and bronsted acidic ionic liquid were mixed evenly to obtain a loaded suspension with a solid content of 13%.

[0038] (3) Using the coaxial microfluidic channel network as a device, the carrier solution is loaded into the innermost syringe, the load solution is loaded into the outermost syringe, and the hydrazine hydrate reducing agent is added to the middle syringe, and the injection pumps are used to separate Control the flow rate of the carrier solution to be 0.15ml / min, the flow rate of the outermost injector to be 0.45ml / min, and the flow rate of...

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Abstract

The invention provides a production method of a supported fiber-type catalyst prepared by a microfluidic one-step method and its application in p-aminophenol. The three-dimensional chitosan sol is slowly added to the graphene oxide solution to obtain the carrier sol; the nickel nitrate The loaded solid superacid powder and the bronsted acidic ionic liquid are evenly mixed to obtain the loaded suspension; the coaxial microfluidic channel network is used as a device to inject the carrier solution, the loaded solution and the reducing agent into the syringe respectively, and the solution is controlled by a numerically controlled syringe pump. The flow rate of the carrier sol forms a stable thick shape in the channel, and the three are mixed and cured by the heating device, and the fibers are collected and further dried to obtain the supported fiber catalyst prepared by the microfluidic one-step method; The loaded fiber-type catalyst prepared by microfluidic one-step method and nitrobenzene are heated and hydrogenated for reaction, stirred until the reaction is completed, the reaction liquid is poured out and the catalyst is filtered to obtain p-aminophenol.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a production method of a fiber-loaded catalyst prepared by a microfluidic one-step method and its application in p-aminophenol. Background technique [0002] p-aminophenol, also known as p-hydroxyaniline, is an important organic intermediate widely used in medicine, dyes, pesticides, antioxidants, photosensitive materials, etc. There are many preparation methods of p-aminophenol. According to its raw materials, there are mainly the following process routes: p-nitrophenol method, p-nitrochlorinated benzene method, nitrobenzene method, phenol method and other process routes. Among them, phenol nitrosation method The products are complex, highly toxic, demanding operating conditions, large consumption of organic solvents, low yield, difficult product separation and solvent recovery, and serious environmental pollution; phenol and aniline coupling methods have relativel...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/02B01J31/06B01J31/26B01J35/06B01J35/10B01J37/04B01J37/16C07C213/02C07C215/76
CPCC07C213/02B01J31/0292B01J31/06B01J31/26B01J37/04B01J37/16B01J2231/641B01J35/58B01J35/60C07C215/76
Inventor 胡海威
Owner 苏州艾博特化工有限公司
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