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Production method for fiber-supported catalyst prepared by using microfluidic one-step method and application of fiber-supported catalyst to paraaminophenol

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, and achieve the effect of ensuring catalytic activity, large volume, and large specific surface area.

Active Publication Date: 2018-05-11
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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  • Production method for fiber-supported catalyst prepared by using microfluidic one-step method and application of fiber-supported catalyst to paraaminophenol

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, respectively, using a numerically controlled syringe pump. 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 t...

Embodiment 2

[0032] (1) Slowly add the three-dimensional chitosan sol with a particle size of 40-80nm into the graphene oxide solution of 5 mg / 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 o...

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 for a fiber-supported catalyst prepared by using a microfluidic one-step method and an application of the fiber-supported catalyst to paraaminophenol. The production method comprises the steps: slowly adding tree-dimensional chitosan sol into a graphene oxide solution to obtain carrier sol; uniformly mixing nickel nitrate supported solid superacid powderwith a bronsted acidic ionic liquid to obtain a supported suspension; respectively injecting the carrier sol, the supported suspension and a reducer into an injector by taking a coaxial microfluidic channel network as a device, controlling the flow speed of the solution by using a numerical control injection pump to make the carrier sol form a stable thick state in a channel, mixing the carrier sol, the supported suspension and the reducer, reducing and solidifying the mixture by using a heating device, collecting fibers to be further dried to obtain the fiber-supported catalyst prepared by using the microfluidic one-step method; and adding the fiber-supported catalyst prepared by using the microfluidic one-step method and nitrobenzene into a high-pressure reactor, carrying out heating fora hydrogenation reaction, carrying out stirring until the reaction is ended, and pouring out a reaction solution, and filtering the catalyst to obtain paraaminophenol.

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 Applications(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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