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Application of supported L-proline catalyst in continuous flow chemistry

A catalyst, proline technology, applied in catalytic reactions, physical/chemical process catalysts, organic chemistry, etc., can solve the problems affecting the normal progress of continuous flow synthesis, clogging, etc.

Inactive Publication Date: 2021-08-06
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, introducing very small particles of supported catalyst directly into the flow reactor, even with a high-power pump, may cause serious clogging problems with prolonged operation, thereby affecting the normal progress of continuous flow synthesis.

Method used

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  • Application of supported L-proline catalyst in continuous flow chemistry
  • Application of supported L-proline catalyst in continuous flow chemistry
  • Application of supported L-proline catalyst in continuous flow chemistry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A kind of continuous flow catalytic reaction device structure of the present embodiment is as follows figure 1 shown. A high-precision micro-syringe pump is used to pump the reaction solution through the columnar reactor at a certain flow rate. The reactor is filled with a certain mass of L-Proline / MWCNTs catalyst (Cat) and additional carrier neutral alumina, the particle size is 100-200 mesh, the mass of neutral alumina is 20 grams, and the fluid containing the product is continuously received at the liquid outlet .

[0037] 15g of L-proline was dissolved in ultrapure water (30mL) and sonicated for 30min to prepare a solution, then 1g of multi-walled carbon nanotubes (MWCNTs) was added to the above solution and stirred at room temperature for 12h. Then, the obtained solid catalyst was washed with water (3 times) by means of centrifugation (5000rpm), and the collected black precipitate was vacuum-dried overnight at 80° C. to obtain the L-proline supported by multi-wal...

Embodiment 2

[0044] In Example 1, keeping the volume and concentration of the reaction solution constant, the flow rate of the reaction solution was doubled to 5mL / h, and the collected product yield was 90.3%.

Embodiment 3

[0046] In embodiment 2, keep adding reaction solution volume and flow velocity constant, increase the concentration of p-nitrobenzaldehyde in the reaction solution to be 0.08mol / L, 0.2mol / L respectively, collect the product yield that obtains at liquid flow outlet They are 78.6% and 56.7% respectively.

[0047] In above-mentioned example 1-3, through comprehensive comparative analysis, can obtain that adding catalytic component is 3.0gCat / 20gAl 2 o 3 , the concentration of the reaction solution is 0.04mol / L, the volume of the reaction solution added each time is 5mL, and the flow rate of the reaction solution pumped into the syringe pump is 5mL / h, which can continuously obtain the product of more than 90% yield.

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Abstract

The invention discloses an application of a supported L-proline catalyst in a continuous flow reaction. The catalytic component comprises an L-proline catalyst and an additional carrier in the reaction container, and the catalytic component is fixed in a columnar reactor. The supported L-proline catalyst designed by the invention is widely applied to various types of continuous flow reactions, and in the process of applying the supported L-proline catalyst to the continuous flow reactions, catalytic components are fixed in a reactor and do not flow out along with products, so that the loss of the catalyst is prevented, the separation step of the catalyst is omitted, and the utilization efficiency and the service life of the catalyst are improved. The wide applicability and compatibility of the composite catalyst in different reaction and solvent systems are also shown.

Description

technical field [0001] The invention specifically relates to a solid-loaded L-proline catalyst used in the continuous flow Mannich, Knoevenagel research reaction, which has wide applicability and compatibility. Background technique [0002] In recent decades, the continuous flow system has developed into an innovative synthesis technology. Its application in the laboratory synthesis and production of fine chemicals and pharmaceuticals not only improves the selectivity, safety and sustainability of chemical production , and speed up the development of new drugs and new functional materials. Different from the traditional flask reaction, the continuous flow system has significant advantages in the innovation of catalytic technology. At the technical level, the biggest advantage is to achieve large-scale preparation by increasing the size of the tower reactor or filling the heterogeneous catalyst for a long time, and another advantage of the continuous flow system is that it h...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/04C07C67/343C07C221/00B01J8/06C07C225/16C07C69/618
CPCB01J31/04C07C221/00C07C67/343B01J8/06B01J2208/00805B01J2208/024B01J2231/346B01J2231/4283C07C225/16C07C69/618
Inventor 张延华黄胜陈虹宇
Owner NANJING UNIV OF TECH
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