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A continuous flow hydrogenation reaction device, a selective reduction method for unsaturated aldehydes and ketones

A hydrogenation reaction and unsaturated technology, applied in chemical instruments and methods, chemical/physical processes, etc., can solve the problems of reduced product yield and inability to separate products in time, so as to achieve a small footprint, improve utilization, and increase output Effect

Active Publication Date: 2022-04-26
南京禾勤生物医药科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, aldehydes and ketone carbonyl groups can still be further reduced by palladium, especially in the batch hydrogenation process, the product obtained by the reaction cannot leave the reaction system in time, so the carbonyl group is further reduced by the catalyst and hydrogen, resulting in a decrease in product yield

Method used

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  • A continuous flow hydrogenation reaction device, a selective reduction method for unsaturated aldehydes and ketones
  • A continuous flow hydrogenation reaction device, a selective reduction method for unsaturated aldehydes and ketones
  • A continuous flow hydrogenation reaction device, a selective reduction method for unsaturated aldehydes and ketones

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Effect test

Embodiment 1

[0032] A continuous flow hydrogenation reactor, such as figure 1 As shown, it includes a reactor 1, a gas path control box 2, a liquid path control box 3, a preheating box 5 and an electrical control box 4. The top of the reactor 1 is provided with a gas path inlet and a liquid path inlet respectively, and the reactor 1 The bottom end is provided with a material outlet, and a catalyst bed is provided in the reactor; the gas path control box 2 is connected to the reactor 1 through the gas path inlet, and the liquid path control box 3 is connected to the reactor 1 through the gas path inlet. The inlet of the liquid path is communicated with the reactor pipe 1, the preheating box 5 is arranged at the inlet end of the reactor 1, the gas path control box 2, the liquid path control box 3 and the preheating box 5 are respectively connected with The electrical control box 4 is electrically connected, the parameter setting of the gas circuit control box 2, the liquid circuit control bo...

Embodiment 2

[0038] A selective reduction method for unsaturated aldehydes and ketones, based on the above-mentioned continuous flow hydrogenation reaction device, comprising: the flow rate of the hydrogen gas is controlled by the gas path control box, the flow rate of the hydrogen gas is controlled to be 100 SCCM, and the hydrogen gas is sent through the inlet of the gas path into the mixer;

[0039] The flow rate of the unsaturated aldehydes and ketones is controlled by the liquid path control box, and the flow rate of the unsaturated aldehydes and ketones is controlled to be 2mL / min, and is sent into the mixer through the inlet of the liquid path. The mass of the unsaturated aldehydes and ketones The concentration is 20%, and the solvent of unsaturated aldehydes and ketones is methanol;

[0040] The hydrogen and unsaturated aldehydes and ketones are mixed in the mixer and then enter the reaction tube. The volume of the reaction tube is 20mL, and flow through the catalyst bed. The cataly...

Embodiment 3

[0042] A selective reduction method for unsaturated aldehydes and ketones, based on the above-mentioned continuous flow hydrogenation reaction device, comprising: the flow rate of the hydrogen gas is controlled by the gas path control box, the flow rate of the hydrogen gas is controlled to be 10 SCCM, and the hydrogen gas is sent through the inlet of the gas path into the mixer;

[0043] The flow rate of the unsaturated aldehydes and ketones is controlled by the liquid circuit control box, and the flow rate of the unsaturated aldehydes and ketones is controlled to be 0.5mL / min, and is sent into the mixer through the inlet of the liquid circuit. The mass concentration is 5%, and the solvent is isopropanol;

[0044] The hydrogen and unsaturated aldehydes and ketones are mixed in the mixer and then enter the reaction tube. The volume of the reaction tube is 5mL, and flow through the catalyst bed. The catalyst bed height is 30cm. The mixture is separated to obtain a reduction pro...

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Abstract

The invention provides a continuous flow hydrogenation reaction device and a method for selectively reducing unsaturated aldehydes and ketones based on the device. The method includes: sending hydrogen and unsaturated aldehydes and ketones into the reactor, and flowing through the catalyst The bed layer is reacted to obtain a gas-liquid mixture, and the gas-liquid mixture is separated to obtain a reduction product. A complete gas-liquid-solid (catalyst) three-phase reaction system is constructed by using a continuous flow hydrogenation reaction device. The entire device occupies a small area, has a large output per unit space, and has a high safety factor. The device of the present invention is used for the selective reduction method of unsaturated aldehydes and ketones, and the continuous hydrogenation method can maximize the timely removal of the product from the catalytic system, avoiding further reduction of the carbonyl group in the product, and helping to further improve the selectivity of the reaction , improve the utilization rate of the catalyst, and increase the output per unit time.

Description

technical field [0001] The invention belongs to the technical field of reduction of unsaturated aldehydes and ketones, in particular to a continuous flow hydrogenation reaction device and a selective reduction method of unsaturated aldehydes and ketones based on the device. Background technique [0002] With the country's increasing requirements and supervision on safe production, the pharmaceutical and fine chemical industries are facing more and more safety challenges when using traditional batch autoclaves for hydrogenation reduction reactions. Therefore, the pharmaceutical and fine chemical industries urgently need to replace the original intermittent hydrogenation reduction process with a continuous hydrogenation reduction process. [0003] In the patent US3520934 published in 1970, the inventor also carried out the double bond selective reduction of cinnamaldehyde compounds with continuous flow equipment. Although this patent also adopts the continuous hydrogenation m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J8/06B01J8/00
CPCB01J8/001B01J8/06
Inventor 杨正浩
Owner 南京禾勤生物医药科技有限公司
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