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Microchannel reactor-based cyano hydrolysis reaction method

A technology of microchannel reactor and hydrolysis reaction, applied in the direction of chemical instruments and methods, chemical/physical/physical chemical reactors, chemical/physical/physical chemical fixed reactors, etc., can solve the problem of difficult control of reactions and product purity Insufficient, low hydrolysis efficiency and other problems, to achieve the effect of increasing the hydrolysis rate, controlling the reaction time, and shortening the reaction time

Active Publication Date: 2018-05-29
大连微凯化学有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This type of reaction can usually be hydrolyzed relatively completely under alkaline conditions, but cannot be completely reacted under acidic conditions. Under normal temperature and pressure conditions, the hydrolysis time of the cyano group is relatively long, and the hydrolysis efficiency is low. Often the reaction cannot be carried out completely, and amides and The mixture of carboxylic acids makes the purity of the final product not enough, so it is necessary to increase the temperature and pH of the hydrolysis, especially under the commonly used alkaline conditions, increasing the temperature will violently produce gas, it is difficult to control the reaction, and the risk is relatively large; and The conventional reaction is incomplete under acidic conditions, and the amount of acid needs to be increased. These excess acids and bases also need to be neutralized, resulting in unnecessary waste and environmental pollution

Method used

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  • Microchannel reactor-based cyano hydrolysis reaction method
  • Microchannel reactor-based cyano hydrolysis reaction method
  • Microchannel reactor-based cyano hydrolysis reaction method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Preparation of β-alanine: 80% aminopropionitrile (technical grade) aqueous solution and 30% sodium hydroxide aqueous solution are used as raw materials.

[0038] Process operation steps:

[0039] 1) Connection of micro-reaction equipment: connect all equipment such as figure 1 Connection shown, using Starlam3000 microreactor;

[0040] 2) Debugging of micro-reaction equipment: Turn on the constant temperature circulator, set the temperature at 110°C, inject water into the micro-reaction equipment through a constant-flow pump, clean the internal pipeline of the micro-reaction equipment for 10 minutes, and open the back pressure valve at the same time to make the system back pressure 5.0MPa , Check whether the equipment has liquid leakage or air leakage, whether the temperature and pressure monitoring equipment are accurate, and proceed to the next step after everything is correct;

[0041] 3) Flow correction of constant flow pump: constant flow pump P01 and P02 use wate...

Embodiment 2

[0050] Preparation of 3-mercaptopropionic acid: use 95% 3-mercaptopropionitrile and 20% hydrochloric acid solution as raw materials without using solvent.

[0051] Process operation steps:

[0052] 1) The microreactor system is connected, and the debugging is the same as the above operation;

[0053] 2) Preparation: 5g of 3‐mercaptopropionitrile with a content of 95% is stored in storage tank V‐01, fed by pump P‐01; 10.92 g of 20% hydrochloric acid solution is placed in storage tank V‐02 The storage is fed by the pump P-02, the inlet temperature of the microreactor for the hydrochloric acid solution is 110°C, the outlet temperature of the microreactor is 114°C, and after an equilibrium time of 5 minutes, the reaction temperature rises to 115°C, and the feeding starts;

[0054] 3) Mix in the micro-mixer U, and complete the hydrolysis reaction through a tube reactor and a heat exchanger within 1 minute;

[0055] 4) The material after the reaction is completed enters the receiv...

Embodiment 3

[0060] Preparation of 7Α-double-condensed pyrrolidine-acetic acid: Pisicani intermediate 7A-double-condensed pyrrolidine-acetonitrile, 36% hydrochloric acid solution as raw material.

[0061] Process operation steps:

[0062] 1) The microreactor system is connected, and the debugging is the same as the above operation;

[0063] 2) Preparation: 10 g of Pisicanilic intermediate 7A-double-condensed pyrrolidine-acetonitrile with a content of 95% is stored in the storage tank V-01 and fed by the pump P-01; the 36% hydrochloric acid solution 14.13 g is placed in the storage tank V-02 and fed by the pump P-02. The inlet temperature of the microreactor of the hydrochloric acid solution is 100°C, and the outlet temperature of the microreactor is 103°C. After the equilibrium time is 5 minutes, the reaction temperature rises to 105°C , start receiving materials;

[0064] 3) Mix in the micro-mixer U, and complete the hydrolysis reaction in 3 minutes through the tube reactor and heat exc...

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Abstract

The invention discloses a microchannel reactor-based cyano compound hydrolysis reaction method, and particularly, a compound comprising a cyano group in the molecule has the cyano hydrolysis reactionby using a microchannel reactor under the action of alkaline or acid-alkaline substances. By using the microchannel reactor in the process, the raw material is instantaneously evenly mixed and efficiently transfers heat; the most important danger of rushing of the material in the production process, caused by hydrolysis of the cyano compound through the alkali, is avoided; meanwhile, the equivalence ratio of the raw material in the reaction process is also reduced; the side reaction is reduced; the reaction time is shortened to dozens of minutes or even dozens of seconds. In a word, the process improves the operation safety of the reaction, the safe enlarged production of the cyano compound is realized, the time for the hydrolysis reaction of the cyano compound is shortened, the reaction selectivity and the reaction efficiency are improved, the energy consumption of the production is reduced, the use ratio of the raw material is increased, the production process is more environmentallyfriendly, the production cost is low, meanwhile, the used equipment occupies a small area, the production capacity of the equipment is high, and the production efficiency and the production capacityare greatly improved.

Description

technical field [0001] The invention relates to a method for carrying out cyano group hydrolysis reaction in a microchannel reactor, specifically, in the microchannel reactor, molecules containing cyano groups are hydrolyzed with lye or acid solution to generate compounds containing carboxyl groups, It belongs to the field of organic synthesis. Background technique [0002] Micro-reaction technology originated in the 1990s. In recent years, the advantages of micro-reactors have gradually become prominent, and they realized that micro-reactors are stronger than conventional mass and heat transfer capabilities, so micro-reactors were applied to the field of chemical synthesis; micro-reactions With the development of the device today, it is no longer simply pursuing the miniaturization of the reaction channel, but changing the fluid flow pattern through the reaction channel to form a micro-scale liquid flow, forming efficient and rapid mass and heat transfer. Utilizing these a...

Claims

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Application Information

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IPC IPC(8): C07D487/04C07C51/08C07C57/32C07C57/58C07C59/68C07C227/26C07C229/08C07C319/12C07C323/52B01J19/00B01J19/24B01F13/00C07B41/08
CPCB01J19/0073B01J19/0093B01J19/2425C07B41/08C07C51/08C07C227/26C07C319/12C07D487/04B01J2219/00087B01J2219/00058B01F33/30C07C57/32C07C57/58C07C59/68C07C229/08C07C323/52
Inventor 曾伟滕坤于淼赫玲爽
Owner 大连微凯化学有限公司
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