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Continuous overflow reactor system and continuous preparation process of 2-methyl-4, 6-pyrimidinedione

A reaction system, pyrimidine diketone technology, applied in the field of multi-stage continuous reactors, can solve the problems of restricting the production and application of new materials, low preparation efficiency, solid phase sticking to the wall, etc., and achieve good product quality, high mixing efficiency, continuous The effect of preparation and delivery

Pending Publication Date: 2022-04-26
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

It usually takes more than 3 hours to prepare the substance by the traditional kettle-type process, and the preparation efficiency is low, which limits the production and application of new materials such as FOX-7.
Moreover, the synthesis process of 2-methyl-4,6-pyrimidinedione will produce solids, and the reaction system is a solid-liquid two-phase system. Using common pipeline continuous or micro-reaction techniques will cause solid phase sticking to the wall and blockage, which is a constraint Its process intensification and continuous bottleneck technology

Method used

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  • Continuous overflow reactor system and continuous preparation process of 2-methyl-4, 6-pyrimidinedione
  • Continuous overflow reactor system and continuous preparation process of 2-methyl-4, 6-pyrimidinedione
  • Continuous overflow reactor system and continuous preparation process of 2-methyl-4, 6-pyrimidinedione

Examples

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Embodiment 1

[0034] Such as figure 1 and 2 As shown, the continuous reactor of this embodiment comprises a circular cylindrical reactor body 3-1 and a disc-shaped cover body 3-6; The chamber or jacket 3-4 is equipped with two inlets and outlets 3-5 for cold and hot medium, and the reaction vessels 3-2 at all levels are arranged in the chamber or jacket for the heat medium and are evenly distributed in a ring shape along the axial direction. An overflow tank 3-3 is provided on the top of the partition wall adjacent to the reaction vessel, and the adjacent reaction vessels are connected, and a plurality of reaction vessels are connected in series through the overflow tank, but no overflow tank is established between the reaction vessels at the head and tail; The disc-shaped cover is provided with a raw material inlet 3-7 and a reactant outlet 3-8. After the cover is covered on the reactor body, the raw material inlet communicates with the first reaction vessel, and the reactant outlet commu...

Embodiment 2

[0037] Such as image 3 As shown, the continuous reaction system of this embodiment includes four reaction raw material storage tanks 1, the continuous reactor 3 of embodiment 1, the acoustic resonance generator 8, the temperature control system 7, the filter 5 and the drier 6; The reactor is placed on the acoustic resonance generator, specifically, a fixed frame 4 is fixed on the acoustic resonance generator, and each raw material storage tank is connected with the raw material inlet on the continuous generator through the delivery pump 2, and the reactant outlet is connected with the filter, and filtered The device is connected with the drier, wherein the temperature control system can adopt related products of the prior art to control the reaction temperature in the continuous reactor.

Embodiment 3

[0039] The system described in Example 2 is used to prepare 2-methyl-4,6-pyrimidinedione. It should be noted that the reactor and reaction system of the present invention are not limited to the production of 2-methyl-4,6-pyrimidinedione Ketones, those skilled in the art can be used to generate other products with liquid-liquid homogeneous, gas-liquid two-phase, and solid-containing multiphase reaction systems according to the reaction principle of related substances and the scheme and effect of the present invention.

[0040]The preparation raw materials are methanol solution of sodium methoxide, acetamidine hydrochloride, diethyl malonate and methanol, wherein acetamidine hydrochloride and diethyl malonate are raw materials, sodium methoxide is a catalyst, and methanol is a solvent. The molar ratio of amidine: diethyl malonate: sodium methoxide is 1:1.05~1.20:2.0~3.0, and the specific preparation process is as follows:

[0041] (1) Dissolve acetamidine hydrochloride in methan...

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Abstract

The invention relates to a continuous overflow reaction system and a continuous preparation process of 2 methyl-4, 6 pyrimidinedione, the disclosed reaction system comprises an acoustic resonance generator and a continuous overflow reactor, the overflow reactor is arranged in or on the acoustic resonance generator; the continuous overflow reactor is provided with a plurality of reaction containers, overflow holes or overflow grooves for communicating two adjacent reaction containers are formed between the adjacent reaction containers, and the plurality of reaction containers are sequentially connected in series through the overflow holes or the overflow grooves; according to the 2-methyl-4, 6-pyrimidinedione preparation system, a plurality of reaction containers are connected in series, no overflow hole or overflow groove is formed between the reaction container located at the head and the reaction container located at the tail in the plurality of reaction containers connected in series, and the overflow hole or overflow groove is located at the top of the corresponding reaction container. The reaction is enhanced in an acoustic resonance external field, and the reaction enhancement degree is adjusted through the acceleration of a reaction platform, so that the 2-methyl-4, 6-pyrimidinedione is efficiently and continuously prepared.

Description

technical field [0001] The invention relates to a multi-stage continuous reactor, in particular to a continuous overflow reactor system and a continuous preparation process for 2-methyl-4,6-pyrimidinedione. Background technique [0002] The traditional kettle-type process has the problems of difficult process scale-up, long reaction time, and low production efficiency, which limits the further application and development of many new materials. [0003] Taking the intermediate 2-methyl-4,6-pyrimidinedione (MPO) used in the synthesis of the low-sensitivity high-energy explosive FOX-7 as an example, 2-methyl-4,6-pyrimidinedione (MPO) is generally prepared by the kettle process at home and abroad. Pyrimidinedione, using methanol as a solvent, reacting sodium methoxide with acetamidine hydrochloride, then adding diethyl malonate dropwise after heating, filtering after the reaction, adding hydrochloric acid to acidify to obtain 2-methyl-4,6-pyrimidinedione product. It usually tak...

Claims

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Application Information

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IPC IPC(8): B01J19/24C07D239/54
CPCB01J19/245C07D239/54
Inventor 张圣龙王锡杰罗志龙廉鹏陈基邹高兴
Owner XIAN MODERN CHEM RES INST