CN218924649U

CN218924649U - Micro-reaction device

Info

Publication number: CN218924649U
Application number: CN202223294433.1U
Authority: CN
Inventors: 任君朋; 朱红伟; 刘聿嘉; 赵辰阳; 朱云峰; 孙冰
Original assignee: China Petroleum and Chemical Corp; Sinopec Safety Engineering Research Institute Co Ltd
Current assignee: China Petroleum and Chemical Corp; Sinopec Safety Engineering Research Institute Co Ltd
Priority date: 2022-12-08
Filing date: 2022-12-08
Publication date: 2023-04-28
Anticipated expiration: 2032-12-08

Abstract

The utility model discloses a microreactor device, which comprises at least one microreactor and at least one tubular reactor which are mutually connected in series, wherein the tubular reactor comprises a tube side and a shell side, one or more inner member units are arranged in the tube side, each inner member unit comprises at least one first disturbance structure and at least one second disturbance structure, the first disturbance structure is formed by stacking a plurality of corrugated plates, and the second disturbance structure is a bending plate with holes. According to the micro-reaction device, a plurality of reaction materials can be fully mixed in the micro-reactor, and after the materials flowing out of the micro-reactor enter the tubular reactor, the materials are kept in a turbulent state and continue to react under the action of the first disturbance structure and the second disturbance structure. Therefore, the micro-reaction device provided by the utility model can be used for reaction to keep the materials in a good mixing state, so that good reaction efficiency is obtained.

Description

Micro-reaction device

Technical Field

The utility model relates to a micro-reaction device, in particular to a high-flux micro-reaction device for mixing and reacting materials.

Background

Microreactors are reaction devices with microstructures (channels, meshes, grooves, etc.) in which a single-phase or multiphase system of micrometer-scale dispersion can be formed to intensify the reaction process. The method has the advantages of small characteristic scale, high transmission efficiency and approximately plug flow, and can realize the accurate control of fluid and reaction conditions. In recent years, the development in pharmaceutical chemical industry and fine chemical product production industry is rapid, and excellent equipment performance is shown.

The characteristic small scale of the microreactor improves mass and heat transfer, and simultaneously brings the problems of large pressure drop, small reaction flux and short material residence time, thereby severely limiting the application and popularization of the microreactor. The current industrial application is in the aspect of small-yield chemicals or specific second-level fast reaction, and large-scale industrial production of most chemicals cannot be performed. The development of reaction equipment with large flux and applicable to industrial production has very important significance.

Patent application CN215901720U discloses a micro-reactor structure and a micro-channel reactor, which adopt an oval cavity structure and a flow guide is arranged in the oval cavity structure to promote material mixing.

Patent application CN211725714U discloses a high throughput microreaction apparatus for preparing di-tert-butyl peroxide. The equipment comprises a feeding device, a micro-reaction device and a post-treatment device; the micro-reaction device comprises a primary micro-reactor and a secondary micro-reactor; the post-treatment device comprises a stirring reaction device or a tubular reactor. If the materials at the outlet of the reactor of the equipment are not completely reacted, and enter a subsequent stirring reaction device similar to the existing kettle type production mode, or enter a tubular reactor, the configuration of the tubular reactor is undefined, and the materials can be layered, so that the reaction is not completely carried out.

Patent application CN105617957a discloses a method for enhancing fluid mixing and reaction in microreactors comprising a tubular reactor with internals, wherein the internals are foam metal, foam ceramic or quartz packing of a mesh structure.

Patent application CN108514855a discloses a reaction device comprising a microreactor and a tubular reactor. The tubular reactor is a coil type reactor or a straight tube type reactor, and when the inner diameter of the tubular reactor is larger, materials can be layered, so that the productivity is limited.

The increase in the size of the pipeline can lead to layering of the reaction materials, and the mass and heat transfer efficiency is affected. The components with proper structures are filled in the pipeline to play a role of mixing materials, so that the requirement of the reaction on mixing can be met, the reaction flux can be increased, and large-scale industrial production can be realized.

Disclosure of Invention

The utility model aims to provide a micro-reactor device suitable for large-scale industrial production, and aims to increase the reaction flux, maintain a higher reaction rate, shorten the material residence time and reduce the equipment investment.

In order to achieve the above object, the present utility model provides a microreactor device comprising at least one microreactor and at least one tubular reactor connected in series with each other, wherein the tubular reactor comprises a tube side and a shell side, one or more inner member units are arranged in the tube side, the inner member units comprise at least one first disturbance structure and at least one second disturbance structure, wherein the first disturbance structure is formed by stacking a plurality of corrugated plates, and the second disturbance structure is a bending plate with holes.

Preferably, each of said inner member units comprises one first perturbation and two second perturbation.

Preferably, in each of said internals units, said first perturbation is located upstream of the flow.

Preferably, the tube side inner diameter of the tube reactor is 1-40cm, and the length of the tube reactor is 0.3-100m.

Preferably, in each of the inner member units, the pitch of two adjacent perturbation structures is 0-1m; the distance between two adjacent inner member units is 0-2m.

Preferably, the microreactor means comprises two or more microreactors and two or more tubular reactors, and the microreactors are spaced apart from the tubular reactors.

Preferably, the first reactor is a microreactor and the last reactor is a tubular reactor along the flow direction of the reaction mass.

Preferably, the microreactor employs microchannels or microreactor plates with mixing and heat dissipation functions.

Preferably, the microreactor sheet is heart-shaped or umbrella-shaped.

Preferably, the micro-reaction device further comprises a plurality of material supply channels for supplying the reaction material and a post-treatment device for treating the reacted material.

According to the micro-reaction device, a plurality of reaction materials can be fully mixed in the micro-reactor, and after the materials flowing out of the micro-reactor enter the tubular reactor, the materials are kept in a turbulent state and continue to react under the action of the first disturbance structure and the second disturbance structure. Therefore, the micro-reaction device provided by the utility model can be used for reaction to keep the materials in a good mixing state, so that good reaction efficiency is obtained.

In addition, the micro-reaction device can realize large-scale continuous production, can reduce the reaction liquid holdup, reduce the reaction risk and simultaneously reduce the occurrence of accidents.

Drawings

FIG. 1 is a schematic view of a microreaction device according to the present utility model;

FIG. 2 is a schematic view of the tube side structure of a tube reactor in the microreactor device according to the present utility model;

FIG. 3 is a schematic structural view of a first perturbation structure in a tubular reactor of the present utility model;

FIG. 4 is a schematic structural view of a second perturbed structure in a tubular reactor according to the utility model.

Description of the reference numerals

1-a first material supply tank; 2-a second material supply tank; 3-a third material supply tank; 4-a first material pump; 5-a second material pump; 6-a third material pump; 7-a first microreactor; 8-a first tubular reactor; 9-a second microreactor; 10-a second tubular reactor; 11-a heat exchanger; 12-an aftertreatment device; 21-a first perturbation structure; 22-second perturbation structure.

Detailed Description

The following describes specific embodiments of the present utility model in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the utility model, are not intended to limit the utility model.

In the description of the present application, the terms "first", "second" are used for descriptive purposes only and are not to be construed as indicating relative importance or implicitly indicating the number of technical features indicated. Thus, unless otherwise indicated, features defining "first", "second" may include one or more such features either explicitly or implicitly; the meaning of "plurality" is two or more. The term "comprises," "comprising," and any variations thereof, are intended to cover a non-exclusive inclusion, a possible presence or addition of one or more other features, elements, components, and/or combinations thereof.

Furthermore, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; either directly or indirectly through intermediaries, or in communication with each other. The specific meaning of the terms in this application will be understood by those of ordinary skill in the art as the case may be.

As shown in FIGS. 1 to 4, the microreactor means according to the present utility model comprises at least one microreactor and at least one tubular reactor connected in series. Preferably, the microreactor means comprises two or more microreactors and two or more tubular reactors, and the microreactors are spaced apart from the tubular reactors. It is further preferred that the first reactor is a microreactor and the last reactor is a tubular reactor along the flow direction of the reaction mass. As a specific embodiment, the microreactor means comprises, in order along the flow direction of the reaction mass, a first microreactor 7, a first tubular reactor 8, a second microreactor 9 and a second tubular reactor 10.

In the microreaction device, the tubular reactor comprises a tube side and a shell side, one or more inner member units are arranged in the tube side, the inner member units comprise at least one first disturbance structure 21 and at least one second disturbance structure 22, the first disturbance structure 21 is formed by stacking a plurality of corrugated plates, and the second disturbance structure 22 is a bending plate with holes. By arranging the inner member units with specific structures, after the reactant enters the tubular reactor, the reactant is kept in a turbulent state and continuously reacts under the action of the first disturbance structure 21 and the second disturbance structure 22. In the tubular reactor, the shell side may be filled with a heat exchange medium for exchanging heat with the reaction mass in the tube side.

In the microreactor device according to the utility model, a plurality of internals units may be provided in the tubular reactor, each internals unit may comprise one or more first perturbation structures 21 and one or more second perturbation structures 22. In a more preferred embodiment, each of said inner member units comprises one first perturbation 21 and two second perturbation 22. Further preferably, in each of said internals units, said first perturbation means 21 is located upstream of the flow. According to the preferred embodiment, a better turbulence effect is obtained in the tubular reactor, so that the reaction mass can be better mixed.

In the microreaction device according to the present utility model, the first disturbance structure 21 is formed by stacking a plurality of corrugated plates. In a specific embodiment, the length direction of the grooves of the corrugated plate is substantially parallel to the tube side axial direction of the tube reactor. The first perturbation structure 21 may be formed by stacking 3-20 layers (preferably 5-15 layers) of corrugated board. Grooves between two adjacent layers of corrugated plates are overlapped in a staggered way. In one embodiment, the bottoms of the grooves of the upper corrugated plate are in contact with the tops of the protrusions of the lower corrugated plate, so that a channel is formed between the protrusions of the upper corrugated plate and the grooves of the lower corrugated plate, and reactant flows can pass through the channel.

In the microreaction device according to the present utility model, the second perturbation structure 22 is a bending plate with holes. The shape of the bent plate is not particularly limited and may be triangular, semicircular, semi-elliptical, or other regular or irregular shape. The apertures in the bending plate may be any shape, such as circular, square, triangular, polygonal, and other regular geometric or any irregular pattern. The aperture ratio in the bending plate may be 30-90%, preferably 40-80%, more preferably 45-70%. The aperture ratio refers to the ratio of the area of the holes on the surface of the bending plate to the total surface area.

In the microreactor according to the utility model, the dimensions of the tube reactor can be adapted to the heat and mass transfer requirements of the material. In a specific embodiment, the tube side inner diameter of the tube reactor may be 1-40cm, preferably 5-20cm; the length of the tubular reactor may be from 0.3 to 100m, preferably from 0.5 to 50m.

In the microreaction device according to the utility model, in each of the inner member units, the spacing between two adjacent perturbation structures may be 0-1m, preferably 0.1-0.5m; the spacing between adjacent two internals units may be 0-2m, preferably 0.1-1m.

In the microreactor device according to the present utility model, the microreactor may use individual microchannels or use microreactor sheets having mixing and heat dissipation functions. The micro-reactor has smaller channel size, mainly realizes rapid mixing and preliminary reaction of materials, and can reduce pressure drop by controlling the length of the micro-channels or the number of micro-reactor sheets. In particular embodiments, the microchannel may have a channel dimension (i.e., channel diameter) of 20 μm to 5mm, preferably 100 μm to 2mm, more preferably 150 μm to 1mm; the length of the micro-channels may be from 0.5 to 20m, preferably from 1 to 15m, more preferably from 1 to 10m. The microreactor sheet may be a heart-shaped, umbrella-shaped or other shaped microreactor sheet. In a more preferred embodiment, the microreactor employs microreactor sheets having mixing and heat dissipation functions. In this preferred embodiment, the microreactor sheet has a heat-extracting function, and the reaction heat can be rapidly removed.

In the present utility model, the micro-reaction device may further include a plurality of material supply channels for supplying the reaction materials and a post-treatment device for treating the reacted materials. In one embodiment, as shown in fig. 1, the micro-reaction device comprises a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first micro-reactor 7, a first tubular reactor 8, a second micro-reactor 9, a second tubular reactor 10, a heat exchanger 11 and a post-treatment device 12, wherein the first material is fed through the first material supply tank 1 and via the first material pump 4, the second material is fed through the second material supply tank 2 and via the second material pump 5, the third material is fed through the third material supply tank 3 and via the third material pump 6, the three materials are sequentially fed into the first micro-reactor 7, the first tubular reactor 8, the second micro-reactor 9 and the second tubular reactor 10 together, the obtained reacted materials are subjected to heat exchange in the heat exchanger 11, and then enter the post-treatment device 12 for product separation.

The microreaction device according to the present utility model is further illustrated by the following examples. The embodiment is implemented on the premise of the technical scheme of the utility model, and detailed implementation modes and specific operation processes are given, but the protection scope of the utility model is not limited to the following embodiment.

The experimental methods in the following examples, unless otherwise specified, are all conventional in the art. The experimental materials used in the examples described below are commercially available unless otherwise specified.

Example 1

This embodiment is implemented in a microreactor apparatus shown in fig. 1, which comprises a first material supply tank 1, a second material supply tank 2, a third material supply tank 3, a first material pump 4, a second material pump 5, a third material pump 6, a first microreactor 7, a first tubular reactor 8, a second microreactor 9, a second tubular reactor 10, a heat exchanger 11 and a post-treatment apparatus 12, wherein the first material is fed through the first material supply tank 1 via the first material pump 4, the second material is fed through the second material supply tank 2 via the second material pump 5, the third material is fed through the third material supply tank 3 via the third material pump 6, the three materials are fed into the first microreactor 7, the first tubular reactor 8, the second microreactor 9 and the second tubular reactor 10 in sequence together, the obtained reacted materials are subjected to heat exchange in the heat exchanger 11, and then enter the post-treatment apparatus 12 for product separation. Wherein the first micro-reactor 7 and the second micro-reactor 9 are sheet-type micro-channel reactors; the first tubular reactor 8 and the second tubular reactor 10 each comprise a shell side and a tube side, a plurality of inner member units are arranged in the tube side, each inner member unit comprises a first disturbance structure 21 and two second disturbance structures 22, the first disturbance structure 21 is formed by stacking a plurality of corrugated plates, and the second disturbance structure 22 is a bending plate with holes.

The first material supply tank 1 is used for supplying 98% of concentrated sulfuric acid, the second material supply tank 2 is used for supplying 95% of concentrated nitric acid, and the third material supply tank 3 is used for supplying chlorobenzene.

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 20m, the distance between two adjacent inner member units is 0.3m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.3m, the aperture ratio of a bending plate serving as a disturbance structure is 55%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 30m, the distance between two adjacent inner member units is 0.3m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.3m, the aperture ratio of a bending plate serving as a disturbance structure is 55%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the dinitrochlorobenzene content of the product is 99.7%.

Comparative example 1

On the basis of example 1, the tube runs in both the first tube reactor 8 and the second tube reactor 10 were set as empty tubes, and no internals unit was provided inside. As a result, the dinitrochlorobenzene content of the product was 84.9%.

Comparative example 2

Based on example 1, the tube passes in both the first tube reactor 8 and the second tube reactor 10 were provided with only the first perturbation structure 21 and without the second perturbation structure 22, and as a result, the dinitrochlorobenzene content was 89.8%.

Comparative example 3

Based on example 1, the tube passes in both the first tube reactor 8 and the second tube reactor 10 were each provided with only the second perturbation 22 and without the first perturbation 21, as a result of which the dinitrochlorobenzene content was 91.3%.

Example 2

The structure and the reaction materials of the microreaction device used were the same as those of example 1.

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 15m, the distance between two adjacent inner member units is 0.2m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.2m, the aperture ratio of a bending plate serving as a disturbance structure is 45%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 20m, the distance between two adjacent inner member units is 0.2m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.2m, the aperture ratio of a bending plate serving as a disturbance structure is 45%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the content of dinitrochlorobenzene in the product is 99.4%.

Example 3

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 30m, the distance between two adjacent inner member units is 0.3m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.3m, the aperture ratio of a bending plate serving as a disturbance structure is 70%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 30m, the distance between two adjacent inner member units is 0.3m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.3m, the aperture ratio of a bending plate serving as a disturbance structure is 70%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the content of dinitrochlorobenzene in the product is 99.8%.

Example 4

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 25m, the distance between two adjacent inner member units is 0.5m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.5m, the aperture ratio of a bending plate serving as a disturbance structure is 65%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 30m, the distance between two adjacent inner member units is 0.5m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.5m, the aperture ratio of a bending plate serving as a disturbance structure is 65%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the content of dinitrochlorobenzene in the product is 99.6%.

Example 5

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 20m, the distance between two adjacent inner member units is 0.5m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.5m, the aperture ratio of a bending plate serving as a disturbance structure is 60%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 20m, the distance between two adjacent inner member units is 0.5m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.5m, the aperture ratio of a bending plate serving as a disturbance structure is 60%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the content of dinitrochlorobenzene in the product is 99.3%.

Example 6

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 30m, the distance between two adjacent inner member units is 0.5m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.5m, the aperture ratio of a bending plate serving as a disturbance structure is 70%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 30m, the distance between two adjacent inner member units is 0.5m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.5m, the aperture ratio of a bending plate serving as a disturbance structure is 70%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the dinitrochlorobenzene content of the product is 99.7%.

Example 7

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 10m, the distance between two adjacent inner member units is 0.5m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.5m, the aperture ratio of a bending plate serving as a disturbance structure is 60%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 20m, the distance between two adjacent inner member units is 0.5m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.5m, the aperture ratio of a bending plate serving as a disturbance structure is 60%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the content of dinitrochlorobenzene in the product is 99.1%.

Example 8

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 20m, the distance between two adjacent inner member units is 0.4m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.4m, the aperture ratio of a bending plate serving as a disturbance structure is 50%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 30m, the distance between two adjacent inner member units is 0.4m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.4m, the aperture ratio of a bending plate serving as a disturbance structure is 50%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the content of dinitrochlorobenzene in the product is 99.6%.

Example 9

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 25m, the distance between two adjacent inner member units is 0.3m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.3m, the aperture ratio of a bending plate serving as a disturbance structure is 50%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 30m, the distance between two adjacent inner member units is 0.3m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.3m, the aperture ratio of a bending plate serving as a disturbance structure is 50%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the content of dinitrochlorobenzene in the product is 99.8%.

Example 10

The method comprises the steps of adopting 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, and feeding sulfuric acid: nitric acid: the mole ratio of chlorobenzene is 2:2.3:1. three separate streams of material were pumped continuously into the reactor section by pumps as shown in figure 1. The liquid holdup of the first micro-reactor is 280ml, and the temperature is controlled to be 80 ℃; the inner diameter of the first tubular reactor is 4cm, the length of the first tubular reactor is 30m, the distance between two adjacent inner member units is 0.4m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.4m, the aperture ratio of a bending plate serving as a disturbance structure is 50%, and the control temperature is 95 ℃; the liquid holdup of the second micro-reactor is 280ml, and the temperature is controlled to be 95 ℃; the inner diameter of the second tubular reactor is 4cm, the length of the second tubular reactor is 20m, the distance between two adjacent inner member units is 0.4m in the tube side, the distance between two adjacent disturbance structures in each inner member unit is 0.4m, the aperture ratio of a bending plate serving as a disturbance structure is 50%, and the control temperature is 100 ℃; the heat exchanger is the same as the microreactor, and the temperature is controlled to be 30 ℃. And (3) carrying out a subsequent separation device on the product, separating water from oil phases, and carrying out alkali washing, water washing and drying on the oil phase to obtain the product, wherein the content of dinitrochlorobenzene in the product is 99.5%.

As can be seen from the above examples and comparative examples, according to the microreaction device of the present utility model, a better reaction effect can be obtained by providing an inner member unit of a specific structure in the tube side of the tubular reactor.

The preferred embodiments of the present utility model have been described in detail above, but the present utility model is not limited thereto. Within the scope of the technical idea of the utility model, a number of simple variants of the technical solution of the utility model are possible, including combinations of the individual technical features in any other suitable way, which simple variants and combinations should likewise be regarded as being disclosed by the utility model, all falling within the scope of protection of the utility model.

Claims

1. The microreactor comprises at least one microreactor and at least one tubular reactor which are connected in series, and is characterized in that the tubular reactor comprises a tube side and a shell side, one or more inner member units are arranged in the tube side, each inner member unit comprises at least one first disturbance structure (21) and at least one second disturbance structure (22), the first disturbance structure (21) is formed by stacking a plurality of corrugated plates, and the second disturbance structure (22) is a bending plate with holes.

2. Microreaction device according to claim 1, characterized in that each of said internals units comprises one first perturbation (21) and two second perturbation (22).

3. Microreaction device according to claim 2, characterized in that in each of the internals units the first disturbing structure (21) is located upstream of the flow.

4. A microreaction device according to any of claims 1-3, characterized in that the tube side inner diameter of the tube reactor is 1-40cm and the length of the tube reactor is 0.3-100m.

5. A microreaction device according to any one of claims 1 to 3, wherein in each of said inner member units, the spacing between adjacent two perturbation structures is 0 to 1m; the distance between two adjacent inner member units is 0-2m.

6. A microreactor arrangement according to any one of claims 1-3, characterized in that the microreactor arrangement comprises two or more microreactors and two or more tubular reactors, and that the microreactors are arranged at intervals from the tubular reactors.

7. The microreactor device according to claim 6, wherein the first reactor is a microreactor and the last reactor is a tubular reactor in the flow direction of the reaction mass.

8. A microreactor device according to any of claims 1 to 3, wherein the microreactor is a microchannel or a microreactor sheet with mixing and heat dissipation functions.

9. The microreactor device according to claim 8, wherein the microreactor sheet is heart-shaped or umbrella-shaped.

10. A micro-reaction apparatus according to any one of claims 1-3, further comprising a plurality of material supply channels for supplying reaction materials and post-treatment means for treating the reacted materials.