CN218924649U - A micro reaction device - Google Patents

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

A micro reaction device

technical field

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

Background technique

Microreactors are reaction devices with microstructures (channels, meshes, grooves, etc.), in which micron-scale dispersed single-phase or multi-phase systems can be formed to strengthen the reaction process. It has the advantages of small characteristic scale, high transfer efficiency, and approximate plug flow, which can realize precise control of fluid and reaction conditions. In recent years, it has developed rapidly in the pharmaceutical chemical industry and fine chemical production industry, showing excellent equipment performance.

The characteristic small scale of the microreactor not only improves the mass transfer and heat transfer, but also brings the problems of large system pressure drop, small reaction flux, and short material residence time, which seriously limits its application and promotion. At present, industrial applications are all in small-volume chemicals or specific second-level fast reactions, and large-scale industrial production cannot be carried out for most chemicals. It is of great significance to develop reaction equipment with large throughput that can be used in industrial production.

Patent application CN215901720U discloses a microreactor structure and a microchannel reactor, which adopts an elliptical cavity structure and guides are arranged in it to promote material mixing.

Patent application CN211725714U discloses a high-throughput micro-reaction device for preparing di-tert-butyl peroxide. The equipment includes a feeding device, a micro-reaction device, and a post-processing device; the micro-reaction device includes a primary micro-reactor and a secondary micro-reactor; the post-processing device includes a stirring reaction device or a tubular reactor. The material at the reactor outlet of this equipment has not been completely reacted. If it enters the subsequent stirring reaction device, which is similar to the existing tank production method, or enters the tubular reactor, the configuration of the tubular reactor is not clear, and the material will be stratified. lead to incomplete reaction.

Patent application CN105617957A discloses a method for enhancing fluid mixing and reaction in a microreactor, including a tubular reactor with internals, wherein the internals are metal foam, ceramic foam or quartz filler with a network structure.

Patent application CN108514855A discloses a reaction device, which includes a microreactor and a tubular reactor. The tubular reactor is a coil reactor or a straight tube reactor. When the inner diameter of the tubular reactor is large, the material will be stratified, which limits the production capacity.

The increase in pipe size will lead to stratification of reaction materials and affect the efficiency of mass and heat transfer. Filling the pipeline with components of suitable structure can play the role of mixed material, which can not only meet the mixing requirements of the reaction, but also increase the reaction flux, and realize large-scale industrial production.

Utility model content

The purpose of the utility model is to provide a micro-reactor device suitable for large-scale industrial production. The purpose is to increase the reaction flux, maintain a high reaction rate, shorten the residence time of materials, and reduce equipment investment.

In order to achieve the above object, the utility model provides a microreactor device, comprising at least one microreactor and at least one tubular reactor connected in series, wherein the tubular reactor includes a tube side and a shell side, so One or more internal member units are arranged in the tube, and the internal member unit includes 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 , the second disturbance structure is a bent plate with holes.

Preferably, each internal member unit includes one first disturbance structure and two second disturbance structures.

Preferably, in each of said internals units, said first disturbance structure is located upstream in flow.

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

Preferably, in each of the internal component units, the distance between two adjacent disturbing structures is 0-1m; the distance between two adjacent internal component units is 0-2m.

Preferably, the micro-reaction device includes more than two micro-reactors and more than two tubular reactors, and the micro-reactors are spaced apart from the tubular reactors.

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

Preferably, the microreactor adopts a microchannel or a microreactor sheet with mixing and heat dissipation functions.

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

Preferably, the micro-reaction device further includes a plurality of material supply channels for supplying reaction materials and a post-processing device for processing the reacted materials.

According to the micro-reaction device described in the utility model, multi-strand reaction materials can be fully mixed in the micro-reactor, and after the material flowing out from the micro-reactor enters the tubular reactor, the first disturbance structure and second disturbance structure Under the action of the material to maintain a turbulent state and continue to react. Therefore, using the micro-reaction device described in the utility model to carry out the reaction can keep the materials in a good mixing state, thereby obtaining better reaction efficiency.

In addition, the micro-reaction device described in the utility model can realize large-scale continuous production, can reduce reaction liquid holding capacity, reduce reaction risk, and reduce accidents at the same time.

Description of drawings

Fig. 1 is the schematic diagram of micro reaction device described in the utility model;

Fig. 2 is the tube pass structure schematic diagram of tubular reactor in the micro-reaction device described in the utility model;

Fig. 3 is the structural representation of the first perturbation structure in the tubular reactor of the present utility model;

Fig. 4 is a structural schematic diagram of the second disturbance structure in the tubular reactor of the present invention.

Explanation of reference signs

1-the first material supply tank; 2-the second material supply tank; 3-the third material supply tank; 4-the first material pump; 5-the second material pump; 6-the third material pump; 7-the first micro Reactor; 8-the first tubular reactor; 9-the second microreactor; 10-the second tubular reactor; 11-heat exchanger; 12-post-treatment device; 21-the first disturbance structure; 22- Second perturbation structure.

Detailed ways

The specific embodiment of the utility model will be described in detail below in conjunction with the accompanying drawings. It should be understood that the specific embodiments described here are only used to illustrate and explain the utility model, and are not intended to limit the utility model.

In the description of the present application, the terms "first" and "second" are used for descriptive purposes only, and cannot be understood as indicating relative importance, or implicitly indicating the quantity of indicated technical features. Therefore, unless otherwise specified, the features defined as "first" and "second" may explicitly or implicitly include one or more of these features; "plurality" means two or more. The term "comprising" and any variations thereof mean that one or more other features, units, components and/or combinations thereof are non-exclusively included, may exist or be added.

In addition, unless otherwise clearly specified and limited, the terms "mounted", "connected" and "connected" should be interpreted in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection , can also be an electrical connection; it can be a direct connection, an indirect connection through an intermediary, or an internal communication between two components. Those of ordinary skill in the art can understand the specific meanings of the above terms in this application according to specific situations.

As shown in Figures 1-4, the micro-reaction device described in the utility model includes at least one micro-reactor and at least one tubular reactor connected in series. In a preferred situation, the micro-reaction device includes more than two micro-reactors and more than two tubular reactors, and the micro-reactors are spaced apart from the tubular reactors. Further preferably, along the flow direction of the reaction materials, the first reactor is a microreactor, and the last reactor is a tubular reactor. As a specific embodiment, along the flow direction of the reactant material, the micro-reaction device includes a first micro-reactor 7, a first tubular reactor 8, a second micro-reactor 9 and a second tubular reaction device 10.

In the micro-reaction device described in the present invention, the tubular reactor includes a tube side and a shell side, and one or more internal member units are arranged in the tube side, and the internal component unit includes at least one first A disturbance structure 21 and at least one second disturbance structure 22, wherein the first disturbance structure 21 is formed by stacking a plurality of corrugated plates, and the second disturbance structure 22 is a bent plate with holes. By setting the internal component unit with a specific structure, after the reactant material enters the tubular reactor, under the action of the first disturbance structure 21 and the second disturbance structure 22, the material maintains a turbulent flow state and continues to react. In the tubular reactor, the shell side can be filled with a heat exchange medium for exchanging heat with the reaction materials in the tube side.

In the micro reaction device described in the present utility model, a plurality of internal member units may be arranged in the tubular reactor, and each internal member unit may include one or more first disturbance structures 21 and one or more second disturbance structures 21 Two perturbation structures 22 . In a preferred embodiment, each internal member unit includes one first disturbance structure 21 and two second disturbance structures 22 . Further preferably, in each internal component unit, the first disturbance structure 21 is located upstream of the flow. According to the preferred embodiment described above, a better disturbance effect can be obtained in the tubular reactor, so that the reaction materials can be better mixed.

In the micro reaction device described in the present invention, the first disturbance structure 21 is formed by stacking a plurality of corrugated plates. In a specific embodiment, the length direction of the groove of the corrugated plate is substantially parallel to the tube side axis of the tube reactor. The first disturbance structure 21 may be formed by stacking 3-20 layers (preferably 5-15 layers) of corrugated plates. The grooves between two adjacent layers of corrugated boards are alternately stacked. In one embodiment, the bottom of the groove of the upper corrugated board is in contact with the top of the protrusion of the next corrugated board, so that A channel is formed between them for the flow of reactants to pass through.

In the micro reaction device described in the present invention, the second disturbance structure 22 is a bent plate with holes. The shape of the bent plate is not particularly limited, and may be triangular, semicircular, semielliptical or other regular or irregular shapes. The shape of the hole on the bent plate can be any shape, for example, it can be a circle, a square, a triangle, a polygon and other regular geometric figures or any irregular figures. The opening ratio of the bent plate may be 30-90%, preferably 40-80%, more preferably 45-70%. The opening ratio refers to the ratio of the area of holes on the surface of the bent plate to the total surface area.

In the micro-reaction device described in the utility model, the size of the tubular reactor can be appropriately configured according to the heat and mass transfer requirements of the materials. In a specific embodiment, the inner diameter of the tube side of the tubular reactor may be 1-40 cm, preferably 5-20 cm; the length of the tubular reactor may be 0.3-100 m, preferably 0.5-50 m.

In the micro-reaction device described in the present invention, in each of the internal component units, the distance between two adjacent disturbance structures can be 0-1m, preferably 0.1-0.5m; two adjacent internal component units The spacing can be 0-2m, preferably 0.1-1m.

In the micro-reaction device described in the utility model, the micro-reactor can use a separate micro-channel, or adopt a micro-reactor sheet with mixing and heat dissipation functions. The channel size of the microreactor is small, mainly to achieve rapid mixing of materials and preliminary reaction, and the pressure drop can be reduced by controlling the length of the microchannel or the number of microreactor pieces. In a specific embodiment, the channel size (ie channel diameter) of the microchannel can be 20 μm to 5 mm, preferably 100 μm to 2 mm, more preferably 150 μm to 1 mm; the length of the microchannel can be 0.5-20 m, It is preferably 1-15m, more preferably 1-10m. The microreactor sheet can be a heart-shaped, umbrella-shaped or other shaped microreactor sheet. In a more preferred embodiment, the microreactor adopts a microreactor sheet with mixing and heat dissipation functions. In this preferred embodiment, the microreactor sheet has a heat extraction function, which can quickly remove the heat of reaction.

In the present invention, the micro-reaction device may further include a plurality of material supply channels for supplying reaction materials and a post-processing device for processing the reacted materials. In a specific embodiment, as shown in Figure 1, the micro-reaction device includes 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 supply tank Pump 5, the third material pump 6, the first microreactor 7, the first tubular reactor 8, the second microreactor 9, the second tubular reactor 10, heat exchanger 11 and aftertreatment device 12, wherein , the first stream of material passes through the first material supply tank 1 and is fed through the first material pump 4, the second stream of material passes through the second material supply tank 2 and is pumped through the second material pump 5, and the third stream of material passes through The third material is supplied to the tank 3 and pumped through the third material pump 6, and the three materials enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9 and the second tubular reactor together in sequence 10 for heat mixing and reaction, the obtained reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12 for product separation.

The micro-reaction device described in the utility model will be further illustrated below by way of examples. The embodiment is implemented on the premise of the technical solution of the utility model, and detailed implementation and specific operation process are given, but the protection scope of the utility model is not limited to the following examples.

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

Example 1

This embodiment is implemented in the micro-reaction device shown in Fig. 1, and this micro-reaction device comprises the first material supply tank 1, the second material supply tank 2, the third material supply tank 3, the first material pump 4, the second material supply tank Pump 5, the third material pump 6, the first microreactor 7, the first tubular reactor 8, the second microreactor 9, the second tubular reactor 10, heat exchanger 11 and aftertreatment device 12, wherein , the first stream of material passes through the first material supply tank 1 and is fed through the first material pump 4, the second stream of material passes through the second material supply tank 2 and is pumped through the second material pump 5, and the third stream of material passes through The third material is supplied to the tank 3 and pumped through the third material pump 6, and the three materials enter the first microreactor 7, the first tubular reactor 8, the second microreactor 9 and the second tubular reactor together in sequence 10 for heat mixing and reaction, the obtained reacted material first enters the heat exchanger 11 for heat exchange, and then enters the post-processing device 12 for product separation. Wherein, the first microreactor 7 and the second microreactor 9 are sheet-type microchannel reactors; the first tubular reactor 8 and the second tubular reactor 10 respectively include a shell side and a tube side, and a There are multiple internal member units, each internal member unit includes 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 Bent plate with holes.

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

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the control temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 20m. Inside the tube side, the distance between two adjacent internal components is 0.3m , in each internal member unit, the distance between two adjacent disturbance structures is 0.3m, the opening ratio of the bent plate as the disturbance structure is 55%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 30m. Inside the tube, the distance between two adjacent internal component units is 0.3m. In each internal component unit , the distance between two adjacent disturbance structures is 0.3m, the opening rate of the bent plate as the disturbance structure is 55%, and the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.7%.

Comparative example 1

On the basis of Example 1, the tube passes in the first tubular reactor 8 and the second tubular reactor 10 are all set as empty tubes, and no internal components are set inside. As a result, the content of dinitrochlorobenzene in the product was 84.9%.

Comparative example 2

On the basis of Example 1, only the first perturbation structure 21 is set in the tube side of the first tubular reactor 8 and the second tubular reactor 10, and the second perturbation structure 22 is not provided. As a result, the product dinitrate The base chlorobenzene content is 89.8%.

Comparative example 3

On the basis of Example 1, only the second perturbation structure 22 is set in the tube side of the first tubular reactor 8 and the second tubular reactor 10, and the first perturbation structure 21 is not provided. As a result, the product dinitrate The content of chlorobenzene is 91.3%.

Example 2

The structure and reaction materials of the micro-reaction device adopted are the same as in Example 1.

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the controlled temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 15m. Inside the tube side, the distance between two adjacent internal components is 0.2m , in each internal member unit, the distance between two adjacent disturbance structures is 0.2m, the opening rate of the bent plate as the disturbance structure is 45%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 20m. Inside the tube, the distance between two adjacent internal member units is 0.2m. In each internal member unit , the distance between two adjacent disturbance structures is 0.2m, the opening rate of the bent plate as the disturbance structure is 45%, and the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.4%.

Example 3

The structure and reaction materials of the micro-reaction device adopted are the same as in Example 1.

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the control temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 30m. Inside the tube side, the distance between two adjacent internal components is 0.3m , in each internal member unit, the distance between two adjacent disturbance structures is 0.3m, the opening ratio of the bent plate as the disturbance structure is 70%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 30m. Inside the tube, the distance between two adjacent internal component units is 0.3m. In each internal component unit , the distance between two adjacent perturbation structures is 0.3m, the opening ratio of the bent plate used as the perturbation structure is 70%, and the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.8%.

Example 4

The structure and reaction materials of the micro-reaction device adopted are the same as in Example 1.

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the controlled temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 25m. Inside the tube side, the distance between two adjacent internal components is 0.5m , in each internal member unit, the distance between two adjacent disturbance structures is 0.5m, the opening rate of the bent plate as the disturbance structure is 65%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 30m. Inside the tube, the distance between two adjacent internal member units is 0.5m. In each internal member unit , the distance between two adjacent disturbance structures is 0.5m, the opening rate of the bent plate as the disturbance structure is 65%, and the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water, and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.6%.

Example 5

The structure and reaction materials of the micro-reaction device adopted are the same as in Example 1.

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the control temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 20m. Inside the tube, the distance between two adjacent internal components is 0.5m , in each internal member unit, the distance between two adjacent disturbance structures is 0.5m, the opening rate of the bent plate as the disturbance structure is 60%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, and the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 20m. Inside the tube, the distance between two adjacent internal member units is 0.5m. In each internal member unit , the distance between two adjacent disturbance structures is 0.5m, the opening rate of the bent plate as the disturbance structure is 60%, and the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water, and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.3%.

Example 6

The structure and reaction materials of the micro-reaction device adopted are the same as in Example 1.

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the controlled temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 30m. Inside the tube side, the distance between two adjacent internal components is 0.5m , in each internal member unit, the distance between two adjacent disturbance structures is 0.5m, the opening rate of the bent plate as the disturbance structure is 70%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 30m. Inside the tube, the distance between two adjacent internal member units is 0.5m. In each internal member unit , the distance between two adjacent perturbation structures is 0.5m, the opening rate of the bent plate as the perturbation structure is 70%, the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.7%.

Example 7

The structure and reaction materials of the micro-reaction device adopted are the same as in Example 1.

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the control temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 10m. Inside the tube side, the distance between two adjacent internal components is 0.5m , in each internal member unit, the distance between two adjacent disturbance structures is 0.5m, the opening rate of the bent plate as the disturbance structure is 60%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, and the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 20m. Inside the tube, the distance between two adjacent internal member units is 0.5m. In each internal member unit , the distance between two adjacent disturbance structures is 0.5m, the opening rate of the bent plate as the disturbance structure is 60%, and the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water, and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.1%.

Example 8

The structure and reaction materials of the micro-reaction device adopted are the same as in Example 1.

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the control temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 20m. Inside the tube side, the distance between two adjacent internal component units is 0.4m , in each internal member unit, the distance between two adjacent disturbance structures is 0.4m, the opening rate of the bent plate as the disturbance structure is 50%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 30m. Inside the tube, the distance between two adjacent internal member units is 0.4m. In each internal member unit , the distance between two adjacent disturbance structures is 0.4m, the opening rate of the bent plate as the disturbance structure is 50%, and the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water, and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.6%.

Example 9

The structure and reaction materials of the micro-reaction device adopted are the same as in Example 1.

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the control temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 25m. Inside the tube side, the distance between two adjacent internal components is 0.3m , in each internal member unit, the distance between two adjacent disturbance structures is 0.3m, the opening rate of the bent plate as the disturbance structure is 50%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 30m. Inside the tube, the distance between two adjacent internal component units is 0.3m. In each internal component unit , the distance between two adjacent disturbance structures is 0.3m, the opening rate of the bent plate as the disturbance structure is 50%, and the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.8%.

Example 10

The structure and reaction materials of the micro-reaction device adopted are the same as in Example 1.

Using 98% concentrated sulfuric acid, 95% concentrated nitric acid and chlorobenzene, the molar ratio of feed sulfuric acid: nitric acid: chlorobenzene is 2:2.3:1. As shown in Figure 1, the three streams of materials are continuously pumped into the reactor part by the pump respectively. The liquid holding capacity of the first microreactor is 280ml, and the control temperature is 80°C; the inner diameter of the first tubular reactor is 4cm, and the length is 30m. Inside the tube side, the distance between two adjacent internal components is 0.4m , in each internal member unit, the distance between two adjacent disturbance structures is 0.4m, the opening rate of the bent plate as the disturbance structure is 50%, and the control temperature is 95°C; the liquid holding capacity of the second microreactor The volume is 280ml, and the control temperature is 95°C; the inner diameter of the second tubular reactor is 4cm, and the length is 20m. Inside the tube, the distance between two adjacent internal member units is 0.4m. In each internal member unit , the distance between two adjacent disturbance structures is 0.4m, the opening rate of the bent plate as the disturbance structure is 50%, and the control temperature is 100°C; the heat exchanger is the same as the microreactor, and the control temperature is 30°C. The product is sent to a follow-up separation device. After the water and oil phases are separated, the oil phase is washed with alkali, washed with water and dried to obtain the product. The content of dinitrochlorobenzene in the product is 99.5%.

It can be seen from the above examples and comparative examples that according to the micro-reaction device described in the present invention, better reaction effects can be obtained by arranging internal component units with specific structures in the tube side of the tubular reactor.

The preferred embodiments of the present invention have been described in detail above, but the present invention is not limited thereto. Within the scope of the technical concept of the utility model, various simple modifications can be made to the technical solution of the utility model, including the combination of various technical features in any other suitable manner, and these simple variations and combinations should also be regarded as disclosed by the utility model. All the contents belong to the protection scope of the present utility model.

Claims (10)

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.

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