Micro-channel reactor for nitration reaction of naphthalene and reaction method

Abstract

The invention relates to the technical field of organic synthesis application, in particular to a microchannel reactor for nitration reaction of naphthalene and a reaction method.The microchannel reactor comprises a microchannel reaction module, a channel module, a mixed acid preparation module, a naphthalene organic solution storage module and a cooling module; by integrating the micro-channel reaction module, the channel module, the mixed acid preparation module, the naphthalene organic solution storage module and the cooling module, efficient and accurate control of the naphthalene nitration reaction process is realized. Wherein the introduction of the cooling module significantly improves the thermal management capability of the system, and effectively solves the local overheating phenomenon, thereby reducing the generation of by-products, improving the purity and yield of the product, and further solving the problem that the by-products are increased due to the local overheating phenomenon in the production process of nitration of naphthalene by the microchannel reactor.

Description

Technical Field

[0001] The invention relates to the technical field of organic synthesis application, and in particular to a microchannel reactor and a reaction method for nitration reaction of naphthalene. Background Art

[0002] Microchannel reactors have been widely used in various chemical processes due to their small size, large specific surface area, and excellent heat and mass transfer effects.

[0003] At present, in the production process of nitration of naphthalene in a microchannel reactor, the generation of by-products increases due to local overheating. Summary of the invention

[0004] The invention aims to provide a microchannel reactor and a reaction method for nitration of naphthalene, aiming to solve the problem of increased by-products due to local overheating in the microchannel reactor during the nitration production process of naphthalene.

[0005] To achieve the above object, in a first aspect, the present invention provides a microchannel reactor for nitration reaction of naphthalene, comprising a microchannel reaction module, a channel module, a mixed acid preparation module, a naphthalene organic solution storage module and a cooling module, wherein the cooling module and the channel module are respectively connected to the microchannel reaction module, and the mixed acid preparation module and the naphthalene organic solution storage module are respectively connected to the channel module;

[0006] The microchannel reaction module is used to perform nitration reaction on naphthalene;

[0007] The channel module is used to introduce nitric acid and naphthalene organic solution into the microchannel reaction module;

[0008] The mixed acid preparation module is used to store nitric acid;

[0009] The naphthalene organic solution storage module is used to store the naphthalene organic solution;

[0010] The cooling module is used to cool the microchannel reaction module.

[0011] Wherein, the channel module comprises an interface unit 1, an interface unit 2, a feed port unit and a discharge port unit, the interface unit 1 and the interface unit 2 are respectively connected to the feed port unit, and the discharge port unit and the feed port unit are respectively connected to the microchannel reaction module;

[0012] The interface unit 1 is used to access nitric acid;

[0013] The interface unit 2 is used to access the naphthalene organic solution;

[0014] The feed port unit is used to connect the nitric acid and naphthalene organic solutions to the microchannel reaction module;

[0015] The discharge port unit is used to discharge the reacted material out of the microchannel reaction module.

[0016] Wherein, the mixed acid preparation module comprises a storage tank unit 1, a filter 1, a flow meter 1 and a metering pump 1, wherein the storage tank unit 1, the filter 1, the flow meter 1 and the metering pump 1 are connected in sequence, and the metering pump 1 is connected to the interface unit 1;

[0017] The storage tank unit 1 is used to store nitric acid;

[0018] The filter 1 is used to filter nitric acid;

[0019] The flow meter 1 is used to measure the flow rate of nitric acid;

[0020] The metering pump 1 is used to control and adjust the flow rate of nitric acid.

[0021] Wherein, the naphthalene organic solution storage module comprises a storage tank unit 2, a filter 2, a flow meter 2 and a metering pump 2, wherein the storage tank unit 2, the filter 2, the flow meter 2 and the metering pump 2 are connected in sequence, and the metering pump 2 is connected to the interface unit 2;

[0022] The storage tank unit 2 is used to store the naphthalene organic solution;

[0023] The filter 2 is used to filter the naphthalene organic solution;

[0024] The flow meter 2 is used to measure the flow of the naphthalene organic solution;

[0025] The metering pump 2 is used to control and adjust the flow rate of the naphthalene organic solution.

[0026] Wherein, the cooling module comprises a liquid storage unit, a circulation unit, a water inlet unit and a water outlet unit, and the liquid storage unit, the circulation unit, the water inlet unit and the water outlet unit are connected in sequence;

[0027] The liquid storage unit is used to store cooling water;

[0028] The circulation unit is used to drive the cooling water circulation to cool the microchannel reaction module;

[0029] The water inlet unit is used to allow cooling water to enter the microchannel reaction module;

[0030] The water outlet unit is used to discharge cooling water out of the microchannel reaction module.

[0031] Wherein, the cooling module further comprises a recovery unit, and the recovery unit is connected to the water outlet unit and to the liquid storage unit;

[0032] The recovery unit is used to recover the cooling water of the water outlet unit and return it to the liquid storage unit.

[0033] In a second aspect, a microchannel reaction method for the nitration reaction of naphthalene, a microchannel reactor for the nitration reaction described in the first aspect, comprises the following steps:

[0034] introducing nitric acid and naphthalene organic solution into the microchannel reaction module to carry out nitration reaction;

[0035] The microchannel reaction module is cooled to reduce the generation of by-products.

[0036] A microchannel reactor for naphthalene nitration reaction of the present invention comprises a microchannel reaction module, a channel module, a mixed acid preparation module, a naphthalene organic solution storage module and a cooling module, wherein the cooling module and the channel module are respectively connected to the microchannel reaction module, and the mixed acid preparation module and the naphthalene organic solution storage module are respectively connected to the channel module; the microchannel reaction module is used for nitration reaction of naphthalene; the channel module is used for introducing nitric acid and naphthalene organic solution into the microchannel reaction module; the mixed acid preparation module is used for storing nitric acid; the naphthalene organic solution storage module is used for storing naphthalene organic solution; and the cooling module is used for cooling the microchannel reaction module. The present invention realizes efficient and precise control of the naphthalene nitration reaction process by integrating the microchannel reaction module, the channel module, the mixed acid preparation module, the naphthalene organic solution storage module and the cooling module. Among them, the introduction of the cooling module significantly improved the thermal management capability of the system and effectively solved the problem of local overheating, thereby reducing the generation of by-products, improving the purity and yield of the product, and further solving the problem of increased by-products due to local overheating in the microchannel reactor during the nitration reaction of naphthalene. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments or the description of the prior art will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0038] Figure 1 The present invention is a schematic diagram of a microchannel reactor for nitration of naphthalene.

[0039] Figure 2 is a schematic diagram of the channel module.

[0040] Figure 3 It is a schematic diagram of the mixed acid preparation module.

[0041] Figure 4 It is a schematic diagram of the naphthalene organic solution storage module.

[0042] Figure 5 is a schematic diagram of the cooling module.

[0043] Figure 6 The present invention provides a flow chart of a microchannel reaction method for nitration of naphthalene.

[0044] 1-microchannel reaction module, 2-channel module, 3-mixed acid preparation module, 4-naphthalene organic solution storage module, 5-cooling module, 21-interface unit one, 22-interface unit two, 23-feed port unit, 24-discharge port unit, 31-storage tank unit one, 32-filter one, 33-flow meter one, 34-metering pump one, 41-storage tank unit two, 42-filter two, 43-flow meter two, 44-metering pump two, 51-liquid storage unit, 52-circulation unit, 53-water inlet unit, 54-water outlet unit, 55-recovery unit. DETAILED DESCRIPTION

[0045] Embodiments of the present invention are described in detail below, examples of which are shown in the accompanying drawings, wherein the same or similar reference numerals throughout represent the same or similar elements or elements having the same or similar functions. The embodiments described below with reference to the accompanying drawings are exemplary and are intended to be used to explain the present invention, and should not be construed as limiting the present invention.

[0046] See also Figures 1 to 5 In the first aspect, the present invention provides a microchannel reactor for nitration reaction of naphthalene, comprising a microchannel reaction module 1, a channel module 2, a mixed acid preparation module 3, a naphthalene organic solution storage module 4 and a cooling module 5, wherein the cooling module 5 and the channel module 2 are respectively connected to the microchannel reaction module 1, and the mixed acid preparation module 3 and the naphthalene organic solution storage module 4 are respectively connected to the channel module 2;

[0047] The microchannel reaction module 1 is used for nitrification of naphthalene;

[0048] The channel module 2 is used to introduce nitric acid and naphthalene organic solution into the microchannel reaction module 1;

[0049] The mixed acid preparation module 3 is used to store nitric acid;

[0050] The naphthalene organic solution storage module 4 is used to store the naphthalene organic solution;

[0051] The cooling module 5 is used to cool the microchannel reaction module 1 .

[0052] In this embodiment, the microchannel reaction module 1 performs a nitration reaction on naphthalene; the channel module 2 introduces nitric acid and naphthalene organic solution into the microchannel reaction module 1; the mixed acid preparation module 3 stores nitric acid; the naphthalene organic solution storage module 4 stores naphthalene organic solution; and the cooling module 5 cools the microchannel reaction module 1. The present invention achieves efficient and precise control of the naphthalene nitration reaction process by integrating the microchannel reaction module 1, the channel module 2, the mixed acid preparation module 3, the naphthalene organic solution storage module 4 and the cooling module 5. Among them, the introduction of the cooling module 5 significantly improves the thermal management capability of the system, effectively solves the local overheating phenomenon, thereby reducing the generation of by-products, improving the purity and yield of the product, and thus solves the problem of an increase in by-products due to the local overheating phenomenon in the microchannel reactor during the nitration reaction production process of naphthalene.

[0053] Further, the channel module 2 includes an interface unit 1 21, an interface unit 22, a feed port unit 23 and a discharge port unit 24, the interface unit 1 21 and the interface unit 22 are respectively connected to the feed port unit 23, and the discharge port unit 24 and the feed port unit 23 are respectively connected to the microchannel reaction module 1;

[0054] The interface unit 21 is used to access nitric acid;

[0055] The interface unit 22 is used to access the naphthalene organic solution;

[0056] The feed port unit 23 is used to connect the nitric acid and naphthalene organic solutions to the microchannel reaction module 1;

[0057] The discharge port unit 24 is used to discharge the reacted materials out of the microchannel reaction module 1 .

[0058] In this embodiment, the interface unit 1 21 and the interface unit 2 22 are responsible for the access of nitric acid and naphthalene organic solution respectively, both of which have high sealing and corrosion resistance, ensuring the safety and stability of raw material transportation. The feed port unit 23 mixes the raw materials accessed by the interface unit 1 21 and the interface unit 2 22 to ensure that they reach a uniform state before entering the microchannel reaction module 1, and the discharge port unit 24 efficiently discharges the reacted materials from the microchannel reaction module 1. The efficient discharge device and filtering device inside it can effectively separate impurities and unreacted raw materials in the reaction product, and improve the purity and quality of the product.

[0059] Further, the mixed acid preparation module 3 includes a storage tank unit 31, a filter 32, a flow meter 33 and a metering pump 34, the storage tank unit 31, the filter 32, the flow meter 33 and the metering pump 34 are connected in sequence, and the metering pump 34 is connected to the interface unit 21;

[0060] The storage tank unit 1 31 is used to store nitric acid;

[0061] The filter 32 is used to filter nitric acid;

[0062] The flow meter 33 is used to measure the flow rate of nitric acid;

[0063] The metering pump 34 is used to control and adjust the flow rate of nitric acid.

[0064] In this embodiment, the storage tank unit 31 is used to store nitric acid; the filter 32 is used to filter the nitric acid; the flow meter 33 is used to measure the flow of nitric acid; and the metering pump 34 is used to control and adjust the flow of nitric acid. The safe storage, purification, accurate metering and stable delivery of nitric acid are achieved, providing a reliable and efficient raw material supply for the nitration reaction in the microchannel reactor system.

[0065] Further, the naphthalene organic solution storage module 4 includes a storage tank unit 2 41, a filter 2 42, a flow meter 2 43 and a metering pump 2 44, and the storage tank unit 2 41, the filter 2 42, the flow meter 2 43 and the metering pump 2 44 are connected in sequence, and the metering pump 2 44 is connected to the interface unit 22;

[0066] The storage tank unit 2 41 is used to store the naphthalene organic solution;

[0067] The filter 2 42 is used to filter the naphthalene organic solution;

[0068] The flow meter 2 43 is used to measure the flow rate of the naphthalene organic solution;

[0069] The metering pump 2 44 is used to control and adjust the flow rate of the naphthalene organic solution.

[0070] In this embodiment, the second storage tank unit 41 is used to store the naphthalene organic solution; the second filter 42 is used to filter the naphthalene organic solution; the second flow meter 43 is used to measure the flow of the naphthalene organic solution; and the second metering pump 44 is used to control and adjust the flow of the naphthalene organic solution. The safe storage, purification, accurate metering and stable delivery of the naphthalene organic solution are achieved, providing a reliable and efficient raw material supply for the nitration reaction in the microchannel reactor system.

[0071] Further, the cooling module 5 includes a liquid storage unit 51, a circulation unit 52, a water inlet unit 53 and a water outlet unit 54, and the liquid storage unit 51, the circulation unit 52, the water inlet unit 53 and the water outlet unit 54 are connected in sequence;

[0072] The liquid storage unit 51 is used to store cooling water;

[0073] The circulation unit 52 is used to drive the cooling water circulation to cool the microchannel reaction module 1;

[0074] The water inlet unit 53 is used to allow cooling water to enter the microchannel reaction module 1;

[0075] The water outlet unit 54 is used to discharge cooling water out of the microchannel reaction module 1 .

[0076] In this embodiment, the liquid storage unit 51 stores cooling water; the circulation unit 52 drives the cooling water to circulate to cool the microchannel reaction module 1; the water inlet unit 53 is used to allow cooling water to enter the microchannel reaction module 1; the water outlet unit 54 is used to discharge cooling water from the microchannel reaction module 1. The cooling water is driven to circulate in the system by the circulation unit 52, so as to effectively cool the microchannel reaction module 1, avoid the occurrence of local overheating, and improve the stability and efficiency of the nitration reaction. The cooling module 5 adopts a circulating cooling method, which reduces the consumption and waste of cooling water, and at the same time reduces the energy consumption and emissions of the system, which meets the requirements of environmental protection and sustainable development.

[0077] Furthermore, the cooling module 5 further includes a recovery unit 55, and the recovery unit 55 is connected to the water outlet unit 54 and to the liquid storage unit 51;

[0078] The recovery unit 55 is used to recover the cooling water of the water outlet unit 54 and return it to the liquid storage unit 51 .

[0079] In this embodiment, the recovery unit 55 recovers the cooling water of the water outlet unit 54 and returns the recovered cooling water to the liquid storage unit 51 , thereby realizing the recycling of cooling water.

[0080] See also Figure 6 In a second aspect, a microchannel reaction method for the nitration reaction of naphthalene, the microchannel reactor for the nitration reaction described in the first aspect, comprises the following steps:

[0081] S1 introduces nitric acid and naphthalene organic solution into microchannel reaction module 1 for nitration reaction;

[0082] Specifically, raw material preparation and pretreatment: nitric acid is taken out from the storage tank unit 1 31 of the mixed acid preparation module 3, and purified through the filter 1 32 to remove impurities and particulate matter therein; naphthalene organic solution is taken out from the storage tank unit 2 41 of the naphthalene organic solution storage module 4, and similar purification is performed through the filter 2 42; the flow rates of nitric acid and naphthalene organic solution are measured respectively by flowmeter 1 33 and flowmeter 2 43 to ensure that the two are mixed in a predetermined ratio.

[0083] Raw material mixing and introduction: nitric acid and naphthalene organic solution are respectively connected at interface unit 1 21 and interface unit 2 22 of channel module 2, and mixed through feed port unit 23; the mixed raw materials are stably introduced into microchannel reaction module 1 through feed port unit 23 to start the nitration reaction process.

[0084] S2 cools down the microchannel reaction module 1 to reduce the generation of by-products.

[0085] Specifically, before the nitration reaction starts or during the reaction, the circulation unit 52 of the cooling module 5 is started to drive the cooling water stored in the liquid storage unit 51 to circulate in the system; the cooling water enters the microchannel reaction module 1 through the water inlet unit 53 to cool the reaction module; according to the actual temperature requirement of the microchannel reaction module 1 and the progress of the nitration reaction, the flow rate and temperature of the cooling water are accurately controlled through the regulating function of the circulation unit 52; the cooling water exchanges heat with the reaction materials inside the microchannel reaction module 1, takes away the heat generated by the reaction, and avoids the occurrence of local overheating. After the reaction is completed or when the cooling water temperature reaches a preset value, the cooling water is discharged from the microchannel reaction module 1 through the water outlet unit 54; the discharged cooling water is recycled through the recovery unit 55, and after removing impurities and heat therein, it is returned to the liquid storage unit 51 for reuse.

[0086] Beneficial effects:

[0087] 1. By precisely controlling the flow and temperature of cooling water, the microchannel reaction module is effectively cooled, local overheating is avoided, thereby reducing the generation of by-products and improving the purity and yield of the product.

[0088] 2. The recycling and reuse of cooling water not only reduces the consumption and waste of water resources, but also reduces the energy consumption and emissions of the system, meeting the requirements of environmental protection and sustainable development.

[0089] 3. The entire cooling process achieves precise control of the nitration reaction process, improves the stability and efficiency of the reaction, and provides a strong guarantee for the efficient and precise control of the microchannel reactor in the nitration reaction production process of naphthalene.

[0090] The above disclosure is only a preferred embodiment of a microchannel reactor and a reaction method for the nitration reaction of naphthalene of the present invention. Of course, the scope of the present invention cannot be limited by this. Those of ordinary skill in the art can understand that all or part of the processes of the above-mentioned embodiments are implemented, and the equivalent changes made according to the claims of the present invention still fall within the scope of the invention.

Claims

1. A microchannel reactor for the nitration reaction of naphthalene, characterized in that: It comprises a microchannel reaction module, a channel module, a mixed acid preparation module, a naphthalene organic solution storage module and a cooling module, wherein the cooling module and the channel module are respectively connected to the microchannel reaction module, and the mixed acid preparation module and the naphthalene organic solution storage module are respectively connected to the channel module; The microchannel reaction module is used to perform nitration reaction on naphthalene; The channel module is used to introduce nitric acid and naphthalene organic solution into the microchannel reaction module; The mixed acid preparation module is used to store nitric acid; The naphthalene organic solution storage module is used to store the naphthalene organic solution; The cooling module is used to cool the microchannel reaction module.

2. The microchannel reactor for the nitration reaction of naphthalene as claimed in claim 1, wherein: The channel module comprises an interface unit 1, an interface unit 2, a feed port unit and a discharge port unit, wherein the interface unit 1 and the interface unit 2 are respectively connected to the feed port unit, and the discharge port unit and the feed port unit are respectively connected to the microchannel reaction module; The interface unit 1 is used to access nitric acid; The interface unit 2 is used to access the naphthalene organic solution; The feed port unit is used to connect the nitric acid and naphthalene organic solutions to the microchannel reaction module; The discharge port unit is used to discharge the reacted material out of the microchannel reaction module.

3. the microchannel reactor for the nitration reaction of naphthalene as claimed in claim 2, is characterized in that: The mixed acid preparation module comprises a storage tank unit 1, a filter 1, a flow meter 1 and a metering pump 1, wherein the storage tank unit 1, the filter 1, the flow meter 1 and the metering pump 1 are connected in sequence, and the metering pump 1 is connected to the interface unit 1; The storage tank unit 1 is used to store nitric acid; The filter 1 is used to filter nitric acid; The flow meter 1 is used to measure the flow rate of nitric acid; The metering pump 1 is used to control and adjust the flow rate of nitric acid.

4. The microchannel reactor for the nitration reaction of naphthalene as claimed in claim 2, characterized in that: The naphthalene organic solution storage module comprises a second storage tank unit, a second filter, a second flow meter and a second metering pump, wherein the second storage tank unit, the second filter, the second flow meter and the second metering pump are connected in sequence, and the second metering pump is connected to the second interface unit; The storage tank unit 2 is used to store the naphthalene organic solution; The filter 2 is used to filter the naphthalene organic solution; The flow meter 2 is used to measure the flow of the naphthalene organic solution; The metering pump 2 is used to control and adjust the flow rate of the naphthalene organic solution.

5. The microchannel reactor for the nitration reaction of naphthalene as claimed in claim 1, characterized in that: The cooling module comprises a liquid storage unit, a circulation unit, a water inlet unit and a water outlet unit, wherein the liquid storage unit, the circulation unit, the water inlet unit and the water outlet unit are connected in sequence; The liquid storage unit is used to store cooling water; The circulation unit is used to drive the cooling water circulation to cool the microchannel reaction module; The water inlet unit is used to allow cooling water to enter the microchannel reaction module; The water outlet unit is used to discharge cooling water out of the microchannel reaction module.

6. The microchannel reactor for the nitration reaction of naphthalene as claimed in claim 5, characterized in that: The cooling module further includes a recovery unit, which is connected to the water outlet unit and to the liquid storage unit; The recovery unit is used to recover the cooling water of the water outlet unit and return it to the liquid storage unit.

7. A microchannel reaction method for the nitration reaction of naphthalene, a microchannel reactor for the nitration reaction according to any one of claims 1 to 6, characterized in that: The following steps are involved: introducing nitric acid and naphthalene organic solution into the microchannel reaction module to carry out nitration reaction; The microchannel reaction module is cooled to reduce the generation of by-products.

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