CN114307902A - Microchannel reactor and method for producing dinitrotoluene - Google Patents

Microchannel reactor and method for producing dinitrotoluene Download PDF

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Publication number
CN114307902A
CN114307902A CN202210018778.XA CN202210018778A CN114307902A CN 114307902 A CN114307902 A CN 114307902A CN 202210018778 A CN202210018778 A CN 202210018778A CN 114307902 A CN114307902 A CN 114307902A
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reaction
heat exchange
microchannel reactor
sealing body
flow channel
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CN202210018778.XA
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CN114307902B (en
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黎孔富
孙大明
方明祥
方容
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Yidu Jovian Industry Co ltd
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Yidu Jovian Industry Co ltd
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Abstract

A microchannel reactor and a method for producing dinitrotoluene comprise a sealing body, wherein a plurality of reaction flow channels and a plurality of heat exchange flow channels which are sequentially communicated are arranged in the sealing body, and the reaction flow channels and the heat exchange flow channels are arranged in a staggered mode. The invention has compact structure and good selectivity, the heat released in the reaction can be removed efficiently, and the production safety level is improved essentially.

Description

Microchannel reactor and method for producing dinitrotoluene
Technical Field
The invention belongs to the field of organic compound manufacturing, and particularly relates to a microchannel reactor and a method for producing dinitrotoluene.
Background
Dinitrotoluene (DNT) is a major basic chemical that is widely used in the synthetic manufacturing of pharmaceuticals, paints, dyes, rubber and many other organic chemical products. It is commonly used for producing chemical products such as diaminotoluene, polyurethane, Toluene Diisocyanate (TDI), etc., and can also be directly used as explosive and propellant in military industry and used for producing trinitrotoluene (TNT). The annual production of dinitrotoluene is below million tons and increases rapidly at a rate of 4-8% per year. Two production ways of dinitrotoluene are available, one is to use nitrotoluene as raw material to react with nitric acid in mixed acid of sulfuric acid and nitric acid for a first time nitration to obtain dinitrotoluene, and the other is to use toluene as raw material to generate dinitrotoluene through a two-time nitration reaction. Two-stage nitration processes are commonly used in commercial processes, and a variety of dinitrotoluene isomers are commonly produced during the process. Because two isomers of 2, 4-dinitrotoluene and 2, 6-dinitrotoluene are generally used in chemical production, the target dinitrotoluene is obtained through a separation process after nitration production in industrial production. Typical process for producing dinitrotoluene the main process for producing dinitrotoluene is a two-stage nitration process, in which toluene is used as raw material and reacted in a nitric-sulfuric acid mixture to form dinitrotoluene by two-stage nitration of toluene. The first reaction step is: generating mononitrotoluene by the nitration of toluene; the second step is: dinitrotoluene is produced by nitration of mononitrotoluene.
The nitration process adopted in the production of dinitrotoluene uses inflammable, explosive and strong corrosive raw materials such as toluene, nitric acid, sulfuric acid and the like in the production process, a large amount of heat is released in the reaction process, and a kettle type reactor or a tubular reactor is adopted in the traditional production, so that the danger is high.
Disclosure of Invention
Based on the above, the invention provides the microchannel reactor and the method for producing the dinitrotoluene, which have the advantages of compact structure, good selectivity, high efficiency in removing heat released in reaction and substantially improved production safety level.
In order to solve the problems, the technical scheme of the invention is as follows:
a microchannel reactor for producing dinitrotoluene comprises a sealing body, wherein a plurality of reaction flow channels and a plurality of heat exchange flow channels which are sequentially communicated are arranged in the sealing body, and the reaction flow channels and the heat exchange flow channels are arranged in a staggered mode.
The seal body is made of submicron silicon carbide.
The sealing body comprises a plurality of reaction chips which are connected into a whole in a bonding mode.
The temperature probes are arranged in the sealing body, the PID valves are arranged on the pipelines communicated with the heat exchange flow channel, the temperature probes transmit detected signals to the controllers, and the controllers control the PID valves.
The invention has the beneficial effects that:
1. the invention has the advantages of compact structure, greatly reduced floor area compared with the traditional reactor, simple and convenient operation, good selectivity and high safety.
2. The invention can realize continuous production of the two-stage nitration reaction and improve the production efficiency.
3. The invention connects the basic reaction units together in parallel or series, can enlarge the productivity and realize the industrialized production.
Drawings
The invention is further described below with reference to the accompanying drawings:
figure 1 is a schematic structural view of the present invention,
figure 2 is a schematic perspective view of the present invention,
fig. 3 is a schematic partial cross-sectional structure of the present invention.
In the figure: the device comprises a raw material A inlet 1, a raw material B inlet 2, a reaction product flow outlet 3, a reaction flow channel 4, a heat exchange medium inlet 5, a heat exchange medium outlet 6, a heat exchange flow channel 7, a sealing body 8, a temperature probe 9, a PID valve 10, a controller 11, a partition plate 12 and a reaction hole 13.
Detailed Description
As shown in fig. 1 to 3, a microchannel reactor for producing dinitrotoluene comprises a sealing body 8, a plurality of reaction flow channels 4 and a plurality of heat exchange flow channels 7 which are sequentially communicated are arranged in the sealing body 8, the reaction flow channels 4 and the heat exchange flow channels 7 are serpentine, the reaction flow channels 4 and the heat exchange flow channels 7 are arranged in a staggered manner, one end of each reaction flow channel 4 is communicated with a raw material a inlet port 1 and a raw material B inlet port 2, the other end of each reaction flow channel 4 is a reaction product flow outlet 3, one end of each heat exchange flow channel 7 is a heat exchange medium inlet 5, and the other end of each heat exchange flow channel 7 is a heat exchange medium outlet 6.
The working process of the invention is as follows: the raw material A, B enters the reaction flow channel 4 through a pump, steam or cooling water is simultaneously fed into the heat exchange flow channel 7, and the reacted material flows out through a PTFE pipe connected with the product flow outlet 3.
The seal body 8 is made of sub-micron silicon carbide. The material has strong corrosion resistance at high temperature.
The sealing body 8 comprises a plurality of reaction chips, each reaction chip is connected into a whole in a bonding mode, the two sides of each reaction chip are connected with a feeding cover plate and a discharging cover plate which are respectively connected with metal, and the reaction channels are not in contact with the metal.
The method for producing the sealing body 8 comprises the steps of firstly processing a reaction groove and a heat exchange groove on a silicon carbide plate, wherein the reaction groove and the heat exchange groove are respectively positioned on the front surface and the back surface of the silicon carbide plate, then overlapping a plurality of silicon carbide plates according to the processed reaction groove and the heat exchange groove, so that two opposite reaction grooves can be combined into a reaction flow channel 4, two opposite heat exchange grooves can be combined into a heat exchange flow channel 7, and the silicon carbide plates (the silicon carbide plates are reaction chips) are connected into a whole in a bonding mode. Therefore, the heat exchange efficiency can be greatly improved, and the leakage risk can be thoroughly eliminated.
The temperature probes 9 are arranged in the sealing body 8, the PID valves 10 are arranged on the pipeline communicated with the heat exchange flow channel 7, the temperature probes 9 transmit detected signals to the controllers 11, and the controllers 11 control the PID valves 10. The temperature of the sealing body 8 is detected by the temperature probe 9 in real time, and the opening degree of the PID valve 10 is controlled by the controller 11 according to the temperature so as to control the flow of the heat exchange medium and adjust the reaction temperature.
The sealing body 8 includes a plurality of sealing bodies 8, and the sealing bodies 8 are connected in parallel. The production capacity can be increased by connecting a plurality of sealing bodies 8 in parallel as shown in fig. 1.
A partition plate 12 is provided in the reaction flow path 4, a plurality of reaction holes 13 are provided in the partition plate 12, and the distance between the reaction holes 13 is gradually shortened along the reaction flow path 4. The partition plate 12 divides the heat exchange flow passage 7 into two flow passages, the raw material A, B enters the reaction flow passage 4 from the two flow passages respectively, when the raw material A, B enters the reaction flow passage 4 from the flow passages on the two sides of the partition plate 12 respectively, the raw material is firstly subjected to contact reaction at the reaction holes 13 on the partition plate 12 to consume a part of reaction heat, then along with the shortening of the distance between the reaction holes 13, the contact frequency of the raw material A, B is gradually increased, the heat generated by the reaction is increased, and the raw material A, B is fully mixed until the partition plate 12 disappears. The effect of this arrangement is: the raw material A, B reacts violently when entering the partition plate 12, so that the inlet temperature of the reaction flow channel 4 is the highest, leakage is easily caused by local expansion of the flow channel due to high temperature, after the partition plate 12 is added, the reaction of the raw material A, B is buffered, the reaction can be started gradually, heat generated by the reaction is converged to the center of the sealing body 8, and the probability of raw material leakage is reduced.

Claims (7)

1. A microchannel reactor for producing dinitrotoluene, comprising: the sealing structure comprises a sealing body (8), wherein a plurality of reaction flow channels (4) which are sequentially communicated and a plurality of heat exchange flow channels (7) which are sequentially communicated are arranged in the sealing body (8), and the reaction flow channels (4) and the heat exchange flow channels (7) are arranged in a staggered mode.
2. A microchannel reactor for producing dinitrotoluene according to claim 1 wherein: the sealing body (8) is made of submicron silicon carbide.
3. A microchannel reactor for producing dinitrotoluene according to claim 2 wherein: the sealing body (8) comprises a plurality of reaction chips which are connected into a whole in a bonding mode.
4. A microchannel reactor for producing dinitrotoluene according to claim 1 wherein: the temperature probes (9) are arranged in the sealing body (8), PID valves (10) are installed on a pipeline communicated with the heat exchange flow channel (7), detected signals are transmitted to the controllers (11) by the temperature probes (9), and the PID valves (10) are controlled by the controllers (11).
5. A microchannel reactor for producing dinitrotoluene according to any one of claims 1 to 4 wherein: the sealing body (8) comprises a plurality of sealing bodies (8), and the sealing bodies (8) are connected in parallel.
6. A microchannel reactor for producing dinitrotoluene according to any one of claims 1 to 4 wherein: a partition plate (12) is arranged in the reaction flow channel (4), a plurality of reaction holes (13) are formed in the partition plate (12), and the distance between every two adjacent reaction holes (13) is gradually shortened along the reaction flow channel (4).
7. A manufacturing method of a microchannel reactor is characterized by comprising the following steps: the method comprises the steps of machining reaction grooves and heat exchange grooves on two sides of a silicon carbide plate respectively, then overlapping and connecting a plurality of silicon carbide plates together in a bonding mode, enabling two opposite reaction grooves to be combined into a reaction flow channel (4), and enabling two opposite heat exchange grooves to be combined into a heat exchange flow channel (7).
CN202210018778.XA 2022-01-09 2022-01-09 Microchannel reactor and method for producing dinitrotoluene Active CN114307902B (en)

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Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030226806A1 (en) * 2002-06-11 2003-12-11 Young Lincoln C. Methods and devices for liquid extraction
US20040028580A1 (en) * 2002-07-12 2004-02-12 Tosoh Corporation Fine channel device and a chemically operating method for fluid using the device
US20040228882A1 (en) * 2003-05-16 2004-11-18 Dongming Qiu Process for forming an emulsion using microchannel process technology
US20130041050A1 (en) * 2011-07-19 2013-02-14 Robert Luzenski Microchannel reactors and fabrication processes
CN204193919U (en) * 2014-10-27 2015-03-11 大连韦德生化科技有限公司 A kind of sectional temperature-controlled reactor assembly that declines with heat-exchange system
CN105107443A (en) * 2015-09-15 2015-12-02 南京新威尔电气有限公司 Efficient mixing heat exchange micro-channel reactor
CN108554326A (en) * 2018-03-02 2018-09-21 四川大学 A kind of grade passage aisle reactor for C4 alkylated reactions
CN108704591A (en) * 2018-08-07 2018-10-26 山东金德新材料有限公司 A kind of integrated silicon carbide microchannel reactor of collection heat-exchange system
CN110961060A (en) * 2018-09-30 2020-04-07 中国石油化工股份有限公司 Micro-channel reactor
CN211487612U (en) * 2019-11-29 2020-09-15 北京渤乐科技有限公司 Pressureless sintering carborundum reactor
CN214076587U (en) * 2020-12-18 2021-08-31 山东诺为制药流体系统有限公司 Combined high-pressure-resistant serial plate type reactor

Patent Citations (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20030226806A1 (en) * 2002-06-11 2003-12-11 Young Lincoln C. Methods and devices for liquid extraction
US20040028580A1 (en) * 2002-07-12 2004-02-12 Tosoh Corporation Fine channel device and a chemically operating method for fluid using the device
US20040228882A1 (en) * 2003-05-16 2004-11-18 Dongming Qiu Process for forming an emulsion using microchannel process technology
US20130041050A1 (en) * 2011-07-19 2013-02-14 Robert Luzenski Microchannel reactors and fabrication processes
CN204193919U (en) * 2014-10-27 2015-03-11 大连韦德生化科技有限公司 A kind of sectional temperature-controlled reactor assembly that declines with heat-exchange system
CN105107443A (en) * 2015-09-15 2015-12-02 南京新威尔电气有限公司 Efficient mixing heat exchange micro-channel reactor
CN108554326A (en) * 2018-03-02 2018-09-21 四川大学 A kind of grade passage aisle reactor for C4 alkylated reactions
CN108704591A (en) * 2018-08-07 2018-10-26 山东金德新材料有限公司 A kind of integrated silicon carbide microchannel reactor of collection heat-exchange system
CN110961060A (en) * 2018-09-30 2020-04-07 中国石油化工股份有限公司 Micro-channel reactor
CN211487612U (en) * 2019-11-29 2020-09-15 北京渤乐科技有限公司 Pressureless sintering carborundum reactor
CN214076587U (en) * 2020-12-18 2021-08-31 山东诺为制药流体系统有限公司 Combined high-pressure-resistant serial plate type reactor

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Denomination of invention: A microchannel reactor and method for producing dinitrotoluene

Granted publication date: 20230901

Pledgee: Bank of China Limited by Share Ltd. Three Gorges Branch

Pledgor: YIDU JOVIAN INDUSTRY CO.,LTD.

Registration number: Y2024980026986