CN114394902A - Production process and production system of N-methyl-p-nitroaniline - Google Patents
Production process and production system of N-methyl-p-nitroaniline Download PDFInfo
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- CN114394902A CN114394902A CN202111484645.3A CN202111484645A CN114394902A CN 114394902 A CN114394902 A CN 114394902A CN 202111484645 A CN202111484645 A CN 202111484645A CN 114394902 A CN114394902 A CN 114394902A
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- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/04—Preparation of compounds containing amino groups bound to a carbon skeleton by substitution of functional groups by amino groups
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Abstract
The invention discloses a production process and a production system of N-methyl-p-nitroaniline. The disclosed production process comprises: reacting a nitrofluorobenzene ethanol solution with a methylamine water solution under the conditions of an acoustic resonance environment, normal pressure and 70-77 ℃, starting to collect a reaction material containing N-methyl-p-nitroaniline after the reaction is carried out for 10-50 min, wherein the acoustic resonance environment conditions comprise a resonance frequency of 58-65 Hz, a phase difference range of 0.01-0.20 and an acceleration range of 50-1000 m.s‑2. The invention generates macro mixing and micro vortex in the reaction system through the resonance external field generated by system resonance to realize active mixing reinforcement, the combination of the two can reduce the reaction limit of the transfer process and shorten the reaction time, and simultaneously can realize high-efficiency dispersion of solid-phase particles under the resonance condition, thereby solving the problem of continuous preparation of solid-containing systemsThe phenomena of wall sticking and blockage in the preparation process can realize the efficient and continuous preparation of the N-methyl-p-nitroaniline by matching with a tubular reactor.
Description
Technical Field
The invention relates to a production technology of N-methyl-p-nitroaniline, in particular to an acoustic resonance production process and a production system of the N-methyl-p-nitroaniline.
Background
N-methyl-p-nitroaniline is an important organic chemical raw material and dye intermediate, is widely used in the industries of medicine, spice, electroplating and the like, is an important stabilizer, is one of important raw materials of nitrate-containing propellants at home and abroad at present, plays an increasingly important role in the field of propellant raw materials, and has better energy contribution to the propellants than that of a conventional stabilizer C2. N-methyl-p-nitroaniline can also be used as a standard for detecting other substances, and is more and more concerned by people now.
The N-methyl-p-nitroaniline is usually prepared by adopting a traditional kettle type process, the reaction is carried out for more than 3 hours at 170 ℃ and 1.7MPa, and the product is subjected to post-treatment to obtain the N-methyl-p-nitroaniline product. The preparation process of the N-methyl-p-nitroaniline can generate solid phase, possibly generate wall sticking and blocking phenomena, the particle size of the product in use needs no more than 5 percent of residues on a sieve with the particle size of 450 mu m, and the product often needs post-treatment to meet the requirements.
Disclosure of Invention
In view of the defects or shortcomings of the prior art, the invention provides a production process of N-methyl-p-nitroaniline.
Therefore, the production process of the N-methyl-p-nitroaniline provided by the invention comprises the following steps:
reacting a nitrofluorobenzene ethanol solution with a methylamine water solution under the conditions of an acoustic resonance environment, normal pressure and 70-77 ℃, starting to collect N-methyl-p-nitroaniline from a reaction material after the reaction is carried out for 10-50 min, wherein the acoustic resonance environment conditions comprise a resonance frequency of 58-65 Hz, a phase difference range of 0.01-0.20 and an acceleration range of 50-1000 m.s-2。
The invention also provides a production system for realizing the production process. To this end, the system provided by the invention comprises: a nitrofluorobenzene storage tank, a methylamine aqueous solution storage tank, an anhydrous ethanol storage tank, an acoustic resonance generator and a continuous reactor; the continuous reactor is arranged on an acoustic resonance generator;
the continuous reactor comprises a shell, a first cold and hot medium cavity is arranged in the shell, a first cold and hot medium inlet and outlet is arranged on the cold and hot medium cavity, a reaction tube is arranged in the cold and hot medium cavity, a first reaction raw material inlet is arranged at one end of the reaction tube, and a first reaction material outlet is arranged at the other end of the reaction tube; the nitrofluorobenzene ethanol solution storage tank, the methylamine water solution storage tank and the anhydrous ethanol storage tank are respectively connected with the reaction raw material inlet; or, the continuous reactor comprises a reactor body, a plurality of reaction vessels are arranged in the reactor body, overflow holes or overflow grooves for communicating two adjacent reaction vessels are arranged between the adjacent reaction vessels, the plurality of reaction vessels are sequentially connected in series through the overflow holes or the overflow grooves, no overflow hole or overflow groove is arranged between the reaction vessel positioned at the head part and the reaction vessel positioned at the tail part in the plurality of reaction vessels connected in series, and the overflow hole or overflow groove is positioned at the top part of the corresponding reaction vessel.
Further, a second cold and hot medium containing cavity is arranged in the reactor body, a second cold and hot medium inlet and outlet is formed in the second cold and hot medium containing cavity, and the plurality of reaction containers are located in the cold and hot medium containing cavity or cold and hot media entering the cold and hot medium containing cavity flow through the outer wall of each reaction container.
Optionally, the reactor body is a circular cylinder, a square cylinder, a polygonal cylinder or an irregular cylinder, and the depths of the reaction vessels are all arranged along the axial direction of the reactor body.
Optionally, the plurality of reaction vessels are uniformly distributed along the circumference of the reactor body.
The reactor further comprises a cover body used for sealing each reaction vessel in the reactor body, wherein a second reaction raw material inlet and a second reactant outlet are arranged on the cover body, the second reaction raw material inlet is communicated with the first reaction vessel in the plurality of reaction vessels connected in series, and the second reactant outlet is communicated with the tail reaction vessel.
Further, the cover body is matched with the top of the reactor body in shape.
Optionally, the volume of each reaction container is 30-50 ml, the height-diameter ratio is 0.5-2, and the ratio of the aperture of the overflow hole or the depth of the overflow groove to the depth of the reaction container is in the range: 0.1-0.5: 1.
Furthermore, a plurality of baffle plates are arranged in the first cold and hot medium containing cavity.
Furthermore, the reaction tubes are arranged in an S shape, a Z shape or a spiral shape in the cold and hot medium containing cavity.
Optionally, the inner diameter of the reaction tube is 1-50 mm, the length of the pipeline is 50-5000 mm, and the flow rate of the reaction tube is 2-250 ml/min.
The production system of the present invention further comprises a filter for filtering the reactant and a dryer for drying the filtered cake.
The process disclosed by the invention uses the acoustic resonance technology to form macroscopic mixing and microscopic vortex to strengthen the reaction transfer process, so that the limitation of the transfer process on the reaction is reduced, the reaction time of the product can be shortened to be within 0.5h from 3h, the reaction time is shortened by 83%, the production efficiency is obviously improved, the pressure is reduced to normal pressure from 1.7MPa, the temperature is reduced to 77 ℃ from 170 ℃, the process conditions are more moderate, and the process is suitable for producing 100 g-100 kg-grade products;
in addition, under the action of the acoustic resonance external field, solid-phase particles generated in the reaction process are uniformly distributed in the reaction medium, the dispersion effect is good, the phenomena of wall adhesion and blockage are avoided, and the continuous production of the N-methyl-p-nitroaniline is facilitated;
meanwhile, the granularity D97 of the N-methyl-p-nitroaniline products prepared by the process is less than 450 mu m, meets the granularity requirement of GJB 8494-.
The process technology provided by the invention carries out field strengthening on the reaction system, and has no obvious size amplification effect in the size range of the invention, thereby being beneficial to engineering amplification and flexible tissue production.
Drawings
FIG. 1 is a schematic diagram of a generation system of the present invention.
FIG. 2 is a schematic diagram showing an example of the structure of a continuous reactor of the present invention.
FIG. 3 is another example of the structure of a continuous reactor according to the present invention.
Fig. 4 is a cross-sectional view of fig. 3.
Detailed Description
Unless otherwise specified, the terms or methods herein are understood or implemented using known related methods as would be recognized by one of ordinary skill in the relevant art.
The terms of direction or orientation such as axial, radial, circumferential, top, deep (high), head and tail are consistent with the corresponding directions or orientations in the drawings, it should be noted that the specific directions or orientations in the drawings are a specific example of the present invention, and those skilled in the art can make equivalent conversions according to the disclosure of the present invention, and these converted schemes all belong to the protection scope of the present invention.
The acoustic resonance generator described herein may be used in connection with the apparatus disclosed in the prior art, such as the apparatus disclosed in ZL 201710058168.1.
In the preparation process, the aqueous solution of nitrofluorobenzene and methylamine is used as raw materials, ethanol is used as a solvent, the selection of the raw materials, the dosage relationship among the raw materials and the collection or recovery method (such as filtration, drying and the like) of the product can be determined by referring to the existing preparation method of related products. Example (c): the mol ratio of p-nitrofluorobenzene to methylamine to ethanol is as follows: 1: 2.1-3.0: 11-16.
The particle size analysis shown in the following examples was performed by using a laser particle sizer to obtain D97, wherein D97 represents the particle size corresponding to 97% of the cumulative particle size distribution of the sample.
Example 1:
as shown in fig. 1, the continuous reaction system of this embodiment comprises three reaction raw material storage tanks 1, a continuous reactor 3, an acoustic resonance generator (not shown in the figure), a temperature control system 6, a filter 4, and a dryer 5; the continuous reactor is arranged on the acoustic resonance generator, each raw material storage tank is respectively connected with a raw material inlet on the continuous generator through a delivery pump 2, a reactant outlet is connected with a filter, and the filter is connected with a dryer, wherein a temperature control system can adopt related products in the prior art and is used for controlling the reaction temperature in the continuous reactor; wherein, the raw material tank, the delivery pump and the reactor are directly connected by using a cutting sleeve and a tetrafluoro pipeline, the reacted materials can be directly collected in a corresponding container after flowing out of the reactor, and the filter and the dryer are not directly connected with other parts.
The structure of the continuous reactor of this embodiment is shown in fig. 2, and includes a housing 33, a cold and hot medium accommodating chamber 31 is arranged in the housing, the cold and hot medium accommodating chamber is externally provided with a cold and hot medium inlet 36, the cold and hot medium accommodating chamber is internally provided with an S-shaped reaction tube 35, one end of the reaction tube is externally provided with a reactant inlet 34, and the other end of the reaction tube is externally provided with a reactant outlet 34. In some schemes, in order to enhance the heat exchange effect between the cold and hot media and the reactant, a baffle plate 32 is further arranged in the cold and hot medium accommodating cavity. As shown in fig. 2, a plurality of cold and hot medium alternating current plates are arranged in a staggered manner. In the specific scheme, the inner diameter and the length of the reaction tube can be designed according to the reaction characteristics and the reaction duration of the prepared substances. For example, the inner diameter of the reaction tube is 1-50 mm, the length of the pipeline is 50-5000 mm, and the flow rate of the reaction tube is 2-250 ml/min.
The production process of the system adopting the embodiment comprises the following steps:
(1) dissolving p-nitrofluorobenzene in ethanol (such as the mass fraction of the p-nitrofluorobenzene is 15.0-20.0%) and then placing the solution in a raw material tank to serve as a mobile phase A, wherein a methylamine aqueous solution (such as the mass fraction of the commercially available product is 40 wt%) is placed in the raw material tank to serve as a mobile phase B, and anhydrous ethanol is used in a raw material tank C;
(2) filling the reactor with ethanol by using a delivery pump, setting the pressure in the reactor to be normal pressure, setting the temperature of a jacket of the reactor to be 70-77 ℃, calculating and setting the flow rates of a mobile phase A and a mobile phase B after the temperature is stable, and starting the delivery pump;
(3) starting an acoustic resonance reaction platform, scanning frequency within the range of 58-65 Hz to determine resonance frequency, and using the resonance frequencyThe working frequency is controlled by adjusting the acceleration of a phase difference adjusting system to control the reaction strengthening degree, the phase difference range is 0.01-0.20, and the acceleration range is 50-1000 m.s-2；
(4) And collecting the reacted materials by using a container, filtering the materials by using a filter, and drying a filter cake after filtering in a dryer to obtain the N-methyl-p-nitroaniline product.
Example 2:
this embodiment differs from embodiment 1 in that the continuous reactor adopts a reactor of the structure shown in FIGS. 3 and 4, and the continuous reactor of this embodiment comprises a reactor body 3-1 of a circular cylindrical shape and a lid body 3-6 of a circular plate shape; a cold and hot medium (such as hot water and cold water) containing cavity or jacket 3-4 is arranged in the reactor body, two cold and hot medium inlets and outlets 3-5 are arranged outwards, each stage of reaction vessel 3-2 is arranged in the hot medium containing cavity or jacket and is uniformly distributed in a ring shape along the axial direction, an overflow groove 3-3 is arranged at the top of a partition wall of the adjacent reaction vessel to communicate the adjacent reaction vessels, a plurality of reaction vessels are sequentially connected in series through the overflow groove, but no overflow groove is arranged between the reaction vessels at the head part and the tail part; the disc-shaped cover body is provided with a raw material inlet 3-7 and a reactant outlet 3-8, after the cover body is covered on the reactor body, the raw material inlet is communicated with the first reaction vessel, the reactant outlet is communicated with the tail reaction vessel, and in the embodiment, the cover body is fixedly connected with the reactor body through a plurality of mounting holes 3-9. When the device is used, reaction raw materials are added into the first reaction container of a plurality of reaction containers connected in series at one time or continuously and controllably, reaction materials sequentially overflow into the subsequent reaction containers through overflow holes or overflow grooves until reaching the tail reaction container, the products are collected from the tail reaction container after the materials are reasonably reacted by controlling the size or/and time of the reaction containers, and the circulation of cold and hot media is realized through the inlet and the outlet of the cold and hot media.
In the specific scheme, the stage number of the reaction container, the volume of the reaction container and the depth of the overflow groove or the aperture of the overflow hole can be designed according to the reaction characteristics and the reaction duration of the prepared substances. For example, the number of the reactor stages is 4-10, each stage of reactor 3-2 is in a cylindrical form, the volume of each stage of reactor is 30-50 ml, the height-diameter ratio is 0.5-2, and the ratio of the depth of an overflow groove between adjacent reactors to the height of the reactor is as follows: 0.1-0.5: 1.
Example 3:
this example produced N-methyl-p-nitroaniline using the system shown in example 1, which had a reaction tube with an inner diameter of 20mm and a length of 1000 mm. The specific process comprises the following steps:
149.4g of p-nitrofluorobenzene is dissolved in 1078.8ml of absolute ethyl alcohol to be used as a material A, 195.9g of methylamine aqueous solution with the mass fraction of 40% is weighed to be used as a material B, 1000ml of absolute ethyl alcohol is weighed to be used as a material C, and the materials A, B, C are respectively placed in a raw material tank with stirring;
setting the normal pressure and the temperature in the reaction tube to be 70 ℃, setting the flow of the delivery pump C to be 20ml/min, turning on the delivery pump C for 20min, then turning off the delivery pump C, and filling the reactor and the transportation pipeline with ethanol;
setting the flow rate of the material A to be 17.65ml/min, the flow rate of the material B to be 3.28ml/min, correspondingly setting the residence time to be 15min, starting an acoustic resonance reaction platform, scanning within the range of 58-65 Hz to determine the resonance frequency to be 63.9Hz, setting the phase difference to be 0.09, and setting the acceleration of the system to be 530m/s at the moment2Taking a 15min sample after the reaction runs stably for 30min (first sampling), taking a 15min sample every 30min, taking 2 times (second and third sampling), wherein the product is yellow suspension, the whole reaction system has no blockage phenomenon, filtering the suspension, drying a filter cake at 60 ℃ overnight to obtain a dry N-methyl-p-nitroaniline product, weighing to obtain a yield, determining the purity by liquid chromatography, and obtaining a particle size D97 by particle size analysis, wherein the first yield of the sample is 92.3%, the purity is 99.3%, and the D97 is 125.43 mu m; the yield of the second sample is 92.5%, the purity is 99.7%, and D97 is 125.76 μm; the yield of sample three was 92.5%, the purity was 99.1%, and the D97 was 126.64 μm.
After sampling and mixing, performing characterization through nuclear magnetic spectrum, mass spectrum, infrared spectrum and element analysis:
nuclear magnetic spectrum:13C NMR(DMSO-d6，125MHz)，δ：155.242，135.509，126.134，110.377，29.120；
1H NMR(DMSO-d6，125MHz)：2.7954，6.5966，6.6152，7.3079，7.9992，8.0177；
infrared spectrum: IR (KBr) v 3365,1598,1542,1460,1303,1104,833;
mass spectrum m/z (%): 152;
elemental analysis: molecular formula C7H8N2O2
Theoretical value: c55.26, H5.263, N18.42
Measured value: c55.24, H5.270, N18.58.
Example 4:
in this example, the production system shown in example 2 was used to prepare N-methyl-p-nitroaniline, the number of reactor stages in this example was 8, the reactor volumes of the respective stages were 40ml, the aspect ratio was 1:1, the total reaction volume was 320ml, and the depth of the groove was 0.1 of the depth of the corresponding reactor.
Using the same material ratio, flow rate and temperature as in example 3, the resonant frequency was determined to be 64.0Hz, the phase difference was set to 0.028, and the acceleration of the system was 500m/s2Taking a 15min sample after the reaction runs for 30min (first sampling), taking a 15min sample every 30min, taking 2 times (second and third sampling), wherein the product is yellow suspension, the reactor has no blockage phenomenon, filtering the suspension, drying at 60 ℃ overnight to obtain a dry N-methyl-p-nitroaniline product, weighing to obtain the yield, determining the purity by liquid chromatography, and analyzing the particle size to obtain the particle size D97. Sample one yield was 94.7%, purity was 99.5%, D97 was 132.41 μm; the yield of the second sample is 93.4%, the purity is 99.2%, and D97 is 134.25 μm; the yield of sample three was 95.6%, the purity was 99.6%, and the D97 was 132.76. mu.m.
Example 5:
this example produced N-methyl-p-nitroaniline using the system shown in example 1, which had a reaction tube with an inner diameter of 10mm and a length of 150 mm. The specific process comprises the following steps:
dissolving 24.8g of p-nitrofluorobenzene in 124.2ml of absolute ethyl alcohol to obtain a material A, weighing 29.8g of methylamine aqueous solution with the mass fraction of 40% to obtain a material B, weighing 500ml of absolute ethyl alcohol to obtain a material C, and respectively placing materials A, B, C in a material tank with stirring;
setting the normal pressure and the temperature in the reactor to be 75 ℃, setting the flow of a delivery pump C to be 20ml/min, starting the delivery pump C for 2min, then closing the delivery pump C, and filling the reactor and a transport pipeline with ethanol;
setting the flow rate of the material A to be 0.38ml/min, the flow rate of the material B to be 0.09ml/min, correspondingly setting the residence time to be 25min, starting an acoustic resonance reaction platform, scanning within the range of 58-65 Hz to determine the resonance frequency to be 64.5Hz, setting the phase difference to be 0.02, and setting the acceleration of the system to be 200m/s at the moment2Taking a 25min sample (first sampling) after the reaction runs for 50min stably, taking a 25min sample every 50min, taking 2 times (second and third sampling), wherein the product is yellow suspension, the whole reaction system has no blockage phenomenon, filtering the suspension, drying at 60 ℃ overnight to obtain a dry N-methyl-p-nitroaniline product, weighing to obtain a yield, determining the purity by liquid chromatography, and obtaining a particle size D97 by particle size analysis, wherein the yield of the sample is 95.8%, the purity is 99.2%, and the D97 is 120.86 mu m; the yield of the second sample is 96.0%, the purity is 99.5%, and D97 is 119.74 μm; the yield of sample three was 95.8%, the purity was 99.2%, and the D97 was 120.13. mu.m.
Example 6:
this example produced N-methyl-p-nitroaniline using the system shown in example 1, which had a reaction tube with an inner diameter of 50mm and a length of 4500 mm. The specific process comprises the following steps:
dissolving 5100g of p-nitrofluorobenzene in 28350ml of absolute ethyl alcohol to serve as a material A, weighing 6700g of methylamine aqueous solution with the mass fraction of 40% to serve as a material B, weighing 10000ml of absolute ethyl alcohol to serve as a material C, and respectively placing A, B, C in a material tank with stirring;
setting the normal pressure and the temperature in the reactor to be 77 ℃, setting the flow of the delivery pump C to be 100ml/min, turning on the delivery pump C for 100min, then turning off the delivery pump C, and filling the reactor and a transport pipeline with ethanol;
setting the flow rate of the material A to be 178.71ml/min, the flow rate of the material B to be 42.07ml/min and the corresponding residence time to be 40min, starting an acoustic resonance reaction platform, scanning within the range of 58-65 Hz to determine the resonance frequency to be 59.1Hz, setting the phase difference to be 0.18, and setting the acceleration of the system to be 800m/s at the moment2The reaction is stableAfter the operation is carried out for 80min, a sample of 40min is taken (first sampling), then a sample of 40min is taken every 80min, 2 times (second sampling and third sampling) are taken, the product is yellow suspension, the whole reaction system has no blockage phenomenon, the obtained suspension is filtered and dried at 60 ℃ overnight to obtain a dry N-methyl-p-nitroaniline product, the yield is obtained after weighing, the purity is determined by liquid chromatography, the particle size D97 is obtained by particle size analysis, the yield of the sample is 98.3%, the purity is 99.6%, and the D97 is 128.74 mu m; the yield of the second sample is 97.9%, the purity is 99.7%, and D97 is 129.38 μm; the yield of sample three was 98.0%, the purity was 99.2%, and the D97 was 127.97 μm.
Claims (12)
1. A production process of N-methyl-p-nitroaniline is characterized by comprising the following steps:
reacting a nitrofluorobenzene ethanol solution with a methylamine water solution under the conditions of an acoustic resonance environment, normal pressure and 70-77 ℃, starting to collect N-methyl-p-nitroaniline from a reaction material after the reaction is carried out for 10-50 min, wherein the acoustic resonance environment conditions comprise a resonance frequency of 58-65 Hz, a phase difference range of 0.01-0.20 and an acceleration range of 50-1000 m.s-2。
2. A production system for implementing the production process of claim 1, wherein the system comprises: a nitrofluorobenzene storage tank, a methylamine aqueous solution storage tank, an anhydrous ethanol storage tank, an acoustic resonance generator and a continuous reactor; the continuous reactor is arranged on an acoustic resonance generator;
the continuous reactor comprises a shell, a first cold and hot medium cavity is arranged in the shell, a first cold and hot medium inlet and outlet is arranged on the cold and hot medium cavity, a reaction tube is arranged in the cold and hot medium cavity, a first reaction raw material inlet is arranged at one end of the reaction tube, and a first reaction material outlet is arranged at the other end of the reaction tube; the nitrofluorobenzene ethanol solution storage tank, the methylamine water solution storage tank and the anhydrous ethanol storage tank are respectively connected with the reaction raw material inlet; or, the continuous reactor comprises a reactor body, a plurality of reaction vessels are arranged in the reactor body, overflow holes or overflow grooves for communicating two adjacent reaction vessels are arranged between the adjacent reaction vessels, the plurality of reaction vessels are sequentially connected in series through the overflow holes or the overflow grooves, no overflow hole or overflow groove is arranged between the reaction vessel positioned at the head part and the reaction vessel positioned at the tail part in the plurality of reaction vessels connected in series, and the overflow hole or overflow groove is positioned at the top part of the corresponding reaction vessel.
3. The production system as claimed in claim 2, wherein a second hot and cold medium accommodating chamber is provided in the reactor body, the hot and cold medium accommodating chamber is provided with a second hot and cold medium inlet and outlet, and the hot and cold medium in the plurality of reaction vessels or entering the hot and cold medium accommodating chamber flows through the outer wall of each reaction vessel.
4. The production system of claim 2, wherein the reactor body is a circular cylinder, a square cylinder, a polygonal cylinder, or an irregular cylinder, and the plurality of reaction vessels are all arranged in the axial direction of the reactor body.
5. The production system of claim 2, wherein the plurality of reaction vessels are evenly distributed along a circumference of the reactor body.
6. The production system of claim 2, further comprising a cover for enclosing each reaction vessel, wherein the cover is provided with a second reaction raw material inlet and a second reactant outlet, the second reaction raw material inlet is communicated with a first reaction vessel of the plurality of reaction vessels connected in series, and the second reactant outlet is communicated with a tail reaction vessel.
7. The production system of claim 6, wherein the cover is shaped to fit the top of the reactor body.
8. The production system of claim 2, wherein each reaction vessel has a volume of 30 to 50ml, a height-diameter ratio of 0.5 to 2, and a ratio of an aperture of the overflow hole or an overflow groove depth to a reaction vessel depth is in a range of: 0.1-0.5: 1.
9. The production system as claimed in claim 2, wherein a plurality of baffles are provided in the first hot and cold medium receiving chamber.
10. The production system of claim 2, wherein the reaction tubes are arranged in an S-shaped, Z-shaped or spiral shape in the cold and hot medium accommodating chamber.
11. The production system of claim 2, wherein the reaction tube has an inner diameter of 1 to 50mm, a length of 50 to 5000mm, and a flow rate of 2 to 250 ml/min.
12. The production system of claim 2, further comprising a filter for filtering the reactant and a dryer for drying the filtered cake.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423895A (en) * | 2008-12-15 | 2009-05-06 | 森松（江苏）重工有限公司 | Overflow type multi-compartment autoclave and process thereof |
| CN102888283A (en) * | 2012-10-11 | 2013-01-23 | 华南理工大学 | Multi-frequency ultrasonic radiation overflow groove continuous biodiesel production device |
| CN103113234A (en) * | 2013-01-21 | 2013-05-22 | 湖北东方化工有限公司 | Method for synthesizing N-methyl paranitroaniline |
| CN106025203A (en) * | 2016-05-27 | 2016-10-12 | 湖南海纳新材料有限公司 | Preparation method of ternary precursor for continuous narrow distributed lithium battery |
| CN209901249U (en) * | 2019-04-30 | 2020-01-07 | 山东道可化学有限公司 | 3, 4-dichloro benzotrifluoride continuous production equipment |
| CN113441100A (en) * | 2021-07-22 | 2021-09-28 | 西安近代化学研究所 | Device and method for enhancing chemical reaction through acoustic resonance |
-
2021
- 2021-12-07 CN CN202111484645.3A patent/CN114394902A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101423895A (en) * | 2008-12-15 | 2009-05-06 | 森松（江苏）重工有限公司 | Overflow type multi-compartment autoclave and process thereof |
| CN102888283A (en) * | 2012-10-11 | 2013-01-23 | 华南理工大学 | Multi-frequency ultrasonic radiation overflow groove continuous biodiesel production device |
| CN103113234A (en) * | 2013-01-21 | 2013-05-22 | 湖北东方化工有限公司 | Method for synthesizing N-methyl paranitroaniline |
| CN106025203A (en) * | 2016-05-27 | 2016-10-12 | 湖南海纳新材料有限公司 | Preparation method of ternary precursor for continuous narrow distributed lithium battery |
| CN209901249U (en) * | 2019-04-30 | 2020-01-07 | 山东道可化学有限公司 | 3, 4-dichloro benzotrifluoride continuous production equipment |
| CN113441100A (en) * | 2021-07-22 | 2021-09-28 | 西安近代化学研究所 | Device and method for enhancing chemical reaction through acoustic resonance |
Non-Patent Citations (2)
| Title |
|---|
| 曾亮等: "连续法流化床串联固定床反应器 合成2，4-二叔丁基苯酚的反应工艺", 《西北民族大学学报（自然科学版）》, vol. 25, no. 53, pages 33 - 37 * |
| 蒋浩龙等: "声共振混合技术及其在火炸药中的应用", 《化工新型材料》, vol. 45, no. 2, pages 236 - 238 * |
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