CN220176837U - Device for preparing fluorobenzene by micro-reflection continuous flow - Google Patents
Device for preparing fluorobenzene by micro-reflection continuous flow Download PDFInfo
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- CN220176837U CN220176837U CN202321467731.8U CN202321467731U CN220176837U CN 220176837 U CN220176837 U CN 220176837U CN 202321467731 U CN202321467731 U CN 202321467731U CN 220176837 U CN220176837 U CN 220176837U
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- pipeline
- storage tank
- fluorobenzene
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- PYLWMHQQBFSUBP-UHFFFAOYSA-N monofluorobenzene Chemical compound FC1=CC=CC=C1 PYLWMHQQBFSUBP-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000003860 storage Methods 0.000 claims abstract description 46
- 230000018044 dehydration Effects 0.000 claims abstract description 34
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 32
- 238000004821 distillation Methods 0.000 claims abstract description 31
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000000197 pyrolysis Methods 0.000 claims abstract description 25
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 24
- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 claims abstract description 14
- 239000000463 material Substances 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 16
- 238000002360 preparation method Methods 0.000 claims description 10
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 5
- 239000002253 acid Substances 0.000 abstract description 3
- 239000002699 waste material Substances 0.000 abstract description 3
- 230000009286 beneficial effect Effects 0.000 abstract description 2
- 238000010924 continuous production Methods 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 12
- 230000008569 process Effects 0.000 description 8
- 239000000047 product Substances 0.000 description 5
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 4
- ZSWFCLXCOIISFI-UHFFFAOYSA-N cyclopentadiene Chemical compound C1C=CC=C1 ZSWFCLXCOIISFI-UHFFFAOYSA-N 0.000 description 4
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 4
- 229910001416 lithium ion Inorganic materials 0.000 description 4
- 239000007795 chemical reaction product Substances 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 1
- 230000010933 acylation Effects 0.000 description 1
- 238000005917 acylation reaction Methods 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- KGBXLFKZBHKPEV-UHFFFAOYSA-N boric acid Chemical compound OB(O)O KGBXLFKZBHKPEV-UHFFFAOYSA-N 0.000 description 1
- 239000004327 boric acid Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 238000006193 diazotization reaction Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 150000008423 fluorobenzenes Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000006396 nitration reaction Methods 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 239000002341 toxic gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model relates to a device for preparing fluorobenzene by micro-reflection continuous flow. The technical proposal is as follows: the upper end of the mixed precooling tank is connected with a hydrofluoric acid storage tank and an aniline storage tank through pipelines, the lower end of the mixed precooling tank is connected with a salifying reaction kettle through a pipeline and a first material conveying pump, the bottom of the salifying reaction kettle is connected with the first inlet end of the microchannel reactor through a pipeline, the nitrite storage tank is connected with the second inlet end of the microchannel reactor through a pipeline, the output end of the microchannel reactor is connected with a pyrolysis tower through a pipeline, the lower end of the pyrolysis tower is connected with a central line of a distillation dehydration tower through a pipeline, the lower end of the distillation dehydration tower is connected with a fluorobenzene storage tank through a pipeline, and the top of the distillation dehydration tower is connected with a condenser through a pipeline. The beneficial effects are that: the utility model changes the traditional intermittent reaction kettle production into continuous production, and improves the reaction efficiency; in addition, the device has high safety, reduces the output of waste acid and improves the quality of fluorobenzene.
Description
Technical Field
The utility model relates to a fluorobenzene preparation device, in particular to a device for preparing fluorobenzene by micro-reflection continuous flow.
Background
Fluorobenzene is an important basic raw material of aromatic fluoride, can be used for synthesizing medicines, pesticides and dyes, and can be further synthesized into fluorobenzene derivative products through reactions such as nitration, chlorination, acylation, reduction and the like for the fields. In recent years, the lithium battery industry production value in China is continuously increased under the drive of products such as smart phones, mobile power supplies and tablet computers. Meanwhile, the application of the lithium ion battery is not limited to consumer electronics products, and the new application directions of power and energy storage are infinite market space for the lithium ion battery. In the next few years, lithium ion batteries will become an expanding global industry. Meanwhile, with the expansion of the applicable field, the requirement for further improving the battery characteristics is also increasing.
At present, research shows that the low-temperature property, the cycle property, the storage property and other battery performances of a lithium ion secondary battery can be improved by adding fluorobenzene into an electrolyte. However, the existing preparation method has various defects, or has complex process, high cost, difficult industrial production, low yield, more byproducts and difficult purification, and the prepared fluorobenzene has low purity and influences the product performance.
There are four main methods for industrial production of fluorobenzene: litz Xie Manfa, anhydrous hydrogen fluoride process (AHF process), cyclohexane process and cyclopentadiene process. The methods such as cyclohexane and cyclopentadiene are mainly used in occasions with limited raw materials and are not popular. The litz Xie Manfa consumes a large amount of boric acid and generates a toxic gas BF during thermal decomposition 3 Is not easy to recycle, has serious pollution to the environment, and has low reaction yield of about 54 percent. The most commonly used mainstream industrial process at present is the anhydrous hydrogen fluoride process (AHF process), whichThe method has the advantages of less investment, short production period, high utilization rate of raw materials, high product quality and the like. At present, the anhydrous hydrogen fluoride preparation method at home and abroad has some problems: 1) The reaction materials are not thorough, and the yield is low; 2) The impurities caused by the non-uniformity of the reaction are more; 3) And the input equipment is more.
Disclosure of Invention
The utility model aims at overcoming the defects in the prior art, and provides a device for preparing fluorobenzene by micro-inverse continuous flow, which reduces the output of waste acid, improves the quality of fluorobenzene and increases the income.
The utility model relates to a device for preparing fluorobenzene by micro-inverse continuous flow, which has the technical scheme that: including hydrofluoric acid storage tank (1), aniline storage tank (2), mix precooling jar (3), first feed pump (4), salt formation reation kettle (5), nitrite storage tank (6), microchannel reactor (7), distillation dehydration tower (8), condenser (9), fluorobenzene storage tank (11) and pyrolysis tower (17), hydrofluoric acid storage tank (1) and aniline storage tank (2) are passed through to the upper end of mixing precooling jar (3), are connected to salt formation reation kettle (5) through pipeline and first feed pump (4) in the lower extreme of mixing precooling jar (3), the first entrance point of microchannel reactor (7) is passed through to the bottom of salt formation reation kettle (5), nitrite storage tank (6) are connected to the second entrance point of microchannel reactor (7) through the pipeline, the output of microchannel reactor (7) is connected to pyrolysis tower (17) through the pipeline, the lower extreme of pyrolysis tower (17) is connected to the central line of distillation dehydration tower (8) through the pipeline, the lower extreme of distillation dehydration tower (8) is connected to benzene (8) through pipeline connection dehydration tower (11), and distillation dehydration tower (9) are passed through at the top of distillation dehydration tower (7).
Preferably, a tube side inlet of the condenser (9) is connected to the top of the distillation dehydration tower (8) through a pipeline, a tube side outlet of the condenser (9) is connected with a buffer tank (10) through a pipeline, and a lower end outlet of the buffer tank (10) is connected with a water storage tank (12) through a pipeline; the shell side inlet of the condenser (9) is connected with a condensate water inlet pipe, and the shell side outlet of the condenser (9) is connected with a condensate water outlet pipe.
Preferably, the tops of the salifying reaction kettle (5) and the pyrolysis tower (17) are respectively connected to the tail gas treatment device (13) through pipelines.
Preferably, the lower end of the salifying reaction kettle (5) is connected to the first inlet end of the microchannel reactor (7) through a pipeline and a second feed pump (14).
Preferably, the nitrite storage tank (6) is connected to the second inlet end of the microchannel reactor (7) via a pipeline and a third feed pump (15).
Preferably, the outer wall of the mixed pre-cooling tank (3) is provided with a wall clamping cavity, the lower end of the wall clamping cavity is connected with a chilled water inlet pipe, and the upper end of the wall clamping cavity is connected with a chilled water outlet pipe.
Preferably, the lower end of the pyrolysis tower (17) is connected to the central line of the distillation dehydration tower (8) through a pipeline and a fourth feed pump (16); the lower side of the pyrolysis tower (17) is provided with a reboiler (17.1).
The beneficial effects of the utility model are as follows: the utility model changes the traditional intermittent reaction kettle production mode into continuous production, and greatly improves the reaction efficiency; in addition, hydrofluoric acid and aniline are cooled and precooled through a mixed precooling tank, and the salification reaction is completed under the low-temperature condition of a salification reaction kettle, so that the reaction efficiency is improved; in addition, the micro-channel reactor has small size, short material spreading distance, quick and accurate mass and heat transfer and control, remarkably improved reaction forwarding rate and selectivity, small liquid holdup, safe reaction process and improved process safety; in addition, the use amount of hydrogen fluoride is reduced, the conversion efficiency is improved to more than 80% from 75-78%, the output of waste acid is reduced, the quality of fluorobenzene is improved, the benefit is increased, and the waste water is recycled.
Drawings
Fig. 1 is a schematic structural view of embodiment 1 of the present utility model;
fig. 2 is a schematic structural view of embodiment 2 of the present utility model;
in the upper graph: hydrofluoric acid storage tank 1, aniline storage tank 2, mixed precooling tank 3, first delivery pump 4, salifying reaction kettle 5, nitrite storage tank 6, microchannel reactor 7, distillation dehydration tower 8, condenser 9, buffer tank 10, fluorobenzene storage tank 11, water storage tank 12, tail gas treatment device 13, second delivery pump 14, third delivery pump 15, fourth delivery pump 16, pyrolysis tower 17, reboiler 17.1.
Detailed Description
The preferred embodiments of the present utility model will be described below with reference to the accompanying drawings, it being understood that the preferred embodiments described herein are for illustration and explanation of the present utility model only, and are not intended to limit the present utility model.
Embodiment 1, referring to fig. 1, the micro-inverse continuous flow fluorobenzene preparation device comprises a hydrofluoric acid storage tank 1, an aniline storage tank 2, a mixed precooling tank 3, a first material conveying pump 4, a salifying reaction kettle 5, a nitrite storage tank 6, a micro-channel reactor 7, a distillation dehydration tower 8, a condenser 9, a fluorobenzene storage tank 11 and a pyrolysis tower 17, wherein the upper end of the mixed precooling tank 3 is connected with the hydrofluoric acid storage tank 1 and the aniline storage tank 2 through pipelines, the lower end of the mixed precooling tank 3 is connected with the salifying reaction kettle 5 through pipelines and the first material conveying pump 4, the bottom of the salifying reaction kettle 5 is connected with the first inlet end of the micro-channel reactor 7 through pipelines, the nitrite storage tank 6 is connected with the second inlet end of the micro-channel reactor 7 through pipelines, the output end of the micro-channel reactor 7 is connected with the pyrolysis tower 17 through pipelines, the lower end of the pyrolysis tower 17 is connected with the central line of the distillation dehydration tower 8 through pipelines, the lower end of the distillation dehydration tower 8 is connected with the fluorobenzene storage tank 11 through pipelines, and the top of the distillation dehydration tower 8 is connected with the condenser 9 through pipelines.
Wherein, the tube side inlet of the condenser 9 is connected to the top of the distillation dehydration tower 8 through a pipeline, the tube side outlet of the condenser 9 is connected with a buffer tank 10 through a pipeline, and the lower end outlet of the buffer tank 10 is connected with a water storage tank 12 through a pipeline; the shell side inlet of the condenser 9 is connected with a condensate water inlet pipe, and the shell side outlet of the condenser 9 is connected with a condensate water outlet pipe.
In addition, the tops of the salifying reaction kettle 5 and the pyrolysis tower 17 are respectively connected to the tail gas treatment device 13 through pipelines, the lower end of the salifying reaction kettle 5 is connected to the first inlet end of the microchannel reactor 7 through a pipeline and the second feed pump 14, and the nitrite storage tank 6 is connected to the second inlet end of the microchannel reactor 7 through a pipeline and the third feed pump 15.
The outer wall of the mixed pre-cooling tank 3 is provided with a wall clamping cavity, the lower end of the wall clamping cavity is connected with a chilled water inlet pipe, and the upper end of the wall clamping cavity is connected with a chilled water outlet pipe for cooling and pre-cooling the mixed pre-cooling tank 3.
The lower end of the pyrolysis tower 17 is connected to the center line of the distillation dehydration tower 8 through a pipeline and a fourth feed pump 16; the lower side of the pyrolysis tower 17 is provided with a reboiler 17.1 for pyrolyzing reaction products to obtain crude fluorobenzene.
The application principle of the utility model is as follows:
firstly, hydrofluoric acid and aniline are measured according to a certain molar ratio, cooled and precooled through a mixed precooling tank 3, and salification reaction is completed under the low-temperature condition of a salification reaction kettle 5;
then, the reaction product and nitrite aqueous solution respectively enter a microchannel reactor 7 through a second material conveying pump 14 and a third material conveying pump 15 according to a certain proportion, and the diazotization reaction is completed at the reaction temperature of-5 ℃ to 5 ℃;
then, sending the reaction product into a pyrolysis tower 17 for pyrolysis to obtain a fluorobenzene crude product;
finally, the crude fluorobenzene is subjected to a distillation, purification and dehydration procedure of a distillation dehydration tower 8 to obtain industrial grade fluorobenzene, and the yield is more than 85%.
Embodiment 2, referring to fig. 1, the micro-inverse continuous flow fluorobenzene preparation device comprises a hydrofluoric acid storage tank 1, an aniline storage tank 2, a mixed precooling tank 3, a first material conveying pump 4, a salifying reaction kettle 5, a nitrite storage tank 6, a micro-channel reactor 7, a distillation dehydration tower 8, a condenser 9 and a fluorobenzene storage tank 11, wherein the upper end of the mixed precooling tank 3 is connected with the hydrofluoric acid storage tank 1 and the aniline storage tank 2 through pipelines, the lower end of the mixed precooling tank 3 is connected with the salifying reaction kettle 5 through pipelines and the first material conveying pump 4, the bottom of the salifying reaction kettle 5 is connected with the first inlet end of the micro-channel reactor 7 through pipelines, the nitrite storage tank 6 is connected with the second inlet end of the micro-channel reactor 7 through pipelines, the output end of the micro-channel reactor 7 is connected with the central line of the distillation dehydration tower 8 through pipelines, the lower end of the distillation dehydration tower 8 is connected with the fluorobenzene storage tank 11 through pipelines, and the top of the distillation dehydration tower 8 is connected with the condenser 9 through pipelines.
The difference from example 1 is that:
this embodiment saves a pyrolysis tower, and realizes the functions of pyrolysis and dehydration by the distillation dehydration tower 8.
The above description is of the preferred embodiments of the present utility model, and any person skilled in the art may modify the present utility model or make modifications to the present utility model with the technical solutions described above. Therefore, any simple modification or equivalent made according to the technical solution of the present utility model falls within the scope of the protection claimed by the present utility model.
Claims (7)
1. A device for preparing fluorobenzene by micro-inverse continuous flow is characterized in that: including hydrofluoric acid storage tank (1), aniline storage tank (2), mix precooling jar (3), first feed pump (4), salt formation reation kettle (5), nitrite storage tank (6), microchannel reactor (7), distillation dehydration tower (8), condenser (9), fluorobenzene storage tank (11) and pyrolysis tower (17), hydrofluoric acid storage tank (1) and aniline storage tank (2) are passed through to the upper end of mixing precooling jar (3), are connected to salt formation reation kettle (5) through pipeline and first feed pump (4) in the lower extreme of mixing precooling jar (3), the first entrance point of microchannel reactor (7) is passed through to the bottom of salt formation reation kettle (5), nitrite storage tank (6) are connected to the second entrance point of microchannel reactor (7) through the pipeline, the output of microchannel reactor (7) is connected to pyrolysis tower (17) through the pipeline, the lower extreme of pyrolysis tower (17) is connected to the central line of distillation dehydration tower (8) through the pipeline, the lower extreme of distillation dehydration tower (8) is connected to benzene (8) through pipeline connection dehydration tower (11), and distillation dehydration tower (9) are passed through at the top of distillation dehydration tower (7).
2. The micro-inverse continuous flow fluorobenzene preparation device as claimed in claim 1, wherein: the tube side inlet of the condenser (9) is connected to the top of the distillation dehydration tower (8) through a pipeline, the tube side outlet of the condenser (9) is connected with the buffer tank (10) through a pipeline, and the lower end outlet of the buffer tank (10) is connected with the water storage tank (12) through a pipeline; the shell side inlet of the condenser (9) is connected with a condensate water inlet pipe, and the shell side outlet of the condenser (9) is connected with a condensate water outlet pipe.
3. The micro-inverse continuous flow fluorobenzene preparation device as claimed in claim 2, wherein: the tops of the salifying reaction kettle (5) and the pyrolysis tower (17) are respectively connected to the tail gas treatment device (13) through pipelines.
4. A micro-inverse continuous flow fluorobenzene preparation device as claimed in claim 3, wherein: the lower end of the salifying reaction kettle (5) is connected to the first inlet end of the microchannel reactor (7) through a pipeline and a second material conveying pump (14).
5. The apparatus for preparing fluorobenzene by micro-inverse continuous flow as claimed in claim 3 or 4, wherein: the nitrite storage tank (6) is connected to the second inlet end of the microchannel reactor (7) through a pipeline and a third feed pump (15).
6. The micro-inverse continuous flow fluorobenzene preparation device as claimed in claim 5, wherein the device is characterized in that: the outer wall of the mixed pre-cooling tank (3) is provided with a wall clamping cavity, the lower end of the wall clamping cavity is connected with a chilled water inlet pipe, and the upper end of the wall clamping cavity is connected with a chilled water outlet pipe.
7. The micro-inverse continuous flow fluorobenzene preparation device as claimed in claim 5, wherein the device is characterized in that: the lower end of the pyrolysis tower (17) is connected to the central line of the distillation dehydration tower (8) through a pipeline and a fourth feed pump (16); the lower side of the pyrolysis tower (17) is provided with a reboiler (17.1).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321467731.8U CN220176837U (en) | 2023-06-09 | 2023-06-09 | Device for preparing fluorobenzene by micro-reflection continuous flow |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202321467731.8U CN220176837U (en) | 2023-06-09 | 2023-06-09 | Device for preparing fluorobenzene by micro-reflection continuous flow |
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| Publication Number | Publication Date |
|---|---|
| CN220176837U true CN220176837U (en) | 2023-12-15 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN202321467731.8U Active CN220176837U (en) | 2023-06-09 | 2023-06-09 | Device for preparing fluorobenzene by micro-reflection continuous flow |
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| Country | Link |
|---|---|
| CN (1) | CN220176837U (en) |
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2023
- 2023-06-09 CN CN202321467731.8U patent/CN220176837U/en active Active
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