CN214735480U - Post-processing device for producing 2,2' -bipyridyl - Google Patents
Post-processing device for producing 2,2' -bipyridyl Download PDFInfo
- Publication number
- CN214735480U CN214735480U CN202120178440.1U CN202120178440U CN214735480U CN 214735480 U CN214735480 U CN 214735480U CN 202120178440 U CN202120178440 U CN 202120178440U CN 214735480 U CN214735480 U CN 214735480U
- Authority
- CN
- China
- Prior art keywords
- pipeline
- delivery pump
- tank
- kettle
- neutralization
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Pyridine Compounds (AREA)
Abstract
The utility model relates to a post-processing apparatus of production 2,2' -bipyridine comprises reaction solution elevated tank, feeding pump, catalyst filter, blowback pipeline, neutralization-extraction cauldron, hydrochloric acid elevated metering tank, extraction agent elevated metering tank, acidimeter, concentrated cauldron, thermometer, crystallization kettle, pressure filter, filtrating receiving tank, desalination jar and agitator. The device has reasonable design, can continuously produce the 2,2' -bipyridyl with the content of more than 99.5 percent and the yield of more than 95 percent, improves the yield by nearly 15 percent and the purity by nearly 5 percent compared with the traditional process, and meets the production requirement of downstream pesticide diquat. Meanwhile, the internal circulation of water and organic solvent in the system is realized, and the sewage discharge is reduced by about 40 tons per ton of product. In addition, the microporous filter rod is designed to be wavy, so that the contact area between the reaction product and the filter rod is fully increased, the solid-liquid two-phase full separation is facilitated, the catalyst loss is reduced, and the production cost is reduced.
Description
Technical Field
The utility model relates to a post-processing apparatus of production 2,2' -bipyridine specifically belongs to chemical production technical field.
Background
2,2' -bipyridine is an important chemical intermediate, is mainly used for pesticides, medical intermediates, organic synthesis and the like, and particularly has a very important function in the field of pesticides, such as the production of a low-concentration high-efficiency pesticide diquat.
The existing process for producing 2,2 '-bipyridine mainly uses 2-chloropyridine as a raw material, uses nickel dichloride, triphenylphosphine and iron (zinc) powder as a catalytic system (Journal of Organic Chemistry,2014,79,777-782), and synthesizes the 2,2' -bipyridine through a series of post-treatments such as coupling reaction and the like. In the synthesis route, the post-treatment process is complicated, the yield of about 80 percent and the purity of about 95 percent are required to be improved, a large amount of iron mud is generated after the reaction, the process is not environment-friendly, and the process is gradually eliminated due to the improvement of the current environment-friendly requirement. Meanwhile, the catalyst system is simply mixed by three components of nickel dichloride, triphenylphosphine and iron (zinc) powder, the catalyst can not be repeatedly used basically, and the production cost is high. Therefore, it is urgently needed to develop a green and environment-friendly production process and production equipment matched with the production process, particularly a post-treatment device for producing 2,2 '-bipyridine, which is particularly important for ensuring the yield and quality of 2,2' -bipyridine.
SUMMERY OF THE UTILITY MODEL
Based on the above problem, the utility model aims at realizing the purpose of producing high-quality and high-yield 2,2 '-bipyridyl through the innovative design of the post-production treatment device for 2,2' -bipyridyl.
The utility model relates to a post-processing apparatus of production 2,2' -bipyridine is by reaction liquid elevated tank (1), No. 1 conveying pump (2-1), catalyst filter (3), blowback pipeline (4), neutralization-extraction cauldron (5), hydrochloric acid elevated metering tank (6), extractant elevated metering tank (7), acidimeter (8), No. 3 conveying pump (2-3), concentrated cauldron (9), No. 1 thermometer (10-1), No. 4 conveying pump (2-4), No. 2 thermometer (10-2), crystallization kettle (11), No. 5 conveying pump (2-5), pressure filter (12), filtrating receiving tank (13), No. 6 conveying pump (2-6), No. 2 conveying pump (2-2), No. 3 thermometer (10-3), desalination tank (14), No. 1 agitator (15-1), A No. 2 stirrer (15-2) and a No. 3 stirrer (15-3);
the bottom of the reaction liquid elevated tank (1) is connected with a No. 1 delivery pump (2-1) through a pipeline; the side surface of the catalyst filter (3) is provided with a back flushing pipeline (4), the other side surface of the catalyst filter is connected with a No. 1 material conveying pump (2-1) through a pipeline, and the top of the catalyst filter is connected with the top of the neutralization-extraction kettle (5) through a pipeline; the neutralization-extraction kettle (5) is provided with a stirrer (15-1) No. 1 and an acidimeter (8), the top of the neutralization-extraction kettle is connected with a hydrochloric acid high-level metering tank (6) and an extractant high-level metering tank (7) through pipelines respectively, and the bottom of the neutralization-extraction kettle is connected with a material conveying pump (2-2) No. 2 and a material conveying pump (2-3) No. 3 through pipelines respectively; the No. 2 delivery pump (2-2) is connected with a desalting tank (14) with a No. 3 thermometer (10-3) through a pipeline; the No. 3 delivery pump (2-3) is connected with the top of the concentration kettle (9) through a pipeline; the concentration kettle (9) is provided with a No. 2 stirrer (15-2) and a No. 1 thermometer (10-1), and the bottom of the concentration kettle is connected with a No. 4 delivery pump (2-4) through a pipeline; the crystallization kettle (11) is provided with a No. 3 stirrer (15-3) and a No. 2 thermometer (10-2), the top of the crystallization kettle is connected with a No. 4 delivery pump (2-4) through a pipeline, and the bottom of the crystallization kettle is connected with a No. 5 delivery pump (2-5) through a pipeline; the other end of the No. 5 delivery pump (2-5) is connected with a filter press (12) through a pipeline; the filter press (12) is connected with the filtrate receiving tank (13) through a pipeline; the filtrate receiving tank (13) is connected with a No. 6 delivery pump (2-6) through a pipeline; the other end of the No. 6 delivery pump (2-6) is connected with the top of the neutralization-extraction kettle (5) through a pipeline.
The internal structure of the catalyst filter (3) is formed by connecting 30 microporous filter rods with wavy surfaces in parallel.
The utility model discloses beneficial effect:
1. the device has reasonable design, can continuously produce the 2,2' -bipyridyl with the content of more than 99.5 percent and the yield of more than 95 percent, improves the yield by nearly 15 percent and the purity by nearly 5 percent compared with the traditional process (Journal of Organic Chemistry,2014,79,777-782), and meets the production requirement of downstream pesticide diquat. Meanwhile, the internal circulation of water and organic solvent in the system is realized, and the sewage discharge is reduced by about 40 tons per ton of product.
2. The inside of the catalyst filter is formed by connecting 30 microporous filter rods with wavy surfaces in parallel, so that the contact area between reaction products and the filter rods is fully increased, and meanwhile, a back-blowing pipeline is designed, so that the solid-liquid two-phase full separation is facilitated, the catalyst loss is reduced, and the production cost is reduced.
Drawings
FIG. 1 is a schematic structural view of the post-processing device of the present invention;
in the figure: 1. a reaction liquid elevated tank; no. 2-1 and No. 1 delivery pumps; 3. a catalyst filter; 4. a blowback pipeline; 5. a neutralization-extraction kettle; 6. a hydrochloric acid high-level metering tank; 7. an extractant high-level metering tank; 8. an acidimeter; no. 2-3 and No. 3 delivery pumps; 9. a concentration kettle; thermometer No. 10-1, 1; no. 2-4 and No. 4 delivery pumps; thermometer No. 10-2, 2; 11. a crystallization kettle; no. 2-5 and No. 5 delivery pumps; 12. a filter press; 13. a filtrate receiving tank; no. 2-6 and No. 6 delivery pumps; no. 2-2 and No. 2 delivery pumps; 10-3, 3 thermometer; 14. A desalting tank; no. 15-1, No. 1 stirrer; no. 15-2 and No. 2 stirrers; no. 15-3 and No. 3 stirrers;
FIG. 2 is a top view of the catalyst filter of the present invention;
FIG. 3 is a schematic view of the wavy microporous filter rod of the present invention;
fig. 4 is a partial enlarged view of the wavy microporous filter rod of the present invention.
Detailed Description
Example 1
Structure composition of post-treatment device for producing 2,2' -bipyridine
A post-processing device for producing 2,2' -bipyridyl is characterized in that: the post-treatment device comprises a reaction liquid elevated tank (1), a No. 1 delivery pump (2-1), a catalyst filter (3), a back flushing pipeline (4), a neutralization-extraction kettle (5), a hydrochloric acid elevated metering tank (6), an extraction agent elevated metering tank (7), an acidimeter (8), a No. 3 delivery pump (2-3), a concentration kettle (9), a No. 1 thermometer (10-1) and a No. 4 delivery pump (2-4), a No. 2 thermometer (10-2), a crystallization kettle (11), a No. 5 delivery pump (2-5), a filter press (12), a filtrate receiving tank (13), a No. 6 delivery pump (2-6), a No. 2 delivery pump (2-2), a No. 3 thermometer (10-3), a desalting tank (14), a No. 1 stirrer (15-1), a No. 2 stirrer (15-2) and a No. 3 stirrer (15-3);
the bottom of the reaction liquid elevated tank (1) is connected with a No. 1 delivery pump (2-1) through a pipeline; the side surface of the catalyst filter (3) is provided with a back flushing pipeline (4), the other side surface of the catalyst filter is connected with a No. 1 material conveying pump (2-1) through a pipeline, and the top of the catalyst filter is connected with the top of the neutralization-extraction kettle (5) through a pipeline; the neutralization-extraction kettle (5) is provided with a stirrer (15-1) No. 1 and an acidimeter (8), the top of the neutralization-extraction kettle is connected with a hydrochloric acid high-level metering tank (6) and an extractant high-level metering tank (7) through pipelines respectively, and the bottom of the neutralization-extraction kettle is connected with a material conveying pump (2-2) No. 2 and a material conveying pump (2-3) No. 3 through pipelines respectively; the No. 2 delivery pump (2-2) is connected with a desalting tank (14) with a No. 3 thermometer (10-3) through a pipeline; the No. 3 delivery pump (2-3) is connected with the top of the concentration kettle (9) through a pipeline; the concentration kettle (9) is provided with a No. 2 stirrer (15-2) and a No. 1 thermometer (10-1), and the bottom of the concentration kettle is connected with a No. 4 delivery pump (2-4) through a pipeline; the crystallization kettle (11) is provided with a No. 3 stirrer (15-3) and a No. 2 thermometer (10-2), the top of the crystallization kettle is connected with a No. 4 delivery pump (2-4) through a pipeline, and the bottom of the crystallization kettle is connected with a No. 5 delivery pump (2-5) through a pipeline; the other end of the No. 5 delivery pump (2-5) is connected with a filter press (12) through a pipeline; the filter press (12) is connected with the filtrate receiving tank (13) through a pipeline; the filtrate receiving tank (13) is connected with a No. 6 delivery pump (2-6) through a pipeline; the other end of the No. 6 delivery pump (2-6) is connected with the top of the neutralization-extraction kettle (5) through a pipeline. The internal structure of the catalyst filter (3) is formed by connecting 30 microporous filter rods with wavy surfaces in parallel.
Example 2
The operation process of the post-treatment device for producing the 2,2' -bipyridyl comprises the following steps:
the reaction product for producing 2,2' -bipyridine in the reaction liquid head tank (1) enters a catalyst filter (3) through a corrosion-resistant No. 1 delivery pump (2-1) for filtration, and after filtration, the catalyst is recovered after the back flushing through a back flushing pipeline (4), the filtrate is conveyed into a neutralization-extraction kettle (5) through a heat-insulating pipeline, a No. 1 stirrer (15-1) is started, hydrochloric acid is added into the neutralization-extraction kettle (5) from a discharge hole at the lower end of a hydrochloric acid high-level metering tank (6) until the pH value is 6-7, then under the stirring state, the extract liquor in the extractant high-level metering tank (7) is put into a neutralization-extraction kettle (5) through a lower end pipeline, fully stirring, standing for layering, allowing the lower water phase to enter a desalting tank (14) through a pipeline and a No. 2 delivery pump (2-2), the upper organic phase enters a concentration kettle (9) through a pipeline and a No. 3 delivery pump (2-3); heating the concentration kettle (9), concentrating the organic phase to a set amount, discharging the concentrated solution through a pipeline at the bottom of the concentration kettle (9), and conveying the concentrated solution into a crystallization kettle (11) through a No. 4 material conveying pump (2-4); and (2) starting a No. 3 stirrer (15-3), freezing the crystallization kettle (11), slowly cooling the crystallization kettle (11) to 0-5 ℃, feeding the crystallized concentrated solution into a filter press (12) through a pipeline and a No. 5 delivery pump (2-5) for filter pressing, wherein a filter cake is a high-purity white solid 2,2' -bipyridyl product, and after the filtrate enters a filtrate receiving tank (13) through the pipeline, the filtrate flows into the neutralization-extraction kettle (5) through the pipeline and the No. 6 delivery pump (2-6).
The catalyst filter (3) has an automatic discharging function, the refrigerating fluid in the crystallization kettle (11) is 0-5 ℃ frozen brine, and water and an organic solvent in a post-treatment device for producing the 2,2' -bipyridyl can be recycled.
Claims (2)
1. A post-processing device for producing 2,2' -bipyridyl is characterized in that: the post-treatment device comprises a reaction liquid elevated tank (1), a No. 1 delivery pump (2-1), a catalyst filter (3), a back flushing pipeline (4), a neutralization-extraction kettle (5), a hydrochloric acid elevated metering tank (6), an extraction agent elevated metering tank (7), an acidimeter (8), a No. 3 delivery pump (2-3), a concentration kettle (9), a No. 1 thermometer (10-1) and a No. 4 delivery pump (2-4), a No. 2 thermometer (10-2), a crystallization kettle (11), a No. 5 delivery pump (2-5), a filter press (12), a filtrate receiving tank (13), a No. 6 delivery pump (2-6), a No. 2 delivery pump (2-2), a No. 3 thermometer (10-3), a desalting tank (14), a No. 1 stirrer (15-1), a No. 2 stirrer (15-2) and a No. 3 stirrer (15-3);
the bottom of the reaction liquid elevated tank (1) is connected with a No. 1 delivery pump (2-1) through a pipeline; the side surface of the catalyst filter (3) is provided with a back flushing pipeline (4), the other side surface of the catalyst filter is connected with a No. 1 material conveying pump (2-1) through a pipeline, and the top of the catalyst filter is connected with the top of the neutralization-extraction kettle (5) through a pipeline; the neutralization-extraction kettle (5) is provided with a stirrer (15-1) No. 1 and an acidimeter (8), the top of the neutralization-extraction kettle is connected with a hydrochloric acid high-level metering tank (6) and an extractant high-level metering tank (7) through pipelines respectively, and the bottom of the neutralization-extraction kettle is connected with a material conveying pump (2-2) No. 2 and a material conveying pump (2-3) No. 3 through pipelines respectively; the No. 2 delivery pump (2-2) is connected with a desalting tank (14) with a No. 3 thermometer (10-3) through a pipeline; the No. 3 delivery pump (2-3) is connected with the top of the concentration kettle (9) through a pipeline; the concentration kettle (9) is provided with a No. 2 stirrer (15-2) and a No. 1 thermometer (10-1), and the bottom of the concentration kettle is connected with a No. 4 delivery pump (2-4) through a pipeline; the crystallization kettle (11) is provided with a No. 3 stirrer (15-3) and a No. 2 thermometer (10-2), the top of the crystallization kettle is connected with a No. 4 delivery pump (2-4) through a pipeline, and the bottom of the crystallization kettle is connected with a No. 5 delivery pump (2-5) through a pipeline; the other end of the No. 5 delivery pump (2-5) is connected with a filter press (12) through a pipeline; the filter press (12) is connected with the filtrate receiving tank (13) through a pipeline; the filtrate receiving tank (13) is connected with a No. 6 delivery pump (2-6) through a pipeline; the other end of the No. 6 delivery pump (2-6) is connected with the top of the neutralization-extraction kettle (5) through a pipeline.
2. The post-processing device for producing 2,2' -bipyridine according to claim 1, characterized in that: the internal structure of the catalyst filter (3) is formed by connecting 30 microporous filter rods with wavy surfaces in parallel.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120178440.1U CN214735480U (en) | 2021-01-22 | 2021-01-22 | Post-processing device for producing 2,2' -bipyridyl |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202120178440.1U CN214735480U (en) | 2021-01-22 | 2021-01-22 | Post-processing device for producing 2,2' -bipyridyl |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN214735480U true CN214735480U (en) | 2021-11-16 |
Family
ID=78640647
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202120178440.1U Active CN214735480U (en) | 2021-01-22 | 2021-01-22 | Post-processing device for producing 2,2' -bipyridyl |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN214735480U (en) |
-
2021
- 2021-01-22 CN CN202120178440.1U patent/CN214735480U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102276483B (en) | Production method of oamino pheylmethyl ether | |
| CN108863760B (en) | Method for continuously producing glyoxylic acid by using microchannel reactor | |
| CN111253284B (en) | Benzyl cyanide production device and process with continuous whole process | |
| CN214735480U (en) | Post-processing device for producing 2,2' -bipyridyl | |
| CN1594302A (en) | Process for continuous preparation of trimellitic anhydride by step catalytic oxidation process | |
| CN108355372B (en) | Method and device for sublimating and receiving maltol | |
| CN112973607A (en) | Continuous production device and process of chlormequat chloride | |
| CN112159332B (en) | Process and device for continuously producing bentazone intermediate isopropyl anthranilate | |
| CN111704538A (en) | Method for preparing p-hydroxyphenylacetic acid by using microreactor | |
| CN102391136B (en) | Method and device for producing 4,4-diaminodiphenyl ethers by using catalytic hydrogenation process | |
| CN105111092B (en) | A kind of continuous preparation method of 3,3 ', 4,4 ' tetra-amino-biphenyls | |
| CN100355647C (en) | Lithium metaphosphorate production process | |
| CN105480991B (en) | Method and device for preparing magnesium hydroxide | |
| CN113845405B (en) | Method for continuously synthesizing diflufenican intermediate m-trifluoromethylphenol | |
| CN115043734A (en) | Continuous production process of 2,4,4 '-trichloro-2' -nitrodiphenyl ether | |
| CN214553573U (en) | Chlormequat chloride continuous production device | |
| CN104292198A (en) | Grignard hydrolysis two-phase separation synthesis method and device in maltol production | |
| CN115286532A (en) | Method for continuously synthesizing methyldopa intermediate DL-aminopropionitrile | |
| CN101759569B (en) | Method for extracting high purity para-nitrochlorobenzene and ortho-nitrochlorobenzene by synthesis method of multistrand side track discharging rectification and continuous crystallization | |
| CN114369044A (en) | Preparation method of p-aminophenyl-beta-hydroxyethyl sulfone and p-aminophenyl-beta-hydroxyethyl sulfone sulfate | |
| CN110746293B (en) | Process for preparing p-toluic acid by continuous catalytic oxidation | |
| CN111001178A (en) | Device and method for producing durene through continuous crystallization | |
| CN211562957U (en) | Synergistic injection apparatus of bromine nitryl alcohol bromination reaction | |
| CN216192002U (en) | Continuous production device for oxamide | |
| CN111362819A (en) | Process and device for producing glycine by alcohol phase method |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |