CN213253114U - 2, 3-dichloropyridine and intermediate continuous extraction industrialization device - Google Patents
2, 3-dichloropyridine and intermediate continuous extraction industrialization device Download PDFInfo
- Publication number
- CN213253114U CN213253114U CN202021975364.9U CN202021975364U CN213253114U CN 213253114 U CN213253114 U CN 213253114U CN 202021975364 U CN202021975364 U CN 202021975364U CN 213253114 U CN213253114 U CN 213253114U
- Authority
- CN
- China
- Prior art keywords
- extraction
- valve
- kettle
- condenser
- dichloropyridine
- 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
Abstract
The utility model discloses a 2, 3-dichloropyridine and midbody continuous extraction industrialization device, the solvent storage tank, extract cauldron and stills three through the pipe connection, all install motor and stirring rake on extract cauldron and the stills, the stirring rake can accelerate stirring speed, install the fourth valve on the pipeline that extract cauldron output and stills are connected, the outer wall of stills is installed and is pressed from both sides the cover, the top of stills is through two repayment union couplings two condensers, the condenser is through the pipe connection extraction cauldron, baffle and distributor are installed to the inboard of extraction cauldron, baffle and distributor play the effect of certain isolation raffinate and extract, guarantee extract and raffinate abundant separation; when the whole device is used, the continuous extraction can be realized, the extraction rate is high, the industrial production is convenient, the solvent recycling is realized, the solvent loss is reduced, the cost is reduced through less equipment, the process is simplified, and the process time is saved by combining the extraction and the solvent recovery.
Description
Technical Field
The utility model relates to the technical field of chemical materials, in particular to a continuous extraction industrialization device for 2, 3-dichloropyridine and an intermediate.
Background
2, 3-dichloropyridine is a key intermediate for synthesizing chlorantraniliprole, the demand of the 2, 3-dichloropyridine must be obviously increased along with the gradual popularization of the chlorantraniliprole, and the synthesis method thereof is also concerned. In the manufacturing method of the patent CN 2017213445383-aminopyridine continuous extraction and purification device, continuous extraction of 3-aminopyridine is realized, but the patent is used for multiple times of extraction devices, a plurality of layering tanks are erected in the middle of the extraction devices, a plurality of pumps are needed to convey feed liquid, the extraction steps are complicated, the number of devices is large, and the energy consumption is high; in addition, the contact between the chloroform and the extraction liquid is insufficient, and the extraction efficiency is low; an extracting agent needs to be added into each layering tank, so that the operation is troublesome; the recycling of the solvent is not realized, and the solvent loss is large; CN 201310514134.0A preparation method of 2, 3-dichloropyridine, the intermediate 3-aminopyridine is extracted by dichloromethane, then hydrochloric acid is used for back extraction, and other intermediates and 2, 3-dichloromethane extraction adopt conventional multiple solvent extraction, such extraction not only has complex operation steps, but also has poor extraction efficiency, the solvent needs to be additionally recovered, the solvent loss is large, and the industrial production is not facilitated; therefore, a simple device, a simple extraction process and low energy consumption are needed; extraction industrialization device that extraction efficiency is high.
SUMMERY OF THE UTILITY MODEL
An object of the utility model is to provide a 2, 3-dichloropyridine and midbody continuous extraction industrialization device possesses through continuous extraction, and the extraction rate is high, and the industrial production of being convenient for realizes solvent cyclic utilization, and the solvent loss reduces, and through less equipment reduce cost, the advantage of simplifying technology can solve the problem among the prior art simultaneously.
In order to achieve the above object, the utility model provides a following technical scheme:
a2, 3-dichloropyridine and intermediate continuous extraction industrialization device comprises a solvent storage tank, an extraction kettle and a distillation kettle, wherein the solvent storage tank, the extraction kettle and the distillation kettle are connected through a pipeline, a power pump, a fifth valve and a sixth valve are installed on the pipeline connecting the solvent storage tank and the extraction kettle, the power pump is positioned at the inner sides of the fifth valve and the sixth valve, a first motor is installed at the top end of the extraction kettle, a first stirring paddle is installed at the output end of the first motor, the first stirring paddle is positioned at the inner side of the extraction kettle, a fourth valve is installed on the pipeline connecting the output end of the extraction kettle and the distillation kettle, the top end of the distillation kettle is connected with the solvent storage tank through a pipeline, a seventh valve is installed on the pipeline, a second motor is installed at the center of the top end of the distillation kettle, a second stirring paddle is installed at the output end of the second motor, and the second stirring paddle is positioned at the inner side of, the outer wall of the distillation kettle is provided with a jacket, the top end of the distillation kettle is connected with a first feedback pipe and a second feedback pipe, one end of the first feedback pipe is connected with a first condenser, one end of the second feedback pipe is connected with a second condenser, the first condenser and the second condenser are both connected with the extraction kettle through pipelines, a first valve is arranged on a connecting pipeline of the first condenser and the extraction kettle, and a second valve is arranged on a connecting pipeline of the second condenser and the extraction kettle.
Preferably, the output end of the extraction kettle is connected with a raffinate discharge port, and a third valve is arranged on a pipeline connected with the raffinate discharge port.
Preferably, the diameters of the first feedback pipe and the second feedback pipe are both 100mm, the eighth valve is installed on the first feedback pipe, and the ninth valve is installed on the second feedback pipe.
Preferably, the inside of extraction cauldron is installed baffle and distributor, and the distributor is located the top of baffle, offers evenly distributed's round hole on the distributor.
Preferably, the inner cavities of the first condenser and the second condenser are both provided with uniformly distributed heat exchange tubes.
Compared with the prior art, the beneficial effects of the utility model are as follows:
the 2, 3-dichloropyridine and intermediate continuous extraction industrialization device comprises a solvent storage tank, an extraction kettle and a distillation kettle which are connected through pipelines, wherein the solvent storage tank supplies materials for the extraction kettle and the distillation kettle, the extraction kettle and the distillation kettle are both provided with a motor and a stirring paddle, the motor can drive the stirring paddle to accelerate the stirring speed when working, a fourth valve is arranged on the pipeline connecting the output end of the extraction kettle and the distillation kettle, the outer wall of the distillation kettle is provided with a jacket, the top end of the distillation kettle is connected with two condensers through two feedback pipes, the condensers are connected with the extraction kettle through the pipelines, the inner side of the extraction kettle is provided with a partition plate and a distributor, and the partition plate and the distributor play a certain role in isolating raffinate from extract liquid and ensuring the extract liquid to be fully separated; when the whole device is used, the continuous extraction can be realized, the extraction rate is high, the industrial production is convenient, the solvent recycling is realized, the solvent loss is reduced, the cost is reduced through less equipment, the process is simplified, and the process time is saved by combining the extraction and the solvent recovery.
Drawings
Fig. 1 is a schematic view of the overall position of the present invention;
FIG. 2 is a schematic view of the structure of the extraction kettle of the present invention;
FIG. 3 is a schematic view of the structure of a distillation still according to the present invention;
fig. 4 is a schematic diagram of the distributor structure of the present invention.
In the figure: 1. a solvent storage tank; 2. an extraction kettle; 3. a distillation kettle; 4. a power pump; 5. a fifth valve; 6. A sixth valve; 7. a first motor; 8. a first stirring paddle; 9. a fourth valve; 10. a seventh valve; 11. A second motor; 12. a second stirring paddle; 13. a jacket; 14. a first feedback pipe; 15. a second feedback tube; 16. a first condenser; 17. a second condenser; 18. an eighth valve; 19. a ninth valve; 20. A third valve; 21. a first valve; 22. a second valve; 23. a partition plate; 24. a distributor.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Referring to fig. 1-4, an industrialization apparatus for continuously extracting 2, 3-dichloropyridine and intermediates comprises a solvent storage tank 1, an extraction kettle 2 and a distillation kettle 3, wherein the solvent storage tank 1, the extraction kettle 2 and the distillation kettle 3 are connected by a pipeline, the solvent storage tank 1 supplies materials to the extraction kettle 2 and the distillation kettle 3, the pipeline connecting the solvent storage tank 1 and the extraction kettle 2 is provided with a power pump 4, a fifth valve 5 and a sixth valve 6, the power pump 4 can drive the materials to be injected into the extraction kettle 2, the power pump 4 is positioned at the inner sides of the fifth valve 5 and the sixth valve 6, the top end of the extraction kettle 2 is provided with a first motor 7, the output end of the first motor 7 is provided with a first stirring paddle 8, the first stirring paddle 8 is positioned at the inner side of the extraction kettle 2, the first motor 7 can drive the first stirring paddle 8 to rotate when in operation, the rotating first stirring paddle 8 accelerates the stirring speed of the extraction kettle 2, the output end of the extraction kettle 2 is connected with a raffinate discharge port, a pipeline connected with the raffinate discharge port is provided with a third valve 20, when the third valve 20 is opened, redundant raffinate of the extraction kettle 2 can be discharged from the raffinate discharge port, a pipeline connecting the output end of the extraction kettle 2 with the distillation kettle 3 is provided with a fourth valve 9, the top end of the distillation kettle 3 is connected with the solvent storage tank 1 through a pipeline, the pipeline is provided with a seventh valve 10, the center of the top end of the distillation kettle 3 is provided with a second motor 11, the output end of the second motor 11 is provided with a second stirring paddle 12, the first stirring paddle 8 and the second stirring paddle 12 are both in a double-blade or multi-blade form, the second stirring paddle 12 is positioned at the inner side of the distillation kettle 3, the second motor 11 can drive the second stirring paddle 12 to rotate when working, the rotating second stirring paddle 12 can accelerate the material reaction in the distillation kettle 3, the outer wall of the distillation kettle 3 is provided with a jacket 13, hot water can be introduced into the jacket 13, the solvent in the distillation kettle 3 can be heated to a temperature above the boiling point by the hot water, steam can enter the condenser, the top end of the distillation kettle 3 is connected with a first feedback pipe 14 and a second feedback pipe 15, the diameters of the first feedback pipe 14 and the second feedback pipe 15 are both 100mm, an eighth valve 18 is installed on the first feedback pipe 14, a ninth valve 19 is installed on the second feedback pipe 15, the eighth valve 18 and the ninth valve 19 are both used for controlling whether the steam is input into the condenser, one end of the first feedback pipe 14 is connected with a first condenser 16, one end of the second feedback pipe 15 is connected with a second condenser 17, the number of the condensers can be added according to requirements, heat exchange pipes which are uniformly distributed are arranged in the inner cavities of the first condenser 16 and the second condenser 17, and can play a role of condensing the steam, first condenser 16 and second condenser 17 all pass through pipe connection extraction cauldron 2, baffle 23 and distributor 24 are installed to extraction cauldron 2's inboard, distributor 24 is located the top of baffle 23, evenly distributed's round hole has been seted up on distributor 24, baffle 23 and distributor 24 play the effect of certain isolation raffinate and extraction liquid, guarantee extraction liquid and raffinate intensive separation, install first valve 21 on first condenser 16 and the connecting tube of extraction cauldron 2, install second valve 22 on second condenser 17 and the connecting tube of extraction cauldron 2.
Example one
Extraction of 2, 3-dichloropyridine: pumping a reaction liquid containing 2, 3-dichloropyridine into an extraction kettle 2, pumping a certain amount of chloroform into the extraction kettle 2, starting a first motor 7 to stir, adjusting the speed of a first stirring paddle 8 to a certain value, stirring for 30min, pumping the rest chloroform into a distillation kettle 3, introducing hot water into a jacket 13, and opening a first valve 21, a second valve 22, an eighth valve 18 and a ninth valve 19 to allow chloroform gas to enter a condenser; after 30min, opening a fourth valve 9, adjusting the fourth valve 9 to a certain opening degree, enabling the extract liquid to enter a distillation kettle 3 at a certain flow rate, continuously extracting for 5h, and detecting the residual content of the 2, 3-dichloropyridine by taking the upper raffinate to be less than or equal to 0.05%; stopping extraction, closing the fourth valve 9, opening the third valve 20 to drain raffinate, then closing the third valve 20, continuing to distill and recover chloroform, discharging after the chloroform is evaporated, and detecting that the content of the 2, 3-dichloropyridine reaches 99.5 percent and the extraction rate reaches 99.5 percent.
Example two
Extraction of 2, 3-dichloropyridine: pumping the reaction solution containing 2, 3-dichloropyridine into the extraction kettle 2 containing the recovered chloroform, starting stirring, adjusting the speed of a stirring paddle to a certain value, stirring for 30min, introducing hot water into a jacket 13 on the outer wall of the distillation kettle 3, opening a first valve 21, a second valve 22, an eighth valve 18 and a ninth valve 19, and introducing chloroform gas into a condenser; after 30min, opening a fourth valve 9, adjusting the fourth valve 9 to a certain opening degree, enabling the extract liquid to enter a distillation kettle 3 at a certain flow rate, continuously extracting for 7h, and detecting the residual content of the 2, 3-dichloropyridine by taking the upper raffinate to be less than or equal to 0.03%; stopping extraction, closing the fourth valve 9, opening the third valve 20 to drain raffinate, then closing the third valve 20, continuing to distill and recover chloroform, after the chloroform is evaporated, discharging, detecting, wherein the content of the 2, 3-dichloropyridine reaches 99.5 percent, and the extraction rate reaches 99.7 percent
EXAMPLE III
Extraction of 2, 3-dichloropyridine intermediate 3-aminopyridine: pumping the reaction liquid containing 3-aminopyridine into an extraction kettle 2, pumping a certain amount of dichloromethane into the extraction kettle 2, starting stirring, adjusting the speed of a stirring paddle to a certain value, stirring for 30min, pumping the rest dichloromethane into a distillation kettle 3, introducing hot water into a jacket 13, opening a first valve 21, a second valve 22, an eighth valve 18 and a ninth valve 19, and enabling chloroform gas to enter a condenser; after 30min, opening a fourth valve 9, adjusting the fourth valve 9 to a certain opening degree, enabling the extract liquid to enter a distillation kettle 3 at a certain flow rate, continuously extracting for 6h, and detecting the residual content of the 2, 3-dichloropyridine by taking the upper raffinate to be less than or equal to 0.04 percent; stopping extraction, closing the fourth valve 9, opening the third valve 20 to completely discharge raffinate, then closing the third valve 20, continuing to distill and recover dichloromethane, discharging after the dichloromethane is evaporated, and detecting that the content of the 3-aminopyridine reaches 99.6 percent and the extraction rate reaches 99.6 percent.
Example four
Extraction of 2, 3-dichloropyridine intermediate 3-aminopyridine: pumping the reaction liquid containing 3-aminopyridine into an extraction kettle 2, pumping a certain amount of chloroform into the extraction kettle 2, starting stirring, adjusting the speed of a stirring paddle to a certain value, stirring for 30min, pumping the rest chloroform into a distillation kettle 3, introducing hot water into a jacket 13, opening a first valve 21, a second valve 22, an eighth valve 18 and a ninth valve 19, and enabling chloroform gas to enter a condenser; after 30min, opening a fourth valve 9, adjusting the fourth valve 9 to a certain opening degree, enabling the extract liquid to enter a distillation kettle 3 at a certain flow rate, continuously extracting for 8h, and detecting the residual content of the 2, 3-dichloropyridine by taking the upper raffinate to be less than or equal to 0.02%; stopping extraction, closing the fourth valve 9, opening the third valve 20 to completely discharge raffinate, then closing the third valve 20, continuing to distill and recover dichloromethane, discharging after the dichloromethane is evaporated, and detecting that the content of the 3-aminopyridine reaches 99.6 percent and the extraction rate reaches 99.7 percent.
In conclusion; the 2, 3-dichloropyridine and intermediate continuous extraction industrialization device comprises a solvent storage tank 1, an extraction kettle 2 and a distillation kettle 3 which are connected through a pipeline, wherein the solvent storage tank 1 supplies materials to the extraction kettle 2 and the distillation kettle 3, the extraction kettle 2 and the distillation kettle 3 are both provided with a motor and a stirring paddle, the motor can drive the stirring paddle to accelerate stirring speed when in work, the pipeline connecting the output end of the extraction kettle 2 and the distillation kettle 3 is provided with a fourth valve 9, the outer wall of the distillation kettle 3 is provided with a jacket 13, the top end of the distillation kettle 3 is connected with two condensers through two feedback pipes, the condensers are connected with the extraction kettle 2 through a pipeline, the inner side of the extraction kettle 2 is provided with a partition plate 23 and a distributor 24, the partition plate 23 and the distributor 24 play a certain role in isolating raffinate from extract liquid, and ensuring that the extract liquid and the raffinate liquid are; when the whole device is used, the continuous extraction can be realized, the extraction rate is high, the industrial production is convenient, the solvent recycling is realized, the solvent loss is reduced, the cost is reduced through less equipment, the process is simplified, and the process time is saved by combining the extraction and the solvent recovery.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (5)
1. The utility model provides a 2, 3-dichloropyridine and midbody continuous extraction industrialization device, includes solvent storage tank (1), extraction cauldron (2) and stills (3), its characterized in that: the solvent storage tank (1), the extraction kettle (2) and the distillation kettle (3) are connected through a pipeline, a power pump (4), a fifth valve (5) and a sixth valve (6) are installed on the pipeline connecting the solvent storage tank (1) and the extraction kettle (2), the power pump (4) is located on the inner side of the fifth valve (5) and the sixth valve (6), a first motor (7) is installed on the top end of the extraction kettle (2), a first stirring paddle (8) is installed at the output end of the first motor (7), the first stirring paddle (8) is located on the inner side of the extraction kettle (2), a fourth valve (9) is installed on the pipeline connecting the output end of the extraction kettle (2) and the distillation kettle (3), the top end of the distillation kettle (3) is connected with the solvent storage tank (1) through a pipeline, a seventh valve (10) is installed on the pipeline, and a second motor (11) is installed at the center of the top end of the distillation kettle (3), second stirring rake (12) are installed to second motor (11) output, and second stirring rake (12) are located the inboard of stills (3), and the outer wall of stills (3) is installed and is pressed from both sides cover (13), and the top of stills (3) is connected with first feedback pipe (14) and second feedback pipe (15), the one end of first feedback pipe (14) is connected with first condenser (16), and the one end of second feedback pipe (15) is connected with second condenser (17), and first condenser (16) and second condenser (17) all through pipe connection extraction cauldron (2), install first valve (21) on the connecting tube of first condenser (16) and extraction cauldron (2), install second valve (22) on the connecting tube of second condenser (17) and extraction cauldron (2).
2. The continuous extraction industrial device for 2, 3-dichloropyridine and intermediates in claim 1, which is characterized in that: the output end of the extraction kettle (2) is connected with a raffinate discharge port, and a third valve (20) is arranged on a pipeline connected with the raffinate discharge port.
3. The continuous extraction industrial device for 2, 3-dichloropyridine and intermediates in claim 1, which is characterized in that: the diameters of the first feedback pipe (14) and the second feedback pipe (15) are both 100mm, an eighth valve (18) is installed on the first feedback pipe (14), and a ninth valve (19) is installed on the second feedback pipe (15).
4. The continuous extraction industrial device for 2, 3-dichloropyridine and intermediates in claim 1, which is characterized in that: baffle (23) and distributor (24) are installed to the inboard of extraction cauldron (2), and distributor (24) are located the top of baffle (23), offer evenly distributed's round hole on distributor (24).
5. The continuous extraction industrial device for 2, 3-dichloropyridine and intermediates in claim 1, which is characterized in that: and heat exchange tubes which are uniformly distributed are arranged in the inner cavities of the first condenser (16) and the second condenser (17).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021975364.9U CN213253114U (en) | 2020-09-10 | 2020-09-10 | 2, 3-dichloropyridine and intermediate continuous extraction industrialization device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021975364.9U CN213253114U (en) | 2020-09-10 | 2020-09-10 | 2, 3-dichloropyridine and intermediate continuous extraction industrialization device |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN213253114U true CN213253114U (en) | 2021-05-25 |
Family
ID=75940544
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202021975364.9U Active CN213253114U (en) | 2020-09-10 | 2020-09-10 | 2, 3-dichloropyridine and intermediate continuous extraction industrialization device |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN213253114U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113671089A (en) * | 2021-09-18 | 2021-11-19 | 云南中烟工业有限责任公司 | Tobacco essence extraction, separation and concentration device with sample feeding bottle and method |
-
2020
- 2020-09-10 CN CN202021975364.9U patent/CN213253114U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113671089A (en) * | 2021-09-18 | 2021-11-19 | 云南中烟工业有限责任公司 | Tobacco essence extraction, separation and concentration device with sample feeding bottle and method |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN103449699B (en) | Device and method for realizing continuous pyrohydrolysis treatment of organic material | |
| CN213253114U (en) | 2, 3-dichloropyridine and intermediate continuous extraction industrialization device | |
| CN101811936B (en) | Benzyl alcohol continuous hydrolysis technology and use equipment thereof | |
| CN101759272B (en) | Supercritical water oxidized organic wastewater treating system | |
| CN108485945B (en) | Reaction system suitable for organic solid waste resource utilization | |
| CN113318677A (en) | DOTP production device and process | |
| CN101818101A (en) | Biodiesel esterification device and process method | |
| CN208802952U (en) | A kind of vacuum distillation dephenolize equipment | |
| CN104085861B (en) | A kind of device of reclaim(ed) sulfuric acid from Graphene acid-bearing wastewater and corresponding technique thereof | |
| CN210944908U (en) | Solid waste landfill leachate evaporation crystallization device | |
| CN115254918A (en) | Continuous high-pressure hydrothermal device for industrial treatment of kitchen waste | |
| CN212236029U (en) | Hypergravity multifunctional separation device | |
| CN210728704U (en) | Linkage distillation tower boiling tower system | |
| CN204417424U (en) | Super-viscous oil SAGD cyclic preheat liquid treating system | |
| CN209662649U (en) | Phenylacetic acid recyclable device | |
| CN203938481U (en) | A kind of from Graphene acid-bearing wastewater the device of reclaim(ed) sulfuric acid | |
| CN220546960U (en) | Epoxy separation and purification device | |
| CN201660618U (en) | Biodiesel esterification device | |
| CN218793922U (en) | Biodiesel methanol continuous recovery device | |
| CN110975316A (en) | THF (tetrahydrofuran) rectifying device for PBT (polybutylene terephthalate) production | |
| CN217188009U (en) | Extraction device is used in extractant production | |
| CN214553488U (en) | Bromination reaction device that bromine high efficiency was utilized | |
| CN201610393U (en) | Supercritical water oxidation organic wastewater treatment system | |
| CN211004598U (en) | Continuous quality-separating crystallization and purification device for sodium chloride and ammonium chloride in industrial mixed salt wastewater | |
| CN220159952U (en) | Production device of fusidic acid sodium salt |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |