CN210496408U - 2-chlorine-5-chloromethyl pyridine apparatus for producing - Google Patents
2-chlorine-5-chloromethyl pyridine apparatus for producing Download PDFInfo
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- CN210496408U CN210496408U CN201921270271.3U CN201921270271U CN210496408U CN 210496408 U CN210496408 U CN 210496408U CN 201921270271 U CN201921270271 U CN 201921270271U CN 210496408 U CN210496408 U CN 210496408U
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Abstract
The utility model relates to a 2-chloro-5-chloromethyl pyridine production device, which comprises a feeding device, a reaction device and a tail gas treatment device, wherein the feeding device comprises a stock bin and a feeding machine; the reaction device comprises a reaction kettle and a stirrer, the stirrer is arranged in the reaction kettle, and the upper end of the reaction kettle is connected with one end of the feeding pipeline far away from the motor; the tail gas treatment device comprises a gas-liquid separation device, a tail gas absorption device and a toluene backflow pipeline. The utility model improves the automation degree and precision of the triphosgene feeding process, and can effectively reduce the phenomenon of material block masses; the gas-liquid separation efficiency is effectively improved, so that the recovery utilization rate of the solvent can be improved, the introduction of impurities (such as organic amines) is reduced, and the adverse effect of the impurities is reduced; the pipeline cleaning is more convenient, and the pipeline cleaning times in the parking state can be effectively reduced.
Description
Technical Field
The utility model belongs to the chemical production device field, concretely relates to 2-chlorine-5-chloromethyl pyridine apparatus for producing.
Background
2-chloro-5-chloromethylpyridine (CCMP) is colorless crystal, has a melting point of 34-35 ℃, and is an important intermediate for synthesizing pyridine pesticides. From the research work of CCMP synthesis in 1999, more than ten synthesis routes are developed in China, which can be basically divided into 3-methylpyridine route, morpholine route and benzylamine route, and the current domestic CCMP main synthesis route is a direct cyclization process using cyclopentadiene and acrolein as raw materials:
because the phosphorus oxychloride process has low reaction yield and is easy to generate a large amount of phosphorus-containing wastewater and a large amount of solid waste, a process for replacing phosphorus oxychloride with triphosgene is developed. Triphosgene, the chemical name of which is bis (trichloromethyl) carbonate, BTC for short, is white crystal at room temperature, has high melting point, low volatility and relatively low toxicity, has the advantages of mild conditions required for synthesis and chemical reaction, strong selectivity, relative safety in use and easiness in transportation and storage, and is widely used as a substitute reactant of phosphorus oxychloride in CCMP preparation at present. However, there are also problems with the use of triphosgene in the production of 2-chloro-5-chloromethylpyridine: since triphosgene is solid and needs to be dissolved and then dripped into the reaction kettle, a preparation kettle is usually required to be arranged, and the use steps are complicated; the automation degree and the precision of triphosgene feeding are low, and the triphosgene needs to be manually and frequently added into the synthesis kettle in the reaction process and is easily subjected to excessive feeding; triphosgene will decompose slightly at temperatures above 130 ℃ to produce phosgene, will start to decompose after moisture absorption at 90 ℃ to produce phosgene, and will decompose at lower temperatures in the presence of certain organic amines. The above problems have caused a great limitation in the use of triphosgene in the production of 2-chloro-5-chloromethylpyridine.
SUMMERY OF THE UTILITY MODEL
The utility model aims to overcome the defects that triphosgene in the prior art has complex use steps, low feeding automation degree and precision and difficult control of dissolution temperature to decompose the triphosgene, the utility model provides a 2-chlorine-5-chloromethylpyridine production device, which realizes the reduction of preparation kettles by introducing a feeding device, and simultaneously, a hot water jacket is arranged outside the reaction kettle to replace the traditional steam heating device to improve the controllability of reaction temperature, and a U-shaped condensing pipe is adopted in a tail gas recovery device to greatly improve the gas-liquid separation degree of tail gas, thereby solving the problems of inconvenient use and easy decomposition of the triphosgene which can not be solved in the traditional 2-chlorine-5-chloromethylpyridine production device, and having the advantages of simple and convenient use and maintenance, high automation degree and precision, controllable temperature, Safe and environment-friendly.
The utility model discloses a realize above-mentioned technical purpose, provide following technical scheme: a2-chloro-5-chloromethylpyridine production device comprises a feeding device, a reaction device and a tail gas treatment device, wherein the feeding device comprises a stock bin and a feeding machine, the feeding machine comprises a motor, a feeding pipeline and a double auger, the double auger is arranged in the feeding pipeline, the motor is arranged at one end of the feeding pipeline and is connected with the double auger through a driving shaft, the stock bin is arranged above the feeding pipeline, and the bottom of the stock bin is connected with the upper side wall of one end of the feeding pipeline, which is close to the motor, through a stock bin pipeline;
the reaction device comprises a reaction kettle and a stirrer, the stirrer is arranged in the reaction kettle, and the upper end of the reaction kettle is connected with one end of the feeding pipeline far away from the motor;
the tail gas treatment device comprises a gas-liquid separation device, a tail gas absorption device and a toluene backflow pipeline, the upper end of the reaction kettle is connected with a gas inlet of the gas-liquid separation device through the gas-liquid separation pipeline, the upper end of the gas-liquid separation device is connected with the tail gas absorption device through the tail gas pipeline, one end of the toluene backflow pipeline is connected with the lower end of the gas-liquid separation device, and the other end of the toluene backflow pipeline is connected with the upper end of the reaction kettle;
further, the gas-liquid separation device is a condenser;
furthermore, the condenser is a condenser with U-shaped or snake-shaped condenser pipes;
further, the upper end of the reaction kettle is connected with one end of the feeding pipeline, far away from the motor, through a reaction kettle feeding pipeline, and a pneumatic valve is arranged on the reaction kettle feeding pipeline;
furthermore, a charging opening is formed in the upper part of the storage bin, and a charging opening cover is arranged on the charging opening;
further, the charging port cover is provided with a sight glass;
furthermore, raised threads are arranged in the feeding pipeline;
further, a jacket heat preservation device is arranged outside the feeding pipeline;
furthermore, the jacket heat preservation device comprises a hot water jacket arranged along the outer part of the feeding pipeline and a heat preservation layer arranged outside the hot water jacket;
further, the hot water jacket is provided with a water inlet and a water outlet.
Owing to adopted above technique, the utility model discloses compare with prior art, it is showing the advantage and is:
1) the feeding mode of the triphosgene is changed by arranging the feeding machine, the automation degree and the precision of the triphosgene feeding process are improved, the feeding amount of the triphosgene can be controlled by controlling the rotating speed and the starting and stopping of the motor, the triphosgene does not need to be manually and frequently added into the synthesis kettle in the reaction process, the possibility of excessive feeding is reduced, and meanwhile, the labor cost is effectively reduced; due to the arrangement of the double packing augers, different feeding modes (such as single packing auger or double packing auger feeding) can be set according to the triphosgene material consumption, and in addition, the phenomenon of material block masses can be effectively reduced due to the arrangement of the convex threads on the inner wall of the feeding pipeline;
2) by arranging the serpentine condenser pipe or the U-shaped condenser pipe, the gas-liquid separation efficiency is effectively improved, so that the recovery rate of the solvent toluene can be improved, the introduction of impurities (such as organic amines) is reduced, and the adverse effect of the impurities on the triphosgene is reduced;
3) the jacket heat preservation device is arranged outside the feeding pipeline, so that the feeding pipeline is more convenient to clean, the triphosgene material in a solid state can be converted into a liquid state by heating, the triphosgene material is separated from the wall of the feeding pipeline, the feeding pipeline or other related pipelines cannot be blocked, and the pipeline cleaning times in a stopping state can be effectively reduced.
Drawings
FIG. 1 is a schematic structural view of a 2-chloro-5-chloromethylpyridine production apparatus of the present invention;
FIG. 2 is a schematic view of a partial structure of a feeding pipe and a jacket heat-insulating device of the apparatus for producing 2-chloro-5-chloromethylpyridine of the present invention;
in the figure: 1-bin, 11-bin pipeline, 12-feed inlet, 13-feed inlet cover, 2-feeding machine, 21-motor, 22-feeding pipeline, 23-double auger, 3-reaction kettle, 4-stirrer, 5-gas-liquid separation device, 51-toluene reflux pipeline, 52-gas-liquid separation pipeline, 53-condenser pipe, 6-tail gas absorption device, 61-tail gas pipeline, 7-jacket heat preservation device, 71-hot water jacket, 72-heat preservation layer, 73-water inlet, and 74-water outlet.
Detailed Description
In order to make the technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail with reference to the following embodiments.
Example 1
The 2-chloro-5-chloromethylpyridine production device shown in fig. 1 comprises a feeding device, a reaction device and a tail gas treatment device, wherein the feeding device comprises a stock bin 1 and a feeding machine 2, the feeding machine comprises a motor 21, a feeding pipeline 22 and a double packing auger 23, the double packing auger 23 is arranged in the feeding pipeline 22, the motor 21 is arranged at one end of the feeding pipeline 22 and is connected with the double packing auger 23 through a driving shaft, the stock bin 1 is arranged above the feeding pipeline 22, and the bottom of the stock bin 1 is connected with the upper side wall of the end, close to the motor 21, of the feeding pipeline 22 through a stock bin pipeline 11; a raised thread is arranged in the feeding pipeline 22; the upper part of the storage bin is provided with a feed inlet 12, and the feed inlet is provided with a feed inlet cover 13; the charging port cover 13 is provided with a sight glass. The feeding mode of the triphosgene is changed by arranging the feeding machine, the automation degree and the precision of the triphosgene feeding process are improved, the feeding amount of the triphosgene can be controlled by controlling the rotating speed and the starting and stopping of the motor, the triphosgene does not need to be manually and frequently added into the synthesis kettle in the reaction process, the possibility of excessive feeding is reduced, and meanwhile, the labor cost is effectively reduced; due to the arrangement of the double packing augers, different feeding modes (such as single packing auger or double packing auger feeding) can be set according to the triphosgene material consumption, and in addition, the phenomenon of material lumps can be effectively reduced due to the arrangement of the convex threads on the inner wall of the feeding pipeline.
Reaction unit includes reation kettle 3, agitator 4 sets up in reation kettle 3, and 3 upper ends of reation kettle are connected with the one end of the motor 21 far away of material loading pipeline 22.
The tail gas treatment device comprises a gas-liquid separation device 5, a tail gas absorption device 6 and a toluene backflow pipeline 51, the upper end of the reaction kettle 3 is connected with a gas inlet of the gas-liquid separation device 5 through a gas-liquid separation pipeline 52, the upper end of the gas-liquid separation device 5 is connected with the tail gas absorption device 6 through a tail gas pipeline 61, one end of the toluene backflow pipeline 51 is connected with the lower end of the gas-liquid separation device 5, and the other end of the toluene backflow pipeline 51 is connected with the upper end of the reaction kettle 3.
The gas-liquid separation device 5 is a condenser, and the condenser is a condenser with U-shaped distribution of a condensation pipe 53; the upper end of the reaction kettle 3 is connected with one end of the feeding pipeline 22 far away from the motor 21 through a reaction kettle feeding pipeline, and a pneumatic valve is arranged on the reaction kettle feeding pipeline. Through setting up snakelike condenser pipe or U type condenser pipe, effectively improved gas-liquid separation efficiency to can improve the recycle of solvent toluene, reduce the introduction of impurity (like organic amine) simultaneously, reduce the harmful effects of impurity to triphosgene.
Preferably, a jacket heat preservation device 7 is arranged outside the feeding pipeline 22; the jacket heat preservation device 7 comprises a hot water jacket 71 arranged along the outer part of the feeding pipeline and a heat preservation layer 72 arranged outside the hot water jacket; the hot water jacket is provided with a water inlet 73 and a water outlet 74, hot water with proper temperature is injected into the hot water jacket through the water inlet 73, flows out through the water outlet 74, is continuously heated and is put into circulation; the jacket heat preservation device is arranged outside the feeding pipeline, so that the feeding pipeline is more convenient to clean, the triphosgene material in a solid state can be converted into a liquid state by heating, the triphosgene material is separated from the wall of the feeding pipeline, the feeding pipeline or other related pipelines cannot be blocked, and the pipeline cleaning times in a stopping state can be effectively reduced.
In the actual production process, triphosgene is added into a storage bin, a single auger mode or a double auger mode is started to feed the triphosgene into a reaction kettle according to the requirements of the feeding amount and the feeding speed, and if the room temperature is too low, hot water circulation of a jacket heat-insulating device can be started to properly heat the triphosgene material; carrying out a reaction of 2-chloro-2-chloromethyl-4-cyanobutyraldehyde and triphosgene in toluene in a reaction kettle, heating to 90 ℃, starting a stirrer for stirring, adjusting the pH value of a system after the reaction is finished, filtering, layering in aluminum industry, carrying out decompression, desolventizing, short steaming and rectifying on organic phase under reduced pressure; the tail gas enters the gas-liquid separation device through a gas-liquid separation pipeline and is separated into a gas phase and a liquid phase, the gas phase is conveyed to the tail gas absorption device through the tail gas pipeline to be absorbed and correspondingly post-treated, and the liquid phase is conveyed to the reaction kettle through a toluene backflow pipeline to be recycled and reused.
The above-mentioned embodiments are merely preferred technical solutions of the present invention, and should not be regarded as limitations of the present invention, and the protection scope of the present invention should be protected by the technical solutions described in the claims, and equivalent alternatives including technical features in the technical solutions described in the claims are also within the protection scope of the present invention.
Claims (10)
1. The production device of the 2-chloro-5-chloromethylpyridine is characterized by comprising a feeding device, a reaction device and a tail gas treatment device, wherein the feeding device comprises a stock bin and a feeding machine, the feeding machine comprises a motor, a feeding pipeline and a double auger, the double auger is arranged in the feeding pipeline, the motor is arranged at one end of the feeding pipeline and is connected with the double auger through a driving shaft, the stock bin is arranged above the feeding pipeline, and the bottom of the stock bin is connected with the upper side wall of one end, close to the motor, of the feeding pipeline through a stock bin pipeline;
the reaction device comprises a reaction kettle and a stirrer, the stirrer is arranged in the reaction kettle, and the upper end of the reaction kettle is connected with one end of the feeding pipeline far away from the motor;
the tail gas treatment device comprises a gas-liquid separation device, a tail gas absorption device and a toluene backflow pipeline, the upper end of the reaction kettle is connected with a gas inlet of the gas-liquid separation device through the gas-liquid separation pipeline, the upper end of the gas-liquid separation device is connected with the tail gas absorption device through the tail gas pipeline, one end of the toluene backflow pipeline is connected with the lower end of the gas-liquid separation device, and the other end of the toluene backflow pipeline is connected with the upper end of the reaction kettle.
2. The apparatus for producing 2-chloro-5-chloromethylpyridine according to claim 1, wherein said gas-liquid separation device is a condenser.
3. The apparatus for producing 2-chloro-5-chloromethylpyridine according to claim 2, wherein said condenser is a U-shaped or serpentine condenser.
4. The apparatus for producing 2-chloro-5-chloromethylpyridine as in claim 1, wherein the upper end of the reaction vessel is connected to the end of the feeding pipe far from the motor through a feeding pipe of the reaction vessel, and the feeding pipe of the reaction vessel is provided with a pneumatic valve.
5. The apparatus for producing 2-chloro-5-chloromethylpyridine according to claim 1, wherein a charging opening is provided at an upper portion of the storage bin, and the charging opening is provided with a charging opening cover.
6. A production apparatus of 2-chloro-5-chloromethylpyridine as in claim 5, wherein said lid is provided with a sight glass.
7. The apparatus for producing 2-chloro-5-chloromethylpyridine according to claim 1, wherein the feeding pipe is internally provided with a raised thread.
8. The apparatus for producing 2-chloro-5-chloromethylpyridine according to claim 1, wherein a jacket heat-insulating device is disposed outside the feeding pipeline.
9. The apparatus for producing 2-chloro-5-chloromethylpyridine according to claim 8, wherein the jacket-insulating means comprises a hot water jacket disposed along the exterior of the feeding pipe and an insulating layer disposed outside the hot water jacket.
10. The apparatus for producing 2-chloro-5-chloromethylpyridine according to claim 9, wherein said hot water jacket is provided with a water inlet and a water outlet.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921270271.3U CN210496408U (en) | 2019-08-07 | 2019-08-07 | 2-chlorine-5-chloromethyl pyridine apparatus for producing |
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| CN201921270271.3U CN210496408U (en) | 2019-08-07 | 2019-08-07 | 2-chlorine-5-chloromethyl pyridine apparatus for producing |
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| CN210496408U true CN210496408U (en) | 2020-05-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036158A (en) * | 2019-12-28 | 2020-04-21 | 邯郸市瑞田农药有限公司 | 2 chlorine-5 chloromethyl thiazole synthesis reaction system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111036158A (en) * | 2019-12-28 | 2020-04-21 | 邯郸市瑞田农药有限公司 | 2 chlorine-5 chloromethyl thiazole synthesis reaction system |
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