CN112604418A - Method and system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas - Google Patents
Method and system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas Download PDFInfo
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- CN112604418A CN112604418A CN202011464574.6A CN202011464574A CN112604418A CN 112604418 A CN112604418 A CN 112604418A CN 202011464574 A CN202011464574 A CN 202011464574A CN 112604418 A CN112604418 A CN 112604418A
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Abstract
The invention relates to the technical field of chemical industry, which comprises the following steps: s1: leading tail gas generated at a tail gas outlet end of the 2-chloro-5-trifluoromethylpyridine reaction vessel to the inside of a system for treating the 2-chloro-5-trifluoromethylpyridine reaction tail gas in a centralized manner; s2: performing primary water washing inside the system for treating the 2-chloro-5-trifluoromethylpyridine reaction tail gas; s3: repeatedly carrying out acid and alkali washing; s4: dehydrating and drying the gas remained after the step of repeatedly washing with acid and alkali; s5: carrying out safe explosion-proof combustion treatment on the dried gas; s6: the combusted gas is continuously washed downstream for the second time and then detected; s7: discharging to the outside after the detection is qualified, otherwise returning to S3; the efficient treatment of the tail gas can be effectively realized, and the qualification of the tail gas finally discharged to the air environment is ensured to reach the standard; the efficiency of harmful tail gas treatment is effectively improved by adopting a mode of combining water washing with multiple acid washing and alkali washing during tail gas purification, and the treatment effect is improved.
Description
Technical Field
The invention relates to the technical field of chemical industry, in particular to a method and a system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas.
Background
The 2-chloro-5-trifluoromethyl pyridine is a chemical substance, has white semisolid appearance and character, and is mainly used for producing agricultural chemicals such as fluazifop-p-butyl and pharmaceuticals. 2-chloro-5-trifluoromethylpyridine products are typically stored in cool, ventilated stores. At present, 3-methylpyridine is generally adopted as a raw material to be firstly chlorinated to obtain 2-chloro-5-trichloromethylpyridine when the synthesis of the 2-chloro-5-trifluoromethylpyridine is carried out, and then the chlorination is further carried out to obtain a product; the product can also be obtained by using 3-methylpyridine as a raw material and carrying out a fluorine chlorination reaction in the presence of a catalyst.
In the existing process of preparing 2-chloro-5-trifluoromethylpyridine through reaction, some harmful gases such as hydrogen fluoride and the like are usually generated and remained inevitably, the gases cannot reach the environmental protection auditing standard if being discharged into the air, and meanwhile, the discharge of excessive harmful gases can also influence the surrounding air environment, thereby influencing the working environment and the body health of workers.
Disclosure of Invention
In order to solve one of the technical problems, the invention adopts the technical scheme that: a method for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas comprises the following steps:
s1: leading tail gas generated at a tail gas outlet end of the 2-chloro-5-trifluoromethylpyridine reaction vessel to the inside of a system for treating the 2-chloro-5-trifluoromethylpyridine reaction tail gas in a centralized manner;
s2: performing primary water washing inside the system for treating the 2-chloro-5-trifluoromethylpyridine reaction tail gas;
s3: removing solid particle impurities carried in the gas after water washing, and then repeatedly carrying out acid and alkali washing;
s4: dehydrating and drying the gas remained after the step of repeatedly washing with acid and alkali;
s5: carrying out safe explosion-proof combustion treatment on the dried gas;
s6: the combusted gas is continuously washed downstream for the second time and then detected;
s7: and discharging to the outside after passing the detection, otherwise returning to S3.
Preferably, in the step of washing with water for the first time in S2, the water temperature is controlled to be 35-45 ℃ and the washing time is 10-20 min.
Preferably, the process of repeating acid and alkali washing in S3 includes acid washing and alkali washing, the acid washing step includes several steps, and one alkali washing step is added between each two successive acid washing steps.
Preferably, the acid washing and the alkali washing are both at the water temperature of 35-45 ℃, the internal sealed reaction pressure environment is 2 atmospheric pressures, and the reaction time is controlled within 20-30 min.
Preferably, the combustion process in S5 is an explosion-proof flow guide process.
A system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas comprises a tail gas collecting tank, wherein the gas inlet end of the tail gas collecting tank is used for collecting the tail gas, the outlet end of the tail gas collecting tank is used for being connected with a first water washing device at the downstream, an acid-base comprehensive treatment device is connected at the downstream of the first water washing device, a drying treatment device is connected at the downstream of the acid-base comprehensive treatment device, a combustion purification device is connected at the downstream of the drying treatment device, a second water washing device is connected at the downstream of the combustion purification device, air detection equipment is connected at the downstream of the second water washing device, a three-way pipeline is arranged at the outlet end of the air detection equipment, a control valve is respectively arranged on the three-way pipeline, and a bypass safety backflow pipeline is arranged on one branch pipeline of the three-way pipeline, and the bypass safety return pipeline is used for being connected with the inlet end of the acid-base comprehensive treatment device.
Preferably, the first water washing device comprises a first water tank, the lower part of the first water tank is connected with the outlet of the tail gas collecting tank through an air inlet pipeline with a valve, water is filled in the inner cavity of the first water tank, and the upper part of the first water tank is connected with the inlet end of the acid-base comprehensive treatment device through an air outlet pipeline with a valve.
Preferably, the second water washing device has the same structure as the first water washing device, and includes a second water tank, the lower portion of the second water tank is connected to the outlet of the combustion purification device through an air inlet pipeline with a valve, the inner cavity of the second water tank is filled with water, and the upper portion of the second water tank is connected to the inlet end of the air detection device through an air outlet pipeline with a valve.
Preferably, the combustion purification device comprises a combustion chamber, the inlet end of the combustion chamber is connected with the air inlet pipeline at the lower part of the second water tank, the top outlet of the combustion chamber is connected with a safety chamber through a pressure regulating pipe, a safety pressure relief valve is installed on the pressure regulating pipe, and the outlet of the safety chamber is connected with the air inlet pipeline of the second water tank of the second water washing device.
Preferably, the acid-base comprehensive treatment device comprises a plurality of pickling tanks arranged at intervals, the pickling tanks are adjacent to each other and connected through a communicating pipeline, an alkaline washing tank is installed on each communicating pipeline, an acid solution used for carrying out acid washing treatment on tail gas is filled in each pickling tank, and an alkaline solution used for carrying out alkaline washing treatment on the tail gas after upstream acid washing is filled in each alkaline washing tank.
Preferably, a power transmission pump body is installed on each of the air inlet pipeline, the air outlet pipeline, the communication pipeline and the bypass safety return pipeline according to requirements.
Preferably, the pickling tank is used for carrying out pickling reaction in an up-in and down-out mode, and the alkaline washing tank is used for carrying out alkaline washing reaction in an up-in and down-out mode.
Preferably, the alkaline washing tank and the alkaline washing tank are both provided with a ram air pipe with an air valve and a pressure gauge.
Preferably, the first water tank adopts a spiral pipe structure; the second water tank is of a spiral pipe structure.
Preferably, the pickling tank adopts a spiral pipe structure; the alkaline washing tank adopts a spiral pipe structure.
The invention has the beneficial effects that:
1. when the method is used for tail gas treatment, the high-efficiency treatment of the tail gas can be effectively realized, and the qualification of the tail gas finally discharged to the air environment is ensured to reach the standard;
2. when tail gas purification is carried out, the efficiency of harmful tail gas treatment is effectively improved by adopting a mode of combining water washing with multiple acid washing and alkaline washing, and the treatment effect is improved;
3. adopt the mode of gaseous spiral shell screwing in rise to guarantee the abundant contact of tail gas and solution when washing and acid, alkali wash, cooperate the burning to handle tail gas here in addition, discharge after finally reaching standard through the inspection, guarantee the qualification rate of tail gas after handling.
Drawings
In order to more clearly illustrate the detailed description of the invention or the technical solutions in the prior art, the drawings that are needed in the detailed description of the invention or the prior art will be briefly described below. Throughout the drawings, like elements or components are generally identified by like reference numerals. In the drawings, elements or components are not necessarily drawn to scale.
FIG. 1 is a schematic structural diagram of the present invention.
Fig. 2 is a schematic structural diagram of the first water tank, the pickling tank and the alkaline washing tank of the present invention.
Fig. 3 is a schematic sectional structure diagram of the first water tank, the pickling tank and the alkaline washing tank according to the present invention.
Fig. 4 is a schematic structural view of a spiral drying duct of the present invention.
In the figure, 1, a tail gas collecting tank; 2. a first water washing device; 3. an acid-base comprehensive treatment device; 4. a drying treatment device; 5. a combustion purification device; 6. a second water washing device; 7. an air detection device; 8. a three-way pipeline; 9. a control valve; 10. bypassing the safety return line; 11. a first water tank; 12. an air intake line; 13. an air outlet pipeline; 14. a second water tank; 15. a combustion chamber; 16. an igniter; 17. a pressure regulating pipe; 18. a safety chamber; 19. a safety relief valve; 20. a pickling tank; 21. a communicating pipeline; 22. an alkaline washing tank; 23. a power delivery pump body; 24. punching an air pipe; 25. a pressure gauge; 26. a spiral tube; 27. a spiral drying tube; 28. an electric heating pipe sleeve; 29. a temperature control system; 30. an inert desiccant.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and therefore are only examples, and the protection scope of the present invention is not limited thereby.
As shown in fig. 1-4, a method for treating 2-chloro-5-trifluoromethylpyridine reaction off-gas comprises the following steps:
s1: leading tail gas generated at a tail gas outlet end of the 2-chloro-5-trifluoromethylpyridine reaction vessel to the inside of a system for treating the 2-chloro-5-trifluoromethylpyridine reaction tail gas in a centralized manner;
s2: performing primary water washing inside the system for treating the 2-chloro-5-trifluoromethylpyridine reaction tail gas;
s3: removing solid particle impurities carried in the gas after water washing, and then repeatedly carrying out acid and alkali washing;
the mode of repeated acid washing and alkali washing can better ensure that the harmful gases in the gas are subjected to sufficient acid washing and alkali washing reaction, thereby effectively ensuring the rapid treatment and purification of different harmful gases.
S4: dehydrating and drying the gas remained after the step of repeatedly washing with acid and alkali;
after drying, the gas combustion treatment can be conveniently carried out at the later stage.
S5: carrying out safe explosion-proof combustion treatment on the dried gas;
after combustion, the residual harmful gas in the gas can be further removed to change into gas such as carbon dioxide and the like as much as possible for emission.
S6: the combusted gas is continuously washed downstream for the second time and then detected;
the purpose of the secondary water washing is to sufficiently dissolve the gas that can be dissolved in water, and to reduce the amount of the finally remaining harmful gas discharged.
S7: and discharging to the outside after passing the detection, otherwise returning to S3.
Preferably, in the step of washing with water for the first time in S2, the water temperature is controlled to be 35-45 ℃ and the washing time is 10-20 min.
The temperature and time of water washing are controlled to better improve the solubility of gas in water and improve the reaction degree with water.
Preferably, the process of repeating acid and alkali washing in S3 includes acid washing and alkali washing, the acid washing step includes several steps, and one alkali washing step is added between each two successive acid washing steps.
The possibility and efficiency of gas which reacts with acid and alkali can be better removed by adopting the intermittent acid washing and alkali washing mode, and the gas is fully neutralized, so that the possibility of subsequent overflow and discharge of harmful gas is reduced.
Preferably, the acid washing and the alkali washing are both at the water temperature of 35-45 ℃, the internal sealed reaction pressure environment is 2 atmospheric pressures, and the reaction time is controlled within 20-30 min.
The temperature and time of water washing are controlled, so that the solubility of gas in water can be better improved, and the degree of reaction with acid-base neutralization is improved.
Preferably, the combustion process in S5 is an explosion-proof flow guide process.
The safety of burning gas is guaranteed, the explosion caused by the fact that the internal pressure is increased rapidly due to the fact that gas burns wantonly is prevented, gas can be discharged into the safety chamber 18 rapidly through the safety relief valve 19, and therefore the stability of the whole burning process is guaranteed.
A system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas comprises a tail gas collecting tank 1, wherein the inlet end of the tail gas collecting tank 1 is used for collecting tail gas, the outlet end of the tail gas collecting tank 1 is used for being connected with a first water washing device 2 at the downstream, the downstream of the first water washing device 2 is connected with an acid-base comprehensive treatment device 3, the downstream of the acid-base comprehensive treatment device 3 is connected with a drying treatment device 4, the downstream of the drying treatment device 4 is connected with a combustion purification device 5, the downstream of the combustion purification device 5 is connected with a second water washing device 6, the downstream of the second water washing device 6 is connected with an air detection device 7, the outlet end of the air detection device 7 is provided with a three-way pipeline 8, and the three-way pipeline 8 is respectively provided with a control valve 9, a bypass safety return pipeline 10 is installed on one branch pipeline of the three-way pipeline 8, and the bypass safety return pipeline 10 is used for being connected with the inlet end of the acid-base comprehensive treatment device 3.
The tail gas in the tail gas collecting tank 1 controls the flow rate of harmful gas discharged to the downstream according to the requirement, so that the gas sequentially passes through the first water washing device 2, the acid-base comprehensive treatment device 3, the drying treatment device 4, the combustion purification device 5 and the second water washing device 6 to complete neutralization and purification treatment, and finally the quality of the gas is detected through the air detection device 7, so that the discharged gas is ensured to meet the environmental protection requirement.
Preferably, the first water washing device 2 comprises a first water tank 11, the lower part of the first water tank 11 is connected with the outlet of the tail gas collecting tank 1 through an air inlet pipeline 12 with a valve, the inner cavity of the first water tank 11 is filled with water, and the upper part of the first water tank 11 is connected with the inlet end of the acid-base comprehensive treatment device 3 through an air outlet pipeline 13 with a valve. The gas adopts the mode of air inlet from the lower part and air exhaust from the upper part, so that the contact time with water flow can be effectively prolonged, and the sufficiency of water washing is ensured.
Preferably, the second water washing device 6 has the same structure as the first water washing device 2, and includes a second water tank 14, the lower portion of the second water tank 14 is connected to the outlet of the combustion purification device 5 through a valved inlet pipe 12, the inner cavity of the second water tank 14 is filled with water, and the upper portion of the second water tank 14 is connected to the inlet end of the air detection device 7 through a valved outlet pipe 13. The gas adopts the mode of air inlet from the lower part and air exhaust from the upper part, so that the contact time with water flow can be effectively prolonged, and the sufficiency of water washing is ensured.
Preferably, the combustion purification apparatus 5 includes a combustion chamber 15 having an igniter 16 disposed therein, an inlet end of the combustion chamber 15 is connected to the air inlet pipeline 12 at the lower portion of the second water tank 14, a safety chamber 18 is connected to an outlet at the top of the combustion chamber 15 through a pressure regulating pipe 17, a safety relief valve 19 is installed on the pressure regulating pipe 17, and an outlet of the safety chamber 18 is connected to the air inlet pipeline 12 of the second water tank 14 of the second water washing apparatus 6. Here, in order to secure the safety reaction, the safety chamber 18 is additionally provided in order to reduce the internal pressure by transferring gas to the safety chamber 18 when the internal pressure is increased by the combustion of the gas, thereby securing the safety of the whole combustion reaction process, and the safety relief valve 19 provided therein may be set to a safety opening pressure or may be manually operated.
Preferably, the acid-base comprehensive treatment device 3 comprises a plurality of pickling tanks 20 arranged at intervals, the pickling tanks 20 are adjacent to each other and connected through a communication pipeline 21, an alkaline washing tank 22 is installed on each communication pipeline 21, an acid solution used for carrying out acid washing treatment on the tail gas is filled in each pickling tank 20, and an alkaline solution used for carrying out alkaline washing treatment on the tail gas after upstream acid washing is filled in each alkaline washing tank 22.
Preferably, a power transmission pump body 23 is installed on each of the air inlet pipeline 12, the air outlet pipeline 13, the communication pipeline 21 and the bypass safety return pipeline 10 as required, and the power transmission pump body 23 is additionally arranged to mainly improve the power of the gas in the transmission process.
Preferably, the pickling tank 20 performs the pickling reaction in a top-in and bottom-out manner, and the alkaline tank 22 performs the alkaline washing reaction in a top-in and bottom-out manner. The gas is fed from the lower part and exhausted from the upper part, so that the contact time with the acid washing solution or the alkali washing solution can be effectively prolonged, and the sufficiency of the neutralization reaction is ensured.
Preferably, the alkaline washing tank 22 and the alkaline washing tank 22 are both provided with a ram air pipe 24 with an air valve and a pressure gauge 25, and the change of the internal air pressure is conveniently observed through the pressure gauge 25.
Preferably, the first water tank 11 is in the structure of a spiral pipe 26; the second water tank 14 is in the form of a coil 26. The first water tank 11 and the second water tank 14 are set to be in a spiral shape, so that gas can be effectively guaranteed to spirally rise in the pipe, the gas is guaranteed to be fully contacted with the water flow in the pipe, and the washing effect is improved.
Preferably, the pickling tank 20 adopts a spiral pipe 26 structure; the alkaline washing tank 22 adopts a spiral pipe 26 structure. The first water tank 11 and the second water tank 14 are set to be spiral, so that gas can be effectively guaranteed to spirally rise in the pipe, the gas is guaranteed to be fully contacted with the water flow in the pipe, the acid washing and alkali washing effects are improved, and the full neutralized reaction of harmful gas is guaranteed.
The drying device comprises a spiral drying pipe 27 which is horizontally arranged, the spiral drying pipe 27 realizes radiation heating through an electric heating pipe sleeve 28 which is sleeved on the outer side wall of the spiral drying pipe 27, an external temperature control system 29 is connected onto the electric heating pipe sleeve 28, the interior of the spiral drying pipe 27 realizes drying treatment of tail gas introduced into the interior of the spiral drying pipe 27 through proper temperature, and an inert drying agent 30 is filled in the spiral drying pipe 27.
The above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; the modifications or the substitutions do not cause the essence of the corresponding technical solutions to depart from the scope of the technical solutions of the embodiments of the present invention, and the technical solutions are all covered in the scope of the claims and the specification of the present invention; it will be apparent to those skilled in the art that any alternative modifications or variations to the embodiments of the present invention may be made within the scope of the present invention.
The present invention is not described in detail, but is known to those skilled in the art.
Claims (9)
1. A method for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas is characterized by comprising the following steps: the method comprises the following steps:
s1: leading tail gas generated at a tail gas outlet end of the 2-chloro-5-trifluoromethylpyridine reaction vessel to the inside of a system for treating the 2-chloro-5-trifluoromethylpyridine reaction tail gas in a centralized manner;
s2: performing primary water washing inside the system for treating the 2-chloro-5-trifluoromethylpyridine reaction tail gas;
s3: removing solid particle impurities carried in the gas after water washing, and then repeatedly carrying out acid and alkali washing;
s4: dehydrating and drying the gas remained after the step of repeatedly washing with acid and alkali;
s5: carrying out safe explosion-proof combustion treatment on the dried gas;
s6: the combusted gas is continuously washed downstream for the second time and then detected;
s7: and discharging to the outside after passing the detection, otherwise returning to S3.
2. The method for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas according to claim 1, wherein: and in the step of primary water washing in the step of S2, the water temperature is controlled to be 35-45 ℃, and the water washing time is 10-20 min.
3. The method for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas according to the claim 2, characterized in that: the process of repeated acid and alkali washing in S3 comprises acid washing and alkali washing, the acid washing step comprises a plurality of acid washing steps, and an alkali washing step is added between each two connected acid washing steps.
4. The method for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas according to claim 3, wherein: the acid washing and the alkali washing are both carried out at the water temperature of 35-45 ℃, the internal sealed reaction pressure environment is 2 atmospheric pressures, and the reaction time is controlled to be 20-30 min.
5. The method for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas according to claim 4, wherein: and performing explosion-proof flow guide treatment on the combustion treatment in the step S5.
6. A system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas is characterized in that: comprises a tail gas collecting tank, the gas inlet end of the tail gas collecting tank is used for collecting tail gas, the outlet end of the tail gas collecting tank is used for connecting with a first water washing device at the downstream, the downstream of the first water washing device is connected with an acid-base comprehensive treatment device, the downstream of the acid-base comprehensive treatment device is connected with a drying treatment device, a combustion purification device is connected with the downstream of the drying treatment device, a second water washing device is connected with the downstream of the combustion purification device, the downstream of the second water washing device is connected with an air detection device, the outlet end of the air detection device is provided with a three-way pipeline, a control valve is respectively arranged on the three-way pipeline, a bypass safety return pipeline is arranged on one branch pipeline of the three-way pipeline, and the bypass safety return pipeline is used for being connected with the inlet end of the acid-base comprehensive treatment device.
7. The system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas according to claim 6, wherein: the first water washing device comprises a first water tank, the lower portion of the first water tank is connected with an outlet of the tail gas collecting tank through an air inlet pipeline with a valve, water is filled in an inner cavity of the first water tank, and the upper portion of the first water tank is connected with an inlet end of the comprehensive acid-base treatment device through an air outlet pipeline with a valve.
8. The system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas according to claim 7, wherein: the structure of the second water washing device is the same as that of the first water washing device, the second water washing device comprises a second water tank, the lower portion of the second water tank is connected with the outlet of the combustion purification device through an air inlet pipeline with a valve, water is filled in the inner cavity of the second water tank, and the upper portion of the second water tank is connected with the inlet end of the air detection device through an air outlet pipeline with a valve.
9. The system for treating 2-chloro-5-trifluoromethylpyridine reaction tail gas according to claim 8, wherein: the combustion purification device comprises a combustion chamber, wherein the inlet end of the combustion chamber is connected with the air inlet pipeline of the lower part of the second water tank, the top outlet of the combustion chamber is connected with a safety chamber through a pressure regulating pipe, a safety pressure relief valve is installed on the pressure regulating pipe, and the outlet of the safety chamber is connected with the air inlet pipeline of the second water tank of the second water washing device.
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Application publication date: 20210406 |