CN112142649A - 2-vinylpyridine reaction post-treatment method and device thereof - Google Patents
2-vinylpyridine reaction post-treatment method and device thereof Download PDFInfo
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- CN112142649A CN112142649A CN202011090982.XA CN202011090982A CN112142649A CN 112142649 A CN112142649 A CN 112142649A CN 202011090982 A CN202011090982 A CN 202011090982A CN 112142649 A CN112142649 A CN 112142649A
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- C07D—HETEROCYCLIC COMPOUNDS
- C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
- C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
- C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D213/06—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom
- C07D213/16—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom containing only hydrogen and carbon atoms in addition to the ring nitrogen atom containing only one pyridine ring
Abstract
The invention discloses a method and a device for post-treatment of 2-vinylpyridine reaction, wherein the method comprises the following steps: 2-vinylpyridine and water mixed solution evaporated from a dehydration reaction kettle under reduced pressure is cooled in two stages by a first condenser and a second condenser, and then is stirred in an extraction kettle, an extraction solvent is added, and the mixture is stirred uniformly and layered after standing; step 2: introducing the upper aqueous phase of the extraction kettle into a water phase storage tank, and introducing the lower organic phase into a distillation kettle to recover dichloromethane; and step 3: and condensing the evaporated phase by a third condenser, introducing the condensed phase into a solvent storage tank, introducing the distillation bottom liquid into a pressure reduction kettle, evaporating the 2-vinylpyridine under reduced pressure, returning the distillate before distillation to the distillation kettle for continuous purification, distilling the middle-stage distillate, namely the finished product of the 2-vinylpyridine, and taking the distillation bottom liquid as the fuel of the incinerator. The invention can effectively solve the problems existing in the post-treatment of the dehydration reaction, improve the production efficiency, reduce the energy consumption, save the production cost and solve the problems of large liquid caustic soda consumption and long standing and layering time in the dehydration reaction of the 2-vinylpyridine.
Description
Technical Field
The invention relates to the technical field of chemical reaction post-treatment, in particular to a 2-vinylpyridine reaction post-treatment method and a device thereof.
Background
The 2-vinylpyridine is an organic synthesis intermediate with wide application, can form terpolymer styrene-butadiene pyridine latex with butadiene and styrene, is a framework material of rubber products such as tires, conveyor belts and the like, and is required for tens of thousands of tons each year and is increased year by year in China. In addition, 2-vinylpyridine is an important polymer monomer, and has important application in medicine, ion exchange resin and chemical film.
The synthesis method of the 2-vinylpyridine mainly comprises a one-step method and a two-step method: the gas phase one-step method has few reaction process steps, adopts a fixed bed reactor for synthesis, is simple to operate, but has the reaction temperature of more than 300 ℃, and the 2-vinylpyridine is easy to carry the intermediate 2-hydroxyethyl pyridine, so the product purity is low; the industrial production generally adopts a liquid phase two-step reaction, including formaldehyde addition and dehydration, wherein the dehydration is the key to the industrial production. The patent CN200410024128.8 and CN201721175803.6 introduce a common dehydration reaction method, 2-hydroxyethyl pyridine and a catalyst are added into a distillation reactor according to a certain proportion, the catalyst is generally inorganic acid, alkali or supported solid alkali, dehydration reaction distillation is carried out under normal pressure, a mixed solution of 2-vinyl pyridine and water is evaporated under reduced pressure, then solid or high-concentration liquid alkali is added into the mixed solution, the mixed solution is dissolved and mixed uniformly, standing is carried out for 3-8 hours for layering, an organic layer rich in 2-vinyl pyridine is obtained, finally the organic layer rich in 2-vinyl pyridine is subjected to reduced pressure distillation, fractions of 60-100 ℃/90-150 mm/Hg are collected, and a finished product of 2-vinyl pyridine is obtained. The production process is simple, the yield is high, the reaction condition is normal pressure, the kettle type reactor can meet the production requirement, but the defects of large consumption of liquid alkali for treatment after reaction and long standing layering time exist, the production cost of the 2-vinylpyridine is increased, and the production efficiency is reduced.
Disclosure of Invention
The invention aims to provide a method and a device for post-treatment of 2-vinylpyridine reaction, which can effectively solve the problems existing in post-treatment of dehydration reaction, improve the production efficiency, reduce the energy consumption, save the production cost and solve the problems of large liquid caustic soda amount and long standing and layering time in the dehydration reaction of 2-vinylpyridine.
In order to achieve the purpose, the invention provides the following technical scheme:
a post-reaction treatment method of 2-vinylpyridine comprises the following steps:
step 1: 2-vinylpyridine and water mixed solution evaporated from a dehydration reaction kettle under reduced pressure is cooled in two stages by a first condenser and a second condenser, and then is stirred in an extraction kettle, an extraction solvent is added, and the mixture is stirred uniformly and layered after standing;
step 2: introducing the upper aqueous phase of the extraction kettle into a water phase storage tank, and introducing the lower organic phase into a distillation kettle to recover dichloromethane;
and step 3: and condensing the evaporated phase by a third condenser, introducing the condensed phase into a solvent storage tank, introducing the distillation bottom liquid into a pressure reduction kettle, evaporating the 2-vinylpyridine under reduced pressure, returning the distillate before distillation to the distillation kettle for continuous purification, distilling the middle-stage distillate, namely the finished product of the 2-vinylpyridine, and taking the distillation bottom liquid as the fuel of the incinerator.
Furthermore, the extraction solvent in the step 1 is an easily-recycled organic solvent which is incompatible with the water phase and has density difference with the water phase, the preferable solvent is dichloromethane, and the volume ratio of the extraction agent to the distilled mixed solution is 1-3: 1.
Further, the extraction stirring time of the step 1 is 5-20min, and the standing time is 10-60 min.
Further, in the step 1, the liquid outlet temperature of the first condenser is 50-80 ℃, and the liquid outlet temperature of the second condenser is 1-10 ℃.
Further, the first distillation of the distillation kettle adopts normal pressure distillation, the gas phase temperature is 40-60 ℃, the distillation is stopped when no liquid phase is distilled, the second distillation is carried out under reduced pressure, distillate with the temperature of 70-100 ℃/30-100 mm/Hg is collected, and the front distillate returns to the distillation kettle.
The invention provides another technical scheme: a2-vinylpyridine post-reaction treatment device comprises a dehydration reaction kettle, a first condenser, a second condenser, a pump A, an extraction kettle, a liquid separation sight glass, a water phase storage tank, a distillation kettle, a third condenser, a solvent storage tank, a pressure reduction kettle, a fourth condenser, a pump B, a four-way regulating valve, a 2-vinylpyridine storage tank and a bottom material tank, wherein a gas phase outlet of the dehydration reaction kettle is connected with a gas inlet of the first condenser, a liquid outlet of the first condenser is connected with a liquid inlet of the second condenser, a liquid outlet of the second condenser is connected with a liquid inlet of the extraction kettle, a liquid outlet of the extraction kettle is connected with one of liquid inlets of the distillation kettle through a lower organic phase of the liquid separation sight glass, an upper water phase is connected with the water phase storage tank, a gas phase outlet of the distillation kettle is connected with a gas inlet of the third condenser, the liquid phase outlet of the distillation kettle is connected with the liquid inlet of the pressure reduction kettle, the gas phase outlet of the pressure reduction kettle is connected with the air inlet of a fourth condenser, the liquid outlet of the fourth condenser is connected with the other liquid inlet of the distillation kettle through a pump B and the front fraction of a four-way regulating valve, the middle fraction of 70-100 ℃/30-100 mm/Hg is connected with the liquid inlet of a 2-vinylpyridine storage tank, and the rest distillation base material is connected with the liquid inlet of a base material tank.
Further, a pump A is connected between the second condenser and the extraction kettle.
Compared with the prior art, the invention has the beneficial effects that:
(1) the invention adopts a low-temperature extraction mode to replace the traditional alkali adding layering, avoids using a large amount of liquid alkali, simultaneously reduces the layering standing time and improves the production efficiency.
(2) The extraction solvent is dichloromethane, the boiling point is low, and the solvent is convenient to recycle.
(3) The temperature of the synthetic liquid is reduced by adopting series connection of secondary condensation, the extraction layering of the synthetic liquid is accelerated, and meanwhile, the primary condensation hydrophobic can be directly used as a heat source for solvent recovery, so that the energy consumption is reduced.
(4) The liquid is distilled out from the pressure reducing kettle, the front fraction is returned to the solvent recovery kettle for continuous purification, and the distillation bottom material is used as the fuel of the incinerator, so that the energy consumption is saved, and the three wastes are reduced.
Drawings
FIG. 1 is a schematic diagram showing the structure of a post-reaction apparatus for 2-vinylpyridine according to the present invention.
In the figure: 1. a dehydration reaction kettle; 2. a first condenser; 3. a second condenser; 4. a pump A; 5. an extraction kettle; 6. a liquid separating sight glass; 7. a water phase storage tank; 8. a distillation kettle; 9. a third condenser; 10. a solvent storage tank; 11. a pressure reduction kettle; 12. a fourth condenser; 13. a pump B; 14. a four-way regulating valve; 15. 2-vinylpyridine storage tank; 16. and (5) a bottom material tank.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1, a 2-vinylpyridine post-reaction treatment device comprises a dehydration reaction kettle 1, a first condenser 2, a second condenser 3, a pump A4, an extraction kettle 5, a liquid separation viewing mirror 6, a water phase storage tank 7, a distillation kettle 8, a third condenser 9, a solvent storage tank 10, a pressure reduction kettle 11, a fourth condenser 12, a pump B13, a four-way regulating valve 14, a 2-vinylpyridine storage tank 15 and a bottom material tank 16, wherein a gas phase outlet of the dehydration reaction kettle 1 is connected with a gas inlet of the first condenser 2, a liquid outlet of the first condenser 2 is connected with a liquid inlet of the second condenser 3, the first condenser 2 and the second condenser 3 are connected in series to gradually reduce the temperature of a synthetic liquid, a refrigerant of the first condenser 2 is cooled by circulating water, the circulating water is used for recycling waste heat, the refrigerant is directly used as a heat source of the distillation kettle 8 for heating and recovering the solvent, a frozen brine is used for cooling the, a liquid outlet of the second condenser 3 is connected with a liquid inlet of an extraction kettle 5, a pump A4 is also connected between the second condenser 3 and the extraction kettle 5, a liquid outlet of the extraction kettle 5 is connected with one liquid inlet of a distillation kettle 8 through a lower organic phase of a liquid separating sight glass 6, an upper aqueous phase is connected with an aqueous phase storage tank 7, a gas phase outlet of the distillation kettle 8 is connected with a gas inlet of a third condenser 9, a liquid outlet of the third condenser 9 is connected with a solvent storage tank 10, a liquid outlet of the solvent storage tank 10 is connected with a solvent liquid inlet of the extraction kettle 5, a liquid phase outlet of the distillation kettle 8 is connected with a liquid inlet of a pressure reducing kettle 11, a gas phase outlet of the pressure reducing kettle 11 is connected with a gas inlet of a fourth condenser 12, a liquid outlet of the fourth condenser 12 is connected with the other liquid inlet of the distillation kettle 8 through a pump B13 and a front, the 2-vinylpyridine storage tank 15 is provided with a cooling system, the temperature of the storage tank is kept at room temperature to prevent the finished product from polymerizing, the residual distillation bottom material is connected with a liquid inlet of the bottom material tank 16, the bottom material tank 16 is provided with a heating and heat-preserving system, and the temperature of the bottom material tank 16 is kept above 60 ℃ to facilitate burning in an incinerator.
The post-treatment method of the 2-vinylpyridine reaction comprises the following steps: the liquid outlet temperature of a 2-vinylpyridine and water mixed solution distilled under reduced pressure from a dehydration reaction kettle 1 is 60 ℃ through a first condenser 2, the liquid outlet temperature is 5 ℃ after cooling through a second condenser 3, the mixed solution is pumped into an extraction kettle 5, an extraction solvent dichloromethane with 2 times of the volume of the distilled liquid is added, the mixed solution is stirred for 10min and then stands for 30min for layering, an upper aqueous phase is introduced into an aqueous phase storage tank 7, a lower organic phase is introduced into a distillation kettle 8 for recycling the dichloromethane, the gas phase temperature of the distillation kettle 8 is 40 ℃, the distilled phase is condensed through a third condenser 9 and then introduced into a solvent storage tank 10, a distillation bottom liquid is introduced into a pressure reduction kettle 11, 2-vinylpyridine is distilled under reduced pressure, colorless transparent fractions with 70-100 ℃/30-100 mm/Hg are collected and pumped into a 2-vinylpyridine storage tank 15 (the content of the 2-vinylpyridine, the distillation bottoms are fed into a bottom tank 16 as incinerator fuel.
Example 2
The liquid outlet temperature of a 2-vinylpyridine and water mixed solution distilled under reduced pressure from a dehydration reaction kettle 1 is 60 ℃ through a first condenser 2, the liquid outlet temperature is 5 ℃ after cooling through a second condenser 3, the mixed solution is pumped into an extraction kettle 5, an extraction solvent dichloromethane with 3 times of the volume of the distilled liquid is added, the mixed solution is stirred for 5min and then stands for 30min for layering, an upper aqueous phase is introduced into an aqueous phase storage tank 7, a lower organic phase is introduced into a distillation kettle 8 for recycling the dichloromethane, the gas phase temperature of the distillation kettle 8 is 60 ℃, the distilled phase is condensed through a third condenser 9 and then introduced into a solvent storage tank 10, a distillation bottom liquid is introduced into a pressure reduction kettle 11, 2-vinylpyridine is distilled under reduced pressure, colorless transparent fractions with the temperature of 70-100 ℃/30-100 mm/Hg are collected and pumped into a 2-vinylpyridine storage tank 15 (the content of the 2, the distillation bottoms are fed into a bottom tank 16 as incinerator fuel.
Example 3
The liquid outlet temperature of a 2-vinylpyridine and water mixed solution distilled under reduced pressure from a dehydration reaction kettle 1 is 60 ℃ through a first condenser 2, the liquid outlet temperature is 10 ℃ after being cooled through a second condenser 3, the mixed solution is pumped into an extraction kettle 5, an extraction solvent dichloromethane with 2 times of the volume of the distilled liquid is added, the mixed solution is stirred for 20min and then is kept stand for 50min for layering, an upper aqueous phase is introduced into an aqueous phase storage tank 7, a lower organic phase is introduced into a distillation kettle 8 for recycling the dichloromethane, the gas phase temperature of the distillation kettle 8 is 50 ℃, the distilled phase is condensed through a third condenser 9 and then is introduced into a solvent storage tank 10, a distillation bottom liquid is introduced into a pressure reduction kettle 11, 2-vinylpyridine is distilled under reduced pressure, colorless transparent fractions with 70-100 ℃/30-100 mm/Hg are collected and pumped into a 2-vinylpyridine storage tank 15 (the content of the, the distillation bottoms are fed into a bottom tank 16 as incinerator fuel.
The invention adopts a low-temperature extraction mode to replace the traditional alkali-adding layering, avoids using a large amount of liquid alkali, simultaneously reduces the layering standing time, improves the production efficiency, adopts series-connection secondary condensation to reduce the temperature of the synthetic liquid, accelerates the extraction layering of the synthetic liquid, simultaneously can directly use primary condensation hydrophobic as a heat source for solvent recovery, reduces the energy consumption, can effectively solve the problems existing in the post-treatment of dehydration reaction, improves the production efficiency and saves the production cost.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be able to cover the technical solutions and the inventive concepts of the present invention within the technical scope of the present invention.
Claims (7)
1. A post-treatment method for 2-vinylpyridine reaction is characterized by comprising the following steps:
step 1: 2-vinylpyridine and water mixed solution evaporated from a dehydration reaction kettle (1) under reduced pressure is cooled in two stages by a first condenser (2) and a second condenser (3), and then is pumped into an extraction kettle (5), an extraction solvent is added, the mixture is stirred uniformly, and the mixture is layered after standing;
step 2: introducing the upper aqueous phase of the extraction kettle (5) into an aqueous phase storage tank (7), and introducing the lower organic phase into a distillation kettle (8) to recover dichloromethane;
and step 3: and (3) condensing the evaporated phase by a third condenser (9), introducing the condensed phase into a solvent storage tank (10), introducing the distillation bottom liquid into a decompression kettle (11), decompressing and evaporating 2-vinylpyridine, wherein the distillate before distillation returns to a distillation kettle (8) for continuous purification, the distillate in the middle section of distillation, namely the finished product of the 2-vinylpyridine, and the distillation bottom material is used as the fuel of an incinerator.
2. The method for post-reaction treatment of 2-vinylpyridine according to claim 1, wherein the extraction solvent of step 1 is selected from easily recoverable organic solvents that are incompatible with the aqueous phase and have a density difference with the aqueous phase, preferably dichloromethane, and the volume ratio of the extraction solvent to the distilled mixture is 1-3: 1.
3. The method for post-treatment of 2-vinylpyridine reaction of claim 1, wherein the extraction stirring time of step 1 is 5-20min, and the standing time is 10-60 min.
4. The process for working up 2-vinylpyridine after-reaction in accordance with claim 1, characterised in that in step 1 the first condenser (2) has an exit temperature of 50-80 ℃ and the second condenser (3) has an exit temperature of 1-10 ℃.
5. The method for post-reaction treatment of 2-vinylpyridine according to claim 1, wherein the first distillation in the distillation still (8) is atmospheric distillation, the gas phase temperature is 40-60 ℃, the distillation is stopped until no liquid phase is distilled, the second distillation is vacuum distillation, a fraction of 70-100 ℃/30-100 mm/Hg is collected, and the former fraction is returned to the distillation still (8).
6. The treatment device used in the 2-vinylpyridine reaction post-treatment method according to claim 1, comprising a dehydration reaction kettle (1), a first condenser (2), a second condenser (3), a pump A (4), an extraction kettle (5), a liquid separating sight glass (6), a water phase storage tank (7), a distillation kettle (8), a third condenser (9), a solvent storage tank (10), a decompression kettle (11), a fourth condenser (12), a pump B (13), a four-way regulating valve (14), a 2-vinylpyridine storage tank (15) and a bottom material tank (16), wherein a gas phase outlet of the dehydration reaction kettle (1) is connected with a gas inlet of the first condenser (2), a liquid outlet of the first condenser (2) is connected with a liquid inlet of the second condenser (3), a liquid outlet of the second condenser (3) is connected with a liquid inlet of the extraction kettle (5), the liquid outlet of the extraction kettle (5) is connected with one of the liquid inlets of the distillation kettle (8) through the lower organic phase of a liquid separating sight glass (6), the upper aqueous phase is connected with a water phase storage tank (7), the gas phase outlet of the distillation kettle (8) is connected with the gas inlet of a third condenser (9), the liquid outlet of the third condenser (9) is connected with a solvent storage tank (10), the liquid outlet of the solvent storage tank (10) is connected with the solvent liquid inlet of the extraction kettle (5), the liquid phase outlet of the distillation kettle (8) is connected with the liquid inlet of a pressure reducing kettle (11), the gas phase outlet of the pressure reducing kettle (11) is connected with the gas inlet of a fourth condenser (12), the liquid outlet of the fourth condenser (12) is connected with the other liquid inlet of the distillation kettle (8) through a pump B (13) and the front fraction of a four-way regulating valve (14), the middle fraction of 70-100 ℃/30, the residual distillation bottom materials are connected with a liquid inlet of a bottom material tank (16).
7. The apparatus for the work-up of 2-vinylpyridine reaction in accordance with claim 6, characterized in that a pump A (4) is also connected between the second condenser (3) and the extraction vessel (5).
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Application publication date: 20201229 |