CN112094217A - Efficient and environment-friendly recovery device and method for N-methylpyrrolidone - Google Patents

Efficient and environment-friendly recovery device and method for N-methylpyrrolidone Download PDF

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Publication number
CN112094217A
CN112094217A CN202010965368.7A CN202010965368A CN112094217A CN 112094217 A CN112094217 A CN 112094217A CN 202010965368 A CN202010965368 A CN 202010965368A CN 112094217 A CN112094217 A CN 112094217A
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China
Prior art keywords
pipe
recovery
methyl pyrrolidone
fixedly arranged
tank
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Chinese (zh)
Inventor
肖彤
王亚
张华�
连超
刘龙波
谷涛
陶斯强
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Anhui Shengjie New Energy Technology Co ltd
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Anhui Shengjie New Energy Technology Co ltd
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Priority to CN202010965368.7A priority Critical patent/CN112094217A/en
Publication of CN112094217A publication Critical patent/CN112094217A/en
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D207/00Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
    • C07D207/02Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
    • C07D207/18Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member
    • C07D207/22Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having one double bond between ring members or between a ring member and a non-ring member with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
    • C07D207/24Oxygen or sulfur atoms
    • C07D207/262-Pyrrolidones
    • C07D207/2632-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
    • C07D207/2672-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to the ring nitrogen atom
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D3/00Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14Fractional distillation or use of a fractionation or rectification column
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/002Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by condensation
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/1487Removing organic compounds
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D53/00Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/14Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by absorption
    • B01D53/18Absorbing units; Liquid distributors therefor

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Pyrrole Compounds (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)

Abstract

The invention discloses a high-efficiency environment-friendly recovery device and a method of N-methyl pyrrolidone, which comprises a three-way pipe, an A regulating valve, a heat exchanger, a B regulating valve, an A connecting pipe, an absorption tank, a spray pipe, a B connecting pipe, a I recovery tank, a plate rectifying tower, a C connecting pipe, a cooler, an active carbon filter and a II recovery tank, and the high-efficiency environment-friendly recovery device and the method of the N-methyl pyrrolidone can firstly realize the effective recovery of N-methyl pyrrolidone-containing gas by a spray absorption recovery method, secondly realize the effective recovery of N-methyl pyrrolidone-containing liquid by a plate rectification recovery method, simultaneously reduce the investment cost and realize good use because the same heat exchanger is shared, and finally achieve the purification purpose of waste gas generated by spray absorption recovery and plate rectification recovery because of adopting a gas filtering structure, in conclusion, the method has multiple process requirements for recovering the N-methyl pyrrolidone, and has higher popularization and application values.

Description

Efficient and environment-friendly recovery device and method for N-methylpyrrolidone
Technical Field
The invention relates to the technical field of recovery of N-methyl pyrrolidone, in particular to a high-efficiency environment-friendly recovery device and method of N-methyl pyrrolidone.
Background
Currently, N-methylpyrrolidone (NMP) is used in the production of lithium batteries. N-methyl pyrrolidone is a toxic chemical, and in the drying process of the lithium battery, N-methyl pyrrolidone is completely changed into gas and is discharged into the atmosphere along with heated air, so that the method of directly discharging the gas into the atmosphere seriously pollutes the air and causes harm to human bodies; secondly, the direct discharge process also causes a great amount of waste of the N-methyl pyrrolidone, and in addition, when some liquid containing the N-methyl pyrrolidone, such as waste liquid in the production process, cannot be directly used due to the fact that impurities are contained in the liquid, at present, measures for recycling the waste liquid containing the N-methyl pyrrolidone are lacked, so that the waste of the N-methyl pyrrolidone is greatly increased.
According to the above, in the prior art, the recovery of the organic solvent N-methylpyrrolidone is mainly carried out by adding a coagulant such as ethanol and the like for coagulation recovery. However, the method introduces a new organic solvent, which increases the manufacturing cost on one hand; on the other hand, poor sealing in the recovery process causes volatilization and waste of new organic solvent, and also causes environmental pollution. The high-temperature waste gas containing organic N-methyl pyrrolidone is condensed by a heat exchanger to obtain liquid N-methyl pyrrolidone, but when the liquid N-methyl pyrrolidone is received, part of uncondensed gas containing gaseous N-methyl pyrrolidone flows out together, and the waste liquid containing N-methyl pyrrolidone cannot be recycled well and efficiently, so that the N-methyl pyrrolidone is not recycled completely, and the environmental pollution is also caused. Therefore, in view of the above drawbacks, it is necessary to design an efficient and environment-friendly recycling device and method for N-methylpyrrolidone.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a high-efficiency environment-friendly recovery device of N-methyl pyrrolidone and a method thereof, which are used for solving the problems in the background technology.
In order to solve the technical problems, the technical scheme of the invention is as follows: a high-efficiency environment-friendly recovery device of N-methyl pyrrolidone and a method thereof comprise a three-way pipe, an A regulating valve, a heat exchanger, a B regulating valve, an A connecting pipe, an absorption tank, a spray pipe, a B connecting pipe, an I recovery tank, a plate-type rectifying tower, a C connecting pipe, a cooler, an activated carbon filter and a II recovery tank, wherein the A regulating valve is fixedly arranged on the right side of the front end of the three-way pipe, the A regulating valve is connected with the three-way pipe in a welding manner, the heat exchanger is fixedly arranged on the right side of the A regulating valve, the heat exchanger is connected with the A regulating valve in a welding manner, the B regulating valve is fixedly arranged on the right side of the heat exchanger, the B regulating valve is connected with the heat exchanger in a welding manner, the A connecting pipe is fixedly arranged on the right side of the B regulating valve, the A connecting pipe is connected with the B regulating valve in a welding manner, the, the spray pipe is fixedly arranged at the upper end inside the absorption tank, the spray pipe is connected with the absorption tank in a welding manner, the B connecting pipe is fixedly arranged at the right side of the absorption tank, the B connecting pipe is connected with the absorption tank in a welding manner, the I recovery tank is fixedly arranged at the right side of the B connecting pipe, the I recovery tank is connected with the B connecting pipe in a welding manner, the plate-type rectifying tower is fixedly arranged at the rear end of the right side of the three-way pipe, the plate-type rectifying tower is connected with the three-way pipe in a welding manner, the C connecting pipe is fixedly arranged at the right side of the plate-type rectifying tower, the C connecting pipe is connected with the plate-type rectifying tower in a welding manner, the cooler is fixedly arranged at the right side of the C connecting pipe, the cooler is connected with the C connecting pipe in a welding manner, the activated carbon filter is fixedly arranged at the right side of the cooler, the activated carbon filter is connected with the cooler, the II recovery tank is connected with the filtering carbon filter by welding.
Furthermore, a three-way valve is fixedly arranged at the middle end of the three-way pipe, and the three-way valve and the three-way pipe are integrally formed.
Further, the heat exchanger top still set firmly the C governing valve, C governing valve and heat exchanger adopt bolted connection, C governing valve top still set firmly the I honeycomb duct, I honeycomb duct and C governing valve adopt bolted connection, just I honeycomb duct and plate-type rectifying column adopt welded connection, I honeycomb duct right side still set firmly the I blast pipe, I blast pipe and I honeycomb duct adopt welded connection, the heat exchanger rear end still set firmly the D governing valve, D governing valve and heat exchanger adopt welded connection, D governing valve rear end still set firmly the II honeycomb duct, II honeycomb duct and D governing valve adopt bolted connection, just II honeycomb duct and plate-type rectifying column adopt welded connection.
Further, the inside middle-end of absorption jar still set firmly the filtration packing layer, filtration packing layer and absorption jar adopt the tight fit to be connected, the inside right side of filtration packing layer still set firmly the catheter, the catheter with filter the packing layer and adopt bolted connection, absorption tank top still set firmly the II blast pipe, II blast pipe and absorption jar adopt welded connection, just II blast pipe and I blast pipe adopt welded connection, II blast pipe bottom still set firmly the gas filtration jar, gas filtration jar and II blast pipe adopt welded connection, gas filtration jar right side lower extreme still set firmly the delivery pipe, delivery pipe and gas filtration jar adopt welded connection.
Furthermore, a suction pump is fixedly arranged at the top of the spray pipe and is connected with the spray pipe in a welding manner.
Further, I retrieve jar and II and retrieve jar right side lower extreme and still set firmly the flowing back valve, the flowing back valve adopt welded connection with I retrieve jar and II respectively.
Further, the top of the plate-type rectifying tower is fixedly provided with a pressure regulator, and the pressure regulator is connected with the plate-type rectifying tower through bolts.
A recovery method of a high-efficiency environment-friendly recovery device of N-methylpyrrolidone is characterized by comprising the following steps: the recovery method comprises a spray absorption recovery method and a plate rectification recovery method:
a spray absorption recovery method is adopted when N-methylpyrrolidone-containing gas needs to be recovered, and comprises the following steps:
step (1): adjusting the three-way valve to facilitate the subsequent gas containing the N-methyl pyrrolidone to flow into the heat exchanger;
step (2): when the gas containing the N-methyl pyrrolidone and with the temperature of 110-140 ℃ enters the heat exchanger through the three-way pipe, the temperature of the gas can be reduced to 50-60 ℃ under the action of the heat exchanger;
and (3): when the N-methyl pyrrolidone in the gas in the step (2) is condensed into a liquid state, the liquid can be fed into the absorption tank through the connecting pipe A;
and (4): after the liquid N-methyl pyrrolidone in the absorption tank in the step (3) passes through the connecting pipe B, the liquid N-methyl pyrrolidone can reach the inside of the recovery tank I;
and (5): when the gas containing part of N-methyl pyrrolidone in the absorption tank in the step (3) rises, the gas is contacted with the water sprayed from the spray pipe through the filter filler layer, so that the residual N-methyl pyrrolidone in the absorption gas is further condensed and is gathered into the I recovery tank from the lower end of the absorption tank through the liquid guide pipe, and at the moment, the spraying, absorbing and recovering treatment of the gas containing N-methyl pyrrolidone is realized through the above;
secondly, when the liquid containing the N-methyl pyrrolidone needs to be recovered, a plate type rectification recovery method can be adopted, and the method comprises the following steps:
step (1): the three-way valve is adjusted, so that the subsequent liquid containing the N-methyl pyrrolidone can flow into the plate-type rectifying tower;
step (2): after the liquid containing the N-methyl pyrrolidone at the temperature of 100-130 ℃ enters the plate type rectifying tower through the three-way pipe, the liquid is rectified under the action of the plate type rectifying tower;
and (3): when the distillation is carried out in the step (2), the pressure inside the plate-type distillation tower is regulated to be between-0.099 MPa and-0.05 MPa under the action of a pressure regulator, so that the distillation effect is improved;
and (4): when the rectified N-methylpyrrolidone stock solution in the step (3) passes through a cooler, the temperature can be reduced, and the N-methylpyrrolidone stock solution is recovered to be at the normal temperature;
and (5): and (4) performing adsorption filtration on the normal-temperature N-methylpyrrolidone stock solution in the step (4) again through an activated carbon filter to ensure that the obtained high-purity N-methylpyrrolidone liquid is converged into a II recovery tank, and realizing plate rectification recovery treatment on the N-methylpyrrolidone-containing liquid through the steps.
Compared with the prior art, the efficient and environment-friendly recovery device and method for N-methylpyrrolidone have the following advantages:
1. firstly, the spraying absorption recovery method can realize the effective recovery of the gas containing the N-methyl pyrrolidone, thereby realizing the pertinence.
2. And secondly, the plate-type rectification recovery method can realize effective recovery of the liquid containing the N-methyl pyrrolidone, thereby not only realizing pertinence, but also improving the operation efficiency.
3. Meanwhile, the same heat exchanger is shared by spray absorption recovery and plate rectification recovery, so that the investment cost of equipment is reduced, and good use is realized.
4. Finally, due to the adoption of a gas filtering structure, the purposes of filtering and purifying waste gas generated in the processes of spraying, absorbing and recovering and plate-type rectifying and recovering can be achieved, the protection of the surrounding environment and air is achieved, and in conclusion, the invention considers various process requirements of N-methyl pyrrolidone recovery and has higher popularization and application values.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
FIG. 1 is a front view of an efficient and environmentally friendly recovery apparatus of N-methylpyrrolidone and a method thereof;
FIG. 2 is a top view of an efficient and environmentally friendly recycling apparatus and method for N-methylpyrrolidone;
FIG. 3 is a sectional view of the apparatus and method for recovering N-methylpyrrolidone in the direction A;
FIG. 4 is a perspective view of an efficient and environmentally friendly recycling apparatus for N-methylpyrrolidone and a method thereof, FIG. 1;
FIG. 5 is a perspective view of an efficient and environmentally friendly recycling apparatus for N-methylpyrrolidone and a method thereof, FIG. 2;
FIG. 6 is a perspective view of an efficient and environmentally friendly recycling apparatus for N-methylpyrrolidone and a method thereof, FIG. 3;
FIG. 7 is a perspective view of an efficient and environmentally friendly recycling apparatus for N-methylpyrrolidone and a method thereof, FIG. 4.
The system comprises a three-way pipe 1, an A regulating valve 2, a heat exchanger 3, a B regulating valve 4, an A connecting pipe 5, an absorption tank 6, a spray pipe 7, a B connecting pipe 8, an I recovery tank 9, a plate rectifying tower 10, a C connecting pipe 11, a cooler 12, an activated carbon filter 13, a II recovery tank 14, a three-way valve 101, a C regulating valve 301, an I guide pipe 302, an I exhaust pipe 303, a D regulating valve 304, an II guide pipe 305, a filtering packing layer 601, a liquid guide pipe 602, an II exhaust pipe 603, a gas filtering tank 604, a discharge pipe 605, a suction pump 701, a liquid discharge valve 901 and a pressure regulator 1001.
The following detailed description will be further described in conjunction with the above-identified drawings.
Detailed Description
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the concepts underlying the described embodiments, however, it will be apparent to one skilled in the art that the described embodiments may be practiced without some or all of these specific details, and in other cases well-known process steps have not been described in detail.
In the description of the present invention, it is to be understood that the terms "upper", "lower", "front", "rear", "left", "right", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, are merely for convenience in describing the invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the invention.
As shown in figures 1, 2, 3, 4, 5, 6 and 7, the device comprises a three-way pipe 1, an A regulating valve 2, a heat exchanger 3, a B regulating valve 4, an A connecting pipe 5, an absorption tank 6, a spray pipe 7, a B connecting pipe 8, an I recovery tank 9, a plate type rectifying tower 10, a C connecting pipe 11, a cooler 12, an activated carbon filter 13 and a II recovery tank 14, wherein the A regulating valve 2 is fixedly arranged at the right side of the front end of the three-way pipe 1, the A regulating valve 2 is connected with the three-way pipe 1 in a welding way, the heat exchanger 3 is fixedly arranged at the right side of the A regulating valve 2, the heat exchanger 3 is connected with the A regulating valve 2 in a welding way, the B regulating valve 4 is fixedly arranged at the right side of the heat exchanger 3, the B regulating valve 4 is connected with the heat exchanger 3 in a welding way, the A connecting pipe 5 is fixedly arranged at the right side of the B regulating valve 4, the A connecting pipe 5 and the B regulating valve 4 are connected by welding, the absorption tank 6 is fixedly arranged on the right side of the A connecting pipe 5, the absorption tank 6 and the A connecting pipe 5 are connected by welding, the spray pipe 7 is fixedly arranged at the upper end inside the absorption tank 6, the spray pipe 7 and the absorption tank 6 are connected by welding, the B connecting pipe 8 is fixedly arranged on the right side of the absorption tank 6, the B connecting pipe 8 and the absorption tank 6 are connected by welding, the I recovery tank 9 is fixedly arranged on the right side of the B connecting pipe 8, the I recovery tank 9 and the B connecting pipe 8 are connected by welding, the plate rectifying tower 10 is fixedly arranged at the rear end of the right side of the three-way pipe 1, the plate rectifying tower 10 is connected with the three-way pipe 1 by welding, the C connecting pipe 11 is fixedly arranged on the right side of the plate rectifying tower 10, the C connecting pipe 11 is connected with the rectifying tower 10 by welding, the cooler 12 is fixedly arranged on the right side of the C connecting pipe 11, the cooler 12 is connected with the C connecting pipe 11 in a welding mode, the activated carbon filter 13 is fixedly arranged on the right side of the cooler 12, the activated carbon filter 13 is connected with the cooler 12 in a welding mode, the II recovery tank 14 is fixedly arranged on the right side of the activated carbon filter 13, and the II recovery tank 14 is connected with the filtering carbon filter 13 in a welding mode;
the efficient and environment-friendly recovery device and the method for the N-methylpyrrolidone have the following functions;
A. through the mutual matching action of the three-way pipe 1, the A regulating valve 2, the heat exchanger 3, the B regulating valve 4, the A connecting pipe 5, the absorption tank 6, the spray pipe 7, the B connecting pipe 8 and the I recovery tank 9, the spray absorption recovery method is realized, N-methyl pyrrolidone-containing gas can be recovered, and meanwhile, when the subsequent plate type rectification recovery method is carried out, the A regulating valve 2 and the B regulating valve 4 can be closed, namely, the liquid in the plate type rectification recovery method is prevented from flowing into the absorption tank 6;
B. the plate type rectification recovery method is realized through the mutual matching effect of the three-way pipe 1, the plate type rectifying tower 10, the heat exchanger 3, the C connecting pipe 11, the cooler 12, the activated carbon filter 13 and the II recovery tank 14, and the liquid containing N-methyl pyrrolidone can be recovered;
the middle end of the three-way pipe 1 is also fixedly provided with a three-way valve 101, and the three-way valve 101 and the three-way pipe 1 are integrally formed;
it should be noted that the three-way valve 101 can facilitate the switching of the flow direction of the three-way pipe 1 by the operator, and facilitate the different recovery processes;
the top of the heat exchanger 3 is fixedly provided with a C regulating valve 301, the C regulating valve 301 is connected with the heat exchanger 3 through a bolt, the top of the C regulating valve 301 is fixedly provided with an I guide pipe 302, the I guide pipe 302 is connected with the C regulating valve 301 through a bolt, the I guide pipe 302 is connected with the plate-type rectifying tower 10 through welding, the right side of the I guide pipe 302 is fixedly provided with an I exhaust pipe 303, the I exhaust pipe 303 is connected with the I guide pipe 302 through welding, the rear end of the heat exchanger 3 is fixedly provided with a D regulating valve 304, the D regulating valve 304 is connected with the heat exchanger 303 through welding, the rear end of the D regulating valve 304 is fixedly provided with a II guide pipe 305, the II guide pipe 305 is connected with the D regulating valve 304 through a bolt, and the II guide pipe 305 is connected with the rectifying plate-type rectifying tower 10 through welding;
it should be noted that the C regulating valve 301 and the D regulating valve 304 can be opened or closed, which is convenient for a worker to switch to open according to different processes, thereby realizing the use of a spray absorption recovery method or a plate rectification recovery method, the I draft tube 302 is convenient for liquid to flow back into the plate rectification tower 10, the I exhaust tube 303 is capable of guiding gas in the plate rectification tower 10 to the II exhaust tube 603, and the II draft tube 305 is convenient for liquid containing N-methylpyrrolidone after heat exchange to flow back into the plate rectification tower 10;
the middle end in the absorption tank 6 is fixedly provided with a filtering filler layer 601, the filtering filler layer 601 is tightly matched and connected with the absorption tank 6, the right side in the filtering filler layer 601 is fixedly provided with a liquid guide pipe 602, the liquid guide pipe 602 is connected with the filtering filler layer 601 through a bolt, the top of the absorption tank 6 is fixedly provided with an II exhaust pipe 603, the II exhaust pipe 603 is connected with the absorption tank 6 through welding, the II exhaust pipe 603 is connected with the I exhaust pipe 303 through welding, the bottom of the II exhaust pipe 603 is fixedly provided with a gas filter tank 604, the gas filter tank 604 is connected with the II exhaust pipe 603 through welding, the lower end of the right side of the gas filter tank 604 is fixedly provided with a discharge pipe 605, and the discharge pipe 605 is connected with the gas filter tank 604 through welding;
it should be noted that the filter filler layer 601 can block the inside of the absorption tank 6, the inside of the filter filler layer contains micropores through which gas can pass, but liquid can be blocked, the liquid guide tube 602 can facilitate liquid to flow into the lower end of the inside of the absorption tank 6, the II gas exhaust tube 603 can facilitate exhaust gas to be discharged into the gas filter tank 604, the gas filter tank 604 can block and adsorb pollution particles in the gas, the purpose of filtering and purifying is achieved, and the exhaust tube 605 facilitates the purified gas to be discharged into the air;
a suction pump 701 is fixedly arranged at the top of the spray pipe 7, and the suction pump 701 is connected with the spray pipe 7 in a welding manner;
it should be noted that the suction pump 701 can be connected to an existing water supply (not shown), and when turned on, facilitates the supply of water through the suction pump 701 to the interior of the shower pipe 7;
the lower ends of the right sides of the I recovery tank 9 and the II recovery tank 14 are fixedly provided with a liquid discharge valve 901, and the liquid discharge valve 901 is respectively connected with the I recovery tank 9 and the II recovery tank 14 in a welding manner;
it should be noted that the drain valve 901 can be connected to an existing N-methylpyrrolidone transportation barrel (not labeled), and when opened, facilitates the outward transportation of the N-methylpyrrolidone product;
a pressure regulator 1001 is fixedly arranged at the top of the plate-type rectifying tower 10, and the pressure regulator 1001 is connected with the plate-type rectifying tower 10 through bolts;
it should be noted that the pressure regulator 1001 is convenient for the staff to perform pressurization or depressurization treatment on the inside of the plate-type rectifying tower 10;
the recovery method of the high-efficiency environment-friendly recovery device for N-methyl pyrrolidone adopts a spray absorption recovery method when N-methyl pyrrolidone-containing gas needs to be recovered, firstly, a three-way valve 101 is adjusted, even if the subsequent N-methyl pyrrolidone-containing gas flows into a heat exchanger 3, when the N-methyl pyrrolidone-containing gas with the temperature of 110-140 ℃ enters the heat exchanger 3 through a three-way pipe 1, the temperature of the N-methyl pyrrolidone-containing gas can be reduced to 50-60 ℃ through the action of the heat exchanger 3, when the N-methyl pyrrolidone of the gas is condensed into liquid, the N-methyl pyrrolidone can reach the inside of a recovery tank I6 through an A connecting pipe 5, when the liquid N-methyl pyrrolidone in the absorption tank 6 passes through a B connecting pipe 8, the N-methyl pyrrolidone can reach the inside of the recovery tank I, when the gas containing part of N-methyl pyrrolidone in the absorption tank 9 rises, namely, the residual N-methyl pyrrolidone in the absorption gas is further condensed by the contact of the filtering filler layer 601 and the water sprayed from the spray pipe 7, and then the residual N-methyl pyrrolidone in the absorption gas is converged into the I recovery tank 9 from the lower end of the absorption tank 6 through the liquid guide pipe 602, at this time, the spraying absorption recovery treatment of the N-methyl pyrrolidone-containing gas is realized through the above steps, when the liquid containing the N-methyl pyrrolidone needs to be recovered, a plate type rectification recovery method can be adopted, firstly, the three-way valve 101 is adjusted, even if the subsequent liquid containing the N-methyl pyrrolidone flows into the plate type rectification tower 10, when the liquid containing the N-methyl pyrrolidone with the temperature of 100-130 ℃ enters the plate type rectification tower 10 through the three-way pipe 1, the liquid is rectified through the action of the plate type rectification tower 10, and when the liquid is rectified, through the action of the pressure regulator 1001, the internal pressure of the plate type rectifying tower 10 is regulated to be between-0.099 MPa and-0.05 MPa, the rectifying effect is improved, when the rectified N-methyl pyrrolidone raw liquid passes through the cooler 12, the temperature can be reduced, the N-methyl pyrrolidone raw liquid is recovered to be at the normal temperature, when the normal temperature N-methyl pyrrolidone raw liquid passes through the activated carbon filter 13 for adsorption and filtration again, the obtained high-purity N-methyl pyrrolidone liquid is gathered in the II recovery tank 14, and at the moment, the plate type rectifying recovery treatment of the N-methyl pyrrolidone liquid is realized through the above steps.

Claims (8)

1. A high-efficiency environment-friendly recovery device of N-methyl pyrrolidone is characterized by comprising a three-way pipe, an A regulating valve, a heat exchanger, a B regulating valve, an A connecting pipe, an absorption tank, a spray pipe, a B connecting pipe, an I recovery tank, a plate type rectifying tower, a C connecting pipe, a cooler, an activated carbon filter and a II recovery tank, wherein the A regulating valve is fixedly arranged on the right side of the front end of the three-way pipe, the heat exchanger is fixedly arranged on the right side of the A regulating valve, the B regulating valve is fixedly arranged on the right side of the heat exchanger, the A connecting pipe is fixedly arranged on the right side of the B regulating valve, the absorption tank is fixedly arranged on the right side of the A connecting pipe, the spray pipe is fixedly arranged at the upper end inside of the absorption tank, the B connecting pipe is fixedly arranged on the right side of the absorption tank, the I recovery tank is fixedly arranged on the right side of the B connecting pipe, the plate type rectifying, the cooler sets firmly in C connecting pipe right side, activated carbon filter set firmly in the cooler right side, II retrieve the jar and set firmly in activated carbon filter right side.
2. The device for recovering N-methylpyrrolidone in an efficient and environment-friendly manner as claimed in claim 1, wherein a three-way valve is further fixedly arranged at the middle end of the three-way pipe.
3. The apparatus as claimed in claim 2, wherein the heat exchanger has a C regulating valve at the top, an I flow guide pipe at the top, a I exhaust pipe at the right side, a D regulating valve at the rear end, a II flow guide pipe at the rear end, and a plate-type rectifying tower at the rear end.
4. The device for recycling N-methylpyrrolidone in an efficient and environment-friendly manner as claimed in claim 3, wherein a filtering filler layer is further fixedly arranged at the middle end inside the absorption tank, a liquid guide pipe is further fixedly arranged at the right side inside the filtering filler layer, a II exhaust pipe is further fixedly arranged at the top of the absorption tank, the II exhaust pipe is connected with the I exhaust pipe in a welding manner, a gas filtering tank is further fixedly arranged at the bottom of the II exhaust pipe, and a discharge pipe is further fixedly arranged at the lower end of the right side of the gas filtering tank.
5. The apparatus for recovering N-methylpyrrolidone with high efficiency and environmental friendliness according to claim 4, wherein a suction pump is further fixedly arranged at the top of the spray pipe.
6. The efficient and environment-friendly recovery device of N-methylpyrrolidone, as claimed in claim 5, wherein the lower ends of the right sides of the recovery tank I and the recovery tank II are further fixedly provided with drain valves.
7. The efficient and environment-friendly recovery device of N-methylpyrrolidone according to claim 6, wherein a pressure regulator is further fixedly arranged at the top of the plate-type rectifying tower.
8. The method for recycling N-methylpyrrolidone, which is a high-efficiency and environment-friendly recycling device, according to claim 7, is characterized in that: the recovery method comprises a spray absorption recovery method and a plate rectification recovery method:
a spray absorption recovery method is adopted when N-methylpyrrolidone-containing gas needs to be recovered, and comprises the following steps:
step (1): adjusting the three-way valve to facilitate the subsequent gas containing the N-methyl pyrrolidone to flow into the heat exchanger;
step (2): when the gas containing the N-methyl pyrrolidone and with the temperature of 110-140 ℃ enters the heat exchanger through the three-way pipe, the temperature of the gas can be reduced to 50-60 ℃ under the action of the heat exchanger;
and (3): when the N-methyl pyrrolidone in the gas in the step (2) is condensed into a liquid state, the liquid can be fed into the absorption tank through the connecting pipe A;
and (4): after the liquid N-methyl pyrrolidone in the absorption tank in the step (3) passes through the connecting pipe B, the liquid N-methyl pyrrolidone can reach the inside of the recovery tank I;
and (5): when the gas containing part of N-methyl pyrrolidone in the absorption tank in the step (3) rises, the gas is contacted with the water sprayed from the spray pipe through the filter filler layer, so that the residual N-methyl pyrrolidone in the absorption gas is further condensed and is gathered into the I recovery tank from the lower end of the absorption tank through the liquid guide pipe, and at the moment, the spraying, absorbing and recovering treatment of the gas containing N-methyl pyrrolidone is realized through the above;
secondly, when the liquid containing the N-methyl pyrrolidone needs to be recovered, a plate type rectification recovery method can be adopted, and the method comprises the following steps:
step (1): the three-way valve is adjusted, so that the subsequent liquid containing the N-methyl pyrrolidone can flow into the plate-type rectifying tower;
step (2): after the liquid containing the N-methyl pyrrolidone at the temperature of 100-130 ℃ enters the plate type rectifying tower through the three-way pipe, the liquid is rectified under the action of the plate type rectifying tower;
and (3): when the distillation is carried out in the step (2), the pressure inside the plate-type distillation tower is regulated to be between-0.099 MPa and-0.05 MPa under the action of a pressure regulator, so that the distillation effect is improved;
and (4): when the rectified N-methylpyrrolidone stock solution in the step (3) passes through a cooler, the temperature can be reduced, and the N-methylpyrrolidone stock solution is recovered to be at the normal temperature;
and (5): and (4) performing adsorption filtration on the normal-temperature N-methylpyrrolidone stock solution in the step (4) again through an activated carbon filter to ensure that the obtained high-purity N-methylpyrrolidone liquid is converged into a II recovery tank, and realizing plate rectification recovery treatment on the N-methylpyrrolidone-containing liquid through the steps.
CN202010965368.7A 2020-09-15 2020-09-15 Efficient and environment-friendly recovery device and method for N-methylpyrrolidone Pending CN112094217A (en)

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Application publication date: 20201218