CN113521782A - Be used for NMP to retrieve refined reactor - Google Patents
Be used for NMP to retrieve refined reactor Download PDFInfo
- Publication number
- CN113521782A CN113521782A CN202110971125.9A CN202110971125A CN113521782A CN 113521782 A CN113521782 A CN 113521782A CN 202110971125 A CN202110971125 A CN 202110971125A CN 113521782 A CN113521782 A CN 113521782A
- Authority
- CN
- China
- Prior art keywords
- defoaming
- nmp
- sliding block
- reactor
- sieve plate
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
- B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
- B01D5/006—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes with evaporation or distillation
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic 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
- C07D207/18—Heterocyclic 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
- C07D207/22—Heterocyclic 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
- C07D207/24—Oxygen or sulfur atoms
- C07D207/26—2-Pyrrolidones
- C07D207/263—2-Pyrrolidones with only hydrogen atoms or radicals containing only hydrogen and carbon atoms directly attached to other ring carbon atoms
- C07D207/267—2-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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention discloses a reactor for recovering and refining NMP, which comprises a tower seat, a tower kettle, a first filler section, a second filler section and a tower top, wherein the tower seat is provided with a first opening and a second opening; an air outlet, a defoaming sieve plate, a reflux driving assembly and a defoaming wire mesh are arranged in the tower top; the defoaming sieve plate is provided with a plurality of fine sieve pores; the backflow driving assembly drives the defoaming sieve plate to rotate through backflow hydraulic pressure so as to remove liquid foam in gas entering the gas outlet; according to the invention, the rotatable defoaming sieve plate is matched with the defoaming wire mesh, so that liquid foam carried by gas can be better removed, and the pollution to products or condensed liquid is avoided; the backflow driving assembly is arranged, the sliding block reciprocates to drive the defoaming sieve plate to rotate for defoaming through the hydraulic change in the driving cavity and the matching of the tension spring, no additional driving element is needed, the structure is simplified, and the cost is reduced; the invention can complete the dehydration and weight removal treatment of the NMP waste liquid recovery, thereby obtaining the NMP product with simple process and stable performance.
Description
Technical Field
The invention relates to the technical field of NMP recovery, in particular to a reactor for recovering and refining NMP.
Background
The chemical name of NMP is N-methyl pyrrolidone (NMP), which is colorless to light yellow transparent liquid, has slight ammonia smell, can be mixed and dissolved with water in any proportion, can also be dissolved in organic solvents such as ether, acetone, ester, halogenated hydrocarbon, aromatic hydrocarbon and the like, and can be almost completely mixed with all solvents. NMP is a high-boiling point and environment-friendly excellent solvent, and has the advantages of low viscosity, good chemical stability and thermal stability, high polarity, low volatility and the like. The NMP has wide application fields, and is mainly focused in industries such as lithium batteries, circuit boards, insulating materials, petrifaction, medicines, pesticides, macromolecules and the like. NMP is produced mainly by ammonification of GBL with monomethylamine. In order to improve economic benefit, the NMP waste liquid in industrial production is generally recycled; in the prior art, NMP waste liquid recovery generally adopts three-tower or four-tower rectification, so that the process is redundant and the energy consumption is high; and liquid foam is easily entrained in the gas flowing out of the reactor during rectification, so that useful products are lost or the condensed liquid is polluted.
Disclosure of Invention
The invention aims to provide a reactor for recovering and refining NMP, which solves the problem of poor defoaming effect in the prior art.
In order to solve the technical problems, the reactor for recovering and refining the NMP provided by the invention comprises a tower seat, a tower kettle, a first filling section, a second filling section and a tower top; an air outlet, a defoaming sieve plate, a reflux driving assembly and a defoaming wire mesh are arranged in the tower top; the defoaming sieve plate is provided with a plurality of fine sieve pores; the backflow driving assembly drives the defoaming sieve plate to rotate through backflow hydraulic pressure so as to remove liquid foam in gas entering the gas outlet.
Preferably, the backflow driving component comprises a backflow pipe, a sliding block, a gear, a rotating shaft and a tension spring; a flow channel is arranged in the return pipe, a stop block is arranged in the flow channel, and a guide rod is arranged at one end of the stop block; the sliding block is connected with the guide rod in a sliding mode, and the sliding block and the stop block form a driving cavity; the tension spring is sleeved on the guide rod, one end of the tension spring is fixedly connected with the stop block, the other end of the tension spring is fixedly connected with the sliding block, and the tension spring forces the sliding block to move towards the direction close to the stop block; the rotating shaft is rotatably connected to the lower end of the defoaming screen, the lower side of the rotating shaft is fixedly connected with the gear, and the upper side of the rotating shaft is fixedly connected with the defoaming sieve plate; the gear is meshed with the rack section on the sliding block; the hydraulic pressure in the driving cavity is used for driving the sliding block to drive the defoaming sieve plate to rotate; the extension spring is used for making the sliding block reset.
Preferably, the bottom of the tower kettle is provided with a discharge pipe, a reboiling connecting pipe and a reboiling steam inlet; the tower kettle is connected with the first packing section through a conical section; the first filling section and the second filling section are both provided with filling materials, the lower end of each filling material is provided with a filling material supporting member, and the upper end of each filling material is provided with a filling material pressing member; and a feeding pipe is arranged between the first filling section and the second filling section.
Preferably, the liquid distribution device is arranged below the return pipe and the feeding pipe, and is used for reducing amplification effect caused by liquid maldistribution.
Preferably, the lower end of the first packing section is provided with a liquid redistribution device for preventing wall flow, the liquid redistribution device is in a circular truncated cone shape, and the peripheral wall of the outer side of the liquid redistribution device is provided with a plurality of flow guide grooves.
Preferably, the tower kettle and the tower top are both provided with a hydraulic pressure measuring port and a temperature measuring port.
Preferably, a seal ring is provided between the slider and the return pipe.
Preferably, a seal ring is provided between the slide block and the guide rod.
Preferably, a reflux liquid outlet for discharging liquid is arranged on the side wall of the reflux pipe.
After adopting the structure, compared with the prior art, the invention has the following advantages: according to the invention, the rotatable defoaming sieve plate is matched with the defoaming wire mesh, so that liquid foam carried by gas can be better removed, and the pollution to products or condensed liquid is avoided; the backflow driving assembly is arranged, the sliding block reciprocates to drive the defoaming sieve plate to rotate for defoaming through the hydraulic change in the driving cavity and the matching of the tension spring, no additional driving element is needed, the structure is simplified, and the cost is reduced; the invention can complete the dehydration and weight removal treatment of the NMP waste liquid recovery, thereby obtaining the NMP product with simple process and stable performance.
Drawings
FIG. 1 is a cross-sectional view of the present invention;
FIG. 2 is an enlarged view of area A of FIG. 1 in accordance with the present invention;
FIG. 3 is an enlarged view of area B of FIG. 1 in accordance with the present invention;
FIG. 4 is an enlarged view of the area C of FIG. 1 in accordance with the present invention;
FIG. 5 is a three-dimensional block diagram of the liquid redistribution device of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
As shown in fig. 1 to 5, the reactor for NMP recovery and purification according to the present invention comprises a column base 1, a column bottom 2, a first packing section 3, a second packing section 4, and a column top 5; an air outlet 51, a defoaming sieve plate 52, a reflux driving assembly 53 and a defoaming wire mesh 54 are arranged in the tower top 5; the defoaming sieve plate 52 is provided with a plurality of fine sieve holes; the backflow driving assembly 53 drives the defoaming sieve plate 52 to rotate through backflow hydraulic pressure, so as to remove liquid foam in the gas entering the gas outlet 51.
The backflow driving assembly 53 comprises a backflow pipe 531, a sliding block 532, a gear 533, a rotating shaft 534 and a tension spring 535; a flow channel 5311 is arranged in the return pipe 531, a stop 5312 is arranged in the flow channel 5311, and a guide rod 5313 is arranged at one end of the stop 5312; the sliding block 532 is connected with the guide rod 5313 in a sliding way, and the sliding block 532 and the stop 5312 form a driving cavity 5314; the tension spring 535 is sleeved on the guide rod 5313, one end of the tension spring 535 is fixedly connected with the stop 5312, the other end of the tension spring 535 is fixedly connected with the sliding block 532, and the tension spring 535 forces the sliding block 532 to move towards the direction close to the stop 5312; the rotating shaft 534 is rotatably connected to the lower end of the defoaming screen 54, the lower side of the rotating shaft 534 is fixedly connected with the gear 533, and the upper side of the rotating shaft 534 is fixedly connected with the defoaming screen plate 52; the gear 533 is meshed with the rack section on the sliding block 532; the hydraulic pressure in the driving cavity 5314 is used for driving the sliding block 532 to drive the defoaming sieve plate 52 to rotate; the tension spring 535 is used to reset the slider 532; when the device works specifically, reflux liquid generated by condensation is pumped into the flow channel 5311 through a pump element, when the hydraulic pressure in the driving cavity 5314 reaches a certain value, the hydraulic pressure pushes the sliding block 532 to move in the direction away from the stop block 5312 by overcoming the acting force of the tension spring 535, in the process, as the rack section on the sliding block 532 is meshed with the gear 533, the gear 533 drives the defoaming sieve plate 52 to rotate until the sliding block 532 moves to the position where the driving cavity 5314 is communicated with the interior of the tower top 5, the liquid in the driving cavity 5314 enters the tower top 5, the tension spring 535 resets the sliding block 532 until the hydraulic pressure in the driving cavity 5314 reaches a certain value next time, and the sliding block 532 repeats the actions; through the hydraulic change in the drive chamber 5314 and the cooperation of extension spring 535 for slider 532 reciprocating motion drives the rotatory defoaming of defoaming sieve 52, has reduced the liquid foam quantity that gets into the condenser, relies on hydraulic drive simultaneously, need not additionally to set up driving element, has simplified the structure, has reduced the cost.
The bottom of the tower kettle 2 is provided with a discharge pipe 21, a reboiling connecting pipe 22 and a reboiling steam inlet 23; the tower kettle 2 is connected with the first filling section 3 through a conical section; the first filler section 3 and the second filler section 4 are both internally provided with fillers 31, the lower end of each filler 31 is provided with a filler supporting member 32, and the upper end of each filler 31 is provided with a filler pressing member 33; a feeding pipe 34 is arranged between the first filling section 3 and the second filling section 4; in the embodiment, the CY700 wire mesh corrugated packing is preferably adopted as the packing 31, and has the advantages of good corrosion resistance, high separation efficiency and small operation pressure drop; the filler support 32 is preferably a grid-type support; the packing hold-down element 33 is preferably a packing cage of parallel flat steel construction.
A liquid distribution device 341 for reducing amplification effect caused by liquid maldistribution is arranged below the return pipe 531 and the feed pipe 34; in this embodiment, the liquid distributor 341 is a calandria distributor.
The lower end of the first packing section 3 is provided with a liquid redistribution device 35 for preventing wall flow, the liquid redistribution device 35 is in a shape of a circular truncated cone, and the peripheral wall of the outer side of the liquid redistribution device is provided with a plurality of flow guide grooves 351.
The tower kettle 2 and the tower top 5 are both provided with a hydraulic pressure measuring port 61 and a temperature measuring port 62; the internal conditions of the reactor can be conveniently monitored through the hydraulic pressure measuring port 61 and the temperature measuring port 62, and the production efficiency and the safety are improved.
And a sealing ring is arranged between the sliding block 532 and the return pipe 531.
And a sealing ring is arranged between the sliding block 532 and the guide rod 5313.
A reflux liquid outlet 5316 for discharging liquid is disposed on a side wall of the reflux pipe 531.
The reactor for recovering and refining the NMP can be used for the dehydration treatment of the NMP waste liquid: pumping NMP waste liquid into a reactor, discharging water from the top of the reactor after negative pressure rectification, condensing, discharging one part of formed condensate as waste water, refluxing the other part of the formed condensate to the reactor, wherein the reflux ratio is 0.65-0.7, and discharging a crude NMP material from a discharge pipe 21 at the bottom of the reactor; simultaneously, the method can also be used for removing the weight of crude NMP materials: sending the crude NMP material into a reactor, discharging NMP gas phase from the top of the reactor after negative pressure de-weighting and condensing, sending out a part of formed condensate as a product, refluxing the other part of the formed condensate into the reactor, wherein the reflux ratio is 0.45-0.55, and sequentially dehydrating and de-weighting NMP waste liquid in the reactor to obtain an NMP product.
The above description is only about the preferred embodiment of the present invention, but it should not be understood as limiting the claims, and the present invention may be modified in other structures, not limited to the above structures. In general, all changes which come within the scope of the invention as defined by the independent claims are intended to be embraced therein.
Claims (9)
1. A reactor for recovering and refining NMP is characterized by comprising a tower base (1), a tower kettle (2), a first filling section (3), a second filling section (4) and a tower top (5); an air outlet (51), a defoaming sieve plate (52), a reflux driving assembly (53) and a defoaming wire mesh (54) are arranged in the tower top (5); the defoaming sieve plate (52) is provided with a plurality of fine sieve holes; the backflow driving assembly (53) drives the defoaming sieve plate (52) to rotate through backflow hydraulic pressure so as to remove liquid foam in the gas entering the gas outlet (51).
2. The NMP recovery refining reactor according to claim 1, wherein the reflux driving assembly (53) comprises a reflux pipe (531), a slide block (532), a gear (533), a rotating shaft (534), and a tension spring (535); a flow channel (5311) is arranged in the return pipe (531), a stop block (5312) is arranged in the flow channel (5311), and a guide rod (5313) is arranged at one end of the stop block (5312); the sliding block (532) is connected with the guide rod (5313) in a sliding mode, and the sliding block (532) and the stop block (5312) form a driving cavity (5314); the tension spring (535) is sleeved on the guide rod (5313), one end of the tension spring (535) is fixedly connected with the stop block (5312), the other end of the tension spring (535) is fixedly connected with the sliding block (532), and the tension spring (535) forces the sliding block (532) to move towards the direction close to the stop block (5312); the rotating shaft (534) is rotatably connected to the lower end of the defoaming screen mesh (54), the lower side of the rotating shaft (534) is fixedly connected with the gear (533), and the upper side of the rotating shaft (534) is fixedly connected with the defoaming screen plate (52); the gear (533) is meshed with the rack section on the sliding block (532); the hydraulic pressure in the driving cavity (5314) is used for driving the sliding block (532) to drive the defoaming sieve plate (52) to rotate; the tension spring (535) is used for resetting the sliding block (532).
3. The NMP recovery finishing reactor as recited in claim 1, wherein said column bottom (2) is provided with an outlet pipe (21), a reboiled connecting pipe (22) and a reboiled steam inlet (23); the tower kettle (2) is connected with the first filling section (3) through a conical section; the first packing section (3) and the second packing section (4) are both internally provided with packing (31), the lower end of each packing (31) is provided with a packing support member (32), and the upper end of each packing (31) is provided with a packing pressing member (33); a feeding pipe (34) is arranged between the first filling section (3) and the second filling section (4).
4. A purification reactor for NMP recovery according to claim 3, wherein a liquid distribution means (341) for reducing an amplification effect due to a liquid maldistribution is provided below the return pipe (531) and the feed pipe (34).
5. The NMP-recovering refining reactor according to claim 1, wherein said first packing section (3) is provided at a lower end thereof with a liquid redistribution means (35) for preventing wall flow, said liquid redistribution means (35) having a truncated cone shape, and an outer peripheral wall thereof is provided with a plurality of guide grooves (351).
6. The NMP recovery refining reactor according to claim 1, wherein the bottom (2) and the top (5) are provided with a hydraulic pressure measuring port (61) and a temperature measuring port (62).
7. The reactor for NMP recovery and purification as defined in claim 2, wherein a packing is provided between said sliding block (532) and said return pipe (531).
8. The reactor for NMP recovery and purification according to claim 2, wherein a seal ring is provided between said slide block (532) and said guide rod (5313).
9. The refining reactor for NMP recovery as defined in claim 2, wherein said return pipe (531) has a return outlet (5316) on a side wall thereof for discharging liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110971125.9A CN113521782A (en) | 2021-08-24 | 2021-08-24 | Be used for NMP to retrieve refined reactor |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110971125.9A CN113521782A (en) | 2021-08-24 | 2021-08-24 | Be used for NMP to retrieve refined reactor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113521782A true CN113521782A (en) | 2021-10-22 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110971125.9A Pending CN113521782A (en) | 2021-08-24 | 2021-08-24 | Be used for NMP to retrieve refined reactor |
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| CN (1) | CN113521782A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116570953A (en) * | 2023-05-29 | 2023-08-11 | 湖北圣灵科技有限公司 | Reaction system for continuously producing glutaraldehyde by pyran method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN208525859U (en) * | 2018-04-27 | 2019-02-22 | 巨野润佳化工有限公司 | A kind of high efficiency packing rectifying column being convenient for changing |
| CN111167146A (en) * | 2019-12-26 | 2020-05-19 | 重庆市中润化学有限公司 | NMP waste liquid is retrieved with dehydration tower |
| CN211411047U (en) * | 2019-12-24 | 2020-09-04 | 无锡嘉宪石化装备有限公司 | Rectifying tower for pretreatment of alcohol-containing wastewater |
| CN212119294U (en) * | 2020-04-07 | 2020-12-11 | 上海环境工程技术有限公司 | Gaseous foam device that removes of landfill |
| CN212575657U (en) * | 2020-06-03 | 2021-02-23 | 广州市华栋香精香料有限公司 | Rectifying tower device for efficient backflow distribution of essence and spice |
| CN212757928U (en) * | 2020-06-03 | 2021-03-23 | 韶关市曲江天瑞德化工有限公司 | High tower NMP waste gas recovery device |
-
2021
- 2021-08-24 CN CN202110971125.9A patent/CN113521782A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN208525859U (en) * | 2018-04-27 | 2019-02-22 | 巨野润佳化工有限公司 | A kind of high efficiency packing rectifying column being convenient for changing |
| CN211411047U (en) * | 2019-12-24 | 2020-09-04 | 无锡嘉宪石化装备有限公司 | Rectifying tower for pretreatment of alcohol-containing wastewater |
| CN111167146A (en) * | 2019-12-26 | 2020-05-19 | 重庆市中润化学有限公司 | NMP waste liquid is retrieved with dehydration tower |
| CN212119294U (en) * | 2020-04-07 | 2020-12-11 | 上海环境工程技术有限公司 | Gaseous foam device that removes of landfill |
| CN212575657U (en) * | 2020-06-03 | 2021-02-23 | 广州市华栋香精香料有限公司 | Rectifying tower device for efficient backflow distribution of essence and spice |
| CN212757928U (en) * | 2020-06-03 | 2021-03-23 | 韶关市曲江天瑞德化工有限公司 | High tower NMP waste gas recovery device |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116570953A (en) * | 2023-05-29 | 2023-08-11 | 湖北圣灵科技有限公司 | Reaction system for continuously producing glutaraldehyde by pyran method |
| CN116570953B (en) * | 2023-05-29 | 2023-12-12 | 湖北圣灵科技有限公司 | Reaction system for continuously producing glutaraldehyde by pyran method |
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Address after: 238200 5th floor, complex building, hi tech Industrial Park (West Zone), he County Economic Development Zone, Ma'anshan City, Anhui Province Applicant after: Anhui Shengjie New Energy Technology Co.,Ltd. Address before: 238200 5th floor, complex building, hi tech Industrial Park (West Zone), he County Economic Development Zone, Ma'anshan City, Anhui Province Applicant before: Anhui Shengjie New Energy Technology Co.,Ltd. |
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Application publication date: 20211022 |