CN111659157B - Back-extraction rotary valve stirring device - Google Patents

Back-extraction rotary valve stirring device Download PDF

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Publication number
CN111659157B
CN111659157B CN202010643142.5A CN202010643142A CN111659157B CN 111659157 B CN111659157 B CN 111659157B CN 202010643142 A CN202010643142 A CN 202010643142A CN 111659157 B CN111659157 B CN 111659157B
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China
Prior art keywords
rotary valve
wall
stirrer
stripping
back extraction
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CN202010643142.5A
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Chinese (zh)
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CN111659157A (en
Inventor
谢明辉
邹晨
张伟鹏
林鹏辉
王洪群
杨超
吴亮
王炳信
虞淑瑶
周国忠
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Zhejiang Greatwall Mixers Co ltd
Institute of Process Engineering of CAS
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Zhejiang Greatwall Mixers Co ltd
Institute of Process Engineering of CAS
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Priority to CN202010643142.5A priority Critical patent/CN111659157B/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D11/04—Solvent extraction of solutions which are liquid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0066—Stirrers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0053—Details of the reactor
    • B01J19/0073—Sealings
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/18—Stationary reactors having moving elements inside
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D223/00—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom
    • C07D223/02—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings
    • C07D223/06—Heterocyclic compounds containing seven-membered rings having one nitrogen atom as the only ring hetero atom not condensed with other rings 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
    • C07D223/08—Oxygen atoms
    • C07D223/10—Oxygen atoms attached in position 2
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D11/00—Solvent extraction
    • B01D2011/002—Counter-current extraction
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/141—Feedstock

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention discloses a back extraction rotary valve stirring device, which comprises a lower driving mechanism (1) and an upper back extraction tower (5), wherein a rotary valve stirrer (4) is installed at the middle lower part of the back extraction tower (5), a lower end flange of the back extraction tower (5) is hermetically connected with an installation bottom cover (3), the rotary valve stirrer (4) is driven by a stirring shaft extending into the back extraction tower from the lower side by the driving mechanism (1), the intersection of the stirring shaft and the installation bottom cover (3) is provided with a sealing mechanism (2), two opposite lateral inlets (52) and two opposite lateral outlets (53) are symmetrically formed in the pipe wall of the back extraction tower (5) corresponding to the periphery of the rotary valve stirrer (4), an upper inlet (51) of the back extraction tower corresponds to the upper part of the rotary valve stirrer (4), and the back extraction tower can improve the product quality and reduce the production cost.

Description

Back-extraction rotary valve stirring device
Technical Field
The invention belongs to the technical field of stirring, and relates to a reverse extraction rotary valve stirring device which is suitable for reversely extracting caprolactam from a solution of cyclohexane into process condensate water and separating caprolactam from oil-soluble impurities.
Background
Caprolactam is an important organic chemical raw material and has very strict requirements on the quality of the caprolactam. The industrial production methods of caprolactam are various, the reaction route is long, the crude caprolactam solution obtained by the reaction contains more impurities, and a series of physical and chemical refining methods such as extraction, back extraction, ion exchange, hydrogenation, multi-effect evaporation, distillation and the like are required to obtain a caprolactam finished product. The extraction is particularly important in the whole caprolactam refining process, is a main guarantee means for the caprolactam quality, and is also a working procedure with larger energy consumption in the whole refining process, and the circulation of an extracting agent and the circulation and removal of a back extracting agent need a large amount of electricity and steam.
The existing impurity back-extraction process is to back extract caprolactam from benzene-hexane solution by using process water in a pulse back-extraction tower, but the product quality and the production cost of the caprolactam are not ideal, and a novel high-efficiency back-extraction device is urgently needed to be developed to improve the impurity extraction process so as to improve the market competitiveness of products.
Disclosure of Invention
In order to solve the technical problems, the invention provides a reverse extraction rotary valve stirring device, which improves the caprolactam product quality and reduces the production cost.
The invention solves the technical problems by adopting the technical means that the stripping rotary valve stirring device comprises a lower driving mechanism and an upper stripping tower, wherein a rotary valve stirrer is arranged at the middle lower part of the stripping tower, a flange at the lower end of the stripping tower is in sealing connection with a mounting bottom cover, the rotary valve stirrer is driven by a stirring shaft which extends into the stripping tower from the lower side by the driving mechanism, a sealing mechanism is arranged at the junction of the stirring shaft and the mounting bottom cover, four openings are symmetrically formed in the wall of the stripping tower pipe on the periphery corresponding to the rotary valve stirrer and comprise two opposite side inlets and two opposite side outlets, and an upper inlet of the stripping tower corresponds to the upper part of the rotary valve stirrer. When the system works, the dispersed phase of the solution of the benzene hexane enters from two opposite side inlets, the process condensate water is added from an upper inlet of the stripping tower, the two phases are in countercurrent contact, and the stripped phase of the aqueous solution of the caprolactam flows out from two opposite side outlets. Tests show that the rotary valve stirrer can obtain better product quality and lower production cost in the process, the rotary valve stirrer comprises a hub and an outer pipe wall, the middle of the hub is assembled with a driving shaft, the inner side of the upper end of the pipe wall is an annular flat plate, the hub is connected with the upper part of the pipe wall through an upper conical wall, the hub is connected with the lower part of the pipe wall through a lower conical wall, the wall surfaces of the upper conical wall and the lower conical wall are respectively provided with an opening, and the pipe wall is transversely provided with two opposite round holes. When the two round holes are overlapped with the two opposite lateral inlets, the phenylcyclohexane solution enters the rotary valve stirrer, and the rotary valve stirrer is subjected to the shearing action of the openings formed in the wall surfaces of the upper conical wall and the lower conical wall in the rotating process, so that liquid drops can be dispersed, the mass transfer is enhanced, smaller phenylcyclohexane liquid drops are obtained, and effective extraction is performed.
From the standpoint of efficiency and manufacturing cost, it is preferable that the lateral inlet and the lateral outlet are both circular.
In view of the effect, it is preferable that the upper conical wall surface is provided with a plurality of upper tooth profile holes, and the lower conical wall surface is provided with a plurality of lower tooth profile holes.
In terms of effect, the number of the lower tooth profile holes is 2 times of the number of the upper tooth profile holes, and the lower tooth profile holes and the upper tooth profile holes are preferably identical in direction and total area.
In view of effects, manufacturing and installation, the distance between the rotary valve stirrer and the back extraction tower is preferably 3-5 mm.
The back-extraction rotary valve stirring device has the advantages that the back-extraction rotary valve stirring device is structurally designed, and particularly the product quality is improved and the production cost is reduced obviously after the back-extraction rotary valve stirring device is matched with a rotary valve stirrer.
Drawings
FIG. 1 is a schematic view showing the structure of a stripping rotary valve stirring apparatus, in which only a portion of a stripping column adjacent to a rotary valve stirrer is shown;
FIG. 2 is a schematic diagram of the construction of a rotary valve agitator;
FIG. 3 schematically shows a top view of the rotary valve agitator with the middle section horizontally split and with the wall of the stripping tower on the outside split to show the two opposite side inlets and the two opposite side outlets;
FIG. 4 is a schematic representation of a top view of a horizontal split in the middle of a rotary valve agitator.
In the figure: 1. a drive mechanism; 2. a sealing mechanism; 3. mounting a bottom plate; 4. rotating the valve agitator; 41. an annular flat plate; 42. a tube wall; 43. an upper conical wall; 44. a hub; 45. a lower conical wall; 46. a circular hole; 47. an upper tooth profile hole; 48. a lower tooth profile bore; 5. a stripping tower; 51. an upper inlet; 52. a lateral inlet; 53. and a lateral outlet.
Detailed Description
An embodiment of the present invention will be described below with reference to the drawings.
Strip rotary valve agitating unit, including actuating mechanism 1 and the strip tower 5 on upper portion of lower part, rotary valve agitator 4 is installed to the lower part in the strip tower 5, 5 lower extreme flanges of strip tower and installation bottom 3 sealing connection, rotary valve agitator 4 is driven by the (mixing) shaft that actuating mechanism 1 stretched into from the downside, the (mixing) shaft is mechanical seal with the sealing mechanism 2 of installing the 3 intersection of bottom, it has four circular ports to correspond on the 5 pipe walls of outlying strip tower with rotary valve agitator 4, including two relative side direction entry 52 and two relative side direction export 53, what correspond in 4 tops of rotary valve agitator is strip tower's top entry 51. The rotary valve stirrer 4 comprises a hub 44 with the middle part assembled with the driving shaft and an outer pipe wall 42, the inner side of the upper end of the pipe wall 42 is welded with an annular flat plate 41, the hub 44 is connected with the upper part of the pipe wall 42 through an upper conical wall 43, and the hub 44 is connected with the lower part of the pipe wall 42 through a lower conical wall 45. Four upper tooth profile holes 47 are formed in the wall surface of the upper conical wall 43, eight lower tooth profile holes 48 are formed in the wall surface of the lower conical wall 45, the lower tooth profile holes 48 and the upper tooth profile holes 47 are in the same direction, the total area of the lower tooth profile holes is equal to that of the upper tooth profile holes 47, and two opposite round holes are also transversely formed in the tube wall 42. The distance between the rotary valve stirrer 4 and the stripping column 5 was 3 mm.

Claims (4)

1. A stripping rotary valve stirring device comprises a lower driving mechanism (1) and an upper stripping tower (5), and is characterized in that a rotary valve stirrer (4) is installed on the lower middle part of the stripping tower (5), a lower end flange of the stripping tower (5) is in sealing connection with an installation bottom cover (3), the rotary valve stirrer (4) is driven by a stirring shaft which is extended from the lower side of the driving mechanism (1), a sealing mechanism (2) is configured at the intersection of the stirring shaft and the installation bottom cover (3), four ports are symmetrically formed in the pipe wall of the stripping tower (5) corresponding to the periphery of the rotary valve stirrer (4), the four ports comprise two opposite lateral inlets (52) and two opposite lateral outlets (53), and an upper inlet (51) of the stripping tower corresponds to the upper part of the rotary valve stirrer (4);
the rotary valve stirrer (4) comprises a hub (44) and an external pipe wall (42), the middle part of the hub is assembled with the driving shaft, the inner side of the upper end of the pipe wall (42) is provided with an annular flat plate (41), the hub (44) is connected with the upper part of the pipe wall (42) through an upper conical wall (43), the hub (44) is connected with the lower part of the pipe wall (42) through a lower conical wall (45), the wall surfaces of the upper conical wall (43) and the lower conical wall (45) are respectively provided with an opening, and the pipe wall (42) is transversely provided with two opposite round holes (46);
the wall surface of the upper conical wall (43) is provided with a plurality of upper tooth profile holes (47), and the wall surface of the lower conical wall (45) is provided with a plurality of lower tooth profile holes (48).
2. A stripping rotary valve agitator apparatus as claimed in claim 1, characterised in that the lateral inlet (52) and the lateral outlet (53) are both circular.
3. Stripping rotary valve agitator apparatus according to claim 1, characterised in that the number of lower profile holes (48) is 2 times the number of upper profile holes (47), the lower profile holes (48) being co-directional with the upper profile holes (47) and having the same total area.
4. A stripping rotary valve agitator according to claim 1, wherein the distance between the rotary valve agitator (4) and the stripping tower (5) is 3-5 mm.
CN202010643142.5A 2020-06-30 2020-06-30 Back-extraction rotary valve stirring device Active CN111659157B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202010643142.5A CN111659157B (en) 2020-06-30 2020-06-30 Back-extraction rotary valve stirring device

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Application Number Priority Date Filing Date Title
CN202010643142.5A CN111659157B (en) 2020-06-30 2020-06-30 Back-extraction rotary valve stirring device

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CN111659157A CN111659157A (en) 2020-09-15
CN111659157B true CN111659157B (en) 2022-06-24

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1306628A (en) * 1970-09-29 1973-02-14 Stamicarbon Device for pulsating a liquid in a column
JP2001165342A (en) * 1999-12-07 2001-06-22 Sumitomo Metal Mining Co Ltd Air pulse generator
CN201179359Y (en) * 2008-02-04 2009-01-14 浙江大学 Pulsed extraction column based on magnetically-actuated rotary valve
CN103285620A (en) * 2013-05-16 2013-09-11 南京化工职业技术学院 Pulsed extraction tower pulse generating device

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1306628A (en) * 1970-09-29 1973-02-14 Stamicarbon Device for pulsating a liquid in a column
JP2001165342A (en) * 1999-12-07 2001-06-22 Sumitomo Metal Mining Co Ltd Air pulse generator
CN201179359Y (en) * 2008-02-04 2009-01-14 浙江大学 Pulsed extraction column based on magnetically-actuated rotary valve
CN103285620A (en) * 2013-05-16 2013-09-11 南京化工职业技术学院 Pulsed extraction tower pulse generating device

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