CN111229332A - Device for washing caprolactam to improve period of ion-exchange resin - Google Patents

Device for washing caprolactam to improve period of ion-exchange resin Download PDF

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Publication number
CN111229332A
CN111229332A CN202010093347.0A CN202010093347A CN111229332A CN 111229332 A CN111229332 A CN 111229332A CN 202010093347 A CN202010093347 A CN 202010093347A CN 111229332 A CN111229332 A CN 111229332A
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China
Prior art keywords
tower
washing
pipeline
pipe connection
pump
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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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CN202010093347.0A
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Chinese (zh)
Inventor
谢文理
瞿亚平
刘期敏
吴望成
张泽渐
刘志强
肖高荣
张方
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Fujian Eversun Technology Co ltd
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Fujian Eversun Technology Co ltd
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Priority to CN202010093347.0A priority Critical patent/CN111229332A/en
Publication of CN111229332A publication Critical patent/CN111229332A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J49/00Regeneration or reactivation of ion-exchangers; Apparatus therefor
    • B01J49/60Cleaning or rinsing ion-exchange beds

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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 device for washing caprolactam to improve the period of ion exchange resin, which comprises a hexane extraction tower connected with the ground through an expansion bolt, wherein the hexane extraction tower is connected with a buffer tank through a pipeline, the buffer tank is connected with an inlet of a benzene hexane buffer feed pump through a pipeline, an outlet of the benzene hexane buffer feed pump is connected with a benzene hexane buffer tank through a pipeline, the benzene hexane buffer tank is connected with an inlet of a washing tower feed pump through a pipeline, an outlet of the washing tower feed pump is connected with the lower part of the washing tower through a pipeline, the washing tower is connected with a mixer A through a pipeline, an electromagnetic valve is arranged on the pipeline, the device can reduce the conductivity of an ion exchange feed from 20-30us/cm3 to 1-5us/cm3, the service period of the ion exchange tower after the conductivity is reduced is more than 30 days and is 4-5 times of the current, the regeneration frequency is only 25% of the current, the acid-base dosage is only 25% of the original dosage, the production cost is greatly reduced, the ion exchange service cycle can be effectively prolonged, and the practicability is strong.

Description

Device for washing caprolactam to improve period of ion-exchange resin
Technical Field
The invention relates to the technical field of washing and impurity removing devices, in particular to a device for washing caprolactam to improve the period of ion-exchange resin.
Background
In the existing caprolactam refining device, the basic composition unit is extraction → benzene evaporation recovery → ion exchange tower → hydrogenation reactor → evaporation concentration → distillation refining, wherein the use period of the ion exchange resin in the ion exchange process is gradually shortened in the long-time use process, the main reason is that the ion exchange resin is easily saturated and needs to be frequently switched due to excessive impurities in the feed liquid, the ion exchange resin needs to be regenerated in each switching, 32% by weight of caustic soda is consumed for about 40t, 36% by weight of nitric acid is 45 tons in each regeneration, the generated wastewater is about 1000t, and the production cost is greatly increased.
A washing tower is not arranged in the traditional flow, the material liquid directly enters an ion exchange process through benzene stripping after passing through an extraction stripping tower, the ionizable inorganic and organic impurities in the material liquid are excessive, the conductivity of the material liquid entering the ion exchange is often more than or equal to 20us/cm3, the use period of the ion exchange is greatly shortened, the use period is only 3-5 days, and the ion exchange has to be frequently switched to ensure the quality of a caprolactam finished product.
The defect that the existing device exists is improved, and a device for washing caprolactam to improve the period of ion-exchange resin is provided.
Disclosure of Invention
The invention aims to provide a device for improving the cycle of an ion-exchange resin by washing caprolactam, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
the device for improving the period of the ion exchange resin by washing caprolactam comprises a hexane extraction tower connected with the ground through expansion bolts, wherein the hexane extraction tower is connected with a buffer tank through a pipeline, the buffer tank is connected with the inlet of a benzene hexane buffer feed pump through a pipeline, the outlet of the benzene hexane buffer feed pump is connected with the inlet of the benzene hexane buffer tank through a pipeline, the inlet of the benzene hexane buffer tank is connected with the inlet of a washing tower feed pump through a pipeline, the outlet of the washing tower feed pump is connected with the lower part of the washing tower through a pipeline, the washing tower is connected with a mixer A through a pipeline, an electromagnetic valve is arranged on the pipeline, the mixer A is connected with the inlet of a washing liquid circulating tower through a pipeline, the outlet of the washing tower circulating pump is respectively connected with the washing tower and a receiving tank through pipelines, the washing tower is connected with the outlet of the washing liquid through a pipeline, and the inlet of the, the washing liquid tank is connected with the mixer B through a pipeline, the receiving tank is connected with the inlet of a discharging pump of the receiving tank through a pipeline, and the outlet of the discharging pump of the receiving tank is connected with the back-extraction tower through a pipeline.
As a further scheme of the invention: the upper part of the mixer B is respectively connected with a caustic soda pipeline and a process condensate pipeline, and a caustic soda solution with the concentration of 1-2% is prepared.
As a further scheme of the invention: the caustic soda in the caustic soda pipeline is sodium hydroxide solution.
As a further scheme of the invention: the washing tower is provided with 10 tower plates from bottom to top, the caustic soda solution is sent to an outlet pipe of a circulating pump of the washing tower through a washing liquid pump and enters the 6 th to 10 th tower plates at the upper part of the washing tower for washing reaction, an electromagnetic valve between the discharging of the circulating pump of the washing tower and the alkali liquor inlet is closed, and the circulating pump of the washing tower is only used as a material pump.
As a further scheme of the invention: the temperature of benzene extraction in the extraction tower is 35-55 ℃, and the extraction tower is vertical equipment with a filler arranged inside.
As a further scheme of the invention: the multistage turntables are arranged in the extraction tower, and the benzene hexane liquid is divided into small unit liquid through rotation of the turntables.
As a further scheme of the invention: the back extraction temperature in the back extraction tower is 35-45 ℃.
Compared with the prior art, the invention has the beneficial effects that: the device can reduce the conductivity of the ion exchange feeding material from 20-30us/cm3 to 1-5us/cm3, the service cycle of the ion exchange tower is longer than 30 days after the conductivity is reduced, the service cycle is 4-5 times of the current service cycle, the regeneration frequency is only 25% of the current service cycle, the acid and alkali consumption is only 25% of the original service cycle, the production cost is greatly reduced, the service cycle of the ion exchange can be effectively prolonged, and the practicability is strong.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
FIG. 2 is a block diagram of the flow process of the present invention.
Fig. 3 is a partial structural schematic diagram of the present invention.
Wherein: the device comprises a hexane extraction tower 1, a buffer tank 2, a benzene hexane buffer feeding pump 3, a benzene hexane buffer tank 4, a washing tower feeding pump 5, a washing tower 6, a mixer A7, an electromagnetic valve 8, a washing tower circulating pump 9, a receiving tank 10, a washing liquid pump 11, a washing liquid tank 12, a mixer B13, a receiving tank discharging pump 14 and a back extraction tower 15.
Detailed Description
In the description of the present invention, it is to be understood that the terms "center", "longitudinal", "lateral", "up", "down", "front", "back", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like, indicate orientations or positional relationships based on those shown in the drawings, and are used only for convenience in describing the present invention and for simplicity in description, and do not indicate or imply that the referenced devices or elements must have a particular orientation, be constructed and operated in a particular orientation, and thus, are not to be construed as limiting the present invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art through specific situations.
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. 1-3, in the embodiment of the present invention, an apparatus for washing and increasing a period of an ion exchange resin with caprolactam includes a hexane extraction tower 1 connected to the ground through an expansion bolt, for extracting crude oil and benzene from the hexane extraction tower 1 to form a benzene hexane solution, the hexane extraction tower 1 is connected to a buffer tank 2 through a pipeline, the buffer tank 2 is used for temporarily storing the benzene hexane solution, the buffer tank 2 is connected to an inlet of a benzene hexane buffer feed pump 3 through a pipeline, an outlet of the benzene hexane buffer feed pump 3 is connected to a benzene hexane buffer tank 4 through a pipeline, the benzene hexane buffer feed pump 3 is used for conveying the benzene hexane solution to the inside of a benzene hexane buffer tank 4, the benzene hexane buffer tank 4 is used for statically layering the benzene hexane solution to separate a small portion of water carried in the benzene hexane solution, the benzene hexane buffer tank 4 is connected to an inlet of a wash tower feed pump 5 through a pipeline, an outlet of the wash tower feed pump 5 is connected to the lower portion of a wash tower 6 through a pipeline, the washing tower feeding pump 5 is used for sending a phenylcyclohexane liquid into the washing tower 6 for reaction, the washing tower 6 is connected with a mixer A7 through a pipeline, the pipeline is provided with an electromagnetic valve 8, the mixer A7 is connected with an inlet of a washing liquid circulating tower 9 through a pipeline, an outlet of the washing tower circulating pump 9 is respectively connected with the washing tower 6 and a receiving tank 10 through pipelines, the receiving tank 10 is used for collecting the phenylcyclohexane liquid, the washing tower 6 is connected with an outlet of a washing liquid pump 11 through a pipeline, an inlet of the washing liquid pump 11 is connected with a washing liquid tank 12 through a pipeline, the washing liquid pump 11 is used for sending the washing liquid into the washing tower 6, the washing liquid tank 12 is connected with a mixer B13 through a pipeline, the mixer B13 is used for configuring the concentration of caustic soda and process cold water, the receiving tank 10 is connected with an inlet of a receiving tank discharging pump 14 through a pipeline, an outlet of the receiving tank discharging pump 14 is connected with a stripping tower 15 through, the stripping column 15 is used for the extraction of benzene.
The upper part of the mixer B13 is respectively connected with a caustic soda pipeline and a process condensate pipeline, and a caustic soda solution with the concentration of 1-2% is prepared.
The caustic soda in the caustic soda pipeline is sodium hydroxide solution and is used for removing acidic organic and inorganic impurities dissolved in the phenylcaprolactam solution.
The washing tower 6 is provided with 10 tower plates from bottom to top, the caustic soda solution is sent into an outlet pipe of a circulating pump 9 of the washing tower through a washing liquid pump 11 and enters the 6 th to 10 th tower plates on the upper part of the washing tower for washing reaction, an electromagnetic valve 8 between the discharging of the circulating pump 9 of the washing tower and the alkali liquor entering is closed, the circulating pump 9 of the washing tower is only used as a material pump, thus the influence of the circulating liquid on a top interface can be reduced, the entering alkali liquor can go down from the upper part of the washing tower 6, and the phenylcyclohexane liquid added at the bottom can go up from the bottom of the washing tower 6 to be fully washed and reacted in the tower.
Example 2
The temperature of benzene extraction in the extraction tower 1 is 35-55 ℃, and the extraction tower 1 is vertical equipment with a filler arranged inside.
The multistage turntables are arranged in the extraction tower 1, and the benzene hexane liquid is divided into small unit liquid through the rotation of the turntables.
The back extraction temperature in the back extraction tower 15 is 35-45 ℃.
The working principle of the invention is as follows: when the device for washing and improving the period of the ion exchange resin by using the caprolactam works, materials are extracted from a hexane extraction tower 1 to form a benzene hexane solution, the benzene hexane solution enters a buffer tank 2 and is sent to a benzene hexane buffer tank 4 through a benzene hexane buffer feeding pump 3 for static layering, a small part of water carried in the benzene hexane solution is separated, the benzene hexane solution still contains more ionizable organic and inorganic impurities, the conductivity of the solution is not less than 20us/cm3, the service period of the ion exchange resin is about 3-5 days, the benzene hexane solution after layering in the benzene hexane buffer tank 4 is sent to a washing tower 6 through a washing tower feeding pump 5 for reaction, a caustic soda solution with the concentration of 1-2% is configured through a caustic soda pipeline at the upper part of a mixer B13 and a process condensate pipeline, the caustic soda solution is sent to an outlet of a washing tower circulating pump 9 through a washing liquid pump 11 and enters a tower plate at the 6 th-10 th part of the washing tower 6, the washing and reaction conditions in the tower can be observed through a tower plate sight glass of the washing tower 6, a circulating pump 9 of the washing tower is only used as a material pump, the influence of circulating liquid on the top reaction and the formation of an interface can be reduced, the entered alkali liquor can move downwards from the upper part of the washing tower 6, the benzene hexane liquid added at the bottom moves upwards from the bottom of the washing tower 6, full washing and reaction are carried out in the washing tower 6, the benzene hexane liquid after the reaction is entered into a receiving tank 10 and then is sent to a back extraction tower 15 through a receiving tank discharge pump 14, the conductivity of the solution is less than 5us/cm3 at the moment, and the service cycle of the ion exchange resin is more than 30 days.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (7)

1. The utility model provides a caprolactam washes promotes device of ion exchange resin cycle, includes and has extracted tower (1) through expansion bolts connection with ground, its characterized in that, it has extracted tower (1) and dashpot (2) through the pipe connection to have passed through, dashpot (2) and the import of the benzene buffer charge pump (3) have passed through the pipe connection, the export of the benzene buffer charge pump (3) has passed through the pipe connection with the benzene buffer tank (4) that has, the benzene buffer tank (4) has passed through the pipe connection with wash tower charge pump (5) import, wash tower charge pump (5) export and wash tower (6) below pass through the pipe connection, wash tower (6) and blender A (7) pass through the pipe connection, be provided with solenoid valve (8) on the pipeline, blender A (7) and wash liquid circulating tower (9) import pass through the pipe connection, wash tower circulating pump (9) export respectively with wash tower (6), Receive jar (10) and pass through the pipe connection, wash column (6) and washing liquid pump (11) export pass through the pipe connection, washing liquid pump (11) import and washing liquid tank (12) pass through the pipe connection, washing liquid tank (12) and blender B (13) pass through the pipe connection, receive jar (10) and receive jar discharge pump (14) import and pass through the pipe connection, receive jar discharge pump (14) export and back extraction tower (15) and pass through the pipe connection.
2. The device for washing and lifting the resin cycle of ion exchange by caprolactam according to claim 1, wherein the upper part of the mixer B (13) is respectively connected with a caustic soda pipeline and a process condensate pipeline and is provided with a caustic soda solution with the concentration of 1-2%.
3. The apparatus for washing and lifting cycle of ion-exchange resin with caprolactam of claim 2, wherein the caustic soda in the caustic soda line is sodium hydroxide solution.
4. The device for washing and lifting the resin cycle of ion exchange by caprolactam according to claim 2, characterized in that the washing tower (6) is provided with 10 trays from bottom to top, the caustic soda solution is sent to an outlet pipe of a circulating pump (9) of the washing tower through a washing liquid pump (11) and enters the 6 th to 10 th trays at the upper part of the washing tower for washing reaction, a solenoid valve (8) between the discharging of the circulating pump (9) of the washing tower and the alkali liquor feeding is closed, and the circulating pump (9) of the washing tower is only used as a material pump.
5. The device for washing and improving the period of the ion exchange resin by the caprolactam according to claim 1, characterized in that the temperature of benzene extraction in the hexane extraction tower (1) is 35-55 ℃, and the hexane extraction tower (1) is a vertical device with a filler arranged inside.
6. The device for washing caprolactam to improve the period of ion-exchange resin according to claim 1, characterized in that a multistage rotating disc is arranged in the hexane extraction tower (1), and the cyclohexane is divided into small unit liquid by the rotation of the rotating disc.
7. The apparatus for stripping off resin cycle with caprolactam washing according to claim 1, characterized in that the temperature of the back extraction in the stripping column (15) is 35-45 ℃.
CN202010093347.0A 2020-02-14 2020-02-14 Device for washing caprolactam to improve period of ion-exchange resin Pending CN111229332A (en)

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CN202010093347.0A CN111229332A (en) 2020-02-14 2020-02-14 Device for washing caprolactam to improve period of ion-exchange resin

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Application Number Priority Date Filing Date Title
CN202010093347.0A CN111229332A (en) 2020-02-14 2020-02-14 Device for washing caprolactam to improve period of ion-exchange resin

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015062189A1 (en) * 2013-11-01 2015-05-07 华东理工大学 Method and apparatus for recovering caprolactam in benzene distillation residue
CN105061311A (en) * 2015-08-13 2015-11-18 江苏三鼎石化科技有限公司 Caprolactam refining technology
CN107556240A (en) * 2016-08-24 2018-01-09 沧州旭阳化工有限公司 A kind of system of caprolactam refining method and refined caprolactam
CN109942492A (en) * 2019-04-11 2019-06-28 江苏凌瑞化工科技有限公司 A kind of caprolactam refining technique

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2015062189A1 (en) * 2013-11-01 2015-05-07 华东理工大学 Method and apparatus for recovering caprolactam in benzene distillation residue
CN105061311A (en) * 2015-08-13 2015-11-18 江苏三鼎石化科技有限公司 Caprolactam refining technology
CN107556240A (en) * 2016-08-24 2018-01-09 沧州旭阳化工有限公司 A kind of system of caprolactam refining method and refined caprolactam
CN109942492A (en) * 2019-04-11 2019-06-28 江苏凌瑞化工科技有限公司 A kind of caprolactam refining technique

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Application publication date: 20200605