CN210085331U - Cyclohexanone oxime purification system in caprolactam production process - Google Patents
Cyclohexanone oxime purification system in caprolactam production process Download PDFInfo
- Publication number
- CN210085331U CN210085331U CN201920800622.0U CN201920800622U CN210085331U CN 210085331 U CN210085331 U CN 210085331U CN 201920800622 U CN201920800622 U CN 201920800622U CN 210085331 U CN210085331 U CN 210085331U
- Authority
- CN
- China
- Prior art keywords
- toluene
- tower
- cyclohexanone oxime
- oxime
- deoximation
- Prior art date
- 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.)
- Active
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model discloses a cyclohexanone oxime purification system in caprolactam production process adopts toluene rectifying column, cyclohexanone oxime tower and toluene to take off oxime tower and constitutes cyclohexanone oxime purification system, and wherein toluene rectifying column operating pressure is 15-20KPa.A, and cyclohexanone oxime tower and toluene take off oxime tower operating pressure and are 6-10kPa.A, and vacuum system all adopts dry vacuum pump. The device adopts the gas phase at the top of the cyclohexanone oxime tower to directly feed into the toluene deoximation tower, cancels the gas phase condensation cooling equipment and the vacuum system at the top of the cyclohexanone oxime tower, saves the equipment investment, reduces the cooling capacity of circulating water, and reduces the steam consumption of the toluene deoximation tower; the vacuum system adopts a dry vacuum pump, reduces the steam consumption and reduces the sewage treatment capacity.
Description
Technical Field
The invention belongs to the technical field of caprolactam production, and particularly relates to a purification, energy optimization and wastewater emission reduction treatment system for cyclohexanone oxime.
Background
Caprolactam is an important chemical raw material, cyclohexanone oxime is an intermediate in the production process of caprolactam, and a cyclohexanone ammoximation device is the most core device in the production of caprolactam. The device takes cyclohexanone, liquid ammonia and hydrogen peroxide as raw materials and tert-butyl alcohol as a solvent, and cyclohexanone oxime is generated by reaction under the action of a silicon-titanium molecular sieve to obtain a cyclohexanone oxime tert-butyl alcohol aqueous solution; rectifying to recover tert-butyl alcohol from the reaction liquid to obtain oxime water solution; adding toluene, extracting cyclohexanone oxime in the oxime water solution, and washing with water to obtain a toluene cyclohexanone oxime solution; the toluene cyclohexanone oxime solution is rectified and purified through a rectification process, and the intermediate product cyclohexanone oxime is obtained.
The rectification process mainly comprises the steps of separating toluene and purifying cyclohexanone-oxime, and the vacuum rectification is adopted in the prior art, and a steam jet pump is utilized to provide vacuum degree. In the prior art, the toluene cyclohexanone oxime solution is purified and separated by 4 towers, each tower is provided with a separate condensation recovery system and a vacuum system, and the repeated condensation recovery systems not only increase the consumption of steam and cooling water, but also increase the equipment investment cost in the system; the steam jet pump is adopted, and the steam adding system is adopted, so that the steam consumption is high, and the amount of generated sewage is large. The process flow has high steam consumption, high equipment investment cost and high material consumption, so that the research on a cyclohexanone oxime purification system, the development of a new separation process, the reduction of steam consumption, circulating water consumption, equipment investment cost, wastewater discharge and the like have great significance.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a cyclohexanone oxime purification system in caprolactam production process effectively reduces the consumption of energy and the emission of waste water.
The technical scheme of the utility model:
a cyclohexanone oxime purification system in the production process of caprolactam mainly comprises a toluene rectifying tower, a cyclohexanone oxime tower and a toluene deoximation tower.
The method comprises the following steps that a toluene cyclohexanone oxime solution pipeline is connected to a toluene rectifying tower, the toluene rectifying tower is connected with a feeding pump of a cyclohexanone oxime tower, the feeding pump of the cyclohexanone oxime tower is connected with the cyclohexanone oxime tower, the cyclohexanone oxime tower is connected with a discharging pump of cyclohexanone oxime, and the discharging pump of cyclohexanone oxime sends purified cyclohexanone oxime out of a system;
the toluene rectifying tower gas phase pipeline is connected with a toluene condenser, the toluene condenser is connected with a toluene rectifying tower vacuum system, the toluene condenser is connected with a reflux pipeline of the toluene rectifying tower, and an outlet pipeline of the toluene condenser is also connected with a toluene recycling pipeline of the device;
the gas phase pipeline at the top of the cyclohexanone oxime tower is connected with a toluene deoximation tower, the discharge pipeline at the bottom of the toluene deoximation tower is connected with the bottom of a toluene rectifying tower, the gas phase pipeline at the top of the toluene deoximation tower is connected with a tolune condenser, and the tolune condenser is connected with a toluene deoximation tower vacuum system; the toluketone condenser is connected with a reflux line of the toluene deoximation tower, and the toluketone condenser is also connected with a toluketone refining treatment device.
The vacuum system of the toluene rectifying tower and the vacuum system of the toluene deoximation tower adopt a dry vacuum system.
In the invention, the gas phases of the toluene rectifying tower vacuum system and the toluene deoximation tower vacuum system are collected and then are treated in a centralized way.
The application of the cyclohexanone oxime purification system in the caprolactam production process is as follows:
delivering a toluene cyclohexanone-oxime solution in a caprolactam production process into a toluene rectifying tower through a pipeline, connecting the toluene rectifying tower with a cyclohexanone-oxime tower feeding pump, connecting the cyclohexanone-oxime tower feeding pump with the cyclohexanone-oxime tower, connecting the cyclohexanone-oxime tower with a cyclohexanone-oxime discharging pump, delivering purified cyclohexanone-oxime out of a system by the cyclohexanone-oxime discharging pump, connecting a toluene rectifying tower gas phase with a toluene condenser, connecting the toluene condenser with a toluene rectifying tower vacuum system, connecting a top gas phase of the cyclohexanone-oxime tower with a toluene deoximation tower, connecting a bottom gas phase of the toluene deoximation tower with a bottom of the toluene rectifying tower, connecting a top gas phase of the toluene deoximation tower with the toluene condenser, connecting the toluene condenser with the toluene deoximation tower vacuum system, collecting and then intensively treating gas phases of the toluene rectifying tower vacuum system and the toluene deoximation tower vacuum system, and taking a part of a liquid condensed in the toluene condenser as reflux of the toluene rectifying tower, and one part of the liquid condensed in the toluketone condenser is sent out for recycling, one part of the liquid is used as reflux of the toluene deoximation tower, and the other part of the liquid is sent out for continuous refining treatment.
The gas phase discharge of the cyclohexanone-oxime tower directly enters a toluene deoximation tower.
The operation pressure of the cyclohexanone-oxime tower and the toluene deoximation tower is 6-8MPa.
The invention has the positive effects that:
(1) the gas phase at the top of the cyclohexanone-oxime tower is not condensed, and the gas phase is directly fed into the toluene deoximation tower, so that the equipment investment of condensation recovery is effectively saved, the circulating water consumption of condensation recovery equipment is saved, and the steam consumption of the toluene deoximation tower is saved.
(2) The dry vacuum system is adopted, so that steam can be effectively prevented from entering a material system, the steam consumption is saved, and the waste water amount of the system is reduced technically.
Drawings
FIG. 1 shows a cyclohexanone oxime purification system in the process of producing caprolactam
1-toluene rectifying tower; a 2-cyclohexanone oxime column feed pump; a 3-cyclohexanone oxime column; 4-cyclohexanone oxime discharge pump; a 5-toluene deoximation tower; 6-toluene condenser; 7-toluene rectifying tower vacuum system; an 8-toluketone condenser; a vacuum system of a 9-toluene deoximation tower;
a-toluene cyclohexanone oxime solution; b-toluene; c, vacuum system tail gas; d-toluketone; e-cyclohexanone oxime; SML-low pressure steam.
Detailed Description
The invention will be further illustrated by the following examples, to which, however, the invention is not restricted.
Example 1:
a cyclohexanone oxime purification system is adopted in the production process of 10 ten thousand tons of caprolactam annually, and the process flow is shown in figure 1, and the feeding of toluene cyclohexanone oxime is 51 t/h.
Feeding a toluene cyclohexanone oxime solution in a caprolactam production process into a toluene rectifying tower 1 through a pipeline, wherein the operating pressure of the toluene rectifying tower 1 is 20kPa.G, vacuum is provided by a dry vacuum pump 7, toluene steam is arranged at the top of the toluene rectifying tower 1, a part of the toluene steam is used as reflux of the toluene rectifying tower 1 after being condensed by a toluene condenser 6, and a part of the toluene cyclohexanone oxime solution is used as a toluene circulating liquid and is circulated back to an ammoximation device; a tower kettle of the toluene rectifying tower 1 is a toluene oxime solution with the cyclohexanone oxime content of 30 percent, the toluene oxime solution is pumped into a cyclohexanone oxime tower 3 through a pump to be continuously rectified and purified to obtain the cyclohexanone oxime, the operation pressure of the cyclohexanone oxime tower 3 is 6kPa.A, and the tower kettle is the cyclohexanone oxime with the purity of 99.99 percent; the tower top is a toluene solution containing 9.4 percent of cyclohexanone-oxime and other organic impurities, the gas phase at the tower top is directly fed into a toluene deoximation tower 5 without being condensed, the operation pressure of the toluene deoximation tower 5 is 6kPa.A, the dry vacuum system 9 is shared with the cyclohexanone-oxime tower 3, part of the gas phase at the tower top of the toluene deoximation tower 5 is used as reflux of the toluene deoximation tower 5 after being condensed by a toluenone condenser 8, part of the gas phase is used as organic phase impurity recovery after being sent into an ammoximation device, cyclohexanone-oxime at the tower bottom of the toluene deoximation tower 5 is detected, the qualified gas phase is used as an intermediate product of cyclohexanone-oxime and sent into the next procedure by a cyclohexanone-oxime discharge pump 4, and the unqualified gas phase is sent into.
Compared with the prior process equipment, the utility model saves about 14000 tons of steam per year, about 240 ten thousand tons of circulating water per year and about 500 ten thousand yuan of investment cost.
Claims (3)
1. A cyclohexanone oxime purification system in the production process of caprolactam mainly comprises a toluene rectifying tower (1), a cyclohexanone oxime tower (3) and a toluene oxime removal tower (5); the method is characterized in that:
the method comprises the following steps that a toluene cyclohexanone oxime solution pipeline is connected into a toluene rectifying tower (1), the toluene rectifying tower (1) is connected with a cyclohexanone oxime tower feeding pump (2), the cyclohexanone oxime tower feeding pump (2) is connected with a cyclohexanone oxime tower (3), the cyclohexanone oxime tower (3) is connected with a cyclohexanone oxime discharging pump (4), and the purified cyclohexanone oxime is sent out of a system by the cyclohexanone oxime discharging pump (4);
a gas phase pipeline of the toluene rectifying tower (1) is connected with a toluene condenser (6), the toluene condenser (6) is connected with a toluene rectifying tower vacuum system (7), the toluene condenser (6) is connected with a reflux pipeline of the toluene rectifying tower (1), and an outlet pipeline of the toluene condenser (6) is also connected with a toluene recycling pipeline of the device;
a gas phase pipeline at the top of the cyclohexanone oxime tower (3) is connected with a toluene deoximation tower (5), a discharge pipeline at the bottom of the toluene deoximation tower (5) is connected with the bottom of a toluene rectifying tower (1), a gas phase pipeline at the top of the toluene deoximation tower (5) is connected with a tolune condenser (8), and the tolune condenser (8) is connected with a vacuum system (9) of the toluene deoximation tower; the toluidine condenser (8) is connected to the reflux line of the toluene deoximation column, and the toluidine condenser (8) is also connected to a toluidine purification treatment apparatus.
2. The cyclohexanone oxime purification system in the production process of caprolactam of claim 1, wherein the vacuum system of the toluene rectification column (7) and the vacuum system of the toluene deoximation column (9) are dry vacuum systems.
3. The cyclohexanone oxime purification system in the production process of caprolactam of claim 1, wherein the gas phase of the toluene rectification column vacuum system (7) and the toluene deoximation column vacuum system (9) is collected and then treated in a centralized manner.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920800622.0U CN210085331U (en) | 2019-05-30 | 2019-05-30 | Cyclohexanone oxime purification system in caprolactam production process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201920800622.0U CN210085331U (en) | 2019-05-30 | 2019-05-30 | Cyclohexanone oxime purification system in caprolactam production process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN210085331U true CN210085331U (en) | 2020-02-18 |
Family
ID=69480798
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201920800622.0U Active CN210085331U (en) | 2019-05-30 | 2019-05-30 | Cyclohexanone oxime purification system in caprolactam production process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN210085331U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111608910A (en) * | 2020-06-22 | 2020-09-01 | 聊城鲁西聚酰胺新材料科技有限公司 | Application and system of Roots liquid ring vacuum pump unit in ammoximation process production |
-
2019
- 2019-05-30 CN CN201920800622.0U patent/CN210085331U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111608910A (en) * | 2020-06-22 | 2020-09-01 | 聊城鲁西聚酰胺新材料科技有限公司 | Application and system of Roots liquid ring vacuum pump unit in ammoximation process production |
| CN111608910B (en) * | 2020-06-22 | 2023-02-21 | 聊城鲁西聚酰胺新材料科技有限公司 | Application and system of Roots liquid ring vacuum pump unit in ammoximation process production |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN210085330U (en) | Separation device for recovering dimethyl sulfoxide | |
| CN109081767B (en) | Synthetic rectification process method and equipment for methane chloride | |
| CN204079685U (en) | A kind for the treatment of unit of high salinity high-COD waste water | |
| CN214571634U (en) | System for retrieve polymerization level tetrahydrofuran in follow esterification waste water | |
| CN106698785A (en) | Coal gasification wastewater phenol and ammonia recovery process | |
| CN210085331U (en) | Cyclohexanone oxime purification system in caprolactam production process | |
| CN103274568B (en) | Method for treating ketone-containing wastewater in cyclohexanone ammoximation device by employing extraction method | |
| CN220572683U (en) | Hexamethylenediamine refining system capable of improving operation period | |
| CN102417265B (en) | Method for effectively removing organic matters in wastewater from nitrochlorobenzene production | |
| CN217511220U (en) | Device for separating and recovering extracted material of MIBK light component tower | |
| CN212102637U (en) | Ammonia and tert-butyl alcohol recovery device in cyclohexanone ammoximation production process | |
| CN205035294U (en) | Cyclohexanone an wosuan amino peptidases chemical industry skill mesocycle tert -butyl alcohol takes off miscellaneous device | |
| CN207877294U (en) | A kind of recycling system for preparing ortho-aminotoluene and generating waste water | |
| CN219423753U (en) | Rectifying device for recycling acetonitrile from low-treatment-capacity ammonia-containing wastewater | |
| CN106380403A (en) | A method for efficiently separating dimethyl oxalate from dimethyl carbonate | |
| CN112520931A (en) | Purification method and device for PTA (purified terephthalic acid) refining mother liquor | |
| CN218422766U (en) | Benzene hydrogenation circulating benzene washing and purifying system | |
| CN113788768B (en) | Refining system for preparing cyclohexanone oxime by ammoximation method | |
| CN202569603U (en) | Azeotropic distillation processing device used for recovering organic solvent from waste water | |
| CN214763389U (en) | Rectification energy-saving device in cyclohexanone oxime production process by cyclohexanone ammoximation method | |
| CN218579646U (en) | BDO hydrogenation unit tail gas recovery plant | |
| CN205461091U (en) | Modified underpressure distillation tower and acetonitrile system of refining | |
| CN217578369U (en) | High-efficient purification and dehydration device for coking wastewater solvent | |
| CN112723992B (en) | Process for preparing high-purity decanediol by side-line vacuum rectification | |
| CN211170278U (en) | Coal chemical wastewater extraction dephenolization resourceful treatment system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |