CN105126374B - A kind of tert-butyl alcohol water ring hexanone oxime differential pressure distillation system - Google Patents
A kind of tert-butyl alcohol water ring hexanone oxime differential pressure distillation system Download PDFInfo
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- CN105126374B CN105126374B CN201510372543.0A CN201510372543A CN105126374B CN 105126374 B CN105126374 B CN 105126374B CN 201510372543 A CN201510372543 A CN 201510372543A CN 105126374 B CN105126374 B CN 105126374B
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Abstract
The invention discloses a kind of tert-butyl alcohol water ring hexanone oxime differential pressure distillation system, the system includes high and low differential pressure rectifying column and corresponding tower reactor reboiler, feed preheater, pump, condenser, compressibility and return-flow system；In the system of the operation present invention by the operating pressure of setting high and low pressure tower, the overhead vapours of high-pressure tower is used for preheat the charging of lower pressure column, to make full use of the latent heat of phase change of high-pressure tower overhead vapours.The operating pressure of control high-pressure tower, controls bottom temperature；Control lower pressure column operating pressure, the wherein bubble point temperature of high-pressure tower overhead vapours are higher than 0～50 DEG C of lower pressure column feeding temperature.After the condensed device condensation of each column overhead steam, a part is used for each rectifier column reflux, and remaining sends into tower bottoms tank field, sends distillation system after the compressed system compresses of fixed gas of system.The consumed quantity of steam of differential pressure distillation system of the present invention for single tower distillation 40～55%.
Description
Technical field
The invention belongs to chemical products technical field of purification, more particularly to a kind of tertiary butanol and water-cyclohexanone oxime differential pressure essence
Evaporate system.
Background technology
In interior acyl ammonia device, be the mass transfer effect for accelerating Ammoximation reaction, the tert-butyl alcohol is introduced in the reaction as hexamethylene
The solvent of ketoxime, makes reactant and product reach uniform mixing in the reactor.Reactant liquor is first by filtering and will be catalyzed
The insoluble matters such as agent are separated with the tert-butyl alcohol, water, cyclohexanone oxime, as the tert-butyl alcohol is used as the organic solvent of cyclohexanone oxime, are not involved in anti-
Should, and follow-up rearrangement is had a negative impact, it is the utilization rate of the yield and the tert-butyl alcohol that improve caprolactam, which need to be carried out back
Receive and utilize.
As the boiling point and relative volatility of tertiary butanol and water-cyclohexanone oxime system differ larger, traditional rectifying can be adopted
Technology is separated, and single tower distillation technique industrial at present has that steam consumption is larger.Patent CN202724720U
There is provided a kind of triple-effect evaporation plant reclaimed for the tert-butyl alcohol, which passes through mechanical compress intensification 1st effective evaporator and two effect evaporations
The steam of device realizes the cascade utilization of energy respectively as 2nd effect evaporator and the thermal source of triple effect evaporator, and the device can lead to
The recovery that triple effect evaporation completes the tert-butyl alcohol is crossed, but due to being heated up with mechanical compress, needs to consume substantial amounts of high-quality energy.Specially
Sharp CN103214346 provides a kind of multi-effect rectifying process reclaimed for the tert-butyl alcohol, and which utilizes classical double-effect rectification by one
Effect rectifying tower top steam is used for two effect rectifying tower reactor reboilers, but as the restriction of cyclohexanone oxime thermal sensitivity causes an effect rectifying column
Overhead vapours and two effect tower bottom of rectifying tower liquid temps are mismatched, it is difficult to for actual production.
The content of the invention
It is an object of the invention to overcome single tower distillation high energy consumption and the unmatched problem of classical double-effect rectification energy, reduce
Steam and the consumption of cooling water, make full use of energy, reduce the operating cost of system, be particularly well-suited to process a large amount of material bodies
A kind of tertiary butanol and water-cyclohexanone oxime differential pressure the distillation system of system.
Technical scheme is summarized as follows：
A kind of tertiary butanol and water-cyclohexanone oxime differential pressure distillation system, including high-pressure tower 2 and lower pressure column 4, raw material A point two-way,
Lead up to after pipeline is connected with the first preheater 1 and be connected with the high-pressure tower charging aperture 15 of high-pressure tower 2；Separately lead up to pipeline with
Lower pressure column feedstock flash device 10 is connected with the bottom of the second preheater 3 after connecting again；The top of the second preheater 3 by pipeline with
The lower pressure column charging aperture 16 of lower pressure column 4 connects；The top of high-pressure tower 2 is connected with the second preheater 3, condenser 6 successively by pipeline
It is connected with return-flow system 13 after connecing, two-way is divided by pipeline in the bottom of high-pressure tower 2, after being connected with the first tower reactor reboiler 5 all the way
It is connected with high pressure tower bottom again, another road is connected with the bottom of the first preheater 1 after being connected with the first pump 11 again, the first preheater
1 top connection high pressure tower bottoms tank field B；Two-way is divided by pipeline in the bottom of lower pressure column 4, all the way with the second tower reactor reboiler 7
It is connected with low pressure tower bottom after connection again, another road is connected with low pressure tower bottoms tank field C after being connected with the second pump 12, lower pressure column 4
Top after pipeline is connected with primary cooler 8 and deep freezer 9 successively point two-way, be vented after leading up to compressibility 14；Separately
Point two-way after pipeline is connected with return-flow system 13 is led up to, pipeline is led up to and is connected to tower top tert-butyl alcohol tank field D, Ling Yilu
It is connected with the top of high-pressure tower and the top of lower pressure column by pipeline respectively.
First preheater, 1 preferred Siphon heat-exchange device, falling-film heat exchanger or autoclave heat exchanger, preferably heat siphon type
Heat exchanger.
Lower pressure column feedstock flash device 10 is preferably choke valve or flash tank.
Second preheater 3 is Siphon heat-exchange device, falling-film heat exchanger or autoclave heat exchanger, and preferably heat siphon type is changed
Hot device.
First tower reactor reboiler, 5 preferred thermosyphon reboiler, kettle type reboiler, falling-film reboiler once pass through formula
Reboiler, preferably once passes through formula reboiler.
Second tower reactor reboiler 7 is thermosyphon reboiler, kettle type reboiler, falling-film reboiler or once passes through formula again
Boiling device, preferably once passes through formula reboiler.
Return-flow system includes return tank, reflux pump and flow control system.
Compressibility is combined by one or more of liquid-ring vacuum pump, ejector vacuum pump and Roots vaccum pump.
Advantages of the present invention：A kind of tertiary butanol and water-cyclohexanone oxime differential pressure the distillation system of the present invention, by high pressure column overhead
The charging of steam and lower pressure column is exchanged heat, and is overcome and is caused the high-pressure tower tower pressure can not as high-pressure tower kettle material thermal sensitivity is limited
Too high caused classical double-effect rectification column overhead steam is difficult matching problem with tower bottoms potential temperature, realizes the abundant profit of energy
With the system can saving energy consumption 40～55% compared with single tower distillation.
Description of the drawings
Fig. 1 is a kind of tertiary butanol and water-cyclohexanone oxime differential pressure distillation system schematic diagram.
In figure, 1：First preheater 2：High-pressure tower 3：Second preheater 4：Lower pressure column 5：First tower reactor reboiler 6：
Condenser 7：Second tower reactor reboiler 8：Primary cooler 9：Deep freezer 10：Lower pressure column feedstock flash device 11：First pump 12：The
Two pumps 13：Return-flow system 14：Compressibility 15：High-pressure tower charging aperture 16：Lower pressure column charging aperture；A：Raw material B：High-pressure tower
Kettle liquid tank field C：Low pressure tower bottoms tank field D：Tower top tert-butyl alcohol tank field
Specific embodiment
By specific embodiment, the invention will be further described below in conjunction with the accompanying drawings, but following examples are descriptive
, it is not determinate, it is impossible to which protection scope of the present invention is limited with this.
A kind of tertiary butanol and water-cyclohexanone oxime differential pressure distillation system, including high-pressure tower 2 and lower pressure column 4, raw material A point two-way,
Lead up to after pipeline is connected with the first preheater 1 and be connected with the high-pressure tower charging aperture 15 of high-pressure tower 2；Separately lead up to pipeline with
Lower pressure column feedstock flash device 10 is connected with the bottom of the second preheater 3 after connecting again；The top of the second preheater 3 by pipeline with
The lower pressure column charging aperture 16 of lower pressure column 4 connects；The top of high-pressure tower 2 is connected with the second preheater 3, condenser 6 successively by pipeline
It is connected with return-flow system 13 after connecing, two-way is divided by pipeline in the bottom of high-pressure tower 2, after being connected with the first tower reactor reboiler 5 all the way
It is connected with high pressure tower bottom again, another road is connected with the bottom of the first preheater 1 after being connected with the first pump 11 again, the first preheater
1 top connection high pressure tower bottoms tank field B；Two-way is divided by pipeline in the bottom of lower pressure column 4, all the way with the second tower reactor reboiler 7
It is connected with low pressure tower bottom after connection again, another road is connected with low pressure tower bottoms tank field C after being connected with the second pump 12, lower pressure column 4
Top after pipeline is connected with primary cooler 8 and deep freezer 9 successively point two-way, be vented after leading up to compressibility 14；Separately
Point two-way after pipeline is connected with return-flow system 13 is led up to, pipeline is led up to and is connected to tower top tert-butyl alcohol tank field D, Ling Yilu
It is connected with the top of high-pressure tower and the top of lower pressure column by pipeline respectively.
First preheater, 1 preferred Siphon heat-exchange device, falling-film heat exchanger or autoclave heat exchanger, preferably heat siphon type
Heat exchanger.
Lower pressure column feedstock flash device 10 is preferably choke valve or flash tank.
Second preheater 3 is Siphon heat-exchange device, falling-film heat exchanger or autoclave heat exchanger, and preferably heat siphon type is changed
Hot device.
First tower reactor reboiler, 5 preferred thermosyphon reboiler, kettle type reboiler, falling-film reboiler once pass through formula
Reboiler, preferably once passes through formula reboiler.
Second tower reactor reboiler 7 is thermosyphon reboiler, kettle type reboiler, falling-film reboiler or once passes through formula again
Boiling device, preferably once passes through formula reboiler.
Return-flow system includes return tank, reflux pump and flow control system.
Compressibility is combined by one or more of liquid-ring vacuum pump, ejector vacuum pump and Roots vaccum pump.
Embodiment 1
Described as a example by processing 100 tons of tertiary butanol and waters-cyclohexanone oxime material liquid per hour.
A kind of tertiary butanol and water-cyclohexanone oxime differential pressure distillation system, as shown in figure 1, from reaction tank field tertiary butanol and water-
Cyclohexanone oxime material liquid A pressure is 4MPaA, and temperature presses high-pressure tower for 85 DEG C：Lower pressure column split ratio is：1:1.25 are divided into two strands,
One sends into the high-pressure tower charging aperture 15 of high-pressure tower 2 after the preheating of the first preheater 1, and preheated rear temperature is 93 DEG C, high pressure
The operating pressure of tower is 0.17MPaA, and tower top temperature is 92 DEG C, and bottom temperature is 120 DEG C, the first tower reactor reboiler 5（Once lead to
Cross formula reboiler）Heated using low-pressure steam, the first pumps of high-pressure tower tower bottoms Jing 11 for reaching separation requirement deliver to the first preheating
Device 1（Siphon heat-exchange device）High pressure tower bottoms tank field B is delivered to after preheating material liquid, 2 tower top of high-pressure tower of separation requirement is reached
Steam drains into the second preheater 3（Siphon heat-exchange device）Condense to bubble point temperature with Jing condensers 6 after the charging heat exchange of lower pressure column 4
Return-flow system 13 is sent to after 70 DEG C；Another strand of material liquid Jing lower pressure column feedstock flash device 10（Choke valve）It is decompressed to 0.45MPaA
The lower pressure column charging aperture 16 that lower pressure column 4 is delivered to after the second preheater 3 is exchanged heat with high-pressure tower overhead vapours is delivered to afterwards, and lower pressure column 4 is grasped
It is 0.04MPaA to make pressure, and tower top temperature is 31 DEG C, and bottom temperature is 84 DEG C, the second tower reactor reboiler 7（Once boiled by formula again
Device）Heated by low-pressure steam, the lower pressure column tower bottoms for reaching separation requirement delivers to low pressure tower bottoms tank Jing after the pressurization of the second pump 12
Area C, the top vapour phase Jing primary cooler 8 of lower pressure column 4 are condensed to 42 DEG C, then Jing deep freezers 9 are condensed to 31 DEG C of bubble point temperature, therein
The not compressed system of condensing 14（Liquid-ring vacuum pump）It is vented after pressurization（Deliver to torch burning）；Remaining divides after delivering to return-flow system 13
Two strands, one delivers to tower top tert-butyl alcohol tank field D, and another stock delivers to the top of high-pressure tower and the top of lower pressure column respectively by pipeline
Portion.
Tertiary butanol and water-cyclohexanone oxime material liquid A from reaction tank field is in high-pressure tower：The scope of lower pressure column split ratio can
With 1:Select between 0.5～2.
Return-flow system includes the corollary equipments such as return tank, reflux pump and flow control system.
Condenser 6 and primary cooler 8 provide colds by recirculated cooling water or other low-temperature receivers, deep freezer 9 by chilled brine or its
Its low-temperature receiver provides cold, sends distillation system after the compressed system compresses of the fixed gas after cooling.
High-pressure tower 2 can also be respectively provided with respective return-flow system with lower pressure column 4, and column overhead condensate liquid Jing is each for high and low pressure
From reflux pump, a part is back in respective tower by a certain percentage, and remaining delivers to tower top tert-butyl alcohol tank field D.
Operating pressure of the present invention by setting high and low pressure tower, by the tower top tert-butyl alcohol steam of high-pressure tower and lower pressure column
Charging is exchanged heat, and is existed with the operating pressure control for making full use of the latent heat of phase change of high-pressure tower overhead vapours, wherein high-pressure tower
0.08～0.50MPaA (absolute pressure), not higher than 120 DEG C of control bottom temperature, the control of lower pressure column operating pressure 0.001～
0.08MPaA, the wherein bubble point temperature of high-pressure tower overhead vapours are higher than 0～50 DEG C of lower pressure column feeding temperature；Each column overhead steam Jing
After condenser condensation, a part is used for each rectifier column reflux, and remaining sends into tower top tert-butyl alcohol tank field, the fixed gas Jing pressures of the system
Distillation system is sent after compression system compression.
Experiment is proved：The present invention can saving energy consumption 40～55% compared with single tower distillation.
Experiment is proved：The first preheater 1 in the present embodiment can also select falling-film heat exchanger or autoclave heat exchanger.
Lower pressure column feedstock flash device 10 can also select flash tank.
Second preheater 3 can also select falling-film heat exchanger or autoclave heat exchanger.
First tower reactor reboiler 5 can also select thermosyphon reboiler, kettle type reboiler or falling-film reboiler.
Second tower reactor reboiler 7 can also select thermosyphon reboiler, kettle type reboiler or falling-film reboiler.
Compressibility can also select the combination of ejector vacuum pump and Roots vaccum pump.
Claims (10)
1. a kind of tertiary butanol and water-cyclohexanone oxime differential pressure distillation system, including high-pressure tower (2) and lower pressure column (4), it is characterised in that
Raw material (A) point two-way, leads up to the high-pressure tower charging aperture (15) with high-pressure tower (2) after pipeline is connected with the first preheater (1)
Connection；Separately lead up to after pipeline is connected with lower pressure column feedstock flash device (10) and be connected with the bottom of the second preheater (3) again；The
The top of two preheaters (3) is connected with the lower pressure column charging aperture (16) of lower pressure column (4) by pipeline；The top of high-pressure tower (2) leads to
Piping is connected with return-flow system (13) after being connected with the second preheater (3), condenser (6) successively, and the bottom of high-pressure tower (2) leads to
Piping point two-way, is connected with high pressure tower bottom after be connected with the first tower reactor reboiler (5) all the way again, another road and the first pump
(11) it is connected with the bottom of the first preheater (1) after connecting again, the top connection high pressure tower bottoms tank field of the first preheater (1)
(B)；The bottom of lower pressure column (4) by pipeline point two-way, after being connected with the second tower reactor reboiler (7) all the way again with low pressure tower bottom
Connection, another road are connected with low pressure tower bottoms tank field (C) after being connected with the second pump (12), and the top of lower pressure column (4) passes through pipeline
After being connected with primary cooler (8) and deep freezer (9) successively, point two-way, leads up to compressibility (14) and is vented afterwards；Separately lead up to
Pipeline divides two-way after being connected with return-flow system (13), leads up to pipeline and is connected to tower top tert-butyl alcohol tank field (D), separately leads up to
Pipeline is connected with the top of high-pressure tower and the top of lower pressure column respectively.
2. a kind of tertiary butanol and water according to claim 1-cyclohexanone oxime differential pressure distillation system, is characterized in that described first
Preheater (1) is Siphon heat-exchange device, falling-film heat exchanger or autoclave heat exchanger.
3. a kind of tertiary butanol and water according to claim 1-cyclohexanone oxime differential pressure distillation system, is characterized in that the low pressure
Tower feedstock flash device (10) is choke valve or flash tank.
4. a kind of tertiary butanol and water according to claim 1-cyclohexanone oxime differential pressure distillation system, is characterized in that described second
Preheater (3) is Siphon heat-exchange device, falling-film heat exchanger or autoclave heat exchanger.
5. a kind of tertiary butanol and water according to claim 1-cyclohexanone oxime differential pressure distillation system, is characterized in that described first
Tower reactor reboiler (5) is thermosyphon reboiler, kettle type reboiler, falling-film reboiler or once passes through formula reboiler.
6. a kind of tertiary butanol and water according to claim 5-cyclohexanone oxime differential pressure distillation system, is characterized in that described first
Tower reactor reboiler (5) is once to pass through formula reboiler.
7. a kind of tertiary butanol and water according to claim 1-cyclohexanone oxime differential pressure distillation system, is characterized in that described second
Tower reactor reboiler (7) is thermosyphon reboiler, kettle type reboiler, falling-film reboiler or once passes through formula reboiler.
8. a kind of tertiary butanol and water according to claim 7-cyclohexanone oxime differential pressure distillation system, is characterized in that described second
Tower reactor reboiler (7) is once to pass through formula reboiler.
9. a kind of tertiary butanol and water according to claim 1-cyclohexanone oxime differential pressure distillation system, is characterized in that the backflow
System includes return tank, reflux pump and flow control system.
10. a kind of tertiary butanol and water according to claim 1-cyclohexanone oxime differential pressure distillation system, is characterized in that the compression
System is constituted by one or more of liquid-ring vacuum pump, ejector vacuum pump and Roots vaccum pump.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510372543.0A CN105126374B (en) | 2015-06-29 | 2015-06-29 | A kind of tert-butyl alcohol water ring hexanone oxime differential pressure distillation system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510372543.0A CN105126374B (en) | 2015-06-29 | 2015-06-29 | A kind of tert-butyl alcohol water ring hexanone oxime differential pressure distillation system |
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| CN105126374A CN105126374A (en) | 2015-12-09 |
| CN105126374B true CN105126374B (en) | 2017-03-29 |
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Families Citing this family (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107434783A (en) * | 2016-05-25 | 2017-12-05 | 天津大学 | A kind of power-economizing method and device of caprolactam system |
| CN107213665B (en) * | 2017-07-14 | 2022-06-14 | 王举才 | Concurrent fractionating device |
| CN107875664B (en) * | 2017-12-21 | 2023-09-26 | 新疆工程学院 | Propylene-propane thermal coupling rectifying energy-saving device |
| CN110218147B (en) * | 2019-06-28 | 2022-07-08 | 天津大学 | Method for recovering tert-butyl alcohol by utilizing cyclohexanone ammoximation reaction heat |
| CN110423206B (en) * | 2019-07-17 | 2022-07-08 | 天津大学 | Method for separating cyclohexanone oxime, cyclohexanone and toluene from ammoximation reaction product |
| CN112159335A (en) * | 2020-10-29 | 2021-01-01 | 江苏凌瑞化工科技有限公司 | Refining process flow of cyclohexanone oxime |
| CN114681942B (en) * | 2020-12-28 | 2023-07-07 | 天津市华瑞奕博化工科技有限公司 | Complete pressure swing coupling rectification device and rectification method for tertiary butanol recovery |
| CN113121313A (en) * | 2021-05-17 | 2021-07-16 | 吴嘉 | Energy-saving recovery device and method for tertiary butanol serving as ammoximation reaction solvent |
| CN113121314B (en) * | 2021-05-17 | 2023-11-24 | 吴嘉 | Device and method for recycling tertiary butanol by combining dividing wall rectifying tower with heat pump technology |
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| JP4814839B2 (en) * | 2007-05-17 | 2011-11-16 | 株式会社熊谷組 | Pile cap |
| CN102701960A (en) * | 2012-05-22 | 2012-10-03 | 天津大学 | Method and device for refining crude products of m-phthaloyl chloride |
| CN202724720U (en) * | 2012-09-11 | 2013-02-13 | 福建锦江石化有限公司 | Device for recycling tert-butyl alcohol |
| CN103214346A (en) * | 2013-04-12 | 2013-07-24 | 湖南百利工程科技股份有限公司 | Recovering process of solvent tertiary butanol in production process of ammoximation |
| CN203609905U (en) * | 2013-12-17 | 2014-05-28 | 山东庆云长信化学科技有限公司 | Rectificationdevice for furfurylalcohol |
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