CN107434784A - Non-energy-consumption reclaims the method and device of caprolactam organic extractant - Google Patents
Non-energy-consumption reclaims the method and device of caprolactam organic extractant Download PDFInfo
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- CN107434784A CN107434784A CN201610355732.1A CN201610355732A CN107434784A CN 107434784 A CN107434784 A CN 107434784A CN 201610355732 A CN201610355732 A CN 201610355732A CN 107434784 A CN107434784 A CN 107434784A
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- organic solvent
- high pressure
- pipeline
- rectifying column
- low pressure
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- JBKVHLHDHHXQEQ-UHFFFAOYSA-N epsilon-caprolactam Chemical compound O=C1CCCCCN1 JBKVHLHDHHXQEQ-UHFFFAOYSA-N 0.000 title claims abstract description 92
- 238000005265 energy consumption Methods 0.000 title claims abstract description 26
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000003960 organic solvent Substances 0.000 claims abstract description 311
- 239000002351 wastewater Substances 0.000 claims abstract description 155
- 239000002904 solvent Substances 0.000 claims abstract description 101
- 238000005191 phase separation Methods 0.000 claims abstract description 37
- 238000007599 discharging Methods 0.000 claims abstract description 36
- 238000011084 recovery Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 26
- AWSFEOSAIZJXLG-UHFFFAOYSA-N azepan-2-one;hydrate Chemical compound O.O=C1CCCCCN1 AWSFEOSAIZJXLG-UHFFFAOYSA-N 0.000 claims description 24
- 239000007791 liquid phase Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 20
- 239000000498 cooling water Substances 0.000 claims description 13
- 239000000470 constituent Substances 0.000 claims description 10
- 238000007670 refining Methods 0.000 claims description 9
- 238000004065 wastewater treatment Methods 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 6
- 238000001704 evaporation Methods 0.000 claims description 6
- 239000012808 vapor phase Substances 0.000 claims description 6
- 230000008676 import Effects 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 3
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 2
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 239000004571 lime Substances 0.000 claims description 2
- 238000009833 condensation Methods 0.000 abstract description 27
- 230000005494 condensation Effects 0.000 abstract description 27
- 230000008878 coupling Effects 0.000 abstract description 14
- 238000010168 coupling process Methods 0.000 abstract description 14
- 238000005859 coupling reaction Methods 0.000 abstract description 14
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 23
- 238000010438 heat treatment Methods 0.000 description 17
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 12
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 12
- VEZUQRBDRNJBJY-UHFFFAOYSA-N cyclohexanone oxime Chemical compound ON=C1CCCCC1 VEZUQRBDRNJBJY-UHFFFAOYSA-N 0.000 description 12
- 238000004134 energy conservation Methods 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000003795 chemical substances by application Substances 0.000 description 9
- 230000008569 process Effects 0.000 description 9
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 8
- 239000006227 byproduct Substances 0.000 description 8
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 8
- 239000002994 raw material Substances 0.000 description 8
- -1 acyl ammonia Chemical compound 0.000 description 5
- 239000007864 aqueous solution Substances 0.000 description 5
- 239000012074 organic phase Substances 0.000 description 5
- 238000000926 separation method Methods 0.000 description 5
- 235000006508 Nelumbo nucifera Nutrition 0.000 description 4
- 240000002853 Nelumbo nucifera Species 0.000 description 4
- 235000006510 Nelumbo pentapetala Nutrition 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000011017 operating method Methods 0.000 description 4
- 239000012071 phase Substances 0.000 description 3
- 150000001408 amides Chemical class 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000009834 vaporization Methods 0.000 description 2
- 230000008016 vaporization Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- 125000002252 acyl group Chemical group 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Natural products N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- 239000008346 aqueous phase Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 150000003951 lactams Chemical class 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000002918 waste heat Substances 0.000 description 1
Classifications
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D201/00—Preparation, separation, purification or stabilisation of unsubstituted lactams
- C07D201/16—Separation or purification
Abstract
The invention discloses a kind of method and device of Non-energy-consumption recovery caprolactam organic extractant, the device includes：High pressure waste water stripper, it is high, in, low pressure organic solvent rectifying column, wastewater feed preheater, organic solvent feed preheater, low pressure overhead condenser, reboiler, phase separation tank, organic solvent discharging cooler, high pressure tower top auxiliary condenser, pump etc., organic extractant recovery of the present invention uses three-effect rectification, high pressure organic solvent rectifying column tower top condensation load is pressed with solvent tower bottom of rectifying tower reboiler heat duty with and matched, in be pressed with solvent rectifying column tower top condensation load and match with low pressure organic solvent tower bottom of rectifying tower reboiler heat duty, realize thermal coupling rectifying；Meanwhile the overhead vapours of high pressure waste water stripper is used to heat high pressure organic solvent tower bottom of rectifying tower reboiler, the Non-energy-consumption recovery of caprolactam organic extractant is realized；Considerably reduce the production cost of caprolactam.
Description
Technical field
The invention belongs to technical field of rectification, more particularly to the method and device of Non-energy-consumption recovery caprolactam organic extractant.
Background technology
In interior acyl ammonia device, cyclohexanone oxime prepares workshop section, and reaction solution is after solvent recovery, extraction, washing recovery reaction dissolvent
The cyclohexanone oxime aqueous solution after extracting, washing caused waste water enter water vaporization tower, stripping tower reactor is met the useless of requirement
Waste water processing station is sent into after water, top discharge separates organic phase after split-phase, and aqueous-phase reflux continues to distill to charging, the waste water vapour
Stripper is because water and internal circulating load are big, high energy consumption, and tower reactor waste water index is different, and the life quantity of steam of consumption is different.
Crude caprolactam refinement, need to extract caprolactam with organic extractant for purification caprolactam, then use water
Caprolactam in organic extractant is stripped., must due to accumulation of the accessory substance in organic extractant in extraction process
Organic extractant must be regenerated.At present, organic extractant regeneration is all using the method distilled, by organic extractant from tower
Top is steamed out purification, domestic mostly to be distilled using single column, high energy consumption, causes the increase of caprolactam production cost.
If can be realized by various means, overhead condensation load and tower reactor heating load consume near minimum, realize the section of production process
It can lower consumption, reduce production cost, the competitive advantage of preparing process of caprolactam can be improved, be significant.
The content of the invention
The purpose of the present invention is overcome the deficiencies in the prior art, there is provided a kind of device of Non-energy-consumption recovery caprolactam organic extractant.
Second object of the present invention is to provide the device of second of Non-energy-consumption recovery caprolactam organic extractant.
Third object of the present invention is to provide a kind of method of Non-energy-consumption recovery caprolactam organic extractant.
Technical scheme is summarized as follows：
A kind of device of Non-energy-consumption recovery caprolactam organic extractant, including high pressure waste water stripper 1, high pressure organic solvent essence
Evaporate tower 2, in be pressed with solvent rectifying column 3, low pressure organic solvent rectifying column 4, wastewater feed preheater 5, organic solvent charging
Preheater 6, low pressure overhead condenser 7, the first high pressure tower reactor reboiler 8, the second high pressure tower reactor reboiler 9, medium pressure column kettle are again
Boil device 10, low pressure tower reactor reboiler 11, phase separation tank 12, organic solvent discharging cooler 13, high pressure tower top auxiliary condenser 14,
First pump 15；Wastewater feed tank field A is connected with the top of wastewater feed preheater 5 and high pressure waste water stripper 1 successively by pipeline
Connect, two-way is divided in the top of high pressure waste water stripper 1 after being connected by pipeline with high pressure tower top auxiliary condenser 14, all the way successively with
Second high pressure tower reactor reboiler 9 and phase separation tank 12 are connected, and another way is directly connected with phase separation tank 12；The top of phase separation tank 12 leads to
Piping is connected with waste water organic solvent tank field I, the bottom of phase separation tank 12 by pipeline successively with the first pump 15 and high pressure waste water
The top connection of stripper 1；The bottom of high pressure waste water stripper 1 passes through the pipeline bottom with the first high pressure tower reactor reboiler 8 respectively
Portion connects with the shell side inlet of wastewater feed preheater 5；The top of first high pressure tower reactor reboiler 8 passes through pipeline and high pressure waste water vapour
The bottom connection of stripper 1；The shell-side outlet of wastewater feed preheater 5 is connected by pipeline with wastewater treatment working section G；Organic solvent
Charging tank field C be connected by pipeline with organic solvent feed preheater 6 tunnels of Hou Fen tri- respectively with high pressure organic solvent rectifying column 2,
In be pressed with solvent rectifying column 3 and connected with the top of low pressure organic solvent rectifying column 4, the top of high pressure organic solvent rectifying column 2
Discharged successively with medium pressure column kettle reboiler 10, organic solvent by pipeline after cooler 13 is connected, then with organic solvent tank field L
Connection；The bottom of high pressure organic solvent rectifying column 2 by pipeline respectively with the bottom of the second high pressure tower reactor reboiler 9 and in be pressed with
The middle part connection of solvent rectifying column 3, the top of the second high pressure tower reactor reboiler 9 passes through pipeline and high pressure organic solvent rectifying column
2 bottom connection；In be pressed with the top of solvent rectifying column 3 by pipeline successively with low pressure tower reactor reboiler 11, organic solvent
The discharging connection of cooler 13 connects with organic solvent tank field L；In be pressed with the bottom of solvent rectifying column 3 by pipeline respectively with
Pressure tower reactor reboiler 10 connects with the middle part of low pressure organic solvent rectifying column 4, and the top of medium pressure column kettle reboiler 10 passes through pipeline
The bottom that solvent rectifying column 3 is pressed with is connected；The top of low pressure organic solvent rectifying column 4 is entered by pipeline and organic solvent
Expect that the shell side inlet of preheater 6 connects, the shell side vapor phase exit of organic solvent feed preheater 6 is cold by pipeline and low pressure tower top
The shell side inlet connection of condenser 7, the shell side liquid-phase outlet of organic solvent feed preheater 6 pass through pipeline and organic solvent tank field L
Connection, the shell-side outlet of low pressure overhead condenser 7 are connected by pipeline with organic solvent tank field L；Low pressure organic solvent rectifying column
4 bottom is connected with the bottom of low pressure tower reactor reboiler 11 and organic solvent heavy constituent separator K respectively by pipeline, low pressure
The top of tower reactor reboiler 11 is connected by pipeline with the bottom of low pressure organic solvent rectifying column 4；Organic solvent discharging cooler
13 shell side import is connected by pipeline with caprolactam water solution tank field D, the shell-side outlet of organic solvent discharging cooler 13
It is connected by pipeline with caprolactam refining workshop section M；Raw steam tank field B by pipeline respectively with the first high pressure tower reactor reboiler 8
The shell side inlet connection of shell side inlet, the second high pressure tower reactor reboiler 9；The shell-side outlet of first high pressure tower reactor reboiler 8 and
The shell-side outlet of two high pressure tower reactor reboiler 9 is connected by pipeline with raw steam condensate tank field H respectively；Recirculated cooling water tank field E
After being connected by pipeline with the tube side of low pressure overhead condenser 7, it is connected with recirculated water backwater tank field F.
The device of second of Non-energy-consumption recovery caprolactam organic extractant, including high pressure waste water stripper 21, high pressure organic solvent
Rectifying column 22, in be pressed with solvent rectifying column 23, low pressure organic solvent rectifying column 24, wastewater feed preheater 25, You Jirong
Agent feed preheater 26, low pressure overhead condenser 27, the first high pressure tower reactor reboiler 28, the second high pressure tower reactor reboiler 29,
Medium pressure column kettle reboiler 30, low pressure tower reactor reboiler 31, phase separation tank 32, organic solvent discharging cooler 33, high pressure tower top are auxiliary
Help condenser 34, the first pump 35, the second pump 36, the 3rd pump 37；Wastewater feed tank field A2 is entered with waste water successively by pipeline
Material preheater 25 connects with the top of high pressure waste water stripper 21, and the top of high pressure waste water stripper 21 passes through pipeline and high-pressure tower
Top auxiliary condenser 34 divides two-way after connecting, and is connected successively with the second high pressure tower reactor reboiler 29 and phase separation tank 32 all the way；It is another
Road is directly connected with phase separation tank 32；The top of phase separation tank 32 is connected by pipeline with waste water organic solvent tank field I2；Phase separation tank 32
Bottom be connected by pipeline with the first pump 35 after, be connected with the top of high pressure waste water stripper 21；High pressure waste water stripper 21
Bottom be connected respectively with the bottom of the first high pressure tower reactor reboiler 28 and the shell side inlet of wastewater feed preheater 25 by pipeline；
The top of first high pressure tower reactor reboiler 28 is connected by pipeline with the bottom of high pressure waste water stripper 21；Wastewater feed preheater
25 shell-side outlets are connected by pipeline with wastewater treatment working section G2；Organic solvent charging tank field C2 is entered by pipeline and organic solvent
Material preheater 26 connect Hou Fen tri- tunnels respectively with high pressure organic solvent rectifying column 22, in be pressed with solvent rectifying column 23, low pressure has
The top connection of solvent rectifying column 24, the top of high pressure organic solvent rectifying column 22 is boiled again with medium pressure column kettle successively by pipeline
Device 30, organic solvent discharge after the connection of cooler 33, then are connected with organic solvent tank field L2；High pressure organic solvent rectifying column 22
Bottom be connected respectively with the bottom of the second high pressure tower reactor reboiler 29 and organic solvent heavy constituent separator K2 by pipeline；
The top of second high pressure tower reactor reboiler 29 is connected by pipeline with the bottom of high pressure organic solvent rectifying column 22；In to be pressed with machine molten
After the top of agent rectifying column 23 is connected with low pressure tower reactor reboiler 31, organic solvent discharging cooler 33 successively by pipeline, then
It is connected with organic solvent tank field L2；In be pressed with the bottom of solvent rectifying column 23 by pipeline respectively with medium pressure column kettle reboiler 30
Bottom and the second pump 36 connect, the second pump 36 is connected by pipeline with the middle part of high pressure organic solvent rectifying column 22；Medium pressure column
The bottom that the top of kettle reboiler 30 is pressed with solvent rectifying column 23 by pipeline with is connected；Low pressure organic solvent rectifying column 24
Top be connected by pipeline with the shell side inlet of organic solvent feed preheater 26；The shell side of organic solvent feed preheater 26
Vapor phase exit is connected by pipeline with the shell side inlet of low pressure overhead condenser 27, the shell side liquid of organic solvent feed preheater 26
Mutually outlet is connected by pipeline with organic solvent tank field L2；The shell-side outlet of low pressure overhead condenser 27 by pipeline with it is organic molten
The L2 connections of agent tank field；The bottom of low pressure organic solvent rectifying column 24 by pipeline respectively with the bottom of low pressure tower reactor reboiler 31 and
3rd pump 37 is connected, and the middle part that the 3rd pump 37 is pressed with solvent rectifying column 23 by pipeline with is connected, low pressure tower reactor reboiler
31 top is connected by pipeline with the bottom of low pressure organic solvent rectifying column 24；The shell side of organic solvent discharging cooler 33 enters
Mouthful be connected by pipeline with caprolactam water solution tank field D2, organic solvent discharge cooler 33 shell-side outlet by pipeline and
The M2 connections of caprolactam refining workshop section；Raw steam tank field B2 is entered with the shell side of the first high pressure tower reactor reboiler 28 respectively by pipeline
Mouth connects with the shell side inlet of the second high pressure tower reactor reboiler 29；The shell-side outlet of first high pressure tower reactor reboiler 28 and second high
The shell-side outlet of tower reactor reboiler 29 is pressed to be connected respectively by pipeline with raw steam condensate tank field H2；Recirculated cooling water tank field E2
After being connected by pipeline with the tube side of low pressure overhead condenser 27, it is connected with recirculated water backwater tank field F2.
A kind of method of Non-energy-consumption recovery caprolactam organic extractant, comprises the following steps：
A) device of usage right requirement 1 or 2；
B) the operating pressure control of high pressure waste water stripper is in 0.1~1.0MPaA, the control of high pressure organic solvent rectifying column operating pressure
In 0.1~0.8MPaA, in be pressed with the control of solvent rectifying column operating pressure in 0.01~0.6MPaA, low pressure organic solvent rectifying
The control of tower operating pressure is higher than high pressure organic solvent rectifying tower in 0.01~0.4MPaA, high pressure waste water stripper overhead vapor (steam) temperature
5~50 DEG C of kettle kettle liquid temperature；High pressure organic solvent rectifying column tower top vapor (steam) temperature is pressed with solvent tower bottom of rectifying tower kettle liquid temperature in being higher than
5~50 DEG C of degree；In be pressed with solvent rectifying column tower top vapor (steam) temperature and be higher than low pressure organic solvent tower bottom of rectifying tower kettle liquid temperature 5~50
℃；
C) overhead vapours of high pressure waste water stripper provides thermal source for high pressure organic solvent rectifying column；
D) overhead vapours of high pressure organic solvent rectifying column is pressed with solvent rectifying column in and provides thermal source；
E) overhead vapours that solvent rectifying column is pressed with provides thermal source for low pressure organic solvent rectifying column；
F) wastewater feed of high pressure waste water stripper and high pressure waste water stripper tower reactor discharging is exchanged heat, organic solvent charging with it is low
The overhead vapours heat exchange of solvent rectifying column is pressed with, high pressure organic solvent rectifying column is pressed with the overhead vapours of solvent rectifying column with
Lime set exchanges heat with caprolactam water solution.
Advantages of the present invention：
1. organic extractant recovery uses three-effect rectification, high pressure organic solvent rectifying column tower top condensation load is pressed with solvent essence with
Tower tower reactor reboiler thermic load is evaporated to match, in be pressed with solvent rectifying column tower top condensation load and low pressure organic solvent rectifying tower
Kettle reboiler heat duty matches, and realizes thermal coupling rectifying.
2. the overhead vapours of high pressure waste water stripper is used to heat high pressure organic solvent tower bottom of rectifying tower reboiler, acyl in oneself is realized
The Non-energy-consumption recovery of amine organic extractant.
3. by being exchanged heat to wastewater feed and the discharging of high pressure waste water stripper tower reactor, organic solvent charging and low pressure organic solvent rectifying
Column overhead steam heat-exchanging, caprolactam water solution are pressed with the discharging of solvent rectifying column tower top condensate liquid with and exchanged heat, and realize energy
Abundant recycling.
Brief description of the drawings
Fig. 1 is the schematic device that a kind of Non-energy-consumption reclaims caprolactam organic extractant.
Fig. 2 is the schematic device that second of Non-energy-consumption reclaims caprolactam organic extractant.
Embodiment
By specific embodiment, the invention will be further described below in conjunction with the accompanying drawings, but following examples be it is descriptive, no
It is limited, it is impossible to which protection scope of the present invention is limited with this.
A kind of device of Non-energy-consumption recovery caprolactam organic extractant, is shown in Fig. 1, including high pressure waste water stripper 1, high pressure are organic
Solvent rectifying column 2, in be pressed with solvent rectifying column 3, low pressure organic solvent rectifying column 4, wastewater feed preheater 5, You Jirong
Agent feed preheater 6, low pressure overhead condenser 7, the first high pressure tower reactor reboiler 8, the second high pressure tower reactor reboiler 9, middle pressure
Tower reactor reboiler 10, low pressure tower reactor reboiler 11, phase separation tank 12, organic solvent discharging cooler 13, high pressure tower top auxiliary are cold
Condenser 14, the first pump 15；Wastewater feed tank field A by pipeline successively with wastewater feed preheater 5 and high pressure waste water stripper 1
Top connection, the top of high pressure waste water stripper 1 divides two-way after being connected by pipeline with high pressure tower top auxiliary condenser 14, one
Road is connected with the second high pressure tower reactor reboiler 9 and phase separation tank 12 successively, and another way is directly connected with phase separation tank 12；Phase separation tank 12
Top be connected by pipeline with waste water organic solvent tank field I, the bottom of phase separation tank 12 by pipeline successively with the first pump 15 and
The top connection of high pressure waste water stripper 1；Boiled again with the first high pressure tower reactor respectively by pipeline the bottom of high pressure waste water stripper 1
The bottom of device 8 connects with the shell side inlet of wastewater feed preheater 5；The top of first high pressure tower reactor reboiler 8 passes through pipeline and height
Press the bottom connection of water vaporization tower 1；The shell-side outlet of wastewater feed preheater 5 is connected by pipeline with wastewater treatment working section G；
It is smart with high pressure organic solvent respectively that organic solvent charging tank field C is connected the tunnels of Hou Fen tri- by pipeline with organic solvent feed preheater 6
Evaporate tower 2, in be pressed with solvent rectifying column 3 and connected with the top of low pressure organic solvent rectifying column 4, high pressure organic solvent rectifying column 2
Top discharged successively with medium pressure column kettle reboiler 10, organic solvent by pipeline after cooler 13 is connected, then with organic solvent
Tank field L connections；The bottom of high pressure organic solvent rectifying column 2 by pipeline respectively with the bottom of the second high pressure tower reactor reboiler 9 and
In be pressed with solvent rectifying column 3 middle part connection, the top of the second high pressure tower reactor reboiler 9 passes through pipeline and high pressure organic solvent
The bottom connection of rectifying column 2；In be pressed with the top of solvent rectifying column 3 by pipeline successively with low pressure tower reactor reboiler 11, have
The solvent discharging connection of cooler 13 connects with organic solvent tank field L；In be pressed with the bottom of solvent rectifying column 3 and pass through pipeline point
Middle part not with medium pressure column kettle reboiler 10 and low pressure organic solvent rectifying column 4 is connected, and the top of medium pressure column kettle reboiler 10 leads to
The bottom that piping is pressed with solvent rectifying column 3 with is connected；The top of low pressure organic solvent rectifying column 4 by pipeline with it is organic
The shell side inlet connection of solvent feed preheater 6, the shell side vapor phase exit of organic solvent feed preheater 6 pass through pipeline and low pressure
The shell side inlet connection of overhead condenser 7, the shell side liquid-phase outlet of organic solvent feed preheater 6 pass through pipeline and organic solvent
Tank field L connections, the shell-side outlet of low pressure overhead condenser 7 are connected by pipeline with organic solvent tank field L；Low pressure organic solvent
The bottom of rectifying column 4 is connected with the bottom of low pressure tower reactor reboiler 11 and organic solvent heavy constituent separator K respectively by pipeline
Connect, the top of low pressure tower reactor reboiler 11 is connected by pipeline with the bottom of low pressure organic solvent rectifying column 4；Organic solvent discharges
The shell side import of cooler 13 is connected by pipeline with caprolactam water solution tank field D, the shell of organic solvent discharging cooler 13
Journey outlet is connected by pipeline with caprolactam refining workshop section M；Raw steam tank field B by pipeline respectively with the first high pressure tower reactor again
Boil the shell side inlet connection of the shell side inlet of device 8, the second high pressure tower reactor reboiler 9；The shell side of first high pressure tower reactor reboiler 8 goes out
Mouth and the shell-side outlet of the second high pressure tower reactor reboiler 9 are connected by pipeline with raw steam condensate tank field H respectively；Recirculated cooling water
After tank field E is connected by pipeline with the tube side of low pressure overhead condenser 7, it is connected with recirculated water backwater tank field F.
The device of second of Non-energy-consumption recovery caprolactam organic extractant, is shown in Fig. 2, including high pressure waste water stripper 21, high pressure
Organic solvent rectifying column 22, in be pressed with solvent rectifying column 23, low pressure organic solvent rectifying column 24, wastewater feed preheater 25,
Organic solvent feed preheater 26, low pressure overhead condenser 27, the first high pressure tower reactor reboiler 28, the second high pressure tower reactor are boiled again
Device 29, medium pressure column kettle reboiler 30, low pressure tower reactor reboiler 31, phase separation tank 32, organic solvent discharging cooler 33, high pressure
Tower top auxiliary condenser 34, the first pump 35, the second pump 36, the 3rd pump 37；Wastewater feed tank field A2 by pipeline successively with
Wastewater feed preheater 25 connects with the top of high pressure waste water stripper 21, the top of high pressure waste water stripper 21 by pipeline with
High pressure tower top auxiliary condenser 34 divides two-way after connecting, and is connected successively with the second high pressure tower reactor reboiler 29 and phase separation tank 32 all the way；
Another way is directly connected with phase separation tank 32；The top of phase separation tank 32 is connected by pipeline with waste water organic solvent tank field I2；Split-phase
After the bottom of tank 32 is connected by pipeline with the first pump 35, it is connected with the top of high pressure waste water stripper 21；High pressure waste water strips
The bottom of tower 21 is connected with the bottom of the first high pressure tower reactor reboiler 28 and the shell side inlet of wastewater feed preheater 25 respectively by pipeline
Connect；The top of first high pressure tower reactor reboiler 28 is connected by pipeline with the bottom of high pressure waste water stripper 21；Wastewater feed is pre-
The hot shell-side outlet of device 25 is connected by pipeline with wastewater treatment working section G2；Organic solvent feed tank field C2 by pipeline with it is organic
Solvent feed preheater 26 connect Hou Fen tri- tunnels respectively with high pressure organic solvent rectifying column 22, in be pressed with solvent rectifying column 23,
The top connection of low pressure organic solvent rectifying column 24, the top of high pressure organic solvent rectifying column 22 by pipeline successively with medium pressure column
Kettle reboiler 30, organic solvent discharge after the connection of cooler 33, then are connected with organic solvent tank field L2；High pressure organic solvent essence
Evaporate the bottom of tower 22 and pass through the pipeline bottom with the second high pressure tower reactor reboiler 29 and organic solvent heavy constituent separator K2 respectively
Connection；The top of second high pressure tower reactor reboiler 29 is connected by pipeline with the bottom of high pressure organic solvent rectifying column 22；Middle pressure
The top of organic solvent rectifying column 23 is connected with low pressure tower reactor reboiler 31, organic solvent discharging cooler 33 successively by pipeline
Afterwards, then with organic solvent tank field L2 it is connected；In be pressed with the bottom of solvent rectifying column 23 by pipeline respectively with medium pressure column kettle again
The bottom and the second pump 36 for boiling device 30 are connected, and the second pump 36 is connected by pipeline with the middle part of high pressure organic solvent rectifying column 22；
The bottom that the top of medium pressure column kettle reboiler 30 is pressed with solvent rectifying column 23 by pipeline with is connected；Low pressure organic solvent essence
The top for evaporating tower 24 is connected by pipeline with the shell side inlet of organic solvent feed preheater 26；Organic solvent feed preheater 26
Shell side vapor phase exit be connected by pipeline with the shell side inlet of low pressure overhead condenser 27, organic solvent feed preheater 26
Shell side liquid-phase outlet is connected by pipeline with organic solvent tank field L2；The shell-side outlet of low pressure overhead condenser 27 by pipeline with
The L2 connections of organic solvent tank field；The bottom of low pressure organic solvent rectifying column 24 by pipeline respectively with low pressure tower reactor reboiler 31
Bottom and the 3rd pump 37 connect, the middle part that the 3rd pump 37 is pressed with solvent rectifying column 23 by pipeline with is connected, lower pressure column
The top of kettle reboiler 31 is connected by pipeline with the bottom of low pressure organic solvent rectifying column 24；Organic solvent discharging cooler 33
Shell side import be connected by pipeline with caprolactam water solution tank field D2, organic solvent discharging cooler 33 shell-side outlet lead to
Piping is connected with caprolactam refining workshop section M2；Raw steam tank field B2 by pipeline respectively with the first high pressure tower reactor reboiler
28 shell side inlets and the connection of the shell side inlet of the second high pressure tower reactor reboiler 29；The shell-side outlet of first high pressure tower reactor reboiler 28
It is connected respectively by pipeline with raw steam condensate tank field H2 with the shell-side outlet of the second high pressure tower reactor reboiler 29；Circulating cooling
After water pot area E2 is connected by pipeline with the tube side of low pressure overhead condenser 27, it is connected with recirculated water backwater tank field F2.
Embodiment 1
Using the first device, technological process A operating method is as follows：
Waste water raw material from wastewater feed tank field A after the preheating of wastewater feed preheater 5 by entering high pressure waste water stripper 1
Stripping separation is carried out, high pressure waste water stripper overhead steam is passed through after high pressure tower top auxiliary condenser 12 condenses waste heat
Second high pressure tower reactor reboiler 9, condensate liquid are passed through phase separation tank 12, and the top organic phase of phase separation tank 12 is produced to waste water organic solvent tank
Area I, lower aqueous enter high pressure waste water stripper 1 after the pressurization of the first pump 15；The tower reactor liquid phase of high pressure waste water stripper 1 is divided into
Two strands, one returns to high pressure waste water stripper 1 after being evaporated by the first high pressure tower reactor reboiler 8, and another stock passes through wastewater feed
Preheater 5 and wastewater feed heat exchange heel row to wastewater treatment working section G；Organic solvent from organic solvent charging tank field C passes through
Respectively enterd after organic solvent feed preheater 6 high pressure organic solvent rectifying column 2, in be pressed with solvent rectifying column 3, low pressure organic
Rectifying is carried out in solvent rectifying column 4, the overhead vapours of high pressure organic solvent rectifying column 2 is pressed with solvent rectifying column 3 as in
Thermal source, again by organic solvent discharging cooler 13 with deriving from caprolactam water solution after the condensation of medium pressure column kettle reboiler 10
To organic solvent tank field L after tank field D caprolactam water solution heat exchange；Caprolactam water solution after heat exchange is passed through caprolactam
Refinement M；The tower reactor liquid phase of high pressure organic solvent rectifying column 2 is divided to two strands, and one is returned after being evaporated by high pressure tower reactor reboiler 9
High pressure organic solvent rectifying column 2 is returned, solvent rectifying column 3 is pressed with another burst of entrance and continues rectifying；In be pressed with solvent rectifying
Thermal source of the overhead vapours of tower 3 as low pressure organic solvent rectifying column 4, again by organic after the condensation of low pressure tower reactor reboiler 11
Solvent discharges cooler 13 with deriving from after caprolactam water solution tank field D caprolactam water solution exchanges heat to organic solvent tank
Area L；In be pressed with the tower reactor liquid phase of solvent rectifying column 3 and be divided to two strands, one is pressed in being returned after being evaporated by medium pressure column kettle reboiler 10
Organic solvent rectifying column 3, another strand enters low pressure organic solvent rectifying column 4 and continues rectifying；Low pressure organic solvent rectifying column 4
Overhead vapor is by organic solvent feed preheater 6 with being fed from organic solvent after tank field C organic solvent exchanges heat again through low
Pressure overhead condenser 7 condenses, condensate liquid to organic solvent tank field L；The condensate liquid of organic solvent feed preheater 6 is to organic molten
Agent tank field L；The tower reactor liquid phase of low pressure organic solvent rectifying column 4 is divided to two strands, and one is returned after being evaporated by low pressure tower reactor reboiler 11
Low pressure organic solvent rectifying column 4, another strand enters organic solvent heavy constituent separator K；From recirculated cooling water tank field E
Recirculated cooling water as the low-temperature receiver of low pressure overhead condenser 7, recirculated water backwater tank field F is passed through after cooling；From raw vapor can
Thermal source of the area B life steam as the first high pressure tower reactor reboiler 8, is passed through raw steam condensate tank field H after heat exchange；Height is pressed with
Solvent rectifying column 2 and in be pressed between solvent rectifying column 3 and in be pressed with solvent rectifying column 3 and low pressure organic solvent rectifying
Fed between tower 4 by pressure difference, without being fed by pump.
Produce 100kt Caprolactam unit per year for Shandong, the quality group of waste water raw material turns into：Water content 99.9%, toluene
Content 0.0301%, cyclohexanone oxime content 0.0184%, other content of reaction byproduct 0.0515%.
Organic solvent charging tank field C organic extractant quality group turns into：Benzene content 99.4%, water content 0.1%, cyclohexanone contains
Amount 0.1%, hexamethylene alcohol content 0.1%, aniline content 0.1%, other content of reaction byproduct 0.2%.
High pressure waste water stripper operating pressure is 0.5MPaA, 147.7 DEG C of tower top temperature, 158.8 DEG C of bottom temperature, tower theoretical stage
Number is 15；High pressure organic solvent rectifying column operating pressure is 0.38MPaA, 130.0 DEG C of tower top temperature, 131.4 DEG C of bottom temperature,
Tower theoretical stage is 8；In to be pressed with solvent rectifying column operating pressure be 0.22MPaA, 107.4 DEG C of tower top temperature, bottom temperature
108.9 DEG C, tower theoretical stage is 8；Low pressure organic solvent rectifying column operating pressure is 0.1MPaA, 79.6 DEG C of tower top temperature, tower
87.3 DEG C of kettle temperature degree, tower theoretical stage are 8.
Through said process, each tower top tower kettle discharging reaches factory's processing requirement.Because the technique considers sufficient thermal coupling, respectively
(thermic load is heated or cooled for what is saved in bracket) in the load of tower such as table 1：
Table 1
| Cool down load/KW | Heating load/KW | Total/KW | |
| High pressure waste water stripper | 300(3000) | 3500 | 3800(6800) |
| High pressure organic solvent rectifying column | (2533) | (2859) | (5392) |
| In be pressed with solvent rectifying column | (2255) | (2475) | (4730) |
| Low pressure organic solvent rectifying column | 1825 | (2000) | 1825(3825) |
| It is total | 2125(9913) | 3500(10834) | 5625(20747) |
When the present embodiment does not couple, the total heating load of each tower is 10834KW, condensation load 9913KW, and total heat is born
Lotus is 20747KW；After coupling, the total heating load of each tower is 3500KW, condensation load 2125KW, and total heat is born
Lotus is 5625KW；Heating load energy-conservation 67.7%, condensation load energy-conservation 79.4%, total thermic load energy-conservation 73.2%.
The recovery thermic load of the caprolactam organic extractant of the present embodiment derives from high pressure waste water stripper, high pressure waste water stripper
Unnecessary thermic load make the recovery of high pressure waste water stripper overhead condensation load and caprolactam organic extractant by auxiliary condenser
Thermic load matches, and is truly realized Non-energy-consumption recovery caprolactam organic extractant.
Embodiment 2
Using second of device, the operating method of process flow B is as follows：
Waste water raw material from wastewater feed tank field A2 after the preheating of wastewater feed preheater 25 by entering high pressure waste water stripper
21 carry out stripping separation, and high pressure waste water stripper overhead steam is by (the auxiliary condenser not work of high pressure tower top auxiliary condenser 34
Make), the second high pressure tower reactor reboiler 29 is passed through, condensate liquid is passed through phase separation tank 32, and the top organic phase of phase separation tank 32 is produced to waste water
Organic solvent tank field I2, lower aqueous enter high pressure waste water stripper 21 after the pressurization of the first pump 35；High pressure waste water stripper 21
Tower reactor liquid phase is divided into two strands, and one returns to high pressure waste water stripper 21 after being evaporated by the first high pressure tower reactor reboiler 28, another
Stock passes through wastewater feed preheater 25 and wastewater feed heat exchange heel row to wastewater treatment working section G2；Tank field is fed from organic solvent
C2 organic solvent by respectively enterd after organic solvent feed preheater 26 high pressure organic solvent rectifying column 22, in be pressed with machine molten
Rectifying, the overhead vapours conduct of high pressure organic solvent rectifying column 22 are carried out in agent rectifying column 23, low pressure organic solvent rectifying column 24
In be pressed with the thermal source of solvent rectifying column 23, again by organic solvent discharging cooler 33 after the condensation of medium pressure column kettle reboiler 30
With after the heat exchange of caprolactam water solution tank field D2 caprolactam water solution to organic solvent tank field L2；Oneself after heat exchange
Lactam aqueous solution is passed through caprolactam refining workshop section M2；The tower reactor liquid phase of high pressure organic solvent rectifying column 22 is divided to two strands, and one is logical
Cross after high pressure tower reactor reboiler 29 is evaporated and return to high pressure organic solvent rectifying column 22, another strand enters the separation of organic solvent heavy constituent
Device K；In be pressed with thermal source of the overhead vapours of solvent rectifying column 23 as low pressure organic solvent rectifying column 24, through lower pressure column
Kettle reboiler 31 condense after again by organic solvent discharging cooler 33 with from caprolactam water solution tank field D2 oneself in
To organic solvent tank field L2 after amide aqueous solution heat exchange；In be pressed with the tower reactor liquid phase of solvent rectifying column 23 and be divided to two strands, one passes through
Medium pressure column kettle reboiler 30 is pressed with solvent rectifying column 23 in being returned after evaporating, another stock-traders' know-how enters height after crossing the pressurization of the second pump 36
It is pressed with solvent rectifying column 22 and continues rectifying；The overhead vapor of low pressure organic solvent rectifying column 24 passes through organic solvent feeding preheating
Device 26 condenses with being condensed again through low pressure overhead condenser 27 after organic solvent charging tank field C2 organic solvent heat exchange
Liquid is to organic solvent tank field L2；The condensate liquid of organic solvent feed preheater 26 is to organic solvent tank field L2；
The tower reactor liquid phase of low pressure organic solvent rectifying column 24 is divided to two strands, and one returns to low pressure after being evaporated by low pressure tower reactor reboiler 31
Organic solvent rectifying column 24, another stock-traders' know-how cross the 3rd pump 37 pressurization after enter in be pressed with solvent rectifying column 4 continue rectifying；Come
Recirculated cooling water tank field E2 recirculated cooling water is come from as the low-temperature receiver of low pressure overhead condenser 27, recirculated water backwater is passed through after cooling
Tank field F2；From thermal source of the steam tank field B2 life steam as the first high pressure tower reactor reboiler 28 is given birth to, life is passed through after heat exchange
Steam condensate tank field H.
Produce 100kt Caprolactam unit per year for Shandong, the quality group of waste water raw material turns into：Water content 99.9%, toluene
Content 0.0301%, cyclohexanone oxime content 0.0184%, other content of reaction byproduct 0.0515%.
Organic solvent charging tank field C organic extractant quality group turns into：Benzene content 99.4%, water content 0.1%, cyclohexanone contains
Amount 0.1%, hexamethylene alcohol content 0.1%, aniline content 0.1%, other content of reaction byproduct 0.2%.
High pressure waste water stripper operating pressure is 0.5MPaA, 147.7 DEG C of tower top temperature, 158.8 DEG C of bottom temperature, tower theoretical stage
Number is 15；High pressure organic solvent rectifying column operating pressure is 0.38MPaA, 130.0 DEG C of tower top temperature, 141.7 DEG C of bottom temperature,
Tower theoretical stage is 8；In to be pressed with solvent rectifying column operating pressure be 0.22MPaA, 107.4 DEG C of tower top temperature, bottom temperature
108.9 DEG C, tower theoretical stage is 8；Low pressure organic solvent rectifying column operating pressure is 0.1MPaA, 79.6 DEG C of tower top temperature, tower
87.3 DEG C of kettle temperature degree, tower theoretical stage are 8.
Through said process, each tower top tower kettle discharging reaches factory's processing requirement.Because the technique considers sufficient thermal coupling, respectively
(thermic load is heated or cooled for what is saved in bracket) in the load of tower such as table 2：
Table 2
| Cool down load/KW | Heating load/KW | Total/KW | |
| High pressure waste water stripper | (3300) | 3500 | 3500(6800) |
| High pressure organic solvent rectifying column | (2833) | (3159) | (5992) |
| In be pressed with solvent rectifying column | (2555) | (2775) | (5330) |
| Low pressure organic solvent rectifying column | 2125 | (2300) | 2125(4425) |
| It is total | 2125(10813) | 3500(11734) | 5625(22547) |
When the present embodiment does not couple, the total heating load of each tower is 11734KW, condensation load 10813KW, and total heat is born
Lotus is 22547KW；After coupling, the total heating load of each tower is 3500KW, condensation load 2125KW, and total heat is born
Lotus is 5625KW；Heating load energy-conservation 70.2%, condensation load energy-conservation 80.3%, total thermic load energy-conservation 75.1%.
The recovery thermic load of the caprolactam organic extractant of the present embodiment derives from high pressure waste water stripper, high pressure waste water stripper
The recovery thermic load of overhead condensation load and caprolactam organic extractant matches, and is truly realized Non-energy-consumption recovery caprolactam
Organic extractant.
Embodiment 3
Using the first device, technological process A operating method is as follows：
Waste water raw material from wastewater feed tank field A after the preheating of wastewater feed preheater 5 by entering high pressure waste water stripper 1
Carry out stripping separation, after the condensation of high pressure tower top auxiliary condenser 12, condensate liquid is passed through point high pressure waste water stripper overhead steam
Phase tank 12, the top organic phase of phase separation tank 12 produces pressurizes laggard to waste water organic solvent tank field I, lower aqueous through the first pump 15
Enter high pressure waste water stripper 1；The tower reactor liquid phase of high pressure waste water stripper 1 is divided into two strands, and one passes through the first high pressure tower reactor reboiler 8
High pressure waste water stripper 1 is returned to after evaporation, another stock is exchanged heat by wastewater feed preheater 5 and wastewater feed at heel row to waste water
Science and engineering section G；Organic solvent from organic solvent charging tank field C after organic solvent feed preheater 6 by respectively enteing high pressure
Organic solvent rectifying column 2, in be pressed with solvent rectifying column 3, low pressure organic solvent rectifying column 4 and carry out rectifying, high pressure is organic molten
The overhead vapours of agent rectifying column 2 is pressed with the thermal source of solvent rectifying column 3 as in, is passed through again after the condensation of medium pressure column kettle reboiler 10
To organic after crossing organic solvent discharging cooler 13 and being exchanged heat from caprolactam water solution tank field D caprolactam water solution
Vent tank farm L；Caprolactam water solution after heat exchange is passed through caprolactam refining workshop section M；The tower of high pressure organic solvent rectifying column 2
Kettle liquid phase is divided to two strands, and one returns to high pressure organic solvent rectifying column 2, another burst of entrance after being evaporated by high pressure tower reactor reboiler 9
In be pressed with solvent rectifying column 3 continue rectifying；In be pressed with the overhead vapours of solvent rectifying column 3 as low pressure organic solvent rectifying
The thermal source of tower 4, again by organic solvent discharging cooler 13 with deriving from caprolactam after the condensation of low pressure tower reactor reboiler 11
To organic solvent tank field L after aqueous solution tank field D caprolactam water solution heat exchange；In be pressed with the tower reactor liquid phase of solvent rectifying column 3
It is divided to two strands, one is pressed with solvent rectifying column 3 in being returned after being evaporated by medium pressure column kettle reboiler 10, another strand has into low pressure
Solvent rectifying column 4 continues rectifying；The overhead vapor of low pressure organic solvent rectifying column 4 by organic solvent feed preheater 6 with
Condensed again through low pressure overhead condenser 7 after organic solvent charging tank field C organic solvent heat exchange, condensate liquid is to organic molten
Agent tank field L；The condensate liquid of organic solvent feed preheater 6 is to organic solvent tank field L, the tower reactor of low pressure organic solvent rectifying column 4
Liquid phase is divided to two strands, and one returns to low pressure organic solvent rectifying column 4 after being evaporated by low pressure tower reactor reboiler 11, and another burst of entrance has
Solvent heavy constituent separator K；Recirculated cooling water from recirculated cooling water tank field E is cold as low pressure overhead condenser 7
Source, recirculated water backwater tank field F is passed through after cooling；Life steam from raw steam tank field B is as the first high pressure tower reactor reboiler
8 and second high pressure tower reactor reboiler 9 thermal source, raw steam condensate tank field H is passed through after heat exchange；High pressure organic solvent rectifying column 2
Be pressed with between solvent rectifying column 3 and in be pressed between solvent rectifying column 3 and low pressure organic solvent rectifying column 4 and pass through pressure
Difference charging, without being fed by pump.
Produce 100kt Caprolactam unit per year for Shandong, the quality group of waste water raw material turns into：Water content 99.9%, toluene
Content 0.0301%, cyclohexanone oxime content 0.0184%, other content of reaction byproduct 0.0515%.
Organic solvent charging tank field C organic extractant quality group turns into：Benzene content 99.4%, water content 0.1%, cyclohexanone contains
Amount 0.1%, hexamethylene alcohol content 0.1%, aniline content 0.1%, other content of reaction byproduct 0.2%.
High pressure waste water stripper operating pressure is 0.1MPaA, 91.5 DEG C of tower top temperature, 97.1 DEG C of bottom temperature, tower theoretical stage
For 15；High pressure organic solvent rectifying column operating pressure is 0.38MPaA, 130.0 DEG C of tower top temperature, 131.4 DEG C of bottom temperature,
Tower theoretical stage is 8；In to be pressed with solvent rectifying column operating pressure be 0.22MPaA, 107.4 DEG C of tower top temperature, bottom temperature
108.9 DEG C, tower theoretical stage is 8；Low pressure organic solvent rectifying column operating pressure is 0.1MPaA, 79.6 DEG C of tower top temperature, tower
87.3 DEG C of kettle temperature degree, tower theoretical stage are 8.
Through said process, each tower top tower kettle discharging reaches factory's processing requirement.Because the technique considers sufficient thermal coupling, respectively
(thermic load is heated or cooled for what is saved in bracket) in the load of tower such as table 3：
Table 3
| Cool down load/KW | Heating load/KW | Total/KW | |
| High pressure waste water stripper | 3300 | 3500 | 6800 |
| High pressure organic solvent rectifying column | (2533) | 2859 | 2859(5392) |
| In be pressed with solvent rectifying column | (2255) | (2475) | (4730) |
| Low pressure organic solvent rectifying column | 1825 | (2000) | 1825(3825) |
| It is total | 1825(6613) | 2859(7334) | 4684(13947) |
The high pressure waste water stripper of the present embodiment and organic solvent rectifying column isolated operation, organic solvent rectifying column use senior middle school's low pressure
Three-effect rectification, when not coupling, the total heating load of its each tower is 7334KW, condensation load 6613KW, total thermic load
For 13947KW；After coupling, the total heating load of each tower is 2859KW, condensation load 1825KW, total thermic load
For 4684KW；Heating load energy-conservation 61.0%, condensation load energy-conservation 72.4%, total thermic load energy-conservation 66.4%.
The present embodiment is not coupled completely, has only been carried out triple effect coupling rectification to organic solvent rectifying column, save considerably organic
The energy consumption of solvent recovery, the system have the advantages of operation is flexible, and the free degree is big, easily operated.
Embodiment 4
Using second of device, the operating method of process flow B is as follows：
Waste water raw material from wastewater feed tank field A2 after the preheating of wastewater feed preheater 25 by entering high pressure waste water stripper
21 carry out stripping separation, and after the condensation of high pressure tower top auxiliary condenser 34, condensate liquid leads to high pressure waste water stripper overhead steam
Enter phase separation tank 32, the top organic phase of phase separation tank 32 is produced to waste water organic solvent tank field I2, lower aqueous and pressurizeed through the first pump 35
Enter high pressure waste water stripper 21 afterwards；The tower reactor liquid phase of high pressure waste water stripper 21 is divided into two strands, and one passes through the first high pressure tower reactor
Reboiler 28 returns to high pressure waste water stripper 21 after evaporating, after another stock is exchanged heat by wastewater feed preheater 25 and wastewater feed
Drain into wastewater treatment working section G2；Organic solvent from organic solvent charging tank field C2 passes through organic solvent feed preheater 26
After respectively enter high pressure organic solvent rectifying column 22, in be pressed with solvent rectifying column 23, low pressure organic solvent rectifying column 24
Row rectifying, the overhead vapours of high pressure organic solvent rectifying column 22 is pressed with the thermal source of solvent rectifying column 23 as in, through medium pressure column
Kettle reboiler 30 condense after again by organic solvent discharging cooler 33 with from caprolactam water solution tank field D2 oneself in
To organic solvent tank field L2 after amide aqueous solution heat exchange；Caprolactam water solution after heat exchange is passed through caprolactam refining workshop section M2；
The tower reactor liquid phase of high pressure organic solvent rectifying column 22 is divided to two strands, and it is organic that one returns to high pressure after being evaporated by high pressure tower reactor reboiler 29
Solvent rectifying column 22, another strand enters organic solvent heavy constituent separator K2；In be pressed with solvent rectifying column 23 tower top steam
Thermal source of the vapour as low pressure organic solvent rectifying column 24, it is cold by organic solvent discharging again after the condensation of low pressure tower reactor reboiler 31
But to organic solvent tank field L2 after caprolactam water solution heat exchange of the device 33 with deriving from caprolactam water solution tank field D2；Middle pressure
The tower reactor liquid phase of organic solvent rectifying column 23 is divided to two strands, and one is pressed with solvent in being returned after being evaporated by medium pressure column kettle reboiler 30
Rectifying column 23, another stock-traders' know-how enter the continuation rectifying of high pressure organic solvent rectifying column 22 after crossing the pressurization of the second pump 36；Low pressure is organic molten
The overhead vapor of agent rectifying column 24 is by organic solvent feed preheater 26 with feeding the organic of tank field C2 from organic solvent
Condensed again through low pressure overhead condenser 27 after solvent heat exchange, condensate liquid to organic solvent tank field L2；Organic solvent feed preheater
26 condensate liquid is to organic solvent tank field L2；The tower reactor liquid phase of low pressure organic solvent rectifying column 24 is divided to two strands, and one passes through lower pressure column
Kettle reboiler 31 returns to low pressure organic solvent rectifying column 24 after evaporating, another stock-traders' know-how is crossed after the pressurization of the 3rd pump 37 enter in be pressed with machine
Solvent rectifying column 23 continues rectifying；Recirculated cooling water from recirculated cooling water tank field E2 is as low pressure overhead condenser 27
Low-temperature receiver, recirculated water backwater tank field F2 is passed through after cooling；From raw steam tank field B2 life steam as the first high pressure tower reactor again
The thermal source of the high pressure tower reactor reboiler 29 of device 28 and second is boiled, raw steam condensate tank field H is passed through after heat exchange.
Produce 100kt Caprolactam unit per year for Shandong, the quality group of waste water raw material turns into：Water content 99.9%, toluene
Content 0.0301%, cyclohexanone oxime content 0.0184%, other content of reaction byproduct 0.0515%.
Organic solvent charging tank field C organic extractant quality group turns into：Benzene content 99.4%, water content 0.1%, cyclohexanone contains
Amount 0.1%, hexamethylene alcohol content 0.1%, aniline content 0.1%, other content of reaction byproduct 0.2%.
High pressure waste water stripper operating pressure is 0.1MPaA, 91.5 DEG C of tower top temperature, 97.1 DEG C of bottom temperature, tower theoretical stage
For 15；High pressure organic solvent rectifying column operating pressure is 0.38MPaA, 130.0 DEG C of tower top temperature, 141.7 DEG C of bottom temperature,
Tower theoretical stage is 8；In to be pressed with solvent rectifying column operating pressure be 0.22MPaA, 107.4 DEG C of tower top temperature, bottom temperature
108.9 DEG C, tower theoretical stage is 8；Low pressure organic solvent rectifying column operating pressure is 0.1MPaA, 79.6 DEG C of tower top temperature, tower
87.3 DEG C of kettle temperature degree, tower theoretical stage are 8.
Through said process, each tower top tower kettle discharging reaches factory's processing requirement.Because the technique considers sufficient thermal coupling, respectively
(thermic load is heated or cooled for what is saved in bracket) in the load of tower such as table 4：
Table 4
| Cool down load/KW | Heating load/KW | Total/KW | |
| High pressure waste water stripper | 3300 | 3500 | 6800 |
| High pressure organic solvent rectifying column | (2833) | 3159 | 3159(5992) |
| In be pressed with solvent rectifying column | (2555) | (2775) | (5330) |
| Low pressure organic solvent rectifying column | 2125 | (2300) | 2125(4425) |
| It is total | 2125(7513) | 3159(8234) | 5284(15747) |
The high pressure waste water stripper of the present embodiment and organic solvent rectifying column isolated operation, organic solvent rectifying column use senior middle school's low pressure
Three-effect rectification, when not coupling, the total heating load of its each tower is 8234KW, condensation load 7513KW, total thermic load
For 15747KW；After coupling, the total heating load of each tower is 3159KW, condensation load 2125KW, total thermic load
For 5284KW；Heating load energy-conservation 61.6%, condensation load energy-conservation 71.7%, total thermic load energy-conservation 66.4%.
The present embodiment is not coupled completely, has only been carried out triple effect coupling rectification to organic solvent rectifying column, save considerably organic
The energy consumption of solvent recovery, the system have the advantages of operation is flexible, and the free degree is big, easily operated.
The method and device of Non-energy-consumption recovery caprolactam organic extractant proposed by the present invention, is entered by preferred embodiment
Gone description, person skilled can substantially do not depart from present invention, in spirit and scope to methods described herein and device
It is modified or suitably changes combination to realize the technology of the present invention.In particular, all similar replacements or change
It is apparent to one skilled in the art, it can all be considered as bag in spirit of the invention, scope and content.
Claims (3)
1. a kind of device of Non-energy-consumption recovery caprolactam organic extractant, including high pressure waste water stripper (1), high pressure organic solvent essence
Evaporate tower (2), in be pressed with solvent rectifying column (3), low pressure organic solvent rectifying column (4), wastewater feed preheater (5), have
Solvent feed preheater (6), low pressure overhead condenser (7), the first high pressure tower reactor reboiler (8), the second high pressure tower reactor are again
Boil device (9), medium pressure column kettle reboiler (10), low pressure tower reactor reboiler (11), phase separation tank (12), organic solvent discharging cooling
Device (13), high pressure tower top auxiliary condenser (14), the first pump (15)；It is characterized in that：(A) passes through pipeline for wastewater feed tank field
The top with wastewater feed preheater (5) and high pressure waste water stripper (1) is connected successively, the top of high pressure waste water stripper (1)
Portion divides two-way after being connected by pipeline with high pressure tower top auxiliary condenser (14), all the way successively with the second high pressure tower reactor reboiler (9)
Connected with phase separation tank (12), another way is directly connected with phase separation tank (12)；The top of phase separation tank (12) is by pipeline with giving up
Water organic solvent tank field (I) connects, the bottom of phase separation tank (12) by pipeline successively with the first pump (15) and high pressure waste water vapour
The top connection of stripper (1)；The bottom of high pressure waste water stripper (1) by pipeline respectively with the first high pressure tower reactor reboiler (8)
Bottom connected with wastewater feed preheater (5) shell side inlet；The top of first high pressure tower reactor reboiler (8) by pipeline with
The bottom connection of high pressure waste water stripper (1)；Wastewater feed preheater (5) shell-side outlet passes through pipeline and wastewater treatment working section
(G) connect；Organic solvent charging tank field (C) is connected the roads of Hou Fen tri- point by pipeline with organic solvent feed preheater (6)
Not with high pressure organic solvent rectifying column (2), in be pressed with the upper of solvent rectifying column (3) and low pressure organic solvent rectifying column (4)
Portion connects, the top of high pressure organic solvent rectifying column (2) by pipeline successively with medium pressure column kettle reboiler (10), organic solvent
Discharge after cooler (13) connection, then be connected with organic solvent tank field (L)；The bottom of high pressure organic solvent rectifying column (2)
By pipeline respectively with the bottom of the second high pressure tower reactor reboiler (9) and in be pressed with the middle part of solvent rectifying column (3) and be connected,
The top of second high pressure tower reactor reboiler (9) is connected by pipeline with the bottom of high pressure organic solvent rectifying column (2)；In be pressed with
The top of solvent rectifying column (3) by pipeline successively with low pressure tower reactor reboiler (11), organic solvent discharge cooler (13)
Connection and organic solvent tank field (L) connection；In be pressed with the bottom of solvent rectifying column (3) by pipeline respectively with medium pressure column kettle
Reboiler (10) connects with the middle part of low pressure organic solvent rectifying column (4), passes through pipe at the top of medium pressure column kettle reboiler (10)
The bottom that road is pressed with solvent rectifying column (3) with is connected；The top of low pressure organic solvent rectifying column (4) is by pipeline with having
The shell side inlet connection of solvent feed preheater (6), the shell side vapor phase exit of organic solvent feed preheater (6) pass through pipe
Road is connected with the shell side inlet of low pressure overhead condenser (7), and the shell side liquid-phase outlet of organic solvent feed preheater (6) passes through
Pipeline is connected with organic solvent tank field (L), and the shell-side outlet of low pressure overhead condenser (7) passes through pipeline and organic solvent tank field
(L) connect；The bottom of low pressure organic solvent rectifying column (4) passes through the pipeline bottom with low pressure tower reactor reboiler (11) respectively
Connected with organic solvent heavy constituent separator (K), the top of low pressure tower reactor reboiler (11) is organic with low pressure by pipeline
The bottom connection of solvent rectifying column (4)；The shell side import of organic solvent discharging cooler (13) passes through pipeline and caprolactam water
Solution tank field (D) connects, and the shell-side outlet of organic solvent discharging cooler (13) passes through pipeline and caprolactam refining workshop section
(M) connect；Raw steam tank field (B) by pipeline respectively with first high pressure tower reactor reboiler (8) shell side inlet, second high
Press the shell side inlet connection of tower reactor reboiler (9)；The shell-side outlet and the second high pressure tower reactor of first high pressure tower reactor reboiler (8)
Reboiler (9) shell-side outlet is connected by pipeline with raw steam condensate tank field (H) respectively；Recirculated cooling water tank field (E)
After being connected by pipeline with the tube side of low pressure overhead condenser (7), it is connected with recirculated water backwater tank field (F).
2. a kind of device of Non-energy-consumption recovery caprolactam organic extractant, including high pressure waste water stripper (21), high pressure organic solvent essence
Evaporate tower (22), in be pressed with solvent rectifying column (23), low pressure organic solvent rectifying column (24), wastewater feed preheater (25),
Organic solvent feed preheater (26), low pressure overhead condenser (27), the first high pressure tower reactor reboiler (28), the second high-pressure tower
Kettle reboiler (29), medium pressure column kettle reboiler (30), low pressure tower reactor reboiler (31), phase separation tank (32), organic solvent go out
Expect cooler (33), high pressure tower top auxiliary condenser (34), the first pump (35), the second pump (36), the 3rd pump (37)；Its
It is characterized in：Wastewater feed tank field (A2) by pipeline successively with wastewater feed preheater (25) and high pressure waste water stripper (21)
Top connection, the top of high pressure waste water stripper (21) is divided after being connected by pipeline with high pressure tower top auxiliary condenser (34)
Two-way, it is connected successively with the second high pressure tower reactor reboiler (29) and phase separation tank (32) all the way；Another way directly with phase separation tank (32)
Connection；The top of phase separation tank (32) is connected by pipeline with waste water organic solvent tank field (I2)；The bottom of phase separation tank (32)
After being connected by pipeline with the first pump (35), it is connected with the top of high pressure waste water stripper (21)；High pressure waste water stripper (21)
Bottom pass through the pipeline bottom with the first high pressure tower reactor reboiler (28) and wastewater feed preheater (25) shell side inlet respectively
Connection；The top of first high pressure tower reactor reboiler (28) is connected by pipeline with the bottom of high pressure waste water stripper (21)；It is useless
Water feed preheater (25) shell-side outlet is connected by pipeline with wastewater treatment working section (G2)；Organic solvent feeds tank field (C2)
Be connected by pipeline with organic solvent feed preheater (26) tunnels of Hou Fen tri- respectively with high pressure organic solvent rectifying column (22), middle pressure
The top connection of organic solvent rectifying column (23), low pressure organic solvent rectifying column (24), high pressure organic solvent rectifying column (22)
Top by pipeline successively with medium pressure column kettle reboiler (30), organic solvent discharge cooler (33) be connected after, then with it is organic
Vent tank farm (L2) connects；Boiled again with the second high pressure tower reactor respectively by pipeline the bottom of high pressure organic solvent rectifying column (22)
The bottom of device (29) and organic solvent heavy constituent separator (K2) connection；The top of second high pressure tower reactor reboiler (29)
It is connected by pipeline with the bottom of high pressure organic solvent rectifying column (22)；In be pressed with the top of solvent rectifying column (23) and pass through
Pipeline successively with low pressure tower reactor reboiler (31), organic solvent discharging cooler (33) be connected after, then with organic solvent tank field (L2)
Connection；In be pressed with the bottom of solvent rectifying column (23) by pipeline respectively with the bottom of medium pressure column kettle reboiler (30) and
Two pumps (36) are connected, and the second pump (36) is connected by pipeline with the middle part of high pressure organic solvent rectifying column (22)；Medium pressure column
The bottom that the top of kettle reboiler (30) is pressed with solvent rectifying column (23) by pipeline with is connected；Low pressure organic solvent essence
The top for evaporating tower (24) is connected by pipeline with the shell side inlet of organic solvent feed preheater (26)；Organic solvent charging is pre-
The shell side vapor phase exit of hot device (26) is connected by pipeline with the shell side inlet of low pressure overhead condenser (27), and organic solvent enters
The shell side liquid-phase outlet of material preheater (26) is connected by pipeline with organic solvent tank field (L2)；Low pressure overhead condenser (27)
Shell-side outlet be connected by pipeline with organic solvent tank field (L2)；The bottom of low pressure organic solvent rectifying column (24) passes through pipe
Road is connected with the bottom of low pressure tower reactor reboiler (31) and the 3rd pump (37) respectively, and the 3rd pump (37) passes through pipeline and middle pressure
The middle part connection of organic solvent rectifying column (23), the top of low pressure tower reactor reboiler (31) passes through pipeline and low pressure organic solvent
The bottom connection of rectifying column (24)；The shell side import of organic solvent discharging cooler (33) is water-soluble with caprolactam by pipeline
Flow container area (D2) connects, and the shell-side outlet of organic solvent discharging cooler (33) passes through pipeline and caprolactam refining workshop section (M2)
Connection；Raw steam tank field (B2) by pipeline respectively with the first high pressure tower reactor reboiler (28) shell side inlet and the second high-pressure tower
The shell side inlet connection of kettle reboiler (29)；The shell-side outlet of first high pressure tower reactor reboiler (28) and the second high pressure tower reactor are again
The shell-side outlet of boiling device (29) is connected by pipeline with raw steam condensate tank field (H2) respectively；Recirculated cooling water tank field (E2)
After being connected by pipeline with the tube side of low pressure overhead condenser (27), it is connected with recirculated water backwater tank field (F2).
A kind of 3. method of Non-energy-consumption recovery caprolactam organic extractant, it is characterized in that comprising the following steps：
A) device of usage right requirement 1 or 2；
B) the operating pressure control of high pressure waste water stripper is in 0.1~1.0MPaA, the control of high pressure organic solvent rectifying column operating pressure
In 0.1~0.8MPaA, in be pressed with the control of solvent rectifying column operating pressure in 0.01~0.6MPaA, low pressure organic solvent rectifying
The control of tower operating pressure is higher than high pressure organic solvent rectifying tower in 0.01~0.4MPaA, high pressure waste water stripper overhead vapor (steam) temperature
5~50 DEG C of kettle kettle liquid temperature；High pressure organic solvent rectifying column tower top vapor (steam) temperature is pressed with solvent tower bottom of rectifying tower kettle liquid temperature in being higher than
5~50 DEG C of degree；In be pressed with solvent rectifying column tower top vapor (steam) temperature and be higher than low pressure organic solvent tower bottom of rectifying tower kettle liquid temperature 5~50
℃；
C) overhead vapours of high pressure waste water stripper provides thermal source for high pressure organic solvent rectifying column；
D) overhead vapours of high pressure organic solvent rectifying column is pressed with solvent rectifying column in and provides thermal source；
E) overhead vapours that solvent rectifying column is pressed with provides thermal source for low pressure organic solvent rectifying column；
F) wastewater feed of high pressure waste water stripper and high pressure waste water stripper tower reactor discharging is exchanged heat, organic solvent charging with it is low
The overhead vapours heat exchange of solvent rectifying column is pressed with, high pressure organic solvent rectifying column is pressed with the overhead vapours of solvent rectifying column with
Lime set exchanges heat with caprolactam water solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610355732.1A CN107434784A (en) | 2016-05-25 | 2016-05-25 | Non-energy-consumption reclaims the method and device of caprolactam organic extractant |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610355732.1A CN107434784A (en) | 2016-05-25 | 2016-05-25 | Non-energy-consumption reclaims the method and device of caprolactam organic extractant |
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| Publication Number | Publication Date |
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| CN107434784A true CN107434784A (en) | 2017-12-05 |
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ID=60454209
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610355732.1A Pending CN107434784A (en) | 2016-05-25 | 2016-05-25 | Non-energy-consumption reclaims the method and device of caprolactam organic extractant |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109821267A (en) * | 2019-03-29 | 2019-05-31 | 扬州惠通化工科技股份有限公司 | A kind of tetrahydrofuran recovery system |
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Application publication date: 20171205 |