CN208726769U - A kind of solvent recovery unit - Google Patents
A kind of solvent recovery unit Download PDFInfo
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- CN208726769U CN208726769U CN201821173596.5U CN201821173596U CN208726769U CN 208726769 U CN208726769 U CN 208726769U CN 201821173596 U CN201821173596 U CN 201821173596U CN 208726769 U CN208726769 U CN 208726769U
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- Prior art keywords
- tower
- column
- rectifying column
- reboiler
- phase separation
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- 238000011084 recovery Methods 0.000 title claims abstract description 20
- 239000002904 solvent Substances 0.000 title claims abstract description 15
- 238000004821 distillation Methods 0.000 claims abstract description 31
- 238000005191 phase separation Methods 0.000 claims description 26
- 238000007599 discharging Methods 0.000 claims description 19
- 238000010992 reflux Methods 0.000 claims description 11
- 239000011552 falling film Substances 0.000 claims description 3
- 238000009833 condensation Methods 0.000 abstract description 8
- 230000005494 condensation Effects 0.000 abstract description 8
- DKGAVHZHDRPRBM-UHFFFAOYSA-N Tert-Butanol Chemical compound CC(C)(C)O DKGAVHZHDRPRBM-UHFFFAOYSA-N 0.000 description 55
- VEZUQRBDRNJBJY-UHFFFAOYSA-N cyclohexanone oxime Chemical compound ON=C1CCCCC1 VEZUQRBDRNJBJY-UHFFFAOYSA-N 0.000 description 20
- 238000000034 method Methods 0.000 description 18
- JHIVVAPYMSGYDF-UHFFFAOYSA-N cyclohexanone Chemical compound O=C1CCCCC1 JHIVVAPYMSGYDF-UHFFFAOYSA-N 0.000 description 14
- 239000007788 liquid Substances 0.000 description 14
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 239000007795 chemical reaction product Substances 0.000 description 7
- 239000012071 phase Substances 0.000 description 7
- 238000004064 recycling Methods 0.000 description 6
- 229910021529 ammonia Inorganic materials 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000007792 gaseous phase Substances 0.000 description 3
- 230000007062 hydrolysis Effects 0.000 description 3
- 238000006460 hydrolysis reaction Methods 0.000 description 3
- 239000007791 liquid phase Substances 0.000 description 3
- 238000002156 mixing Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 150000002923 oximes Chemical class 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- CSKROPPOPPCYRH-UHFFFAOYSA-N cyclohexanone;hydrate Chemical compound O.O=C1CCCCC1 CSKROPPOPPCYRH-UHFFFAOYSA-N 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The utility model provides a kind of solvent recovery unit, including first rectifying column, Second distillation column, the first reboiler and condenser system；The tower reactor of the first rectifying column is connected with the Second distillation column；First reboiler is connected with the tower top of the tower reactor of the first rectifying column and the Second distillation column respectively；The condenser system is connected with the first rectifying column, and a current return circuit is provided between the condenser system and the first rectifying column.The recyclable device of one embodiment of the utility model, can make full use of the latent heat of vapor condensation, reduces steam consumption.
Description
Technical field
The utility model relates to solvent recovery unit, specially one kind can be used for recycling tertiary fourth in cyclohexanone oxamidinating technique
The device of alcohol.
Background technique
Cyclohexanone oxamidinating reaction uses the tert-butyl alcohol for solvent, and reaction product is to contain cyclohexanone oxime, the tert-butyl alcohol, ammonia and water
Mixed solution.Industrial at present, the recycling of the tert-butyl alcohol uses single tower distillation technique, but there is a problem of that steam consumption is high.
Patent application CN 103214346A propose use three-effect rectification technique, using previous effect rectifying tower top gaseous phase as
The heat source of latter effect rectifying tower reboiler, steam consumed by the technique is about the 45%~65% of single tower distillation technique.But
The process requirement meets a heat transfer temperature difference for imitating tower and two effect towers, two effect towers and triple effect tower cross-exchange, so that an effect tower is to add
The problem of pressure tower, bottom temperature are excessively high, easily lead to the hydrolytic condensation of cyclohexanone oxime, and an effect tower contains ammonia, and cyclohexanone oxime hydrolyzes
It is more serious.
Patent application CN 105126374A discloses a kind of tertiary butanol and water-cyclohexanone oxime differential pressure rectification process, the technique
Using two-tower process, a tower positive pressure operation, two tower negative-pressure operations, reaction product is divided into two strands, in 1.25:1 ratio respectively with
It is sent into a tower and two towers after one column overhead steam and tower tower reactor discharging heat exchange, the consumed quantity of steam of the technique is single tower distillation
40%~55%.But in the technique, since a column overhead steam contains ammonia, to reach the temperature difference required with the charging heat exchange of two towers,
It needs to pressurize to a tower, causes bottom temperature higher, at such a temperature, cyclohexanone oxime has hydrolysis, condensation, is difficult to realize
Industrial application.
Utility model content
One main purpose of the utility model is to provide a kind of solvent recovery unit, including first rectifying column, second
Rectifying column, the first reboiler and condenser system；The tower reactor of the first rectifying column is connected with the Second distillation column；Described
One reboiler is connected with the tower top of the tower reactor of the first rectifying column and the Second distillation column respectively；The condenser system and institute
It states first rectifying column to be connected, a current return circuit is provided between the condenser system and the first rectifying column.
According to one embodiment of the utility model, described device includes the first phase separation tank and is connected with first phase separation tank
Discharging pump, first phase separation tank and the discharging pump are set to the current return circuit.
According to one embodiment of the utility model, described device further includes the vacuum system being sequentially connected, condenser and
Two phase separation tanks, the vacuum system are connected with first phase separation tank.
According to one embodiment of the utility model, the discharging pump respectively with the tower top of the first rectifying column, described
One phase separation tank and the condenser are connected.
According to one embodiment of the utility model, the vacuum system uses Roots vaccum pump, liquid-jet vacuum pump or liquid
Ring vacuum pump.
According to one embodiment of the utility model, first reboiler by reflux pump respectively with the condenser system,
The tower top of the Second distillation column is connected.
According to one embodiment of the utility model, the first rectifying column, Second distillation column are packed tower or plate column.
According to one embodiment of the utility model, described device includes second to be connected with the tower reactor of the Second distillation column
Reboiler.
According to one embodiment of the utility model, first reboiler, the second reboiler be heat siphon type, falling film type or
Autoclave heat exchanger.
The recyclable device of one embodiment of the utility model, can make full use of the latent heat of vapor condensation, reduces steam
Consumption.
Detailed description of the invention
Consider the detailed description of the following preferred embodiment to the utility model in conjunction with the accompanying drawings, the utility model it is each
Kind target, feature and advantage will become apparent.Attached drawing is only the exemplary diagram of the utility model, is not necessarily
It is drawn to scale.In the accompanying drawings, same appended drawing reference always shows same or similar component.Wherein:
Fig. 1 is the structural schematic diagram of the solvent recovery unit of one embodiment of the utility model；
Fig. 2 is the structural schematic diagram of the single column recyclable device of the prior art.
Specific embodiment
The exemplary embodiment for embodying the utility model features and advantages will describe in detail in the following description.It should be understood that
Be that the utility model can have various variations in different embodiments, all do not depart from the model of the utility model
It encloses, and the descriptions and illustrations are essentially for illustration purposes, rather than to limit the utility model.
One embodiment of the utility model provides a kind of solvent recovery unit, can be used in cyclohexanone oxamidinating technique returning
Receive the tert-butyl alcohol.As shown in Figure 1, solvent recovery unit includes first rectifying column 1, Second distillation column 9, the first reboiler 10 and condensation
System 2；Wherein, the tower reactor of first rectifying column 1 is connected with Second distillation column 9, the first reboiler 10 respectively with first rectifying column 1
The tower top of tower reactor and Second distillation column 9 is connected, and condenser system 2 is connected with the tower top of first rectifying column 1, in condenser system 2 and the
A current return circuit is provided between the tower top of one rectifying column 1.
In an embodiment, cyclohexanone oxamidinating technological reaction product enters from the middle part of first rectifying column 1, the first essence
Evaporating operating pressure in tower 1 can be 0~70KPa of absolute pressure, and reaction product handles through first rectifying column 1 and is separated into tower bottoms
Body and overhead vapours.Tower reactor liquid enters the middle part of Second distillation column 9, the tower top comprising the tert-butyl alcohol under the action of discharging pump 8
Steam enters condenser system 2.
Into Second distillation column 9 liquid after processing, be further separated into overhead vapours and tower reactor liquid, overhead vapours
The shell side side for entering the first reboiler 10 after Second distillation column 9 is left, as the heat source of the first reboiler 10, tower reactor liquid discharge
Material is oxime aqueous solution.The tower reactor of Second distillation column 9 connects the second reboiler 12, and it is the hottest that steam can be used in the second reboiler 12
Source.
First reboiler 10 can be connected by reflux pump 11 with the tower top of Second distillation column 9, at the same also with condenser system 2 or
Access between person's condenser system 2 and 1 tower top of first rectifying column is connected.Steam is cold in the shell side release heat of the first reboiler 10
It coagulates for after liquid, under the action of reflux pump 11, a part enters second near tower top as the phegma of Second distillation column 9
Rectifying column 9, another part enter condenser system 2 after can mixing with the overhead vapours of first rectifying column 1.
After mixed vapour enters condenser system 2, be condensed into liquid, the liquid it is reflowable to first rectifying column 1 carry out into
One step separating treatment, the discharging recycling tert-butyl alcohol after multiple condensation, reflow treatment.
In an embodiment, recyclable device includes the first phase separation tank 3 and the discharging pump 5 that is connected with the first phase separation tank 3.The
One phase separation tank 3, discharging pump 5 are set to the current return circuit between condenser system 2 and first rectifying column 1, condenser system 2 and first point
Phase tank 3 is connected, and discharging pump 5 is connected with the tower top of first rectifying column 1.Overhead vapours are after condenser system 2 is condensed, into first
Phase separation tank 3 is further separated into gas-liquid two-phase through the first phase separation tank 3, and liquid can be back to first rectifying column by discharging pump 5
1 carries out further separating treatment, the discharging recycling tert-butyl alcohol after multiple condensation, split-phase, reflow treatment.
In an embodiment, recyclable device further includes the vacuum system 4 being sequentially connected, condenser 6 and the second phase separation tank
7, vacuum system 4 is connected with the first phase separation tank 3, discharging pump 5 can be connected with condenser 6 or with vacuum system 4, condenser 6 it
Between access be connected.Enter condenser 6 by the processing of vacuum system 4 through the isolated gas of the first phase separation tank 3 to condense, autocondensation
The mixture that device 6 is discharged enters the second phase separation tank 7, is further separated into fixed gas and liquid substance through the second phase separation tank 7, the liquid
Body substance discharges from the second phase separation tank 7 and recycles the tert-butyl alcohol.In addition, from the liquid that the first phase separation tank 3 is isolated, in discharging pump 5
Under effect, after a part of reflowable material to discharge to first rectifying column 1, another part and vacuum system 4 mixes, entrance is cold
Condenser 6.
In an embodiment, vacuum system 4 is using Roots vaccum pump, liquid-jet vacuum pump or liquid-ring vacuum pump.
In an embodiment, first rectifying column 1, Second distillation column 9 are packed tower or plate column.
In an embodiment, the first reboiler 10, the second reboiler 12 are heat siphon type, falling film type or autoclave heat exchange
Device.
Ammoximation reaction product when operation, is sent into the first essence by the solvent recovery unit of one embodiment of the utility model
1 middle part of tower is evaporated, later, overhead vapours enter condenser system 2, and condensed material is divided into gas-liquid two-phase in the first phase separation tank 3,
Gas phase be sent into vacuum system 4, reflux of the liquid phase through 5 pressure-raising rear portion of discharging pump as first rectifying column 1, rest part with very
Cooling in condenser 6 after the 4 discharging mixing of empty set system, then split-phase, gas phase are fixed gas in the second phase separation tank 7, and liquid phase is
Recycle the tert-butyl alcohol；
1 tower reactor of first rectifying column is sent into 9 middle part of Second distillation column after 8 pressure-raising of discharging pump, and top gaseous phase is sent into the first essence
The 10 shell side side of the first reboiler of 1 tower reactor of tower is evaporated, condensed liquid phase is used as the second rectifying through 11 pressure-raising of reflux pump, a part
The reflux of tower 9, rest part are sent into condenser system 2 after mixing with 1 top gaseous phase of first rectifying column, and 9 tower reactor of Second distillation column goes out
Material is oxime aqueous solution.
In an embodiment, the tower top temperature of first rectifying column 1 can for 65 DEG C, bottom temperature can be 75 DEG C.
The solvent recovery unit of one embodiment of the utility model, low energy consumption, and steam consumption can be the 40% of single column technique
~60%.
The solvent recovery unit of one embodiment of the utility model, can reduce bottom temperature, so that the hydrolysis of cyclohexanone oxime
Degree is low, suitable with existing commercial plant, ensure that the yield of cyclohexanone oxime.
The solvent recovery unit of one embodiment of the utility model, for recycling the tert-butyl alcohol in cyclohexanone oxamidinating technique,
The energy consumption in tert-butyl alcohol removal process is not only reduced, and the hydrolysis of cyclohexanone oxime, thermal condensation can be prevented, guarantees cyclohexanone
The yield of oxime.
Hereinafter, by the embodiment of the recycling tert-butyl alcohol in cyclohexanone oxamidinating technique to one embodiment of the utility model
The use of solvent recovery unit is described further.
Embodiment
It is carried out in the present embodiment device shown in Fig. 1, related component, technological parameter include:
Ammoximation reaction product is sent into first rectifying column 1, feed composition are as follows: cyclohexanone oxime~the 20wt% ,~tert-butyl alcohol
39wt% ,~water 38wt% ,~ammonia 3wt%.Control 1 tower top pressure of first rectifying column be 0.6bar (a), 65 DEG C of tower top temperature,
75 DEG C of bottom temperature, reflux ratio 0.2；Control 9 tower top pressure of Second distillation column is 1.5bar (a), 95 DEG C of tower top temperature, tower reactor
110 DEG C of temperature, reflux ratio 0.8.
Concrete outcome is shown in Table 1.
1 tert-butyl alcohol recovery system energy consumption of table
Comparative example
The comparative example carries out in the single column recyclable device described in Fig. 2, the device include recovery tower 101, condenser system 20,
Return tank 30, reflux pump 40, reboiler 50.
Ammoximation reaction product is sent into 101 middle part of tert-butyl alcohol recovery tower, feed composition are as follows: cyclohexanone oxime~20wt% ,~
Tert-butyl alcohol 39wt% ,~water 38wt% ,~ammonia 3wt%.101 pressure of recovery tower be 1.06bar (a), 80 DEG C of tower top temperature, tower reactor
106 DEG C of temperature, reflux ratio 0.5.
Concrete outcome is shown in Table 2.
2 tert-butyl alcohol single column recovery process energy consumption of table
As can be seen from the above Examples and Comparative Examples, compared with tert-butyl alcohol single column recovery process, the utility model is implemented
Energy consumption in example reduces~49%, and 9 bottom temperature of Second distillation column is suitable with single column technique, has both realized energy-efficient purpose,
In turn ensure the yield of cyclohexanone oxime.
Unless limited otherwise, term used in the utility model is the normally understood meaning of those skilled in the art.
Embodiment described in the utility model is merely for exemplary purpose, not to limit the guarantor of the utility model
Range is protected, those skilled in the art can make various other replacements, changes and improvements in the scope of the utility model, thus,
The present invention is not limited to the above embodiments, and is only defined by the claims.
Claims (9)
1. a kind of solvent recovery unit characterized by comprising
First rectifying column；
Second distillation column, the tower reactor of the first rectifying column are connected with the Second distillation column；
First reboiler is connected with the tower top of the tower reactor of the first rectifying column and the Second distillation column respectively；And
Condenser system is connected with the first rectifying column, is provided with one between the condenser system and the first rectifying column
Current return circuit.
2. the apparatus according to claim 1, which is characterized in that be connected including the first phase separation tank and with first phase separation tank
Discharging pump, first phase separation tank and the discharging pump are set to the current return circuit.
3. the apparatus of claim 2, which is characterized in that further include the vacuum system being sequentially connected, condenser and
Two phase separation tanks, the vacuum system are connected with first phase separation tank.
4. device according to claim 3, which is characterized in that the discharging pump tower with the first rectifying column respectively
Top, first phase separation tank and the condenser are connected.
5. device according to claim 3, which is characterized in that the vacuum system is true using Roots vaccum pump, injecting type
Sky pump or liquid-ring vacuum pump.
6. the apparatus according to claim 1, which is characterized in that first reboiler by reflux pump respectively with it is described cold
Solidifying system, the tower top of the Second distillation column are connected.
7. device according to any one of claim 1 to 6, which is characterized in that the first rectifying column, Second distillation column
For packed tower or plate column.
8. device according to any one of claim 1 to 6, which is characterized in that including the tower with the Second distillation column
The second connected reboiler of kettle.
9. device according to claim 8, which is characterized in that first reboiler, the second reboiler be heat siphon type,
Falling film type or autoclave heat exchanger.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821173596.5U CN208726769U (en) | 2018-07-24 | 2018-07-24 | A kind of solvent recovery unit |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201821173596.5U CN208726769U (en) | 2018-07-24 | 2018-07-24 | A kind of solvent recovery unit |
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| Publication Number | Publication Date |
|---|---|
| CN208726769U true CN208726769U (en) | 2019-04-12 |
Family
ID=66026704
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| CN201821173596.5U Active CN208726769U (en) | 2018-07-24 | 2018-07-24 | A kind of solvent recovery unit |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111138246A (en) * | 2019-12-30 | 2020-05-12 | 聊城鲁西聚酰胺新材料科技有限公司 | Energy-saving process for recycling tertiary butanol in ammoximation reaction |
| CN114681942A (en) * | 2020-12-28 | 2022-07-01 | 天津市华瑞奕博化工科技有限公司 | Tert-butyl alcohol recovery complete variable-voltage coupling rectification device and rectification method |
-
2018
- 2018-07-24 CN CN201821173596.5U patent/CN208726769U/en active Active
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111138246A (en) * | 2019-12-30 | 2020-05-12 | 聊城鲁西聚酰胺新材料科技有限公司 | Energy-saving process for recycling tertiary butanol in ammoximation reaction |
| CN111138246B (en) * | 2019-12-30 | 2023-06-27 | 聊城鲁西聚酰胺新材料科技有限公司 | Energy-saving process for recovering tert-butanol through ammoximation reaction |
| CN114681942A (en) * | 2020-12-28 | 2022-07-01 | 天津市华瑞奕博化工科技有限公司 | Tert-butyl alcohol recovery complete variable-voltage coupling rectification device and rectification method |
| 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 |
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Effective date of registration: 20240914 Address after: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee after: CHINA PETROLEUM & CHEMICAL Corp. Country or region after: China Patentee after: Sinopec Petrochemical Research Institute Co.,Ltd. Address before: 100728 No. 22 North Main Street, Chaoyang District, Beijing, Chaoyangmen Patentee before: CHINA PETROLEUM & CHEMICAL Corp. Country or region before: China Patentee before: RESEARCH INSTITUTE OF PETROLEUM PROCESSING, SINOPEC |