CN107501100A - A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower - Google Patents
A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower Download PDFInfo
- Publication number
- CN107501100A CN107501100A CN201710796677.4A CN201710796677A CN107501100A CN 107501100 A CN107501100 A CN 107501100A CN 201710796677 A CN201710796677 A CN 201710796677A CN 107501100 A CN107501100 A CN 107501100A
- Authority
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- China
- Prior art keywords
- level
- level tail
- tail cooler
- cooler
- mpd
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- WZCQRUWWHSTZEM-UHFFFAOYSA-N 1,3-phenylenediamine Chemical compound NC1=CC=CC(N)=C1 WZCQRUWWHSTZEM-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 229940018564 m-phenylenediamine Drugs 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000000463 material Substances 0.000 claims description 20
- 239000000498 cooling water Substances 0.000 claims description 14
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 10
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 10
- 239000004571 lime Substances 0.000 claims description 10
- 239000007788 liquid Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 239000000945 filler Substances 0.000 claims description 3
- 238000011084 recovery Methods 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 7
- 239000007789 gas Substances 0.000 description 24
- GEYOCULIXLDCMW-UHFFFAOYSA-N 1,2-phenylenediamine Chemical compound NC1=CC=CC=C1N GEYOCULIXLDCMW-UHFFFAOYSA-N 0.000 description 13
- 239000000047 product Substances 0.000 description 12
- CBCKQZAAMUWICA-UHFFFAOYSA-N 1,4-phenylenediamine Chemical compound NC1=CC=C(N)C=C1 CBCKQZAAMUWICA-UHFFFAOYSA-N 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 230000008676 import Effects 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000009835 boiling Methods 0.000 description 2
- 238000009903 catalytic hydrogenation reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000007711 solidification Methods 0.000 description 2
- 230000008023 solidification Effects 0.000 description 2
- 150000001412 amines Chemical class 0.000 description 1
- 239000000987 azo dye Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000012043 crude product Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- DMBHHRLKUKUOEG-UHFFFAOYSA-N diphenylamine Chemical class C=1C=CC=CC=1NC1=CC=CC=C1 DMBHHRLKUKUOEG-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 239000000985 reactive dye Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000008400 supply water Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010257 thawing Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/82—Purification; Separation; Stabilisation; Use of additives
- C07C209/86—Separation
-
- 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
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower, including rectifying column, overhead condenser, return tank, surge tank and vavuum pump, the tower top outlet of the rectifying column sets overhead condenser, the overhead condenser is connected with return tank, the outlet of the surge tank is connected with the vavuum pump, and the evacuation process system also includes an one-level tail cooler and two two level tail coolers；The fixed gas outlet of the return tank connects with the shell side inlet of the one-level tail cooler, two two level tail coolers are arranged in parallel, the entrance that the one-level fixed gas of the one-level tail cooler exports respectively with two level tail cooler is connected, and the two level fixed gas outlet of two two level tail coolers connects with the surge tank entrance.The present invention provide a kind of heat exchange efficiency is higher, system energy consumption compared with school, service life of equipment is longer, improves the evacuation process system of the m-phenylene diamine (MPD) vacuum rectification tower of product yield.
Description
Technical field
The invention belongs to fine chemistry industry specialty chemicals technical field, more particularly to rectification under vacuum separation m-phenylene diamine (MPD) process
In evacuation process system.
Background technology
Diaminobenzene between m-phenylene diamine (MPD) is also referred to as, is widely used in azo dyes, fur dyes, reactive dye and vulcanization
The synthesis of the intermediate of dyestuff.Its isomer includes o-phenylenediamine and p-phenylenediamine.Catalytic hydrogenation method is to research and develop in recent years
What is gone out prepares the cleaning technology of preparing of m-phenylene diamine (MPD), and key reaction is as follows：
Catalytic hydrogenation method simultaneously, can produce o-phenylenediamine and p-phenylenediamine simultaneously in reaction generation m-phenylene diamine (MPD), so raw
Output be mixing phenylenediamine, it is necessary to by m-phenylene diamine (MPD) from mixing phenylenediamine in separate.Utilize o-phenylenediamine and p-phenylenediamine
Volatility is more than the characteristics of m-phenylene diamine (MPD), is separated o-phenylenediamine, p-phenylenediamine from mixed diphenylamines with rectificating method, tower
Bottom obtains m-phenylene diamine (MPD) crude product.Because boiling point is 287 DEG C, it is necessary to do rectifying column with 300 DEG C of conduction oils under m-phenylene diamine (MPD) normal pressure
Thermal source, after being decompressed to 4kPa, boiling point can be reduced to 205 DEG C, you can do rectifying column thermal source using 220 DEG C of conduction oils.Therefore to be real
Existing rectification under vacuum, needs vacuum pumping.
The pumped vacuum systems of conventional vacuum rectifying column does not coagulate tail as shown in figure 1, typically being extracted out from rectifying column top return tank
Gas, but gaseous phase materials can be carried when exhaust temperature is higher secretly, thus extract out tail gas needed before vavuum pump is entered it is cold by tail cooler
Solidifying cooling, the effect of tail cooler are exactly that the high-temperature material in vacuum system gas bleeding is condensed and stored wherein.When these things
When the fusing point of material is higher than vacuum pump operation temperature, material can condense into solid and block tail cooler and pipeline.Blocking amount is larger then must
Need be that rectifying column match somebody with somebody two sets tail coolers, when the solids doses stored in a tail cooler it is big to a certain extent when, switch separately
A set of tail cooler accesses vacuum system.The water vapour that the solid material stored in the tail cooler shell side changed is passed through by tube side
Open, collect product and cleaning equipment uses for switching next time.Generally it need to just switch once within every two days.
Current m-phenylene diamine (MPD) rectification under vacuum vacuum system only has one group of tail cooler (one open one standby), due to phenylenediamine freezing point
It is higher, solid-state is easily congealed into tail cooler, blocks tail cooler, the heat exchange efficiency of tail cooler is reduced, one can be caused when serious
Divide phenylenediamine to be drawn into vacuum pump set, trigger system shutdown.In order to protect vacuum pump set, manufacturing enterprise just needs for generally every two days
Switch a tail cooler, the labor intensity of operating personnel is not only increased for this, the rectification under vacuum system more to m-phenylene diamine (MPD) is made
Into disturbing, the quality of product is influenceed, more increases the energy consumption of vacuum system.
The content of the invention
In order to overcome the heat exchange efficiency for vacuumizing mode of existing m-phenylene diamine (MPD) vacuum rectification tower is relatively low, system energy consumption compared with
Greatly, service life of equipment is shorter, influences the deficiency of product yield, the present invention provide a kind of heat exchange efficiency is higher, system energy consumption compared with
School, service life of equipment is longer, improves the evacuation process system of the m-phenylene diamine (MPD) vacuum rectification tower of product yield.
The technical solution adopted for the present invention to solve the technical problems is：
A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower, including rectifying column, overhead condenser, return tank,
Surge tank and vavuum pump, the tower top outlet of the rectifying column set overhead condenser, and the overhead condenser is connected with return tank,
The outlet of the surge tank is connected with the vavuum pump, and the evacuation process system also includes an one-level tail cooler and two
Two level tail cooler；The fixed gas outlet of the return tank connects with the shell side inlet of the one-level tail cooler, and two two level tails are cold
Device is arranged in parallel, and the entrance that the one-level fixed gas of the one-level tail cooler is exported respectively with two level tail cooler is connected, described in two
The two level fixed gas outlet of two level tail cooler connects with the surge tank entrance；
The one-level tail cooler is horizontal fixed tube sheet type heat exchanging, and the horizontal fixed tube sheet type heat exchanging includes heat supply
Water does the tube side that cryogen is walked and the shell side for supplying the fixed gas of return tank to walk, material liquid outlet of the shell side lime set from one-level tail cooler
Produce and import overhead product pipeline, exported at the top of the one-level tail cooler for one-level fixed gas, the lime set temperature of one-level tail cooler
Degree is on its setting temperature；
The two level tail cooler is vertical coil heat exchanger, and the vertical coil heat exchanger divides two sections, the one-level
The one-level fixed gas outlet of tail cooler is changed with two sections heat exchanger tube respectively with connecting in the middle part of the two level tail cooler
Heat, condensation, the material mouth of the two level tail cooler bottom is condensate outlet, and the condensate outlet connects with recovery product pipeline
It is logical；The two level tail cooler top exit exports for one-level fixed gas.
Further, the two level tail cooler uses recirculated cooling water as cryogen；Recirculated cooling water is from two level tail cooler
Portion enters epimere coiled pipe tube side, enters hypomere coiled pipe tube side from top to bottom from bottom to top.
Further, low-pressure steam is incorporated to two level tail cooler hypomere recirculated cooling water pipeline.
Further, the inner cavity top of the two level tail cooler sets one section may be drawn into the liquid of vacuum system to remove
The filler of drop.
The present invention technical concept be：The evacuation process system of the present invention is by three common two level multi-form condenser structures
Into.
One-level tail cooler is horizontal fixed tube sheet type condenser, to ensure rectifying tower top fixed gas under current operation pressure
Will not occur the phenomenon of condensate in one-level tail cooler, this patent is using 105 DEG C~110 DEG C of hot water as one-level tail cooler
Cryogen, the shell side lime set of one-level tail cooler are produced by the outlet at bottom of tail cooler and import the tower top production of backflow pot bottom extraction
QC line.Hot water walks one-level tail cooler tube side, the adjoining pipe thermal source after heat exchange as overhead product pipeline.
By controlling the chilling temperature of one-level tail cooler, most of isophthalic in return tank incoagulable gas has not only been reclaimed
Diamines, improve product yield；The phenylenediamine content taken in two level tail cooler is greatly reduced simultaneously, so as to extend two level
The cycle of tail cooler normal work, that is, extend the normal work cycle of m-phenylene diamine (MPD) rectifier unit.
Two level tail cooler is vertical two-part coil condenser.Two sections of coiled pipes are set to condense the benzene two in fixed gas rapidly
Amine.One-level fixed gas enters the middle part of two sections of vertical two level tail coolers, is condensed in shell side.Recirculated cooling water from it is middle from bottom to top
Exchanged heat into epimere coiled pipe tube side, with one-level fixed gas cocurrent, allow it to cool down rapidly.Recirculated cooling water enters from top to bottom from centre
Enter hypomere coiled pipe tube side, exchanged heat with one-level fixed gas cocurrent, also allow for its rapid cooling.
Two level tail cooler considers the thawing function of phenylenediamine material after solidification simultaneously, and hypomere coiled pipe can be by recirculated cooling water
Switch to low-pressure steam to enter tube side, can be used for material when condensate amount is larger.Epimere maintains circulating cooling water condensation simultaneously
Material, material is avoided to enter vavuum pump, so as to also extend the system normal operation cycle.
Two level tail cooler upper space (two level fixed gas outlet lower section) sets one section of structured packing, has further blocked not
Phenylenediamine material in solidifying gas is drawn into vavuum pump, reduces the probability of damage to vacuum system.
Common m-phenylene diamine (MPD) rectification under vacuum vacuum system, it need to just switch a tail cooler within every 2 days.After the present invention,
Every 15 working days need to just switch once according to preliminary estimation.
The hot water of one-level tail cooler tube side outlet can be as the adjoining pipe thermal source of overhead product pipeline；Needed for two level tail cooler
Thermic load is relatively low, reduces the energy consumption of cooling tower indirectly；Meanwhile switching steam melts the time of solid-state phenylenediamine and measured all big
It is big to reduce, also reduce the energy consumption of system.
Beneficial effects of the present invention are mainly manifested in：The present invention is applied to m-phenylene diamine (MPD) rectification under vacuum evacuation process system
System, not only extends the system worked well cycle, reduces system energy consumption, improve the service life of equipment, also also improve
Product yield.
Brief description of the drawings
Fig. 1 is the schematic diagram of existing m-phenylene diamine (MPD) vacuum rectification tower evacuation process system.
Fig. 2 is the schematic diagram of the m-phenylene diamine (MPD) vacuum rectification tower evacuation process system of the present invention.
Embodiment
The invention will be further described below in conjunction with the accompanying drawings.
Reference picture 2, a kind of m-phenylene diamine (MPD) vacuum rectification tower evacuation process system, including rectifying column (1), overhead condensation
Device (1), return tank (1), one-level tail cooler (1), two level tail cooler (2, one open one standby), surge tank (1), vacuum
Pump (1).
One-level tail cooler (b) is horizontal fixed tube sheet type heat exchanging.Hot water (SW) does cryogen and walks tube side, rectifier column reflux tank
Fixed gas (a) walk shell side, shell side lime set produces from one-level tail cooler (b) material liquid outlet and imports overhead product pipeline, one-level
Fixed gas (d) produces at the top of one-level tail cooler (b), is drawn into the middle part of two level tail cooler (c1/c2) between two sections of coiled pipes.One-level
The lime set temperature of tail cooler is on its setting temperature, it is ensured that will not occur to block the phenomenon of heat exchanger because of lime set solidification.
Two level tail cooler (c1/c2) is vertical coil (or coiled pipe) heat exchanger.Heat exchanger tube divides two sections, works independently.
One-level fixed gas (d) is drawn into the middle part of two level tail cooler, is exchanged heat, condensed with two sections heat exchanger tube respectively, condensation
Liquid is discharged from the material mouth of tail cooler bottom, into recovery product pipeline.Two level tail cooler is using recirculated cooling water as cryogen.Follow
Ring cooling water (CWS) enters epimere coiled pipe tube side, enters hypomere from top to bottom from bottom to top in the middle part of two level tail cooler (c1/c2)
Coiled pipe tube side.
Consider that condensate liquid may solidify in tail cooler, so as to occur to block the phenomenon of heat exchanger.The present invention will be low
Pressure steam (LS) is incorporated to two level tail cooler hypomere recirculated cooling water pipeline, when there is lime set frozen plug heat exchanger, under closing
Section recirculated cooling water inlet valve, opens low-pressure steam valve, is liquid from heat exchanger bottom so as to which the solidifying material of hypomere be melted again
Portion's material liquid outlet discharge.Hypomere uses the low-pressure steam melting material stage, and one-level fixed gas (d) is as usual to be drawn into two level tail cooler, and two
The heat exchanger tube still normal work of the epimere of level tail cooler, therefore the operation to whole system has no impact.
One section of filler is set at the top of two level tail cooler, to remove the drop that may be drawn into vacuum system.Two level fixed gas
(e) produced at the top of two level tail cooler (c1/c2), buffered tank (v) enters vavuum pump (f) afterwards.
When the serious frozen plug phenomenon of lime set occurs in two level tail haustorium, one-level fixed gas (d) is switched to standby two
Level tail cooler is exchanged heat, and blocked tail cooler opens steam and carries out melting material, and melting material turns into new standby tail cooler after terminating.
Claims (4)
1. a kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower, including it is rectifying column, overhead condenser, return tank, slow
Tank and vavuum pump are rushed, the tower top outlet of the rectifying column sets overhead condenser, and the overhead condenser is connected with return tank, institute
The outlet for stating surge tank is connected with the vavuum pump, it is characterised in that：The evacuation process system also includes an one-level tail
Cooler and two two level tail coolers；The fixed gas outlet of the return tank connects with the shell side inlet of the one-level tail cooler, and two
Individual two level tail cooler is arranged in parallel, and the one-level fixed gas of the one-level tail cooler exports the entrance phase with two level tail cooler respectively
Connect, the two level fixed gas outlet of two two level tail coolers connects with the surge tank entrance；
The one-level tail cooler is horizontal fixed tube sheet type heat exchanging, and the horizontal fixed tube sheet type heat exchanging is done including supplying hot water
The tube side that cryogen is walked and the shell side that the fixed gas of confession return tank is walked, the shell side lime set produce from the material liquid outlet of one-level tail cooler
And overhead product pipeline is imported, exported at the top of the one-level tail cooler for one-level fixed gas, the lime set temperature of one-level tail cooler exists
On its setting temperature；
The two level tail cooler is vertical coil heat exchanger, and the vertical coil heat exchanger divides two sections, and the one-level tail is cold
The one-level fixed gas of device is exported and connected in the middle part of the two level tail cooler, and exchanged heat respectively with two sections heat exchanger tube,
Condensation, the material mouth of the two level tail cooler bottom is condensate outlet, and the condensate outlet connects with recovery product pipeline；Institute
Two level tail cooler top exit is stated to export for one-level fixed gas.
2. the evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower as claimed in claim 1, it is characterised in that：The two level
Tail cooler is using recirculated cooling water as cryogen；Recirculated cooling water enters epimere coiled pipe pipe from bottom to top in the middle part of two level tail cooler
Journey, enter hypomere coiled pipe tube side from top to bottom.
3. the evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower as claimed in claim 1 or 2, it is characterised in that：Low pressure
Steam is incorporated to two level tail cooler hypomere recirculated cooling water pipeline.
4. the evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower as claimed in claim 1 or 2, it is characterised in that：It is described
The inner cavity top of two level tail cooler sets one section to remove the filler for the drop that may be drawn into vacuum system.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710796677.4A CN107501100B (en) | 2017-09-06 | 2017-09-06 | Vacuumizing process system of m-phenylenediamine vacuum rectification tower |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710796677.4A CN107501100B (en) | 2017-09-06 | 2017-09-06 | Vacuumizing process system of m-phenylenediamine vacuum rectification tower |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN107501100A true CN107501100A (en) | 2017-12-22 |
| CN107501100B CN107501100B (en) | 2024-03-22 |
Family
ID=60695683
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710796677.4A Active CN107501100B (en) | 2017-09-06 | 2017-09-06 | Vacuumizing process system of m-phenylenediamine vacuum rectification tower |
Country Status (1)
| Country | Link |
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| CN (1) | CN107501100B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111617508A (en) * | 2020-06-05 | 2020-09-04 | 滨州裕能化工有限公司 | GBL parallel flow multi-effect rectifying device |
| WO2021096421A1 (en) * | 2019-11-16 | 2021-05-20 | Polywin Pte. Ltd. | Method for purification of meta-phenylenediamine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021096421A1 (en) * | 2019-11-16 | 2021-05-20 | Polywin Pte. Ltd. | Method for purification of meta-phenylenediamine |
| CN111617508A (en) * | 2020-06-05 | 2020-09-04 | 滨州裕能化工有限公司 | GBL parallel flow multi-effect rectifying device |
| CN111617508B (en) * | 2020-06-05 | 2022-02-08 | 滨州裕能化工有限公司 | GBL parallel flow multi-effect rectifying device |
Also Published As
| Publication number | Publication date |
|---|---|
| CN107501100B (en) | 2024-03-22 |
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