CN207267848U - 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
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- CN207267848U CN207267848U CN201721136145.XU CN201721136145U CN207267848U CN 207267848 U CN207267848 U CN 207267848U CN 201721136145 U CN201721136145 U CN 201721136145U CN 207267848 U CN207267848 U CN 207267848U
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- level
- tail
- tail cooler
- cooler
- mpd
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- 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 22
- 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
- 238000004064 recycling Methods 0.000 claims description 3
- 238000005265 energy consumption Methods 0.000 abstract description 6
- 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
- 238000001816 cooling Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 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
- 238000000605 extraction 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
- 238000010992 reflux Methods 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
- 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
- 238000003908 quality control method Methods 0.000 description 1
- 239000000985 reactive dye Substances 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
-
- 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
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- 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 vacuum 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 vacuum pump, and the evacuation process system further includes a level-one tail cooler and two two level tail coolers；The fixed gas outlet of the return tank connects with the shell side inlet of the level-one tail cooler, two two level tail coolers are arranged in parallel, the entrance that the level-one fixed gas of the level-one 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 utility model 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 utility model belongs to fine chemistry industry specialty chemicals technical field, more particularly to rectification under vacuum separation m-phenylene diamine (MPD)
During 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 at the same time, can produce o-phenylenediamine and p-phenylenediamine at the same time 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.Since 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
Heat source, after being decompressed to 4kPa, boiling point can be reduced to 205 DEG C, you can do rectifying column heat 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 from the extraction of rectifying column top return tank as shown in Figure 1, generally do not coagulate tail
Gas, but when exhaust temperature is higher can carry gaseous phase materials secretly, therefore extract out tail gas needed before vacuum pump is entered it is cold by tail cooler
Solidifying cooling, the effect of tail cooler are exactly to condense the high-temperature material in vacuum system gas bleeding and store 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 rectifying column match somebody with somebody two sets tail coolers, when the solids doses stored in a tail cooler greatly 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 is used for switching next time.Usually 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 solidification 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 usually every two days
Switch a tail cooler, not only increase the labor intensity of operating personnel for this, the rectification under vacuum system more to m-phenylene diamine (MPD) is made
Into disturbing, the quality of product is influenced, 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, and a kind of heat exchange efficiency of the utility model offer is higher, system energy
Consume 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.
Technical solution is used by the utility model solves its technical problem：
A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower, including rectifying column, overhead condenser, return tank,
Surge tank and vacuum 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 vacuum pump, and the evacuation process system further includes a level-one tail cooler and two
Two level tail cooler；The fixed gas outlet of the return tank connects with the shell side inlet of the level-one tail cooler, and two two level tails are cold
Device is arranged in parallel, and the entrance that the level-one fixed gas of the level-one 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 level-one 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 level-one tail cooler
Produce and import overhead product pipeline, exported at the top of the level-one tail cooler for level-one fixed gas, the lime set temperature of level-one 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 level-one
The level-one 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 lower part is condensate outlet, and the condensate outlet connects with recycling product pipeline
It is logical；The two level tail cooler top exit exports for level-one 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 technical concept of the utility model is：The evacuation process system of the utility model is by three common two level multi-forms
Condenser is formed.
Level-one 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 level-one tail cooler, this patent is using 105 DEG C~110 DEG C of hot water as level-one tail cooler
Cryogen, the shell side lime set of level-one tail cooler are produced by the outlet at bottom of tail cooler and import the tower top production of reflux pot bottom extraction
Quality control line.Hot water walks level-one tail cooler tube side, the adjoining pipe heat source after heat exchange as overhead product pipeline.
By controlling the cooling temperature of level-one tail cooler, most of isophthalic in return tank incoagulable gas has not only been recycled
Diamines, improves product yield；The phenylenediamine content taken in two level tail cooler is greatly reduced at the same time, 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.Level-one 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
Exchange heat into epimere coiled pipe tube side, with level-one fixed gas cocurrent, allow it to cool down rapidly.Recirculated cooling water from it is middle from top to bottom into
Enter hypomere coiled pipe tube side, exchange heat with level-one fixed gas cocurrent, also allow for its rapid cooling.
Two level tail cooler considers the thawing function of phenylenediamine material after solidification at the same time, and hypomere coiled pipe can be by recirculated cooling water
It is switched to low-pressure steam and enters tube side, can be used for material when condensate amount is larger.Epimere maintains circulating cooling water condensation at the same time
Material, avoids material from entering vacuum 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 vacuum pump, reduces the probability of damage to vacuum system.
Common m-phenylene diamine (MPD) rectification under vacuum vacuum system, need to just switch a tail cooler in every 2 days.Using the utility model
Afterwards, every 15 working days need to just switch once according to preliminary estimation.
The hot water of level-one tail cooler tube side outlet can be as the adjoining pipe heat 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 measures all big
It is big to reduce, also reduce the energy consumption of system.
The beneficial effects of the utility model are mainly manifested in：The utility model is vacuumized applied to m-phenylene diamine (MPD) rectification under vacuum
Process system, not only extends the system worked well cycle, reduces system energy consumption, improves the service life of equipment, yet
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 utility model.
Embodiment
The utility model is further described below in conjunction with the accompanying drawings.
With reference to Fig. 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), level-one tail cooler (1), two level tail cooler (2, one open one standby), surge tank (1), vacuum
Pump (1).
Level-one 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 level-one tail cooler (b) material liquid outlet and imports overhead product pipeline, level-one
Fixed gas (d) produces at the top of level-one tail cooler (b), is drawn into the middle part of two level tail cooler (c1/c2) between two sections of coiled pipes.Level-one
The lime set temperature of tail cooler is on its setting temperature, it is ensured that will not there is a phenomenon where because lime set solidify block heat exchanger.
Two level tail cooler (c1/c2) is vertical coil (or coiled pipe) heat exchanger.Heat exchanger tube divides two sections, works independently.
Level-one 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 lower part, into recycling 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 that there is a phenomenon where block heat exchanger.The utility model
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, is closed
Close hypomere recirculated cooling water inlet valve, open low-pressure steam valve, so that it is liquid from heat exchange that the solidifying material of hypomere is melted again
The material liquid outlet discharge of device bottom.Hypomere uses the low-pressure steam melting material stage, and level-one fixed gas (d) is as usual, and to be drawn into two level tail cold
Device, the heat exchanger tube of the epimere of two level tail cooler still works normally, 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 vacuum pump (f) afterwards.
When the serious frozen plug phenomenon of lime set occurs in two level tail haustorium, level-one fixed gas (d) is switched to spare two
Level tail cooler exchanges heat, and blocked tail cooler opens steam and carries out melting material, becomes new spare tail cooler after melting material.
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 vacuum 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 vacuum pump, it is characterised in that：The evacuation process system further includes a level-one tail
Cooler and two two level tail coolers；The fixed gas outlet of the return tank connects with the shell side inlet of the level-one tail cooler, and two
A two level tail cooler is arranged in parallel, and the level-one fixed gas of the level-one 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 level-one 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 for supplying the fixed gas of return tank to walk, the shell side lime set are produced from the material liquid outlet of level-one tail cooler
And overhead product pipeline is imported, exported at the top of the level-one tail cooler for level-one fixed gas, the lime set temperature of level-one 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 level-one tail is cold
The level-one 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 lower part is condensate outlet, and the condensate outlet is connected with recycling product pipeline；Institute
Two level tail cooler top exit is stated to export for level-one 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 |
|---|---|---|---|
| CN201721136145.XU CN207267848U (en) | 2017-09-06 | 2017-09-06 | A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721136145.XU CN207267848U (en) | 2017-09-06 | 2017-09-06 | A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower |
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| Publication Number | Publication Date |
|---|---|
| CN207267848U true CN207267848U (en) | 2018-04-24 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201721136145.XU Active CN207267848U (en) | 2017-09-06 | 2017-09-06 | A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower |
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| CN (1) | CN207267848U (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107501100A (en) * | 2017-09-06 | 2017-12-22 | 浙江工业大学 | A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower |
-
2017
- 2017-09-06 CN CN201721136145.XU patent/CN207267848U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107501100A (en) * | 2017-09-06 | 2017-12-22 | 浙江工业大学 | A kind of evacuation process system of m-phenylene diamine (MPD) vacuum rectification tower |
| CN107501100B (en) * | 2017-09-06 | 2024-03-22 | 浙江工业大学 | Vacuumizing process system of m-phenylenediamine vacuum rectification tower |
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