CN106492495A - Improved vacuum distillation tower and acetonitrile refining system - Google Patents
Improved vacuum distillation tower and acetonitrile refining system Download PDFInfo
- Publication number
- CN106492495A CN106492495A CN201510564796.8A CN201510564796A CN106492495A CN 106492495 A CN106492495 A CN 106492495A CN 201510564796 A CN201510564796 A CN 201510564796A CN 106492495 A CN106492495 A CN 106492495A
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- CN
- China
- Prior art keywords
- vacuum distillation
- tower
- distillation tower
- acetonitrile
- stripping section
- 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.)
- Pending
Links
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 title claims abstract description 138
- 238000005292 vacuum distillation Methods 0.000 title claims abstract description 55
- 238000007670 refining Methods 0.000 title claims abstract description 10
- 238000012856 packing Methods 0.000 claims abstract description 20
- 238000004821 distillation Methods 0.000 claims description 21
- 239000000126 substance Substances 0.000 claims description 18
- 238000007255 decyanation reaction Methods 0.000 claims description 8
- 239000000945 filler Substances 0.000 claims description 4
- 208000031481 Pathologic Constriction Diseases 0.000 claims description 2
- 210000001215 vagina Anatomy 0.000 claims description 2
- LELOWRISYMNNSU-UHFFFAOYSA-N hydrogen cyanide Chemical compound N#C LELOWRISYMNNSU-UHFFFAOYSA-N 0.000 description 21
- 239000000463 material Substances 0.000 description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 8
- 230000006837 decompression Effects 0.000 description 7
- 239000012535 impurity Substances 0.000 description 7
- 238000000034 method Methods 0.000 description 7
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 239000003513 alkali Substances 0.000 description 5
- 239000000470 constituent Substances 0.000 description 4
- FVSKHRXBFJPNKK-UHFFFAOYSA-N propionitrile Chemical compound CCC#N FVSKHRXBFJPNKK-UHFFFAOYSA-N 0.000 description 4
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000007789 gas Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 150000002825 nitriles Chemical class 0.000 description 3
- PBCJIPOGFJYBJE-UHFFFAOYSA-N acetonitrile;hydrate Chemical compound O.CC#N PBCJIPOGFJYBJE-UHFFFAOYSA-N 0.000 description 2
- 150000008044 alkali metal hydroxides Chemical class 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- XLJMAIOERFSOGZ-UHFFFAOYSA-N cyanic acid Chemical compound OC#N XLJMAIOERFSOGZ-UHFFFAOYSA-N 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 230000007774 longterm Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012071 phase Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- -1 Alkene nitrile Chemical class 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 229910001860 alkaline earth metal hydroxide Inorganic materials 0.000 description 1
- 238000010533 azeotropic distillation Methods 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- NGZNCESUZDJUTH-UHFFFAOYSA-N cyanic acid;hydrate Chemical compound O.OC#N NGZNCESUZDJUTH-UHFFFAOYSA-N 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- NWJZFGOFYNPABH-UHFFFAOYSA-N prop-1-ene;prop-2-enenitrile Chemical compound CC=C.C=CC#N NWJZFGOFYNPABH-UHFFFAOYSA-N 0.000 description 1
- 125000004368 propenyl group Chemical group C(=CC)* 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of vacuum distillation tower for acetonitrile refining system, the vacuum distillation tower includes rectifying section and stripping section, wherein, arranges structured packing as rectifying section inner member in the rectifying section.According to the vacuum distillation tower of the present invention, while obtaining compared with high separating efficiency, additionally it is possible to effectively reduce tower height, save equipment investment.
Description
Technical field
The present invention relates to a kind of improved vacuum distillation tower and the acetonitrile essence using the vacuum distillation tower
System processed.
Background technology
In ammoxidation of propylene acrylonitrile production production technology, acetonitrile, hydrocyanic acid are returned as by-product
Receive.Generally using by decyanation tower, chemical treatment, decompression, pressurization azeotropic distillation group technology,
Acetonitrile is continuously reclaimed, effectively can remove water and hydrocyanic acid in acetonitrile, acrylonitrile, third
The impurity such as nitrile, propenyl.
For example, EP055920 discloses a kind of continuous technique for reclaiming acetonitrile.The technique is using essence
Evaporate the removing Light ends such as hydrocyanic acid, plus alkali and plus formaldehyde chemical treatment further remove hydrocyanic acid,
Rectification under vacuum and the method for compression rectification combined dehydration, improve the refined recovery rate of acetonitrile, can
Obtain the acetonitrile product of higher degree.But the process adds plus formaldehyde chemical treatment step, grasp
Make complicated.CN1328993A also reports a kind of continuous technique for reclaiming acetonitrile.By in tradition
Vacuum rectification tower and the rectifying section of compression rectification tower set up an alkali metal hydroxide or alkaline earth
The charging aperture of metal hydroxidess, local add alkali compoundss, using cyanalcohol in alkalescence heating
Under conditions of can decomposite free HCN, and the HCN for decompositing is easily and alkaline metal cpds
Stable compound is generated, so as to pass through the characteristic that rectification is removed, makes to decomposite in distillation process
The HCN for coming successfully can be discharged from tower bottom of rectifying tower, reach micro HCN in removing acetonitrile
Purpose.
In the prior art, for the vacuum distillation tower in acetonitrile refining system, in scale
In the case of less, using filler as inner member in tower, and in the case of larger,
Board-like tower tray is adopted in tower as inner member more.
Structured packing due to specific surface area big, pressure drop is little, fluid point uniform, mass-and heat-transfer
The advantages of efficiency high, therefore it is widely used.Particularly screen waviness packings, have
Efficiently, the advantage that pressure drop is low and flux is big, is more suitable for the rectification under vacuum for difficult separation mixture.
But containing heavy constituent and polymeric impurities in the charging of the system vacuum distillation tower, easily in charging
The blocking of structured packing is partly caused below mouthful, so as to affect the long-term operation of equipment.Therefore,
Reasonably combined column inner member, is this tower height effect, the key of stable operation.
Content of the invention
The present inventor is had found through long-term research, is made by the different tower sections in vacuum distillation tower
With different inner members, can realize reducing tower height and tower pressure drop, make plant running more stable,
The more low effect of equipment investment.
[1] a first aspect of the present invention provides a kind of improved decompression for acetonitrile refining system
Distillation column, the vacuum distillation tower include rectifying section and stripping section, wherein, in the rectifying section
Structured packing is set used as rectifying section inner member.
[2] in the vacuum distillation tower described in [1], it is preferable that the structured packing is filled out for ripple
Material.
[3] in the vacuum distillation tower described in [2], it is preferable that the ripple packing is silk screen ripple
Stricture of vagina filler.
[4] in the vacuum distillation tower described in [1], it is preferable that arranging plate in the stripping section
Formula tower tray is used as stripping section inner member.
[5] in the vacuum distillation tower described in [1], it is preferable that arrange in the stripping section and dissipate
Heap filler is used as stripping section inner member.
[6] in the vacuum distillation tower described in any one of [1]～[5], it is preferable that the decompression
Distillation column is configured with 1～60 piece of theoretical plate.
[7] in the vacuum distillation tower described in [6], it is preferable that the stripping section is configured with 1～30
Block theoretical plate.
[8] in the vacuum distillation tower described in [6], it is preferable that the rectifying section is configured with 1～30
Block theoretical plate.
[9] another aspect of the present invention provides a kind of acetonitrile refining system, including：
Decyanation tower；
Chemical treatment kettle；
[1]～[8] vacuum distillation tower described in any one；And
Distillation under pressure tower.
Invention effect
Using the vacuum distillation tower of the present invention, tower height and tower pressure drop can not only be reduced, additionally it is possible to real
The characteristics of existing equipment operation is more stable, equipment investment is lower.
Description of the drawings
Fig. 1 is the schematic diagram of the vacuum distillation tower of the present invention.
List of reference signs
1：Vacuum distillation tower
2：Vacuum distillation tower condenser
3：Vacuum distillation tower return tank
Specific embodiment
Specific embodiment below with reference to the Description of Drawings present invention.
The acetonitrile refining process of the present invention, comprises the following steps：
A) raw material crude acetonitrile is separated through decyanation tower, and the Light ends such as most of HCN are discharged by tower top,
Part water and weight Organic substance are discharged by tower reactor；
B) extracting out from decyanation tower stripping section bottom side line gas phase containing water-acetonitrile for Light ends is stripped of
Add alkali chemical treatment by chemical treatment kettle；
C) through plus the free HCN of alkali chemical treatment removing after enter vacuum distillation tower containing water-acetonitrile,
In tower reactor removing weight Organic substance；
D) the acetonitrile entrance distillation under pressure for being stripped of most of water is steamed from vacuum distillation column overhead
Tower, tower top steam aqueous acetonitrile material and return vacuum distillation tower charging, in stripping pars infrasegmentalis gas
High-purity acetonitrile is mutually extracted out.
In step a), raw material crude acetonitrile can come from any suitable source, such as from third
Alkene nitrile device acetonitrile desorbing tower top, by weight percentage, its composition can include 20～80% second
Nitrile, 1～4%HCN, 0.1～0.3% acrylonitrile, 0.3～0.7% propionitrile, 20～79% water.Raw material is thick
Acetonitrile extracts the acetonitrile containing about acetonitrile 75% out from stripping section bottom side line gas phase after decyanation column distillation
Material removes chemical treatment kettle.The actual conditions of decyanation tower is as follows：Tower top pressure be 0.10～
0.125Mpa, feeding temperature are 30～80 DEG C, and tower top drop temperature is 35～60 DEG C, stripping section
Lateral line withdrawal function temperature is 85～100 DEG C, and bottom temperature is 105～120 DEG C.
Chemical reaction kettle is entered from the acetonitrile material containing about acetonitrile 75% of decyanation tower side line is carried out
Chemical treatment, the free impurity such as hydrocyanic acid and a small amount of acrylonitrile of removing, the reaction after chemical treatment
Liquid enters vacuum distillation tower 1.In terms of chemical treatment kettle, the alkali for being added is alkali metal hydroxide
Thing or alkaline earth metal hydroxide；Preferably sodium hydroxide or potassium hydroxide；More preferably hydrogen-oxygen
Change sodium.
In terms of vacuum distillation tower 1, tower top pressure be 0.013～0.04Mpa, feeding temperature be 30～
50 DEG C, tower top temperature is 30～50 DEG C, and bottom temperature is 50～75 DEG C.
The acetonitrile for containing less moisture content from the part of the return tank of top of the tower 3 of vacuum distillation tower 1 is entered
Distillation under pressure column distillation, and acetonitrile of high purity product is obtained from distillation under pressure tower side line.In pressurization
In terms of distillation column, tower top pressure is 0.1～0.5Mpa, and feeding temperature is 30～90 DEG C, tower top temperature
To spend for 90～140 DEG C, stripping section lateral line withdrawal function temperature is 100～135 DEG C, bottom temperature is 110～
145℃.
Below with reference to the vacuum distillation tower that Fig. 1 describes the present invention in detail.
As shown in figure 1, coming from the aqueous of the chemical treatment kettle of the acetonitrile refining system of the present invention
Enter from the middle part of vacuum distillation tower 1 with the acetonitrile material 7 of heavy constituent impurity.Vacuum distillation tower 1
Pipeline connection port 8 is configured with, for receiving the raw material for entering this tower.Tower interior conduit connector 8 with
Under be configured with the board-like tower tray of polylith or random packing 5, for separation water and heavy constituent impurity；In tower
Pipeline connection port more than 8 is configured with structured packing 6, for concentrating and can obtain containing acetonitrile about 90%
Acetonitrile material 9.
Vacuum distillation tower system configuration has overhead condenser 2 and return tank 3, through vacuum distillation tower
After distillation, top gaseous phase material 9 sends into return tank 3 after sending into the condensation cooling of overhead condenser 2.
Return tank 3 is configured with pipe joint 4, and pipe joint 4 is arranged to connect pumped vacuum systems,
So that decompression Tower System obtains required vacuum.Enter an overhead condensation liquid part for return tank
10 are admitted to vacuum distillation tower overhead reflux mouth as backflow, and another part 14 sends to distillation under pressure
Tower is used as charging.Through vacuum distillation column distillation, the kettle liquid 11 of aqueous and heavy constituent impurity is from tower reactor
Discharge wastewater treatment.
The vacuum distillation tower of the present invention is configured with 1～60 piece of theoretical plate；Preferably, 10～50 are configured
Block theoretical plate；It is highly preferred that 24～36 pieces of theoretical plates of configuration.
As described above, stripping section inner member is using board-like tower tray or random packing；Preferably, subtract
Pressure distillation column stripping section inner member is using high-efficient tower plate or efficient random packing.The decompression of the present invention
Distillation column stripping section is configured with 1～30 piece of theoretical plate；Preferably, 10～20 pieces of theoretical plates are configured；
It is highly preferred that 12～18 pieces of theoretical plates of configuration.
As described above, rectifying section inner member adopts structured packing；Preferably, vacuum distillation tower essence
Evaporate a section inner member and adopt ripple packing；It is highly preferred that vacuum distillation tower rectifying section inner member is adopted
Screen waviness packings.The vacuum distillation tower rectifying section of the present invention is configured with 1～30 piece of theoretical plate；More
Preferably, 10～20 pieces of theoretical plates are configured；It is highly preferred that 12～18 pieces of theoretical plates of configuration.
Embodiment
Below by way of specific embodiment, the invention will be further elaborated.
【Embodiment 1】
With weight, the raw material crude acetonitrile containing acetonitrile 50%, hydrocyanic acid 1.5%, from
The middle part of dehydrogenation cyanic acid tower adds, and operating pressure is normal pressure, and tower top temperature is 50 DEG C, tower reactor temperature
Spend for 115 DEG C, stripping section lateral line withdrawal function temperature is 92 DEG C.Removed overhead hydrocyanic acid, stripping section
Lateral line withdrawal function concentration is that 75% acetonitrile goes chemical treatment.Add enough 40%NaOH solution
Reaction 4～6 hours.Vacuum distillation tower decompression dehydration is entered after chemical treatment and distillation under pressure tower adds
Press-dehydrating.
Vacuum distillation tower adopts 30 pieces of theoretical plates, from the second that the concentration of chemical treatment kettle is 75%
Nitrile is entered in the middle of 15～16 pieces of theoretical plates from the middle part of tower, and stripping section adopts plate spacing for 500mm's
28 pieces of light-duty float valves, rectifying section are designed with BX type screen waviness packings, 7 meters of packed height,
Tower top pressure is 0.026Mpa, and 40 DEG C of tower top temperature, 64 DEG C of bottom temperature, from vacuum distillation tower
Tower reactor excludes the impurity such as water and propionitrile, and tower top obtains the acetonitrile material that concentration is 90%.Decompression is steamed
Evaporate a column overhead material part and pass back into tower top, another part removes distillation under pressure tower.
Distillation under pressure column overhead pressure be 0.3MPa, 108 DEG C of tower top temperature, bottom temperature 125
DEG C, finished product acetonitrile is obtained from distillation under pressure tower side line.Through the refined of above flow process, finished product acetonitrile
Middle acetonitrile 99.95%, propionitrile 148ppm, water 345ppm.
【Comparative example 1】
In addition to rectifying section adopts spacing for 28 pieces of light-duty float valves of 450mm, adopt and reality
1 identical equipment of example and condition is applied, raw material crude acetonitrile is refined.As a result, obtained
Acetonitrile 99.95%, propionitrile 150ppm, water 350ppm in finished product acetonitrile.
By adopting the vacuum distillation tower of the present invention, the essentially identical acetonitrile product of quality is being obtained
In the case of, make total tower height reduce by 5 meters, the equipment investment of tower rectifying section reduces 25%.
Claims (9)
1. a kind of vacuum distillation tower for acetonitrile refining system, the vacuum distillation tower include rectification
Section and stripping section, wherein, arrange structured packing as rectifying section inner member in the rectifying section.
2. vacuum distillation tower according to claim 1, wherein, the structured packing is ripple
Stricture of vagina filler.
3. vacuum distillation tower according to claim 2, wherein, the ripple packing is silk
Corrugated wire gauze packing.
4. vacuum distillation tower according to claim 1, wherein, sets in the stripping section
Board-like tower tray is put as stripping section inner member.
5. vacuum distillation tower according to claim 1, wherein, sets in the stripping section
Random packing is put as stripping section inner member.
6. the vacuum distillation tower according to Claims 1 to 5 any one, wherein, described subtracts
Pressure distillation column is configured with 1～60 piece of theoretical plate.
7. vacuum distillation tower according to claim 6, wherein, the stripping section is configured with
1～30 piece of theoretical plate.
8. vacuum distillation tower according to claim 6, wherein, the rectifying section is configured with
1～30 piece of theoretical plate.
9. a kind of acetonitrile refining system, including：
Decyanation tower；
Chemical treatment kettle；
Vacuum distillation tower described in claim 1～8 any one；And
Distillation under pressure tower.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510564796.8A CN106492495A (en) | 2015-09-07 | 2015-09-07 | Improved vacuum distillation tower and acetonitrile refining system |
| KR1020160109226A KR102256553B1 (en) | 2015-08-26 | 2016-08-26 | Method for refining acetonitrile, system thereof, and method for reutilizing acid waste water |
| TW105127578A TWI740840B (en) | 2015-08-26 | 2016-08-26 | Acetonitrile refining method, acetonitrile refining system and acid waste water reuse method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510564796.8A CN106492495A (en) | 2015-09-07 | 2015-09-07 | Improved vacuum distillation tower and acetonitrile refining system |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106492495A true CN106492495A (en) | 2017-03-15 |
Family
ID=58287278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510564796.8A Pending CN106492495A (en) | 2015-08-26 | 2015-09-07 | Improved vacuum distillation tower and acetonitrile refining system |
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| Country | Link |
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| CN (1) | CN106492495A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112079405A (en) * | 2020-09-29 | 2020-12-15 | 湖北江汉石化装备有限公司 | Coking residual ammonia water negative pressure ammonia distillation energy-saving device |
| CN115177964A (en) * | 2022-06-10 | 2022-10-14 | 武汉北湖云峰环保科技有限公司 | Regeneration device and process of waste organic solvent acetonitrile |
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Cited By (2)
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| CN112079405A (en) * | 2020-09-29 | 2020-12-15 | 湖北江汉石化装备有限公司 | Coking residual ammonia water negative pressure ammonia distillation energy-saving device |
| CN115177964A (en) * | 2022-06-10 | 2022-10-14 | 武汉北湖云峰环保科技有限公司 | Regeneration device and process of waste organic solvent acetonitrile |
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