CN110003054A - A kind of water scavenging system and water-eliminating method of phosgenation production isocyanate plant - Google Patents

A kind of water scavenging system and water-eliminating method of phosgenation production isocyanate plant Download PDF

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Publication number
CN110003054A
CN110003054A CN201910237026.0A CN201910237026A CN110003054A CN 110003054 A CN110003054 A CN 110003054A CN 201910237026 A CN201910237026 A CN 201910237026A CN 110003054 A CN110003054 A CN 110003054A
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China
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tower
solvent
reactor
phosgene
phosgenation
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CN201910237026.0A
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CN110003054B (en
Inventor
岳永峰
马海洋
王京奎
曹友念
陈毅峰
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Wanhua Chemical Group Co Ltd
Wanhua Chemical Ningbo Co Ltd
Wanhua Chemical Fujian Co Ltd
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Wanhua Chemical Group Co Ltd
Wanhua Chemical Ningbo Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C263/00Preparation of derivatives of isocyanic acid
    • C07C263/10Preparation of derivatives of isocyanic acid by reaction of amines with carbonyl halides, e.g. with phosgene
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C263/00Preparation of derivatives of isocyanic acid
    • C07C263/18Separation; Purification; Stabilisation; Use of additives
    • C07C263/20Separation; Purification
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00Systems containing only non-condensed rings
    • C07C2601/12Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/14The ring being saturated

Abstract

The present invention discloses the water scavenging system and water-eliminating method of a kind of phosgenation production isocyanate plant.It is driven initial stage by producing isocyanate plant in phosgenation, is operated in water scavenging system using solvent, in a solvent by moisture remaining in system dissolution, recycled solvent, moisture is enriched with outlet.The technology can effectively reduce moisture in system, reduces moisture after feeding intake and there is corrosion of the acidic environment formed to equipment, reduces moisture and side reaction occurs for isocyanate products.It can effectively reduce the energy consumption in removal process simultaneously, shorten the solvent operating water removal time.The water scavenging system and water-eliminating method process are simple and convenient to operate, are energy-efficient.

Description

A kind of water scavenging system and water-eliminating method of phosgenation production isocyanate plant
Technical field
The invention belongs to chemical process field, it is related to a kind of process units water scavenging system and water-eliminating method, is specifically related to A kind of water scavenging system and water-eliminating method of phosgenation production isocyanate plant.
Technical background
Isocyanates is widely used in the industries such as household electrical appliances, automobile, building, shoes industry, furniture, adhesive.Existing industry metaplasia Producing isocyanate products mainly uses primary amine light phosgenation to produce: so that chlorine and reaction of carbon monoxide is generated phosgene first, secondly It reacts phosgene in a solvent with organic amine and generates isocyanates and hydrogen chloride, again by isocyanates and hydrogen chloride from solvent It separates.
Reactor, storage tank, the tower etc. of phosgenation production isocyanate plant work at high temperature under high pressure, exist because of equipment Corrode and induces the risks such as intoxication accident and fire explosion, and the presence of moisture is that equipment corrodes most important original in system Cause.
Due to containing unsaturated bond in isocyanate structural, there is high activity, reacted with water and generate amine and titanium dioxide Carbon, amine, which is further reacted with isocyanates, generates urea, and isocyanate products loss is caused to decline with quality.
Phosgenation produces isocyanate plant during normal production, is not easily introduced moisture.Moisture mainly after a stoppage, if Standby introducing system during opening maintenance etc..It is full in order to guarantee that, when phosgene enters device, device moisture can reach zone of reasonableness Sufficient production requirement, phosgenation, which produces isocyanate plant, must take moisture content in method reduction system at driving initial stage.
A kind of acrylate chemical product de-watering apparatus is disclosed in patent CN104311454A, which passes through liter Magnificent tower, condenser and with gun barrel removing by-product water is used in combination, the patent is not to grease layered effect and draining side Method is described, and package unit System drainage is not described, and the tower that distils uses packed tower, needs to pump toluene solution It is transmitted back to distillation tower to wash filler, waste of energy.
It is not yet found that technical literature discloses isocyanate plant water-eliminating method, therefore, produced for current phosgenation different The water removal of cyanic acid ester apparatus there are the problem of, need to develop a kind of efficient phosgenation production isocyanate plant water removal techniques.
Summary of the invention
Object of the present invention is to overcome the shortage of prior art, a kind of water scavenging system of phosgenation production isocyanate plant is provided And water-eliminating method.It drives initial stage in phosgenation production isocyanate plant, is operated in water scavenging system using solvent, it will be in system In a solvent, recycled solvent, moisture is enriched with outlet for remaining moisture dissolution.Both the moisture in effective removing system meets Production requirement, but it is energy-efficient, to strive for more production times for device, improve unit service factor.
In order to reach the goals above, the present invention adopts the following technical scheme:
A kind of water scavenging system of phosgenation production isocyanate plant, comprising: absorption tower 1, phosgenation reactor 2, phosgene Change reactor tower reactor reboiler 10, de- phosgene tower 3, de- phosgene tower reactor reboiler 11, solvent removal tower 4, solvent removal tower reactor again Boil device 12, solvent removal tower top cooler 15, solvent removal tower top knockout drum 8, thick solvent surge tank 6, solvent refining tower 5, solvent refining tower reactor reboiler 13, de- phosgene tower and solvent refining tower top cooler 14, de- phosgene tower and solvent refining tower top Knockout drum 9, solvent tank 7;
1 top of absorption tower be arranged absorption tower solvent feed pipe 16,1 tower reactor bottom of absorption tower by liquid phase pipeline 20 with slightly it is molten Agent surge tank 6 connects, and thick solvent surge tank 6 is connect with 5 top of solvent refining tower, and the top of solvent refining tower 5 passes through gas phase pipe Line is connect with de- phosgene tower and solvent refining tower top cooler 14,
5 tower reactor bottom of solvent refining tower is connect by liquid phase pipeline with solvent tank 7;
Phosgenation reactor solvent feed pipe 17 is arranged in 2 top of phosgenation reactor, and the top of phosgenation reactor 2 passes through Vapor delivery line is connect with 1 tower reactor of absorption tower;
2 tower reactor bottom of phosgenation reactor takes off the top of phosgene tower 3 by connecting in the middle part of liquid phase pipeline and de- phosgene tower 3 It is connect by vapor delivery line with de- phosgene tower and solvent refining tower top cooler 14, de- 3 tower reactor bottom of phosgene tower passes through liquid-phase tube Line is connect with 4 top of solvent removal tower, and the top of solvent removal tower 4 is connected by vapor delivery line and solvent removal tower top cooler 15 It connects, solvent removal tower top cooler 15 is connect with solvent removal tower top knockout drum 8, solvent removal tower top knockout drum 8 Bottom is connect by liquid phase pipeline 21 with solvent tank 7, passes through vapor delivery line and suction at the top of solvent removal tower top knockout drum 8 Receive the connection of 1 tower reactor of tower;
De- phosgene tower and solvent refining tower top cooler 14 and de- phosgene tower and solvent refining tower top knockout drum 9 connect It connects, de- phosgene tower and 9 bottom of solvent refining tower top knockout drum are connect by liquid phase pipeline with 5 top of solvent refining tower, are taken off It is connect with 1 tower reactor of absorption tower at the top of phosgene tower and solvent refining tower top knockout drum 9 by vapor delivery line, de- phosgene tower and molten Agent refines tower overhead gas liquid knockout drum 9 and drainpipe 19 is arranged;
Tail gas discharging pipe 18 is arranged in the top on absorption tower 1.
The tower reactor point of phosgenation reactor 2 of the present invention, de- phosgene tower 3, solvent removal tower 4 and solvent refining tower 5 Not An Zhuan reboiler, for will corresponding column bottom liquid phase heating after be recycled back to tower bottom.Wherein, light is installed in 2 bottom of phosgenation reactor Gasification reactor tower reactor reboiler 10.The bottom of de- phosgene tower 3 is installed by de- phosgene tower reactor reboiler 11.4 bottom of solvent removal tower Solvent removal tower reactor reboiler 12 is installed.5 bottom of solvent refining tower is installed by solvent refining tower reactor reboiler 13.
As a preferred option, solvent tank 7 of the present invention by pipeline and absorption tower solvent feed pipe 16 and/or Phosgenation reactor solvent feed pipe 17 connects, optional in solvent tank 7 and absorption tower solvent feed pipe 16 and/or phosgenation Cooler is set on the pipeline that reactor solvent feed pipe 17 connects.
A method of it is removed water, is included the following steps using system of the present invention;
Solvent is added into absorption tower 1 from absorption tower solvent feed pipe 16, it is slow to go to thick solvent from 1 tower reactor bottom of absorption tower Rush tank 6;The solvent of thick solvent surge tank 6 enters 5 top of solvent refining tower, and the top gas phase of solvent refining tower 5 is by de- phosgene Tower and solvent refining tower top cooler 14 enter de- phosgene tower and solvent refining tower top knockout drum 9 after condensing;Solvent refining 5 tower reactor bottom of tower extraction liquid phase enters solvent tank 7;
Solvent, the top of phosgenation reactor 2 are added from phosgenation reactor solvent feed pipe 17 to phosgenation reactor 2 Gas phase enters 1 tower reactor of absorption tower, and the tower reactor bottom liquid phases of phosgenation reactor 2 enter de- 3 middle part of phosgene tower;
De- 3 top gaseous phase of phosgene tower enters de- phosgene tower after de- phosgene tower and solvent refining tower top cooler 14 condense With solvent refining tower top knockout drum 9;
Gas phase and liquid phase are obtained in de- phosgene tower and solvent refining tower top knockout drum 9, gained gas phase enters absorption tower 1 Tower reactor, gained liquid phase enter 5 top of solvent refining tower, water is enriched in de- phosgene tower and solvent refining tower top knockout drum 9, Layering, is discharged by drainpipe 19;
De- 3 tower reactor bottom of phosgene tower extraction liquid phase enters 4 top of solvent removal tower, the top gas phase warp of solvent removal tower 4 It crosses after solvent removal tower top cooler 15 condenses and obtains gas phase and liquid phase into solvent removal tower top knockout drum 8, brought about the desired sensation Mutually enter 1 tower reactor of absorption tower, gained liquid phase enters solvent tank 7;
Tail gas is discharged from tail gas discharging pipe 18.
Solvent in solvent tank 7 of the present invention can be used as solvent be supplied to absorption tower solvent feed pipe 16 and/or Phosgenation reactor solvent feed pipe 17.
In method of the present invention, the solvent be selected from dimethyl isophthalate, benzene,toluene,xylene, chlorobenzene and One of o-dichlorohenzene is a variety of, preferably chlorobenzene and o-dichlorohenzene, more preferably chlorobenzene.
In method of the present invention, moisture content is 0-0.400wt%, preferably 0-0.0300wt% in the solvent.
In method of the present invention, the temperature of the solvent is 10-60 DEG C, preferably 20-50 degree, more preferably 30-40 ℃。
In method of the present invention, the gauge pressure on the absorption tower 1 is 100-150KPa, preferably 100-130KPa, more excellent Select 100-110KPa.
In method of the present invention, the gauge pressure of the phosgenation reactor 2 is 100-150KPa, preferably 100- 130KPa, more preferable 100-110KPa;The bottom temperature of the phosgenation reactor 2 be 130-170 DEG C, preferably 140-160 DEG C, More preferably 150-160 DEG C.
In method of the present invention, the gauge pressure of the de- phosgene tower 3 is 100-150KPa, preferably 100-130KPa, more It is preferred that 100-110KPa;The bottom temperature of the de- phosgene tower 3 be 130-170 DEG C, preferably 140-160 DEG C, more preferable 150-160 ℃。
In method of the present invention, the gauge pressure of the solvent removal tower 4 is 20-80KPa, preferably 30-70KPa, more excellent Select 40-60KPa;The bottom temperature of the solvent removal tower 4 be 100-150 DEG C, preferably 110-140 DEG C, more preferable 120-130 ℃。
In method of the present invention, the gauge pressure of the solvent refining tower 5 is 100-150KPa, preferably 100-130KPa, More preferable 100-110KPa;The bottom temperature of the solvent refining tower 5 be 130-180 DEG C, preferably 140-170 DEG C, more preferably 150-160℃。
Condensation liquidus temperature in method of the present invention, in the de- phosgene tower and solvent refining tower top cooler 14 It is 50-100 DEG C, preferably 60-90 DEG C, more preferable 70-80 DEG C.
In method of the present invention, the condensation liquidus temperature in the solvent removal tower top cooler 15 is 50-100 DEG C, preferably 60-90 DEG C, more preferable 70-80 DEG C.
Absorption tower of the present invention, phosgenation reactor, de- phosgene tower, solvent removal tower, solvent refining tower can be Equipment well known in the art.
Preferably, absorption tower of the present invention is packed tower;Phosgenation reactor of the present invention is plate column;The present invention The de- phosgene tower is plate column;Solvent removal tower of the present invention is plate column;Solvent refining tower of the present invention is board-like Tower.
Water scavenging system and water-eliminating method of the invention is suitable for the reaction unit that light phosgenation prepares isocyanates, institute Stating isocyanates includes but is not limited to toluene di-isocyanate(TDI) (TDI), isophorone diisocyanate (IPDI), diphenyl methane Diisocyanate (MDI), dicyclohexyl methyl hydride diisocyanate (HMDI), hexamethylene diisocyanate (HDI) etc..
In the technique of phosgenation production isocyanates, absorption tower 1 is used to absorb the light in the exhaust of phosgenation reactor 2 Gas;Phosgenation reactor 2 is for carrying out phosgenation reaction;De- phosgene tower 3 is in the mixed liquor after removing phosgenation reaction Phosgene;Solvent removal tower 4 is for the solvent in the mixed liquor after removing phosgenation reaction;Solvent refining tower 5 is miscellaneous for that will contain The solvent of matter is refined;Surge tank of the thick solvent surge tank 6 for the solvent containing impurity that removing comes out in system;Solvent Storage tank 7 is used to store the solvent after purification qualification.
Water-eliminating method of the present invention can be used in combination with other water-eliminating methods well known in the art, including but not It is limited to nitrogen purging.As a preferred scheme, nitrogen purging can be first carried out, then uses water removal of the present invention again Method further removes water.
Using in water-eliminating method of the present invention treated phosgenation production isocyanate plant, biodiversity content 100ppm can be reached hereinafter, representing moisture content in device with the moisture content in the solvent in thick solvent surge tank 6.
Water scavenging system and method for the invention opens maintenance etc. especially suitable for removing phosgenation production isocyanate plant The water being introduced into system in the process improves driving efficiency.Solvent operating water removal is quick, efficient in the present invention, especially in solvent It operates in process route selection, takes and system upstream solvent is delivered to downstream solvent treating column with minimal path, avoid downstream Aqueous solvent returns to up-stream system, removes water the principle that qualified solvent is sent directly into qualified solvent tank, dramatically simplifies Process route shortens the solvent duration of runs, improves efficiency.
Detailed description of the invention
Fig. 1 is the schematic diagram of water scavenging system of the present invention;
Fig. 2 is the schematic diagram of the water scavenging system of comparative example 1;
1. absorption tower;2. phosgenation reactor;3. de- phosgene tower;4. solvent removal tower;5. solvent refining tower;6. thick solvent Surge tank;7 solvent tanks;8. solvent removal tower top knockout drum;9. de- phosgene tower and solvent refining tower top knockout drum; 10. phosgenation reactor tower reactor reboiler;11. de- phosgene tower reactor reboiler;12. solvent removal tower reactor reboiler;13. solvent is smart Tower reactor reboiler processed;14. de- phosgene tower and solvent refining tower top cooler;15. solvent removal tower top cooler;16. absorption tower Solvent feed pipe;17. phosgenation reactor solvent feed pipe;18. tail gas discharging pipe;19. drainpipe;20. connecting 1 tower of absorption tower The liquid phase pipeline in bottom portion and thick solvent surge tank 6;21. connecting the liquid of solvent removal tower top knockout drum 8 and solvent tank 7 Phase pipeline;22. connecting the liquid phase pipeline of absorption tower 1 tower reactor bottom and 2 tower reactor of phosgenation reactor;23. connecting solvent removal tower Push up the liquid phase pipeline of knockout drum 8 and thick solvent surge tank 6.
Specific embodiment
The following examples will to will be further described to method provided by the present invention, but the present invention is not limited to Listed embodiment should also include other any well known changes in scope of the presently claimed invention.
In the present invention, it is to be understood that term " on ", "top", "bottom", " in " etc. instructions positional relationship be based on Positional relationship shown in the drawings, is merely for convenience of description of the present invention and simplification of the description, rather than the dress of indication or suggestion meaning It sets or element must have specific position, with specific placement configurations and operation, therefore should not be understood as to limit of the invention System.
Moisture content is measured using karl Fischer moisture teller in solvent.
Embodiment 1
Water scavenging system for phosgenation production isocyanate plant as shown in Figure 1 comprising: absorption tower 1, phosgenation It is reactor 2, phosgenation reactor tower reactor reboiler 10, de- phosgene tower 3, de- phosgene tower reactor reboiler 11, solvent removal tower 4, molten Agent removes tower reactor reboiler 12, solvent removal tower top cooler 15, solvent removal tower top knockout drum 8, thick solvent surge tank 6, solvent refining tower 5, solvent refining tower reactor reboiler 13, de- phosgene tower and solvent refining tower top cooler 14, de- phosgene tower and Solvent refining tower top knockout drum 9, solvent tank 7;
1 top of absorption tower be arranged absorption tower solvent feed pipe 16,1 tower reactor bottom of absorption tower by liquid phase pipeline 20 with slightly it is molten Agent surge tank 6 connects, and thick solvent surge tank 6 is connect with 5 top of solvent refining tower, and the top of solvent refining tower 5 passes through gas phase pipe Line is connect with de- phosgene tower and solvent refining tower top cooler 14,
5 tower reactor bottom of solvent refining tower is connect by liquid phase pipeline with solvent tank 7;
Phosgenation reactor solvent feed pipe 17 is arranged in 2 top of phosgenation reactor, and the top of phosgenation reactor 2 passes through Vapor delivery line is connect with 1 tower reactor of absorption tower;
2 tower reactor bottom of phosgenation reactor takes off the top of phosgene tower 3 by connecting in the middle part of liquid phase pipeline and de- phosgene tower 3 It is connect by vapor delivery line with de- phosgene tower and solvent refining tower top cooler 14, de- 3 tower reactor bottom of phosgene tower passes through liquid-phase tube Line is connect with 4 top of solvent removal tower, and the top of solvent removal tower 4 is connected by vapor delivery line and solvent removal tower top cooler 15 It connects, solvent removal tower top cooler 15 is connect with solvent removal tower top knockout drum 8, solvent removal tower top knockout drum 8 Bottom is connect by liquid phase pipeline 21 with solvent tank 7, passes through vapor delivery line and suction at the top of solvent removal tower top knockout drum 8 Receive the connection of 1 tower reactor of tower;
De- phosgene tower and solvent refining tower top cooler 14 and de- phosgene tower and solvent refining tower top knockout drum 9 connect It connects, de- phosgene tower and 9 bottom of solvent refining tower top knockout drum are connect by liquid phase pipeline with 5 top of solvent refining tower, are taken off It is connect with 1 tower reactor of absorption tower at the top of phosgene tower and solvent refining tower top knockout drum 9 by vapor delivery line, de- phosgene tower and molten Agent refines tower overhead gas liquid knockout drum 9 and drainpipe 19 is arranged;
Tail gas discharging pipe 18 is arranged in the top on absorption tower 1.
Phosgenation reactor 2, the tower reactor for taking off phosgene tower 3, solvent removal tower 4 and solvent refining tower 5 install reboiler respectively, For corresponding column bottom liquid phase circulation to be returned tower bottom.Wherein, phosgenation reactor tower reactor reboiler is installed in 2 bottom of phosgenation reactor 10.The bottom of de- phosgene tower 3 is installed by de- phosgene tower reactor reboiler 11.4 bottom of solvent removal tower installation solvent removal tower reactor is boiled again Device 12.5 bottom of solvent refining tower is installed by solvent refining tower reactor reboiler 13.
Capital equipment capacity parameter is as follows:
Absorption tower 1: size φ 1800mm × 30225mm, tower reactor capacity 9m3
Phosgenation reactor 2: size φ 5200mm × 38350mm, tower reactor capacity 70m3
De- phosgene tower 3: size φ 2200mm × 25650mm, tower reactor capacity 10m3
Solvent removal tower 4: size φ 5200mm × 15350mm, tower reactor capacity 17m3
Solvent refining tower 5: size φ 3000mm × 26080mm, tower reactor capacity 12m3
Thick solvent surge tank 6: size φ 2500mm × 5590mm, capacity 24m3
Solvent tank 7: size φ 3500mm × 8013mm, capacity 70m3
Embodiment 2
The present embodiment is the water scavenging system using embodiment 1, the dewatering process for phosgenation production isocyanate plant. Into before solvent, under normal pressure, it is -40 DEG C that system, which purges drying to dew point using nitrogen,.
Solvent is chlorobenzene, and moisture content is 0.0125wt% in chlorobenzene, and solvent-based quality, temperature is 30 DEG C.
Absorption tower 1 is packed tower, and tower top operating pressure is gauge pressure 100KPa.
The tower top operating pressure of phosgenation reactor 2 is gauge pressure 110KPa, and tower reactor operation temperature is 130 DEG C.
De- 3 operating pressure of phosgene tower is gauge pressure 110KPa, and 150 DEG C of tower reactor operation temperature, overhead condensation liquid phase is 70 DEG C.
4 operating pressure of solvent removal tower is gauge pressure 50KPa, and tower reactor operation temperature is 130 DEG C, and overhead condensation liquid phase temperature is 80℃。
5 operating pressure of solvent refining tower is gauge pressure 102KPa, and bottom temperature is 160 DEG C.Overhead condensation liquid phase temperature is 70 ℃。
Chlorobenzene, inlet amount about 20m are added into absorption tower 1 from absorption tower solvent feed pipe 163/ h, from 1 tower reactor of absorption tower Bottom is delivered to thick solvent surge tank 6.
Chlorobenzene, inlet amount about 80m are added from phosgenation reactor solvent feed pipe 17 to phosgenation reactor 23/ h, phosgene Change 2 top gaseous phase of reactor and enter 1 tower reactor of absorption tower, the tower bottom liquid phase of phosgenation reactor 2 enters de- 3 middle part of phosgene tower.
De- 3 top gaseous phase of phosgene tower enters de- phosgene tower after de- phosgene tower and solvent refining overhead condenser 14 condense In solvent refining tower top knockout drum 9;De- 3 tower reactor liquid phase of phosgene tower enters 4 top of solvent removal tower.
The top gaseous phase of solvent removal tower 4 enters solvent removal tower overhead gas after the condensation of solvent removal tower top cooler 15 Liquid knockout drum 8 obtains gas phase and liquid phase, and gained gas phase enters 1 tower reactor of absorption tower, and liquid phase enters solvent tank 7.
The solvent of thick solvent surge tank 6 enters 5 top of solvent refining tower, and 5 top gaseous phase of solvent refining tower is by de- phosgene Tower and solvent refining tower top cooler 14 enter after condensing in de- phosgene tower and solvent refining tower top knockout drum 9;
Gas-liquid separation is carried out in de- phosgene tower and solvent refining tower top knockout drum 9 and obtains gas phase and liquid phase, is brought about the desired sensation Mutually enter 1 tower reactor of absorption tower;After the operating of solvent refining tower 5 is stablized, take off in phosgene tower and solvent refining tower top knockout drum 9 Liquid phase contained in moisture enrichment, layering, every 2 hours by water of 19 row of drainpipe, every time with 1m3/ h flow row 0.5 hour, intermittently by the water discharge system after layering, to reduce moisture in system.5 tower reactor liquid phase of solvent refining tower is sent to molten Agent storage tank 7.
Tail gas is discharged from tail gas discharging pipe 18.
It operates under such an approach, the timing since operating when (temperature, pressure) is stablized solvent refining tower 5 monitors thick solvent When the biodiversity content of chlorobenzene is reduced to 100ppm (thick solvent surge tank chlorobenzene is up to standard) in surge tank 6, the System drainage used time As shown in table 1.
Embodiment 3
The present embodiment is the water scavenging system using embodiment 1, the dewatering process for phosgenation production isocyanate plant. Into before solvent, under normal pressure, it is -40 DEG C that system, which purges drying to dew point using nitrogen,.
Solvent is chlorobenzene, and moisture content is 0.0270wt% in chlorobenzene, and solvent-based quality, temperature is 30 DEG C.
Absorption tower 1 is packed tower, and tower top operating pressure is gauge pressure 120KP.
The tower top operating pressure of phosgenation reactor 2 is gauge pressure 130KPa, and tower reactor operation temperature is 150 DEG C
De- 3 operating pressure of phosgene tower is gauge pressure 130KPa, and 165 DEG C of tower reactor operation temperature, overhead condensation liquid phase is 80 DEG C.
4 operating pressure of solvent removal tower is gauge pressure 30KPa, and tower reactor operation temperature is 110 DEG C, and overhead condensation liquid phase temperature is 80℃。
5 operating pressure gauge pressure 130KPa of solvent refining tower, bottom temperature are 170 DEG C, and overhead condensation liquid phase temperature is 80 DEG C.
Chlorobenzene, inlet amount about 20m are added into absorption tower 1 from absorption tower solvent feed pipe 163/ h, from 1 tower reactor of absorption tower Bottom is delivered to thick solvent surge tank 6.
Chlorobenzene, inlet amount about 80m are added from phosgenation reactor solvent feed pipe 17 to phosgenation reactor 23/ h, phosgene Change 2 top gaseous phase of reactor and enter 1 tower reactor of absorption tower, the tower bottom liquid phase of phosgenation reactor 2 enters de- 3 middle part of phosgene tower.
De- 3 top gaseous phase of phosgene tower enters de- phosgene tower after de- phosgene tower and solvent refining overhead condenser 14 condense In solvent refining tower top knockout drum 9;De- 3 tower reactor liquid phase of phosgene tower enters 4 top of solvent removal tower.
The top gaseous phase of solvent removal tower 4 enters solvent removal tower overhead gas after the condensation of solvent removal tower top cooler 15 Liquid knockout drum 8 obtains gas phase and liquid phase, and gained gas phase enters 1 tower reactor of absorption tower, and liquid phase enters solvent tank 7.
The solvent of thick solvent surge tank 6 enters 5 top of solvent refining tower, and 5 top gaseous phase of solvent refining tower is by de- phosgene Tower and solvent refining tower top cooler 14 enter after condensing in de- phosgene tower and solvent refining tower top knockout drum 9;
Gas-liquid separation is carried out in de- phosgene tower and solvent refining tower top knockout drum 9 and obtains gas phase and liquid phase, is brought about the desired sensation Mutually enter 1 tower reactor of absorption tower;After the operating of solvent refining tower 5 is stablized, take off in phosgene tower and solvent refining tower top knockout drum 9 Liquid phase contained in moisture enrichment, layering, every 2 hours by water of 19 row of drainpipe, every time with 1m3/ h flow row 0.5 hour, intermittently by the water discharge system after layering, to reduce moisture in system.5 tower reactor liquid phase of solvent refining tower is sent to molten Agent storage tank 7.
Tail gas is discharged from tail gas discharging pipe 18.
It operates under such an approach, the timing since operating when (temperature, pressure) is stablized solvent refining tower 5 monitors thick solvent When the biodiversity content of chlorobenzene is reduced to 100ppm (thick solvent surge tank chlorobenzene is up to standard) in surge tank 6, the System drainage used time As shown in table 1.
Comparative example 1
Using the water scavenging system for phosgenation production isocyanate plant as shown in Figure 2, cancel liquid phase in embodiment 1 The setting of pipeline 20,21 is changed to connect 1 tower reactor bottom of absorption tower and 2 tower reactor of phosgenation reactor, liquid phase using liquid phase pipeline 22 Pipeline 23 connects solvent removal tower top knockout drum 8 and thick solvent surge tank 6.The system is that phosgenation produces isocyanates dress The normal production system set.Into before solvent, under normal pressure, it is -40 DEG C that system, which purges drying to dew point using nitrogen,.
Solvent is chlorobenzene, and moisture content is 0.0270wt% in chlorobenzene, and solvent-based quality, temperature is 30 DEG C.
Absorption tower 1 is packed tower, and tower top operating pressure is gauge pressure 100KPa.
The tower top operating pressure gauge pressure 110KPa of phosgenation reactor 2, tower reactor operation temperature are 130 DEG C.
De- 3 operating pressure of phosgene tower is gauge pressure 110KPa, and 150 DEG C of tower reactor operation temperature, overhead condensation liquid phase is 70 DEG C.
4 operating pressure gauge pressure 50KPa of solvent removal tower, tower reactor operation temperature are 110 DEG C, and overhead condensation liquid phase temperature is 80 ℃。
5 operating pressure gauge pressure 110KPa of solvent refining tower, bottom temperature are 165 DEG C.Overhead condensation liquid phase temperature is 70 DEG C.
Chlorobenzene, inlet amount about 20m are added into absorption tower 1 from absorption tower solvent feed pipe 163/ h, from 1 tower reactor of absorption tower Bottom is delivered to 2 tower reactor of phosgenation reactor.
Chlorobenzene, inlet amount about 80m are added from phosgenation reactor solvent feed pipe 17 to phosgenation reactor 23/ h, phosgene Change 2 top gaseous phase of reactor and enter 1 tower reactor of absorption tower, the tower bottom liquid phase of phosgenation reactor 2 enters de- 3 middle part of phosgene tower.
De- 3 top gaseous phase of phosgene tower enters de- phosgene tower after de- phosgene tower and solvent refining overhead condenser 14 condense In solvent refining tower top knockout drum 9;De- 3 tower reactor liquid phase of phosgene tower enters 4 top of solvent removal tower.
The top gaseous phase of solvent removal tower 4 enters solvent removal tower overhead gas after the condensation of solvent removal tower top cooler 15 Liquid knockout drum 8 obtains gas phase and liquid phase, and gained gas phase enters 1 tower reactor of absorption tower, and liquid phase enters thick solvent surge tank 6.
The solvent of thick solvent surge tank 6 enters 5 top of solvent refining tower, and 5 top gaseous phase of solvent refining tower is by de- phosgene Tower and solvent refining tower top cooler 14 enter after condensing in de- phosgene tower and solvent refining tower top knockout drum 9;
Gas-liquid separation is carried out in de- phosgene tower and solvent refining tower top knockout drum 9 and obtains gas phase and liquid phase, is brought about the desired sensation Mutually enter 1 tower reactor of absorption tower;After the operating of solvent refining tower 5 is stablized, take off in phosgene tower and solvent refining tower top knockout drum 9 Liquid phase contained in moisture enrichment, layering, every 2 hours by water of 19 row of drainpipe, every time with 1m3/ h flow row 0.5 hour, intermittently by the water discharge system after layering, to reduce moisture in system.5 tower reactor liquid phase of solvent refining tower is sent to molten Agent storage tank 7.
Tail gas is discharged from tail gas discharging pipe 18.
It operates under such an approach, the timing since operating when (temperature, pressure) is stablized solvent refining tower 5 monitors thick solvent When the biodiversity content of chlorobenzene is reduced to 100ppm (thick solvent surge tank chlorobenzene is up to standard) in surge tank 6, the System drainage used time As shown in table 1.
1 embodiment of table and comparative example result
It drives initial stage as it can be seen from table 1 the method for the present invention can quickly, efficiently reduce phosgenation production isocyanate plant Moisture in system, greatly shortening device are driven the water removal time at initial stage, and energy consumption is saved.

Claims (10)

1. a kind of water scavenging system of phosgenation production isocyanate plant, comprising: absorption tower (1), phosgenation reactor (2) take off It is phosgene tower (3), solvent removal tower (4), solvent removal tower top cooler (15), solvent removal tower top knockout drum (8), thick molten Agent surge tank (6), solvent refining tower (5), de- phosgene tower and solvent refining tower top cooler (14), de- phosgene tower and solvent refining Tower top knockout drum (9), solvent tank (7);
Absorption tower (1) top be arranged absorption tower solvent feed pipe (16), absorption tower (1) tower reactor bottom by liquid phase pipeline (20) with Thick solvent surge tank (6) connection, thick solvent surge tank (6) connect with solvent refining tower (5) top, the top of solvent refining tower (5) Portion is connect by vapor delivery line with de- phosgene tower and solvent refining tower top cooler (14),
Solvent refining tower (5) tower reactor bottom is connect by liquid phase pipeline with solvent tank (7);
Phosgenation reactor solvent feed pipe (17) are arranged in phosgenation reactor (2) top, and the top of phosgenation reactor (2) is logical Vapor delivery line is crossed to connect with absorption tower (1) tower reactor;
Phosgenation reactor (2) tower reactor bottom takes off the top of phosgene tower (3) by connecting in the middle part of liquid phase pipeline and de- phosgene tower (3) Portion is connect by vapor delivery line with de- phosgene tower and solvent refining tower top cooler (14), and de- phosgene tower (3) tower reactor bottom passes through Liquid phase pipeline is connect with solvent removal tower (4) top, and the top of solvent removal tower (4) passes through vapor delivery line and solvent removal tower top Cooler (15) connection, solvent removal tower top cooler (15) are connect with solvent removal tower top knockout drum (8), solvent removal Tower top knockout drum (8) bottom is connect by liquid phase pipeline (21) with solvent tank (7), solvent removal tower top knockout drum (8) top is connect by vapor delivery line with absorption tower (1) tower reactor;
De- phosgene tower and solvent refining tower top cooler (14) and de- phosgene tower and solvent refining tower top knockout drum (9) are even It connects, takes off phosgene tower and solvent refining tower top knockout drum (9) bottom and connected by liquid phase pipeline and solvent refining tower (5) top It connects, is connect, taken off with absorption tower (1) tower reactor by vapor delivery line at the top of de- phosgene tower and solvent refining tower top knockout drum (9) Phosgene tower and solvent refining tower top knockout drum (9) setting drainpipe (19);
Tail gas discharging pipe (18) are arranged in the top on absorption tower (1).
2. water scavenging system according to claim 1, which is characterized in that the solvent tank (7) is by pipeline and absorbs Tower solvent feed pipe (16) and/or phosgenation reactor solvent feed pipe (17) connection, it is optional in solvent tank (7) and to absorb Cooler is set on tower solvent feed pipe (16) and/or the pipeline of phosgenation reactor solvent feed pipe (17) connection.
3. system according to claim 1 or 2, which is characterized in that install phosgenation in phosgenation reactor (2) bottom The bottom of reactor tower reactor reboiler (10), the de- phosgene tower (3) is installed de- phosgene tower reactor reboiler (11), and the solvent is de- Except solvent removal tower reactor reboiler (12) are installed in tower (4) bottom, solvent refining tower (5) the bottom installation solvent refining tower reactor is again It boils device (13).
4. a kind of method that water scavenging system according to claim 1-3 is removed water, includes the following steps;
Solvent is added in from absorption tower solvent feed pipe (16) to absorption tower (1), goes to thick solvent from absorption tower (1) tower reactor bottom Surge tank (6);The solvent of thick solvent surge tank (6) enters solvent refining tower (5) top, the top gas phase of solvent refining tower (5) Enter de- phosgene tower and solvent refining tower top gas-liquid separation after de- phosgene tower and solvent refining tower top cooler (14) condensation Tank (9);Solvent refining tower (5) tower reactor bottom extraction liquid phase enters solvent tank (7);
Solvent, the top of phosgenation reactor (2) are added from phosgenation reactor solvent feed pipe (17) to phosgenation reactor (2) Portion's gas phase enters absorption tower (1) tower reactor, and the tower reactor bottom liquid phases of phosgenation reactor (2) enter in the middle part of de- phosgene tower (3);
De- phosgene tower (3) top gaseous phase enters de- phosgene tower after de- phosgene tower and solvent refining tower top cooler (14) condensation With solvent refining tower top knockout drum (9);
Gas phase and liquid phase are obtained in de- phosgene tower and solvent refining tower top knockout drum (9), gained gas phase enters absorption tower (1) Tower reactor, gained liquid phase enter solvent refining tower (5) top, and water is in de- phosgene tower and solvent refining tower top knockout drum (9) Enrichment, layering, are discharged by drainpipe (19);
De- phosgene tower (3) tower reactor bottom extraction liquid phase enters solvent removal tower (4) top, the top gas phase of solvent removal tower (4) Enter solvent removal tower top knockout drum (8) after solvent removal tower top cooler (15) condensation and obtain gas phase and liquid phase, Gained gas phase enters absorption tower (1) tower reactor, and gained liquid phase enters solvent tank (7);
Tail gas is discharged from tail gas discharging pipe (18).
5. according to the method described in claim 4, it is characterized in that, the solvent in the solvent tank (7) is provided as solvent To absorption tower solvent feed pipe (16) and/or phosgenation reactor solvent feed pipe (17).
6. method according to claim 4 or 5, which is characterized in that the solvent be selected from dimethyl isophthalate, benzene, One of toluene, dimethylbenzene, chlorobenzene and o-dichlorohenzene are a variety of, preferably chlorobenzene and o-dichlorohenzene, more preferably chlorobenzene.
7. according to the described in any item methods of claim 4-6, which is characterized in that moisture content is 0- in the solvent 0.400wt%, preferably 0-0.0300wt%.
8. according to the described in any item methods of claim 4-7, which is characterized in that the temperature of the solvent is 10-60 DEG C, preferably 20-50 degree, more preferably 30-40 DEG C.
9. according to the described in any item methods of claim 4-8, which is characterized in that the gauge pressure of the absorption tower (1) is 100- 150KPa, preferably 100-130KPa, more preferable 100-110KPa;
The gauge pressure of the phosgenation reactor (2) is 100-150KPa, preferably 100-130KPa, more preferable 100-110KPa;Institute The bottom temperature for stating phosgenation reactor (2) is 130-170 DEG C, preferably 140-160 DEG C, more preferable 150-160 DEG C;
The gauge pressure of the de- phosgene tower (3) is 100-150KPa, preferably 100-130KPa, more preferable 100-110KPa;It is described de- The bottom temperature of phosgene tower (3) is 130-170 DEG C, preferably 140-160 DEG C, more preferable 150-160 DEG C;
The gauge pressure of the solvent removal tower (4) is 20-80KPa, preferably 30-70KPa, more preferable 40-60KPa;The solvent is de- Except the bottom temperature of tower (4) is 100-150 DEG C, preferably 110-140 DEG C, more preferable 120-130 DEG C;
The gauge pressure of the solvent refining tower (5) is 100-150KPa, preferably 100-130KPa, more preferable 100-110KPa;It is described The bottom temperature of solvent refining tower (5) is 130-180 DEG C, preferably 140-170 DEG C, more preferable 150-160 DEG C.
10. according to the described in any item methods of claim 4-9, which is characterized in that the de- phosgene tower and solvent refining tower top Condensation liquidus temperature in cooler (14) is 50-100 DEG C, preferably 60-90 DEG C, more preferable 70-80 DEG C;
Condensation liquidus temperature in the solvent removal tower top cooler (15) is 50-100 DEG C, preferably 60-90 DEG C, more preferably 70-80℃。
CN201910237026.0A 2019-03-27 Water removal system and water removal method of isocyanate production device by phosgenation Active CN110003054B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103613515A (en) * 2013-12-13 2014-03-05 青岛科技大学 Method for recycling phosgene during isocyanate production process
CN107353231A (en) * 2017-07-17 2017-11-17 薛永和 A kind of method for preparing organic isocyanate
CN107652208A (en) * 2017-08-30 2018-02-02 万华化学(宁波)有限公司 The method and system of desolvation in a kind of isocyanate product obtained from phosgenation reaction
CN107935889A (en) * 2017-11-29 2018-04-20 万华化学集团股份有限公司 The preparation method and system of a kind of monoisocyanates
CN210001801U (en) * 2019-03-27 2020-01-31 万华化学集团股份有限公司 Water removal system of phosgenation isocyanate production device

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103613515A (en) * 2013-12-13 2014-03-05 青岛科技大学 Method for recycling phosgene during isocyanate production process
CN107353231A (en) * 2017-07-17 2017-11-17 薛永和 A kind of method for preparing organic isocyanate
CN107652208A (en) * 2017-08-30 2018-02-02 万华化学(宁波)有限公司 The method and system of desolvation in a kind of isocyanate product obtained from phosgenation reaction
CN107935889A (en) * 2017-11-29 2018-04-20 万华化学集团股份有限公司 The preparation method and system of a kind of monoisocyanates
CN210001801U (en) * 2019-03-27 2020-01-31 万华化学集团股份有限公司 Water removal system of phosgenation isocyanate production device

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