CN107056582A - Coal-ethylene glycol carbonylation system reclaims the system and method for methyl nitrite - Google Patents
Coal-ethylene glycol carbonylation system reclaims the system and method for methyl nitrite Download PDFInfo
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- CN107056582A CN107056582A CN201710093216.0A CN201710093216A CN107056582A CN 107056582 A CN107056582 A CN 107056582A CN 201710093216 A CN201710093216 A CN 201710093216A CN 107056582 A CN107056582 A CN 107056582A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C201/00—Preparation of esters of nitric or nitrous acid or of compounds containing nitro or nitroso groups bound to a carbon skeleton
- C07C201/04—Preparation of esters of nitrous acid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
- C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/88—Separation; Purification; Use of additives, e.g. for stabilisation by treatment giving rise to a chemical modification of at least one compound
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Abstract
The present invention relates to coal-ethylene glycol chemical field, more particularly to a kind of coal-ethylene glycol carbonylation system reclaims the system and method for methyl nitrite, this method is mainly the method being combined in coal-ethylene glycol carbonylation system by air lift, flash distillation, nitrate reductase and reaches the purpose for effectively reclaiming methyl nitrite gas.The recovery system mainly includes preceding air lift system, nitrate reductase system and the rear air lift system of methyl nitrite；The preceding air lift system is provided with liquid phase preheater, preceding stripping tower and liquid phase discharging centrifugal pump；The nitrate reductase sets liquid phase feeding preheater and nitrate reductase tower；Air lift sets flash tank, liquid phase feeding centrifugal pump and rear stripping tower afterwards.It is an object of the invention to the method being combined by physical process and chemical reaction, to ensure nitric oxide and methyl nitrite stable content in synthesis system gaseous component, high degree avoids the loss of nitric oxide and methyl nitrite, turns waste into wealth, reduces the wasting of resources and pollution of waterhead.
Description
Technical field
Reclaim sub- the present invention relates to coal-ethylene glycol chemical field, more particularly to a kind of coal-ethylene glycol carbonylation system
The system and method for methyl nitrate.
Background technology
Ethylene glycol is a kind of important industrial chemicals, is mainly used as the original of solvent, antifreezing agent and synthesizing polyester resin etc.
Material.At present, ethylene glycol is mainly prepared using oxirane direct hydration method.Because the preparation of oxirane is using ethene as original
Material, a large amount of productions depend on petroleum resources.And the total energy of China is characterized as rich coal, has gas, few oil, thus coal is efficient
The industrial chemicals such as ethylene glycol are converted into, dependence of the industrial chemicals to petroleum resources is reduced, are conducive to the optimization energy, resource structures,
Have great importance.
In recent years, with the progressively maturation of coal-ethylene glycol technology, the country has built large quantities of coal-ethylene glycol enterprises.
According to reliable statistics, in the coming years, the production capacity of China's coal-ethylene glycol is up to more than 5,000,000 tons.In coal-ethylene glycol production
During, substantial amounts of dust technology waste liquid can be produced.Current processing method is that the NaOH for adding metering is neutralized, and then will be contained
The waste liquid for having a large amount of sodium nitrate is directly discharged, and causes the pollution of water resource.Although nitrate is safe from harm to human body in itself, nitre
Partly be reduced into nitrite in the presence of reductive bacterium after hydrochlorate intake human body, nitrite easily with blood
Hemoglobin reacts to form ferrihemoglobin, so as to influence blood to the transmittability of oxygen.Therefore, how by dust technology waste liquid
Rationally utilize, be during coal-ethylene glycol, to concern the important engineering of people's livelihood safe drinking water.
Dust technology is reduced to methyl nitrite, gone during can further participating in coal-ethylene glycol, can not only
Turn waste into wealth, increase economic efficiency, and can effectively reduce the discharge containing nitric acid waste liquor of sodium, reduce the pollution to water resource,
The cost in coal-ethylene glycol art production process is reduced simultaneously, reduces the wasting of resources.
The content of the invention
It is an object of the invention to overcome present in above-mentioned prior art in coal-ethylene glycol production process due to a large amount of
The directly discharge of the waste liquid of sodium nitrate and provide the problem of cause the pollution of water resource one kind turn waste into wealth, reduce the wasting of resources and
The coal-ethylene glycol carbonylation system of pollution of waterhead reclaims the system and method for methyl nitrite.
To achieve these goals, present invention employs such technical scheme：A kind of coal-ethylene glycol carbonylation system
The system that system reclaims methyl nitrite, including preceding air stripping unit, nitrate reductase unit and rear air stripping unit, the preceding air stripping unit
Including preceding stripping tower liquid phase preheater, preceding stripping tower and preceding air lift tower bottoms discharging centrifugal pump, preceding stripping tower lower end is provided with gas
Phase entrance；Nitrate reductase unit includes nitrate reductase liquid phase heater and nitrate reductase reactor, nitrate reductase reactor upper end
It is provided with gas phase entrance；Air stripping unit includes rear stripping tower liquid phase feeding pump and rear stripping tower afterwards；The preceding stripping tower liquid phase is pre-
Hot device is connected by the liquid phase inlet duct of preceding stripping tower with end entrance on preceding stripping tower, the connection of preceding stripping tower lower end liquid-phase outlet
There is preceding air lift tower bottoms discharging centrifugal pump, preceding air lift tower bottoms discharging centrifugal pump is connected on nitrate reductase liquid heater, nitric acid
Reducing solution heater is connected to the porch of nitrate reductase reactor, stripping tower after the lower end outlet connection of nitrate reductase reactor
Liquid phase feeding pump, rear stripping tower liquid phase feeding pump is connected on rear stripping tower, and the top gaseous phase of rear stripping tower is connected to coal second
In glycol synthesis system.
The rear air stripping unit also includes a flash tank, and it is anti-that the liquid phase entrance of flash tank is connected to nitrate reductase by pipeline
Answer at the liquid-phase outlet of device, stripping tower liquid phase feeding pump, rear stripping tower liquid phase feeding pump after being connected at the liquid-phase outlet of flash tank
It is connected on rear stripping tower.
The liquid phase inlet duct of the preceding stripping tower is provided with temperature control valve (TCV), the gas phase inlet duct of preceding stripping tower and set
There is flow control valve.
The nitrate reductase liquid phase heater liquid-phase outlet connects 0.5MPa jet chimneys, on the 0.5MPa jet chimneys
Provided with temperature control valve (TCV).
The nitrate reductase reactor gas phase inlet duct is provided with flow control valve.
Vaccum-pumping equipment is connected with the flash tank, the sub- ester component for being flashed in flash tank is recycled to synthesis system
In, the entrance of vaccum-pumping equipment is provided with pressure-regulating valve, for stablizing flash tank pressure.
The rear stripping tower gas phase inlet duct is provided with flow control valve.
The preceding stripping tower specification is 1~2 meter of diameter, 10~25 meters of height, 10~30 layers of the column plate number of plies, and tray type is
Bubble-cap type, float-valve type or sieve-board type.
The rear stripping tower specification is 0.5~2 meter of diameter, 6~15 meters of height, 3~5 meters of dumped packing height, earthfill rockfill concrete riprap RCC
Type is Raschig ring, Pall ring, square saddle or ripple packing.
A kind of method that coal-ethylene glycol carbonylation system reclaims methyl nitrite, this method includes：Ethylene glycol is produced
During esterification reaction solution be admitted to through pipeline before in stripping tower liquid phase preheater, be preheated to the liquid after 60~80 DEG C through pipe
The tower top that road enters preceding stripping tower by the upper end entrance of preceding stripping tower is sprayed, and the gas phase filled into preceding air lift tower bottom exists
Packing layer is inversely contacted；The premenstrual air lift tower bottoms discharging centrifugal pump of liquid after contact enters nitrate reductase liquid phase heater
In, nitrate reductase reactor tower top is sent to after heating, carrying out following current with the gas phase that nitrate reductase reactor tower top is filled into connects
Touch, in nitrate reductase beds nitric acid and methanol and gas nitric oxide reduction generation methyl nitrite at 50~90 DEG C；
The methyl nitrite of generation is and rear in the nitrate reductase reactor column kettle liquid mutually stripping tower liquid phase feeding pumping stripping tower backward after
The gas phase that air lift tower bottom is filled into inversely is contacted in packing layer, and the methyl nitrite after air lift is sent back to by gaseous phase outlet
Into coal-ethylene glycol synthesis system.
The methyl nitrite of generation is sent to flash tank in nitrate reductase reactor column kettle liquid using pressure difference, in flash tank
The interior physical process flashed；Flash tank kettle liquid stripping tower liquid phase feeding after pumps stripping tower backward.
The coal-ethylene glycol esterification amount of liquid phase is 40~60 tons/h, and concentration of nitric acid is 1~5wt%.
The nitrate reductase reaction equation is。
The preceding stripping tower preheater uses 0.5MPa steam preheatings；The nitrate reductase liquid phase heater uses 0.5MPa
Steam is heated.
Hot(test)-spot temperature is preferably controlled to 75~90 DEG C in the nitrate reductase reactor.
The good effect that technical scheme is produced is as follows：The coal-ethylene glycol carbonylation system of the present invention is reclaimed
The system and method for methyl nitrite combines physics flash distillation, a kind of new new side of physics air lift, nitrate reductase chemical reaction
Method, air lift is first passed through by the methyl nitrite gas dissolved in esterification liquid phase, then by esterification liquid phase component nitric acid in
Reduction chemical reaction is carried out continuously in fixed bed reactors, in the presence of catalyst, 50~90 DEG C gentle with methanol by nitric acid
Body nitric oxide reduction generates methyl nitrite, returns to synthesis system, finally before esterification liquid phase sends out synthesis system
Through flash distillation and air lift, the methyl nitrite of flash distillation and air lift is returned to and supplemented in coal-ethylene glycol synthesis system, reduced
Methyl nitrite goes out the emptying of coal-ethylene glycol synthesis system by being dissolved in esterification reaction solution facies tract, is effectively recycled,
Production cost is saved, is increased economic efficiency, waste liquor contamination is reduced.
The system and method for the recovery methyl nitrite of the present invention is gone into operation through overtesting to be run, and greatly solves coal second
The problem of methyl nitrite consumption is big in glycol production technique, exemplified by producing 550 tons of ethylene glycol daily, 12 tons of reduction nitric acid discharge/
My god, the ton day of alkali lye amount 7.5 is neutralized, while nitric acid is carried out to be reduced to available gas component nitrous acid in coal-ethylene glycol technique
The amount of methyl nitrite is filled into methyl esters, high degree reduction carbonylation system, is exceeded according to calculating is cost-saved every year
14000000 yuan.
Brief description of the drawings
Fig. 1 is the connection diagram for the system that coal-ethylene glycol carbonylation system of the present invention reclaims methyl nitrite.
It is labeled as in figure：1. before stripping tower liquid phase preheater；2. before stripping tower；3. before air lift tower bottoms discharging centrifugal pump；
4. nitrate reductase liquid phase heater；5. nitrate reductase reactor；6. flash tank；7. after stripping tower liquid phase feeding pump；8. vacuumize
Equipment；9. after stripping tower；10. first flow regulating valve；11. second flow regulating valve；12. the 3rd flow control valve；13. first
Temperature control valve (TCV)；14. second temperature regulating valve；15. pressure-regulating valve.
Embodiment
The present invention is further elaborated and illustrated with reference to specific embodiment and accompanying drawing.
Embodiment one
The system that coal-ethylene glycol carbonylation system reclaims methyl nitrite, as shown in figure 1, including preceding air stripping unit, nitric acid
Reduction unit and rear air stripping unit, the preceding air stripping unit include preceding stripping tower liquid phase preheater 1, preceding stripping tower 2 and preceding air lift
Tower bottoms discharging centrifugal pump 3, the preceding stripping tower upper end is provided with gaseous phase outlet；Nitrate reductase unit includes nitrate reductase liquid phase
Heater 4 and nitrate reductase reactor 5, nitrate reductase reactor upper end are provided with gas phase entrance；Air stripping unit includes flash distillation afterwards
Tank 6, rear stripping tower liquid phase feeding pump 7 and rear stripping tower 9；The preceding stripping tower liquid phase preheater is entered by the liquid phase of preceding stripping tower
Mouth pipeline is connected with end entrance on preceding stripping tower, and preceding stripping tower lower end is provided with gas phase entrance, preceding stripping tower lower end liquid-phase outlet
Air lift tower bottoms discharging centrifugal pump before being connected with, preceding air lift tower bottoms discharging centrifugal pump is connected on nitrate reductase liquid heater,
Nitrate reductase liquid heater is connected to the porch of nitrate reductase reactor, the lower end outlet connection flash distillation of nitrate reductase reactor
Stripping tower liquid phase feeding pump after being connected at the liquid phase porch of tank, the liquid-phase outlet of flash tank, rear stripping tower liquid phase feeding pump connects
It is connected on rear stripping tower, the top gaseous phase of rear stripping tower is connected in coal-ethylene glycol synthesis system.
The liquid phase inlet duct of the preceding stripping tower is provided with the first temperature control valve (TCV) 13, is controlled by adjusting steam aperture
Inlet temperature is constant.The gas phase inlet duct of preceding stripping tower is provided with first flow regulating valve 10, by adjusting control valve opening
Control air lift tolerance, it is ensured that the stabilization of sub- ester air lift amount, Simultaneous Stabilization synthetic reaction gaseous component.
The nitrate reductase liquid phase heater carries out liquid phase preheating using 0.5MPa steam, on the 0.5MPa jet chimneys
Provided with second temperature regulating valve 14, control nitrate reductase tower top temperature constant by adjusting steam aperture.
The nitrate reductase reactor gaseous phase outlet pipeline is provided with second flow regulating valve 11.Stream is set on inlet duct
Gauge, second flow regulating valve, using linkage regulative mode, sets inlet flow rate meter scope as 2000 with inlet duct flowmeter
~5000Nm3/h, is adjusted according to system loading change, when system loading is below 80%, and flow adjustment range 2000~
3000Nm3/h, when load is more than 80%, 3000~5000Nm3/h of flow adjustment range.
Vaccum-pumping equipment 8 is connected with the flash tank, the sub- ester component for being flashed in flash tank is recycled to synthesis system
In system, the entrance of vaccum-pumping equipment is provided with pressure-regulating valve 15, for stablizing flash tank pressure.Flash tank pressure control to the greatest extent may be used
Can be low, sub- ester flash distillation amount is more.- 10~10KPa of the flash tank pressure control range, according to ethylene glycol process units size,
Control flash tank pressure constant by the treating capacity of vaccum-pumping equipment 8, it is ensured that the stabilization of sub- ester flash distillation amount, Simultaneous Stabilization synthetic reaction
Gaseous component.The flash tank pressure is adjusted with vacuum equipment load using linkage.
The rear stripping tower gas phase inlet duct is provided with the 3rd flow control valve 12, by adjusting control valve opening control
Air lift tolerance, it is ensured that the stabilization of sub- ester flash distillation amount, Simultaneous Stabilization synthetic reaction gaseous component.
The preceding stripping tower specification is 1~2 meter of diameter, 10~25 meters of height, 10~30 layers of the column plate number of plies, and tray type is
Bubble-cap type, float-valve type or sieve-board type can also.
The rear stripping tower specification is 0.5~2 meter of diameter, 6~15 meters of height, 3~5 meters of dumped packing height, earthfill rockfill concrete riprap RCC
Type is Raschig ring, and Pall ring, square saddle or ripple packing can also be met.
The nitrate reductase reactor use coal-ethylene glycol synthesis system circulating air, nitrate reductase catalyst therein without
Need heating reduction and passivation.
The nitrate reductase reactor specification is 1~3 meter of diameter, 20~30 meters of height.
The preceding stripping tower and rear stripping tower gas phase use pure carbon monoxide.
Embodiment two
The method that coal-ethylene glycol carbonylation system reclaims methyl nitrite, this method includes：In ethylene glycol production process
Before esterification reaction solution is admitted to through pipeline in stripping tower liquid phase preheater, be preheated to the liquid after 60~80 DEG C pass through through pipeline it is preceding
The tower top that the upper end entrance of stripping tower enters preceding stripping tower is sprayed, and the gas phase filled into preceding air lift tower bottom is entered in packing layer
The reverse contact of row, preceding stripper overhead gas phase containing methyl nitrite returns to synthesis system, is used as supplement；The premenstrual gas of liquid after contact
Stripper kettle liquid discharging centrifugal pump enters in nitrate reductase liquid phase heater, and nitrate reductase reactor tower top is sent to after heating,
Co-current contact is carried out with the gas phase that nitrate reductase reactor tower top is filled into, in nitrate reductase beds nitric acid at 50~90 DEG C
With methanol and gas nitric oxide reduction generation methyl nitrite；The methyl nitrite of generation is in nitrate reductase reactor column kettle liquid
Flash tank is sent to using pressure difference, the physical process flashed in flash tank；Flash tank kettle liquid stripping tower liquid phase after
Feed pump is sent to rear stripping tower, and the gas phase filled into rear air lift tower bottom is inversely contacted in packing layer, the nitrous after air lift
Sour methyl esters is sent back in coal-ethylene glycol synthesis system by gaseous phase outlet, and liquid phase returns to methanol fractionation system and recycled.
The coal-ethylene glycol esterification amount of liquid phase is 40~60 tons/h, and concentration of nitric acid is 1~5wt%.
The nitrate reductase reaction equation is。
The preceding stripping tower preheater uses 0.5MPa steam preheatings；The nitrate reductase liquid phase heater uses 0.5MPa
Steam is heated.
Hot(test)-spot temperature is preferably controlled to 75~90 DEG C in the nitrate reductase reactor.
The method for reclaiming methyl nitrite using the coal-ethylene glycol carbonylation system in embodiment two carries out nitrous acid
Methyl esters is reclaimed, and have recorded three groups of production removal process, wherein first two groups are the data analyses made for independent air lift system, it is main
Illustrate its air lift effect.Three groups of data are as follows：
First group of each phase data：Preceding stripping tower tolerance is 1000Nm3/h, component carbon monoxide content 99%, methyl nitrite
Content is 0%, 55 tons/h of esterifying liquid phase flow rate, component methanol content 60%, and preceding stripping tower liquid phase preheater controls temperature 60 C, preceding
Stripping tower gas phase inlet pressure 0.35MPa, top gaseous phase outlet pressure 0.15MPa, obtaining gaseous phase outlet component analysis data is
CO contents 75%, methyl nitrite content 18%.It is computed, preceding stripping tower gaseous phase outlet methyl nitrite amount is 237.6Nm3/h,
Air lift and 237.6Nm3/h methyl nitrite gases are flashed off namely from esterification liquid phase.Nitrate reductase liquid phase is heated
Device controls tower top temperature to be 70 DEG C, and nitrate reductase reactor inlet tolerance is 4000Nm3/h, and component carbon monoxide content 40% is sub-
Methyl nitrate content 6%, liquid phase nitric acid content is 3%, obtains outlet liquid phase analysis data nitric acid content 0.5%.It is computed, nitric acid
Reduction is converted into methyl nitrite amount for 489Nm3/h.Stripping tower entrance tolerance 1000Nm3/h, component carbon monoxide content afterwards
99%, methyl nitrite content is 0%, and rear stripping tower gas phase inlet pressure 0.35MPa, top gaseous phase outlet pressure 0.15MPa are obtained
It is CO contents 95%, methyl nitrite content 3% to gaseous phase outlet component analysis data.It is computed, rear stripping tower gaseous phase outlet is sub-
Methyl nitrate amount is 31Nm3/h.
Second group of each phase data：Preceding stripping tower tolerance is 1000Nm3/h, component carbon monoxide content 99%, nitrous acid
Methyl ester content is 0%, 55 tons/h of esterifying liquid phase flow rate, component methanol content 60%, and preceding stripping tower liquid phase preheater controls temperature 70
DEG C, preceding stripping tower gas phase inlet pressure 0.35MPa, top gaseous phase outlet pressure 0.15MPa obtain gaseous phase outlet component analysis number
According to for CO contents 70%, methyl nitrite content 22%.It is computed, preceding stripping tower gaseous phase outlet methyl nitrite amount is 311Nm3/
H, that is, air lift and flash off 311Nm3/h methyl nitrite gases from esterification liquid phase.Nitrate reductase liquid phase is heated
Device controls tower top temperature to be 80 DEG C, and nitrate reductase reactor inlet tolerance is 4000Nm3/h, and component carbon monoxide content 40% is sub-
Methyl nitrate content 6%, liquid phase nitric acid content is 3%, obtains outlet liquid phase analysis data nitric acid content 0.3%.It is computed, nitric acid
Reduction is converted into methyl nitrite amount for 528Nm3/h.Stripping tower entrance tolerance 2000Nm3/h, component carbon monoxide content afterwards
99%, methyl nitrite content is 0%, and rear stripping tower gas phase inlet pressure 0.35MPa, top gaseous phase outlet pressure 0.15MPa are obtained
It is CO contents 90%, methyl nitrite content 6% to gaseous phase outlet component analysis data.It is computed, rear stripping tower gaseous phase outlet is sub-
Methyl nitrate amount is 132Nm3/h.
3rd group of each phase data：Preceding stripping tower tolerance is 1500Nm3/h, component carbon monoxide content 99%, nitrous acid
Methyl ester content is 0%, 55 tons/h of esterifying liquid phase flow rate, component methanol content 60%, and preceding stripping tower liquid phase preheater controls temperature 70
DEG C, preceding stripping tower gas phase inlet pressure 0.35MPa, top gaseous phase outlet pressure 0.15MPa obtain gaseous phase outlet component analysis number
According to for CO contents 66%, methyl nitrite content 25%.It is computed, preceding stripping tower gaseous phase outlet methyl nitrite amount is 562.5Nm
3/h, that is, air lift and flash off 562.5Nm3/h methyl nitrite gases from esterification liquid phase.Flash tank pressure control
0KPa, gaseous phase outlet flow 360Nm3/h are made as, gas phase analysis data, component methyl nitrite content is 75%.It is computed, dodges
Methyl nitrite amount is flashed off in steaming pot nitrate reductase liquid phase for 270Nm3/h.
The present invention is illustrated by above-described embodiment, rather than the limitation to invention protection domain, it is possible to understand that closed above
In the technical scheme described by the embodiment of the present invention, it will be understood by those within the art that, can be to present invention progress
Modification or equivalent substitution, to reach identical technique effect；As long as meeting practical needs, all protection scope of the present invention it
It is interior.
Claims (10)
1. the system that a kind of coal-ethylene glycol carbonylation system reclaims methyl nitrite, it is characterised in that：Before the system includes
Air stripping unit, nitrate reductase unit and rear air stripping unit, the preceding air stripping unit include preceding stripping tower liquid phase preheater, preceding air lift
Tower and preceding air lift tower bottoms discharging centrifugal pump, preceding stripping tower lower end is provided with gas phase entrance；Nitrate reductase unit includes nitric acid also
Stoste heat phase device and nitrate reductase reactor, nitrate reductase reactor upper end are provided with gas phase entrance；Air stripping unit includes afterwards
Stripping tower liquid phase feeding pump and rear stripping tower afterwards；The liquid phase inlet duct that the preceding stripping tower liquid phase preheater passes through preceding stripping tower
It is connected with end entrance on preceding stripping tower, air lift tower bottoms discharging centrifugal pump, preceding gas before preceding stripping tower lower end liquid-phase outlet is connected with
Stripper kettle liquid discharging centrifugal pump is connected on nitrate reductase liquid heater, and nitrate reductase liquid heater is connected to nitrate reductase reaction
The porch of device, stripping tower liquid phase feeding pump, rear stripping tower liquid phase feeding pump after the lower end outlet connection of nitrate reductase reactor
It is connected on rear stripping tower, the top gaseous phase of rear stripping tower is connected in coal-ethylene glycol synthesis system.
2. the system that coal-ethylene glycol carbonylation system according to claim 1 reclaims methyl nitrite, its feature exists
In：The rear air stripping unit also includes a flash tank, and the liquid phase entrance of flash tank is connected to nitrate reductase reactor by pipeline
Liquid-phase outlet at, stripping tower liquid phase feeding pump after being connected at the liquid-phase outlet of flash tank, the connection of rear stripping tower liquid phase feeding pump
On rear stripping tower.
3. the system that coal-ethylene glycol carbonylation system according to claim 1 reclaims methyl nitrite, its feature exists
In：The liquid phase inlet duct of the preceding stripping tower is provided with temperature control valve (TCV), and the gas phase inlet duct of preceding stripping tower is provided with stream
Adjustable valve；The nitrate reductase liquid phase heater liquid-phase outlet connects 0.5MPa jet chimneys, in the 0.5MPa jet chimneys
It is provided with temperature control valve (TCV).
4. the system that coal-ethylene glycol carbonylation system according to claim 1 reclaims methyl nitrite, its feature exists
In：The nitrate reductase reactor gas phase inlet duct is provided with flow control valve；It is connected with to vacuumize on the flash tank and sets
Standby, the sub- ester component for being flashed in flash tank is recycled in synthesis system, and the entrance of vaccum-pumping equipment is provided with pressure regulation
Valve, for stablizing flash tank pressure；The rear stripping tower gas phase inlet duct is provided with flow control valve.
5. the system that coal-ethylene glycol carbonylation system according to claim 1 reclaims methyl nitrite, its feature exists
In：The preceding stripping tower specification be 1~2 meter of diameter, height 10~25 meters, 10~30 layers of the column plate number of plies, tray type is bubble-cap
Formula, float-valve type or sieve-board type.
6. the system that coal-ethylene glycol carbonylation system according to claim 1 reclaims methyl nitrite, its feature exists
In：The rear stripping tower specification is 0.5~2 meter of diameter, and highly 6~15 meters, 3~5 meters of dumped packing height, wire feeding is drawing
Western ring, Pall ring, square saddle or ripple packing.
7. a kind of system using described in claim 1 carries out the side that coal-ethylene glycol carbonylation system reclaims methyl nitrite
Method, it is characterised in that：This method includes：Stripping tower liquid phase before esterification reaction solution in ethylene glycol production process is admitted to through pipeline
In preheater, the tower top that the liquid after 60~80 DEG C enters preceding stripping tower through pipeline by the upper end entrance of preceding stripping tower is preheated to
Sprayed, the gas phase filled into preceding air lift tower bottom is inversely contacted in packing layer；The premenstrual stripping tower of liquid after contact
Kettle liquid discharging centrifugal pump enters in nitrate reductase liquid phase heater, nitrate reductase reactor tower top is sent to after heating, with nitre
The gas phase that sour reduction reactor tower top is filled into carries out co-current contact, in nitrate reductase beds nitric acid and first at 50~90 DEG C
Alcohol and gas nitric oxide reduction generation methyl nitrite；The methyl nitrite of generation is mutually passed through in nitrate reductase reactor column kettle liquid
Stripping tower liquid phase feeding pumps stripping tower backward afterwards, and the gas phase filled into rear air lift tower bottom is inversely contacted in packing layer,
Methyl nitrite after air lift is sent back in coal-ethylene glycol synthesis system by gaseous phase outlet.
8. the method that coal-ethylene glycol carbonylation system according to claim 7 reclaims methyl nitrite, its feature exists
In：The methyl nitrite of generation is sent to flash tank in nitrate reductase reactor column kettle liquid using pressure difference, is sent out in flash tank
The physical process of raw flash distillation；Flash tank kettle liquid stripping tower liquid phase feeding after pumps stripping tower backward.
9. the method that coal-ethylene glycol carbonylation system according to claim 7 reclaims methyl nitrite, its feature exists
In：The preceding stripping tower preheater uses 0.5MPa steam preheatings；The nitrate reductase liquid phase heater uses 0.5MPa steam
Heating.
10. the method that coal-ethylene glycol carbonylation system according to claim 7 reclaims methyl nitrite, its feature exists
In：Hot(test)-spot temperature is preferably controlled to 75~90 DEG C in the nitrate reductase reactor.
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| CN109456197A (en) * | 2018-10-26 | 2019-03-12 | 新疆天智辰业化工有限公司 | A kind of method that low concentration nitric acid solution recycles in calcium carbide stove exhaust preparing ethylene glycol |
| CN109734559A (en) * | 2019-03-05 | 2019-05-10 | 西南化工研究设计院有限公司 | The energy saving technique and system of nitrous acid ester regeneration by-product dust technology in ethylene glycol preparation |
| CN110551025A (en) * | 2019-09-02 | 2019-12-10 | 湖北三宁化工股份有限公司 | system and method for recovering and refining by-product methyl formate in coal-to-ethylene glycol process |
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| CN109734559A (en) * | 2019-03-05 | 2019-05-10 | 西南化工研究设计院有限公司 | The energy saving technique and system of nitrous acid ester regeneration by-product dust technology in ethylene glycol preparation |
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| CN113979867A (en) * | 2020-07-27 | 2022-01-28 | 中国石油化工股份有限公司 | Nitric acid reduction equipment and method |
| CN113979867B (en) * | 2020-07-27 | 2024-03-26 | 中国石油化工股份有限公司 | Nitric acid reduction equipment and method |
| CN114768700A (en) * | 2022-03-31 | 2022-07-22 | 中国神华煤制油化工有限公司 | Nitric acid reduction device and method for reducing nitric acid |
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