CN101643220A - Natural gas type synthesis ammonia energy-saving and emission-reduction technology - Google Patents
Natural gas type synthesis ammonia energy-saving and emission-reduction technology Download PDFInfo
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Abstract
The invention discloses a natural gas type synthesis ammonia energy-saving and emission-reduction technology, which is characterized in that: a methodology of process systems engineering is adopted torealize mass-energy comprehensive integration, particularly comprising the following steps: carbon dioxide in one section of furnace flue gas is recovered by adopting a combined method of membrane separation and chemical adsorption; deeply cooling, distilling and recovering argon gas in purge gas of a hydrogen recovery device; a great quantity of low-temperature waste heat at the outlet positionof the top of a regenerating tower and an ice engine is recycled by adopting heat pump technology, so as to save cold of the ice engine and pre-heating boiler water; a similar device is used as a reference, the proposal is close to zero discharge, greenhouse gas emission load can be reduced by 50 percent to 100 percent, and carbon dioxide and argon gas are by-products at the same time, and the unit consumption of a product can reach 31GJ/tNH3, and compared with the original process, the energy saving can reach 5 percent to 15 percent. The technology is particularly suitable for the existing synthesis ammonia device which takes natural gas as raw material, so as to carry out energy-saving and emission-reduction technology reconstruction, the energy consumption of the natural gas type synthesis ammonia device based on the design of the proposal is the lowest level in the national similar devices.
Description
Technical field
The invention belongs to process industry technical fields such as petrochemical industry and chemical fertilizer, be specifically related to a kind of energy-saving and emission-reduction technology of natural gas type synthesis ammonia device.
Background technology
Ammonia is one of important chemical product, occupies critical role in national economy.The nitrogenous fertilizer that uses on the agricultural all is raw material production with ammonia mostly.The annual synthetic ammonia output in the world has reached more than 100,000,000 tons, wherein has 80% ammonia to be used for producing chemical fertilizer, 20% raw material as other Chemicals approximately.The synthetic raw material mainly comprises Sweet natural gas, light oil, heavy oil and coal.Consider that based on the device economy China is with coal and the Sweet natural gas raw material main body as synthetic ammonia installation.At present, about 22 covers of large-scale natural gas type synthetic ammonia installation are arranged, its derived product is urea except that 1 covering device is produced nitrophosphate fertilizer.Wherein the natural gas type synthesis ammonia device is external imported technology, according to the patented technology branch: Kellogg traditional technology (10 cover), Kellogg-TEC technology (2 cover), Topsoe technology (3 cover) are arranged, and the nineties in 20th century energy-saving AMV technology (2 cover), Braun technology (4 cover), the KBR technology (1 cover) introduced, compiled natural gas type synthesis ammonia Technology main in the world today.The about 37GJ/tNH of average energy consumption of present imported unit
3, the off gas treatment aspect is removed red skyization stack gas is recycled, and other is all directly arranged to atmosphere.
Situation analysis according to the synthetic ammonia technical development, the change of principle will can not appear in the basic production principle of estimating following synthetic ammonia, its technical development will continue closely to center on the elementary object of " reduce production costs, improve the cycle of operation; improve economy ", further concentrates on aspects such as " maximization, less energy-consumption, structural adjustment, cleaner production, long-term operations " and carries out the Study on Technology exploitation.Do not generate or seldom generate by product, refuse in the production process, realize or will reach its maturity and constantly perfect near the clearer production technology of " zero release ".
Main less energy-consumption natural gas type synthesis ammonia technology mainly is published in the external relevant patent, and offshore companies such as Kellogg, Braun and ICI all developed the Sweet natural gas ammonia synthesis process of less energy-consumption.Foreign patent mainly comprises: WO070189; WO042050; US5,523,483; US5,223,238; US5,176,800; US4,464,228; US6,015,537 etc., the reaction that these patents are set forth with separate, associated viscera such as energy-conservation and consumption reduction is important references of the present invention.But the main power-economizing method of these technologies concentrates on the structure of modification of primary reformer and secondary reformer, the conversion catalyst reduction conversion furnace temperature of using the advanced person and the research of novel low pressure synthetic catalyst etc., and exhaust gas emission in the technology, low temperature exhaust heat utilization etc. does not take into full account.
Proposition that Chinese patent CN01134103.3 " reclaims the compound amine solvent of low fractional pressure carbon dioxide " is used amine aqueous solution directly to reclaim low fractional pressure carbon dioxide and is applied to the red skyization stack gas in Guizhou and reclaims, but the carbon dioxide recovery amount only is three to four tphs.Chinese patent CN98801269.3 " purification of argon method and device thereof " has proposed refining processing method and the device thereof that contains the argon gas of impurity and reclaim high purity argon, is applicable to refining argon gas of discharging from the pulling single crystal silicon device.Chinese patent CN94101106.2 " reclaims the technology of argon gas " to greatest extent from air-seperation system with high recovery of argon, CN93119154.8 " low temperature distillation system of band thermally integrated argon column " has proposed to reclaim from air-seperation system argon gas technology and device.And the using heat pump technology reclaims the process unit that low temperature exhaust heat is used to save cold and yet there are no report in synthetic ammonia installation.
By with can and the technical Analysis of emission level, domestic is that the synthetic ammonia installation of raw material still has the space of energy-saving and emission-reduction greatly with the Sweet natural gas on technology.
Summary of the invention
The energy-saving and emission-reduction technology that the purpose of this invention is to provide a kind of natural gas type synthesis ammonia device promptly adopts the methodology of process system engineering to realize the mass-energy comprehensive integration, be specially adapted to existing be that the synthetic ammonia installation of raw material carries out technological transformation with the Sweet natural gas.Adopt membrane separating method pre-treatment primary reformer stack gas, improve gas concentration lwevel, re-use the technical grade carbonic acid gas that the hot potassium carbonate chemical absorption method obtains 99% concentration, be used for urea synthesis, or the further refining food-grade carbon-dioxide of producing; Argon gas during the employing cryogenic rectification speeds to exit to hydrogen recovery unit is recycled; In conjunction with the low temperature exhaust heat in the heat pump techniques recovery process, be used to save cold and preboiler water.Same device energy consumption based on this conceptual design is domestic minimum level.
Technical scheme of the present invention comprises the recovery of carbonic acid gas in the stack gas, the recovery of argon gas during hydrogen recovery unit speeds to exit, and low temperature exhaust heat utilizes three aspects.
1. the recovery of carbonic acid gas in the stack gas (referring to accompanying drawing 1)
The main component of synthetic ammonia primary reformer flue gas is generally (volumetric molar concentration): CO
27.18%, N
273.7%, O
25.41% and H
2O 13.71%.At CO in the flue gas
2The characteristics that concentration is low at first adopt membrane sepn pre-treatment stack gas, utilize CO
2Easier characteristics by film improve CO
2Concentration, and can be according to actual CO
2Demand adjust flue gas and cross film pressure.The gas concentration lwevel of carrying after dense can reach 30%～60%, by conventional hot potassium carbonate chemical absorption process, can obtain 99% technical grade carbonic acid gas again.
The technical grade carbonic acid gas mainly can be used for the further production of ammonia synthesis urea.Can see by ammonia synthesis reaction and urea synthesis reaction, if synthetic ammonia all is used for producing urea, the byproduct amount of carbon dioxide of synthetic ammonia process itself is insufficient, so the carbonic acid gas that reclaims from flue gas not only can reduce the discharging of greenhouse gases, more balance ammonia and urea production, further the urea of expanding production provides necessary carbonic acid gas.Unnecessary technical grade carbonic acid gas also can be used for oil production, welding, industrial uses such as steel furnace bottom air blowing.If further through overdraft, smart desulfurization, purge drying and sterilization taste removal, condensation enters rectifying tower and is refined into food-grade carbon-dioxide more than 99.95% then, can be used for foodstuff additive, a plurality of fields such as fresh-keeping.
2. the recovery (referring to accompanying drawing 2) of argon gas during hydrogen reclaims and speeds to exit
Generally contain molar fraction during hydrogen reclaims and to speed to exit near about 10% argon gas, argon is the very wide rare gas of present industrial application.In Metal smelting, aircraft manufacturing, shipbuilding, nuclear industry and electronic industry, need make protection gas with argon in a large number.
Argon gas reclaims the method that adopts cryogenic rectification, and the main component of speeding to exit is hydrogen, nitrogen, methane and argon gas, and through at first passing through the washing cooling of cyclic nitrogen after the simple dry pre-treatment, most hydrogen separates to walk from scrubber overhead; Methane at the bottom of the tower, argon gas and nitrogen enter demethanizing tower and remove methane, demethanizer pressure is 1MPa, tower top temperature then enters the purification of argon tower for-170 ℃ argon gas and nitrogen, be 99.9% straight argon product at the bottom of the purification of argon Tata, send into the ammonia synthesis unit behind the hydrogen mixing match of the nitrogen of cat head and rough segmentation tower as the required nitrogen hydrogen of reaction.
3. the utilization of low temperature exhaust heat
In routine is in the synthetic ammonia process of raw material with the Sweet natural gas, a large amount of low temperature exhaust heats is arranged because the recovery difficulty is wasted, and is mainly the condensation (42 ℃) of decarburization flow process regenerator column cat head steam condensation (100 ℃) and ice maker outlet high pressure ammonia.Though these low temperature exhaust heat temperature are not high, heat is very big.So this programme in conjunction with heat pump techniques, adopts LiBr-H
2The heat of the O absorption type heat umformer reclaiming cat head gas that generates after low-temperature cold water cools off ammonia synthesis, the cold of saving ice maker; Adopt compression heat pump to reclaim ice maker outlet ammonia refrigerative heat and be used for preboiler water.
Referring to accompanying drawing 3, lithium bromide absorbing type refrigeration is to be that 100 ℃ low temperature exhaust heat (condensation of regenerator column cat head steam) is as the driving heat source of heat pump producer with temperature; Temperature is the vaporizer that 13 ℃ low-temperature circulating water infeeds heat pump, exports the low-temperature receiver as synthetic gas in vaporizer after the reduction temperature; With recirculated cooling water the resorber and the condenser heat of heat pump are taken away.Drive heat Q
1In the input generator, the heating lithium-bromide solution makes it the desorb of seething with excitement, and produces water vapor, and lithium-bromide solution thickens simultaneously, and water vapor enters condenser and is condensed into liquid, heat Q
4Taken away by recirculated cooling water, water-setting is become liquid state and enter vaporizer after throttling, under low pressure is evaporated to steam, absorbs vaporization heat Q
2, steam enters resorber, and the strong solution that is absorbed in the device absorbs the hot Q of the absorption of emitting
3Taken away by recirculated cooling water, the bromize lithium dilute solution of formation is delivered in the producer by solution pump, finishes a circulation.
Referring to accompanying drawing 4, compression heat pump is the states of matter variation by working medium in the system, i.e. the characteristic of vaporization heat absorption, condensation heat release realizes heat supply.With the driving heat of 42 ℃ of low temperature exhaust heats (ice maker outlet ammonia condensing) as vaporizer, the working medium R134a (CF of vaporizer opposite side
3CH
2F) the heat Q of absorption low temperature exhaust heat
1Back vaporization, steam is sucked by compressor, and adiabatic compression is to condensing pressure, temperature increase to 90 ℃.Under this pressure, working medium is emitted heat Q
2Preboiler water is converted to liquid from steam.Liquid refrigerant is by throttling valve then, and pressure enters the vaporizer circulation after reducing to evaporating pressure again.
The present invention has significantly reduced the energy consumption and the discharging of natural gas type synthesis ammonia device, by stack gas and off-gas reclaim, the utilization of low temperature exhaust heat realized energy-saving and emission-reduction.Based on the same device of above-mentioned serial conceptual design, discharging reduces significantly with energy consumption.Present technique has good controllability and stability, is very suitable for the technological transformation of existing apparatus.
Description of drawings
Fig. 1: stack gas carbon dioxide recovery process flow sheet
Fig. 2: the recovery process flow sheet of argon gas during hydrogen reclaims and speeds to exit
Fig. 3: absorption type heat umformer process flow sheet
Fig. 4: compression heat pump process flow sheet
Accompanying drawing 1---accompanying drawing 4 marks are as follows:
1. dry preprocessor 2. preliminary treatment heat exchangers 3. membrane separators 4. carbon dioxide absorption towers 5. hydraulic turbines 6. carbon-dioxide regenerating towers 7. carbon-dioxide regenerating tower steam reboilers 8. lean solution coolers 9. lean pumps 10. flash tanks 11. semi-leanpumps 12. carbon-dioxide regenerating tower evaporator overhead condensers 13. carbon-dioxide regenerating tower return tanks 14. carbon-dioxide regenerating tower evaporator overhead condensers 15. regenerator return tanks 16. absorber 17. inlet outlet heat exchangers 18. scrubbing towers 19. domethanizing columns 20. argon gas treating columns 21. basins 22. nitrogen hydrogen valves 23. compressors 24. heat exchangers 25. heat exchangers 26. decompressors 27. absorbers 28. evaporimeters 29. condensers 30. generators 31. heat exchangers 32. choke valves 33. compressors 34. heat exchangers 35. choke valves 36. heat exchangers of speeding to exit
Embodiment
Be described in detail the specific embodiment of the invention below in conjunction with technical scheme and accompanying drawing.
With reference to throughput is the Kellogg type synthetic ammonia installation of 62.5t/h, and this scheme unit consumption of product is compared previous level decline 2.5GJ/t.Reclaim the carbonic acid gas 34t/h of discharging, argon gas 1t/h.Be suitable for existing Sweet natural gas synthetic ammonia installation is carried out the energy-saving and emission-reducing technique transformation.
1. details are as follows for stack gas carbon dioxide recovery part:
The flue gas that the back flow of pressurization is 380t/h is through the super-dry pre-treatment, after most of water is removed, enter membrane separation apparatus, because the easier film that passes through of carbonic acid gas, about 80% carbonic acid gas has entered infiltration gas, permeate simultaneously that concentration of carbon dioxide has reached more than 30% in the gas, other consist of nitrogen and a spot of oxygen.Permeate gas then and enter CO
2Absorption tower, gas enter at the bottom of by tower, and the two layers of filler of upwards flowing through contact most of CO with the Benfield solution that flows down
2Be absorbed.Benfield solution highly enters CO from two
2The absorption tower.The hypomere of tower is removed most of CO in the gas with semi lean solution
2, lean solution is taken out the sparger at past top, absorption tower from the bottom of regenerator column with lean pump.Lean pump export some by mechanical filter to remove the solid impurity that may sneak into continuously.
Mixed salt of wormwood rich solution gathers in the bottom on absorption tower, by the top of delivering to regenerator column after the fluid level controller adjusting liquid level.Because the pressure on absorption tower is higher, can be used to drive hydraulic turbine recovered energy from effusive salt of wormwood rich solution.The salt of wormwood rich solution is emitted a part of CO in the top flash distillation
2Regenerator column solution divides two sections operations, and the epimere of tower has two-layer integrated filler, and rich solution is taken a part of CO out of from top to bottom and by mobile steam from bottom to top
2, some delivers to the semi lean solution flash drum from the catch tray of second layer filler bottom this semi lean solution.Remaining semi lean solution continues to be downward through packing layer, and solution is assembled in the catch tray of the bottom of regenerator column, flows into reboiler more thus.The absorption tower circulation is sent into after reclaiming heat through heat exchange in the bottom that lean solution accumulates in regenerator column.
Above the regenerator column rich solution ingress scum dredger is arranged, be used for reducing the salt of wormwood drop that gas is carried secretly, on foam-removing layer, also have three layers of bubble plate to be used for the solution of potassium carbonate that washing gas takes out of with further minimizing.Washings is exactly the phlegma above the regenerator column.The CO that desorbs
2Leave the regenerator column top and just pass through CO later on
2The regenerator column water cooler, the moisture of carrying secretly in the gas just separates in separating tank later in this condensation.Part phlegma is returned system through regenerator reflux pump.Last volumetric molar concentration is about 99% technical grade CO2 and is sent to urea plant or food-grade carbon-dioxide device after by foam-removing layer.
Details are as follows for the argon gas recovery part:
The hydrogen recovery unit mole of speeding to exit consists of 9% argon gas, 16% hydrogen, 54% nitrogen and 21% methane, speed to exit and at first remove water and the ammonia of carrying secretly on a small quantity by adsorption unit, in case they freeze at cold zone, through importing and exporting interchanger and product gas (methane and hydrogen and nitrogen gas) heat exchange, reach the purpose of precooling air inlet and heating products gas again.
The venting of speeding after the precooling enters at the bottom of the washing Tata, and through scrubbing with liquid nitrogen, most hydrogen mixes with nitrogen from cat head, as synthetic pneumatic transmission synthesis unit.1.4MPa at the bottom of the tower (cutting off), about-159 ℃ methane, argon and nitrogen are sent into demethanizing tower, and demethanizer is pressed and is about 1MPa (cutting off), and tower top temperature is about-170 ℃, and the cat head discharging is nitrogen and argon, and wherein methane content is less than 0.1%.Nitrogen and argon are sent into the purification of argon tower subsequently, are separated into synthetic nitrogen (cat head) and the pure hydrogen (bottom) used in the purification of argon tower, and the purification of argon Tata is pressed about 0.75MPa (cutting off), is 99.9% straight argon product at the bottom of the tower, and temperature is-160 ℃, flow 1t/h.The elevated pressure nitrogen circulation of band decompressor produces the required cold of argon liquefaction, and as the compensation of heat waste and imperfect heat exchange.
Details are as follows for the low temperature exhaust heat recovery part:
The steam of Benfield decarburization flow process regenerator column cat head is 100 ℃ of left and right sides condensations, the about altogether 60GJ/h of the low temperature exhaust heat that brings, wherein about 40GJ/h is that the lithium-bromide solution of 70mmHg makes it the desorb of seething with excitement as the driving heat heated pressure of producer, produce water vapor, lithium-bromide solution thickens simultaneously, water vapor enters condenser and is condensed into liquid, heat is taken away by recirculated cooling water, water-setting is become liquid state and is entered vaporizer through being throttled to 7mmHg, under low pressure be evaporated to steam, absorb vaporization heat, making temperature is that 13 ℃ low-temperature circulating water reduces the temperature to 6 ℃ of low-temperature receivers as synthetic gas at the vaporizer opposite side.Steam behind the absorption heat enters resorber, and the strong solution that is absorbed in the device absorbs, and the absorption heat of emitting is taken away by recirculated cooling water, and the bromize lithium dilute solution of formation is delivered in the producer by solution pump, continues circulation next time.This flow process utilizes low temperature exhaust heat to produce 6 ℃ cold water, and behind supercooled water, it is cold to increase by 6 ℃ of cold water at original synthetic gas, and it is cold to carry out ammonia again, can save the cold of ice maker 30GJ/h.
The high pressure ammonia of ice maker outlet is 42 ℃ of left and right sides condensations, and the low temperature exhaust heat total amount of bringing reaches 90GJ/h, and with its driving heat as vaporizer, the working medium R134a of vaporizer opposite side vaporizes behind the heat that absorbs low temperature exhaust heat under the evaporating pressure of 0.6MPa (cutting off).Steam after the vaporization is sucked by compressor, and adiabatic compression is to condensing pressure 1.8MPa (cutting off), temperature increase to 90 ℃.Under this pressure, working medium is emitted heat with the feedwater heat exchange that needs heating, is liquid from vapor condensation.Liquid refrigerant is reduced to evaporating pressure by throttling valve and is entered vaporizer more then, enters circulation next time.This flow process reclaims low temperature exhaust heat 49GJ/h altogether and is used for preboiler water and heat supply in winter.
Claims (1)
1. the energy-saving and emission-reduction technology of a natural gas type synthesis ammonia device, promptly adopt the methodology of process system engineering to realize the mass-energy comprehensive integration, comprise that specifically the method for using membrane sepn to combine with the hot potassium carbonate chemical absorption reclaims the carbonic acid gas in the primary reformer flue gas, be used to produce urea, or the further refining food-grade carbon-dioxide of producing; Argon gas in by cryogenic rectification hydrogen recovery unit being speeded to exit is further recycled; Use a large amount of low temperature exhaust heats in heat pump techniques reclaiming column overhead and ice maker exit, be used to save ice maker cold and preboiler water, it is characterized in that:
(1). carbon dioxide recovery in the primary reformer stack gas: primary reformer stack gas is not directly arranged to atmosphere, passes through membrane separation apparatus earlier after most water is removed in the super-dry pre-treatment.Reach more than 30% by carbon dioxide content in the infiltration gas behind the membrane separation apparatus, enter CO then
2Absorption tower, gas enter at the bottom of by tower, and the packing layer of upwards flowing through contacts CO with the Benfield solution that flows down
2Be absorbed, accumulating in becomes the salt of wormwood rich solution at the bottom of the tower and delivers to the regenerator column top, and rich solution is taken out of carbonic acid gas by mobile steam from top to bottom, the CO that desorbs
2Leave after the regenerator column top by water cooler and foam-removing layer, remaining mass is formed and is about 99% carbonic acid gas and is sent to urea plant or food-grade carbon-dioxide device.
(2). the argon gas during hydrogen recovery unit speeds to exit reclaims: the venting of speeding of hydrogen recovery unit is not directly arranged to atmosphere, reclaims the argon gas of wherein enrichment through cryogenic rectification.Speed to exit and pass through washing tower, demethanizing tower and argon gas rectifying tower successively after the precooling, remove hydrogen, methane and nitrogen at low temperatures successively, the elevated pressure nitrogen circulation of band decompressor produces speeds to exit the required cold of liquefaction, as the compensation of thermosteresis and imperfect heat exchange.Hydrogen and nitrogen are sent synthesizing section back to as the synthetic unstripped gas, are the argon gas product of composition more than 99.9% at the bottom of the argon gas rectifying Tata.
(3). adopt LiBr-H2O absorption type heat umformer to reclaim the low temperature exhaust heat of decarburization flow process regenerator column cat head steam condensation: the steam of decarburization flow process regenerator column cat head is 100 ℃ of left and right sides condensations, the low temperature exhaust heat that brings is as driving heat, the heating lithium-bromide solution makes it the desorb of seething with excitement, and produces water vapor.Lithium-bromide solution thickens simultaneously, water vapor enters condenser and is condensed into liquid, heat is taken away by recirculated cooling water, water-setting is become the liquid vaporizer that enters after throttling, under low pressure absorbing heat of vaporization is steam, meanwhile temperature is that low-temperature circulating water between 13 ℃ to 20 ℃ reduces the temperature to 6 ℃ at the vaporizer opposite side, and output is as synthetic gas refrigerating low-temperature receiver.Water vapor enters resorber after leaving vaporizer, and the strong solution that is absorbed in the device absorbs, and the absorption heat of emitting is taken away by recirculated cooling water, and the bromize lithium dilute solution of formation is delivered in the producer by solution pump, finishes once circulation.
(4). adopt compression heat pump to reclaim the low temperature exhaust heat of ice maker outlet high pressure ammonia condensation: the high pressure ammonia of ice maker outlet is 42 ℃ of left and right sides condensations, and the low temperature exhaust heat that brings is as the driving heat of vaporizer, the working medium R134a (CF of opposite side
3CH
2F) vaporize behind the heat that absorbs low temperature exhaust heat under the evaporating pressure of 600KPa (cutting off), steam is sucked by compressor, and adiabatic compression is to condensing pressure 1.8MPa (cutting off), temperature increase to 90 ℃.Under this pressure, working medium is emitted heat preboiler water, is converted to liquid from steam.Liquid refrigerant is by throttling valve then, and pressure enters vaporizer after reducing to evaporating pressure again, finishes once circulation.
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| CN103398547A (en) * | 2013-07-30 | 2013-11-20 | 江苏中核华纬工程设计研究有限公司 | Process of treating purge gas from synthetic ammonia by LNG cold energy |
| CN104787778A (en) * | 2014-01-17 | 2015-07-22 | 气体产品与化学公司 | System and process for producing ammonia using ion transport membrane, gasifier, and ammonia synthesis unit |
| CN104913540A (en) * | 2015-06-25 | 2015-09-16 | 林兆晟 | Air separation waste heat and material integrated utilization system |
| CN105646290A (en) * | 2015-12-30 | 2016-06-08 | 中国石油大学(北京) | Method for recycling CO2 in flue gas of fossil fuel or biomass power plant |
| CN106039960A (en) * | 2016-06-13 | 2016-10-26 | 大连理工大学 | Carbon dioxide capturing and liquefying process stepwise utilizing smoke waste heat |
| CN107514873A (en) * | 2017-08-30 | 2017-12-26 | 浙江大学 | A kind of device and method of synthesis gas isolation of purified |
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| CN109665976A (en) * | 2018-11-15 | 2019-04-23 | 锦西天然气化工有限责任公司 | A kind of ammonia process recycling flue gas CO2With the technique of urea Joint Production |
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