CN1021904C - Method for the production of ammonia and carbon dioxide - Google Patents
Method for the production of ammonia and carbon dioxide Download PDFInfo
- Publication number
- CN1021904C CN1021904C CN87106172A CN87106172A CN1021904C CN 1021904 C CN1021904 C CN 1021904C CN 87106172 A CN87106172 A CN 87106172A CN 87106172 A CN87106172 A CN 87106172A CN 1021904 C CN1021904 C CN 1021904C
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- Prior art keywords
- gas
- steam
- steam reforming
- reaction
- conduit
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/02—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen
- C01B3/025—Preparation or purification of gas mixtures for ammonia synthesis
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/50—Carbon dioxide
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
A process is proposed for preparing ammonia and carbon dioxide, wherein a feed gas rich in light hydrocarbons is converted into a cracked gas by steam reforming. The cracked gas is subjected to carbon monoxide conversion and separated into hydrogen, carbon dioxide and residual gas. The hydrogen thus obtained is fed together with nitrogen into an ammonia synthesis. At least a substream of the feed gas is reacted with oxygen or with oxygen-rich gas, optionally in the presence of steam, and the gas mixture thus generated is supplied to steam reforming combined with the remaining feed gas and the remaining steam required for steam reforming.
Description
The present invention is a kind of method of producing ammonia and carbonic acid gas.In the method, a kind of unstripped gas of rich light hydrocarbon is changed into reacted gas, with separating reacted gas is become hydrogen, carbonic acid gas and residual gas through the carbon monoxide conversion operation again with steam reforming.Hydrogen and nitrogen that this technology makes are delivered to the synthetic ammonia operation together simultaneously.
Using the light hydrocarbon unstripped gas, for example natural gas is produced in the process of synthetic ammonia, at first obtains the reacted gas of hydrogen and carbon oxides with steam reforming, further it is handled making the unstripped gas that is suitable for the synthetic ammonia operation then.In this respect, according to the conventional method, at first make gas that steam reforming operation emits in the twice transformation stove further with air reaction.The hydrocarbon that adopts this technology still to be present in the gas on the one hand further is converted to reacted gas, on the other hand the required nitrogen of synthetic ammonia operation is input into reacted gas.The carbon monoxide that contains in the reacted gas becomes hydrogen and carbonic acid gas with steam reforming again, before not containing remaining carbon oxides impurity in the residual gas, in the methanation step carbonic acid gas is separated from reacted gas at last, delivers to the synthetic ammonia operation.In this reacted gas preparation process, carbonic acid gas is to prepare in the operation of the gas washing of carbonic acid gas as byproduct, can make carbonic acid gas in follow-up urea synthesis operation with the ammonia effect.
In the report of Linde-Berichten aus Technik und Wissenschaft(Linde in 1985 science and technology) a kind of method that further prepares synthetic ammonia gas with simple process is disclosed in 40～43 pages of the 57th phases.This method is that the reacted gas of will emit from steam converter directly leads in the carbon monoxide conversion operation, has omitted the middle-chain of twice transformation device.Operate in the reacted gas that makes conversion by pressure conversion absorption then and produce flow of pure hydrogen, the required nitrogen of pure hydrogen and synthetic ammonia is mixed.Provide nitrogen with an air separation plant, at last nitrogen and hydrogen mixture is supplied with ammonia synthesis reaction.If in this process, generate the carbonic acid gas composition simultaneously, before absorbing operation, once more carbonic acid gas is carried out gas washing so.
About existing these processing methodes, the weak point under some particular case is, only can make the carbonic acid gas of relatively small amount.For example, this phenomenon just appears when to the further Processing of Preparation urea of ammonia.Especially, in this case, the amount as the carbonic acid gas of synthesis gas of preparation simultaneously only can change into urea with about 85～95% ammonia.Therefore, in this case, common way is nothing more than there being two kinds: or before the synthetic ammonia operation, remove excessive hydrogen, that is to say the output that reduces ammonia; Or excess of ammonia is used to produce other products, for example produce ammonium nitrate or ammonium phosphate.
The objective of the invention is to begin the described technology of part, use this technology can increase the output of carbonic acid gas than prior art by a kind of specification sheets.
The present invention is achieved in that under the condition that has or do not have steam to exist, make the reaction of at least a portion flow of feed gas and oxygen or oxygen rich gas, the gaseous mixture in this step operation is charged into the steam reforming operation with remaining unstripped gas and the required steam of steam reforming operation.
In the method for the invention, additional carbonic acid gas makes by at least a portion unstripped gas and oxygen reaction, and this can realize by accurate stoichiometric calculation mode (quasi-stoichiometric manner) burning.In this course, generate the stack gas of forming by carbonic acid gas and water vapor substantially.Yet also useful indirect method improves the possibility of carbonic acid gas output.For this purpose, one embodiment of the present of invention provide a kind of like this technology, carry out even be reflected to exist under the excessive unstripped gas condition, partial oxidation takes place and produce the stack gas of rich carbon monoxide.The carbon monoxide that forms in this process by conversion reaction, just can be converted into carbonic acid gas at next step.The advantage of this operating procedure is to need the lower work output that has not been cooked or heated long enough in steam converter.
If do not take other measure, the burning of part material air-flow and oxygen can cause very high flame and produce the stack gas that temperature surpasses 3000 ℃, therefore, the invention provides with the water that adds water vapor or evaporation when the time comes and controls the pyritous method.In this, it should be noted that especially this technology will use a part for transforming another part flow of feed gas, in any case be essential water or water vapor in order to control high temperature.
Can reach the effect of limit temperature with several different methods.In one embodiment of the invention, directly reduce temperature at combustion phases by adding entry and/or water vapor, thereby flame temperature is lowered also.Be in another embodiment of the present invention before burn operation, water vapor is fed in part material air-flow and/or the rich oxygen reach effect same.Equally; as an alternative embodiment of the invention, and then combustion phases that is to say lowering the temperature in water and/or the water vapor feeding stack gas; after producing, high flame temperature obtains cooling-down effect again, to reach the purpose that protection is installed in following apparatus assembly.
When adding entry and/or water vapor before the burn operation or in burn operation, should be noted that to keep suitable high temperature, mixture is ignited and burn guaranteeing.In the natural gas burning process, the temperature of flame is remained between 1500～1800 ℃, particularly help burning between 1600～1700 ℃ and carry out.
According to another one embodiment of the present invention, by indirect heat exchange, the gas that produces when making the burning of part material air-flow further cools off.This gas cooling mode is normally essential because with the direct secondary reaction that can cause unallowable high temperature and not wish to take place that mixes of part material air-flow that will be by steam converter.When with Sulfur Contained Raw Gas stream, as Sweet natural gas, be exactly this situation particularly.Flow of feed gas is passed through desulfurization stage earlier before conversion reaction operation, at the state of temperature that raise, for example be output during 400 ℃ of left and right sides.The temperature range of commonly using when entering steam converter is 500～550 ℃, and the temperature of flue gas cools is 500～1100 ℃ before mixing, preferably 600～1000 ℃.For transpiring moisture, preferably cool off indirectly, can obtain the part steam reforming like this and operate needed steam.About this point, in an initial embodiment of the present invention, under the operation pressure of steam reforming operation, just can obtain middle pressure steam, resulting middle pressure steam can be directly used in the steam reforming operation as mentioned above.In another embodiment, also can prepare high pressure steam.Steam enters the high pressure steam device that is connected with equipment through after overheated, expands then.Often be used to steam reforming operation as steam, before superheated vapour further being done work expand, at first make it expand into middle pressure usually.The a part of middle pressure steam that is produced so just can be used further to the steam reforming operation.
In advantageous embodiments of the present invention, the reaction of unstripped gas and oxygen realizes under pressure, the pressure size that is suitable for reacting is not having under the impressed pressure, should reach the gaseous mixture that makes generation and can mix with other air-flow and can charge into steam converter.Therefore, being reflected at the transfer pressure of commonly using and taking place down, is to carry out between 10～35 crust at pressure promptly, and the pressure range that is more suitable for reacting is 15～30 crust.
Reaction can be carried out in general roasting kiln, and for example in this stove, the combustion chamber inwall has fire-resistant lining or ceramic cladding.A specific embodiments of the present invention provides the method for carrying out in immersion heater or the immersion roasting kiln that is reflected at that makes.In this case, stack gas directly makes direct heat exchange produce steam by water-bath, and this part steam can be used as process steam again.Another embodiment of the present invention also has such advantage, and the gaseous mixture that a part can be made circulation feeds roasting kiln, with the temperature of restriction flame.
In another embodiment of the present invention, the reaction of unstripped gas and oxygen is carried out under katalysis.In this working method, a part reaches steam reforming and operates desired an amount of steam and can mix mutually with reaction gas flow.The advantage of this method is noncatalytic combustion will not occur and operate necessary high temperature.On the contrary, temperature of reaction reduces greatly in the production process, and for example, temperature is at 700～900 ℃, especially at 750～800 ℃.
Therefore, described as the beginning part of specification sheets of the present invention, the present invention is particularly suitable for and the ammonia synthesis process logotype, and in the method, the production of synthesis gas can be finished under the situation of applying pressure conversion absorption unit at the different secondary convertor.This technology uses an air cracker to prepare the required nitrogen composition of synthetic ammonia.According to method of the present invention, produce in the air cracker, only be used for and the required combustion air of steam converter blended oxygen mutually so far, have at least a part can be used for and the unstripped gas reaction, saved the step that in the past reaches the necessary both expensive of same purpose.
Represented embodiment further describes feature of the present invention below in conjunction with synoptic diagram of the present invention.
Fig. 1 illustrates the ultimate principle of the inventive method.
Fig. 2 represents a specific embodiment of the present invention.
The embodiment of the invention as shown in Figure 1, unstripped gas, for example Sweet natural gas provides with conduit 1, enters steam converter 3 by conduit 2.Roasting kiln 5 is shunted and passed to partial raw gas with conduit 4, and in roasting kiln, unstripped gas becomes divided combustion with the oxygen that conduit 6 is provided.With adding water into or/and the method for steam is adjusted in the burn operation or the temperature after the burning.Concrete measure is to provide water or water vapor with conduit 7, and water and steam perhaps is provided simultaneously, with conduit 8 it is fed roasting kiln 5 again.The conduit 9 that the steam that conversion operation further needs is represented by a dotted line or 10 is introduced from the stack gas that roasting kiln 5 discharges by conduit 11, feeds conduit 2 at last and enters steam converter with unstripped gas.By conduit 11 from 5 li stack gases of drawing of roasting kiln, with before part material air-flow that conduit 2 provides begins to mix, earlier heat exchanger 12 in the indirect heat exchange process will cooling, so can make process steam.
(do not provide the figure) after overcooling from the reacted gas of 3 li discharges of steam converter, deliver to the carbon monoxide transformation stage 14, make carbon monoxide contained in the reacted gas transform into carbonic acid gas and hydrogen through conduit 13.The gaseous mixture that this conversion operation forms is passed to carbonic acid gas gas washing operation 16 with conduit 15.Through gas washing, carbonic acid gas is discharged out, separates through conduit 17 simultaneously.Remaining air-flow leads to pressure with conduit 18 and transforms absorption unit 19, obtains pure hydrogen at this from reacted gas.Conduit 20 is drawn flow of pure hydrogen, and conduit 21 is drained residual gas simultaneously.Contain the methane that does not react in steam reforming operation 3 in the residual gas, methane can be used as the heated air that has not been cooked or heated long enough of steam reformer 3.Mixed mutually with the nitrogen that conduit 22 provides and become synthetic ammonia gas from installing 19 the hydrogen stream of discharging with conduit 20, then after overdraft (not expressing among the figure) and being heated to synthesis temperature, in synthetic ammonia installation 23, begin to react.The ammonia of producing in 23 is exported by conduit 24 as the product of this technology.
The amount that part is delivered to the flow of feed gas 4 of burn operation 5 can be defined as, make from the ratio of the amount of two kinds of products of conduit 17 and conduit 24 outputs just can be urea synthesis process complete reaction simultaneously.
Supply with the oxygen of burn operation 5 and all preferably be taken from air cracker, particularly low temperature pyrolyzer device with conduit 6 with the nitrogen that the synthetic ammonia that conduit 22 provides is used.
The embodiment of the invention as shown in Figure 2, provide Sweet natural gas as raw material by conduit 25, this gas includes 0.4 mole of % of propane, butane, 1.1 moles of % of phosgene and 0.7 mole of % of nitrogen of the ethane of the methane of 83.3 moles of %, 10.3 moles of %, 4.2 moles of %.Sweet natural gas at first leads to desulfurization stage 26 under the pressure of 30 crust, slough sulphur impurity contained in the Sweet natural gas at this place.Natural gas through desulfurization passes through conduit 27, discharges under 410 ℃ of temperature, is divided into the two-way air-flow then, and the gas of being shunted by conduit 28 burns.The amount of shunting can change according to the required amount of carbon dioxide of technology, for example, can be 5～20% of whole airsheds.In the present embodiment, 11% the gas that accounts for general gas flow by conduit 28 shuntings after, mix with water vapor and oxygen enrichment composition mixing station 29.Specific practice is, conduit 30 provides 121 ℃ to be the oxygen rich gas compositions of 30 crust with pressure, wherein contain the nitrogen of the oxygen of 64.5 moles of %, 32.7 moles of % and the argon gas of 2.8 moles of %, simultaneously 270 ℃ of temperature and pressure are provided is the generation steam of 56 crust to conduit 31, and to expand into pressure be 30 to cling to mixing station to allow steam.Conduit 32 is delivered to roasting kiln 33 to gas mixture from mixing station output, and gas mixture burns under 214 ℃ temperature in roasting kiln.Contain the argon gas of the nitrogen of the propane of the ethane of the methane of the oxygen of the steam of 69.5 moles of %, 15.3 moles of %, 5.6 moles of %, 0.7 mole of %, 0.3 mole of %, 7.8 moles of %, 0.7 mole of % and the carbonic acid gas of 0.1 mole of % in this gas mixture.What discharge from roasting kiln 33 is stack gas 1600 ℃ of generations, wherein contains the argon gas of the carbonic acid gas of the steam of 83.5 moles of %, 8.0 moles of %, 0.7 mole of % and the nitrogen of 7.8 moles of %.Stack gas is by conduit 34 input heat exchangers 35, carries out indirect heat exchange at this and water in the vaporization and forms steam, and conduit 31 cools off the steam that forms and is passed in the mixing section 29 from 35.Stack gas is cooled in heat exchanger 35 after 1188 ℃, enters in next step the heat exchanger 37 by conduit 36 again, at this, in the heat exchanger 35 water that is vaporized is further heated the ebullient temperature.In heat exchanger 39, after stack gas was cooled to 991 ℃, conduit 38 was sent stack gas to mixing section 39, and stack gas is mixed with conduit 40 partial desulfurization Sweet natural gases that provide, that discharge from conduit 27 at mixing section, and then mixes with process steam and process water.
The required whole steam of steam reforming operation (not illustrating at Fig. 2) provide with water by conduit 41.A part with will carry out incendiary part air-flow mutually the blended current through conduit 42, make its pressure be elevated to 56 by pump 43 to cling to, in heat exchanger 37, be heated to boiling temperature then, in heat exchanger 35, vaporize again.It is then straight-through to mixing section 39 by conduit 44 that another part is used to form the water that accounts for steam total amount about 63%.This strand current are divided into two-way through conduit 45 and 46 again.The conduit 45 of leading up to that numerical value is less is supplied with mixing section 39, is heated to 110 ℃ at this water, because indirect heat exchange makes water vapor, mixes under liquid state then.Meanwhile, the current that another way amount is bigger are by conduit 46 input heat exchangers 47.Be heated to 383 ℃ earlier at this, make it vaporization then and import mixing section 39 again.Gas by mixing section 39 outputs will be sent to steam reformer.The pressure of this gas is 29.5 crust, and temperature is 550 ℃.Gas contains the nitrogen of the carbonic acid gas of the propane of the ethane of the methane of the steam of 74.4 moles of %, 16.3 moles of %, 2.0 moles of %, 0.8 mole of %, 3.2 moles of %, 3.0 moles of % and the argon gas of 0.3 mole of %.
Claims (10)
1, a kind of method that when producing ammonia, improves carbonic acid gas output, with steam reforming a kind of unstripped gas of rich light hydrocarbon is changed into reacted gas, with separating reacted gas is become hydrogen through the carbon monoxide conversion operation again, carbonic acid gas and residual gas, wherein hydrogen and nitrogen are delivered to the synthetic ammonia operation together simultaneously, it is characterized in that, under the condition that has or do not have steam to exist, make the reaction of at least a portion flow of feed gas and oxygen or oxygen rich gas, the gaseous mixture that this step operation is produced fills into steam reforming operation with remaining unstripped gas and needed all the other steam of steam reforming operation.
2, in accordance with the method for claim 1, it is characterized in that reacting being actually and under the pressure condition of steam reforming operation, carry out.
3, in accordance with the method for claim 1, it is characterized in that, with the temperature of the method conditioned reaction that adds entry and/or water vapor.
4,, it is characterized in that before the reaction that water vapor and unstripped gas and/or oxygen or oxygen rich gas mix mutually according to claim 1 to 3 any one described method wherein.
5, according to claim 1 to 3 any one described method wherein, it is characterized in that, make the gaseous mixture cooling that produces in the reaction with indirect heat exchange process will.
6, in accordance with the method for claim 5, it is characterized in that, produce a part of steam reforming at least by indirect heat exchange and operate needed steam.
7, in accordance with the method for claim 5, it is characterized in that, in the indirect heat exchange process, make high pressure steam, after high pressure steam expands through overheated and acting, have at least a part to be used to satisfy the needs of steam reforming operation.
8, according to one of them described method of claim 1 to 3, it is characterized in that, be reflected in the immersion burner and carry out.
9, in accordance with the method for claim 8, it is characterized in that the gaseous mixture that part is produced is recirculated to this burner in the immersion burner.
According to one of them described method of claim 1 to 3, it is characterized in that 10, reaction is undertaken by catalyzer.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DEP3630311.9 | 1986-09-05 | ||
| DE19863630311 DE3630311A1 (en) | 1986-09-05 | 1986-09-05 | Process for preparing ammonia and carbon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN87106172A CN87106172A (en) | 1988-06-01 |
| CN1021904C true CN1021904C (en) | 1993-08-25 |
Family
ID=6309016
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN87106172A Expired - Fee Related CN1021904C (en) | 1986-09-05 | 1987-09-04 | Method for the production of ammonia and carbon dioxide |
Country Status (4)
| Country | Link |
|---|---|
| CN (1) | CN1021904C (en) |
| AR (1) | AR241177A1 (en) |
| DE (1) | DE3630311A1 (en) |
| IN (1) | IN169625B (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5011625A (en) * | 1989-12-11 | 1991-04-30 | The M. W. Kellogg Company | Autothermal steam reforming process |
| TR25395A (en) * | 1991-04-05 | 1993-03-01 | Kellogg M W Co | AUTOTHERMAL REQUESTING PROCESS FOR THE PRODUCTION OF AMNIA SYNTHESIS GAS, HYDROGEN AND NITROGEN FROM HYDRO CARBONS OF NATURAL GAS. |
| DE10136970C2 (en) * | 2001-07-28 | 2003-11-27 | Ballard Power Systems | Device for generating hydrogen-containing gas for a fuel cell system |
| EP2199253A1 (en) | 2008-12-18 | 2010-06-23 | Ammonia Casale S.A. | Process and equipment for the production of ammonia make-up syngas with an air separation unit as nitrogen source |
| CN103449367B (en) * | 2012-05-30 | 2016-05-11 | 北京中寰工程项目管理有限公司 | A kind of emptying end gas treatment system and processing method of synthetic ammonia/methanol device |
| WO2018098495A1 (en) * | 2016-11-28 | 2018-05-31 | Seerstone Llc | Methods and systems for forming ammonia and solid carbon products |
| DE102017011601A1 (en) * | 2017-12-14 | 2019-06-19 | Linde Aktiengesellschaft | Ammonia synthesis with internal cooling circuit |
-
1986
- 1986-09-05 DE DE19863630311 patent/DE3630311A1/en not_active Withdrawn
-
1987
- 1987-07-03 IN IN480/MAS/87A patent/IN169625B/en unknown
- 1987-08-31 AR AR87308575A patent/AR241177A1/en active
- 1987-09-04 CN CN87106172A patent/CN1021904C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN87106172A (en) | 1988-06-01 |
| DE3630311A1 (en) | 1988-03-17 |
| AR241177A1 (en) | 1992-01-31 |
| IN169625B (en) | 1991-11-23 |
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