CN102765733B - Device and technique of producing liquid ammonia by coke oven gas and methanol relief gas - Google Patents
Device and technique of producing liquid ammonia by coke oven gas and methanol relief gas Download PDFInfo
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Abstract
The invention relates to a device and a technique of producing liquid ammonia by coke oven gas and methanol relief gas. A methanol relief gas material pipe is connected with a relief gas hydrogen extraction system; the relief gas hydrogen extraction system is connected with a desorption gas compressor and a hydrogen-nitrogen combination compressor; the hydrogen-nitrogen combination compressor is connected with a deoxidizing drying device, a nitrogen material pipe and an ammonia synthesis system; the ammonia synthesis system is respectively connected with an ammonia synthesis circulator, an ice machine system and a liquid ammonia spherical-tank; the coke oven gas material pipe is connected with the combination compressor; the combination compressor is connected with an active carbon rough-distillate device; the active carbon rough-distillate device is connected with a temperature change absorption system; the temperature change absorption system is connected with the coke oven gas hydrogen extraction system; the coke oven gas hydrogen extraction system is connected with a hydrolysis fine-desulfurization system; the hydrolysis fine-desulfurization system is connected with the deoxidizing drying device; the deoxidizing drying device is further connected with the combination compressor; and the combination compressor is further connected with the hydrogen-nitrogen combination compressor.
Description
Technical field
The present invention relates to chemical field, be specifically related to a kind of equipment and technique of producing liquefied ammonia, particularly a kind of equipment and technique of producing liquefied ammonia with coke-oven gas, methanol purge gas.
Background technology
Synthetic ammonia main raw material has Sweet natural gas, petroleum naphtha, mink cell focus and coal etc., and at present, China has now grasped the technology of producing synthetic ammonia with gas-solid-liquid plurality of raw materials such as coke, hard coal, brown coal, coke(oven)gas, Sweet natural gas and associated gas and liquid hydrocarbons.The energy that traditional synthesis ammonia production method consumes is higher, and equipment is outmoded, and technique is loaded down with trivial details, and output is lower.
Traditional production synthetic ammonia method can not meet the demand that people utilize synthetic ammonia, therefore, researches and develops a kind of equipment and technique of producing liquefied ammonia with coke-oven gas, methanol purge gas, has wide market outlook.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of equipment and technique of producing liquefied ammonia with coke-oven gas, methanol purge gas of efficient energy-saving.
Technical scheme of the present invention is achieved in that a kind of with coke-oven gas, methanol purge gas is produced the equipment of liquefied ammonia, comprise methanol purge gas raw material pipeline, coke(oven)gas raw material pipeline, nitrogen raw material pipeline, described methanol purge gas raw material pipeline is carried hydrogen system with the venting of speeding and is connected, the venting of speeding is carried hydrogen system and by pipeline, is combined compressor with stripping gas compressor with hydrogen nitrogen and be connected, hydrogen nitrogen associating compressor is by pipeline and deoxidation drying installation, nitrogen raw material pipeline, ammonia synthesis system is connected, ammonia synthesis system is respectively by pipeline and ammonia synthesis circulator, ice maker system, liquid ammonia ball tank is connected, described coke(oven)gas raw material pipeline with combine compressor and be connected, associating compressor is connected by the thick distillation unit of pipeline and gac, the thick distillation unit of gac is connected with temperature swing adsorption system by pipeline, temperature swing adsorption system is connected with coke oven air lift hydrogen system by pipeline, coke oven air lift hydrogen system is connected with the smart desulphurization system of hydrolysis by pipeline, being hydrolyzed smart desulphurization system is connected with deoxidation dehumidification system by pipeline, deoxidation dehumidification system again by pipeline with combine compressor and be connected, associating compressor is combined compressor by pipeline with hydrogen nitrogen again and is connected.
Between described ammonia synthesis system and ammonia synthesis circulator, be provided with ammonia synthesis purge gas pipeline, ammonia synthesis purge gas pipeline is connected with methyl alcohol gas pipe network pipeline, methyl alcohol gas pipe network pipeline is connected with stripping gas compressor, in stripping gas compressor and the venting of speeding, carries and between hydrogen system, is provided with coking gas pipe network pipeline.
Utilize an above-mentioned technique of producing the device fabrication liquid nitrogen of liquefied ammonia with coke-oven gas, methanol purge gas, its technique is as follows:
1) methanol purge gas is carried hydrogen
Methanol purge gas from methanol purge gas raw material pipeline, after the 3.2MPa that reduces pressure, enter the venting of speeding and carry hydrogen system, experience absorption successively, multistage pressure equilibrium falls, along putting, inverse put, flushing, multistage pressure is balanced rises, finally boosts, in inverse put, in earlier stage press the gas in stage to enter surge tank, when installing without inverse put, send into mixing tank; At the gas in inverse put later stage and the gas of flushing part, enter stripping gas mixing tank; Stripping gas is through stripping gas surge tank and mixing tank voltage stabilizing, and pressure is 10 to 30kPa, and a part is sent methyl alcohol gas pipe network pipeline through stripping gas compressor boost after 0.3MPa, and remaining whole stripping gass must not send coking gas pipe network pipeline through pressurization; Product hydrogen dehydrogenation nitrogen associating compressor pressurizes to after 14MPa as synthetic ammonia fresh feed pneumatic transmission ammonia synthesis system;
2) coke oven air lift hydrogen
From the coke(oven)gas of coke(oven)gas raw material pipeline, after associating compressor compresses, pressure is 0.8MPa, then through the thick distillation unit of gac by the H in coke(oven)gas
2s is removed to 1mg/Nm
3below, after temperature swing adsorption system, send again coke oven air lift hydrogen system, experience absorption successively, multistage pressure equilibrium falls, along putting, inverse put, vacuumize desorb, multistage pressure is balanced rises, finally boosts, at inverse put gas in earlier stage, enter surge tank, when installing without inverse put, send into mixing tank; Gas in inverse put later stage part enters stripping gas mixing tank with the gas that vacuumizes desorb part; Extraction sends into the smart desulphurization system of hydrolysis after please gas and deoxidation dehumidification system carries out deoxidization desulfuration, is then sent to associating compressor boost and send ammonia synthesis system after 3.0MPa;
3) nitrogen deoxidation
Carry out the nitrogen of nitrogen raw material pipeline, through hydrogen nitrogen associating compressor boost, to entering after 14.25MPa, in deoxidation drying installation, remove oxygen wherein, then the ratio needing in ammonia synthesis is after drying sent ammonia synthesis system;
4) ammonia synthesis
By step 1) and step 2) in the hydrogen that makes and step 3) the dried nitrogen of deoxidation send into ammonia synthesis system, and finally synthesize liquefied ammonia after ammonia synthesis circulator and ice maker system, the off-gas forming in this process is through ammonia synthesis purge gas pipeline, deliver to methyl alcohol gas pipe network pipeline, it is standby that liquefied ammonia is sent to liquid ammonia ball tank storage.
The present invention has following positively effect: utilize the pressure of the 5.0MP that methanol production keeps when speeding to exit separation as the source pressure of pressure swing adsorption technique, the impurity that macromole is easily adsorbed carries out separation, increase no longer in addition power set consumed energy, realize adsorption process energy-conservation; According to makings composition and the technique of the venting of speeding, analyze and study, the pressure of the 5.0MP keeping while rationally utilizing the hydrogen component of speeding to exit in gas composition and methanol purge gas separated is realized energy-conservation, research and develop new and effective pressure-variable adsorption agent and improve hydrogen purity, be condensed into production synthetic ammonia with the nitrogen pressure of air separation facility affluence.
Accompanying drawing explanation
Fig. 1 is present device and process flow diagram.
Embodiment
As shown in Figure 1, a kind of with coke-oven gas, methanol purge gas is produced the equipment of liquefied ammonia, comprise methanol purge gas raw material pipeline 1, coke(oven)gas raw material pipeline 20, nitrogen raw material pipeline 11, described methanol purge gas raw material pipeline 1 is carried hydrogen system 2 with the venting of speeding and is connected, the venting of speeding is carried hydrogen system 2 and by pipeline, is combined compressor 3 with stripping gas compressor 4 with hydrogen nitrogen and be connected, hydrogen nitrogen associating compressor 3 is by pipeline and deoxidation drying installation 5, nitrogen raw material pipeline 11, ammonia synthesis system 7 is connected, ammonia synthesis system 7 is respectively by pipeline and ammonia synthesis circulator 6, ice maker system 8, liquid ammonia ball tank 9 is connected, described coke(oven)gas raw material pipeline 20 with combine compressor 12 and be connected, associating compressor 12 is connected by the thick distillation unit 13 of pipeline and gac, the thick distillation unit 13 of gac is connected with temperature swing adsorption system 14 by pipeline, temperature swing adsorption system 14 is connected with coke oven air lift hydrogen system 15 by pipeline, coke oven air lift hydrogen system 15 is connected with the smart desulphurization system 16 of hydrolysis by pipeline, being hydrolyzed smart desulphurization system 16 is connected with deoxidation dehumidification system 17 by pipeline, deoxidation dehumidification system 17 again by pipeline with combine compressor 12 and be connected, associating compressor 12 is combined compressor 3 by pipeline with hydrogen nitrogen again and is connected.
Between described ammonia synthesis system 7 and ammonia synthesis circulator 6, be provided with ammonia synthesis purge gas pipeline 10, ammonia synthesis purge gas pipeline 10 is connected with methyl alcohol gas pipe network pipeline 18, methyl alcohol gas pipe network pipeline 18 is connected with stripping gas compressor 4, in stripping gas compressor 4 and the venting of speeding, carries and between hydrogen system 2, is provided with coking gas pipe network pipeline 19.
Utilize an above-mentioned technique of producing the device fabrication liquid nitrogen of liquefied ammonia with coke-oven gas, methanol purge gas, its technique is as follows:
1) methanol purge gas is carried hydrogen
Methanol purge gas from methanol purge gas raw material pipeline 1, after the 3.2MPa that reduces pressure, enter the venting of speeding and carry hydrogen system 2, experience absorption successively, multistage pressure equilibrium falls, along putting, inverse put, flushing, multistage pressure is balanced rises, finally boosts, in inverse put, in earlier stage press the gas in stage to enter surge tank, when installing without inverse put, send into mixing tank; At the gas in inverse put later stage and the gas of flushing part, enter stripping gas mixing tank; Stripping gas is through stripping gas surge tank and mixing tank voltage stabilizing, and pressure is 10 to 30kPa, and a part is sent methyl alcohol gas pipe network pipeline 18 after stripping gas compressor 4 is pressurized to 0.3MPa, and remaining whole stripping gass must not send coking gas pipe network pipeline 19 through pressurization; Product hydrogen dehydrogenation nitrogen associating compressor 3 is pressurized to after 14MPa as synthetic ammonia fresh feed pneumatic transmission ammonia synthesis system 7;
2) coke oven air lift hydrogen
From the coke(oven)gas of coke(oven)gas raw material pipeline 20, after 12 compressions of associating compressor, pressure is 0.8MPa, then through the thick distillation unit 13 of gac by the H in coke(oven)gas
2s is removed to 1mg/Nm
3below, after temperature swing adsorption system 14, send again coke oven air lift hydrogen system 15, experience absorption successively, multistage pressure equilibrium falls, along putting, inverse put, vacuumize desorb, multistage pressure is balanced rises, finally boosts, at inverse put gas in earlier stage, enter surge tank, when installing without inverse put, send into mixing tank; Gas in inverse put later stage part enters stripping gas mixing tank with the gas that vacuumizes desorb part; Extraction sends into the smart desulphurization system 16 of hydrolysis after please gas and deoxidation dehumidification system 17 carries out deoxidization desulfuration, then
Be sent to after associating compressor 12 is pressurized to 3.0MPa and send ammonia synthesis system 7;
3) nitrogen deoxidation
Carry out the nitrogen of nitrogen raw material pipeline 11, after hydrogen nitrogen associating compressor 3 is pressurized to 14.25MPa, enter and in deoxidation drying installation 5, remove oxygen wherein, then the ratio needing in ammonia synthesis is after drying sent ammonia synthesis system 7;
4) ammonia synthesis
By step 1) and step 2) in the hydrogen that makes and step 3) the dried nitrogen of deoxidation send into ammonia synthesis system 7, and finally synthesize liquefied ammonia after ammonia synthesis circulator 6 and ice maker system 8, the off-gas forming in this process is through ammonia synthesis purge gas pipeline 10, deliver to methyl alcohol gas pipe network pipeline 18, it is standby that liquefied ammonia is sent to liquid ammonia ball tank 9 storages.
Step 2) in the hydrogen that in, coke(oven)gas pressure-variable adsorption extracts, residual approximately 200 O to 3000ppm still
2, must be removed to 1ppm and just can be sent to subsequent handling below, otherwise will cause damage to ammonia synthesis catalyst.Hydrogen deoxidation adopts catalytic deoxidation method, first by low-pressure steam, hydrogen is heated to approximately 80 to 120 ℃, under palladium catalyst effect, and the O in hydrogen
2with H
2react and generate H
2o.In the hydrogen that coke(oven)gas pressure-variable adsorption extracts, the COS of residual total amount≤1ppm still, this part sulfide can not be delivered to subsequent handling, otherwise will cause damage to dehydrogenation catalyst and ammonia synthesis catalyst, must be removed to below 0.1ppm.The desulfurization of hydrogen essence adopts the way of ordinary-temp hydrolysis, and the moisture content that utilizes approximately 80～120 ℃ of temperature of deoxidation hydrogen and deoxygenation to generate is converted into COS the H that is easy to remove under hydrolyst effect
2s, then the H absorbing with normal temperature ZnO sweetening agent
2s, can guarantee total sulfur≤0.1ppm in hydrogen.After refrigerated separation, after moisture content, by molecular sieve adsorption, be dried residual saturated moisture content to <2ppm again, be sent to the bright compressor boost of coke(oven)gas/hydrogen is incorporated in the Hydrogen Line of methanol purge gas extraction, in the lump as ammonia-synthesizing material gas after about 3.0MPa.
In step 3) from the nitrogen of methanol device space division system, the about 3kPa of pressure, to it, allocate into after the purification that a small amount of pressure-variable adsorption extracts after hydrogen, after hydrogen nitrogen associating compressor 3 is pressurized to about 14.25MPa, enter in deoxygenator, under the effect of palladium catalyst, hydrogen and oxygen water generation reaction, thereby remove oxygen wherein, dry through mole sieve drier again, the moisture removing be wherein fitted in the raw hydrogen of 14MPa after pressurization in the ratio of ammonia synthesis needs to < 2ppm, send ammonia synthesis system together with hydrogen.
Adsorbent of molecular sieve is used from methanol device space division system nitrogen and is regenerated.Because sky divides nitrogen very dry, can complete at normal temperatures the regeneration task of adsorbent of molecular sieve, although pressure only has 3kPa left and right, be enough to low speed and take away the moisture content in adsorbent of molecular sieve by adsorber.The direct emptying of regeneration nitrogen.
Always there is a moisture eliminator any time in absorption algorithm, and standby after another moisture eliminator regeneration.
The ammonia synthetic fresh gas making that is mixed after pressurization in step 4) mixes with the circulation gas of recycle compressor outlet, enters together ammonia synthesis converter.Go out 320 ℃ of synthetic tower gas temperatures, enter waste heat boiler.At waste heat boiler, produce 1.1MPa steam, be cooled to 205 ℃ of left and right, enter heat exchanger (in pipe), temperature is down to 80 ℃ of left and right, the water cooler of intaking again, temperature is down to after normal temperature, enters successively that cool exchanger, primary amine are cold, secondary amine enters ammonia separator after cold, the recycle gas of separator outlet is used for cooling synthetic tower exit gas at cool exchanger, then gets back to synthesic gas compressor circulation section entrance.A small amount of unreacting gas (being off-gas), sends outside battery limit (BL) to methanol device process furnace and makes fuel.The product liquefied ammonia that separator separates, in relief groove, about 3.6MPa is arrived in decompression, then 1.6MPa ammonia basin groove is sent in decompression.
Because the finished product are liquefied ammonia, and ammonia must could liquefy by freezing way under lower pressure, therefore ice maker system is set.The way that adopts liquefied ammonia evaporation to take away ammonia synthesis gas mixture heat makes ammoniacal liquor in ammonia synthesis gas mixture separated with ammonia synthesis circulation gas, thereby obtains liquefied ammonia product.Gas ammonia is got back to ice maker systemic circulation and is used.The gas ammonia of ammonia compressor outlet, after reflux cooler and ammonia condenser condensation, flow to liquefied ammonia storage tank certainly, and then the liquefied ammonia of liquefied ammonia storage tank is sent to synthesis procedure ammonia condenser shell sweat cooling again and forms circulation.The supplementary liquefied ammonia of refrigeration system is by synthesis system supply.After collecting from the blowdown of ammonia cooler shell-side and liquefied ammonia storage tank, being sent to oil trap processes.Adopt 2 of the pressure type spherical holders that large and medium-sized synthetic ammonia installation is conventional, every 400m
3, consider the seasonality of liquefied ammonia sale and the possibility that short-term is interrupted, by period of storage>=3 day, consider temporarily.The liquefied ammonia being come by synthesis procedure enters in liquefied ammonia spherical holder to be stored, the about 1.6MPa of spherical tank working pressure, main outer the selling of liquefied ammonia.
Claims (3)
1. one kind with coke-oven gas, methanol purge gas is produced the equipment of liquefied ammonia, comprise methanol purge gas raw material pipeline (1), coke(oven)gas raw material pipeline (20), nitrogen raw material pipeline (11), it is characterized in that: described methanol purge gas raw material pipeline (1) is carried hydrogen system (2) with the venting of speeding and is connected, the venting of speeding is carried hydrogen system (2) and by pipeline, is combined with hydrogen nitrogen compressor (3) with stripping gas compressor (4) and be connected, hydrogen nitrogen associating compressor (3) is by pipeline and deoxidation drying installation (5), nitrogen raw material pipeline (11), ammonia synthesis system (7) is connected, ammonia synthesis system (7) is respectively by pipeline and ammonia synthesis circulator (6), ice maker system (8), liquid ammonia ball tank (9) is connected, described coke(oven)gas raw material pipeline (20) with combine compressor (12) and be connected, associating compressor (12) is connected by the thick distillation unit of pipeline and gac (13), the thick distillation unit of gac (13) is connected with temperature swing adsorption system (14) by pipeline, temperature swing adsorption system (14) is connected with coke oven air lift hydrogen system (15) by pipeline, coke oven air lift hydrogen system (15) is connected with the smart desulphurization system of hydrolysis (16) by pipeline, being hydrolyzed smart desulphurization system (16) is connected with deoxidation dehumidification system (17) by pipeline, deoxidation dehumidification system (17) again by pipeline with combine compressor (12) and be connected, associating compressor (12) is combined again compressor (3) and is connected with hydrogen nitrogen by pipeline.
2. use coke-oven gas according to claim 1, methanol purge gas are produced the equipment of liquefied ammonia, it is characterized in that: between described ammonia synthesis system (7) and ammonia synthesis circulator (6), be provided with ammonia synthesis purge gas pipeline (10), ammonia synthesis purge gas pipeline (10) is connected with methyl alcohol gas pipe network pipeline (18), methyl alcohol gas pipe network pipeline (18) is connected with stripping gas compressor (4), in stripping gas compressor (4) and the venting of speeding, carries and between hydrogen system (2), is provided with coking gas pipe network pipeline (19).
3. utilize the technique of producing the device fabrication liquid nitrogen of liquefied ammonia with coke-oven gas, methanol purge gas described in claim 1, it is characterized in that, its technique is as follows:
1) methanol purge gas is carried hydrogen
Methanol purge gas from methanol purge gas raw material pipeline (1), after the 3.2MPa that reduces pressure, enter the venting of speeding and carry hydrogen system (2), experience absorption successively, multistage pressure equilibrium falls, along putting, inverse put, flushing, multistage pressure is balanced rises, finally boosts, in inverse put, in earlier stage press the gas in stage to enter surge tank, when installing without inverse put, send into mixing tank; At the gas in inverse put later stage and the gas of flushing part, enter stripping gas mixing tank; Stripping gas is through stripping gas surge tank and mixing tank voltage stabilizing, pressure is 10 to 30kPa, a part is sent methyl alcohol gas pipe network pipeline (18) after stripping gas compressor (4) is pressurized to 0.3MPa, and remaining whole stripping gass must not send coking gas pipe network pipeline (19) through pressurization; Product hydrogen dehydrogenation nitrogen associating compressor (3) is pressurized to after 14MPa as synthetic ammonia fresh feed pneumatic transmission ammonia synthesis system (7);
2) coke oven air lift hydrogen
From the coke(oven)gas of coke(oven)gas raw material pipeline (20), after associating compressor (12) compression, pressure is 0.8MPa, then through the thick distillation unit of gac (13) by the H in coke(oven)gas
2s is removed to 1mg/Nm
3below, after temperature swing adsorption system (14), send again coke oven air lift hydrogen system (15), experience absorption successively, multistage pressure equilibrium falls, along putting, inverse put, vacuumize desorb, multistage pressure is balanced rises, finally boosts, at inverse put gas in earlier stage, enter surge tank, when installing without inverse put, send into mixing tank; Gas in inverse put later stage part enters stripping gas mixing tank with the gas that vacuumizes desorb part; Extract and to send into hydrolysis smart desulphurization system (16) after hydrogen and deoxidation dehumidification system (17) carries out deoxidization desulfuration, then
Be sent to after associating compressor (12) is pressurized to 3.0MPa and send ammonia synthesis system (7);
3) nitrogen deoxidation
From the nitrogen of nitrogen raw material pipeline (11), after hydrogen nitrogen associating compressor (3) is pressurized to 14.25MPa, enters in deoxidation drying installation (5) and remove oxygen wherein, then the ratio needing in ammonia synthesis is after drying sent ammonia synthesis system (7);
4) ammonia synthesis
By step 1) and step 2) in the hydrogen that makes and step 3) the dried nitrogen of deoxidation send into ammonia synthesis system (7), and finally synthesize liquefied ammonia after ammonia synthesis circulator (6) and ice maker system (8), the off-gas forming in this process is through ammonia synthesis purge gas pipeline (10), deliver to methyl alcohol gas pipe network pipeline (18), liquefied ammonia is sent to liquid ammonia ball tank (9) and stores standby.
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Families Citing this family (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103011198B (en) * | 2012-12-20 | 2014-09-17 | 赛鼎工程有限公司 | Process for preparing synthetic ammonia with coke-oven gas |
| CN103055660B (en) * | 2013-01-15 | 2015-04-22 | 山东吉安化工有限公司 | Method and system for treating cyclohexane oxidation tail gas |
| CN107694283A (en) * | 2017-09-14 | 2018-02-16 | 山西龙智能源化工有限公司 | A kind of voltage-stabilizing system of Utilization of PSA Relief Gas |
| CN107469566A (en) * | 2017-09-14 | 2017-12-15 | 山西龙智能源化工有限公司 | A kind of voltage stabilizing technique of Utilization of PSA Relief Gas |
| CN113666386B (en) * | 2021-08-26 | 2023-04-14 | 宁波中科远东催化工程技术有限公司 | Method for synthesizing ammonia from coke oven gas |
| CN116177564A (en) * | 2022-12-08 | 2023-05-30 | 金能科技股份有限公司 | Method for preparing methanol and co-producing synthetic ammonia and extracting ammonia from coke oven gas |
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| CN101368010A (en) * | 2008-09-25 | 2009-02-18 | 曲靖市众一煤化有限公司 | Method for producing semi-reinforcing hydrocarbon black, methanol, liquid ammonia with coke oven gas |
| CN101780964A (en) * | 2010-03-09 | 2010-07-21 | 南京聚拓化工科技有限公司 | Process for synthesizing ammonia by utilizing purge gas of methanol device |
| CN202808384U (en) * | 2012-08-01 | 2013-03-20 | 河南中鸿集团煤化有限公司 | Device for producing liquid ammonia by using coke oven gas and methanol purge gas |
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| US7892511B2 (en) * | 2004-07-02 | 2011-02-22 | Kellogg Brown & Root Llc | Pseudoisothermal ammonia process |
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| CN101368010A (en) * | 2008-09-25 | 2009-02-18 | 曲靖市众一煤化有限公司 | Method for producing semi-reinforcing hydrocarbon black, methanol, liquid ammonia with coke oven gas |
| CN101780964A (en) * | 2010-03-09 | 2010-07-21 | 南京聚拓化工科技有限公司 | Process for synthesizing ammonia by utilizing purge gas of methanol device |
| CN202808384U (en) * | 2012-08-01 | 2013-03-20 | 河南中鸿集团煤化有限公司 | Device for producing liquid ammonia by using coke oven gas and methanol purge gas |
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