CN102849680A - Method for synthesis and purification of hydrogen from natural gas - Google Patents
Method for synthesis and purification of hydrogen from natural gas Download PDFInfo
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- CN102849680A CN102849680A CN2012103144852A CN201210314485A CN102849680A CN 102849680 A CN102849680 A CN 102849680A CN 2012103144852 A CN2012103144852 A CN 2012103144852A CN 201210314485 A CN201210314485 A CN 201210314485A CN 102849680 A CN102849680 A CN 102849680A
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Abstract
The invention discloses a method for synthesis and purification of hydrogen from natural gas. According to the invention, hydrogenation catalysis is used to remove sulfur in natural gas; both CO-MO hydro-conversion and ZnO desulfurization technology are employed for treatment of feed gas; methane reacts with water vapor at a high temperature in the presence of the conversion catalyst NiO to produce mixed gas of H2, CO, CO2, etc.; the mixed gas of H2, CO and CO2 obtained in conversion procedure of water vapor undergoes a water gas reaction in a shifting furnace filled with a high temperature shift catalyst Fe2O3; CO further reacts with water vapor, and the majority of CO is converted into CO2 and H2; two-stage purification at an ordinary hydrogen section and a purification section is carried out. With the method, H2 with a high purity of more than 99.999% can be obtained.
Description
Technical field
The present invention relates to a kind of synthetic and purification process of gas, particularly a kind of from Sweet natural gas synthetic hydrogen and purifying be the method for High Purity Hydrogen.
Background technology
Hydrogen is one of human beings cleaning and eternal energy.The formation of world energy sources experienced from solidify (bavin, coal, nucleon), liquefaction (oil), to the process of vaporize (Sweet natural gas, hydrogen), hydrocarbon proportion wherein is on the way down: 90% (bavin), 60% (coal) 30% (oil), 20% (Sweet natural gas), 0% (hydrogen), the content of hydrogen is more and more higher, and the content of carbon is then more and more lower.As everyone knows, carbonic acid gas is to pollute the chief culprit who causes global greenhouse effect, and the minimizing of carbon content means the energy of cleaning.Hydrogen is because its special character is widely used in the industries such as petrochemical complex, aviation, metallurgy, electronics, electric power, building materials, gas manufacturing.Along with the attention that reaches environmental issue in short supply of world energy sources, hydrogen more and more receives the concern in the world as high-octane carrier.Because the development of solar electrical energy generation, electrolysis hydrogen, fuel cell, hydrogen storage technology, it is the substitute of petroleum-based energy that the status of hydrogen is about to from general industrial gas transition.
The technology that present hydrogen manufacturing industry generally adopts mainly contains: water electrolysis, methanol decomposition, natural gas pyrolysis, ammonia decomposition, hydrogen production from coal gasification, hydrogen rich off gas recovery etc.The main source of hydrogen is divided into three major types at present: the one, and traditional water electrolysis hydrogen producing; The 2nd, utilize the industrial gaseous waste purified hydrogen; The 3rd, adopt fossil oil, obtain the again hydrogen of separating-purifying of hydrogeneous source of the gas such as methods such as the gas making such as coal gas, Sweet natural gas, heavy oil or propane, liquefied ammonia, methanol decompositions.And in this three class, technology maturation can obtain hydrogen producing technology that High Purity Hydrogen is used for industrial application and mainly contain five kinds of water electrolysis, natural gas pyrolysis, ammonia decomposition, coal generating gas, methanol decomposition.
Wherein, natural gas pyrolysis hydrogen manufacturing is take cheap clean Sweet natural gas as raw material, after overdraft, desulfurization, preheating, mix with water vapor, under 800～850 ℃ temperature, 1.3～1.6MPa left and right sides pressure condition, pass through converter, under catalyst action, catalytic cracking reaction and part carbon monodixe conversion reaction occurs simultaneously, generate hydrogen, carbonic acid gas and carbon monoxide, for taking full advantage of thermal source and hydrogen source, reforming gas through further conversion, Multi-stage heat reclaim and condensation after, enter the pressure-variable adsorption operation as the unstripped gas of pressure swing adsorption hydrogen production.Be H as the natural gas pyrolysis gas main ingredient of extracting pure hydrogen raw material
2, CO, CO
2And CH
4, after conversion of natural gas gas is removed liquid composition through gas-liquid separator, behind the pressure swing adsorption system that enters adsorber and a series of sequence valve formation about 1.2 ~ 1.5MPa and under 40 ℃, obtain highly purified hydrogen.But processing method of the prior art is only suitable for small-scale hydrogen manufacturing, does not also have a kind of row to know effective technique, can support greater than 1000m
3/ h is to the extensive hydrogen manufacturing of several ten thousand steres.
Summary of the invention
Goal of the invention of the present invention is in order to overcome the weak point of prior art, by the hydrogen manufacturing of gas water steam reforming process, and adopts the pressure swing adsorption purified hydrogen, provide a kind of economy, rationally, support the natural gas pyrolysis hydrogen producing technology of extensive hydrogen manufacturing.
Goal of the invention of the present invention is achieved by the following technical solution: take Sweet natural gas as raw material, adopt unstripped gas processing, steam reforming, CO variation, hydrogen purification.Can be with hydrogen purification to 99.999%, O
2+ Ar≤1ppm, N
2≤ 3ppm, CO≤1ppm, CO
2≤ 1ppm, CH
4≤ 1ppm, H
2O≤2ppm.
1. unstripped gas is processed: mainly adopt hydrogenation catalyst to remove sulphur in the Sweet natural gas, use C
O-M
OHydrocracking series connection ZnO desulfurization technology: unstripped gas is preheating to approximately 350～400 ℃ at the converter convection zone first, adopts first C
O-M
OThe catalyst hydrogenation method is converted into inorganic sulfur (H with the organosulfur in the gas raw material in hydrogenator
2S), remove H with ZnO adsorption desulfurize groove again
2S can drop to 0.1mg.m with the total sulfur content in the unstripped gas at last
-3Below.
2. steam reforming: the unstripped gas after the desulfurization is under conversion catalyst NiO existence and hot conditions, makes methane and steam reaction, generates H
2, CO, CO
2Deng mixed gas, this reaction is strong heat absorption, needs extraneous heat supply.The key equipment of steam reforming operation is main converter, and it comprises radiation section and convection zone.Raw material need to carry out pre-inversion in pre reformer before entering main converter, pre-inversion can all be converted into CH with the heavy hydrocarbon polymer in the Sweet natural gas
4And CO
2Thereby can greatly reduce the possibility of main converter coking.Sulphur remaining in the unstripped gas all can be removed simultaneously, be made conversion catalyst sulfur poisoning can not occur, prolong the work-ing life of conversion catalyst.
3.CO change: be the gas mixture H that makes from the steam reforming operation
2, CO, CO
2Hts catalyst Fe is being housed
2O
3The variation stove in carry out water-gas reaction, CO further with steam reaction, most of CO is converted into CO
2And H
2Its process using high temperature shift, the gas after the conversion is behind separating technology phlegma after the cooling, and gas is sent into the hydrogen purification operation.
4. hydrogen purification: adopt general hydrogen section and purification section two-stage purifying process.General hydrogen section adopts 8-2-5/PSA technique, and namely this operation is comprised of 8 adsorption towers, and 2 simultaneously chargings of adsorption tower are all pressed the normal pressure desorption mode 5 times; Purification section adopts 6-2-3/PSA technique, and namely this operation is comprised of 6 adsorption towers, and 2 simultaneously chargings of adsorption tower are all pressed the normal pressure desorption mode 3 times.
The invention has the beneficial effects as follows: use technique of the present invention can satisfy the needs of the hydrogen producing technology of extensive hydrogen manufacturing, and transformation efficiency is high, refining effect is good, can obtain H
2Purity is at the high-purity hydrogen more than 99.999%.The heat that reaction generates in the technique is by reclaiming and other step heat-shifts, and this technique that is is economical rationality more.
Description of drawings
Accompanying drawing 1 has represented a kind of process flow sheet of natural gas hydrogen preparation method of the present invention.
Embodiment
Example below in conjunction with accompanying drawing 1 further specifies method of the present invention.
The present invention generates hydrogen take Sweet natural gas as raw material by cracking, contains CH in its Sweet natural gas
4: 92.5%, C
2H
6: 3.96%, C
3H
8: 0.335%, IC
4H
10: 0.12%, NC
4H
10: 0.08%, IC
5H
12: 0.22%, H
2S:0.0001%, N
2: 0.85%, CO
2: 1.89%, H
20:0.0005%; A whole set of technique expected capacity 2400Nm
3/ h.
Come the Sweet natural gas of medium pressure tank car, through emergency episode intercepting valve, the voltage stabilizing of Sweet natural gas pressure maintaining valve to 2.0MPa, small part goes the converter burner to make fuel after falling reducing valve, most of by steam/hydrocarbons ratio flow control valve adjust flux and with mix from the circulating hydrogen that returns hydrogen compressor, enter the unstripped gas preheat coil of steam reformer convection zone, be preheated to about 350～400 ℃, enter hydrogenator and desulfurizer, the sulphur in the unstripped gas is taken off to 0.1ppm.
Raw material after the desulfurization is by water with the process steam that regulates flow: enter the charge heating coil pipe after carbon mol ratio 3:5 mixes, further be preheating to 580 ℃, enter converter radiation section conversion tube, methane and steam reaction generate H in catalyst layer
2With CO, CO
2, methane conversion institute heat requirement is supplied by the top combustion burner air lift.
Reforming gas goes out the converter temperature and is about 830～850 ℃, and remaining methane content approximately＜4.0% enters waste heat boiler by-product 2.2MPa saturation steam personal.The reforming gas temperature that goes out waste heat boiler is down to 360 ℃, enters shift converter again, and the CO in the reforming gas and unreacted excessive water steam generate H with steam reaction under the effect of hts catalyst
2And CO
2, and emit a large amount of reaction heat, make gas temperature be elevated to 400～430 ℃.Go out in the high temperature shift gas of shift converter CO content less than 1.5%.
Above-mentioned high temperature shift gas enters after the feedwater interchanger reclaims heat after the middle change, temperature is down to 165 ℃, enters the de-salted water preheater again, and the outlet conversion gas enters water recirculator again and is as cold as 40 ℃, after water trap is isolated process condensate, deliver to pressure-swing absorption apparatus.After process condensate entered sour water gas tower, the byproduct steam that the filling surface in gas stripping column and bottom pass into carried out mass transfer and heat transfer effect, with HCO wherein
3 -Fully remove, then return deoxygenator and mix with the de-salted water that replenishes, recycle.
Put forward the hydrogen operation and adopt general hydrogen section+purification section configuration, two cover conversion systems share.General hydrogen section adopts 8-2-5/P PSA technique, and namely this operation is comprised of individual 8 adsorption towers, and 2 simultaneously chargings of adsorption tower are all pressed the normal pressure desorption mode 5 times.Purification section adopts 6-2-3/P technique, and namely this operation is comprised of individual 6 adsorption towers, and 2 simultaneously chargings of adsorption tower are all pressed for 3 times, the normal pressure desorption mode, and resolution gas returns the leading portion operation by compressor, consumes to save.
Each impurity composition content in table 1. High Purity Hydrogen
Claims (4)
1. one kind is synthesized the method that reaches purifying hydrogen from Sweet natural gas, it is characterized in that its processing step is:
1) unstripped gas is processed: mainly adopt hydrogenation catalyst to remove sulphur in the Sweet natural gas, use C
O-M
OHydrocracking series connection ZnO desulfurization technology, unstripped gas is preheating to approximately 350～400 ℃ at the converter convection zone first, adopts first C
O-M
OThe catalyst hydrogenation method is converted into inorganic sulfur H with the organosulfur in the gas raw material in hydrogenator
2S removes H with ZnO adsorption desulfurize groove again
2S can drop to 0.1mg.m with the total sulfur content in the unstripped gas at last
-3Below;
2) steam reforming: the unstripped gas after the desulfurization is under conversion catalyst NiO existence and hot conditions, makes methane and steam reaction, generates H
2, CO, CO
2Deng mixed gas, this reaction is strong heat absorption, need extraneous heat supply, the key equipment of steam reforming operation is main converter, it comprises radiation section and convection zone, raw material need to carry out pre-inversion in pre reformer before entering main converter, pre-inversion can all be converted into CH with the heavy hydrocarbon polymer in the Sweet natural gas
4And CO
2Thereby can greatly reduce the possibility of main converter coking, sulphur remaining in the unstripped gas all can be removed simultaneously, make conversion catalyst sulfur poisoning can not occur, prolong the work-ing life of conversion catalyst;
3) CO changes: be the gas mixture H that makes from the steam reforming operation
2, CO, CO
2Hts catalyst Fe is being housed
2O
3The variation stove in carry out water-gas reaction, CO further with steam reaction, most of CO is converted into CO
2And H
2, its process using high temperature shift, the gas after the conversion is behind separating technology phlegma after the cooling, and gas is sent into the hydrogen purification operation;
4) hydrogen purification: adopt general hydrogen section and purification section two-stage purifying process, general hydrogen section adopts 8-2-5/PSA technique, and namely this operation is comprised of 8 adsorption towers, and 2 simultaneously chargings of adsorption tower are all pressed the normal pressure desorption mode 5 times; Purification section adopts 6-2-3/PSA technique, and namely this operation is comprised of 6 adsorption towers, and 2 simultaneously chargings of adsorption tower are all pressed the normal pressure desorption mode 3 times.
As claimed in claim 1 from Sweet natural gas the method for synthetic and purifying hydrogen, it is characterized in that described step 2) in the steam reforming step in, raw material after the desulfurization and the process steam that regulates flow are by water: enter the charge heating coil pipe after carbon mol ratio 3:5 mixes, further be preheating to 580 ℃, enter converter radiation section conversion tube, methane and steam reaction generate H in catalyst layer
2With CO, CO
2, methane conversion institute heat requirement is supplied by the top combustion burner air lift.
As claimed in claim 1 from Sweet natural gas the method for synthetic and purifying hydrogen, it is characterized in that described step 2) in reforming gas go out the converter temperature and be about 830～850 ℃, remaining methane content approximately＜4.0% enters waste heat boiler by-product 2.2MPa saturation steam personal.
As claimed in claim 1 from Sweet natural gas the method for synthetic and purifying hydrogen, it is characterized in that in the described step 3) CO further with steam reaction, most of CO is converted into CO
2And H
2And emit a large amount of reaction heat, make gas temperature be elevated to 400～430 ℃, go out in the high temperature shift gas of shift converter CO content less than 1.5%, high temperature shift gas enters after the feedwater interchanger reclaims heat after the middle change, temperature is down to 165 ℃, enter again the de-salted water preheater, the outlet conversion gas enters water recirculator again and is as cold as 40 ℃, after water trap is isolated process condensate, deliver to pressure-swing absorption apparatus, after process condensate enters sour water gas tower, the byproduct steam that filling surface in gas stripping column and bottom pass into carries out mass transfer and heat transfer effect, with HCO wherein
3 -Fully remove, then return deoxygenator and mix with the de-salted water that replenishes, recycle.
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|---|---|---|---|
| CN2012103144852A CN102849680A (en) | 2012-08-30 | 2012-08-30 | Method for synthesis and purification of hydrogen from natural gas |
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|---|---|---|---|
| CN2012103144852A CN102849680A (en) | 2012-08-30 | 2012-08-30 | Method for synthesis and purification of hydrogen from natural gas |
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| CN104807955A (en) * | 2014-01-24 | 2015-07-29 | 上海华林工业气体有限公司 | Method for increasing hydrogen analysis detection rate of hydrogen and carbon monoxide production apparatus |
| CN106564861A (en) * | 2016-11-09 | 2017-04-19 | 华南理工大学 | Process for efficiently recovering reforming gas energy in hydrocarbon steam reforming hydrogen production process |
| CN106629599A (en) * | 2015-10-28 | 2017-05-10 | 上海华林工业气体有限公司 | Hydrogen production system by natural gas reforming |
| CN106809804A (en) * | 2017-01-25 | 2017-06-09 | 中国天辰工程有限公司 | A kind of natural gas reforming unit technique lime set recycling system and method |
| CN109179320A (en) * | 2018-11-08 | 2019-01-11 | 新地能源工程技术有限公司 | A kind of natural gas hydrogen production plant and method |
| CN109666520A (en) * | 2019-01-28 | 2019-04-23 | 安庆市泰发能源科技有限公司 | Butane dehydrogenation hydrogen rich off gas recycle device |
| CN110541690A (en) * | 2019-09-04 | 2019-12-06 | 中海石油气电集团有限责任公司 | method for improving recovery ratio by decarbonization of natural gas at gas field wellhead and CO2 reinjection |
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| CN113213425A (en) * | 2021-06-08 | 2021-08-06 | 金川集团股份有限公司 | System and method for preparing hydrogen by using natural gas |
| CN113620244A (en) * | 2020-05-07 | 2021-11-09 | 中国石油化工股份有限公司 | System and method for hydrogen production by reforming natural gas steam |
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| CN115368210A (en) * | 2022-09-06 | 2022-11-22 | 浙江清和新材料科技有限公司 | Method for treating tail gas hydrogen of hydrogenation reaction |
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| CN116621117A (en) * | 2023-05-24 | 2023-08-22 | 上海汉兴化工科技有限公司 | Preparation method of high-purity hydrogen for fuel cell |
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| CN102173381A (en) * | 2011-02-28 | 2011-09-07 | 四川亚联高科技股份有限公司 | Method for preparing hydrogen with natural gas as raw material |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102173381A (en) * | 2011-02-28 | 2011-09-07 | 四川亚联高科技股份有限公司 | Method for preparing hydrogen with natural gas as raw material |
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| CN104807955A (en) * | 2014-01-24 | 2015-07-29 | 上海华林工业气体有限公司 | Method for increasing hydrogen analysis detection rate of hydrogen and carbon monoxide production apparatus |
| CN104807955B (en) * | 2014-01-24 | 2017-01-04 | 上海华林工业气体有限公司 | Improve and produce the method that the hydrogen of hydrogen and carbon monoxide device analyzes detection rates |
| CN106629599A (en) * | 2015-10-28 | 2017-05-10 | 上海华林工业气体有限公司 | Hydrogen production system by natural gas reforming |
| CN106564861A (en) * | 2016-11-09 | 2017-04-19 | 华南理工大学 | Process for efficiently recovering reforming gas energy in hydrocarbon steam reforming hydrogen production process |
| CN106809804B (en) * | 2017-01-25 | 2019-01-22 | 中国天辰工程有限公司 | A kind of natural gas reforming unit technique lime set recycling system and method |
| CN106809804A (en) * | 2017-01-25 | 2017-06-09 | 中国天辰工程有限公司 | A kind of natural gas reforming unit technique lime set recycling system and method |
| CN109179320A (en) * | 2018-11-08 | 2019-01-11 | 新地能源工程技术有限公司 | A kind of natural gas hydrogen production plant and method |
| CN109666520A (en) * | 2019-01-28 | 2019-04-23 | 安庆市泰发能源科技有限公司 | Butane dehydrogenation hydrogen rich off gas recycle device |
| WO2021031894A1 (en) * | 2019-08-20 | 2021-02-25 | 四川亚联高科技股份有限公司 | Integrated small to medium-sized natural gas steam reforming reactor, and reforming reaction process |
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| CN110937573B (en) * | 2019-10-28 | 2023-08-22 | 中科液态阳光(苏州)氢能科技发展有限公司 | Hydrogen mixed residual gas reforming method |
| CN110950304A (en) * | 2019-12-16 | 2020-04-03 | 简阳绿杉新能源设备有限公司 | Method for preparing high-purity hydrogen by using natural gas |
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| CN113620244A (en) * | 2020-05-07 | 2021-11-09 | 中国石油化工股份有限公司 | System and method for hydrogen production by reforming natural gas steam |
| CN111620304A (en) * | 2020-06-12 | 2020-09-04 | 云南省能源研究院有限公司 | Hydrogen preparation method |
| CN111960382A (en) * | 2020-09-02 | 2020-11-20 | 西南化工研究设计院有限公司 | Efficient natural gas conversion hydrogen production method convenient for skid-mounting |
| CN112813454A (en) * | 2021-03-03 | 2021-05-18 | 中海石油气电集团有限责任公司 | Natural gas reforming and carbon dioxide combined hydrogen production power generation system and method |
| CN113213425A (en) * | 2021-06-08 | 2021-08-06 | 金川集团股份有限公司 | System and method for preparing hydrogen by using natural gas |
| CN114988364A (en) * | 2022-06-13 | 2022-09-02 | 重庆科技学院 | Power generation system based on natural gas hydrogen production and fuel cell technology |
| CN115368210A (en) * | 2022-09-06 | 2022-11-22 | 浙江清和新材料科技有限公司 | Method for treating tail gas hydrogen of hydrogenation reaction |
| CN115368210B (en) * | 2022-09-06 | 2024-04-30 | 浙江清和新材料科技有限公司 | Treatment method of tail gas hydrogen of hydrogenation reaction |
| CN115849304A (en) * | 2022-12-13 | 2023-03-28 | 江苏省特种设备安全监督检验研究院 | Preparation method and device for hydrogen production from natural gas |
| CN116621117A (en) * | 2023-05-24 | 2023-08-22 | 上海汉兴化工科技有限公司 | Preparation method of high-purity hydrogen for fuel cell |
| CN116621117B (en) * | 2023-05-24 | 2024-02-02 | 上海汉兴化工科技有限公司 | Preparation method of high-purity hydrogen for fuel cell |
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Application publication date: 20130102 |