CN1034066C - Method for preparation of low pressure high pure hydrogen nitrogen mixed gas - Google Patents
Method for preparation of low pressure high pure hydrogen nitrogen mixed gas Download PDFInfo
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- CN1034066C CN1034066C CN92108638A CN92108638A CN1034066C CN 1034066 C CN1034066 C CN 1034066C CN 92108638 A CN92108638 A CN 92108638A CN 92108638 A CN92108638 A CN 92108638A CN 1034066 C CN1034066 C CN 1034066C
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- mixed gas
- pressure
- ammonia
- nitrogen mixed
- gas
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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
- C01B3/04—Production of hydrogen or of gaseous mixtures containing a substantial proportion of hydrogen by decomposition of inorganic compounds, e.g. ammonia
- C01B3/047—Decomposition of ammonia
-
- 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
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Inorganic Chemistry (AREA)
- Hydrogen, Water And Hydrids (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention relates to a method for preparing high purity hydrogen-nitrogen mixed gas by pressurizing ammonia decomposition. The technological process of the present invention is convenient and simple; compared with the traditional method, the method of the present invention omits the two processes of low pressure storage and pressurization of hydrogen and nitrogen gas, decreases the expense of equipment investment, omits hydrogen-nitrogen compressors, reduces the power consumption and lowers the gas preparation cost by 30%; the present invention has the advantages of convenient maintenance of the whole technological process, high safety, reliability and gas preparation cost decrease. In the impurity content of the high purity hydrogen-nitrogen mixed gas prepared by the method of the present invention, the remnant ammonia content is less than 1 ppm and the remnant oxygen content is less than 1 ppm; the water dew point is less than-70 DEG C; the high purity hydrogen-nitrogen mixed gas can be used as protective atmosphere in the bright heat treatment process in metallurgy industries.
Description
The present invention's ammonia that relates to pressurize decomposes the method that prepare high pure hydrogen nitrogen mixed gas, is used for the metal polish thermal treatment field of annealing.
In prior art, CN92108401.3 is that ammonia decomposes the system high pure hydrogen nitrogen mixed gas and is used in the protection gas of WU groove in the float glass industry, protects atmosphere but also need to go bail for High Purity Hydrogen nitrogen in metallurgical industry.As when powder metallurgy, Special Alloy Steel and stainless steel are produced, passing to shielding gas, improve the quality of product.Add man-hour in metal treatment, also must adopt hydrogen and nitrogen gas to make protection gas, with the quality of stable prod to corrosion-resistant high temperature process cold rolling or siliconized plate.After in metal polish annealing thermal treatment industry, having adopted protective atmosphere, can make after the annealing the part light is flawless in addition.The copper material industry mostly adopted the device flow process of the product introduction of Austrian Ai Baile company (ABRON Co.) in bright heat treatment in the past, decomposing the branch of producing 75% hydrogen and 25% nitrogen with normal pressure ammonia vents one's spleen, import the combustion chamber after sending storage cabinet, allocate air in certain amount simultaneously into, make its partial combustion, the gas mixture that contains 70～99.5% nitrogen and 0.5～30% hydrogen with producing uses the gas mixture supercharging with hydrogen nitrogen compressor again after purifying.Though dependable performance like this, index is feasible.But have some problems, as ammonia decomposition combustion system nitrogen and a small amount of hydrogen gas mixture, this method is uneconomical.Big with the investment of hydrogen nitrogen compressor boost, build compressor plant separately, special messenger's operation, the equipment complexity, power consumption is big, safeguards inconvenience, and also requirement of explosion proof will be arranged to hydrogen nitrogen compressor, and is relatively more dangerous.
The objective of the invention is to reduce the facility investment expense, saved hydrogen nitrogen compressor and can reduce power consumption, make whole technological process easy to maintenance, safe and reliable, reach this low purpose of system pneumatolytic in order to economize two processes of denitrification hydrogen low pressure storage and supercharging.
What the present invention used is that industrial dense ammonia is raw material, behind the liquefied ammonia carburation by evaporation, enters ammonia destruction furnace through heat exchanger, it is to carry out having under the situation of pressure that ammonia decomposes, and pressure is 0.25～0.9MPa, and temperature is 550～950 ℃, adopt nickel-base catalyst, ferrum-based catalyst, preferably use nickel-base catalyst.
It is to carry out having under the situation of pressure that the used ammonia of the present invention decomposes, and best pressure range is 0.3～0.6MPa, and best temperature range is 650～850 ℃.
Decompose the direct drawing-in system of pressure hydrogen nitrogen mixed gas that obtains through ammonia, residual ammonia 500～2000PPm in the mixed decomposition gas, residual water is below 2%.
Divide vent one's spleen and nitrogen that the absorption of carbonaceous molecular sieve transformation makes wait depress directly mixed mutually.A nitrogen content that the absorption of carbonaceous molecular sieve transformation makes is generally about 99%.Pass through catalytic deoxidation together, deoxidation temperature is a normal temperature, and the catalyzer of deoxidation is high efficiency deoxidiser, palladium platinum bimetal, and best choice is with the deoxidation of palladium platinum bimetallic catalytic.
After condensation dewaters, send into the adsorption cleaning device through the gas mixture of deoxidation, depress adsorption cleaning adding.Sorbent material in the adsorption cleaning device is made up of bilayer absorption.Mainly remove ammonia and water in the gas mixture.
The used ammonia destruction furnace inside of the present invention is three sleeve type structures, is full of nickel-base catalyst at the urceolus annular space.Decomposition temperature measure by the secondary instrument electronic regulator by temperature thermocouple and with contact relay system and interlocks.Decomposition pressure is interlocked by the pressure controller measurement and with heating unit by liquefied ammonia evaporation control.
Sorbent material in the used adsorption cleaning device of the present invention is made up of molecular sieve and the double-deck absorption of silica gel institute.Adsorbed gas and resurgent gases can have heating unit in the reverse cleaner by adsorption layer, a card is arranged with adsorption cleaning device separated into two parts in the adsorption cleaning device, put sorbent material at an upper portion thereof, described heating unit extends to the hot cell of giving under the card by the cleaner top through adsorption layer always.
In the high pure hydrogen nitrogen mixed gas of 0.25～0.9MPa that the present invention makes, hydrogen is at 0.1～40% (volume), and surplus is a nitrogen.Wherein the residual ammonia of foreign matter content is＜1PPm, and residual oxygen is＜1PPm that the dew point of residual water is between-70～-80 ℃.
With regard to ammonia decomposed, pressing technology was disadvantageous, certainly will influence branch vent one's spleen in the content of residual ammonia can rise to some extent, but favourable to adsorption cleaning.Therefore the present invention decomposes with normal pressure ammonia---and adsorption cleaning is compared, and adsorption deeply is constant, and the processed in units of sorbent material does not reduce, so pressurization nitrogen decomposes---the technology of adsorption cleaning is feasible.
The high pure hydrogen nitrogen mixed gas of the inventive method preparation can be used in metallurgical industry, and the photothermal treatment process that can be used on especially in the metallurgy industry is made protection atmosphere.
The present invention compares with the flow process of Austrian Ai Baile company, and technology is easy, has saved expensive hydrogen nitrogen compressor and huge low pressure gas holder, and replaces adding the air portion divided combustion with carbonaceous molecular sieve making nitrogen by pressure swing adsorption gas, and the facility investment expense is reduced significantly.The present invention can reduce power consumption owing to saved hydrogen nitrogen compressor, makes whole technological process easy to maintenance, safe and reliable, has reached to reduce system pneumatolytic purpose originally.The system pneumatolytic is originally compared with traditional method can descend 30%.
Embodiment 1:
Behind the liquefied ammonia carburation by evaporation, enter ammonia destruction furnace through heat exchanger, it is to carry out under the situation of pressurization that ammonia decomposes, and pressure is 0.28MPa, and temperature is 720 ℃, adopts nickel-base catalyst, decomposes the wherein residual ammonia 2000PPm of back hydrogen 75% nitrogen 25%.
Divide and to vent one's spleen and 99% nitrogen that the absorption of carbonaceous molecular sieve transformation makes is depressed directly mixedly mutually waiting, pass through catalytic deoxidation together at normal temperatures, employing palladium platinum bimetal dehydrogenation catalyst.
Behind the gaseous mixture condensation, depress adsorption catalysis adding, the sorbent material in the adsorption cleaning device is molecular sieve and silica gel.
The residual ammonia 0.7PPm of foreign matter content in the product high pure hydrogen nitrogen mixed gas that makes, residual oxygen 0.5PPm, residual water are not more than-70 ℃ of dew points, and this gas mixture is applicable to that the bright heat treatment process is made protection atmosphere in the metallurgy industry.
Embodiment 2:
The preparation process of High Purity Hydrogen nitrogen is with embodiment 1.
The ammonia decomposition pressure is 0.7MPa, 900 ℃ of temperature, residual ammonia 1500PPm during branch is vented one's spleen; the residual ammonia 0.6PPm of foreign matter content in the product high pure hydrogen nitrogen mixed gas that makes; residual oxygen 0.4PPm, residual water are not more than-80 ℃ of dew points, and this gas mixture is applicable to that the bright heat treatment process is made protection atmosphere in the metallurgy industry.
Embodiment 3:
The preparation process of High Purity Hydrogen nitrogen is with embodiment 1.
The ammonia decomposition pressure is 0.4MPa, 780 ℃ of temperature, and residual ammonia 1000PPm during branch is vented one's spleen, the residual ammonia 0.5PPm of foreign matter content in the product high pure hydrogen nitrogen mixed gas that makes, residual oxygen 0.4PPm, residual water are not more than-75 ℃ of dew points.This gas mixture is applicable to that the bright heat treatment process is made protection atmosphere in the metallurgy industry.
Claims (3)
1, a kind of preparation method of high pure hydrogen nitrogen mixed gas is characterized in that this method comprises the steps:
1. enter ammonia destruction furnace after the liquefied ammonia vaporization, decompose having under the situation of pressure, temperature is 550～950 ℃, and pressure is 0.25～0.9MPa, adopts nickel-base catalyst, the direct drawing-in system of pressure hydrogen nitrogen mixed gas that obtains,
2. the nitrogen that makes of carbonaceous molecular sieve transformation absorption and above-mentioned branch vent one's spleen directly mixed mutually under identical pressure 0.25～0.9MPa, in the gas mixture hydrogen content at 0.1～40% (volume),
3. after mixing mutually (pressure be 0.25～0.9MPa) gas mixture through catalytic deoxidation, temperature is a normal temperature, catalyzer is a palladium platinum bimetal,
4. after the deoxidation (pressure be 0.25～0.9MPa) gas mixture after condensation dewaters, send into the adsorption cleaning device and remove ammonia and water, the sorbent material in the adsorption cleaning device is made up of bilayer absorption institute.
2, according to the preparation method of the described high pure hydrogen nitrogen mixed gas of claim 1, it is characterized in that: the temperature that pressurization ammonia decomposes is 650～850 ℃.
3, according to the preparation method of the described high pure hydrogen nitrogen mixed gas of claim 1, it is characterized in that: the pressure that pressurization ammonia decomposes is 0.3～0.6MPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92108638A CN1034066C (en) | 1992-11-19 | 1992-11-19 | Method for preparation of low pressure high pure hydrogen nitrogen mixed gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN92108638A CN1034066C (en) | 1992-11-19 | 1992-11-19 | Method for preparation of low pressure high pure hydrogen nitrogen mixed gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1087319A CN1087319A (en) | 1994-06-01 |
| CN1034066C true CN1034066C (en) | 1997-02-19 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN92108638A Expired - Fee Related CN1034066C (en) | 1992-11-19 | 1992-11-19 | Method for preparation of low pressure high pure hydrogen nitrogen mixed gas |
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| CN (1) | CN1034066C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7867300B2 (en) * | 2001-03-02 | 2011-01-11 | Intelligent Energy, Inc. | Ammonia-based hydrogen generation apparatus and method for using same |
| CN100571850C (en) * | 2003-06-30 | 2009-12-23 | 上海化工研究院 | The recycling technology of molecular sieve adsorption product gas during neon isotope separates |
| CN101575102B (en) * | 2009-06-12 | 2012-09-05 | 武汉高安新材料有限公司 | Preparation of high-purity ammonia by integrating three steps of ammonia catalytic pyrolysis, hydrogen and nitrogen purification and ammonia synthesis |
| CN102431967A (en) * | 2011-07-18 | 2012-05-02 | 何巨堂 | Method for preparing hydrogen and nitrogen gas with specific composition from multi-ingredient gas containing H2 and N2 |
| CN102910580B (en) * | 2012-11-09 | 2015-03-11 | 湖南高安新材料有限公司 | Energy-saving device and method for decomposing ammonia to prepare high-purity hydrogen-nitrogen mixture gas |
| CN103449362A (en) * | 2013-08-08 | 2013-12-18 | 兴城市粉末冶金有限公司 | Method for producing nitrogen for forging gas shield by using liquid ammonia |
| KR20230072223A (en) * | 2021-11-17 | 2023-05-24 | 주식회사 포스코 | Method for manufacturing hydrogen gas from ammonia by using pressure swing adsorption |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1161457A1 (en) * | 1983-01-07 | 1985-06-15 | Ленинградский Ордена Октябрьской Революции И Ордена Трудового Красного Знамени Технологический Институт Им.Ленсовета | Method of ammonia decomposition |
| SU324814A1 (en) * | 1969-12-08 | 1986-08-30 | Golosman E Z | Method of dissociating ammonia |
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1992
- 1992-11-19 CN CN92108638A patent/CN1034066C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU324814A1 (en) * | 1969-12-08 | 1986-08-30 | Golosman E Z | Method of dissociating ammonia |
| SU1161457A1 (en) * | 1983-01-07 | 1985-06-15 | Ленинградский Ордена Октябрьской Революции И Ордена Трудового Красного Знамени Технологический Институт Им.Ленсовета | Method of ammonia decomposition |
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| Publication number | Publication date |
|---|---|
| CN1087319A (en) | 1994-06-01 |
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Granted publication date: 19970219 Termination date: 20091221 |