CN1034066C - 低压高纯氢氮混合气的制备方法 - Google Patents
低压高纯氢氮混合气的制备方法 Download PDFInfo
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 229910052757 nitrogen Inorganic materials 0.000 title claims abstract description 38
- 239000007789 gas Substances 0.000 title claims abstract description 37
- 239000001257 hydrogen Substances 0.000 title claims abstract description 31
- 229910052739 hydrogen Inorganic materials 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 24
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 125000004435 hydrogen atom Chemical class [H]* 0.000 title 1
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 70
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 35
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000002431 hydrogen Chemical class 0.000 claims description 23
- 238000001179 sorption measurement Methods 0.000 claims description 17
- 238000004140 cleaning Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 11
- 238000010521 absorption reaction Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 7
- 239000002808 molecular sieve Substances 0.000 claims description 7
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims description 7
- 210000000952 spleen Anatomy 0.000 claims description 7
- 239000002594 sorbent Substances 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 4
- 230000006378 damage Effects 0.000 claims description 4
- JRTYPQGPARWINR-UHFFFAOYSA-N palladium platinum Chemical group [Pd].[Pt] JRTYPQGPARWINR-UHFFFAOYSA-N 0.000 claims description 4
- 230000009466 transformation Effects 0.000 claims description 4
- 238000009833 condensation Methods 0.000 claims description 3
- 230000005494 condensation Effects 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims 1
- 238000009834 vaporization Methods 0.000 claims 1
- 230000008016 vaporization Effects 0.000 claims 1
- 238000010438 heat treatment Methods 0.000 abstract description 8
- 238000000354 decomposition reaction Methods 0.000 abstract description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 5
- 238000005272 metallurgy Methods 0.000 abstract description 5
- 239000001301 oxygen Substances 0.000 abstract description 5
- 229910052760 oxygen Inorganic materials 0.000 abstract description 5
- 238000012423 maintenance Methods 0.000 abstract description 3
- 238000003860 storage Methods 0.000 abstract description 3
- 229910001873 dinitrogen Inorganic materials 0.000 abstract description 2
- 230000001681 protective effect Effects 0.000 abstract description 2
- 230000007423 decrease Effects 0.000 abstract 2
- 239000012535 impurity Substances 0.000 abstract 1
- 238000002485 combustion reaction Methods 0.000 description 4
- 238000000137 annealing Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- 230000008020 evaporation Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 239000000741 silica gel Substances 0.000 description 2
- 229910002027 silica gel Inorganic materials 0.000 description 2
- 238000007669 thermal treatment Methods 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000005097 cold rolling Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000006356 dehydrogenation reaction Methods 0.000 description 1
- 230000000994 depressogenic effect Effects 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000005329 float glass Substances 0.000 description 1
- 239000008246 gaseous mixture Substances 0.000 description 1
- 230000008676 import Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
Classifications
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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
本发明是涉及加压氨分解制备高纯氢氮混合气的方法，工艺过程简便，和传统法相比，省去了氢氮气低压贮存和增压二个过程，减少设备投资费用，省去了氢氮压缩机，可以减少动力消耗，使整个工艺过程维护方便，安全可靠，达到了降低制气成本，本发明的制气成本和传统的方法相比可下降30%。
用本发明的方法制备的高纯氢氮混合气中杂质含量残氨＜1ppm，残氧＜1ppm，水的露点＜-70℃此产品气可用于冶金行业中光亮热处理过程作保护气氛。
Description
本发明是涉及加压氨分解制备高纯氢氮混合气的方法，用于金属光亮退火热处理领域。
在已有技术中，CN92108401.3是氨分解制高纯氢氮混合气用在浮法玻璃工业中钖槽的保护气，但在冶金工业中也需要用高纯氢氮气作保护气氛。如在粉末冶金、特种合金钢和不锈钢生产时需要通以保护气体，提高产品的质量。在金属处理加工时，也必须对耐腐蚀冷轧或硅钢片的高温加工采用氢氮气作保护气，以稳定产品的质量。在金属光亮退火热处理工业中采用了保护气氛后，可使退火后的另件光亮无疵。以往铜材行业大都采用奥地利埃柏勒公司(ABRON Co.)在光亮热处理中的产品介绍的装置流程，用常压氨分解制取75％氢气和25％氮气的分解气，送贮柜后导入燃烧室，同时配入一定量的空气，使其部分燃烧，将产生的含70～99.5％氮气和0.5～30％氢的混合气，再用氢氮压缩机把混合气增压经净化后使用。这样虽然性能可靠，指标可行。但存在一些问题，如氨分解燃烧制氮及少量氢混合气，这种方法不经济。用氢氮压缩机增压投资大，要单独建压缩机房，专人操作，设备复杂，动力消耗大，维护不便，而且对氢氮压缩机还要有防爆要求，比较危险。
本发明的目的是为了省去氮氢气低压贮存及增压二个过程，减少设备投资费用，省去了氢氮压缩机可以减少动力消耗，使整个工艺过程维护方便，安全可靠，达到制气成本低的目的。
本发明使用的是工业浓氨为原料，液氨蒸发汽化后，经热交换器进入氨分解炉，氨分解是在有压力的情况下进行，压力是0.25～0.9MPa，温度是550～950℃，采用镍基催化剂、铁基催化剂，最好是用镍基催化剂。
本发明所用的氨分解是在有压力的情况下进行，最佳的压力范围是0.3～0.6MPa，最佳的温度范围是650～850℃。
经过氨分解得到的低压氢氮混合气直接引入系统，混合分解气中残氨500～2000PPm，残水在2％以下。
分解气和碳分子筛变压吸附制得的氮气在等压下直接相混。碳分子筛变压吸附制得的氮气含量一般在99％左右。一起经过催化脱氧，脱氧温度是常温，脱氧的催化剂是高效脱氧剂、钯铂双金属，最好的选择是用钯铂双金属催化脱氧。
经过脱氧的混合气经冷凝除水后，送入吸附净化器，在加压下吸附净化。吸附净化器中的吸附剂是由双层吸附所组成。主要除去混合气中的氨和水。
本发明所用的氨分解炉内部为三套管式结构，在外筒环隙充满镍基催化剂。分解温度由测温热电偶通过二次仪表电子控制器测量并与接触继电装置联锁。分解压力由液氨蒸发控制，通过压力控制器测量并与加热装置联锁。
本发明所用的吸附净化器中的吸附剂是由分子筛和硅胶双层吸附所组成。吸附气和再生气可逆向通过吸附层的净化器内有加热元件，吸附净化器中有一块花板将吸附净化器分成两部分，在其上部放吸附剂，所述的加热元件由净化器顶部经吸附层一直延伸至花板下的予热室。
本发明制得的0.25～0.9MPa的高纯氢氮混合气中，氢气在0.1～40％(体积)，余量为氮气。其中杂质含量残氨是＜1PPm，残氧是＜1PPm，残水的露点在-70～-80℃之间。
就氨分解而言，加压工艺是不利的，势必影响分解气中残氨的含量会有所上升，但对吸附净化有利。因此本发明和常压氨分解——吸附净化相比，吸附深度不变，而吸附剂的单位处理并不降低，所以加压氮分解——吸附净化的工艺是可行的。
本发明方法制备的高纯氢氮混合气可以用在冶金工业，特别可用在冶金行业中的光热处理过程作保护气氛。
本发明和奥地利埃柏勒公司的流程相比，工艺简便，省去了昂贵的氢氮压缩机和庞大的低压气柜，并且用碳分子筛变压吸附制氮气代替加空气部分燃烧，使设备投资费用大幅度降低。本发明由于省去了氢氮压缩机，可以减少动力消耗，使整个工艺过程维护方便、安全可靠，达到了降低制气成本的目的。制气成本和传统的方法相比可下降30％。
实施例1：
液氨蒸发汽化后，经热交换器进入氨分解炉，氨分解是在加压的情况下进行，压力是0.28MPa，温度是720℃，采用镍基催化剂，分解后氢气75％氮气25％其中残氨2000PPm。
分解气和碳分子筛变压吸附制得的99％氮气在等压下直接相混，一起在常温下经过催化脱氧，采用钯铂双金属脱氧催化剂。
混合气冷凝后，在加压下吸附催化，吸附净化器中的吸附剂是分子筛和硅胶。
制得的产品高纯氢氮混合气中杂质含量残氨0.7PPm，残氧0.5PPm，残水不大于-70℃露点，此混合气适用于冶金行业中光亮热处理过程作保护气氛。
实施例2：
高纯氢氮气的制备过程同实施例1。
氨分解压力是0.7MPa，温度900℃，分解气中残氨1500PPm，制得的产品高纯氢氮混合气中杂质含量残氨0.6PPm，残氧0.4PPm，残水不大于-80℃露点，此混合气适用于冶金行业中光亮热处理过程作保护气氛。
实施例3：
高纯氢氮气的制备过程同实施例1。
氨分解压力是0.4MPa，温度780℃，分解气中残氨1000PPm，制得的产品高纯氢氮混合气中杂质含量残氨0.5PPm，残氧0.4PPm，残水不大于-75℃露点。此混合气适用于冶金行业中光亮热处理过程作保护气氛。
Claims (3)
1、一种高纯氢氮混合气的制备方法，其特征在于该方法包括如下步骤：
①液氨汽化后进入氨分解炉，在有压力的情况下进行分解，温度是550～950℃，压力是0.25～0.9MPa，采用镍基催化剂，得到的低压氢氮混合气直接引入系统，
②碳分子筛变压吸附制得的氮气与上述分解气在相同的压力0.25～0.9MPa下直接相混，混合气中氢气含量在0.1～40％(体积)，
③相混后的(压力是0.25～0.9MPa)混合气经催化脱氧，温度是常温，催化剂是钯铂双金属，
④脱氧后的(压力是0.25～0.9MPa)混合气经冷凝除水后，送入吸附净化器除氨和水，吸附净化器中的吸附剂是由双层吸附所组成。
2、据权利要求1所述的高纯氢氮混合气的制备方法，其特征是：加压氨分解的温度是650～850℃。
3、据权利要求1所述的高纯氢氮混合气的制备方法，其特征是：加压氨分解的压力是0.3～0.6MPa。
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| Application Number | Priority Date | Filing Date | Title |
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| CN92108638A CN1034066C (zh) | 1992-11-19 | 1992-11-19 | 低压高纯氢氮混合气的制备方法 |
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| CN92108638A CN1034066C (zh) | 1992-11-19 | 1992-11-19 | 低压高纯氢氮混合气的制备方法 |
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| CN1087319A CN1087319A (zh) | 1994-06-01 |
| CN1034066C true CN1034066C (zh) | 1997-02-19 |
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| CN92108638A Expired - Fee Related CN1034066C (zh) | 1992-11-19 | 1992-11-19 | 低压高纯氢氮混合气的制备方法 |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US7867300B2 (en) * | 2001-03-02 | 2011-01-11 | Intelligent Energy, Inc. | Ammonia-based hydrogen generation apparatus and method for using same |
| CN100571850C (zh) * | 2003-06-30 | 2009-12-23 | 上海化工研究院 | 氖同位素分离中分子筛吸附产品气的回收利用工艺 |
| CN101575102B (zh) | 2009-06-12 | 2012-09-05 | 武汉高安新材料有限公司 | 氨催化裂解、氢氮气纯化和氨合成三步集成制备高纯氨的方法 |
| CN102431967A (zh) * | 2011-07-18 | 2012-05-02 | 何巨堂 | 一种用含h2、n2多组分气制备特定组成氢氮气的方法 |
| CN102910580B (zh) * | 2012-11-09 | 2015-03-11 | 湖南高安新材料有限公司 | 节能型氨分解获得高纯氢氮混合气的装置及其方法 |
| CN103449362A (zh) * | 2013-08-08 | 2013-12-18 | 兴城市粉末冶金有限公司 | 用于锻造气体保护的液氨制氮方法 |
| KR20230072223A (ko) * | 2021-11-17 | 2023-05-24 | 주식회사 포스코 | 압력변동흡착을 이용한 암모니아로부터 수소의 제조방법 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| SU1161457A1 (ru) * | 1983-01-07 | 1985-06-15 | Ленинградский Ордена Октябрьской Революции И Ордена Трудового Красного Знамени Технологический Институт Им.Ленсовета | Способ разложени аммиака |
| SU324814A1 (ru) * | 1969-12-08 | 1986-08-30 | Golosman E Z | Способ диссоциации аммиака |
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| SU324814A1 (ru) * | 1969-12-08 | 1986-08-30 | Golosman E Z | Способ диссоциации аммиака |
| SU1161457A1 (ru) * | 1983-01-07 | 1985-06-15 | Ленинградский Ордена Октябрьской Революции И Ордена Трудового Красного Знамени Технологический Институт Им.Ленсовета | Способ разложени аммиака |
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| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
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Granted publication date: 19970219 Termination date: 20091221 |