TWI812634B - 自熱性氨裂解製程 - Google Patents
自熱性氨裂解製程 Download PDFInfo
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- TWI812634B TWI812634B TW107126906A TW107126906A TWI812634B TW I812634 B TWI812634 B TW I812634B TW 107126906 A TW107126906 A TW 107126906A TW 107126906 A TW107126906 A TW 107126906A TW I812634 B TWI812634 B TW I812634B
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 143
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 70
- 238000000034 method Methods 0.000 title claims abstract description 51
- 238000005336 cracking Methods 0.000 title claims abstract description 25
- 239000007789 gas Substances 0.000 claims abstract description 63
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 54
- MWUXSHHQAYIFBG-UHFFFAOYSA-N nitrogen oxide Inorganic materials O=[N] MWUXSHHQAYIFBG-UHFFFAOYSA-N 0.000 claims abstract description 39
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000001257 hydrogen Substances 0.000 claims abstract description 34
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 34
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 26
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000001301 oxygen Substances 0.000 claims abstract description 25
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 25
- 230000003197 catalytic effect Effects 0.000 claims abstract description 17
- 230000003647 oxidation Effects 0.000 claims abstract description 16
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 16
- 239000003054 catalyst Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910001868 water Inorganic materials 0.000 claims abstract description 15
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 14
- 238000006243 chemical reaction Methods 0.000 claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 claims abstract description 7
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 238000011084 recovery Methods 0.000 claims description 8
- 230000003750 conditioning effect Effects 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 3
- 238000002485 combustion reaction Methods 0.000 claims description 2
- 238000005201 scrubbing Methods 0.000 claims 1
- QJGQUHMNIGDVPM-UHFFFAOYSA-N nitrogen group Chemical group [N] QJGQUHMNIGDVPM-UHFFFAOYSA-N 0.000 abstract description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 8
- 238000000926 separation method Methods 0.000 description 7
- 239000000203 mixture Substances 0.000 description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 description 4
- 230000001590 oxidative effect Effects 0.000 description 4
- 230000005611 electricity Effects 0.000 description 3
- 239000007800 oxidant agent Substances 0.000 description 3
- 238000009825 accumulation Methods 0.000 description 2
- 239000003570 air Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000000446 fuel Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 239000012080 ambient air Substances 0.000 description 1
- 238000002453 autothermal reforming Methods 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 238000004523 catalytic cracking Methods 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003546 flue gas Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000003345 natural gas Substances 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000004227 thermal cracking Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
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- 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
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Abstract
本發明係關於一種自氨製造含氮氣及氫氣之產物氣體之方法，其包含以下步驟：用含氧氣體將氨非催化性部分氧化成含氮氣、水、一定量之氮氧化物及餘量為氨之製程氣體；藉由與含鎳催化劑接觸，將至少部分餘量氨裂解成製程氣體中之氫氣及氮氣，同時藉由與在藉由將製程氣體與含鎳催化劑接觸來裂製程氣體期間所形成之部分氫氣反應，將一定量之氮氧化物還原成氮氣及水；及抽出含氫氣及氮氣之產物氣體。
Description
本發明係關於一種含氮氣及氫氣之氣體之製造。更具體來說，本發明提供一種藉由一系列用含氧氣體將氣態氨非催化性部分氧化並且將部分氧化之製程氣體中所含之餘量氨裂解成氮氣及氫氣產物氣體來製造此氣體之方法。
液態氨為一種製造氫氣或重要能源載體之重要來源，尤其用於在具有少數或沒有燃料源之區域中產生電力。作為能源載體，液態氨亦可作為一種穩定由諸如風力、太陽能及水力發電等可再生能源技術所製造之波動電力之來源。氨作為能源載體之優點在於液態氨比例如天然氣或氫氣更易於運輸及儲存。
為了適合作為用於電力生產之燃料，需要將氨裂解成由氫氣及氮氣所組成之氣體混合物。
在氨裂解製程中，氣態氨在可逆反應中離解成氫氣及氮氣之混合物：2 NH3 
N2+3 H2
該反應為吸熱，需要加熱來維持氨裂解反應。
已發現，藉由以下反應在氨之放熱非催化部分氧化中所產生之熱量當隨後進行氨之吸熱催化裂解時足以提供必要的熱量。
2 NH3+3/2 O2 → N2+3 H2O
亦觀察到，當藉由與含鎳催化劑接觸進行氨之裂解時，在部分氧化氣體中所形成之氮氧化物被還原成氮氣及水。藉由在氨裂解反應期間所形成之氫氣將氮氧化物還原成無害的氮氣及水，並且不需要進一步的步驟來移除經裂解之氣體之氮氧化物。
另一個優點為根據本發明之方法使得氫氣產物氣體中無CO2生成，其意指該方法不產生任何CO2。若使用空氣作為氧化劑，則少量二氧化碳會與空氣一起添加至製程中，但由於製程反應不會形成額外的CO2，因此相同量之CO2會再次被釋放。
根據上述觀察，本發明提供一種自氨製造含氮氣及氫氣之產物氣體之方法，其包含以下步驟：用含氧氣體將氨非催化性部分氧化成含氮氣、水、大量氮氧化物及餘量為氨之製程氣體；藉由與含鎳催化劑接觸，將至少部分餘量氨裂解成製程氣體中之氫氣及氮氣，同時藉由與在藉由將製程氣體與含鎳催化劑接觸來裂製程氣體期間所形成之部分氫氣反應，將大量氮氧化物還原成氮氣及水；及抽出含氫氣及氮氣之產物氣體。
藉由本發明之方法，由於藉由與含鎳催化劑接觸而將氮氧化物與氫氣反應，該非催化性部分氧化步驟中所產生之氮氧化物之量受到熱力學平衡之限制係減少80%，實際上減少高達100%。
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圖1為根據本發明特定具體實例之氨裂解製程之示意圖，其包括自熱氨裂解反應器、氨分離步驟、產物氣體調節及氨回收。
圖2說明已知的自熱重組反應器。
在本發明一個較佳具體實例中，氨之非催化性部分氧化係藉由用低於化學計量之氧氣以氣態形式燃燒氨而在燃燒器中進行。
在另一個較佳具體實例中，非催化性部分氧化步驟及裂解步驟係在單一反應器容器中進行。由此，最佳化地保存來自放熱部分氧化之反應熱，以進行吸熱氨裂解反應。
單一反應器容器較佳經組態為自熱裂解反應器，其具有位於反應器容器入口側之燃燒器及位於燃燒器下游之催化劑床，類似於圖2所示之已知自熱重組反應器。
與含鎳催化劑接觸之後的平衡溫度可藉由改變進入非催化性部分氧化步驟中之氧氣與氨饋入流速而調節。此相當於改變λ值，該λ值為實際氧氣饋入流量與氨饋入成為氮氣及水之完全化學計量燃燒所需之流量之間之比例。對於固定的氨流速，可藉由增加含氧氣體中之氧濃度及/或藉由增加含氧氣體之流速來增加平衡溫度。
較佳地，調節非催化性部分氧化步驟之氧氣與氨饋入流速以在與含鎳催化劑接觸之後測量到產物氣體之平衡溫度在700至1100℃之間。
因此，在本發明一個具體實例中，含氧氣體中之氧含量以相應於λ=0.18至λ=0.30之間之λ值而變化，致使平衡溫度Teq=700-1100℃。
較佳地，在非催化性部分氧化步驟中所使用之含氧氣體含有10至100體積%之間的氧。
因此，用於含氧氣體之合適來源可為煙道氣至純氧或其混合物範圍內。
離開裂解步驟之所得產物氣體混合物係由氫氣、氮氣及水以及一定量之殘餘未裂解的氨所構成。
因此，在一個具體實例中，根據本發明之方法包含另一個步驟：將產物氣體中另外所含之未裂解的氨分離。
較佳地，該分離步驟係藉由水洗滌該產物氣體來進行。在此分離步驟中，來自熱裂解反應器之水之主要部分會與氨一起離開分離步驟。
在氨分離步驟中自產物氣體所分離之一定量之氨可在氨回收步驟(諸如蒸餾)中回收，並且經回收之氨較佳在該製程中再循環至非催化性部分氧化步驟。同時，該氨回收步驟會清潔製程冷凝物。
取決於最終氫氣/氮氣產物氣體之用途，可調節產物氣體中氫氣與氮氣之莫耳比以用於預期用途。
因此，在本發明另一個具體實例中，該方法包含另一個步驟：調節產物氣體調節單元中產物氣體之氫氣與氮氣莫耳比。該產物氣體調節步驟可包含膜或變壓吸附單元(Pressure Swing Adsorption；PSA)。
本發明一個較佳具體實例進一步含有將氫氣源添加至氨饋入中或直接添加至裂解反應器中之燃燒器中之可能性。將氫氣添加至氨饋入可將自燃溫度降低多達100℃，從而在較低的預熱溫度下自動點燃氨，並且在正常操作期間增加可燃性。氫氣源較佳為產物氣體或調節氨含量、水及/或氫氣/氮氣比之產物氣體。亦可使用來自各種公用事業來源及其他方法之氫氣。
用於裂解步驟之含氧氣體(諸如環境空氣)可含有少量CO2。眾所皆知，CO2及氨在水溶液中反應，此會致使氨回收區之結垢及/或腐蝕。此外，若不採取措施，CO2可能會在此製程中累積。本發明之較佳具體實例含有 自氧化劑移除CO2之措施，例如藉由用NaOH溶液洗滌氧化劑，或者在氨回收區中添加NaOH溶液至蒸餾塔以達到在汽提冷凝物中移除以Na2CO3形式表示之CO2之目的。
在該製程中避免CO2累積之另一種方法為在自熱氨裂解器與氨分離步驟之間包括甲烷化反應器。藉由此方法，利用自上游裂解反應器所獲得之氫氣將CO2轉化成甲烷：CO2+4 H2 
CH4+2 H2O
含鎳或貴金屬之催化劑可催化此反應。優點為甲烷不與水溶液中之氨反應，此意指在甲烷化反應器中藉由CO2轉化避免了CO2累積，並且所產生之甲烷隨後自氨分離步驟與產物氣體一起離開製程，而不挾帶冷凝物至回收區。
根據本發明之方法之特定具體實例展示於圖式中。
實施例
以下表1展示對應於λ值=0.21之用於氨裂解製程之製程氣體流量及組成物，以及在自熱氨裂解反應器中與含鎳催化劑接觸之後產物氣體所得之平衡溫度為800℃。流編號參見圖1。
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Claims (17)
- 一種自氨製造含氮氣及氫氣之產物氣體之方法，其包含以下步驟：用含氧氣體將氨非催化性部分氧化成含氮氣、水、一定量之氮氧化物及餘量為氨之製程氣體；藉由與含鎳催化劑接觸，將至少部分餘量氨裂解成該製程氣體中之氫氣及氮氣，同時藉由與在藉由將該製程氣體與該含鎳催化劑接觸來裂該製程氣體期間所形成之部分氫氣反應，將一定量之氮氧化物還原成氮氣及水；及抽出含氫氣及氮氣之產物氣體。
- 如請求項1所述之方法，其中藉由與該含鎳催化劑接觸而將氮氧化物與氫氣反應，非催化性部分氧化步驟中所產生之氮氧化物之量受到熱力學平衡之限制係減少大於80%，及高達100%。
- 如請求項1或請求項2所述之方法，其中該氨之非催化性部分氧化係藉由用低於化學計量之含氧氣體在燃燒器中以氣態形式燃燒氨來進行。
- 如請求項1或請求項2所述之方法，其中該非催化性部分氧化步驟及該裂解步驟係在單一反應器容器中進行。
- 如請求項4所述之方法，其中該單一反應器容器經組態為自熱裂解反應器。
- 如請求項1或請求項2所述之方法，其中調節該非催化性部分氧化步驟之氧氣與氨饋入流速以在與該含鎳催化劑接觸之後得到該產物氣體之700至1100℃之間之平衡溫度。
- 如請求項1或請求項2所述之方法，其中含氧氣體中之氧含量以相應於λ=0.18至λ=0.30之間之λ值而變化，其中λ為實際氧氣饋入流量與氨成為氮氣及水之完全化學計量燃燒所需之流量之間之比例。
- 如請求項1或請求項2所述之方法，其中含氧氣體含有10至100體 積%之間的氧。
- 如請求項1或請求項2所述之方法，其包含另一個步驟：藉由自該氨裂解步驟所獲得之氫氣在甲烷化反應器中將CO2轉化為甲烷。
- 如請求項1或請求項2所述之方法，其包含另一個步驟：將該產物氣體中另外所含之未裂解的氨分離。
- 如請求項8所述之方法，其中該未裂解的氨係藉由水洗滌自該產物氣體分離。
- 如請求項10所述之方法，其中所分離之氨係在氨回收步驟中回收，並且再循環至該非催化性部分氧化步驟。
- 如請求項10所述之方法，其包含添加NaOH至該氨回收步驟中。
- 如請求項1或請求項2所述之方法，其包含另一個步驟：調節產物氣體調節單元中該產物氣體之氫氣與氮氣莫耳比。
- 如請求項1或請求項2所述之方法，其包含將氫氣源添加至氨饋入中或直接添加至裂解反應器中之燃燒器中。
- 如請求項15所述之方法，其中該氫氣源為氨裂解產物氣體或調節氨含量及/或氫氣與氮氣比之產物氣體。
- 如請求項1或請求項2所述之方法，其包含含氧氣體之CO2移除洗滌。
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| WO2019038251A1 (en) | 2019-02-28 |
| CA3067780A1 (en) | 2019-02-28 |
| PL3672906T3 (pl) | 2023-05-15 |
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| ES2941070T3 (es) | 2023-05-16 |
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| AU2018320335A1 (en) | 2020-01-23 |
| TW201912565A (zh) | 2019-04-01 |
| EP3672906A1 (en) | 2020-07-01 |
| AU2018320335B2 (en) | 2024-07-18 |
| DK3672906T3 (da) | 2023-02-27 |
| US20200123006A1 (en) | 2020-04-23 |
| JP7319965B2 (ja) | 2023-08-02 |
| JP2020531388A (ja) | 2020-11-05 |
| CN110799451A (zh) | 2020-02-14 |
| CN110799451B (zh) | 2023-08-08 |
| US11511991B2 (en) | 2022-11-29 |
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