CN1190414C - 氨和脲的联合制备方法 - Google Patents
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- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 229910021529 ammonia Inorganic materials 0.000 title claims abstract description 63
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000004202 carbamide Substances 0.000 title claims abstract description 27
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 39
- 238000003786 synthesis reaction Methods 0.000 claims abstract description 39
- 238000000034 method Methods 0.000 claims abstract description 30
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000000376 reactant Substances 0.000 claims abstract description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 229910002092 carbon dioxide Inorganic materials 0.000 claims abstract description 14
- 239000001569 carbon dioxide Substances 0.000 claims abstract description 13
- BVCZEBOGSOYJJT-UHFFFAOYSA-N ammonium carbamate Chemical compound [NH4+].NC([O-])=O BVCZEBOGSOYJJT-UHFFFAOYSA-N 0.000 claims abstract description 10
- KXDHJXZQYSOELW-UHFFFAOYSA-N carbonic acid monoamide Natural products NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims abstract description 10
- 239000007864 aqueous solution Substances 0.000 claims abstract description 8
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 5
- 238000005201 scrubbing Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 abstract description 4
- 239000007789 gas Substances 0.000 description 29
- 238000004519 manufacturing process Methods 0.000 description 10
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 3
- KXDHJXZQYSOELW-UHFFFAOYSA-M Carbamate Chemical group NC([O-])=O KXDHJXZQYSOELW-UHFFFAOYSA-M 0.000 description 3
- 239000006096 absorbing agent Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 description 3
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000001099 ammonium carbonate Substances 0.000 description 2
- 235000012501 ammonium carbonate Nutrition 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 238000005057 refrigeration Methods 0.000 description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 229910002091 carbon monoxide Inorganic materials 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002808 molecular sieve Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 238000010926 purge Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C273/00—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups
- C07C273/02—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds
- C07C273/10—Preparation of urea or its derivatives, i.e. compounds containing any of the groups, the nitrogen atoms not being part of nitro or nitroso groups of urea, its salts, complexes or addition compounds combined with the synthesis of ammonia
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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
- C01B3/025—Preparation or purification of gas mixtures for ammonia synthesis
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- C01B3/00—Hydrogen; Gaseous mixtures containing hydrogen; Separation of hydrogen from mixtures containing it; Purification of hydrogen
- C01B3/50—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification
- C01B3/52—Separation of hydrogen or hydrogen containing gases from gaseous mixtures, e.g. purification by contacting with liquids; Regeneration of used liquids
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- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/02—Preparation, purification or separation of ammonia
- C01C1/04—Preparation of ammonia by synthesis in the gas phase
- C01C1/0405—Preparation of ammonia by synthesis in the gas phase from N2 and H2 in presence of a catalyst
- C01C1/0488—Processes integrated with preparations of other compounds, e.g. methanol, urea or with processes for power generation
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- C01B2203/0465—Composition of the impurity
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Abstract
用于脲和氨反应物的联合制备的方法，该方法包含以下步骤：提供含二氧化碳的氨合成气以及将合成气转化成氨反应物，使氨反应物与合成气中的二氧化碳发生反应生成氨基甲酸铵和生成脲产品，该方法还包含以下步骤：在合成气转化成氨反应物之前，(i)以氨反应物的水溶液洗涤合成气并形成富含氨基甲酸铵的溶液；(ii)通过用水洗涤从洗涤过的合成气中除去过量的氨反应物并排出氨反应物的水溶液；(iii)通过除去残留的水和氨而净化水洗涤过的合成气；并且(iv)使净化过的合成气输送到气体转化至氨反应物的反应中。
Description
发明领域
本发明涉及通过在合成脲工艺中结合入氨反应物的制备而生产脲的方法。
发明背景
脲目前是经以下反应从氨基甲酸铵制得的：
大多数脲的生产与合成氨工厂有关，因为所需的二氧化碳可从氨工厂前段的合成气净化系统获得。
世界氨产量的很大一部分都用于脲的生产。因此，脲生产的联合工艺可能会有其技术和经济优势。但是按现有技术，脲和氨的生产是在相互无甚关联的工厂中进行的。
某些联合工艺是已知的，例如在美国专利4,235,816中公开了一种用于氨/脲生产的工艺。原料合成气中的二氧化碳通过用氨的水溶液洗涤而除去，形成氨基甲酸铵，并进一步转化为脲。气体进一步用碳酸铵的溶液洗涤，提纯除去一氧化碳和水，并随后转化为用于氨水溶液的氨。但是该工艺需要碳酸铵的水溶液作为原料进料。
另一种联合工艺描述于英国专利GB 1 470 489中，其中含有二氧化碳的合成气分别用氨的浓和稀水溶液洗涤两次。洗涤后的气体通入氨转化装置中，并且转化后的气体用水洗涤，然后再循环到氨转化装置入口处。在该工艺中，进入氨转化装置的原料是一种合成气和水洗涤流体气体的混合物。这就使得必须要除去水，以不污染转化催化剂和大大降低催化剂的活性。
发明内容
本发明的一般目的是提供一种经由二氧化碳与氨生成氨基甲酸铵以及氨基甲酸盐分解成脲产品的上述反应制备脲的改进方法，其中通过向合成氨的合成气净化中结合入二氧化碳和氨反应物的制备而将氨的生产和脲的生产结合在一个单一的流程中。
根据该一般目的，本发明提供用于脲和氨反应物的联合制备的方法，该方法包含以下步骤：提供含二氧化碳的氨合成气以及将合成气转化成氨反应物，使氨反应物与合成气中的二氧化碳发生反应生成氨基甲酸铵以至脲产品，该方法还包含以下步骤：
在合成气转化成氨反应物之前，
(i)以氨反应物的水溶液洗涤合成气并形成富含氨基甲酸铵的溶液；
(ii)通过用水洗涤从洗涤过的合成气中除去过量的氨反应物并排出氨反应物的水溶液；
(iii)通过吸附残留的水和氨而净化水洗涤过的合成气；并且
(iv)使净化过的合成气输送到气体转化至氨反应物的反应中。
附图说明
附图是描述一种根据本发明一个特定的实施方案从二氧化碳和氨反应物制备脲的联合方法的方框图。
具体实施方案
在由常规HDS、转化和变换区(Reforming and Shift Section)构成的气体制备单元后是一个使CO2含量高的气体的压力提高到适于合成氨的压力的单元。然后以氨水溶液洗涤该气体以除去绝大部分的CO2。形成的氨基甲酸盐溶液输送到脲反应器中去。在溶液中溶解的气体可从此处循环至压缩机的吸入端。
大部分已洗涤过的气体此时用作氨合成的补充气体。首先CO选择性methanisation除去残留的CO。从methanisation步骤出料的气体被NH3饱和并与从氨合成塔出料的气体混合。将混合料流导入洗涤单元中，在此处经水洗除氨。因为该工艺是放热性的，所以优选两阶段工艺：在第一阶段中，气体与相对较浓的氨溶液接触，吸收掉约一半量的氨。在第二阶段中，用出自脲单元的水进行最终的吸收。
离开吸收单元的气体含有一些氨，但也含一些水，在进入氨合成塔之前必需除去。该过程可借助分子筛或氧化铝在质量吸收器中进行。质量吸收器可经清洗气再生。在质量吸收器的下游，气体流过循环压缩机，然后输入由高温热交换器、合成塔和蒸汽发生器构成的常规合成单元。冷却至室温后，气体如上所述输送至水吸收单元中。
因为氨基甲酸盐反应在高温进行而且因为在工艺过程中产生大量的水，所以无需为此制造低温的无水氨。很明显，所生产的氨中含水量太高会对脲工艺有不利影响，因为水会降低脲的产率并因此而加剧循环量。因此，需要一定程度提高氨的浓度。在常规氨工艺中，在操作于中压，典型地15-17kg/cm2g的氨浓缩单元中所用的低温热量一般总有过剩。在该压力下，通过在低于120℃的低温下蒸馏的方法可使氨的浓度显著升至高达85％。
该工艺省去了两个压缩机(冷冻和CO2)、一个冷冻回路和氨工厂中的一个除CO2单元。因为合成塔入口处NH3的浓度可接近零，所以可达到减小合成塔尺寸或降低循环率的目的。脲工厂中的设备有很大一部分是用以回收CO2和NH3的。通过用氨洗涤除去CO2；经水洗涤以及蒸馏，随后除去氨。主要为氢和氮的“惰性”成分最终排放到大气中。
通过使惰性气体循环至合成气压缩机的吸入端，可简化工艺并减少脲工厂中单元数目。而且，脲工厂采用了一种工艺凝液汽提系统以净化工艺水，从而使其适用于锅炉给水。氨工厂中采用了一种类似的系统，并且两个系统的联用可以具有某些潜在的益处。
Claims (2)
1.一种用于脲和氨反应物的联合制备的方法，该方法包含以下步骤：
(a)提供含二氧化碳的合成气；
(b)将合成气转化成氨反应物；
(c)使氨反应物与合成中的二氧化碳发生反应生成氨基甲酸铵；
(d)使氨基甲酸铵反应成为脲产品；
特征在于步骤(b)和(c)包含：
(i)以氨反应物的水溶液洗涤合成气并形成步骤(c)的富含氨基甲酸铵的溶液，并从洗涤后的合成气中除去残余的二氧化碳；
(ii)将洗涤后的合成气与氨合成流出物混合，通过水洗从混合后的合成气流中除去氨反应物，并排出氨反应物水溶液，所述溶液在浓缩步骤(i)的氨反应物水溶液后形成；
(iii)通过除去残余量的水和氨提纯水洗后的合成气；和
(iV)使提纯后的合成气通到气体向氨反应物转化中，形成步骤(ii)的氨合成流出物。
2.权利要求1的方法，其中由步骤(ii)的浓缩形成的水返回作为步骤(ii)的洗涤水。
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DKPA200001371 | 2000-09-15 | ||
| DKPA200001371 | 2000-09-15 |
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| CN1190414C true CN1190414C (zh) | 2005-02-23 |
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| Country | Link |
|---|---|
| US (1) | US6723876B2 (zh) |
| EP (1) | EP1188710A3 (zh) |
| JP (1) | JP2002114752A (zh) |
| CN (1) | CN1190414C (zh) |
| CA (1) | CA2357256C (zh) |
| RU (1) | RU2283832C2 (zh) |
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| EP1626042A1 (en) | 2004-08-10 | 2006-02-15 | Urea Casale S.A. | Process for urea production from ammonia and carbon dioxide |
| US7642377B1 (en) | 2008-07-21 | 2010-01-05 | Kellogg Brown & Root Llc | Systems and methods for integrated ammonia-urea process |
| EP2321390A4 (en) * | 2008-08-12 | 2012-11-28 | 4A Technologies Llc | MODULAR SYSTEM AND PROCESS FOR PRODUCING UREA USING BIOMASS-FORMED FEED CHARGE |
| EP2402308A1 (en) | 2010-06-24 | 2012-01-04 | DSM IP Assets B.V. | Urea plant |
| RU2564308C1 (ru) * | 2011-12-15 | 2015-09-27 | Мицубиси Хеви Индастриз, Лтд. | Способ эксплуатации промышленной установки по производству мочевины, содержащей несколько систем |
| NO2617708T3 (zh) * | 2012-01-17 | 2018-01-13 | ||
| US9428449B2 (en) | 2013-01-16 | 2016-08-30 | Alstom Technology Ltd | Method of forming urea by integration of an ammonia production process in a urea production process and a system therefor |
| DE102013113980A1 (de) * | 2013-12-12 | 2015-06-18 | Thyssenkrupp Ag | Verfahren zur Herstellung von Ammoniakgas und CO2 für eine Harnstoffsynthese |
| EP2957544A1 (en) * | 2014-06-18 | 2015-12-23 | Casale SA | Process for production of ammonia and derivatives, in particular urea |
| EP2993158A1 (en) | 2014-09-05 | 2016-03-09 | Casale SA | Process for production of ammonia and derivatives, in particular urea |
| DE102016203277A1 (de) | 2016-02-29 | 2017-08-31 | Thyssenkrupp Ag | Integrierte Synthese von Ammoniak und Harnstoff |
| DE102016122374A1 (de) | 2016-11-21 | 2018-05-24 | Thyssenkrupp Ag | Vollintegrierter Ammoniak-Harnstoff-Komplex |
| IT201700121364A1 (it) * | 2017-10-25 | 2019-04-25 | Saipem Spa | Apparato e metodo per il trattamento di vapori di processo provenienti da una sezione di concentrazione sottovuoto di un impianto urea |
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| US3303215A (en) * | 1962-03-09 | 1967-02-07 | Toyo Koatsu Ind Inc | Synthesis of urea |
| US3349126A (en) * | 1962-09-10 | 1967-10-24 | Pullman Inc | Integrated ammonia and urea process |
| JPS4830258B1 (zh) | 1969-02-08 | 1973-09-18 | ||
| IT1014987B (it) * | 1974-06-12 | 1977-04-30 | Snam Progetti | Procedimento integrato urea am moniaca |
| IT1034674B (it) * | 1975-03-28 | 1979-10-10 | Snam Progetti | Processo flessibile intergrato per la produzione di ammoniaca edurea |
| US4291006A (en) * | 1977-03-03 | 1981-09-22 | Snamprogetti S.P.A | Combined process for the production of urea and ammonia |
| US4235816A (en) | 1979-03-08 | 1980-11-25 | Snamprogetti S.P.A. | Integrated ammonia-urea process |
| US4988491A (en) * | 1989-04-11 | 1991-01-29 | Christiaan Van Dijk | Flexible integration of the production of ammonia and urea |
| US5523483A (en) * | 1995-06-16 | 1996-06-04 | The M. W. Kellogg Company | Integrated urea/ammonia process |
| DE69708627T2 (de) * | 1997-09-20 | 2002-08-08 | Urea Casale S.A., Lugano | Verfahren zur kombinierten Erzeugung von Ammoniak und Harnstoff |
| JP2000159519A (ja) * | 1998-11-25 | 2000-06-13 | Chiyoda Corp | アンモニア・尿素製造プラントおよび製造方法 |
-
2001
- 2001-08-31 EP EP01120959A patent/EP1188710A3/en not_active Withdrawn
- 2001-09-14 JP JP2001279482A patent/JP2002114752A/ja active Pending
- 2001-09-14 US US09/952,678 patent/US6723876B2/en not_active Expired - Lifetime
- 2001-09-14 RU RU2001125149/04A patent/RU2283832C2/ru not_active IP Right Cessation
- 2001-09-14 CN CNB011331089A patent/CN1190414C/zh not_active Expired - Fee Related
- 2001-09-14 CA CA002357256A patent/CA2357256C/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| EP1188710A3 (en) | 2003-10-29 |
| US6723876B2 (en) | 2004-04-20 |
| CN1344711A (zh) | 2002-04-17 |
| CA2357256C (en) | 2007-06-19 |
| CA2357256A1 (en) | 2002-03-15 |
| EP1188710A9 (en) | 2004-08-18 |
| EP1188710A2 (en) | 2002-03-20 |
| RU2283832C2 (ru) | 2006-09-20 |
| JP2002114752A (ja) | 2002-04-16 |
| US20020035293A1 (en) | 2002-03-21 |
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