CN113544118A - 生产脲甲醛浓缩物的方法 - Google Patents
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- 238000000034 method Methods 0.000 title claims description 15
- 229920001807 Urea-formaldehyde Polymers 0.000 title claims description 10
- 239000012141 concentrate Substances 0.000 title claims description 10
- ODGAOXROABLFNM-UHFFFAOYSA-N polynoxylin Chemical compound O=C.NC(N)=O ODGAOXROABLFNM-UHFFFAOYSA-N 0.000 title claims description 10
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 103
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 57
- 230000015572 biosynthetic process Effects 0.000 claims abstract description 45
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 37
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004202 carbamide Substances 0.000 claims abstract description 17
- 238000002453 autothermal reforming Methods 0.000 claims abstract description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 50
- 238000003786 synthesis reaction Methods 0.000 claims description 43
- 239000007789 gas Substances 0.000 claims description 42
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 36
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 25
- 239000001569 carbon dioxide Substances 0.000 claims description 25
- 229910052757 nitrogen Inorganic materials 0.000 claims description 18
- 239000001257 hydrogen Substances 0.000 claims description 15
- 229910052739 hydrogen Inorganic materials 0.000 claims description 15
- 229930195733 hydrocarbon Natural products 0.000 claims description 12
- 150000002430 hydrocarbons Chemical class 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- 239000004215 Carbon black (E152) Substances 0.000 claims description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 8
- 238000004821 distillation Methods 0.000 claims description 5
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000000446 fuel Substances 0.000 claims description 4
- 150000002431 hydrogen Chemical class 0.000 claims description 4
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 238000004064 recycling Methods 0.000 claims description 2
- 238000000629 steam reforming Methods 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 6
- 238000007254 oxidation reaction Methods 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 12
- 238000002407 reforming Methods 0.000 description 4
- 239000006096 absorbing agent Substances 0.000 description 3
- 238000009835 boiling Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 239000003345 natural gas Substances 0.000 description 3
- 239000002826 coolant Substances 0.000 description 2
- 239000003949 liquefied natural gas Substances 0.000 description 2
- 238000005201 scrubbing Methods 0.000 description 2
- 238000009825 accumulation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910002090 carbon oxide Inorganic materials 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012776 robust process Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000010977 unit operation Methods 0.000 description 1
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Abstract
凭借自热重整、中间甲醇和氨形成、以及氨至脲产物的转化和甲醇至甲醛的催化氧化，由含烃原料生产甲醇和脲产物的平行联产方法。
Description
本发明涉及由烃进料原料生产脲甲醛浓缩物的方法。
更尤其，本发明涉及凭借自热重整、中间甲醇和氨形成、以及氨至脲产物的转化和甲醇至甲醛的催化氧化，由含烃原料生产甲醇和脲产物的平行联产方法。
通过氨和二氧化碳的转化来生产脲是众所周知的方法，并且在工业中常规采用。
本发明的总体目的是提供在需要最少的设备和单元操作的单元中生产脲甲醛浓缩物的成本有效、简单和稳健的方法。
因此，本发明提供了由烃原料生产脲甲醛浓缩物的方法，其包括以下步骤：
(a)通过将烃原料部分燃烧并在自热重整阶段中蒸汽重整来生产含有氢气、一氧化碳和二氧化碳的合成气；
(b) 将来自步骤的合成气分成第一合成气和第二合成气；
(c) 使来自步骤(b)的第二合成气按序经受高温水煤气变换转化和中温水煤气变换转化；
(d)从来自步骤(c)的第二合成气中去除至少一部分的二氧化碳，以获得贫二氧化碳的第二合成气；
(e)按用以获得2.8-3.2的氢气与氮气的摩尔比的量将氮气加入到贫二氧化碳的第二合成中，并去除惰性物质和一氧化碳；
(f)在不含惰性物质的氨合成阶段中催化转化来自步骤(e)的纯化的第二合成气中的氮气和氢气，并取出含有氨的流出物；和
(g)将至少一部分的含有氨的流出物通入脲合成阶段，并通过与在步骤(d)中从合成气中去除的至少一部分的二氧化碳反应将流出物中的氨转化为脲产物，
(h) 在单程甲醇合成阶段中催化转化来自步骤(c)的第一合成气中的一氧化碳、二氧化碳和氢气，并取出含有粗甲醇的流出物和含有未经转化的第一合成气的流出物；
(i)将含有未经转化的第一合成气的流出物再循环至步骤(c)中的中温变换转化且/或作为燃料再循环至火焰加热器且/或再循环至步骤(e)；
(j) 使含有粗甲醇的流出物经受蒸馏，并从该蒸馏中提取纯化的甲醇；
(k) 将至少一部分的来自步骤(j)的纯化的甲醇氧化成甲醛；
(l)将来自步骤(k)的甲醛吸收在水和制备自步骤(g)中的脲产物的水性脲溶液中，以获得脲甲醛浓缩物。
如本文中进一步使用的，术语“自热重整”表示使用氧气作为氧化剂，在自热重整器（ATR)中进行的重整。
用于在本发明中使用的合适的烃原料包括甲烷、天然气、LPG、石脑油和高级烃。
优选地，烃原料包含甲烷，例如呈天然气、液化天然气(LNG)或代用天然气(SNG)的形式。
当采用石脑油和含有高级烃的原料时，优选在自热重整阶段之前使这些原料经受预重整步骤。
然而，预重整可以用于所有类型的烃原料。
使用ATR代替初级重整和空气氧化（air blown）二级重整的优点在于相当大地减少了下游设备中的气流。因此，来自ATR的合成气包含一氧化碳、二氧化碳、甲烷、氢气，且不含氮气。在根据本发明的方法中，将用于氨合成的所需量的氮气以对应于化学计算所需量的量加入到变换反应和二氧化碳去除阶段下游的第二合成气中。实际上，最佳氨合成所需的氮气的量对应于介于 2.8 和 3.2 之间的氢气与氮气的摩尔比。
优选地，在氮气洗涤单元(NWU)中凭借氮气洗涤将氮气加入到第二合成气中。
作为进一步的优点，氮气洗涤从氨合成气中去除惰性物质、残留量的烃、二氧化碳和一氧化碳。可利用这些化合物作为火焰处理加热器或蒸汽过热器中的燃料。
火焰加热器是烃原料的预热系统的一部分。
应理解，如本文中所使用的术语“惰性物质”是指在氨合成中不经历化学反应的化合物。
通过以下方式来获得对用以满足用于氨合成的所需量的氢气连同将氨转化成脲所必需的所需量的二氧化碳的一氧化碳/二氧化碳比率的最终控制：在步骤(d)中去除二氧化碳之前使第二合成气经受高温水煤气变换反应和中温水煤气变换反应。
可以通过如本领域已知的物理或化学洗涤中的任何常规方法来实施从第二合成气中去除二氧化碳。
优选地，通过可获得自BASF的OASE方法来实施去除二氧化碳，该方法允许容易地回收所吸收的二氧化碳，用于在脲合成中使用。
优选通过使合成气在适中的压力（例如30-60巴）和温度150-300℃下通过至少一个容纳至少一个但优选两个甲醇催化剂固定床的单程甲醇反应器来进行甲醇合成阶段。特别优选的甲醇反应器是通过合适的冷却剂（例如沸水）冷却的固定床反应器，例如沸水反应器(BWR)。
在步骤(h)中，富含甲醇的流出物优选是液体粗甲醇流出物。通过冷却和冷凝来自甲醇反应器的流出气体来获得该流出物。
因此，本发明的方法可以进一步包括冷却从每个甲醇反应器中取出的合成气以冷凝甲醇，并使该气体通过分离器，从分离器中取出含有粗甲醇的塔底馏分，取出含有未经转化的合成气的流出气体，将其通入火焰加热器作为燃料且/或通入中温变换转化，用于提高经变换的第二合成气中的氢气浓度。
优选地，向NWU中加入流出气体，在NWU中利用塔顶馏分中所含的氢气，同时洗掉碳氧化物和惰性化合物。
可以借助于喷射器将流出气体通入NWU，在喷射器中贫二氧化碳的气体的主流充当原动流（motive flow），并且流出物（充当）吸入流。
或者，可经由喷射器或增压压缩机/鼓风机将流出物循环至中温变换反应，所述喷射器或增压压缩机/鼓风机增加流出物压力，以适合主工艺气体流。
应理解，如本文中所使用的术语“甲醇反应器”包括绝热固定床反应器和冷却反应器，例如沸水反应器和冷凝-甲醇型反应器，其在共同的壳内包括甲醇催化剂颗粒的固定床和适于用冷却剂间接冷却甲醇合成气的冷却装置。
在步骤(f)中，使来自正确比例的氢气和氮气(H2:N2摩尔比为2.8-3.2)的第二合成气通过压缩机，以获得所需的氨合成压力，例如120-250巴，优选约190巴。然后在包含至少一个氨转化器的氨合成回路中生产氨。可以通过冷凝和随后的分离从含有氨的流出物中以液氨形式回收氨。
为了改进该方法的效率，将来自步骤(f)的含有氢气、氮气和氨的废气流送至步骤(f)中的合成气压缩机。
然后通过与如上所描述的回收自步骤(d)的二氧化碳反应，将从氨合成中取出的氨转化成脲产物。
为了生产在制备脲甲醛浓缩物中采用的甲醛，将至少一部分的从步骤(j)中的蒸馏中提取的纯化的甲醇送至步骤(l)中的甲醛单元，在该甲醛单元中将甲醇预热并猝灭入预热的空气中或者蒸发并与预热的空气混合，然后将其在氧化催化剂上氧化成甲醛。
随后将在甲醇氧化步骤(j)中生产的甲醛通入甲醛吸收器中。在甲醛吸收器中，将来自氧化步骤的气态甲醛流出物吸收在水和水性脲悬浮液中，以形成脲甲醛浓缩物。
将离开吸收器顶部的大部分流出气体送回到(k)中的预热空气中，同时将其余的流出气体预热并在焚烧炉反应器中催化焚烧，然后将其吹扫，以避免惰性物质的积聚。
Claims (5)
1.由烃原料生产脲甲醛浓缩物的方法，其包括以下步骤：
(a)通过将所述烃原料部分燃烧并在自热重整阶段中蒸汽重整来生产含有氢气、一氧化碳和二氧化碳的合成气；
(b) 将来自步骤的合成气分成第一合成气和第二合成气；
(c)使来自步骤(b)的第二合成气按序经受高温水煤气变换转化和中温水煤气变换转化；
(d)从来自步骤(c)的第二合成气中去除至少一部分的二氧化碳，以获得贫二氧化碳的第二合成气；
(e)按用以获得2.8-3.2的氢气与氮气的摩尔比的量将氮气加入到贫二氧化碳的第二合成中；
(f)在不含惰性物质的氨合成阶段中催化转化来自步骤(e)的纯化的第二合成气中的氮气和氢气，并取出含有氨的流出物； 和
(g)将至少一部分的所述含有氨的流出物通入脲合成阶段，并通过与在步骤(d)中从合成气中去除的至少一部分的二氧化碳反应将所述流出物中的氨转化为脲产物，
(h) 在单程甲醇合成阶段中催化转化来自步骤(c)的第一合成气中的一氧化碳、二氧化碳和氢气，并取出含有粗甲醇的流出物和含有未经转化的第一合成气的流出物；
(i) 将所述含有未经转化的第一合成气的流出物再循环至步骤(c)中的中温变换转化且/或作为燃料再循环至火焰加热器且/或再循环至步骤(e)；
(j) 使所述含有粗甲醇的流出物经受蒸馏，并从所述蒸馏中提取纯化的甲醇；
(k)将至少一部分的来自步骤(j)的纯化的甲醇氧化成甲醛；
(l)将来自步骤(k)的甲醛吸收在水和制备自步骤(g)中的脲产物的水性脲溶液中，以获得脲甲醛浓缩物。
2.根据权利要求1所述的方法，其中凭借氮气洗涤将氮气加入到步骤(f)中的贫二氧化碳的第二合成气中。
3.权利要求1或2所述的方法，其中凭借喷射器将所述含有未经转化的第一合成气的流出物再循环。
4.根据权利要求1-3中任一项所述的方法，其中在至少一个容纳一个或两个固定床甲醇催化剂的甲醇反应器中实施步骤(i)中的甲醇合成阶段。
5.根据权利要求1-4中任一项所述的方法，其中步骤(a)中的合成气中的蒸汽碳比率介于0.4 和1.0之间。
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| US20070299144A1 (en) * | 2004-03-22 | 2007-12-27 | William Davey | Coproduction Of Methanol And Ammonia From Natural Gas |
| CN104024149A (zh) * | 2012-01-04 | 2014-09-03 | 赫多特普索化工设备公司 | 甲醇和脲的联合生产 |
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| WO2018078318A1 (en) * | 2016-10-26 | 2018-05-03 | Johnson Matthey Public Limited Company | Process for the production of formaldehyde-stabilised urea |
| CN108368037A (zh) * | 2015-12-18 | 2018-08-03 | 庄信万丰股份有限公司 | 生产甲醛稳定的脲的整合方法 |
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| US20070299144A1 (en) * | 2004-03-22 | 2007-12-27 | William Davey | Coproduction Of Methanol And Ammonia From Natural Gas |
| CN104024149A (zh) * | 2012-01-04 | 2014-09-03 | 赫多特普索化工设备公司 | 甲醇和脲的联合生产 |
| CN107250106A (zh) * | 2015-02-20 | 2017-10-13 | 庄信万丰股份有限公司 | 用于生产甲醛稳定化的尿素的整合方法 |
| CN108368037A (zh) * | 2015-12-18 | 2018-08-03 | 庄信万丰股份有限公司 | 生产甲醛稳定的脲的整合方法 |
| WO2018078318A1 (en) * | 2016-10-26 | 2018-05-03 | Johnson Matthey Public Limited Company | Process for the production of formaldehyde-stabilised urea |
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