CN107532847B - 用于从富烃馏分去除氮的方法 - Google Patents

用于从富烃馏分去除氮的方法 Download PDF

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CN107532847B
CN107532847B CN201680019896.5A CN201680019896A CN107532847B CN 107532847 B CN107532847 B CN 107532847B CN 201680019896 A CN201680019896 A CN 201680019896A CN 107532847 B CN107532847 B CN 107532847B
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nitrogen
rich fraction
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hydrocarbon
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H.鲍尔
M.瓦尔特
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Abstract

本发明涉及一种用于获得具有≤1 mol％的氮含量的经液化的富烃馏分（产品馏分）的方法，其中，采用制冷回路使所述富烃馏分液化并过冷并且随后使所述富烃馏分经历氮的精馏去除。根据本发明，经液化和过冷的富烃馏分（2）经膨胀（V1）并被供给到氮汽提塔（T1），产品馏分（4）被从所述氮汽提塔（T1）的底部抽离，富氮馏分（5）被从所述氮汽提塔（T1）的顶部抽离，被压缩（C1）、采用所述制冷回路（K）被液化并过冷（E1‑E3）、经膨胀（V2）并被供给到高压氮塔（T2），已经采用所述制冷回路（K）被冷却的所述富氮馏分的子流作为再沸腾流（9）被供给进入所述高压氮塔（T2），以及氮耗尽馏分（11）被从所述高压氮塔（T2）的底部抽离并被供给到所述汽提塔（T1），其中，所述两个塔（T1、T2）经由热量交换器（E4）热联接，所述热量交换器（E4）充当用于所述氮汽提塔（T1）的再沸腾器并且充当用于所述高压氮塔（T2）的顶部冷凝器，以及在所述两个塔（T1、T2）之间布置有回流收集器（D1），从所述回流收集器（D1），气态和/或液态高纯度氮流被抽离。

Description

用于从富烃馏分去除氮的方法
技术领域
本发明涉及一种获得具有≤1 mol％的氮含量的经液化的富烃馏分（产品馏分）的方法，其中，采用制冷回路使富烃馏分液化并过冷并且随后使富烃馏分经历氮的精馏去除。
背景技术
术语“制冷回路”在下文中应该被理解为意味着如下的任何制冷***和任何制冷回路，借助于所述制冷***和所述制冷回路可以使富烃馏分液化并随后使其过冷。仅仅是示意性的示例包括具有或不具有相变的冷却剂（混合物）回路、膨胀器回路、吸收制冷***等。
含氮天然气需要合适的液化措施以不允许LNG（液化天然气）中的氮浓度增长至超过1 mol％，因为在该情形中有可能在LNG储存槽罐中出现不希望的和危险的具有不同密度的LNG层。排出氮的已知方法是在天然气液化过程的冷端处抽离燃料气流，其与原料气（Rohgas）相比具有明显提升的氮浓度。因此可能的是，LNG实现不多于1 mol％的氮的规格，即使原料气中的氮浓度远超过1 mol％。如果燃气涡轮机将接收该燃料气（Brenngas）的至少一部分，根据燃气涡轮机的设计，应该在此也观测到15至45 mol％的最大容许氮浓度。
然而，如果天然气中的氮含量高到使得不可能同时遵从LNG中的以及燃料气中的最大容许氮含量，则照惯例是抽离包含≥99 mol％的氮的高浓度氮流并将其直接释放至大气。该高浓度氮流可以通过如下方式得以实现：经由在实际天然气液化过程的下游的所谓的NRU（氮排除装置,Nitrogen Rejection Unit）中的燃料气的分离或者借助于集成至天然气液化过程中的N2/CH4分离，如例如从美国专利7,520,143已知的那样。在该N2/CH4分离中，高浓度氮馏分、氮/烃混合物以及LNG产品馏分被从分离过程抽离。氮在此从塔（Kolonne）中的总原料气流分离并且以技术品级纯度来释放。通常高达≥99 mol％的氮的来自于原料气中的氮含量的该显著氮富集需要比较高的分离强度以及因此需要比较高的能量强度，其发生在由于提升的压力而导致的不良气体/液体平衡下。然而在许多情形中，所期望的是，不释放除了LNG和高浓度氮馏分之外的任何另外的馏分。
发明内容
本发明的目的在于详细说明一种通用类型的用于获得具有≤1 mol％的氮含量的经液化的富烃产品馏分的方法，其中，避免了释放氮/烃混合物而同时维持低资金和操作成本，并且除了经液化的富烃产品馏分之外，仅获得具有至少98 mol％的氮含量的，优选地具有≥99 mol％的氮含量的高浓度氮馏分。
为了实现该目的，提出了一种通用类型的用于获得具有≤1 mol％的氮含量的经液化的富烃产品馏分的方法，所述方法的特征在于
a）经液化和过冷的富烃馏分经膨胀并被供给到氮汽提塔（Stickstoff-Strippkolonne），
b）产品馏分被从所述氮汽提塔的底部抽离，
c）富氮馏分被从所述氮汽提塔的顶部抽离，被压缩、采用制冷回路被液化并过冷、经膨胀并被供给到高压氮塔，
d）已经采用所述制冷回路被冷却的所述富氮馏分的子流作为再沸腾流被供给进入所述高压氮塔，以及
e）氮耗尽馏分被从所述高压氮塔的底部抽离并被供给到所述汽提塔，
f）其中，所述两个塔经由热量交换器热联接，所述热量交换器充当用于所述氮汽提塔的再沸腾器（Aufkocher）并且充当用于所述高压氮塔的顶部冷凝器（Kopfkondensator），以及
g）在所述两个塔之间布置有回流收集器（Rücklaufsammler），从所述回流收集器，气态和/或液态高纯度氮流被抽离。
用于获得具有≤1 mol％的氮含量的经液化的富烃产品馏分的本发明的方法使得能够进行待液化的富烃馏分的分馏或者待液化的天然气的分馏以给出符合规定的LNG以及所谓的技术品级纯度的氮。没有获得另外的一种或多种产品流，更特别地，没有获得氮/甲烷混合物。以对于气体/液体平衡而言以及因此对于分离复杂性而言是有利的比较低的压力，氮汽提塔将从氮汽提塔底部抽离的产品馏分中的氮含量降低至≤1 mol％，而没有对在该塔顶部处抽离的富氮馏分的关于其氮含量的纯度提出特别的需求。该富氮馏分仅仅是待液化的富烃馏分的一部分。由于仅是该富氮馏分在高压氮塔中经历最终氮富集至>98mol％，所以与从现有技术已知的方法相比显著降低了设备复杂性和能量强度。
作为从属权利要求的主题的对用于获得经液化的富烃产品馏分的本发明的方法的其他有利配置的特征在于
- 所述待液化的富烃馏分具有至少2 mol％的氮含量，优选地具有至少3 mol％的氮含量，
- 所述经液化和过冷的富烃馏分膨胀至压力在1.1和2.0 bar之间，优选地在1.15和1.5 bar之间，
- 在所述氮汽提塔的顶部处抽离的富氮馏分被压缩至压力在25和50 bar之间，优选地在30和45 bar之间，
- 所述高压氮塔以20和30 bar之间的压力来操作，优选地以22和27 bar之间的压力来操作，
- 所述再沸腾流的量在所述经压缩的富氮馏分的量的10％和70％之间，优选地在20％和50％之间，
- 从所述回流收集器抽离的高纯度氮流具有至少98 mol％的氮含量，优选地具有至少99 mol％的氮含量，
- 在所述氮汽提塔的顶部处抽离的富氮馏分具有在10和60 mol％之间的氮含量，优选地具有在30和50 mol％之间的氮含量，
- 如果在所述方法中的至少一个位置处需要燃料气，则所使用的燃料气是所述待液化的富烃馏分的子流和/或所述待冷却的经压缩的富氮馏分的子流。
附图说明
由图1中所示的工作示例详细说明用于获得经液化的富烃产品馏分的本发明的方法以及其另外的有利配置。
具体实施方式
在具有制冷回路的热量交换器或热量交换区域E1、E2和E3中使待液化的富烃馏分1液化并使其过冷。为了清楚起见，仅以示意形式示出制冷回路K。其构造对于实施本发明的方法并不重要。其仅必须被设计成使得其可以提供足够的制冷输出以便对富烃馏分进行液化和过冷并且以便对氮汽提塔T1的顶部处抽离的富氮馏分5进行液化和过冷，这将在下文中详细讨论。在图1中所示的实施例中，对富烃馏分1以及前述富氮馏分5进行液化和过冷在三个热量交换器或热量交换区域E1-E3中实现，其中，热量交换器E1用于冷却，热量交换器E2用于液化，并且热量交换器E3用于前述馏分的过冷。除了所示的三个热量交换器E1-E3之外，热量交换器的任意组合是能够实施的，这意味着也有可能使用例如所谓的螺旋盘卷式热量交换器。
过冷的富烃馏分2具有在-150和-160 ℃之间的温度。其在阀V1中膨胀至压力在1.1和2.0 bar之间，优选地在1.15和1.5 bar之间，并且在氮汽提塔T1的顶部区域中作为回流3而施加至氮汽提塔T1。借助于热量交换器或再沸腾器E4，在氮汽提塔T1的底部中建立了≤1 mol％的氮含量，热量交换器或再沸腾器E4的加热将在下文中说明。因此可能的是，从氮汽提塔T1的底部抽离具有≤1 mol％的氮含量的产品馏分4。该产品馏分4随后被发送至其进一步的用途，例如中间存储在LNG存储容器中。
在氮汽提塔T1的顶部处，抽离富氮馏分5，其与经液化的富烃馏分3相比具有更高的氮含量。其氮含量在10和60 mol％之间，优选地在30和50 mol％之间。其在压缩机C1中被压缩至压力在25和50 bar之间，优选地在30和45 bar之间。在下游的热量交换器E5中，压缩的热量被去除并且经压缩的富氮馏分6被冷却至环境温度。随后，类似于富烃馏分1，富氮馏分6在热量交换器E1-E3中被冷却至温度在-150和-160 ℃之间；这导致对富氮馏分的完全冷凝以及随后的过冷。
经液化的富氮馏分7在阀V2中膨胀并且经由管道8被供给到高压氮塔T2。这以20-30bar的压力操作，优选地以22-27 bar的压力来操作。在高压氮塔T2中使用的顶部冷凝器是上述热量交换器E4，在热量交换器E4中，来自高压氮塔T2的冷凝氮涵盖了在氮汽提塔T1底部中再沸腾的富烃流或LNG的热量需求。存在布置于两个塔T1/T2之间的回流收集器D1，从回流收集器D1，气态和/或液态高纯度氮流10被抽离。这是所谓的技术品级纯度的氮，其具有至少98 mol%的氮含量，优选地具有至少99 mol％的氮含量。
以合适的温度经由阀V3作为再沸腾流为高压氮塔T2供应富氮馏分5/6的子流，该子流已经采用制冷回路K得到冷却。再沸腾流9的量优选地在经压缩的富氮馏分6的量的10％和70％之间，特别是在20％和50％之间。再沸腾流9可以在热量交换器E1和E2之间被抽离，但是也可以在热量交换器E2和E3之间被抽离。
从高压氮塔T2的底部抽离氮耗尽馏分11，其与富氮馏分5相比具有较低的氮含量。氮耗尽馏分11在阀V4中膨胀并在经液化的富烃馏分3的供给点下方被供给到氮汽提塔T1。
如果在方法中的至少一个位置处需要燃料气，则所使用的燃料气可以是待液化的富烃馏分1的子流和/或待冷却的经压缩的富氮馏分6的子流。

Claims (17)

1.一种获得具有≤1 mol％的氮含量的经液化的富烃产品馏分的方法，其中，采用制冷回路使富烃馏分液化并过冷并且随后使所述富烃馏分经历氮的精馏去除，
其特征在于
a）经液化和过冷的富烃馏分（2）经膨胀（V1）并被供给到氮汽提塔（T1），
b）所述富烃产品馏分（4）被从所述氮汽提塔（T1）的底部抽离，
c）富氮馏分（5）被从所述氮汽提塔（T1）的顶部抽离，被压缩（C1）、采用所述制冷回路（K）被液化并过冷（E1-E3）、经膨胀（V2）并被供给到高压氮塔（T2），
d）已经采用所述制冷回路（K）被冷却的所述富氮馏分的子流作为再沸腾流（9）被供给进入所述高压氮塔（T2），以及
e）氮耗尽馏分（11）被从所述高压氮塔（T2）的底部抽离并被供给到所述汽提塔（T1），
f）其中，所述两个塔（T1、T2）经由热量交换器（E4）热联接，所述热量交换器（E4）充当用于所述氮汽提塔（T1）的再沸腾器并且充当用于所述高压氮塔（T2）的顶部冷凝器，以及
g）在所述两个塔（T1、T2）之间布置有回流收集器（D1），从所述回流收集器（D1），气态和/或液态高纯度氮流被抽离。
2.根据权利要求1所述的方法，其特征在于，待液化的所述富烃馏分（1）具有至少2mol％的氮含量。
3.根据权利要求2所述的方法，其特征在于，待液化的所述富烃馏分（1）具有至少3mol％的氮含量。
4.根据权利要求1-3中任一项所述的方法，其特征在于，所述经液化和过冷的富烃馏分（2）膨胀（V1）至压力在1.1和2.0 bar之间。
5.根据权利要求1或2所述的方法，其特征在于，所述经液化和过冷的富烃馏分（2）膨胀（V1）至压力在1.15和1.5 bar之间。
6.根据权利要求1-3中的任一项所述的方法，其特征在于，在所述氮汽提塔（T1）的顶部处抽离的富氮馏分被压缩（C1）至压力在25和50 bar之间。
7.根据权利要求6所述的方法，其特征在于，在所述氮汽提塔（T1）的顶部处抽离的富氮馏分被压缩（C1）至压力在30和45 bar之间。
8.根据权利要求1-3中的任一项所述的方法，其特征在于，所述高压氮塔（T2）以20和30bar之间的压力来操作。
9.根据权利要求8所述的方法，其特征在于，所述高压氮塔（T2）以22和27 bar之间的压力来操作。
10.根据权利要求1-3中的任一项所述的方法，其特征在于，所述再沸腾流（9）的量在经压缩的所述富氮馏分（5、6）的量的10％和70％之间。
11.根据权利要求10所述的方法，其特征在于，所述再沸腾流（9）的量在经压缩的所述富氮馏分（5、6）的量的20％和50％之间。
12.根据权利要求1-3中的任一项所述的方法，其特征在于，从所述回流收集器（D1）抽离的高纯度氮流具有至少98 mol％的氮含量。
13.根据权利要求12所述的方法，其特征在于，从所述回流收集器（D1）抽离的高纯度氮流具有至少99 mol％的氮含量。
14.根据权利要求1-3中的任一项所述的方法，其特征在于，在所述氮汽提塔（T1）的顶部处抽离的富氮馏分具有在10和60 mol％之间的氮含量。
15.根据权利要求14所述的方法，其特征在于，在所述氮汽提塔（T1）的顶部处抽离的富氮馏分具有在30和50 mol％之间的氮含量。
16.根据权利要求1-3中的任一项所述的方法，其中，在所述方法中的至少一个位置处需要燃料气，其特征在于，所使用的燃料气是待液化的所述富烃馏分（1）的子流和/或待液化的所述经压缩的富氮馏分（6）的子流。
17.根据权利要求16所述的方法，其中，所述燃料气为用于压缩机驱动的燃料。
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