CN115069057B - 一种低温精馏提纯回收二氧化碳的方法 - Google Patents

一种低温精馏提纯回收二氧化碳的方法 Download PDF

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CN115069057B
CN115069057B CN202210689090.4A CN202210689090A CN115069057B CN 115069057 B CN115069057 B CN 115069057B CN 202210689090 A CN202210689090 A CN 202210689090A CN 115069057 B CN115069057 B CN 115069057B
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carbon dioxide
outlet
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subcooler
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CN115069057A (zh
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缪樟臻
丁传琪
柳春来
张行东
王淑勇
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China National Air Separation Engineering Co ltd
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Abstract

本发明提供一种低温精馏提纯回收二氧化碳的方法，直接利用原料气作为制冷剂，通过采用二氧化碳自身高压节流提供冷量，不需其他装置提供冷量，能耗低，工艺流程简单可靠。原料气进入压缩机压缩后进入冷却器；原料气送入主换热器后再进入再沸器中；原料气在过冷器中被返流气体进一步冷却，再经一号节流阀降压降温后，送入一号气液分离器；一号气液分离器冷凝的液体二氧化碳送入精馏塔作为回流液参与精馏，一号气液分离器出来的气体经过冷器和主换热器复热后作为吸附器的再生气体；从精馏塔得到的粗制气体经过冷器冷却后进入二号气液分离器；精馏塔获得的二氧化碳液体经二号节流阀降压后，经过冷器和主换热器复热后送入二氧化碳产品管网。

Description

一种低温精馏提纯回收二氧化碳的方法
技术领域
本发明涉及一种低温精馏提纯回收二氧化碳的方法，适用于化工装置排放废气的二氧化碳回收再利用。
背景技术
天然气、焦炭及重油等燃料及其燃烧，合成氨、乙二醇的生产、石油化工行业生产过程中需要排放大量二氧化碳。二氧化碳的大量排放，对环境造成影响，导致温室效应的形成，导致全球气温上升。石化重点行业的绿色低碳转型，在碳中和背景下，直接排放到大气中的含大量二氧化碳的废气具有收集回收再利用的价值。
二氧化碳捕集是电力、钢铁、水泥、化工等行业实行碳捕集、封存与利用（CarbonCapture Utilization and Storage, CCUS的首要环节，对节能减排及温室效应的控制具有关键作用。二氧化碳的捕集方式主要有三种：燃烧前捕集（Pre-combustion）、富氧燃烧（Oxy-fuel combustion）和燃烧后捕集（Post-combustion）。目前行业内燃烧后捕集技术主要采用化学吸收法、物理吸收法及膜分离法。其中化学吸收法是当前最普遍的从燃烧之后的烟气中分离二氧化碳技术，化学吸收法以醇胺、复合胺等为吸附剂，利用吸附剂在不同压力温度下对二氧化碳的吸收能力，实现对二氧化碳的回收利用。
低温精馏法是利用原料气各组分沸点的差异，通过精馏塔实现原料气的分离，该流程具有能耗低、运行成本低、分离效率高，而且适用于大规模的工业化生产。目前，如果采用该技术提纯二氧化碳，需要利用冷水机组、氨制冷系统等装置提供额外冷量，增加了能耗，且工艺流程比较复杂。
发明内容
本发明的目的在于克服现有技术中存在的上述不足，而提供一种结构设计合理的低温精馏提纯回收二氧化碳的方法，直接利用原料气作为制冷剂，通过采用二氧化碳自身高压节流提供冷量，不需其他装置提供冷量，能耗低，工艺流程简单可靠。
本发明解决上述问题所采用的技术方案是：一种低温精馏提纯回收二氧化碳的方法，其特征在于：该方法采用一装置进行，该装置包括压缩单元、脱硫单元、干燥单元和低温精馏单元；压缩单元包括压缩机和冷却器；干燥单元包括吸附器和电加热器；低温精馏单元包括主换热器、过冷器、再沸器、精馏塔、一号节流阀、二号节流阀、一号气液分离器、二号气液分离器和降压降温装置；主换热器具有第一冷流道、第二冷流道、第三冷流道和热流道；过冷器具有第一冷流道、第二冷流道、第三冷流道、第一热流道和第二热流道； 压缩机的进口用于进原料气，出口与冷却器的进口连接，冷却器的出口与脱硫单元连接； 脱硫单元与吸附器的进口连接，吸附器的出口与主换热器的热流道进口连接；再沸器与精馏塔连接；主换热器的热流道出口与再沸器的进口连接，再沸器的出口与过冷器的第二热流道进口连接，过冷器的第二热流道出口通过一号节流阀与一号气液分离器的进口连接；一号气液分离器的液体出口与精馏塔的回流液进口连接，一号气液分离器的气体出口与过冷器的第二冷流道进口连接，过冷器的第二冷流道出口与主换热器的第二冷流道进口连接，主换热器的第二冷流道出口与电加热器的进口连接，电加热器的出口与吸附器的再生气进口连接；精馏塔顶部的气体出口与过冷器的第一热流道进口连接，过冷器的第一热流道出口与二号气液分离器的进口连接；二号气液分离器的液体出口与精馏塔的回流液进口连接；二号气液分离器的气体出口通过降压降温装置与过冷器的第三冷流道进口连接，过冷器的第三冷流道出口与主换热器的第三冷流道进口连接； 精馏塔的液体出口通过二号节流阀与过冷器的第一冷流道进口连接，过冷器的第一冷流道出口与主换热器的第一冷流道进口连接，主换热器的第一冷流道出口连接二氧化碳产品管网；
该方法包括如下步骤：
1）、原料气进入压缩机压缩，增压至1.5～2.5Mpa，然后进入冷却器被冷却至常温，再送入脱硫床脱离硫组分杂质后，送入干燥单元；
2）、原料气在吸附器中进行干燥；
3）、经干燥单元脱水后的原料气送入主换热器，被返流气体冷却至-9℃～-11℃后进入再沸器中，在再沸器中作为精馏塔的热源被精馏塔底部的液体二氧化碳冷却至-27℃～-29℃；原料气在过冷器中被返流气体进一步冷却至-55℃～-60℃，再经一号节流阀降压降温后，送入一号气液分离器，在一号气液分离器中进行气液两相分离；
4）、一号气液分离器冷凝的液体二氧化碳送入精馏塔作为回流液参与精馏，在精馏塔底部得到提纯精制的液体二氧化碳，一号气液分离器出来的气体经过冷器和主换热器复热后作为吸附器的再生气体，再生气体在电加热器中升温至170℃～190℃后，进入吸附器；
5）、从精馏塔顶部得到的粗制气体，经过冷器冷却后，进入二号气液分离器中进行气液两相分离，二号气液分离器的液体进入精馏塔参与精馏；二号气液分离器分离出来的气体经降压降温后作为冷流体，在过冷器和主换热器中回收冷量；
6）、从精馏塔底部获得的二氧化碳液体，经二号节流阀降压至0.3MPa.A～0.4MPa.A，经过冷器和主换热器复热后送入二氧化碳产品管网。
本发明所述的脱硫单元为脱硫床。
本发明所述的主换热器和过冷器均为板翅式换热器。
本发明所述的冷却器为水冷却器。
本发明所述的吸附器为两个，并联设置。
本发明所述的主换热器的第三冷流道出口连接放空。
本发明所述的降压降温装置包括三号节流阀和膨胀机，三号节流阀和膨胀机并联。
本发明所述的一号气液分离器和二号气液分离器均位于精馏塔的上方。
本发明步骤2）中，原料气在吸附器中干燥后，含水量<1ppm。
本发明所述的再沸器与精馏塔为一体，再沸器集成设置在精馏塔的底部。
本发明与现有技术相比，具有以下优点和效果：
1、本发明的低温所需冷量来自二氧化碳压缩后节流，无需额外的制冷剂或制冷装置提供精馏所需冷量，减少了制冷循环中冷剂储罐的配置，减少了额外的制冷循环装置，整套装置仅有1台压缩机，使整个流程更简单，操作可靠。
2、本发明采用精馏塔进行二氧化碳提纯，与化学吸附法相比，具有更高的二氧化碳回收率，可回收原料气中的93%二氧化碳，单位能耗低。
3、本发明采用两级气液分离器，可进一步提高二氧化碳回收率。
4、本发明利用分离原料气的废气作为干燥单元的再生气体，不需额外提供氮气等再生气体。
5、本发明采用的精馏塔可采用板式塔或填料塔，精馏分离效果好，操作弹性大，可根据原料气情况，进行变工况操作。
6、本发明采用的再沸器可与精馏塔合成布置，冷箱内低温精馏设备较少，冷箱布置紧凑，有利于设计成撬块，可明显节省设备投资和节约占地。
7、本发明装置选用节流阀，降低投资和方便操作。
因此，本发明具有流程简单、占地面积小、投资省，并且装置能耗低，适合范围广，易于适用等优点，尤其适用于化工装置排放废气的二氧化碳浓度在60%～90%之间的二氧化碳回收再利用。
附图说明
图1为本发明实施例采用的装置的结构示意图。
具体实施方式
下面结合附图并通过实施例对本发明作进一步的详细说明，以下实施例是对本发明的解释而本发明并不局限于以下实施例。
本发明实施例采用的装置包括压缩单元、脱硫单元、干燥单元和低温精馏单元四个单元。
压缩单元包括压缩机1和冷却器2。脱硫单元为装填有脱硫剂的脱硫床3。干燥单元包括吸附器4和电加热器5。低温精馏单元设置在冷箱16内，其包括主换热器6、过冷器7、精馏塔8、再沸器9、一号节流阀10、一号气液分离器11、二号气液分离器12、降压降温装置和二号节流阀15。
主换热器6具有第一冷流道、第二冷流道、第三冷流道和热流道。过冷器7具有第一冷流道、第二冷流道、第三冷流道、第一热流道和第二热流道。主换热器6和过冷器7均为真空钎焊板翅式换热器。
压缩机1的进口用于进原料气101，出口与冷却器2的进口连接。冷却器2的出口与脱硫床3的进口连接。冷却器2为水冷却器。
脱硫床3的出口与吸附器4的进口连接，吸附器4的出口与主换热器6的热流道进口连接。吸附器4为两个，并联设置，两个吸附器4是成对交替使用的，一只工作时，另一只被再生。吸附器4可根据原料气工作压力、流量选择立式轴向流、卧式或立式径向流床层。吸附器4的再生一般分四步进行，第一步：降压；第二步：加热；第三步：吹冷；第四步：升压，再生四步骤结束后，该只吸附器就可投入工作，进行约3分钟的并联运行后，再完成切换过程。
精馏塔可以是板式精馏塔或填料精馏塔，再沸器为真空钎焊式板翅式换热器。再沸器9可选择与精馏塔8为一体，再沸器9集成设置在精馏塔8的底部；再沸器也可选择为管壳式换热器，单独设置在精馏塔8外，通过管道与精馏塔8连接。主换热器6的热流道出口与再沸器9的进口连接，再沸器9的出口与过冷器7的第二热流道进口连接，过冷器7的第二热流道出口通过一号节流阀10与一号气液分离器11的进口连接。
一号气液分离器11底部的液体出口与精馏塔8顶部的回流液进口连接，一号气液分离器11顶部的气体出口与过冷器7的第二冷流道进口连接，过冷器7的第二冷流道出口与主换热器6的第二冷流道进口连接，主换热器6的第二冷流道出口与电加热器5的进口连接，电加热器5的出口与吸附器4的再生气进口连接。电加热器5选用二台，一用一备，增加流程的可靠性。
精馏塔8顶部的气体出口与过冷器7的第一热流道进口连接，过冷器7的第一热流道出口与二号气液分离器12的进口连接。
二号气液分离器12的底部的液体出口与精馏塔8顶部的回流液进口连接。二号气液分离器12的顶部的气体出口通过降压降温装置与过冷器7的第三冷流道进口连接，过冷器7的第三冷流道出口与主换热器6的第三冷流道进口连接。主换热器6的第三冷流道出口连接放空。降压降温装置包括三号节流阀13和膨胀机14，三号节流阀13和膨胀机14并联。
精馏塔8底部的液体出口通过二号节流阀15与过冷器7的第一冷流道进口连接，过冷器7的第一冷流道出口与主换热器6的第一冷流道进口连接，主换热器6的第一冷流道出口连接二氧化碳产品管网。
一号气液分离器11和二号气液分离器12均位于精馏塔8的上方，二级气液分离器利用其与精馏塔顶部入口之间的液柱高度来实现分离液体重新进入精馏塔进行精馏分离。
一种低温精馏提纯回收二氧化碳的方法及方法，包括如下步骤：
1）、原料气的温度为14℃，压力为0.11MPa.A，流量为76000Nm3/h，原料气21中各组分的浓度分别为：86.68%二氧化碳、10.96%N2、1.43%H2O、0.48%CH4、0.18%C2H4、0.24%C2H6、0.03%C3H8、0.02% CO、2ppm COS、120ppm CH3OH。原料气进入压缩机1压缩，增压至1.5～2.5Mpa，然后进入冷却器2被循环水冷却至常温，再送入脱硫床3脱离硫组分杂质后，送入干燥单元。
2）、为防止原料气中硫组分腐蚀设备和管道，需要在原料气进入冷箱前利用吸附法进行预处理，脱除组分中的硫；为防止原料气中水分子在低温下结冰堵塞换热器和管道，需要在原料气进入冷箱前利用吸附法进行预处理，脱除组分中的水。原料气自下而上通过吸附器4时，原料气中所含的H2O、C2H2等杂质相继被吸附剂清除，净化后的原料气含水量<1ppm。
3）、经干燥单元脱水后的原料气送入主换热器6，被返流气体冷却至-10℃后进入精馏塔8的再沸器9中，在再沸器9中作为精馏塔8的热源被精馏塔底部的液体二氧化碳冷却至-28℃；原料气在过冷器7中被返流气体进一步冷却至-55℃～-60℃，再经一号节流阀10降压降温后，送入一号气液分离器11，在一号气液分离器11中进行气液两相分离。
4）、一号气液分离器11底部冷凝的液体二氧化碳送入精馏塔8顶部作为回流液参与精馏，进行精馏提纯，在精馏塔8底部得到提纯精制的液体二氧化碳，一号气液分离器11顶部出来的气体经过冷器7和主换热器6复热后作为吸附器4的再生气体，再生气体在加热阶段经过电加热器5升温至180℃后，进入吸附器4，在冷吹阶段则直接进入吸附器4，从吸附器4出来后高处放空。
5）、从精馏塔8顶部得到的粗制气体，经过冷器7冷却后，进入二号气液分离器12中进行气液两相分离，二号气液分离器12底部液体从精馏塔8顶部进入参与精馏。二号气液分离器12顶部分离出来的气体经三号节流阀13或膨胀机14降压降温后作为冷流体，在过冷器7和主换热器8中回收冷量后放空。
6）、从精馏塔8底部获得的99.91%纯度的二氧化碳液体，经二号节流阀15降压至0.35MPa.A，经过冷器7和主换热器6复热后送入二氧化碳产品管网。
本实施例中，采用本发明，通过低温精馏、最终二氧化碳产品的纯度为99.91%、流量为61600Nm3/h，压力为0.35MPa.A的二氧化碳气态产品，整体装置二氧化碳回收率达93%。所需冷量来自原料气本身的压缩节流制冷。整套装置的主要耗电设备为二氧化碳压缩机和电加热器，装置耗电量为10958Kw，制取二氧化碳气态产品的单位能耗0.09 Kw/kg。
以上只通过说明的方式描述了本发明的某些示范性实施例，毋庸置疑，对于本领域的普通技术人员，在不偏离本发明的精神和范围的情况下，可以用各种不同的方式对所描述的实施例进行修正。因此，上述附图和描述在本质上是说明性的，不应理解为对本发明权利要求保护范围的限制。

Claims (10)

1. 一种低温精馏提纯回收二氧化碳的方法，其特征在于：该方法采用一装置进行，该装置包括压缩单元、脱硫单元、干燥单元和低温精馏单元；压缩单元包括压缩机和冷却器；干燥单元包括吸附器和电加热器；低温精馏单元包括主换热器、过冷器、再沸器、精馏塔、一号节流阀、二号节流阀、一号气液分离器、二号气液分离器和降压降温装置；主换热器具有第一冷流道、第二冷流道、第三冷流道和热流道；过冷器具有第一冷流道、第二冷流道、第三冷流道、第一热流道和第二热流道； 压缩机的进口用于进原料气，出口与冷却器的进口连接，冷却器的出口与脱硫单元连接； 脱硫单元与吸附器的进口连接，吸附器的出口与主换热器的热流道进口连接；再沸器与精馏塔连接；主换热器的热流道出口与再沸器的进口连接，再沸器的出口与过冷器的第二热流道进口连接，过冷器的第二热流道出口通过一号节流阀与一号气液分离器的进口连接；一号气液分离器的液体出口与精馏塔的回流液进口连接，一号气液分离器的气体出口与过冷器的第二冷流道进口连接，过冷器的第二冷流道出口与主换热器的第二冷流道进口连接，主换热器的第二冷流道出口与电加热器的进口连接，电加热器的出口与吸附器的再生气进口连接；精馏塔顶部的气体出口与过冷器的第一热流道进口连接，过冷器的第一热流道出口与二号气液分离器的进口连接；二号气液分离器的液体出口与精馏塔的回流液进口连接；二号气液分离器的气体出口通过降压降温装置与过冷器的第三冷流道进口连接，过冷器的第三冷流道出口与主换热器的第三冷流道进口连接； 精馏塔的液体出口通过二号节流阀与过冷器的第一冷流道进口连接，过冷器的第一冷流道出口与主换热器的第一冷流道进口连接，主换热器的第一冷流道出口连接二氧化碳产品管网；
该方法包括如下步骤：
1）、原料气进入压缩机压缩，增压至1.5～2.5Mpa，然后进入冷却器被冷却至常温，再送入脱硫床脱离硫组分杂质后，送入干燥单元；
2）、原料气在吸附器中进行干燥；
3）、经干燥单元脱水后的原料气送入主换热器，被返流气体冷却至-9℃～-11℃后进入再沸器中，在再沸器中作为精馏塔的热源被精馏塔底部的液体二氧化碳冷却至-27℃～-29℃；原料气在过冷器中被返流气体进一步冷却至-55℃～-60℃，再经一号节流阀降压降温后，送入一号气液分离器，在一号气液分离器中进行气液两相分离；
4）、一号气液分离器冷凝的液体二氧化碳送入精馏塔作为回流液参与精馏，在精馏塔底部得到提纯精制的液体二氧化碳，一号气液分离器出来的气体经过冷器和主换热器复热后作为吸附器的再生气体，再生气体在电加热器中升温至170℃～190℃后，进入吸附器；
5）、从精馏塔顶部得到的粗制气体，经过冷器冷却后，进入二号气液分离器中进行气液两相分离，二号气液分离器的液体进入精馏塔参与精馏；二号气液分离器分离出来的气体经降压降温后作为冷流体，在过冷器和主换热器中回收冷量；
6）、从精馏塔底部获得的二氧化碳液体，经二号节流阀降压至0.3MPa.A～0.4MPa.A，经过冷器和主换热器复热后送入二氧化碳产品管网。
2.根据权利要求1所述的低温精馏提纯回收二氧化碳的方法，其特征在于：所述的脱硫单元为脱硫床。
3.根据权利要求1所述的低温精馏提纯回收二氧化碳的方法，其特征在于：所述的主换热器和过冷器均为板翅式换热器。
4.根据权利要求1所述的低温精馏提纯回收二氧化碳的方法，其特征在于：所述的冷却器为水冷却器。
5.根据权利要求1所述的低温精馏提纯回收二氧化碳的方法，其特征在于：所述的吸附器为两个，并联设置。
6.根据权利要求1所述的低温精馏提纯回收二氧化碳的方法，其特征在于： 所述的主换热器的第三冷流道出口连接放空。
7.根据权利要求1所述的低温精馏提纯回收二氧化碳的方法，其特征在于：所述的降压降温装置包括三号节流阀和膨胀机，三号节流阀和膨胀机并联。
8.根据权利要求1所述的低温精馏提纯回收二氧化碳的方法，其特征在于：所述的一号气液分离器和二号气液分离器均位于精馏塔的上方。
9.根据权利要求1所述的低温精馏提纯回收二氧化碳的方法，其特征在于：步骤2）中，原料气在吸附器中干燥后，含水量<1ppm。
10.根据权利要求1所述的低温精馏提纯回收二氧化碳的方法，其特征在于：所述的再沸器与精馏塔为一体，再沸器集成设置在精馏塔的底部。
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