CN107300295B - 一种用原料氮气深冷法生产高纯氮产品的装置及方法 - Google Patents

一种用原料氮气深冷法生产高纯氮产品的装置及方法 Download PDF

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CN107300295B
CN107300295B CN201710129225.0A CN201710129225A CN107300295B CN 107300295 B CN107300295 B CN 107300295B CN 201710129225 A CN201710129225 A CN 201710129225A CN 107300295 B CN107300295 B CN 107300295B
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韩一松
谭芳
艾绍华
夏鸿雁
张振
钱吉庆
李玲
姚蕾
蒋云云
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Hang Yang Group Co ltd
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Abstract

一种用原料氮气深冷法生产高纯氮产品的装置及方法，所述的装置包括：一个压缩系统，一个精馏塔系统，一个换热系统以及一个膨胀机制冷系统，四者通过管道和阀门相连通，精馏塔系统由一个高纯氮塔、一个塔顶冷凝蒸发器和一个塔底冷凝蒸发器组成；由经所述换热系统换热后的带压氮气作为热源驱动所述高纯氮塔底部液体的蒸发，所述带压氮气被冷凝后的液体与经所述换热系统换热后的带压液氮经节流后作为冷源驱动所述高纯氮塔顶部气体的冷凝，并在高纯氮塔的相应位置获得所需纯度的高纯液氮产品；它具有能生产多种不同纯度要求的液氮产品，减少设备投资，降低设备运行能耗等特点。

Description

一种用原料氮气深冷法生产高纯氮产品的装置及方法
技术领域
本发明涉及一种用深冷法从原料氮气中生产高纯氮产品的装置及方法，属于低温精馏制高纯氮技术领域。
背景技术
在电子工业，如半导体集成电路制造中，需要使用高纯氮作为化学反应气的携带气、惰性保护气和封装气。以分子筛净化空气作原料，由常规双塔低温精馏法的空分分离装置得到的氮产品，由于分子筛并不吸附大气中的氢和一氧化碳，且氮和一氧化碳的沸点接近，使得氢和一氧化碳的含量高于大气中氢和一氧化碳的含量。典型的除去氮中杂质以获得高纯氮的方法是氧化催化吸附法，但不论是用于原料空气进分子筛净化前或深冷分离法后得到的氮，冷箱外常温或高温催化吸附法或是位于冷箱内的低温催化吸附法，都至少需要一吸附和再生的吸附容器，且催化剂和吸附剂需周期性进行投资，这些都增加了投资费用；而吸附容器周期性的切换工作，也导致了切换过程中原料气的切换泄露损失。再者，吸附剂的再生需要一定量的热量，也导致了能量的损失。为降低设备投资，减少设备运行能耗，需要能够找到一种设备投资便宜，运行能耗低的装置和方法。
发明内容
本发明的目的在于克服现有技术存在的不足，而提供了一种结构组成合理，能降低设备投资，减少设备运行能耗的用原料氮气深冷法生产高纯氮产品的装置及方法。
本发明的目的是通过如下技术方案来完成的，一种用原料氮气深冷法生产高纯氮产品的装置，它至少包括：一个压缩系统，精馏塔系统，一个换热系统以及一个膨胀机制冷系统，四者通过管道和阀门相连通，所述的精馏塔系统由一个高纯氮塔、一个塔顶冷凝蒸发器和一个塔底冷凝蒸发器 组成；所述塔顶冷凝蒸发器出口端有两个通道，一个通道通过管道连通排气通道，另一个通道通过管道连通所述高纯氮塔顶部，即所述精馏塔系统具有供从所述塔顶冷凝蒸发器出口端出来的不凝气体排放的第一通道；所述精馏塔系统还设置有一供从所述塔顶冷凝蒸发器出口端出来的冷凝液体回到所述高纯氮塔顶部的第二通道；
所述塔底冷凝蒸发器冷凝侧的一端通过管道连通主换热器冷端，所述塔底冷凝蒸发器冷凝侧的另一端通过管道和阀门连通所述塔顶冷凝蒸发器的蒸发侧；所述换热系统以及所述膨胀机制冷系统获得的液氮流体可通过管道和阀门连通所述塔顶冷凝蒸发器的蒸发侧；所述塔顶冷凝蒸发器的蒸发侧有供从所述塔顶冷凝蒸发器蒸发的气体引出的通道；
所述膨胀机制冷系统由一个或二个带膨胀叶轮的膨胀端、一个或二个带增压叶轮的增压端以及其他辅助性部件组成；所述膨胀端和所述增压端可以通过单轴直接连接或通过齿轮箱间接连接；
所述的换热系统包括一可将纯化、干燥和带压原料氮气的一部分冷却至饱和或近饱和状态的主换热器，所述主换热器冷端设置有一供从所述主换热器复热后去原料压缩机或去低压管网或去放空的气体的第一通道，该所述第一通道冷端入口通过管道直接或经过冷器E2间接连通所述塔顶冷凝蒸发器的蒸发侧；所述主换热器至少设置有一供去所述膨胀端膨胀的气体冷却的第二通道；所述主换热器至少设置有一供去节流阀节流的气体冷却的第三通道；
所述主换热器还可设置有一供所述高纯液氮复热的第四通道。
一种利用上述装置生产高纯氮产品的方法，该方法包括如下步骤：
将纯化、干燥、带压和经膨胀机膨胀后饱和或近饱和状态的氮气的全部或至少部分的进入高纯氮塔中部进行精馏；
经膨胀机膨胀后的液体与经高压节流阀节流后的液体至少部分的作为冷源驱动高纯氮塔顶部气体的冷凝；由经换热系统冷却至饱和或近饱和状态的带压氮气作为热源驱动高纯氮塔底部液体的蒸发，带压氮气被冷凝后的液体经阀后作为冷源驱动高纯氮塔顶部气体的冷凝。高纯氮塔的顶部气体经过塔顶冷凝蒸发器后，其不凝气体排出，其被冷凝的液体进入高纯氮塔的顶部作为回流液。在高纯氮塔的底部抽出含氧量高的液氮，并在高纯氮塔的相应位置获得所需纯度的高纯液氮产品；
作为优选：作为热源驱动高纯氮塔底部液体蒸发的所述带压氮气，其压力不小于0.05MPaG；当高纯氮塔的操作压力提高时，所述带压氮气的压力也需相应提高。
本发明的一个优点是仅用深冷精馏法用高纯氮塔及塔顶冷凝器和塔底蒸发器从容易获得的常规原料氮气中生产高纯氮产品，大大降低了设备投资，减少了设备运行能耗。
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图1是本发明所述的一个实施例流程图。
图2是图1所示实施例的变形实例流程图。
图3是本发明所述的另一个实施例流程图。
图4是图3所示实施例的变形实例流程图。
图5是本发明所述的又一个实施例流程图。
图6是图5所示实施例的变形实例流程图。
图7是本发明所述的又一个实施例流程图。
图8是图7所示实施例的变形实例流程图。
图9是本发明所述的又一个实施例流程图。
具体实施方式
下面将结合附图对本发明作详细的介绍：图1-5和图5-9所示，本发明所述的一种用原料氮气深冷法生产高纯氮产品的装置，它至少包括：一个压缩系统，精馏塔系统，一个换热系统以及一个膨胀机制冷系统，四者通过管道和阀门相连通，其特征在于所述的精馏塔系统由一个高纯氮塔C1、一个塔顶冷凝蒸发器K1和一个塔底冷凝蒸发器 K2组成；所述塔顶冷凝蒸发器K1出口端有两个通道，一个通道通过管道连通排气通道，另一个通道通过管道连通所述高纯氮塔C1顶部，即所述精馏塔系统具有供从所述塔顶冷凝蒸发器K1出口端出来的不凝气体排放的第一通道；所述精馏塔系统还设置有一供从所述塔顶冷凝蒸发器K1出口端出来的冷凝液体回到所述高纯氮塔C1顶部的第二通道。
图中所示，所述塔底冷凝蒸发器K2冷凝侧的一端通过管道连通所述主换热器E1冷端，所述塔底冷凝蒸发器K2冷凝侧的另一端通过管道和阀门连通所述塔顶冷凝蒸发器K1的蒸发侧；所述换热系统以及所述膨胀机制冷系统获得的液氮流体可通过管道和阀门连通所述塔顶冷凝蒸发器K1的蒸发侧；所述塔顶冷凝蒸发器K1的蒸发侧有供从所述塔顶冷凝蒸发器K1蒸发的气体引出的通道；
所述膨胀机制冷系统由一个或二个带膨胀叶轮的膨胀端ET、一个或二个带增压叶轮的增压端BT以及其他辅助性部件组成；所述膨胀端ET和所述增压端BT可以通过单轴直接连接或通过齿轮箱间接连接；
所述的换热系统包括一可将纯化、干燥和带压的原料氮气01的一部分03冷却至饱和或近饱和状态的主换热器E1，所述主换热器E1冷端设置有一供从所述主换热器E1复热后去原料压缩机NTC1或去低压管网或去放空的气体22的第一通道，该所述第一通道冷端入口通过管道直接或经过冷器E2间接连通所述塔顶冷凝蒸发器K1的蒸发侧；所述主换热器E1至少设置有一供去所述膨胀端膨胀的气体09冷却的第二通道；所述主换热器E1至少设置有一供去节流阀V1节流的气体11冷却的第三通道。
本发明所述主换热器E1还可设置有一供所述高纯液氮复热的第四通道。
一种用深冷法从原料氮气中生产高纯氮产品的的方法，该方法包括如下步骤：
将纯化、干燥、带压和经膨胀机膨胀后饱和或近饱和状态的氮气的全部或至少部分的进入高纯氮塔中部进行精馏；
经膨胀机膨胀后的液体与经高压节流阀节流后的液体至少部分的作为冷源驱动高纯氮塔顶部气体的冷凝；由经换热系统冷却至饱和或近饱和状态的带压氮气作为热源驱动高纯氮塔底部液体的蒸发，带压氮气被冷凝后的液体经阀后作为冷源驱动高纯氮塔顶部气体的冷凝。高纯氮塔的顶部气体经过塔顶冷凝蒸发器后，其不凝气体排出，其被冷凝的液体进入高纯氮塔的顶部作为回流液。在高纯氮塔的底部抽出含氧量高的液氮，并在高纯氮塔的相应位置获得所需纯度的高纯液氮产品；
本发明所述作为热源驱动高纯氮塔底部液体蒸发的所述带压氮气，其压力不小于0.05MPaG；当高纯氮塔的操作压力提高时，所述带压氮气的压力也需相应提高。
实施例：
在图1的实施例中，常压的纯化、干燥原料氮气00（杂质含量如氧含量10PPM、氢含量50PPM、一氧化碳含量50PPM、总烃含量10PPM）和从塔顶冷凝蒸发器K1出来经过冷器E2和主换热器E1复热后的气体22的全部或一部分进入压缩机NTC1压缩到约0.2MPaG。氮气01的一部分进入压缩机NTC2压缩到约2.5MPaG，一部分氮气07进入主换热器E1后又从主换热器E1中部抽出进入膨胀端ET1膨胀，膨胀后的氮气08又进入主换热器E1复热后回到压缩机NTC2入口；另一部分氮气05先后进入膨胀机增压端BT1和增压端BT2增压，后进入主换热器E1后又从主换热器E1中下部抽出一部分气体09进入膨胀端ET2膨胀，其另一部分气体11从主换热器冷端出来经节流阀V1节流后与从膨胀端ET2出来的10进入气液分离器SEP，其气体的一部分14反流进入主换热器E1复热后回到压缩机NTC2入口，其气体的另一部分15与氮气01的另一部分03经主换热器冷却后的流体16的一部分进入高纯氮塔C1的中下部参与精馏。流体16的另一部分17进入塔底冷凝蒸发器K2作为高纯氮塔C1的热源，其本身被冷凝后的流体18经过冷器E2过冷和节流阀V3节流后进入塔顶冷凝蒸发器K1作为冷源。从气液分离器SEP出来的液体12经过冷器E2过冷和节流阀V2节流后进入塔顶冷凝蒸发器K1作为冷源。流体20和流体19经塔顶冷凝蒸发器K1加热后的气体21经过冷器E2和主换热器E1复热后的气体22或回到低压管网或放空或其中至少一部分进入压缩机NTC1。
进入高纯氮塔C1的气体100经精馏后，高纯氮塔C1的顶部气体经过塔顶冷凝蒸发器K1冷凝后，其富含低沸点杂质的不凝气体23排出，其被冷凝的液体进入高纯氮塔的顶部作为回流液。在高纯氮塔的上部相应位置获得所需纯度的高纯液氮28产品。并在高纯氮塔的底部抽出含一氧化碳量较高的废液氮27。也可在塔顶冷凝蒸发器K1的蒸发侧抽取一定氮纯度的液氮24，从液体13中抽取一定氮纯度的液氮25，从液体18中抽取一定氮纯度的液氮26。
在图2的实施例中，从高纯氮塔的上部相应位置获得所需纯度的高纯液氮29，经液体泵P1加压后进入主换热器E1复热，获得带压的高纯气氮30。
上述两个实施例仅是本发明的优选实施方式，但本发明并不限制于以上描述的具体实施例。
如图3和图4描述的生产高纯液氮28和高纯气氮30的变形实例，其高低温膨胀机的流程形式是气体05先进入低温膨胀机的增压端BT2增压后再进入高温膨胀机的增压端BT1增压，其它流路同图1和图2描述，这些都是空分流程可以组织的常规形式。
如图5和图6描述的生产高纯液氮28和高纯气氮30的另一变形实例，其高低温膨胀机的流程形式是气体07先进入高温膨胀机的膨胀端ET1膨胀后再进入低温膨胀机的膨胀端ET2膨胀，这些也是空分流程可以组织的常规形式。
如图7和图8描述的生产高纯液氮28和高纯气氮30的再一变形实例，其制冷系统流程形式是气体05先进入膨胀机的增压端BT1增压后再进入冷冻机组RU冷却后其一部分气体09再进入膨胀端ET1，这些也是空分流程可以组织的常规形式。
如图9描述的生产高纯液氮28和高纯气氮30的再一变形实例，其制冷系统流程形式是气体05只进入膨胀机的增压端BT1增压后其一部分气体09再进入膨胀端ET1，这些也是空分流程可以组织的常规形式。
因此，在本发明的范畴下所作的各种变型或优化，也在本发明的保护范围内。

Claims (3)

1.一种用原料氮气深冷法生产高纯氮产品的装置，它至少包括：一个压缩系统，精馏塔系统，一个换热系统以及一个膨胀机制冷系统，四者通过管道和阀门相连通，其特征在于所述的精馏塔系统由一个高纯氮塔（C1）、一个塔顶冷凝蒸发器（K1）和一个塔底冷凝蒸发器（K2）组成；所述塔顶冷凝蒸发器（K1）出口端有两个通道，一个通道通过管道连通排气通道，另一个通道通过管道连通所述高纯氮塔（C1）顶部，即所述精馏塔系统具有供从所述塔顶冷凝蒸发器（K1）出口端出来的不凝气体排放的第一通道；所述精馏塔系统还设置有一供从所述塔顶冷凝蒸发器（K1）出口端出来的冷凝液体回到所述高纯氮塔（C1）顶部的第二通道，所述塔底冷凝蒸发器（K2）冷凝侧的一端通过管道连通主换热器（E1）冷端，所述塔底冷凝蒸发器（K2）冷凝侧的另一端通过管道和阀门连通所述塔顶冷凝蒸发器（K1）的蒸发侧；所述换热系统以及所述膨胀机制冷系统获得的液氮流体可通过管道和阀门连通所述塔顶冷凝蒸发器（K1）的蒸发侧；所述塔顶冷凝蒸发器（K1）的蒸发侧有供从所述塔顶冷凝蒸发器（K1）蒸发的气体引出的通道；
所述膨胀机制冷系统由一个或二个带膨胀叶轮的膨胀端（ET）、一个或二个带增压叶轮的增压端（BT）以及其他辅助性部件组成；所述膨胀端（ET）和所述增压端（BT）通过单轴直接连接或通过齿轮箱间接连接；
所述的换热系统包括一可将纯化、干燥和带压原料氮气（01）的一部分（03）冷却至饱和或近饱和状态的主换热器（E1），所述主换热器（E1）冷端设置有一供从所述主换热器（E1）复热后去原料压缩机（NTC1）或去低压管网或去放空的气体（22）的第一通道，该所述第一通道冷端入口通过管道直接或经过冷器（E2）间接连通所述塔顶冷凝蒸发器（K1）的蒸发侧；所述主换热器（E1）至少设置有一供去所述膨胀端膨胀的气体（09）冷却的第二通道；所述主换热器（E1）至少设置有一供去节流阀（V1）节流的气体（11）冷却的第三通道；
所述主换热器（E1）还可设置有一供高纯液氮复热的第四通道。
2.一种利用权利要求1所述装置生产高纯氮产品的方法，其特征在于该方法包括如下步骤：
将纯化、干燥、带压和经膨胀机膨胀后饱和或近饱和状态的氮气的全部或至少部分的进入高纯氮塔中部进行精馏；
经膨胀机膨胀后的液体与经高压节流阀节流后的液体至少部分的作为冷源驱动高纯氮塔顶部气体的冷凝；由经换热系统冷却至饱和或近饱和状态的带压氮气作为热源驱动高纯氮塔底部液体的蒸发，带压氮气被冷凝后的液体经阀后作为冷源驱动高纯氮塔顶部气体的冷凝，高纯氮塔的顶部气体经过塔顶冷凝蒸发器后，其不凝气体排出，其被冷凝的液体进入高纯氮塔的顶部作为回流液，在高纯氮塔的底部抽出含氧量高的液氮，并在高纯氮塔的相应位置获得所需纯度的高纯液氮产品。
3.根据权利要求2所述生产高纯氮产品的方法，其特征在于作为热源驱动高纯氮塔底部液体蒸发的所述带压氮气，其压力不小于0.05MPaG；当高纯氮塔的操作压力提高时，所述带压氮气的压力也需相应提高。
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