CN114923313B - 粗氩精制液氩***及其精制工艺 - Google Patents

粗氩精制液氩***及其精制工艺 Download PDF

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CN114923313B
CN114923313B CN202210535759.4A CN202210535759A CN114923313B CN 114923313 B CN114923313 B CN 114923313B CN 202210535759 A CN202210535759 A CN 202210535759A CN 114923313 B CN114923313 B CN 114923313B
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argon
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reflux
tower
condenser
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CN114923313A (zh
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刘建国
刘杰
崔静思
李慧军
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Shaanxi Juneng New Coal Chemical Technology Co ltd
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Abstract

本发明属于液氩制备技术领域，涉及一种粗氩精制液氩***及其精制工艺，***包括隔板塔、回流槽、塔顶气压缩机和蒸发冷凝器；隔板塔内从上自下依次设置塔顶段、传质段以及塔底段；传质段内的轴向上设置隔板，隔板将传质段分割成左腔室和右腔室；蒸发冷凝器置于塔底段内；左腔室上设置进料口，右腔室上设置出料口，进料口依次经塔顶段、塔顶气压缩机、蒸发冷凝器、回流槽回流至右腔室内并经出料口排出；右腔室与塔顶段连通。本发明具有能耗低、成本小、氩纯度高以及调节灵活的优点。

Description

粗氩精制液氩***及其精制工艺
技术领域
本发明属于液氩制备技术领域，涉及一种粗氩精制液氩***及其精制工艺。
背景技术
氩气是一种惰性气体，在常温下与其他物质均不起化学反应，在高温下也不溶于液态金属中，在焊接有色金属时更能显示其优越性，可用于灯泡充气和对不锈钢、镁、铝等的电弧焊接，即“氩弧焊”。
现有的氩气提取一般采用精馏法，提取工艺为两塔精馏或是三塔精馏，精馏过程中，采用液体空气做热源，液氮做冷源，虽然能实现液氩氩的提取，但是现有的提取工艺存在以下问题：液体空气和液氮消耗量大，空分中能耗大，提取成本高。
发明内容
针对现有氩气提取存在的原料消耗量大以及能耗大的技术问题，本发明提供一种粗氩精制液氩***及其精制工艺，具有能耗低、成本小、氩纯度高以及调节灵活的优点。
为了实现上述目的，本发明采用的技术方案是：
一种粗氩精制液氩***，包括隔板塔、回流槽、塔顶气压缩机和蒸发冷凝器；所述隔板塔内从上自下依次设置塔顶段、传质段以及塔底段；所述传质段内的轴向上设置隔板，所述隔板将传质段分割成左腔室和右腔室；所述蒸发冷凝器置于塔底段内；所述回流槽和塔顶气压缩机均置于隔板塔外部；所述左腔室上设置进料口，所述右腔室上设置出料口，所述进料口依次经塔顶段、塔顶气压缩机、蒸发冷凝器、回流槽回流至右腔室内并经出料口排出；所述右腔室与塔顶段连通。
进一步的，所述回流槽包括上下依次连通的冷凝罐和回流罐，所述回流罐上设置回流进口以及与回流进口连通的回流出口；所述冷凝罐上设置与回流进口连通的排气口；所述回流进口与蒸发冷凝器连通，所述回流出口与右腔室连通。
进一步的，所述粗氩精制液氩***还包括设置在冷凝罐内的塔顶冷凝器；所述回流进口经塔顶冷凝器与排气口连通；所述冷凝罐上还分别设置冷料进口以及位于冷料进口上方的冷料出口，所述冷料进口经塔顶冷凝器与冷料出口连通。
进一步的，所述粗氩精制液氩***还包括外接在排气口上的排放管路，所述排放管路上设置排放控制阀。
进一步的，所述粗氩精制液氩***还包括节流阀和回流泵；所述回流出口依次经回流泵、节流阀与右腔室连通。
进一步的，所述粗氩精制液氩***还包括换热器以及与换热器连通的冷凝器；所述冷凝器与进料口连通；所述冷凝器上设置与冷凝器内部连通的液氮管路；所述换热器上设置与换热器内部连通的气氮管路。
一种所述粗氩精制液氩***的液氩精制工艺，包括以下步骤：
1)粗氩进入隔板塔的左腔室换热传质得到氩氮气体和富氧液，氩氮气体不断向上在塔顶段富集，富氧液向下在塔底段富集；
2)同时，塔顶段富集的氩氮气体经压缩换热冷凝，得到的冷凝液回流至右腔室换热传质得到氩氮气体、精氩液和富氧液，氩氮气体向上在塔顶段富集，富氧液向下在塔底段富集，精氩液作为产品采出；得到的未冷凝气经塔顶冷凝器冷凝控制排放。
进一步的，所述步骤1)中，粗氩是直接从空分送入的或是利用液氮将粗氩气常温降低至-180℃以下得到的。
进一步的，所述粗氩中，氮气体积占比小于0.5％。
进一步的，所述步骤2)中，冷凝液回流过程中，通过排放控制阀控制未冷凝气的排放量及冷凝液的回流量。
本发明的有益效果是：
1、本发明提供的精制***和精制工艺，利用隔板塔塔底蒸发冷凝器的热泵精馏技术，将塔底冷量带入塔顶，塔顶热量带入塔底，完成回流及氩富积纯化，节省外界输入的热量和冷量，降低成本，达到节能降耗的目的。
2、本发明中，塔顶气经压缩冷凝作为回流液，对隔板塔进行减压提高氩纯度，回流过程中，通过压缩机转速来调节回流比，实现热量平衡及氩纯度的提高，能耗低，调节灵活。
附图说明
图1为本发明提供的液氩精制***；
其中：
1—隔板塔；2—回流槽；3—塔顶气压缩机；4—冷凝器；5—换热器；6—蒸发冷凝器；7—塔顶冷凝器；8—排放控制阀；9—回流泵；10—节流阀。
具体实施方式
现结合附图以及实施例对本发明做详细的说明。
实施例
参见图1，本实施例提供的粗氩精制液氩***包括隔板塔1、回流槽2、塔顶气压缩机3和蒸发冷凝器6；隔板塔1内从上自下依次设置塔顶段、传质段以及塔底段；传质段内的轴向上设置隔板，隔板将传质段分割成左腔室和右腔室；回流槽2和塔顶气压缩机3均置于隔板塔1外，蒸发冷凝器6置于塔底段内；左腔室侧壁上设置进料口，右腔室侧壁上设置出料口，进料口依次经塔顶段、塔顶气压缩机3、蒸发冷凝器6、回流槽2回流至右腔室内并经出料口排出；右腔室与塔顶段连通。
回流槽2包括上部的冷凝罐以及下部的回流罐，冷凝罐与回流罐连通；回流罐上设置回流进口以及与回流进口连通的回流出口；冷凝罐上设置与回流进口连通的排气口；回流进口与蒸发冷凝器6连通，回流出口与右腔室连通。
粗氩精制液氩***还包括设置在冷凝罐内的塔顶冷凝器7；回流进口经塔顶冷凝器7与排气口连通；冷凝罐上还分别设置冷料进口以及位于冷料进口上方的冷料出口，冷料进口经塔顶冷凝器7与冷料出口连通。
粗氩精制液氩***还包括外接在排气口上的排放管路，排放管路上设置排放控制阀8。
粗氩精制液氩***还包括节流阀10和回流泵9；回流出口依次经回流泵9、节流阀10与右腔室连通。
粗氩精制液氩***还包括换热器5以及与换热器5连通的冷凝器4；冷凝器4与进料口连通；冷凝器4上设置与冷凝器4内部连通的液氮管路；换热器5上设置与换热器5内部连通的气氮管路。
具体的，隔板塔1为圆柱塔，隔板塔1轴向放置，隔板塔1内从上自下依次设置塔顶段、传质段以及塔底段；传质段通过隔板分为两个独立的左腔室和右腔室，左腔室顶部和右腔室顶部均与塔顶段连通，左腔室底部和右腔室底部均与塔底段连通。左腔室塔侧中部设置进料口，右腔室塔侧中部设置出料口，塔顶段上设置塔顶气出口，塔顶气出口经塔顶气压缩机3、蒸发冷凝器6与回流槽2连通，经冷凝后分为两路，第一路凝液经回流泵9和节流阀10连通，并经节流阀10回流至隔板塔1右侧出料口上方的塔板处，隔板塔1塔顶设置塔底液出口；第二路未凝气经塔顶冷凝器7从排放管路排出。
实施时，回流槽2包括上部的冷凝罐以及下部的回流罐，冷凝罐和回流罐均为圆柱形罐体，冷凝罐直径小于回流罐直径，冷凝罐和回流罐同轴设置且相连通组成凸形结构。回流罐的侧部设置回流进口，回流罐的底部设置回流出口，冷凝罐内的顶部位置处设置塔顶冷凝器7，冷凝罐侧壁上分别设置冷料进口和冷料出口，冷凝罐顶部设置排气口，回流进口与蒸发冷凝器6连通，回流出口与回流泵9连通；排气口外接排放管路；排放管路上设置排放控制阀8，通过排放控制阀8控制回流槽2内的未凝气，保证氮平衡。
实施时，冷凝器4和换热器5均为管壳式结构，冷凝器4的管侧和换热器5管侧均流过粗氩原料气，冷凝器4的壳侧分别与液氮管路和换热器5壳侧连通，利用液氮作为冷源，对粗氩原料气进行降温冷凝，换热器5壳侧还设置气氮管路，液氮换热升温后从气氮管路排出。
塔顶气压缩机3是变频电机驱动的压缩机。
实施时，通过节流阀10控制回流至隔板塔1塔侧的液体的流量，通过回流泵9控制回流速度。
本实施例提供的粗氩精制液氩的精制工艺包括以下步骤：
1)粗氩进入隔板塔1的左腔室换热传质得到氩氮气体和富氧液，氩氮气体不断向上在塔顶段富集，富氧液向下在塔底段富集；
2)同时，塔顶段富集的氩氮气体经压缩换热冷凝，得到的冷凝液(液氩氮)回流至右腔室换热传质得到氩氮气体、精氩液和富氧液，氩氮气体向上在塔顶段富集，富氧液向下在塔底段富集，从塔顶排出收集，精氩液作为产品从出料口采出；得到的未冷凝气经塔顶冷凝器7冷凝控制排放。
步骤1)中，粗氩是直接从空分送来的。粗氩中主要包括氩气、氮气和氧气，且氮气小于0.5％。
步骤2)中，冷凝液(液氩氮)回流过程中，通过排放控制阀8通过排放控制阀8控制未冷凝气的排放量及冷凝液的回流量。
具体的，塔顶采集的合格氩氮气体经塔顶气压缩机3压缩后，塔顶氩氮气体加压后冷凝温度升高，并流经蒸发冷凝器6和隔板塔1塔底的介质(富氧液体)换热，氩氮气体自身冷凝后进入回流槽2中，具体的，从回流罐侧部的回流进口进入回流槽2中，氩氮气体自身冷凝得到液氩氮以及未冷凝氮气，未冷凝氮气向上进入冷凝罐中流经塔顶冷凝器7，此时，液氮从冷料进口也进入塔顶冷凝器7，未冷凝氮气(含有部分氩气)与液氮进行热量交换，未冷凝氮气中携带的氩气进一步降温冷凝得到液氩和氮气，液氮升温后成气态氮气从冷料出口排出，与液态冷凝后的氮气继续从排气口排出，经排放控制阀8后进入排放管路排放收集，液氩向下进入回流罐与液氩氮混合，从回流罐塔底的回流出口经回流泵9和节流阀10返回隔板塔1的右侧出料口上方的塔板处，实现减压回流提高液氩的富积。
从粗氩气中精制液氩，液氩的精制工艺包括以下步骤。
首先，要对粗氩气进行降温，使其从气态变成液态然后进行精制。具体的，粗氩进入换热器5的管侧，与从冷凝器4壳侧送入的液氮进行热交换，粗氩的温度降低，然后粗氩进一步进入冷凝器4管侧，与进入冷凝器4壳侧的液氮进行交换，粗氩温度从室温降低至-180℃。
然后，粗氩进入隔板塔1的左腔室换热传质得到氩氮气体和富氧液，氩氮气体不断向上在塔顶段富集，富氧液向下在塔底段富集；同时，塔顶段富集的氩氮气体经压缩换热冷凝，得到的冷凝液(液氩氮)回流至右腔室换热传质得到氩氮气体、精氩液和富氧液，氩氮气体向上在塔顶段富集，富氧液向下在塔底段富集，精氩液作为产品采出；得到的未冷凝气经塔顶冷凝器7冷凝控制排放。
采用本实施例的精制***及精制工艺，精氩液体的纯度为99.99％。
本实施例中，冷凝液(液氩氮)作为回流液减压回流至隔板塔1内，为了保证塔顶气与蒸发冷凝器6的换热冷凝交换平衡，同时为了实现隔板塔1内液氩的富集，通过排放控制阀8控制排出***的氮气含量及及冷凝液的回流量，以保证***氮的平衡。
本实施例提供的液氩精制工艺的原理是：粗氩气经冷却成粗氩液或者空分来的粗氩液，进入隔板塔传质段，与塔内介质换热传质，塔底压缩塔顶气给塔底加热，促进塔底氩气的蒸发及氧的富集，氩氮富集塔顶，高浓度液氧富集塔底，塔顶高浓度回流液氩与氩氮气传质，隔板右侧富集高纯度的***氩作为产品采出，压缩塔顶气经蒸发冷凝器，与隔板塔1塔底的介质换热自身冷凝后，冷凝液经回流后回流至隔板塔1，塔底蒸发的气体上升与隔板两侧下降液体传质，使得隔板右侧的氩富集及塔底氩的提取，实现氩气的提浓得到精制液氩；部分未冷凝气经塔顶冷凝器7冷凝控制排放，以保证***氮的平衡。
本发明提供的精制***及精制工艺，利用热泵精馏技术，将隔板塔塔底冷量带入隔板塔塔顶，隔板塔塔顶热量带入隔板塔塔底，完成回流及氩富积纯化，节省外界输入的热量和冷量，能对回流量、氨平衡和液氩纯度进行调控，能耗低，调节灵活。

Claims (9)

1.一种粗氩精制液氩***，其特征在于，包括隔板塔(1)、回流槽(2)、塔顶气压缩机(3)和蒸发冷凝器(6)；所述隔板塔(1)内从上自下依次设置塔顶段、传质段以及塔底段；所述传质段内的轴向上设置隔板，所述隔板将传质段分割成左腔室和右腔室；所述蒸发冷凝器(6)置于塔底段内；所述回流槽(2)和塔顶气压缩机(3)均置于隔板塔(1)外部；所述左腔室上设置进料口，所述右腔室上设置出料口，进入进料口的粗氩依次经塔顶段、塔顶气压缩机(3)、蒸发冷凝器(6)、回流槽(2)回流至右腔室内并经出料口排出；所述右腔室与塔顶段连通；
所述回流槽(2)包括上下依次连通的冷凝罐和回流罐，所述回流罐上设置回流进口以及与回流进口连通的回流出口；所述冷凝罐上设置与回流进口连通的排气口；所述回流进口与蒸发冷凝器(6)连通，所述回流出口与右腔室连通。
2.根据权利要求1所述的粗氩精制液氩***，其特征在于，所述粗氩精制液氩***还包括设置在冷凝罐内的塔顶冷凝器(7)；所述回流进口经塔顶冷凝器(7)与排气口连通；所述冷凝罐上还分别设置冷料进口以及位于冷料进口上方的冷料出口，所述冷料进口经塔顶冷凝器(7)与冷料出口连通。
3.根据权利要求2所述的粗氩精制液氩***，其特征在于，所述粗氩精制液氩***还包括外接在排气口上的排放管路，所述排放管路上设置排放控制阀(8)。
4.根据权利要求3所述的粗氩精制液氩***，其特征在于，所述粗氩精制液氩***还包括节流阀(10)和回流泵(9)；所述回流出口依次经回流泵(9)、节流阀(10)与右腔室连通。
5.根据权利要求4所述的粗氩精制液氩***，其特征在于，所述粗氩精制液氩***还包括换热器(5)以及与换热器(5)连通的冷凝器(4)；所述冷凝器(4)与进料口连通；所述冷凝器(4)上设置与冷凝器(4)内部连通的液氮管路；所述换热器(5)上设置与换热器(5)内部连通的气氮管路。
6.一种基于权利要求4或5所述粗氩精制液氩***的液氩精制工艺，其特征在于，所述液氩精制工艺包括以下步骤：
1)粗氩进入隔板塔(1)左腔室换热传质得到氩氮气体和富氧液，氩氮气体不断向上在塔顶段富集，富氧液向下在塔底段富集；
2)同时，塔顶段富集的氩氮气体经压缩换热冷凝，得到的冷凝液回流至右腔室换热传质得到氩氮气体、精氩液和富氧液，氩氮气体向上在塔顶段富集，富氧液向下在塔底段富集，精氩液作为产品采出；得到的未冷凝气经塔顶冷凝器(7)冷凝排放。
7.根据权利要求6所述的液氩精制工艺，其特征在于，所述步骤1)中，粗氩是直接从空分送入的或是利用液氮将粗氩气常温降低至-180℃以下得到的。
8.根据权利要求7所述的液氩精制工艺，其特征在于，所述粗氩中，氮气体积占比小于0.5％。
9.根据权利要求8所述的液氩精制工艺，其特征在于，所述步骤2)中，冷凝液回流过程中，通过排放控制阀(8)控制未冷凝气的排放量及冷凝液的回流量。
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