CN113154795A - 一种低温精馏富集低丰度18o同位素的装置及其使用方法 - Google Patents
一种低温精馏富集低丰度18o同位素的装置及其使用方法 Download PDFInfo
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Abstract
一种低温精馏富集低丰度18O同位素的装置,它主要由三个精馏塔、浓缩塔、换热器、杂质吸附器组成,每个塔之间前后串联,其中前三级精馏塔,每一级塔底部液体为顶部蒸汽的冷凝提供冷量,后作为下一级精馏塔的进料;浓缩塔底部蒸发热源主要为三个精馏塔顶部排气与常温氧气混合气体,所述杂质吸附器进口通过氧气截止阀与外部原料高压氧连接,杂质吸附器出口分别连气动增压阀出口、主换热器热端进口,主换热器热端出口连接精馏富集塔原料进口,所述杂质吸附器底部排渣口连接截止阀进口,本发明装置用来生产低丰度18O同位素,具有较好的节能效果。
Description
技术领域
本发明涉及的一种低温精馏富集低丰度18O同位素的技术、装置及其适用方法,属于低温精馏领域。
背景技术
18O同位素具有战略稀缺性,深冷精馏富集同位素技术长期被西方国家垄断。18O同位素在诸如癌症早期检查、核磁共振造影、生命科学等领域内具有重要应用。目前,国内18O同位素市场基本被美日欧等发达国家和地区所垄断。利用低温精馏技术分离18O同位素具有较大的液氮消耗量,从而导致能耗较高。因此开发节能型同位素深冷精馏富集技术具有战略层面意义。本发明涉及一种低温精馏富集低丰度18O同位素的技术及装置,本发明装置前两级精馏塔,每一级塔底部液体蒸发潜热用于顶部蒸汽的冷凝,塔底部低温液体蒸发后气体作为下一级精馏塔的进料,节能效果明显;第三级精馏塔塔底部液体液态出顶部冷凝器,作为浓缩塔进料。浓缩塔底部蒸发热源主要为三个精馏塔顶部排气与常温氧气混合气体。本发明装置用来生产低丰度18O同位素,具有较好的节能效果。
发明内容
本发明开发了一种低温精馏富集低丰度18O同位素的技术及装置,将精馏塔底部液体节流,作为塔顶蒸汽冷凝冷源,较大减少了液氮消耗量,具有显著的节能效果。为实现本发明的目的,一种低温精馏富集低丰度18O同位素的装置,它主要由三个精馏塔、浓缩塔、换热器、杂质吸附器组成,每个塔之间前后串联,其中前三级精馏塔,每一级塔底部液体为顶部蒸汽的冷凝提供冷量,后作为下一级精馏塔的进料;浓缩塔底部蒸发热源主要为三个精馏塔顶部排气与常温氧气混合气体,所述杂质吸附器进口通过氧气截止阀与外部原料高压氧连接,杂质吸附器出口分别连气动增压阀出口、主换热器热端进口,主换热器热端出口连接精馏富集塔原料进口,所述杂质吸附器底部排渣口连接截止阀进口,截止阀出口接外界环境,所述精馏富集塔底部液体出口连接液体截止阀进口,液体截止阀出口连接减压阀进口,减压阀出口连接精馏富集塔顶部冷凝器冷端进口,精馏富集塔顶部冷凝器冷端出口连接截止阀进口。精馏富集塔顶部排气口连接冷凝器热端进口,冷凝器热端出口连接截止阀进口,所述截止阀出口连接精馏富集塔原料进口。精馏富集塔底部液体出口连接液体截止阀进口,液体截止阀出口连接减压阀进口,减压阀出口连接精馏富集塔顶部冷凝器冷端进口,精馏富集塔顶部冷凝器冷端出口连接截止阀进口。精馏富集塔顶部排气口连接冷凝器热端进口,冷凝器热端出口连接截止阀进口。
作为优选:所述截止阀出口连接精馏富集塔原料进口。精馏富集塔底部液体出口连接液体截止阀进口,液体截止阀出口连接减压阀进口,减压阀出口连接精馏富集塔顶部冷凝器冷端进口,精馏富集塔顶部冷凝器冷端出口连接截止阀进口。精馏富集塔顶部排气口连接冷凝器热端进口,冷凝器热端出口连接截止阀进口。
作为优选:所述截止阀出口连接浓缩塔原料进口。浓缩塔底部液体出口分别连再沸器冷端进口、主换热器冷端进口;再沸器冷端出口连接浓缩塔下部气体入口。浓缩塔顶部排气口连接截止阀进口,截止阀出口连接主换热器冷端进口,再沸器热端进口连接混合器出口;再沸器热端出口连接主换热器冷端进口。
作为优选:所述主换热器冷端出口连接压缩机进口,压缩机出口高压氧气回收利用。主换热器冷端出口连接18O产品充装系统;主换热器冷端出口连接截止阀进口,截止阀出口连接气动增压阀进口,气动增压阀压力源口连接仪表气源,所述主换热器冷端进口连接外部冷源冷媒出口,主换热器冷端出口连接外部冷源冷媒进口。
作为优选:所述混合器进口分别连接截止阀出口、截止阀出口。截止阀进口连接常温氧气管道。需要指出,截止阀出口、截止阀出口、截止阀出口共同连接混合器进口,混合器出口分别连接截止阀进口、截止阀进口,截止阀出口连接大气排空。
一种低温精馏富集低丰度18O同位素的装置的使用方法为:
1).本发明装置启动前,所有阀门均关闭,系统启动前需用0.3~0.4MPa的常温氮气吹扫系统管路1~2h,然后系统抽真空至2Pa以下。系统仪电控检测完毕后,本发明装置启动前需要裸冷至液氧温区,启用前需通过辅助管路往精馏富集塔灌注液氧。
2).启动外部冷源循环,外部冷媒通过主换热器冷端为整套装置提供冷源,打开截止阀,高压原料氧气进入杂质吸附塔,过滤原料氧气中的CO2、CO、CmHn等;过滤后原料氧气进入主换热器热端,然后进入精馏富集塔。打开阀门,缓慢开启减压阀,减压过冷后液氧进入顶部冷凝器冷端,冷凝精馏富集塔顶部氧气。精馏富集塔底部液氧减少由顶部冷凝液氧补充。
3).建立精馏富集塔全回流工况,然后缓慢打开截止阀,精馏富集塔底部液氧蒸发后进入精馏富集塔。打开阀门,缓慢开启减压阀,减压过冷后液氧进入顶部冷凝器冷端,冷凝精馏富集塔顶部氧气。精馏富集塔底部液氧减少由顶部冷凝液氧补充。
4).建立精馏富集塔全回流工况,然后缓慢打开截止阀,精馏富集塔底部液氧蒸发后进入精馏富集塔。打开阀门,缓慢开启减压阀,减压过冷后液氧进入顶部冷凝器冷端,冷凝精馏富集塔顶部氧气。精馏富集塔底部液氧减少由顶部冷凝液氧补充。
5).建立精馏富集塔全回流工况。联动精馏富集塔,建立精馏平衡工况,直至精馏富集塔底部液氧18O同位素丰度达标。
6).缓慢打开阀门,精馏富集塔底部液氧经过顶部冷凝器进入浓缩塔。 缓慢打开阀门 ,精馏富集塔顶部开始排气,精馏富集塔顶部排气通过混合器汇合。打开阀门,精馏富集塔顶部排气进入再沸器热端,作为浓缩塔底部蒸发氧气热源。打开阀门,浓缩塔顶部排气进入主换热器冷端,打开阀门、气动增压阀,复热后浓缩塔顶部排气与原料氧气汇合。
7).当再沸器提供热源不足时,可通过混合器提供常温氧气,与精馏富集塔顶部排气汇流。再沸器热端出口氧气进入主换热器冷端,复热后经过压缩机压缩后回收, 浓缩塔底部产品进入主换热器冷端,复热后产品18O去产品充装系统。
本发明一种低温精馏富集低丰度18O同位素的技术及装置,具体来说整套装置由三个精馏塔加一个浓缩塔构成,塔段之间前后串联。本发明装置前两级精馏塔,每一级塔底部液体蒸发潜热用于顶部蒸汽的冷凝,塔底部低温液体蒸发后气体作为下一级精馏塔的进料,节能效果明显;第三级精馏塔塔底部液体液态出顶部冷凝器,作为浓缩塔进料。浓缩塔底部蒸发热源主要为三个精馏塔顶部排气与常温氧气混合气体。本发明装置用来生产低丰度18O同位素,具有较好的节能效果。
附图说明
图1为本发明构成示意图。
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所示,一种低温精馏富集低丰度18O同位素的装置,它主要由三个精馏塔、浓缩塔、换热器、杂质吸附器组成,每个塔之间前后串联,其中前三级精馏塔,每一级塔底部液体为顶部蒸汽的冷凝提供冷量,后作为下一级精馏塔的进料;浓缩塔底部蒸发热源主要为三个精馏塔顶部排气与常温氧气混合气体,所述杂质吸附器2进口通过氧气截止阀1与外部原料高压氧连接,杂质吸附器2出口分别连气动增压阀出口、主换热器6热端进口35,主换热器6热端出口39连接精馏富集塔7原料进口,所述杂质吸附器2底部排渣口连接截止阀4进口,截止阀4出口接外界环境,所述精馏富集塔7底部液体出口连接液体截止阀10进口,液体截止阀10出口连接减压阀5进口,减压阀5出口连接精馏富集塔7顶部冷凝器8冷端进口,精馏富集塔7顶部冷凝器8冷端出口连接截止阀9进口。精馏富集塔7顶部排气口连接冷凝器8热端进口,冷凝器8热端出口连接截止阀30进口,所述截止阀9出口连接精馏富集塔12原料进口。精馏富集塔12底部液体出口连接液体截止阀15进口,液体截止阀15出口连接减压阀11进口,减压阀11出口连接精馏富集塔12顶部冷凝器13冷端进口,精馏富集塔12顶部冷凝器13冷端出口连接截止阀14进口。精馏富集塔12顶部排气口连接冷凝器13热端进口,冷凝器13热端出口连接截止阀31进口,所述截止阀14出口连接精馏富集塔17原料进口。精馏富集塔17底部液体出口连接液体截止阀20进口,液体截止阀20出口连接减压阀16进口,减压阀16出口连接精馏富集塔17顶部冷凝器18冷端进口,精馏富集塔17顶部冷凝器18冷端出口连接截止阀19进口。精馏富集塔17顶部排气口连接冷凝器18热端进口,冷凝器18热端出口连接截止阀32进口,所述截止阀19出口连接浓缩塔21原料进口。浓缩塔21底部液体出口分别连再沸器23冷端进口、主换热器6冷端进口41;再沸器23冷端出口连接浓缩塔21下部气体入口。浓缩塔21顶部排气口连接截止阀22进口,截止阀22出口连接主换热器6冷端进口42,再沸器23热端进口连接混合器24出口;再沸器23热端出口连接主换热器6冷端进口40,所述主换热器6冷端出口36连接压缩机28进口,压缩机28出口高压氧气回收利用。主换热器6冷端出口37连接18O产品充装系统;主换热器6冷端出口38连接截止阀27进口,截止阀27出口连接气动增压阀3进口,气动增压阀3压力源口45连接仪表气源,所述主换热器6冷端进口43连接外部冷源26冷媒出口,主换热器6冷端出口44连接外部冷源26冷媒进口,所述混合器24进口分别连接截止阀25出口、截止阀29出口。截止阀25进口连接常温氧气管道。需要指出,截止阀30出口、截止阀31出口、截止阀32出口共同连接混合器33进口,混合器33出口分别连接截止阀34进口、截止阀29进口,截止阀34出口连接大气排空。
一种低温精馏富集低丰度18O同位素的装置的使用方法为:
1).本发明装置启动前,所有阀门均关闭,系统启动前需用0.3~0.4MPa的常温氮气吹扫系统管路1~2h,然后系统抽真空至2Pa以下。系统仪电控检测完毕后,本发明装置启动前需要裸冷至液氧温区,启用前需通过辅助管路往精馏富集塔7、12、17、21灌注液氧。
2).启动外部冷源循环26,外部冷媒通过主换热器6冷端43、44为整套装置提供冷源,打开截止阀21,高压原料氧气进入杂质吸附塔2,过滤原料氧气中的CO2、CO、CmHn等;过滤后原料氧气进入主换热器6热端35、39,然后进入精馏富集塔7。打开阀门10,缓慢开启减压阀6,减压过冷后液氧进入顶部冷凝器(8)冷端,冷凝精馏富集塔7顶部氧气。精馏富集塔7底部液氧减少由顶部冷凝液氧补充。
3).建立精馏富集塔7全回流工况,然后缓慢打开截止阀9,精馏富集塔7底部液氧蒸发后进入精馏富集塔12。打开阀门15,缓慢开启减压阀11,减压过冷后液氧进入顶部冷凝器13冷端,冷凝精馏富集塔12顶部氧气。精馏富集塔12底部液氧减少由顶部冷凝液氧补充。
4).建立精馏富集塔12全回流工况,然后缓慢打开截止阀14,精馏富集塔12底部液氧蒸发后进入精馏富集塔17。打开阀门20,缓慢开启减压阀16,减压过冷后液氧进入顶部冷凝器18冷端,冷凝精馏富集塔(17)顶部氧气。精馏富集塔17底部液氧减少由顶部冷凝液氧补充。
5).建立精馏富集塔17全回流工况。联动精馏富集塔7、12、17,建立精馏平衡工况,直至精馏富集塔(17)底部液氧18O同位素丰度达标。
6).缓慢打开阀门19,精馏富集塔17底部液氧经过顶部冷凝器18进入浓缩塔21。缓慢打开阀门 30、31、32,精馏富集塔7、12、17顶部开始排气,精馏富集塔7、12、17顶部排气通过混合器33汇合。打开阀门29,精馏富集塔7、12、17顶部排气进入再沸器23热端,作为浓缩塔21底部蒸发氧气热源。打开阀门22,浓缩塔21顶部排气进入主换热器6冷端42、38,打开阀门27、气动增压阀3,复热后浓缩塔21顶部排气与原料氧气汇合。
7).当再沸器23提供热源不足时,可通过混合器24提供常温氧气,与精馏富集塔7、12、17顶部排气汇流。再沸器23热端出口氧气进入主换热器6冷端40、36,复热后经过压缩机28压缩后回收, 浓缩塔21底部产品进入主换热器6冷端41、37,复热后产品18O去产品充装系统。
本发明一种低温精馏富集低丰度18O同位素的技术及装置,由三个精馏塔加一个浓缩塔构成,塔段之间前后串联。本发明装置前两级精馏塔,每一级塔底部液体蒸发潜热用于顶部蒸汽的冷凝,塔底部低温液体蒸发后气体作为下一级精馏塔的进料,节能效果明显;第三级精馏塔塔底部液体液态出顶部冷凝器,作为浓缩塔进料。浓缩塔底部蒸发热源主要为三个精馏塔顶部排气与常温氧气混合气体。本发明装置用来生产低丰度18O同位素,具有较好的节能效果。
Claims (6)
1.一种低温精馏富集低丰度18O同位素的装置,它主要由三个精馏塔、浓缩塔、换热器、杂质吸附器组成,每个塔之间前后串联,其中前三级精馏塔,每一级塔底部液体为顶部蒸汽的冷凝提供冷量,后作为下一级精馏塔的进料;浓缩塔底部蒸发热源主要为三个精馏塔顶部排气与常温氧气混合气体,其特征在于所述杂质吸附器(2)进口通过氧气截止阀(1)与外部原料高压氧连接,杂质吸附器(2)出口分别连气动增压阀出口、主换热器(6)热端进口(35),主换热器(6)热端出口(39)连接精馏富集塔(7)原料进口,所述杂质吸附器(2)底部排渣口连接截止阀(4)进口,截止阀(4)出口接外界环境,所述精馏富集塔(7)底部液体出口连接液体截止阀(10)进口,液体截止阀(10)出口连接减压阀(5)进口,减压阀(5)出口连接精馏富集塔(7)顶部冷凝器(8)冷端进口,精馏富集塔(7)顶部冷凝器(8)冷端出口连接截止阀(9)进口,精馏富集塔(7)顶部排气口连接冷凝器(8)热端进口,冷凝器(8)热端出口连接截止阀(30)进口,所述截止阀(9)出口连接精馏富集塔(12)原料进口,精馏富集塔(12)底部液体出口连接液体截止阀(15)进口,液体截止阀(15)出口连接减压阀(11)进口,减压阀(11)出口连接精馏富集塔(12)顶部冷凝器(13)冷端进口,精馏富集塔(12)顶部冷凝器(13)冷端出口连接截止阀(14)进口,精馏富集塔(12)顶部排气口连接冷凝器(13)热端进口,冷凝器(13)热端出口连接截止阀(31)进口。
2.根据权利要求1所述的低温精馏富集低丰度18O同位素的装置,其特征在于所述截止阀(14)出口连接精馏富集塔(17)原料进口,精馏富集塔(17)底部液体出口连接液体截止阀(20)进口,液体截止阀(20)出口连接减压阀(16)进口,减压阀(16)出口连接精馏富集塔(17)顶部冷凝器(18)冷端进口,精馏富集塔(17)顶部冷凝器(18)冷端出口连接截止阀(19)进口,精馏富集塔(17)顶部排气口连接冷凝器(18)热端进口,冷凝器(18)热端出口连接截止阀(32)进口。
3.根据权利要求2所述的低温精馏富集低丰度18O同位素的装置,其特征在于所述截止阀(19)出口连接浓缩塔(21)原料进口,浓缩塔(21)底部液体出口分别连再沸器(23)冷端进口、主换热器(6)冷端进口(41);再沸器(23)冷端出口连接浓缩塔(21)下部气体入口,浓缩塔(21)顶部排气口连接截止阀(22)进口,截止阀(22)出口连接主换热器(6)冷端进口(42),再沸器(23)热端进口连接混合器(24)出口;再沸器(23)热端出口连接主换热器(6)冷端进口(40)。
4.根据权利要求1或3所述的低温精馏富集低丰度18O同位素的装置,其特征在于所述主换热器(6)冷端出口(36)连接压缩机(28)进口,压缩机(28)出口高压氧气回收利用,主换热器(6)冷端出口(37)连接18O产品充装系统;主换热器(6)冷端出口(38)连接截止阀(27)进口,截止阀(27)出口连接气动增压阀(3)进口,气动增压阀(3)压力源口(45)连接仪表气源,所述主换热器(6)冷端进口(43)连接外部冷源(26)冷媒出口,主换热器(6)冷端出口(44)连接外部冷源(26)冷媒进口。
5.根据权利要求4所述的低温精馏富集低丰度18O同位素的装置,其特征在于所述混合器(24)进口分别连接截止阀(25)出口、截止阀(29)出口,截止阀(25)进口连接常温氧气管道,需要指出,截止阀(30)出口、截止阀(31)出口、截止阀(32)出口共同连接混合器(33)进口,混合器(33)出口分别连接截止阀(34)进口、截止阀(29)进口,截止阀(34)出口连接大气排空。
6.一种根据权利要求1-5任意一项权利要求中的低温精馏富集低丰度18O同位素的装置的使用方法为:
1).本发明装置启动前,所有阀门均关闭,系统启动前需用0.3~0.4MPa的常温氮气吹扫系统管路1~2h,然后系统抽真空至2Pa以下,系统仪电控检测完毕后,本发明装置启动前需要裸冷至液氧温区,启用前需通过辅助管路往精馏富集塔(7、12、17、21)灌注液氧;
2).启动外部冷源循环(26),外部冷媒通过主换热器(6)冷端(43、44)为整套装置提供冷源,打开截止阀(1),高压原料氧气进入杂质吸附塔(2),过滤原料氧气中的CO2、CO、CmHn等;过滤后原料氧气进入主换热器(6)热端(35、39),然后进入精馏富集塔(7),打开阀门(10),缓慢开启减压阀(5),减压过冷后液氧进入顶部冷凝器(8)冷端,冷凝精馏富集塔(7)顶部氧气,精馏富集塔(7)底部液氧减少由顶部冷凝液氧补充;
3).建立精馏富集塔(7)全回流工况,然后缓慢打开截止阀(9),精馏富集塔(7)底部液氧蒸发后进入精馏富集塔(12),打开阀门(15),缓慢开启减压阀(11),减压过冷后液氧进入顶部冷凝器(13)冷端,冷凝精馏富集塔(12)顶部氧气,精馏富集塔(12)底部液氧减少由顶部冷凝液氧补充;
4).建立精馏富集塔(12)全回流工况,然后缓慢打开截止阀(14),精馏富集塔(12)底部液氧蒸发后进入精馏富集塔(17),打开阀门(20),缓慢开启减压阀(16),减压过冷后液氧进入顶部冷凝器(18)冷端,冷凝精馏富集塔(17)顶部氧气,精馏富集塔(17)底部液氧减少由顶部冷凝液氧补充;
5).建立精馏富集塔(17)全回流工况,联动精馏富集塔(7、12、17),建立精馏平衡工况,直至精馏富集塔(17)底部液氧18O同位素丰度达标;
6).缓慢打开阀门(19),精馏富集塔(17)底部液氧经过顶部冷凝器(18)进入浓缩塔(21), 缓慢打开阀门 (30、31、32),精馏富集塔(7、12、17)顶部开始排气,精馏富集塔(7、12、17)顶部排气通过混合器(33)汇合,打开阀门(29),精馏富集塔(7、12、17)顶部排气进入再沸器(23)热端,作为浓缩塔(21)底部蒸发氧气热源,打开阀门(22),浓缩塔(21)顶部排气进入主换热器(6)冷端(42、38),打开阀门(27)、气动增压阀(3),复热后浓缩塔(21)顶部排气与原料氧气汇合;
7).当再沸器(23)提供热源不足时,可通过混合器(24)提供常温氧气,与精馏富集塔(7、12、17)顶部排气汇流,再沸器(23)热端出口氧气进入主换热器(6)冷端(40、36),复热后经过压缩机(28)压缩后回收, 浓缩塔(21)底部产品进入主换热器(6)冷端(41、37),复热后产品18O去产品充装系统。
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CN104474898A (zh) * | 2014-11-24 | 2015-04-01 | 上海化工研究院 | 生产高丰度13c的低温精馏多塔级联节能装置 |
JP2021041356A (ja) * | 2019-09-12 | 2021-03-18 | 大陽日酸株式会社 | 一酸化炭素安定同位体濃縮装置および一酸化炭素安定同位体装置の運転方法 |
CN111714912A (zh) * | 2020-05-09 | 2020-09-29 | 杭州制氧机集团股份有限公司 | 一种双同位素低温同步分离装置及分离方法 |
CN112569786A (zh) * | 2020-12-10 | 2021-03-30 | 中国工程物理研究院材料研究所 | 一种高效低成本的氢同位素氧化物分离工艺 |
CN216048687U (zh) * | 2021-04-09 | 2022-03-15 | 杭州制氧机集团股份有限公司 | 一种低温精馏富集低丰度18o同位素的装置 |
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