CN102430337A - A cryogenic rectification system for producing stable isotope 13C from CO - Google Patents

A cryogenic rectification system for producing stable isotope 13C from CO Download PDF

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CN102430337A
CN102430337A CN2011103553760A CN201110355376A CN102430337A CN 102430337 A CN102430337 A CN 102430337A CN 2011103553760 A CN2011103553760 A CN 2011103553760A CN 201110355376 A CN201110355376 A CN 201110355376A CN 102430337 A CN102430337 A CN 102430337A
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rectifying column
stable isotope
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许保云
李虎林
陈大昌
周建跃
李良君
杜晓宁
蔡扬
龙磊
吉永喆
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Shanghai Research Institute of Chemical Industry SRICI
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Abstract

本发明涉及一种由CO生产稳定同位素13C的低温精馏系统,该系统为水平放置的n级精馏塔组成的级联装置,其中,精馏塔由塔顶冷凝器、塔底再沸器和精馏柱组成,各级精馏塔之间经管道连接。与现有技术相比,本发明利用在水平级联各塔中设置提取段来减小级联各塔之间的物料输送流量,可确保级联装置长期、稳定、连续运转。

Figure 201110355376

The present invention relates to a cryogenic distillation system for producing stable isotope 13 C from CO, which is a cascade device composed of n-stage distillation towers placed horizontally, wherein the distillation towers are composed of a tower top condenser, a tower bottom reboiler and a distillation column, and each stage of the distillation towers is connected by pipelines. Compared with the prior art, the present invention reduces the material conveying flow rate between the cascade towers by arranging extraction sections in each tower of the horizontal cascade, thereby ensuring the long-term, stable and continuous operation of the cascade device.

Figure 201110355376

Description

一种由CO生产稳定同位素13C的低温精馏系统A cryogenic rectification system for producing stable isotope 13C from CO

技术领域 technical field

本发明涉及碳的稳定同位素分离技术,尤其是涉及一种采用低温精馏CO生产13C的低温精馏系统。The invention relates to a carbon stable isotope separation technology, in particular to a low-temperature rectification system for producing 13 C by low-temperature rectification of CO.

背景技术 Background technique

含碳化合物中,碳元素以稳定同位素12C、13C和放射性14C存在于自然界中,其中12C与13C的天然丰度比约为98.9∶1.1。随着科技的发展,13C作为示踪原子已经广泛应用于医学、药理学、生物化学和生命科学等领域。此外,高丰度的12C合成的金刚石比天然产品更好的物理性质也得到关注。In carbon-containing compounds, carbon exists in nature as stable isotopes 12 C, 13 C and radioactive 14 C, and the natural abundance ratio of 12 C to 13 C is about 98.9:1.1. With the development of science and technology, 13 C as a tracer atom has been widely used in the fields of medicine, pharmacology, biochemistry and life science. In addition, the better physical properties of high-abundance 12 C synthetic diamonds than natural products have also received attention.

现有技术中,已经有多种稳定同位素13C的生产方法,例如热扩散法、气体扩散法、化学交换法、低温精馏法、激光法等。其中低温精馏法是工业中生产13C的主要方法,但是由于同位素组分之间的蒸气压相差很小,获得高丰度的碳-13必须采用多塔级联操作。In the prior art, there are various production methods of stable isotope 13 C, such as thermal diffusion method, gas diffusion method, chemical exchange method, cryogenic rectification method, laser method and so on. Among them, cryogenic distillation is the main method for producing 13 C in industry, but because the vapor pressure difference between isotopic components is very small, multi-column cascade operation must be used to obtain high-abundance carbon-13.

早在1949年,英国Harwell原子能研究中心就建立了低温精馏CO分离13C的装置(T.F.Johns,H.London,enrichment of isotopes 13C and 18O,AERE Harwell reportG/R 661,1951),该装置由垂直连接的两座塔构成,全长32ft,产品中13C丰度为60%,产率为0.4g13C/d。As early as 1949, the British Harwell Atomic Energy Research Center established a device for the separation of 13 C by cryogenic rectification of CO (TFJohns, H.London, enrichment of isotopes 13 C and 18 O, AERE Harwell report G/R 661, 1951). Consisting of two vertically connected towers with a total length of 32ft, the abundance of 13 C in the product is 60%, and the yield is 0.4g 13 C/d.

前苏联梯比利斯实验室(П.Я.Асаmuанu,B.A.

Figure BDA0000107313330000011
,Е.Л.
Figure BDA0000107313330000012
,et al.,Получение изотоnа C13 метолом ректификации окиси уrлерола,Isotopenpraxis,4.Jahrgang,Heft 7,1968,275-277)建造的CO低温精馏装置由三座塔构成,该装置全长36m,第一级塔径为4.3cm、高15m,第二级塔径为2.0cm、高10m,第三级塔径为1.0cm、高11m,三塔垂直连接。塔内装填三角螺旋圈填料,保温形式为真空绝热,产品中13C丰度为60%。Former Soviet Union Tbilisi Laboratory (П.Я.Асаmuанu, BA
Figure BDA0000107313330000011
, E.L.
Figure BDA0000107313330000012
, et al., Получение изотоnа C 13 метолом ректификации окиси уrлерола, Isotopenpraxis, 4. Jahrgang, Heft 7, 1968, 275-277) built a CO cryogenic rectification device consisting of three towers. The diameter of the first-stage tower is 4.3cm, and the height is 15m. The diameter of the second-stage tower is 2.0cm, and the height is 10m. The diameter of the third-stage tower is 1.0cm, and the height is 11m. The three towers are connected vertically. The tower is filled with triangular spiral packing, and the heat preservation form is vacuum insulation, and the 13 C abundance in the product is 60%.

1969年7月,美国Los Alamos实验室建成一套CO低温精馏装置(D.E.Armstrong,A.C.Briesmeister,B.B.Mclnteer,et a1.,A carbon-13 production plantusing carbon monoxide distillation,LASL report,LA-4391,1970),是当时规模最大的CO低温精馏装置,该装置由垂直串联起来的七段塔组成,一起放入直径为15.24cm的真空夹套中,再用聚苯乙烯泡沫塑料以及40层铝合金Mylar薄膜绝热,最后放入直径0.9144米、深38.1米的地穴中。该装置经过6个星期的平衡期,获得13C丰度为92.37%的产品。该装置后被1979年建成的8kg/a的13C装置代替(B.B.Mclnteer,isotope separation by distillation:design of a carbon-13 plant,separationscience and technology,vol.15,No.3,1980,491-508),即Cola-Colita装置,Cola-Colita装置的主塔由垂直串联连接的两段塔及同位素转化反应器和精馏副塔组成,其中第一段为长100米的6根塔,第二段为长100米的1根塔,精馏副塔长55米。In July 1969, Los Alamos Laboratory in the United States built a CO cryogenic distillation unit (DEArmstrong, AC Briesmeister, BBMclnteer, et a1., A carbon-13 production plant using carbon monoxide distillation, LASL report, LA-4391, 1970), is The largest CO low-temperature rectification device at that time, the device was composed of seven-section towers connected vertically in series, put together in a vacuum jacket with a diameter of 15.24 cm, and then insulated with polystyrene foam and 40 layers of aluminum alloy Mylar film , and finally placed in a crypt with a diameter of 0.9144 meters and a depth of 38.1 meters. After 6 weeks of equilibration, the device obtained a product with 13 C abundance of 92.37%. This device was replaced by the 8kg/a 13 C device built in 1979 (BBMclnteer, isotope separation by distillation: design of a carbon-13 plant, separationscience and technology, vol.15, No.3, 1980, 491-508) , that is, the Cola-Colita unit. The main column of the Cola-Colita unit consists of two vertically connected columns, an isotope conversion reactor and a sub-column for rectification. The first section is 6 columns with a length of 100 meters. It is a tower with a length of 100 meters, and the sub-column for rectification is 55 meters long.

1999年,俄罗斯人杨.格.柴列万西克(杨.格.柴列万西克,阿.勃.哈劳西劳夫,低温精馏碳氧化物制备稳定同位素,Хим.пром.1999,No.4,229-235)设计了一套采用CO低温精馏分离13C的四塔级联装置,四座塔采用水平连接的方式,原料加入到第一级塔的塔釜,第2~4级塔全部为浓缩段,四座塔采用等高设计,塔内填料的高度均为20米。前级塔塔底的气体物料通过压力的推动自动流动至后级塔顶部的冷凝器中,冷凝后从冷凝器底部流到后级塔顶部,作为后级塔的喷淋液体,后级塔的蒸气从顶部流出,经过鼓风机输送至前级塔的底部,实现级联之间的物料流动。该流程降低了对场地的要求,但增加了级间物料的动力输送设备。In 1999, Russian Yang. Ge. Chalevansik (Yang. Ge. Chalevansik, A. Bo. Harausilauf, low-temperature rectification of carbon oxides to prepare stable isotopes, Хим.пром.1999 , No.4, 229-235) designed a set of four-tower cascade device using low-temperature distillation of CO to separate 13 C. The four towers are connected horizontally, and the raw materials are added to the bottom of the first-stage tower, and the second to second The 4th stage towers are all enrichment sections, the four towers adopt the same height design, and the height of the packing in the towers is 20 meters. The gas material at the bottom of the former tower automatically flows to the condenser at the top of the latter tower through pressure, and flows from the bottom of the condenser to the top of the latter tower after being condensed as the spray liquid of the latter tower. The steam flows out from the top and is transported to the bottom of the front tower through the blower to realize the material flow between the cascades. This process reduces the requirements on the site, but increases the power conveying equipment for interstage materials.

综合以上文献可知,采用CO低温精馏法浓缩13C需要进行多塔级联操作,现有技术中,级联装置有垂直级联和水平级联两种连接方式。垂直级联中,前级塔的液体依靠重力进入后级塔,后级塔的蒸汽依靠压力进入前级塔,容易实现级联各塔之间的物料输送。但是由于同位素分离过程需要的理论板数很多,造成塔设备很高,因此,施工难度比较大;另外,由于级联装置的压降比较大,降低系统的分离系数,对分离不利。相比较之下,水平级联的施工难度小得多,但是,在现有技术的n级水平级联装置中,第2~n级精馏塔塔顶进料、出料维持液相和气相的浓度相差一个α的差值,因此级联各塔间的物料流量很大,一方面造成输送设备的能耗比较大,另一方面,这种级联装置对自动控制、仪器仪表的要求比较高,并要求每级必须连续、稳定运转,任何一级塔出现事故,都会造成级联装置不好衔接。Based on the above documents, it can be seen that the concentration of 13 C by CO cryogenic rectification requires multi-tower cascade operation. In the prior art, cascade devices have two connection modes: vertical cascade and horizontal cascade. In the vertical cascade, the liquid in the first stage tower enters the rear stage tower by gravity, and the steam in the latter stage tower enters the front stage tower by pressure, so it is easy to realize the material transportation between the cascaded towers. However, due to the large number of theoretical plates required in the isotope separation process, the tower equipment is very high, so the construction is relatively difficult; in addition, due to the relatively large pressure drop of the cascade device, the separation coefficient of the system is reduced, which is not good for separation. In comparison, the construction difficulty of the horizontal cascade is much less, but, in the n-level horizontal cascade device of the prior art, the top feed and output of the 2nd to n-stage rectification towers maintain the liquid phase and the gas phase Therefore, the material flow rate between the cascaded towers is very large. On the one hand, the energy consumption of the conveying equipment is relatively large. On the other hand, this cascade device has relatively high requirements for automatic control and instrumentation. High, and requires continuous and stable operation of each stage. An accident in any stage of the tower will cause poor connection of the cascade device.

发明内容 Contents of the invention

本发明的目的就是为了克服上述现有技术存在的缺陷而提供一种低温精馏CO生产稳定同位素13C的水平级联系统,该系统可确保同位素组分间具有比较高的分离系数,且容易实现低温精馏系统长期、稳定的运行。The purpose of the present invention is to provide a horizontal cascade system for producing stable isotope 13 C by low-temperature rectification CO in order to overcome the above-mentioned defects in the prior art. Realize the long-term and stable operation of the cryogenic rectification system.

本发明的目的可以通过以下技术方案来实现:The purpose of the present invention can be achieved through the following technical solutions:

一种由CO生产稳定同位素13C的低温精馏系统,为水平放置的n级精馏塔组成的级联装置,其中,所述精馏塔由塔顶冷凝器、塔底再沸器和精馏柱组成,各级精馏塔之间经管道连接。A low-temperature rectification system for producing stable isotope 13 C from CO, which is a cascade device composed of n-stage rectification towers placed horizontally, wherein the rectification tower consists of a top condenser, a bottom reboiler and a rectification tower. The distillation columns are composed of distillation columns, and the distillation columns at all levels are connected by pipelines.

所述的n级精馏塔的直径逐渐变细。The diameter of the n-stage rectification tower gradually becomes smaller.

所述的n级精馏塔为2~10级精馏塔。The n-stage rectification tower is a 2-10-stage rectification tower.

第一级精馏塔可以从中部或塔顶输入原料。The first-stage distillation column can input raw materials from the middle or the top of the column.

所述的级联装置中后级精馏塔塔顶的蒸气由气体输送泵经管道输送到前级精馏塔的塔中部,前级精馏塔的塔釜产生的液体在管道中汽化后在压力作用下输送到后级精馏塔的中部。In the cascading device, the steam at the top of the rectifying tower in the rear stage is transported to the middle part of the rectifying tower in the preceding stage through a pipeline by the gas delivery pump, and the liquid produced in the bottom of the rectifying tower in the preceding stage is vaporized in the pipeline Under the action of pressure, it is transported to the middle part of the rear stage rectification tower.

所述的后级精馏塔塔顶的蒸气可以返回到前级精馏塔的进料点位置。The steam at the top of the rear stage rectification tower can be returned to the feeding point of the front stage rectification tower.

所述的后级精馏塔塔顶的蒸气可以返回到比前级精馏塔的进料点位置高的位置。The steam at the top of the rear stage rectification tower can be returned to a position higher than the feed point of the front stage rectification tower.

所述的后级精馏塔塔顶的蒸气可以返回到比前级精馏塔的进料点位置低的位置。The steam at the top of the rear-stage rectification tower can be returned to a position lower than the feeding point of the front-stage rectification tower.

所述的气体输送泵可以是气体增压泵、鼓风机、屏蔽电泵、隔膜泵或磁力驱动泵。The gas delivery pump can be a gas booster pump, a blower, a canned electric pump, a diaphragm pump or a magnetic drive pump.

所述的精馏塔内填充有分离填料。The rectification tower is filled with separation packing.

所述的分离填料为金属板波纹规整填料、金属丝网规整填料、金属网孔波纹填料、栅格填料或脉冲填料。The separation packing is metal plate corrugated structured packing, wire mesh structured packing, metal mesh corrugated packing, grid packing or pulse packing.

与现有技术相比,本发明利用在水平级联各塔中设置提取段来减小级联各塔之间的物料输送流量,可确保级联装置长期、稳定、连续运转。Compared with the prior art, the present invention utilizes the arrangement of extraction sections in each horizontal cascading tower to reduce the material delivery flow between each cascading tower, which can ensure long-term, stable and continuous operation of the cascading device.

附图说明 Description of drawings

图1为本发明的级联系统示意图;Fig. 1 is the cascade system schematic diagram of the present invention;

图2为实施例1的流程示意图;Fig. 2 is the schematic flow sheet of embodiment 1;

图3为实施例1中级联精馏塔内各同位素组分的浓度分布图;Fig. 3 is the concentration distribution diagram of each isotope component in the cascaded rectification column in embodiment 1;

图4为实施例2的流程示意图;Fig. 4 is the schematic flow sheet of embodiment 2;

图5为实施例2中级联精馏塔内各同位素组分的浓度分布图。Fig. 5 is a concentration distribution diagram of each isotopic component in the cascaded rectification column in Example 2.

具体实施方式 Detailed ways

下面结合附图和具体实施例对本发明进行详细说明。The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.

图1为本发明的由n级精馏塔组成的低温精馏系统的流程示意图,该系统是由n级水平连接的精馏塔构成的级联装置。本发明中的级联装置中,各级塔是这样连接的:原料加入级联装置的第一级精馏塔的中部,第1级塔塔顶采出部分低丰度的13CO气体,第1~第n-1级塔再沸器气化的一部分蒸气经计量后在压力作用下分别进入第2~第n级精馏塔的中部,第2~第n级精馏塔塔顶的部分蒸气经气体输送泵分别输送至第1~第n-1级精馏塔的中部,第n级塔的再沸器气化的蒸气一部分进入精馏塔内与塔顶冷凝器下来的液体进行气、液传质,一部分高丰度的13CO气体作为产品离开级联装置。Fig. 1 is the schematic flow chart of the cryogenic rectification system composed of n-stage rectification towers of the present invention, the system is a cascade device composed of n-stage horizontally connected rectification towers. In the cascade device in the present invention, the towers at all levels are connected in this way: raw materials are added to the middle part of the first-stage rectification tower of the cascade device, part of the low-abundance 13 CO gas is extracted from the top of the first-stage tower, and the second-stage Part of the steam vaporized by the reboiler of the 1st to n-1st stage towers is metered and then enters the middle part of the 2nd to nth stage rectification towers and the top part of the 2nd to nth stage rectification towers under the action of pressure The steam is transported to the middle of the 1st to n-1th stage rectification towers respectively through the gas delivery pump, and part of the steam vaporized by the reboiler of the nth stage tower enters the rectification tower to be vaporized with the liquid coming down from the top condenser. , liquid mass transfer, a part of high-abundance 13 CO gas leaves the cascade device as a product.

第1级~第n级精馏塔的塔顶分别连接冷凝器C1~Cn,每个冷凝器均连接与本级精馏塔连通的气体管道、液体管道,和向前一级精馏塔输送物料的管道,此外,每个冷凝器还具有供冷凝介质进、出的管道。The tower tops of the first-stage to n-stage rectification towers are respectively connected to condensers C1 to Cn, and each condenser is connected to the gas pipeline and liquid pipeline connected to the rectification tower of this stage, and to the rectification tower of the previous stage. In addition, each condenser also has a pipeline for the condensing medium to enter and exit.

塔顶冷凝器C1~Cn可以是盘管式换热器、列管式换热器、套管式换热器、板片式换热器、螺旋板式换热器、板翅式换热器等,优选板翅式换热器。The top condensers C1~Cn can be coil heat exchangers, shell and tube heat exchangers, casing heat exchangers, plate heat exchangers, spiral plate heat exchangers, plate-fin heat exchangers, etc. , preferably a plate-fin heat exchanger.

图1所示的级联装置中,第1~第n级精馏塔塔内装填高比表面积的规整填料,其类型可以是板波纹填料、栅格填料、丝网波纹规整填料、脉冲填料等,优选孔板波纹填料和丝网波纹填料。In the cascade device shown in Figure 1, structured packing with high specific surface area is filled in the 1st to nth stages of rectification column, and its type can be plate corrugated packing, grid packing, wire mesh corrugated structured packing, pulse packing, etc. , preferably orifice corrugated packing and wire mesh corrugated packing.

第1级~第n级精馏塔的塔底分别连接再沸器B1~Bn,每个再沸器均连接与本级精馏塔连通的气体管道、液体管道,和向后级精馏塔输送物料的管道。The tower bottoms of the first to nth stages of rectification towers are respectively connected to reboilers B1 to Bn, and each reboiler is connected to the gas pipeline and liquid pipeline connected to the rectification tower of this stage, and to the rectification tower of the next stage Pipelines for transporting materials.

后级塔塔顶物料经气体输送泵输送至前级塔的中部,其中所述气体输送泵可以是气体增压泵、鼓风机、屏蔽电泵、隔膜泵、磁力驱动泵等,优选隔膜泵。The material at the top of the rear tower is transported to the middle of the front tower through the gas delivery pump, wherein the gas delivery pump can be a gas booster pump, a blower, a shielded electric pump, a diaphragm pump, a magnetic drive pump, etc., preferably a diaphragm pump.

参照图1,CO原料经由流量计F1计量后由管线L3输送至第一级塔T1的中部,T1塔内装填分离填料,为塔顶冷凝器C1中冷凝回流的液体与塔底再沸器B1中汽化的蒸气提供传热、传质的表面,从T1塔顶经由管线L2取出高丰度的碳-12。从T1塔釜取出一部分蒸气,在压力的驱动下经由阀V1与流量计F2计量后沿管线L4输送到塔T2的中部,T2塔内装填分离填料,为塔顶冷凝器C2中冷凝回流的液体与塔底再沸器B2中汽化的蒸气提供传热、传质的表面,从T2塔顶取出一部分蒸气,由气体输送泵P1沿管线L5输送到塔T1的中部。从T2塔釜取出一部分蒸气,在压力的驱动下经由阀V2与流量计F3计量后沿管线L6输送到塔T3的中部,T3塔内装填分离填料,为塔顶冷凝器C3中冷凝回流的液体与塔底再沸器B3中汽化的蒸气提供传热、传质的表面,从T3塔顶取出一部分蒸气,由气体输送泵P2沿管线L7输送到塔T2的中部。类似地,第四塔T4、第五塔T5直到第n塔Tn,均采用这样的连接方式。在第n塔Tn的塔釜采出高丰度的碳-13产品。Referring to Figure 1, the CO raw material is measured by the flow meter F1 and then transported to the middle of the first-stage tower T1 by the pipeline L3. The T1 tower is filled with separation packing, which is the liquid condensed and refluxed in the top condenser C1 and the bottom reboiler B1 The steam evaporated in the medium provides a surface for heat transfer and mass transfer, and high-abundance carbon-12 is taken out from the top of the T1 column through the line L2. A part of the steam is taken out from the T1 tower kettle, driven by the pressure, it is measured by the valve V1 and the flow meter F2, and then transported to the middle of the tower T2 along the pipeline L4, and the T2 tower is filled with separation packing, which is the liquid condensed and refluxed in the top condenser C2 The steam vaporized in the bottom reboiler B2 provides a surface for heat and mass transfer, and a part of the steam is taken from the top of the T2 column, and is transported to the middle of the column T1 by the gas delivery pump P1 along the line L5. A part of the steam is taken out from the T2 tower kettle, driven by the pressure, it is measured by the valve V2 and the flow meter F3, and then transported to the middle of the tower T3 along the pipeline L6. The T3 tower is filled with separation packing, which is the liquid condensed and refluxed in the top condenser C3. The steam vaporized in the bottom reboiler B3 provides a surface for heat transfer and mass transfer, and a part of the steam is taken from the top of the T3 column, and is transported to the middle of the column T2 by the gas delivery pump P2 along the line L7. Similarly, the fourth tower T4, the fifth tower T5 up to the nth tower Tn all adopt such a connection method. A high-abundance carbon-13 product is extracted from the bottom of the nth tower Tn.

整个级联装置中,各级塔塔顶压力相同,级联各塔之间传输的物料均为气体,前级塔塔釜物料在压力作用下输送到后级塔的中部,后级塔塔顶蒸气由气体输送泵输送到前一级塔的中部,这种级联方式可确保级联装置的连续、稳定的操作,且由于各塔等压操作,同位素组分间的分离系数也比较高。In the whole cascading device, the pressure at the top of the towers at each level is the same, and the materials transmitted between the cascading towers are all gases. The steam is transported to the middle of the previous column by the gas transport pump. This cascading method can ensure the continuous and stable operation of the cascade device, and due to the equal pressure operation of each column, the separation coefficient between isotopic components is also relatively high.

此外,本发明中还提供了使用以上低温精馏系统分离富集13C时,级联装置内的各同位素组分的丰度分布的计算机模拟结果。本发明中,使用精馏理论进行级联装置的设计和优化,考虑到体系中氧同位素的影响,计算过程中考察天然丰度比较高的12C16O、13C16O和12C18O三种组分。根据同位素分离级联理论和精密精馏理论设计本发明中提出的低温精馏级联装置,也可以获得类似的结果。In addition, the present invention also provides computer simulation results of the abundance distribution of each isotopic component in the cascade device when using the above cryogenic rectification system to separate and enrich 13 C. In the present invention, the rectification theory is used to design and optimize the cascade device. Considering the influence of oxygen isotopes in the system, 12 C 16 O, 13 C 16 O and 12 C 18 O with relatively high natural abundance are considered during the calculation process. three components. Similar results can also be obtained by designing the cryogenic rectification cascade device proposed in the present invention according to the isotope separation cascade theory and precision rectification theory.

下面结合实施例对本发明作进一步的阐述。The present invention will be further elaborated below in conjunction with embodiment.

实施例1Example 1

实施例1中的级联装置由4级精馏塔组成,级联装置的工艺流程简图如图2所示。CO原料经流量计F1计量后由管线L3输送至第一级塔T1的中部,T1塔内装填金属丝网波纹填料,为塔顶冷凝器C1中冷凝回流的液体与塔底再沸器B1中汽化的蒸气提供传热、传质的表面。从T1塔顶经由管线L2取出高丰度的碳-12,从T1塔釜取出一部分蒸气,在压力的驱动下经由阀V1与流量计F2计量后沿管线L4输送到塔T2的中部。T2塔内装填金属丝网波纹填料,为塔顶冷凝器C2中冷凝回流的液体与塔底再沸器B2中汽化的蒸气提供传热、传质的表面。从T2塔顶取出一部分蒸气,由隔膜泵P1沿管线L5输送到塔T1的中部,与天然丰度的原料一起加入到塔T1中,从T2塔釜取出一部分蒸气,在压力的驱动下经由阀V2与流量计F3计量后沿管线L6输送到塔T3的中部。T3塔内装填金属丝网波纹填料,为塔顶冷凝器C3中冷凝回流的液体与塔底再沸器B3中汽化的蒸气提供传热、传质的表面。从T3塔顶取出一部分蒸气,由隔膜泵P2沿管线L7输送到塔T2的中部,其中管线L7与管线L4在同一位置与塔T2连接,从T3塔釜取出一部分蒸气,在压力的驱动下经由阀V3与流量计F4计量后沿管线L8输送到塔T4的中部。T4塔内装填金属丝网波纹填料,为塔顶冷凝器C4中冷凝回流的液体与塔底再沸器B4中汽化的蒸气提供传热、传质的表面。从T4塔顶取出一部分蒸气,由隔膜泵P3沿管线L9输送到塔T3的中部,其中管线L6与管线L9在同一位置与塔T3连接,在第4塔T4的塔釜B4采出高丰度的碳-13产品。The cascade device in Example 1 is composed of 4 stages of rectification towers, and the schematic flow chart of the cascade device is shown in Figure 2. The CO raw material is measured by the flow meter F1 and transported to the middle of the first stage tower T1 by the pipeline L3. The T1 tower is filled with metal mesh corrugated packing, which is the liquid condensed and refluxed in the top condenser C1 and the bottom reboiler B1. The vaporized vapor provides a surface for heat and mass transfer. The high-abundance carbon-12 is taken out from the top of the T1 tower through the pipeline L2, and a part of the steam is taken out from the bottom of the T1 tower. Driven by the pressure, it is metered through the valve V1 and the flow meter F2 and then sent to the middle of the tower T2 along the pipeline L4. The T2 column is filled with wire mesh corrugated packing to provide heat and mass transfer surfaces for the liquid condensed and refluxed in the top condenser C2 and the vaporized vapor in the bottom reboiler B2. A part of the steam is taken out from the top of the T2 tower, and is transported to the middle of the tower T1 by the diaphragm pump P1 along the pipeline L5, and is added to the tower T1 together with the raw material of natural abundance, and a part of the steam is taken out from the bottom of the T2 tower, driven by the pressure through the valve V2 is measured by flowmeter F3 and transported to the middle of tower T3 along pipeline L6. The T3 column is filled with wire mesh corrugated packing to provide heat and mass transfer surfaces for the liquid condensed and refluxed in the top condenser C3 and the evaporated vapor in the bottom reboiler B3. A part of the steam is taken from the top of the T3 tower, and is transported to the middle of the tower T2 by the diaphragm pump P2 along the pipeline L7, where the pipeline L7 and the pipeline L4 are connected to the tower T2 at the same position, and a part of the steam is taken out from the bottom of the T3 tower, driven by the pressure through After metering by valve V3 and flowmeter F4, it is transported to the middle of tower T4 along pipeline L8. The T4 column is filled with wire mesh corrugated packing to provide heat and mass transfer surfaces for the liquid condensed and refluxed in the top condenser C4 and the vaporized vapor in the bottom reboiler B4. A part of steam is taken from the top of T4 tower, and is transported to the middle of tower T3 by diaphragm pump P3 along pipeline L9, wherein pipeline L6 and pipeline L9 are connected to tower T3 at the same position, and the high-abundance steam is extracted from the tower still B4 of the fourth tower T4 carbon-13 products.

实施例1中,原料为碳-13丰度为1.1%的天然CO,经过四级塔的分离后,碳-13富集到90%,表1是年产净13C 100kg、丰度为90%的级联装置的工艺参数,级联各塔内的同位素丰度分布如图3所示。In Example 1, the raw material is natural CO with a carbon-13 abundance of 1.1%. After separation in a four-stage tower, carbon-13 is enriched to 90%. Table 1 shows the annual net 13 C 100kg with an abundance of 90 The process parameters of the cascade device, and the isotope abundance distribution in each column of the cascade are shown in Figure 3.

表1实施例1中年产100kg碳-13的四级联装置的工艺参数The process parameters of the four-cascade device with an annual output of 100kg carbon-13 in the embodiment 1 of table 1

Figure BDA0000107313330000061
Figure BDA0000107313330000061

从表1中的数据可以看出,后级塔返回到前级塔的物料量远远低于后级塔塔底再沸器内汽化的物料量,降低了级联各塔间连接管路内的滞料量,且中间级联塔出现问题时,可以进行单塔全回流操作,待问题解决后再将级联装置连起来,级联装置可以很快恢复操作。由于各级塔塔顶压力相同,同位素组分间具有比较高的分离系数。It can be seen from the data in Table 1 that the amount of material returned to the front tower by the latter stage tower is far lower than the amount of vaporized material in the bottom reboiler of the latter stage tower, which reduces the amount of material in the connecting pipeline between cascaded towers. When there is a problem with the intermediate cascade tower, the full reflux operation of the single tower can be carried out. After the problem is solved, the cascade device can be connected again, and the cascade device can quickly resume operation. Due to the same pressure at the top of each column, the isotopic components have a relatively high separation factor.

实施例2Example 2

实施例2中的级联装置由4级精馏塔组成,级联装置的工艺流程简图如图4所示。CO原料经由流量计F1计量后由管线L3输送至第一级塔T1的中部,T1塔内装填金属丝网波纹填料,为塔顶冷凝器C1中冷凝回流的液体与塔底再沸器B1中汽化的蒸气提供传热、传质的表面。从T1塔顶经由管线L2取出高丰度的碳-12,从T1塔釜取出一部分蒸气,在压力的驱动下经由阀V1与流量计F2计量后沿管线L4输送到塔T2的中部(图4中点d位置)。T2塔内装填金属丝网波纹填料,为塔顶冷凝器C2中冷凝回流的液体与塔底再沸器B2中汽化的蒸气提供传热、传质的表面。从T2塔顶取出一部分蒸气,由隔膜泵P1沿管线L5输送到塔T1的中部偏下的位置(图4中点a位置)。从T2塔釜取出一部分蒸气,在压力的驱动下经由阀V2与流量计F3计量后沿管线L6输送到塔T3的中部(图4中点h位置)。T3塔内装填金属丝网波纹填料,为塔顶冷凝器C3中冷凝回流的液体与塔底再沸器B3中汽化的蒸气提供传热、传质的表面。从T3塔顶取出一部分蒸气,由隔膜泵P2沿管线L7输送到塔T2的中部偏下的位置(图4中点e位置),从T3塔釜取出一部分蒸气,在压力的驱动下经由阀V3与流量计F4计量后沿管线L8输送到塔T4的中部(图4中点1位置)。T4塔内装填金属丝网波纹填料,为塔顶冷凝器C4中冷凝回流的液体与塔底再沸器B4中汽化的蒸气提供传热、传质的表面。从T4塔顶取出一部分蒸气,由隔膜泵P3沿管线L9输送到塔T3的中部偏下的位置(图4中点i位置),在第4塔T4的塔釜采出高丰度的碳-13产品。The cascade device in Example 2 is composed of 4 stages of rectification towers, and the schematic flow chart of the cascade device is shown in Figure 4. The CO raw material is measured by the flow meter F1 and then transported to the middle of the first stage tower T1 by the pipeline L3. The T1 tower is filled with corrugated wire mesh packing, which is the liquid condensed and refluxed in the top condenser C1 and the bottom reboiler B1. The vaporized vapor provides a surface for heat and mass transfer. The high-abundance carbon-12 is taken out from the top of the T1 tower through the pipeline L2, and a part of the steam is taken out from the bottom of the T1 tower, which is metered by the valve V1 and the flow meter F2 under the drive of the pressure and then transported to the middle of the tower T2 along the pipeline L4 (Fig. 4 Midpoint d position). The T2 column is filled with wire mesh corrugated packing to provide heat and mass transfer surfaces for the liquid condensed and refluxed in the top condenser C2 and the vaporized vapor in the bottom reboiler B2. A part of the steam is taken from the top of the T2 tower, and is transported by the diaphragm pump P1 along the pipeline L5 to the lower part of the middle of the tower T1 (point a in Figure 4). A part of the steam is taken out from the bottom of the T2 column, driven by the pressure, it is metered through the valve V2 and the flow meter F3, and then sent to the middle of the column T3 along the pipeline L6 (point h in Figure 4). The T3 column is filled with wire mesh corrugated packing to provide heat and mass transfer surfaces for the liquid condensed and refluxed in the top condenser C3 and the evaporated vapor in the bottom reboiler B3. A part of the steam is taken from the top of the T3 tower, and is transported by the diaphragm pump P2 along the pipeline L7 to the lower part of the middle of the tower T2 (point e position in Figure 4), and a part of the steam is taken out from the bottom of the T3 tower, driven by the pressure through the valve V3 After metering with the flow meter F4, it is transported to the middle of the tower T4 along the pipeline L8 (point 1 position in Figure 4). The T4 column is filled with wire mesh corrugated packing to provide heat and mass transfer surfaces for the liquid condensed and refluxed in the top condenser C4 and the vaporized vapor in the bottom reboiler B4. A part of the steam is taken from the top of the T4 tower, and is transported by the diaphragm pump P3 along the pipeline L9 to the position lower in the middle of the tower T3 (point i position in Figure 4), and the high-abundance carbon is produced in the bottom of the fourth tower T4- 13 products.

实施例2中,原料为碳-13丰度为1.1%的天然CO,经过四级塔的分离后,碳-13富集到90%,表1是年产100kg、丰度为90%的净碳-13的级联装置的工艺参数,级联各塔内的同位素丰度分布如图5所示。In Example 2, the raw material is natural CO with a carbon-13 abundance of 1.1%. After the separation of the four-stage tower, the carbon-13 is enriched to 90%. Table 1 is the net CO with an annual output of 100kg and an abundance of 90%. The process parameters of the carbon-13 cascade device and the isotope abundance distribution in each column of the cascade are shown in Fig. 5 .

表2实施例1中年产100kg碳-13的四级联装置的工艺参数The process parameters of the four-cascade device with an annual output of 100kg carbon-13 in the embodiment 1 of table 2

Figure BDA0000107313330000071
Figure BDA0000107313330000071

从表2中的数据可以看出,后级塔返回到前级塔的物料量远远低于后级塔塔底再沸器内汽化的物料量,降低了级联各塔间连接管路内的滞料量,且中间级联塔出现问题时,可以进行单塔全回流操作,待问题解决后再将级联装置连起来,级联装置可以很快恢复操作。由于各级塔塔顶压力相同,同位素组分间具有比较高的分离系数。As can be seen from the data in Table 2, the amount of material returned to the front tower by the latter stage tower is far lower than the amount of vaporized material in the reboiler at the bottom of the rear stage tower, which reduces the amount of material in the connecting pipeline between cascaded towers. When there is a problem with the intermediate cascade tower, the full reflux operation of the single tower can be carried out. After the problem is solved, the cascade device can be connected again, and the cascade device can quickly resume operation. Due to the same pressure at the top of each column, the isotopic components have a relatively high separation factor.

实施例3Example 3

一种由CO生产稳定同位素13C的低温精馏系统,为水平放置的2级直径逐渐变细精馏塔组成的级联装置,其中,精馏塔由塔顶冷凝器、塔底再沸器和精馏柱组成,各级精馏塔之间经管道连接。第一级精馏塔可以从中部输入原料。级联装置中后级精馏塔塔顶的蒸气由气体输送泵经管道输送到前级精馏塔的塔中部,前级精馏塔的塔釜产生的液体在管道中汽化后在压力作用下输送到后级精馏塔的中部。后级精馏塔塔顶的蒸气可以返回到前级精馏塔的进料点位置。使用的气体输送泵为气体增压泵,在精馏塔内填充有栅格填料作为分离填料。A low-temperature rectification system for the production of stable isotope 13 C from CO, which is a cascade device composed of two horizontal rectification towers with gradually tapered diameters, wherein the rectification tower consists of a top condenser and a bottom reboiler It is composed of a rectification column, and the rectification columns at all levels are connected by pipelines. The first-stage rectifying column can input raw materials from the middle. The steam at the top of the rectifying tower in the cascade device is transported by the gas delivery pump to the middle of the rectifying tower in the previous stage through the pipeline, and the liquid produced in the bottom of the rectifying tower in the preceding stage is vaporized in the pipeline and then under pressure It is sent to the middle part of the rear stage rectification tower. The vapor at the top of the rear stage rectification tower can be returned to the feeding point of the front stage rectification tower. The gas delivery pump used is a gas booster pump, and the rectification column is filled with grid packing as separation packing.

实施例4Example 4

一种由CO生产稳定同位素13C的低温精馏系统,为水平放置的10级直径逐渐变细精馏塔组成的级联装置,其中,精馏塔由塔顶冷凝器、塔底再沸器和精馏柱组成,各级精馏塔之间经管道连接。第一级精馏塔可以从塔顶输入原料。级联装置中后级精馏塔塔顶的蒸气由气体输送泵经管道输送到前级精馏塔的塔中部,前级精馏塔的塔釜产生的液体在管道中汽化后在压力作用下输送到后级精馏塔的中部。后级精馏塔塔顶的蒸气可以返回到前级精馏塔的进料点位置,也可以返回到比前级精馏塔的进料点位置高的位置,还可以返回到比前级精馏塔的进料点位置低的位置。使用的气体输送泵为鼓风机或磁力驱动泵。精馏塔内填充有属丝网规整填料、金属网孔波纹填料作为分离填料。A low-temperature rectification system for producing stable isotope 13 C from CO, which is a cascade device composed of 10 stages of horizontal rectification towers with gradually tapered diameters, wherein the rectification tower consists of a tower top condenser and a bottom reboiler It is composed of a rectification column, and the rectification columns at all levels are connected by pipelines. The first-stage rectification column can input raw materials from the top of the column. The steam at the top of the rectifying tower in the cascade device is transported by the gas delivery pump to the middle of the rectifying tower in the previous stage through the pipeline, and the liquid produced in the bottom of the rectifying tower in the preceding stage is vaporized in the pipeline and then under pressure It is sent to the middle part of the rear stage rectification tower. The vapor at the top of the rear stage rectification tower can be returned to the feed point position of the front stage rectification tower, or can be returned to a position higher than the feed point position of the front stage rectification tower, or can be returned to a position higher than that of the front stage rectification tower. The feed point of the distillation column is at a low position. The gas delivery pumps used are blower or magnetic drive pumps. The rectification column is filled with wire mesh structured packing and metal mesh corrugated packing as separation packing.

尽管结合具体的实施方案描述了本系统,本领域内熟练的技术人员可认识到在本发明权利要求的范围和精神内有各种其它的实施例。Although the system has been described in connection with specific embodiments, those skilled in the art will recognize various other embodiments within the scope and spirit of the invention as claimed.

Claims (11)

1. produce stable isotope by CO for one kind 13The low temperature distillation system of C is characterized in that, this system is the cascade unit that the n level rectifying column of horizontal positioned is formed, and wherein, said rectifying column is made up of overhead condenser, tower bottom reboiler and rectifying column, connects through pipeline between the rectifying columns at different levels.
2. according to claim 1 a kind of by CO production stable isotope 13The low temperature distillation system of C is characterized in that, the diameter of described n level rectifying column is tapered.
3. according to claim 1 and 2 a kind of by CO production stable isotope 13The low temperature distillation system of C is characterized in that, described n level rectifying column is 2~10 grades of rectifying columns.
4. according to claim 1 a kind of by CO production stable isotope 13The low temperature distillation system of C is characterized in that, first order rectifying column can be from the middle part or cat head input raw material.
5. according to claim 1 a kind of by CO production stable isotope 13The low temperature distillation system of C; It is characterized in that; The steam of back level rectifying column cat head is transported to the tower middle part of prime rectifying column by gas transfer pump through pipeline in the described cascade unit, is transported to the middle part of back grade rectifying column after the liquid that the tower still of prime rectifying column produces vaporize in pipeline under pressure.
6. according to claim 5 a kind of by CO production stable isotope 13The low temperature distillation system of C is characterized in that, the steam of described back level rectifying column cat head can turn back to the feed points position of prime rectifying column.
7. according to claim 5 a kind of by CO production stable isotope 13The low temperature distillation system of C is characterized in that, the steam of described back level rectifying column cat head can turn back to the position higher than the feed points position of prime rectifying column.
8. according to claim 5 a kind of by CO production stable isotope 13The low temperature distillation system of C is characterized in that, the steam of described back level rectifying column cat head can turn back to the position lower than the feed points position of prime rectifying column.
9. according to claim 5 a kind of by CO production stable isotope 13The low temperature distillation system of C is characterized in that, described gas transfer pump can be gas boosting pump, air blast, shielded electric pump, membrane pump or magnetic force driving pump.
10. according to claim 1 a kind of by CO production stable isotope 13The low temperature distillation system of C is characterized in that, is filled with separating filler in the described rectifying column.
11. it is according to claim 10 a kind of by CO production stable isotope 13The low temperature distillation system of C is characterized in that, described separating filler is metallic plate corrugated regular filler, woven wire structured packing, metal mesh opening ripple packing, grid packing or pulse filler.
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