WO2023125494A1 - 一种高效率超临界设备 - Google Patents

一种高效率超临界设备 Download PDF

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WO2023125494A1
WO2023125494A1 PCT/CN2022/142210 CN2022142210W WO2023125494A1 WO 2023125494 A1 WO2023125494 A1 WO 2023125494A1 CN 2022142210 W CN2022142210 W CN 2022142210W WO 2023125494 A1 WO2023125494 A1 WO 2023125494A1
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gas
carbon dioxide
liquid
liquid separator
filter
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PCT/CN2022/142210
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English (en)
French (fr)
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刘杰
刘根水
李青松
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江苏汉邦科技股份有限公司
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Publication of WO2023125494A1 publication Critical patent/WO2023125494A1/zh

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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/26—Selective adsorption, e.g. chromatography characterised by the separation mechanism
    • B01D15/40—Selective adsorption, e.g. chromatography characterised by the separation mechanism using supercritical fluid as mobile phase or eluent
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D15/00—Separating processes involving the treatment of liquids with solid sorbents; Apparatus therefor
    • B01D15/08—Selective adsorption, e.g. chromatography
    • B01D15/10—Selective adsorption, e.g. chromatography characterised by constructional or operational features
    • B01D15/16—Selective adsorption, e.g. chromatography characterised by constructional or operational features relating to the conditioning of the fluid carrier
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D5/00—Condensation of vapours; Recovering volatile solvents by condensation
    • B01D5/0057—Condensation of vapours; Recovering volatile solvents by condensation in combination with other processes
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/32—Control of physical parameters of the fluid carrier of pressure or speed
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/26—Conditioning of the fluid carrier; Flow patterns
    • G01N30/28—Control of physical parameters of the fluid carrier
    • G01N30/36—Control of physical parameters of the fluid carrier in high pressure liquid systems

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  • the invention relates to the technical field related to chromatography, in particular to a high-efficiency supercritical equipment.
  • Supercritical fluid chromatography uses a large amount of supercritical carbon dioxide instead of organic solvents as the mobile phase. Compared with ordinary liquid chromatography systems, it has the advantages of fast separation speed and environmental protection.
  • the laboratory-grade supercritical fluid chromatography has a small flow rate and the carbon dioxide consumption is not very large, but the industrial-grade supercritical fluid chromatography system consumes a lot of carbon dioxide. If it is discharged directly, it is necessary to frequently replenish the liquid carbon dioxide in the storage tank, supercritical fluid
  • the chromatographic system cannot meet the conditions of long-term uninterrupted operation of industrial-grade equipment. Therefore, in an industrial-grade supercritical fluid chromatography system, it is often considered to collect the emitted gaseous carbon dioxide and reuse it.
  • the current technical difficulty lies in how to obtain pure carbon dioxide in the component collection part of industrial-grade supercritical fluid chromatography.
  • the purpose of the present invention is to provide a kind of high-efficiency supercritical equipment, to solve the problems of the above-mentioned prior art, can obtain pure carbon dioxide in the collection part of industrial-grade supercritical fluid chromatographic components, solve the problem of industrial-grade supercritical fluid chromatographic system The consumption of carbon dioxide is large and cannot be recycled.
  • the present invention provides the following scheme:
  • the invention provides a high-efficiency supercritical device, which includes a gas-liquid separator and a carbon dioxide filter connected through pipelines, the gas-liquid separator is used to separate the gas-liquid mixture inside, and the gas passes through the gas-liquid separator The upper end of the liquid is collected through the lower end of the gas-liquid separator, and the separated gas is sent to the carbon dioxide filter, which is used to filter the gas, and the filtered carbon dioxide is passed through the supercritical fluid chromatography system. Reuse after cooling down in the freezer.
  • the heating machine also includes a heating machine, the heating machine is connected in series with a heat exchanger, and the gas-liquid mixture enters the gas-liquid separator after being heated by the heat exchanger;
  • Heat exchange medium the liquid heat exchange medium can be water, the heater provides hot water to the heat exchanger and the gas-liquid separator, and allows the hot water to circulate, and changes the temperature of the hot water after passing through the heat exchanger by controlling the temperature of the hot water at the outlet of the heater.
  • the temperature of the gas-liquid mixture, while the hot water is connected in series to control the temperature of the gas-liquid separator, changing the environment of the gas-liquid mixture during gas-liquid separation, adjusting the temperature for different processes can achieve different gas-liquid separation effects, and the heat exchanger will
  • the mixture of gaseous carbon dioxide and organic solvent at a lower temperature is heated to relieve the mist state of the gas-liquid mixture before gas-liquid separation, and to ensure the separation effect after entering the gas-liquid separator.
  • the gas-liquid separator is covered with a heating part, and the heating machine, the heat exchanger and the heating part are connected in series through pipelines.
  • the inside of the carbon dioxide filter is filled with tray packing, and the tray packing can filter and condense the residual organic solvent and sample in the gas after passing through the gas-liquid separator again to obtain pure gaseous carbon dioxide, To the supercritical fluid chromatography system for repeated use.
  • the carbon dioxide discharge port at the top of the carbon dioxide filter is connected to the refrigerator through a pipeline, and a temperature sensor is arranged at the pipeline between the carbon dioxide discharge port and the refrigerator, and the temperature sensor is connected to the refrigerator.
  • the control terminal of the heating machine is electrically connected, and the temperature sensor is used to detect the temperature of gaseous carbon dioxide after gas-liquid separation, and the temperature detected here is fed back to the heating machine, and the temperature of the heating machine is changed by setting different temperature sensor temperatures.
  • the temperature of the hot water is used to obtain a more suitable state in the gas-liquid separation process.
  • the liquid heat exchange medium is water.
  • the present invention solves the atomization state of the gas-liquid mixture by changing the temperature of the gas-liquid mixture before the gas-liquid separator; realizes that the temperature of the gas-liquid mixture is consistent with the internal temperature of the gas-liquid separator through hot water in series; Purify gaseous carbon dioxide to ensure the purity of carbon dioxide; through the feedback control of the temperature sensor, it can automatically adjust the ambient temperature of gas-liquid separation to ensure the effect of gas-liquid separation.
  • Fig. 1 is the structural representation of high-efficiency supercritical equipment of the present invention
  • 1 is the heater
  • 101 is the hot water outlet of the heater
  • 102 is the hot water return port of the heater
  • 2 is the heat exchanger
  • 3 is the gas-liquid separator
  • 4 is the carbon dioxide filter
  • 5 is the temperature sensor
  • 6 is the Gas-liquid mixture
  • 7 is a refrigerator.
  • the purpose of the present invention is to provide a kind of high-efficiency supercritical equipment, to solve the problems of the above-mentioned prior art, can obtain pure carbon dioxide in the collection part of industrial-grade supercritical fluid chromatographic components, solve the problem of industrial-grade supercritical fluid chromatographic system The consumption of carbon dioxide is large and cannot be recycled.
  • the present invention provides a high-efficiency supercritical equipment, as shown in FIG. 1 , including a heater 1 , a heat exchanger 2 , a gas-liquid separator 3 , a carbon dioxide filter 4 , and a temperature sensor 5 .
  • the heater 1 comprises a heater hot water outlet 101 and a heater hot water return port 102, the heater hot water outlet 101 is connected to the inlet of the heat exchanger 2 hot water with pipelines, and the outlet of the heat exchanger 2 hot water is pipelined Connect to the inlet of the hot water of the gas-liquid separator 3, and the outlet of the hot water of the gas-liquid separator 3 is connected to the hot water return port 102 of the heater with a pipeline, and the hot water of the heater 1 separates the heat exchanger 2 from the gas-liquid through the pipeline
  • the device 3 is connected in series to ensure that the temperature of the gas-liquid mixture is consistent with the temperature inside the gas-liquid separator.
  • the gas-liquid mixture 6 is connected to the inlet of the heat exchanger 2 through a pipeline, the outlet of the heat exchanger 2 is connected to the inlet of the gas-liquid separator 3 through a pipeline, and the carbon dioxide discharge port at the top of the gas-liquid separator 3 is connected to the carbon dioxide through a pipeline.
  • the inlet of the filter 4 and the carbon dioxide discharge outlet at the top of the carbon dioxide filter 4 are connected to the refrigerator 7 through a pipeline for recycling.
  • a temperature sensor 5 is set in the middle of this pipeline to measure the temperature of the carbon dioxide after gas-liquid separation, and the temperature sensor 5 detects
  • the carbon dioxide gas temperature can give real-time feedback on the gas-liquid separation effect, and feed back the signal to the heating machine 1 to automatically control the hot water temperature of the heating machine 1 to ensure a good effect of gas-liquid separation.
  • the supercritical fluid chromatography system is in the component collection stage, the supercritical carbon dioxide is depressurized and becomes gaseous. At this time, the mobile phase becomes a low-temperature gas-liquid mixture composed of gaseous carbon dioxide and a small amount of organic solvent, which is in the form of mist in the pipeline. Available in aerosol form.
  • the present invention heats the gas-liquid mixture 6 through the heat exchanger 2 before the gas-liquid mixture enters the gas-liquid separator 3 to alleviate the state of the misty aerosol, and at this time the gas-liquid mixture 6 is more easily separated from the gas-liquid.
  • gas-liquid separation is carried out, and a trace amount of organic solvent or sample will be mixed in the discharged carbon dioxide gas.
  • the carbon dioxide filter 4 connected at the back, when passing through the tray packing in the filter, a small amount of organic solvent or sample will gradually condense to form small droplets, which flow to the bottom along the inner wall of the carbon dioxide filter 4, and the liquid temporarily stores carbon dioxide
  • the valve at the bottom of the carbon dioxide filter 4 is controlled by software to discharge regularly. At this time, the gaseous carbon dioxide discharged from the top of the carbon dioxide filter 4 is purer and can be reused after being cooled by the refrigerator in the supercritical fluid chromatography system.

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  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Biochemistry (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Immunology (AREA)
  • Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Treatment Of Liquids With Adsorbents In General (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Separation By Low-Temperature Treatments (AREA)

Abstract

一种高效率超临界设备，包括通过管路连通的气液分离器（3）和二氧化碳过滤器（4），气液分离器（3）用于将气液混合物（6）分离，并将分离后的气体输送至二氧化碳过滤器（4），二氧化碳过滤器（4）用于将气体过滤，并将过滤后的二氧化碳通过超临界流体色谱系统中的制冷器（7）冷却后重复使用。

Description

一种高效率超临界设备 技术领域
本发明涉及色谱相关技术领域，特别是涉及一种高效率超临界设备。
背景技术
超临界流体色谱使用大量超临界态二氧化碳代替有机溶剂作为流动相，相比于普通的液相色谱系统，有着分离速度快、绿色环保等优势。实验室级超临界流体色谱仪流量小，二氧化碳消耗量不是很大，但是工业级超临界流体色谱系统二氧化碳消耗量非常大，如果直接排放，需要频繁的补充储罐中的液态二氧化碳，超临界流体色谱系统也不能满足工业级设备长时间不间断运行的条件。因此在工业级超临界流体色谱系统中，往往会考虑将排放的气态二氧化碳收集后再重复使用。目前技术难点在于如何能够在工业级超临界流体色谱组分收集部分得到纯净的二氧化碳。
发明内容
本发明的目的是提供一种高效率超临界设备，以解决上述现有技术存在的问题，能够在工业级超临界流体色谱组分收集部分得到纯净的二氧化碳，解决了工业级超临界流体色谱系统二氧化碳消耗量大，无法循环使用的问题。
为实现上述目的，本发明提供了如下方案：
本发明提供一种高效率超临界设备，包括通过管路连通的气液分离器和二氧化碳过滤器，所述气液分离器用于将气液混合物在内部进行气液分离，气体通过气液分离器的上端，液体通过气液分离器的下端进行收集，并将分离后的气体输送至二氧化碳过滤器，所述二氧化碳过滤器用于将气体过滤，并将过滤后的二氧化碳通过超临界流体色谱系统中的制冷器冷却后重复使用。
可选的，还包括加热机，所述加热机串行连接有换热器，所述气液混合物经所述换热器加热后进入所述气液分离器；所述加热机内设置有液态换热介质，液态换热介质可以采用水，加热机给换热器和气液分离器提供热水，并让热水循环流动，通过控制加热机出口热水的温度来改变经过换热器后的气液混合物的温度，同时热水串联对气液分离器控制温度，改变气液混合物在气液分 离时的环境，针对不同的工艺调整温度能够起到不同的气液分离效果，换热器将温度较低的气态二氧化碳和有机溶剂的混合物加热，在气液分离前缓解气液混合物的雾状的状态，保证进入气液分离器后的分离效果。
可选的，所述气液分离器外包覆有加热部，所述加热机、换热器和加热部通过管道串行连接。
可选的，所述二氧化碳过滤器内部装填有塔板填料，所述塔板填料能够将经过气液分离器后的气体中残留的有机溶剂和样品进行再次过滤和冷凝，得到纯净的气态二氧化碳，给超临界流体色谱系统进行重复使用。
可选的，所述二氧化碳过滤器顶端的二氧化碳排放口通过管路连接到所述制冷器，所述二氧化碳排放口与所述制冷器之间的管路处设置有温度传感器，所述温度传感器与所述加热机的控制端电连接，温度传感器用来检测经过气液分离后气态二氧化碳的温度，并将此处检测到的温度反馈给加热机，通过设定不同的温度传感器温度来改变加热机热水的温度，得到气液分离工艺中比较合适的状态。
可选的，所述液态换热介质为水。
本发明相对于现有技术取得了以下技术效果：
本发明通过对气液分离器前气液混合物温度的改变，解决了气液混合物雾化的状态；通过热水串联实现气液混合物的温度和气液分离器内部温度一致；通过使用二氧化碳过滤器进一步净化气态二氧化碳，保证二氧化碳纯度；通过温度传感器的反馈控制，能够自动调整气液分离的环境温度，保证气液分离效果。
附图说明
为了更清楚地说明本发明实施例或现有技术中的技术方案，下面将对实施例中所需要使用的附图作简单地介绍，显而易见地，下面描述中的附图仅仅是本发明的一些实施例，对于本领域普通技术人员来讲，在不付出创造性劳动的前提下，还可以根据这些附图获得其他的附图。
图1为本发明高效率超临界设备的结构示意图；
其中，1为加热机、101为加热机热水出口、102为加热机热水回流口、2 为换热器、3为气液分离器、4为二氧化碳过滤器、5为温度传感器、6为气液混合物、7为制冷器。
具体实施方式
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。基于本发明中的实施例，本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例，都属于本发明保护的范围。
本发明的目的是提供一种高效率超临界设备，以解决上述现有技术存在的问题，能够在工业级超临界流体色谱组分收集部分得到纯净的二氧化碳，解决了工业级超临界流体色谱系统二氧化碳消耗量大，无法循环使用的问题。
为使本发明的上述目的、特征和优点能够更加明显易懂，下面结合附图和具体实施方式对本发明作进一步详细的说明。
本发明提供一种高效率超临界设备，如图1所示，包括加热机1、换热器2、气液分离器3、二氧化碳过滤器4、温度传感器5。加热机1包括加热机热水出口101和加热机热水回流口102，加热机热水出口101用管路连接到换热器2热水的入口，换热器2热水的出口用管路连接到气液分离器3热水的入口，气液分离器3热水的出口用管路连接到加热机热水回流口102，加热机1热水通过管路将换热器2和气液分离器3串联，保证气液混合物的温度和气液分离器内部的温度一致。
气液混合物6通过管路连接到换热器2的入口，换热器2的出口通过管路连接到气液分离器3的入口，气液分离器3顶端二氧化碳排放口通过管路连接到二氧化碳过滤器4的入口，二氧化碳过滤器4顶端二氧化碳排放口通过管路连接到制冷器7进行循环使用，在此段管路中间设置温度传感器5测量气液分离后二氧化碳的温度，温度传感器5检测出的二氧化碳气体温度能够实时反馈气液分离效果，并通过信号反馈至加热机1，自动控制加热机1的热水温度，保证气液分离良好的效果。超临界流体色谱系统在组分收集阶段时，超临界态二氧化碳泄压变成气态，此时的流动相变成了气态二氧化碳和少量有机溶剂组成的低温气液混合物，在管路中是雾状气溶胶形式存在。
本发明在气液混合物进入气液分离器3前通过换热器2对气液混合物6进行加热处理，缓解雾状气溶胶的状态，此时气液混合物6更容易进行气液分离。在进入气液分离器3后进行气液分离，排放出的二氧化碳气体中会夹杂着微量的有机溶剂或样品。通过后面接入的二氧化碳过滤器4，在经过过滤器中的塔板填料时，微量的有机溶剂或样品会逐渐冷凝形成小液滴，顺着二氧化碳过滤器4内壁流至底部，液体暂存在二氧化碳过滤器4底部，通过软件控制二氧化碳过滤器4底部的阀门定期进行排放。此时二氧化碳过滤器4顶部排出的气态二氧化碳更为纯净，可以通过超临界流体色谱系统中的制冷器冷却后重复使用。
在本发明的描述中，需要说明的是，术语“中心”、“顶”、“底”、“左”、“右”、“竖直”、“水平”、“内”、“外”等指示的方位或位置关系为基于附图所示的方位或位置关系，仅是为了便于描述本发明和简化描述，而不是指示或暗示所指的装置或元件必须具有特定的方位、以特定的方位构造和操作，因此不能理解为对本发明的限制。此外，术语“第一”、“笫二”仅用于描述目的，而不能理解为指示或暗示相对重要性。
本发明中应用了具体个例对本发明的原理及实施方式进行了阐述，以上实施例的说明只是用于帮助理解本发明的方法及其核心思想；同时，对于本领域的一般技术人员，依据本发明的思想，在具体实施方式及应用范围上均会有改变之处。综上所述，本说明书内容不应理解为对本发明的限制。

Claims (6)

  1. 一种高效率超临界设备，其特征在于：包括通过管路连通的气液分离器和二氧化碳过滤器，所述气液分离器用于将气液混合物分离，并将分离后的气体输送至二氧化碳过滤器，所述二氧化碳过滤器用于将气体过滤，并将过滤后的二氧化碳通过超临界流体色谱系统中的制冷器冷却后重复使用。
  2. 根据权利要求1所述的高效率超临界设备，其特征在于：还包括加热机，所述加热机串行连接有换热器，所述气液混合物经所述换热器加热后进入所述气液分离器；所述加热机内设置有液态换热介质。
  3. 根据权利要求2所述的高效率超临界设备，其特征在于：所述气液分离器外包覆有加热部，所述加热机、换热器和加热部通过管道串行连接。
  4. 根据权利要求1所述的高效率超临界设备，其特征在于：所述二氧化碳过滤器内部装填有塔板填料，所述塔板填料能够将经过气液分离器后的气体中残留的有机溶剂和样品进行再次过滤和冷凝，得到纯净的气态二氧化碳。
  5. 根据权利要求2所述的高效率超临界设备，其特征在于：所述二氧化碳过滤器顶端的二氧化碳排放口通过管路连接到所述制冷器，所述二氧化碳排放口与所述制冷器之间的管路处设置有温度传感器，所述温度传感器与所述加热机的控制端电连接。
  6. 根据权利要求2所述的高效率超临界设备，其特征在于：所述液态换热介质为水。
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