Device and method for continuously and efficiently dehydrating gas
By combining a double-layer multi-way rotary valve and a multifunctional quartz microreactor, continuous and efficient dehydration of gas is achieved, solving the problems of sample loss, inaccurate temperature control and poor adaptability of existing devices, and ensuring deep dehydration of high-humidity gas and accuracy of detection results.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- DALIAN INSTITUTE OF CHEMICAL PHYSICS CHINESE ACADEMY OF SCIENCES
- Filing Date
- 2025-12-30
- Publication Date
- 2026-04-17
AI Technical Summary
Existing gas dehydration devices cannot achieve continuous processing and suffer from problems such as sample loss, inaccurate temperature control, easy condensation, and poor adaptability, thus failing to meet the deep dehydration requirements of high-humidity gases.
Employing a double-layer, dead-volume-free multi-port rotary valve and a multifunctional quartz microreactor, combined with a temperature control component consisting of a semiconductor cooling chip, a heat sink, and a thermistor, continuous gas switching for dehydration between the two microreactors is achieved. Seamless switching is realized through a 90° rotation of the multi-channel rotary valve assembly. Combined with inert gas protection and precise temperature control, sample loss and condensation are avoided.
It achieves continuous and efficient dehydration of gases, avoids sample loss, improves the accuracy of temperature control, expands the sample compatibility range, and ensures the stable operation of the device and the accuracy of the test results.
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Figure CN121869053A_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of gas sample pretreatment and analysis technology, and more particularly to a continuous and efficient gas dehydration device and method. Background Technology
[0002] In fields such as gas composition detection, environmental monitoring, and biomedical analysis, water vapor in high-humidity gas samples can severely affect the accuracy of detection results, leading to problems such as column failure, decreased detector sensitivity, and peak shape distortion. Therefore, thorough dehydration of gas samples is an indispensable and crucial step before detection.
[0003] Existing gas dehydration devices suffer from several technical defects: for example, traditional dehydration devices are mostly single-channel structures, requiring shutdown to replace the adsorbent or clean the condensate during dehydration, leading to interruptions in sample detection and failing to meet the requirements for continuous online monitoring; some devices use adsorption-based dehydration, where the adsorbent easily adsorbs target gas components, resulting in sample loss; and the adsorbent needs to be replaced after saturation, easily introducing contamination; low-temperature condensation dehydration is highly efficient, but existing devices lack precise temperature control mechanisms, where excessively low temperatures can cause target components to condense, while excessively high temperatures result in incomplete dehydration; when the cold components are working, surrounding air moisture easily condenses into water droplets, which can seep into the device, causing short circuits or component corrosion; and the dehydration chamber structure cannot be adjusted according to gas viscosity and target component characteristics, resulting in insufficient compatibility with gas samples containing trace amounts of active components.
[0004] Specifically, CN201156026Y discloses a semiconductor-cooled dehydration device for ion mobility spectrometers, which uses a baffle structure to extend the gas residence time and achieves a dehydration efficiency of approximately 50%. However, this device is a single-channel design, requiring periodic shutdowns for drainage, and cannot achieve continuous sample injection. Furthermore, its temperature control range is limited (0-10℃), failing to meet the needs of dehydration over a wide temperature range, and it does not solve the problems of condensation and sample loss. CN221752829U proposes a condensate removal system that uses a semiconductor cooling chip combined with a gas-liquid separator and secondary condensation through a heat exchanger. Although it can remove some condensate, it is still a single-channel processing mode, requiring shutdown for maintenance during switching. Moreover, the system structure is fragmented and has low integration, resulting in problems such as sample retention and inaccurate temperature control. KR1020240034644A discloses a dual-pipe alternating moisture removal device, which achieves alternating use of two cooling pipes through valve switching. However, its structure is complex, with a large number of valves and a long flow path switching time. Furthermore, it does not employ inert atmosphere protection, still posing a risk of condensation and short circuit. In addition, its temperature control method is singular and cannot achieve refrigeration. The heating linkage control has poor adaptability to gases containing easily condensable components.
[0005] In addition, existing devices generally suffer from the following common problems: low integration of multi-port valves and reactors, resulting in large dead volumes at connection points, leading to sample residue and loss; fixed reactor cavity clearances, unable to adapt to gases of different viscosities; poor fit between temperature control components and reactors, resulting in low heat transfer efficiency; and lack of overall sealing and inert gas protection mechanisms, making them prone to circuit failures due to condensation. Therefore, there is an urgent need for an integrated, continuous, precisely temperature-controlled, and dead-volume-free deep gas dehydration device. Summary of the Invention
[0006] In response to the aforementioned technical problems, a continuous and efficient gas dehydration device and method are provided to solve the technical problems of existing devices, such as inability to process continuously, sample loss, inaccurate temperature control, easy condensation, and poor adaptability. This enables deep dehydration of high-humidity gases, continuous sample injection, no sample loss, and stable operation.
[0007] The technical means employed in this invention are as follows: A continuous and efficient gas dehydration device, comprising: The sealed cavity is equipped with a vacuum port and a nitrogen filling port; The multi-channel rotary valve assembly, located within the sealed cavity, is a double-layered multi-channel rotary valve with no dead volume and has at least 8 passages, including 4 sample passages and 4 temperature control component connection passages. Two multifunctional quartz microreactors are both located in the sealed cavity and are respectively connected to the multi-channel rotary valve assembly via connecting hoses. A temperature control component, adapted to each multifunctional quartz microreactor, includes a semiconductor cooling chip, a heat sink, a cooling fan, and a thermistor. The temperature control component is used to realize cooling or cooling-heating linkage control. The multi-channel rotary valve assembly can rotate 90° to switch between two working modes, enabling continuous switching and dehydration of gas between two multifunctional quartz microreactors without changing the sample inlet and outlet pipelines.
[0008] Furthermore, the multi-channel rotary valve assembly includes a stator assembly with a square frame structure and a rotor assembly that is adapted for installation. The stator has communication ports on its four sides, and the rotor has two parallel passages inside. The stator and rotor are made of PEEK, polytetrafluoroethylene or ceramic material for precise fitting, with a fitting gap of ≤0.02mm.
[0009] Furthermore, the multifunctional quartz microreactor includes a first quartz cover plate and a second quartz cover plate that are parallel to each other, an inlet pipe, an outlet pipe, and a gap adjustment assembly. The outer surface of the quartz cover plate is provided with a groove for installing a thermistor.
[0010] Furthermore, the multifunctional quartz microreactor is divided into two types: Type 1 is a single-sided groove structure, with a groove for installing a thermistor on only one side; Type 2 is a double-sided groove structure, with grooves for installing thermistors on both sides, respectively adaptable to single-sided temperature control and double-sided temperature control scenarios.
[0011] Furthermore, the temperature control component also includes a heating element, which and the semiconductor cooling element are respectively disposed on both sides of the multifunctional quartz microreactor, and both are equipped with thermistors for real-time temperature feedback.
[0012] Furthermore, it also includes a microreactor height adjustment component, which is a telescopic structure or a detachable structure with replaceable length, located between the multifunctional quartz microreactor and the temperature control component, to adapt to semiconductor cooling chips of different thicknesses and ensure that the two fit tightly together.
[0013] Furthermore, the control method of the semiconductor cooling chip includes full-load power output and temperature closed-loop feedback control. The temperature closed-loop feedback control collects temperature signals through a thermistor and adjusts the output voltage to achieve temperature control within the range of -40℃ to 120℃.
[0014] Furthermore, the multi-channel rotary valve assembly is configured with a positioning component and an anti-blocking circuit. The positioning component includes a slot on the top of the rotor and two pairs of vertical optocouplers on the stator. The anti-blocking circuit collects the motor current through a resistor voltage divider and automatically cuts off the power when the current exceeds a threshold.
[0015] Furthermore, the gap adjustment component of the multifunctional quartz microreactor is a high-temperature resistant gasket or a quartz outer frame support. The gasket is 0.1-2mm thick, and the outer frame support is 1-5mm thick, respectively adaptable to low-viscosity and high-viscosity gas samples.
[0016] The present invention also discloses a method of using the above-mentioned continuous and efficient gas dehydration device, comprising the following steps: S1. After evacuating the sealed cavity, fill it with nitrogen gas. S2. Start the temperature control component to cool the multifunctional quartz microreactor to the target dehydration temperature through the semiconductor cooling chip; S3. The gas sample flows in from the sample inlet of the multi-channel rotary valve assembly, enters the first multifunctional quartz microreactor through the currently open path, and the water vapor condenses and dehydrates in the cavity. S4. When it is necessary to switch the processing channel, the multi-channel rotary valve assembly rotates 90° and the gas sample is switched to the second multifunctional quartz microreactor to achieve continuous dehydration. S5. The dehydrated gas flows out from the sample outlet of the multi-channel rotary valve assembly and enters the subsequent detection equipment.
[0017] In summary, the above-mentioned continuous gas dehydration method employs two parallel dehydration units, with the flow path controlled by a multi-way rotary valve. The method includes: allowing gas to flow through a first dehydration unit for dehydration; when switching is required, controlling the multi-way rotary valve to rotate by a preset angle to switch the gas to the second dehydration unit for continued dehydration, while simultaneously causing the first dehydration unit to disconnect from the main gas flow and perform a drainage regeneration operation; wherein, the drainage regeneration operation includes heating and melting ice in the first dehydration unit and / or purging with inert gas.
[0018] Compared with the prior art, the present invention has the following advantages: 1. This invention employs a combined design of two microreactors and a multi-port rotary valve. Rapid gas switching between the two microreactors is achieved by rotating the multi-port valve 90°, with a switching time ≤1 second. No downtime is required to replace consumables or clean condensate, enabling 24-hour continuous sample injection and dehydration. Compared to traditional single-channel devices, detection efficiency is improved, making it particularly suitable for online continuous monitoring scenarios; it ensures continuous sample transmission while avoiding sample loss during switching.
[0019] 2. The multifunctional quartz microreactor adopts a dead-volume-free design, with a stator-rotor fit gap ≤0.02mm. Piping connections utilize tightly fitted silicone flexible tubing to prevent sample retention. The grid-like raised structure on the inner surface of the microreactor stabilizes the gas flow field, ensuring sufficient contact between water vapor and the low-temperature chamber, resulting in high dehydration efficiency. Simultaneously, the low-temperature condensation dehydration method eliminates the need for adsorbents, avoiding adsorption loss of target components and ensuring accurate detection results, balancing dehydration depth and sample integrity.
[0020] 3. The temperature control component supports a wide temperature range of -40℃ to 120℃, and the dehydration temperature can be flexibly set according to the dew point and target component characteristics of the gas sample to avoid condensation of the target component. At the same time, the cooling-heating linkage design can maintain the temperature on one side of the chamber through the heating element for easily condensable reactive gases, and cool only the other side to achieve water vapor condensation, further expanding the sample adaptability range and solving the problems of low temperature control accuracy and poor adaptability of traditional devices. 4. The sealed cavity is sealed with a sealing ring and an inert atmosphere is formed by vacuuming and nitrogen filling, which completely isolates external moisture and prevents condensation from the surrounding air from seeping into the device when the temperature control component is cooling. This prevents short circuits or component corrosion and specifically solves the condensation problem of the low temperature dehydration device. 5. The device integrates a multi-way valve, microreactor, and temperature control components into a compact unit, eliminating the need for additional auxiliary equipment. The electrically driven multi-way valve can be switched via serial port commands, and temperature control parameters can be set via a touchscreen, making operation convenient. Furthermore, the microreactor height adjustment mechanism can accommodate cooling coils of varying thicknesses, simplifying installation and maintenance and lowering the barrier to entry for users. Attached Figure Description
[0021] To more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0022] Figure 1 This is a schematic diagram of the overall structure of the present invention.
[0023] Figure 2 This is an exploded view of the internal structure of the present invention.
[0024] Figure 3 This is a schematic diagram illustrating the connection method for continuously switching between the microreactor and the single-sided cooling plate.
[0025] Figure 4 The diagram illustrates the position A of the pipeline through which the double-layer multi-way valve of the present invention flows through the sample. (a) is a top cross-sectional view, and (b) is a bottom cross-sectional view.
[0026] Figure 5 Figure (a) shows the top section view and (b) shows the bottom section view of the pipeline through which the double-layer multi-way valve of the present invention flows through the sample.
[0027] Figure 6 This is a schematic diagram of an explosion on one side of the microreactor and the cooling chip of the present invention.
[0028] Figure 7 This is a schematic diagram of the explosion of the microreactor and the cooling chip on both sides of the present invention.
[0029] Figure 8 This diagram illustrates the positional relationship between the cooling element, heating element, and microreactor of the present invention.
[0030] Figure 9 This is an illustrative diagram showing the installation of a cooling chip on one side of the square sealed cavity of the present invention.
[0031] Figure 10 This is an exploded view of the method for fixing the position of the cooling chip and the microreactor in this invention.
[0032] Figure 11 This is an exploded view of the rear side of the position adjustment component of the microreactor cavity support of the present invention.
[0033] Figure 12 This is an assembly diagram of the rear side of the position adjustment component of the microreactor cavity support of the present invention.
[0034] Figure 13 This is a schematic diagram of the assembly of the microreactor and the double-layer cooling plate of the present invention.
[0035] Figure 14This is a schematic diagram of the assembly of the microreactor and the four-layer cooling plate of the present invention.
[0036] Figure 15 This is a schematic diagram of the microreactor containing the cooling and heating elements of the present invention.
[0037] Figure 16 This is a schematic diagram of the microreactor containing the cooling and heating elements of the present invention.
[0038] Figure 17 This is a schematic diagram of the assembly structure of the microreactor of the present invention, in which cooling chips are placed on both sides.
[0039] Figure 18 The present invention provides a method for continuously switching the connection between the microreactor and the double-sided cooling plate.
[0040] Figure 19 This is an overall assembly diagram of the microreactor of the present invention, with cooling chips placed on both sides.
[0041] Figure 20 This is an exploded view of the microreactor of the present invention with cooling plates placed on both sides.
[0042] Figure 21 This is an exploded view of the microreactor of the present invention with cooling and heating elements placed on both sides.
[0043] In the figure: 1. Multi-channel rotary valve assembly; 2. Microreactor; 3. Thermistor; 4. Cooling chip; 5. Heat sink fin; 6. Fan support; 7. Cooling fan; 8. Heating element; 101. Four-sided support frame; 102. Frame outer fittings; 103. Microreactor height adjustment component; 210. Sample inlet; 211. Sample outlet. Detailed Implementation
[0044] It should be noted that, unless otherwise specified, the embodiments and features described in the present invention can be combined with each other. The present invention will now be described in detail with reference to the accompanying drawings and embodiments.
[0045] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. The following description of at least one exemplary embodiment is merely illustrative and is in no way intended to limit the present invention or its application or use. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0046] It should be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of exemplary embodiments according to the invention. As used herein, the singular form is intended to include the plural form as well, unless the context clearly indicates otherwise. Furthermore, it should be understood that when the terms "comprising" and / or "including" are used in this specification, they indicate the presence of features, steps, operations, devices, components, and / or combinations thereof.
[0047] Unless otherwise specifically stated, the relative arrangement, numerical expressions, and values of the components and steps described in these embodiments do not limit the scope of the invention. It should also be understood that, for ease of description, the dimensions of the various parts shown in the drawings are not drawn to actual scale. Techniques, methods, and devices known to those skilled in the art may not be discussed in detail, but where appropriate, such techniques, methods, and devices should be considered part of the specification. In all examples shown and discussed herein, any specific values should be interpreted as merely exemplary and not as limitations. Therefore, other examples of exemplary embodiments may have different values. It should be noted that similar reference numerals and letters in the following figures denote similar items; therefore, once an item is defined in one figure, it need not be further discussed in subsequent figures.
[0048] In the description of this invention, it should be understood that the orientation or positional relationship indicated by directional terms such as "front, back, up, down, left, right", "horizontal, vertical, horizontal" and "top, bottom" is generally based on the orientation or positional relationship shown in the accompanying drawings, and is only for the convenience of describing this invention and simplifying the description. Unless otherwise stated, these directional terms do not indicate or imply that the device or element referred to must have a specific orientation or be constructed and operated in a specific orientation, and therefore should not be construed as a limitation on the scope of protection of this invention. The directional terms "inner" and "outer" refer to the inner and outer contours relative to the outline of each component itself.
[0049] For ease of description, spatial relative terms such as "above," "over," "on the upper surface of," "above," etc., are used herein to describe the spatial positional relationship of a device or feature as shown in the figures to other devices or features. It should be understood that spatial relative terms are intended to encompass different orientations in use or operation besides the orientation of the device as described in the figures. For example, if the device in the figures is inverted, a device described as "above" or "above" other devices or structures would subsequently be positioned as "below" or "under" other devices or structures. Thus, the exemplary term "above" can include both "above" and "below." The device may also be positioned in other different ways (rotated 90 degrees or in other orientations), and the spatial relative descriptions used herein will be interpreted accordingly.
[0050] Furthermore, it should be noted that the use of terms such as "first" and "second" to define components is merely for the purpose of distinguishing the corresponding components. Unless otherwise stated, the above terms have no special meaning and therefore should not be construed as limiting the scope of protection of this invention.
[0051] This embodiment discloses a continuous and efficient gas dehydration device, comprising: The sealed cavity is equipped with a vacuum port and a nitrogen filling port. In this embodiment, the sealed cavity is a hexahedral square structure, with each of the six faces sealed and surrounded by a sealing ring. This design prevents condensation of water vapor around the semiconductor cooling structure when it is under cooling conditions. Figure 9 The diagram shows a schematic of a square sealed cavity with a cooling chip 4 installed on one side.
[0052] The multi-channel rotary valve assembly 1, located within the sealed cavity, is a double-layered, dead-volume-free multi-way rotary valve with at least eight passages, including four sample passages and four temperature control component connection passages; for example... Figure 1 , Figure 2 As shown, the multi-channel rotary valve assembly 1, the microreactor 2, and the temperature control assembly are integrated into a closed cavity. Two multifunctional quartz microreactors 2 are both located in the sealed cavity and are respectively connected to the multi-channel rotary valve assembly 1 through connecting hoses. Each multifunctional quartz microreactor 2 has a corresponding inlet pipe and an outlet pipe, which can realize the cooling and heating treatment of gas and liquid samples. A temperature control component, adapted to each multifunctional quartz microreactor 2, includes a semiconductor cooling chip 4, a heat sink 5, a cooling fan 7, and a thermistor 3. The temperature control component is used to realize cooling or cooling-heating linkage control. The multi-channel rotary valve assembly 1 can rotate 90° to switch between two working modes, enabling continuous switching of gas for dehydration between the two multifunctional quartz microreactors 2 without replacing the sample inlet 210 and outlet 211 pipelines; wherein, the flow path state at pipeline position A is as follows Figure 4 As shown (a is a top section view, b is a bottom section view), the flow path at pipe location B is as follows: Figure 5 As shown (a is a top section view, b is a bottom section view).
[0053] Furthermore, the multi-channel rotary valve assembly 1 includes a stator assembly with a square frame structure and a rotor assembly for adaptation. The stator has communication ports on its four sides, and the rotor has two parallel passages inside. The stator and rotor are precisely fitted using PEEK, polytetrafluoroethylene, or ceramic materials, with a fit clearance ≤0.02mm. Its connection to the microreactor 2 can be determined through… Figure 1 , Figure 2 The overall structure and disassembled structure are clearly visible. This invention achieves a dead-volume-free design for the entire flow path from sample inlet to outlet by combining a precision fit gap of ≤0.02mm between the multi-port valve rotor and stator, a matching design of the inner diameter of the valve body passage and the connecting hose, and a streamlined cavity inside the microreactor with a smooth transition between inlet and outlet. This completely eliminates sample residue and cross-contamination.
[0054] Specifically, such as Figure 4 , Figure 5 As shown, the stator of this double-layer valve has two connecting ports on each of its four sides, connecting to the inlet and outlet pipes of two microreactors, as well as the external inlet and outlet. The rotor has two parallel, non-interconnected pathways inside. When the rotor is in position A, pathway one connects the external inlet to the sample inlet pipe of microreactor A, and pathway two connects the sample outlet pipe of microreactor A to the external outlet; at this time, A is operating. Simultaneously, the inlet and outlet of microreactor B are connected to the non-pathed area on the rotor through other ports on the stator, remaining isolated. When the rotor rotates 90° to position B, the two pathways switch synchronously, connecting the external inlet and outlet to the inlet and outlet pipes of microreactor B, respectively; B begins operating, while A is isolated. A single rotation of the valve body synchronously completes the switching of the flow path and the isolation of the backup channel, achieving a seamless and continuous switching function.
[0055] Furthermore, the multifunctional quartz microreactor 2 includes a first quartz cover plate and a second quartz cover plate that are parallel to each other, a sample inlet pipe, a sample outlet pipe, and a gap adjustment assembly. The outer surface of the quartz cover plate is provided with a groove for mounting the thermistor 3. The interior is a hollow structure. Of course, optionally, the inner surface may also be provided with serpentine channels, grid-like protrusions, or a combination thereof functionalized microstructures according to the actual application scenario.
[0056] The quartz microreactor, with its pre-designed grooves and flat outer surface, provides a precise and reliable physical interface for the temperature control components. Its streamlined internal cavity and optional functional microstructures ensure efficient capture of condensate and stable flow field. Its standardized pipeline interface facilitates leak-free, modular, and rapid connection with multi-port valves, thus becoming the core functional unit for constructing this continuous dehydration device.
[0057] Furthermore, the multifunctional quartz microreactor 2 is divided into two types: Type 1 is a single-sided groove structure, with a groove for mounting the thermistor 3 on only one side, suitable for single-sided temperature control scenarios. Its assembly structure is as follows: a semiconductor cooling chip 4 is placed behind the microreactor 2, and a thermistor 3 is placed between the microreactor 2 and the cooling chip 4. Thermal grease is applied during the bonding process between multiple components. A heat sink 5 is placed behind the semiconductor cooling chip 4, and a profile bracket is placed at the rear end of the heat sink 5 for mounting the cooling fan 7. Figure 3 , Figure 6 The diagram shows the connection method between the continuously switching microreactor 2 and the single-sided cooling plate 4, as well as the single-sided explosion structure. Type 2 is a double-recessed structure, with recesses on both sides for mounting thermistors 3, suitable for double-sided temperature control scenarios. Its assembly structure is as follows: thermistors 3 are placed on both sides of the microreactor 2; a semiconductor cooling chip 4 is placed on the other side of the thermistor 3; a heat sink 5 is placed on the other side of the cooling chip 4; and a cooling fan 7 is placed at the rear end of the heat sink 5. Figure 7 , Figure 13 , Figure 17 , Figure 19 , Figure 20 The diagram shows the explosion and assembly structure of the double-sided cooling system.
[0058] Furthermore, the temperature control component also includes a heating element 8, which and the semiconductor cooling element 4 are respectively disposed on both sides of the multifunctional quartz microreactor 2, and both are equipped with thermistors 3 for real-time temperature feedback. The thermistors 3 corresponding to the heating element 8 can realize real-time feedback of the heating temperature, ensuring heating accuracy, such as... Figure 8 , Figure 15 , Figure 16 , Figure 21 The diagram shows the positional relationship and assembly structure of the cooling element 4 and the heating element 8 on the microreactor 2.
[0059] Furthermore, as an optional implementation, the microreactor height adjustment component 103 is a rigid connector. Depending on the thickness of the different thermoelectric coolers, the microreactor height adjustment component 103 can be replaced with different lengths for support, thus securely fixing the microreactor to the front end of the cooler. The key feature is that the length of the microreactor height adjustment component 103 can be replaced individually as needed without affecting other components. This configuration dynamically compensates for thickness tolerances and cumulative assembly errors of different thermoelectric coolers 4, thereby achieving a zero-gap, tight fit between the microreactor 2 and the cooler 4 at the thermal interface. While a fixed structure limits the selection of coolers, a replaceable length adjustment component allows users to flexibly select the appropriate length based on the precise thickness of the new cooler, without replacing the entire support or reactor module, significantly reducing upgrade costs and maintenance complexity. During long-term thermal cycling (cooling-heating-cooling), slight differences in thermal expansion may exist between the materials. Adjustable rigid support provides a continuous and stable clamping force to counteract minor deformations or loosening that may be caused by thermal stress, prevent local overheating or temperature control failure caused by poor contact, and ensure the long-term stability and reliability of the device during continuous operation.
[0060] Furthermore, as an optional implementation, a microreactor height adjustment component 103 is also included. This height adjustment component 103 is a telescopic structure, located between the multifunctional quartz microreactor 2 and the temperature control component. It is used to adapt to semiconductor cooling chips 4 of different thicknesses. By adjusting the length, it ensures that the microreactor 2 and the cooling chip 4 are always in close contact, guaranteeing heat transfer efficiency. Figure 10 The image shown is an exploded view of the fixed positions of the cooling element 4 and the microreactor 2. Figure 11 , Figure 12 The images show the exploded rear view and assembly view of the microreactor cavity support position adjustment component 103. The microreactor height adjustment component 103 includes a base fixed to the four-sided support frame 101, an adjustment rod with external threads, and a locking nut. Rotating the adjustment rod allows its top end to press against the bottom of the microreactor 2, thereby eliminating the assembly gap between the microreactor 2 and the semiconductor cooling chip 4. After adjustment, it is secured by the locking nut.
[0061] In this embodiment, the four-sided support frame 101 is integrally formed from a high-strength metal material (such as aluminum alloy) and has a square frame structure with evenly distributed mounting holes and positioning reference surfaces. It is used to support the core components inside the device and ensure assembly accuracy. It is fixedly connected to the inner wall of the sealed cavity by bolts. The outer frame fittings 102 are screwed into the edge holes of the four-sided support frame 101 to form a closed internal installation space. The frame has reserved mounting slots for the microreactor 2 and the multi-channel rotary valve assembly 1, providing a stable support reference for each component, ensuring that the relative positions between components are fixed, and avoiding loosening of the connection due to vibration during operation.
[0062] Furthermore, the control method of the semiconductor cooling chip 4 includes full-load power output and temperature closed-loop feedback control. The temperature closed-loop feedback control collects temperature signals through the thermistor 3 and adjusts the output voltage to achieve temperature control within the range of -40℃ to 120℃. During full-load power output, the temperature can be reduced to -40℃ or even lower, with the minimum temperature depending on room temperature conditions. Its bonding with the microreactor 2 and the temperature control-related structure can be combined... Figure 3 , Figure 6 , Figure 7 Please refer to the attached diagram for further understanding.
[0063] Furthermore, the multi-channel rotary valve assembly 1 is configured with a positioning component and an anti-blocking circuit. The positioning component includes a slot on the top of the rotor and two pairs of vertical optocouplers on the stator. The anti-blocking circuit collects the motor current through a resistor voltage divider and automatically cuts off the power when the current exceeds the threshold.
[0064] Furthermore, the gap adjustment component of the multifunctional quartz microreactor 2 is a high-temperature resistant gasket or a quartz outer frame support. The gasket thickness is 0.1-2mm, and the outer frame support thickness is 1-5mm, respectively adapted to low-viscosity and high-viscosity gas samples.
[0065] Optionally, an enhanced temperature control structure with dual-sided cooling and dual-sided heating can be configured: semiconductor cooling pads 4 are placed on both sides of each microreactor 2, paired with thermistors 3 to provide cooling temperature feedback. Simultaneously, heating pads 8 and corresponding thermistors 3 are added to the other two sides of the microreactor 2, achieving precise control of the linkage between cooling and heating, such as... Figure 14 , Figure 15 , Figure 16 , Figure 21 The diagram shows an assembly of multiple sets of cooling elements 4 and a cooling-heating linkage.
[0066] Specifically, in this embodiment, the gap adjustment component of the multifunctional quartz microreactor can adopt two adaptation schemes: one is a high-temperature resistant gasket with a thickness of 0.1mm to 2mm, selected from graphite, ceramic or quartz fiber materials, which is sealed to the two quartz cover plates by high-temperature welding, suitable for low viscosity samples such as gases; the other is a quartz outer frame support with a thickness of 1mm to 5mm, in which the quartz cover plate and the outer frame support are sealed by welding or quartz-specific high-temperature resistant adhesive, suitable for samples containing cell fluids and other samples that require a large flow space, and avoids the functional layer of the coated cover plate from failing due to high-temperature welding.
[0067] The inner surface of the quartz cover plate of the multifunctional quartz microreactor can be equipped with functionalized microstructures, including serpentine channels, island-shaped protrusions, grid-shaped protrusions, or combinations thereof, which are made by machining, photolithography, or molding processes. The channel width is 0.5mm–5mm and the protrusion height is 0.5mm–3mm. The serpentine channels can realize the orderly arrangement of cell-containing samples, and the grid-shaped protrusions can stabilize the gas flow field and break the eddies.
[0068] The connection method of the sample inlet and outlet pipelines of the microreactor can be flexibly selected, including coaxially symmetrical arrangement on both sides of the cavity, at least one pipeline is bent and parallel to the cavity, and at least one pipeline is arranged perpendicular to the cavity (single vertical, double vertical in the same direction or double vertical in opposite directions). The outer diameter of the pipeline is uniformly 3mm and the inner diameter is 1-1.5mm to ensure stable fluid flow.
[0069] For parallel pipelines, a dedicated limiting component is configured. This component is made of high-temperature resistant, high-strength insulating material (such as ceramic or quartz) and has positioning holes that match the outer diameter of the pipeline to ensure the coaxiality and spacing consistency of the pipelines and improve the consistency of mass production.
[0070] The fluid cavity of the microreactor adopts a streamlined design, and can be selected in the shape of rhombus, square, circle, ellipse, pear or teardrop. It has a smooth transition near the pipeline connection to avoid fluid stagnation and the formation of dead volume, while reducing flow resistance and reducing the difficulty of pipeline welding.
[0071] In addition to thermoelectric coolers, external temperature control components can also be equipped with heat-conducting blocks, thin-film heaters, or combinations thereof. In single-sided temperature control scenarios, a thermistor is placed in a groove on one side of the microreactor, with a thermoelectric cooler attached to its outer side. Thermal grease is applied to the contact surface, and a heat sink and cooling fan are installed on the hot end of the cooler. In double-sided temperature control scenarios, thermistors and thermoelectric coolers are placed in grooves on both sides to form a symmetrical temperature control structure, achieving rapid and uniform temperature rise and fall.
[0072] In this embodiment, the stator connection port of the multi-channel rotary valve assembly can adopt three connection methods, including directly machining the pipeline outlet from the outside, machining threaded holes and assembling pipeline connectors, and providing protruding pipelines on opposite sides and threaded hole pipeline connectors on the other two sides. The choice can be made flexibly according to the integration scenario to improve adaptability.
[0073] In manual drive mode, the top of the stator is equipped with a groove structure. This groove can accurately determine the flow path connection mode, avoid positioning deviations during manual rotation, and ensure the accuracy of flow path switching.
[0074] The stator's extension tube can be directly connected to the sample inlet and outlet tubes of the multifunctional quartz microreactor via a silicone tube, further reducing the dead volume at the tube connection and preventing gas sample retention.
[0075] In the multi-layer structure design, the multi-layer valve body shares a set of external stators, the inner stator and the outer rotor cooperate with each other, and the upper and lower flow paths can be arranged in parallel or vertically according to the installation space requirements. Non-connected areas are hollowed out to avoid flow path interference.
[0076] When electrically controlled, a dedicated motor fixing structure is configured, including a drive motor support connector. This connector is machined with a groove hole adapted to the shape of the motor, a round hole in the middle through which the motor shaft passes, and screw holes around the perimeter, which respectively realize the motor fastening and stator positioning, thereby improving the structural stability.
[0077] The stepper motor selected for the electric drive uses an encoder to precisely control the step angle, ensuring a 90° rotation positioning accuracy; the selected DC motor is paired with a worm gear reducer to achieve stable vertical drive and adapt to different installation layout requirements.
[0078] The anti-blocking circuit collects the motor current in real time through a resistor voltage divider. When the motor current exceeds the set threshold and continues for a preset time (e.g., 5s), the power supply is automatically cut off to avoid damage to components caused by rotor and stator jamming, thus improving the reliability of the device.
[0079] The present invention also discloses a method of using the above-mentioned continuous and efficient gas dehydration device, comprising the following steps: S1. After evacuating the sealed cavity, nitrogen is introduced to create an inert protective atmosphere, preventing condensation during the cooling process. This step completely eliminates air and moisture, creating a dry and inert environment. This is a crucial pretreatment step not explicitly mentioned in existing technologies. It ensures that even at deep cooling temperatures of -40°C, no condensation droplets will form inside the device, eliminating the risk of short circuits or contamination of optical components due to condensation. Specifically, existing low-temperature condensation and dehydration devices typically only focus on external moisture protection, neglecting the fact that when cooling components (such as the cold end of a semiconductor cooling chip) operate at extremely low temperatures (such as -40°C), the powerful cooling capacity they generate causes residual air inside the sealed cavity to quickly reach its dew point and condense. Water droplets can also damage internal circuits and optical components. This invention, through the pretreatment step of evacuating the cavity and then introducing a dry inert gas (such as nitrogen), physically removes the source of condensable moisture, creating an inherently safe internal dehydration environment. This is a prerequisite for achieving deep low-temperature (below -40°C) dehydration and long-term stable operation.
[0080] S2. The temperature control component is activated, and the multifunctional quartz microreactor 2 is cooled to the target dehydration temperature via the semiconductor cooling chip 4. If a closed-loop temperature feedback control is used, the temperature signal is collected in real time by the thermistor 3, and the output voltage is adjusted to maintain the target temperature. In actual use, the user can flexibly set the optimal dehydration temperature according to the dew point and condensation characteristics of different gas samples and target components. For example, for gases containing volatile organic compounds, a low temperature slightly higher than their boiling point (such as -20℃) can be used to condense only water vapor, thus avoiding the loss of the target substance. This wide-range, programmable, and precise temperature control capability is superior to the fixed 0-10℃ low-temperature range of existing technologies, and also superior to some secondary condensation modes.
[0081] S3. The gas sample flows in from the sample inlet 210 of the multi-channel rotary valve assembly 1, enters the first multifunctional quartz microreactor 2 through the currently open passage, and in the low-temperature chamber, water vapor rapidly condenses on the inner wall of the quartz, resulting in deep dehydration of the gas; the positions of the sample inlet 210 and outlet 211 can be referenced. Figure 4 , Figure 5 The identifiers 210 and 211 in the text; S4. When switching processing channels is required, that is, after the first reactor has been running for a period of time (which can be determined based on a preset time or differential pressure signal), the system issues a command to drive the multi-channel rotary valve assembly 1 to rotate 90°, and the gas sample is switched to the second multifunctional quartz microreactor 2 to achieve continuous dehydration. The flow path changes corresponding to the switching process can be detected by... Figure 4 , Figure 5 The comparison and understanding; S5, the dehydrated gas flows out from the sample outlet 211 of the multi-channel rotary valve assembly 1 and enters the subsequent detection equipment. At this time, the physical connection between the sample inlet 210 and the outlet 211 has not changed, but the gas has automatically and seamlessly switched to the second microreactor 2 for dehydration.
[0082] During the switching process, the gas supply remains uninterrupted, and the dehydration process continues without any downtime. At this time, the first microreactor can be automatically heated briefly above freezing point by the temperature control component, melting the frost inside and draining it through the preset drainage structure, thus improving switching efficiency and automation.
[0083] The dehydrated gas flows out stably from sample outlet 211 and can be directly connected to subsequent analysis equipment such as gas chromatography and mass spectrometry to achieve online, continuous, and high-quality detection.
[0084] In practical applications, single-sided cooling is suitable for dehydrating most conventional gases and has a simple structure. Dual-sided cooling, with cooling pads 4 arranged on both sides of the microreactor 2, achieves faster cooling and a more uniform temperature field within the chamber, making it suitable for applications sensitive to temperature gradients or requiring extremely fast dehydration rates. The linkage between cooling and heating involves arranging cooling pads 4 on one side of the microreactor and heating pads 8 on the other, each independently controlled by a thermistor 3. This mode is particularly suitable for gases containing easily condensable active components. Through precise control, one side of the chamber is maintained at a low temperature while the other side is kept at a suitable high temperature, achieving selective dehydration and maximizing sample integrity.
[0085] After implementing this invention, when the flow rate is set to 50 ml / min and the dehydration device of this invention is used, the humidity value at the outlet is measured and is close to the theoretical dew point humidity, indicating that the dehydration effect is excellent.
[0086] After implementation of this invention, the test compound acetone is mixed with water vapor with a relative humidity of over 90%, and the signal strength is increased by 85 times after passing through a dehydration device, which is better than that of the Nafion tube.
[0087] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them. Although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features therein. Such modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.
Claims
1. A continuous and efficient gas dehydration device, characterized in that, include: The sealed cavity is equipped with a vacuum port and a nitrogen filling port; The multi-channel rotary valve assembly, located within the sealed cavity, is a double-layered multi-channel rotary valve with no dead volume and has at least 8 passages, including 4 sample passages and 4 temperature control component connection passages. Two multifunctional quartz microreactors are both located in the sealed cavity and are respectively connected to the multi-channel rotary valve assembly via connecting hoses. A temperature control component, adapted to each multifunctional quartz microreactor, includes a semiconductor cooling chip, a heat sink, a cooling fan, and a thermistor. The temperature control component is used to realize cooling or cooling-heating linkage control. The multi-channel rotary valve assembly can rotate 90° to switch between two working modes, enabling continuous switching and dehydration of gas between two multifunctional quartz microreactors without changing the sample inlet and outlet pipelines.
2. The gas continuous high-efficiency dehydration device according to claim 1, characterized in that, The multi-channel rotary valve assembly includes a stator assembly with a square frame structure and a rotor assembly that is adapted for installation. The stator has communication ports on its four sides, and the rotor has two parallel passages inside. The stator and rotor are made of PEEK, polytetrafluoroethylene or ceramic material with a precision fit and a fit gap of ≤0.02mm.
3. The gas continuous high-efficiency dehydration device according to claim 1, characterized in that, The multifunctional quartz microreactor includes a first quartz cover plate and a second quartz cover plate that are parallel to each other, an inlet pipe, an outlet pipe, and a gap adjustment assembly. The outer surface of the quartz cover plate is provided with a groove for installing a thermistor.
4. The gas continuous high-efficiency dehydration device according to claim 1, characterized in that, The multifunctional quartz microreactor is divided into two types: Type 1 is a single-sided groove structure, with a groove for installing a thermistor on only one side; Type 2 is a double-sided groove structure, with grooves for installing thermistors on both sides, respectively adaptable to single-sided temperature control and double-sided temperature control scenarios.
5. The gas continuous high-efficiency dehydration device according to claim 1, characterized in that, The temperature control component also includes a heating element, which and the semiconductor cooling element are respectively located on both sides of the multifunctional quartz microreactor, and both are equipped with thermistors for real-time temperature feedback.
6. The gas continuous high-efficiency dehydration device according to claim 1, characterized in that, It also includes a microreactor height adjustment component, which is a telescopic structure or a detachable structure with replaceable length, located between the multifunctional quartz microreactor and the temperature control component, to adapt to semiconductor cooling chips of different thicknesses and ensure that the two fit tightly together.
7. The gas continuous high-efficiency dehydration device according to claim 1, characterized in that, The control method of the semiconductor cooling chip includes full-load power output and temperature closed-loop feedback control. The temperature closed-loop feedback control collects temperature signals through a thermistor and adjusts the output voltage to achieve temperature control within the range of -40℃ to 120℃.
8. The gas continuous high-efficiency dehydration device according to claim 1, characterized in that, The multi-channel rotary valve assembly is equipped with a positioning component and an anti-blocking circuit. The positioning component includes a slot on the top of the rotor and two pairs of vertical optocouplers on the stator. The anti-blocking circuit collects the motor current through a resistor voltage divider and automatically cuts off the power when the current exceeds the threshold.
9. The gas continuous high-efficiency dehydration device according to claim 1, characterized in that, The gap adjustment component of the multifunctional quartz microreactor is a high-temperature resistant gasket or a quartz outer frame support. The gasket thickness is 0.1-2mm, and the outer frame support thickness is 1-5mm, respectively adapted to low-viscosity and high-viscosity gas samples.
10. A method of using the gas continuous high-efficiency dehydration device according to any one of claims 1 to 9, characterized in that, Includes the following steps: S1. After evacuating the sealed cavity, fill it with nitrogen gas. S2. Start the temperature control component to cool the multifunctional quartz microreactor to the target dehydration temperature through the semiconductor cooling chip; S3. The gas sample flows in from the sample inlet of the multi-channel rotary valve assembly, enters the first multifunctional quartz microreactor through the currently open path, and the water vapor condenses and dehydrates in the cavity. S4. When it is necessary to switch the processing channel, the multi-channel rotary valve assembly rotates 90° and the gas sample is switched to the second multifunctional quartz microreactor to achieve continuous dehydration. S5. The dehydrated gas flows out from the sample outlet of the multi-channel rotary valve assembly and enters the subsequent detection equipment.
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