CN111650321B - Electrically driven programmable valve with zero dead volume and sample injection gas circuit system - Google Patents

Electrically driven programmable valve with zero dead volume and sample injection gas circuit system Download PDF

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Publication number
CN111650321B
CN111650321B CN202010540835.1A CN202010540835A CN111650321B CN 111650321 B CN111650321 B CN 111650321B CN 202010540835 A CN202010540835 A CN 202010540835A CN 111650321 B CN111650321 B CN 111650321B
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China
Prior art keywords
valve
dead volume
valve body
gas
gas circuit
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CN202010540835.1A
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CN111650321A (en
Inventor
王少楠
陈春玉
谭依玲
马昌宁
唐霞梅
方艾黎
李威
徐龙
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Haohua Gas Co Ltd
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Southwest Research and Desigin Institute of Chemical Industry
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Publication of CN111650321A publication Critical patent/CN111650321A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02Column chromatography
    • G01N30/04Preparation or injection of sample to be analysed
    • G01N30/16Injection
    • G01N30/20Injection using a sampling valve
    • G01N2030/201Injection using a sampling valve multiport valves, i.e. having more than two ports

Abstract

The invention discloses a zero dead volume electrically driven program control valve which mainly comprises a valve body, a transmission device and a driving motor, wherein the valve body is provided with a valve seat; the invention also provides a sample injection gas path system, which realizes sample injection by matching a program control valve with a gas path; the valve body is connected with the gas circuit through a zero dead volume sealing joint, the gas circuit is designed with a small drift diameter of 0.5-1 mm, and the tolerance of the outer diameter of a pipeline used for gas circuit connection is within +/-0.002 mm. The valve switching device drives the motor to rotate through the external power supply, and the driving motor drives the transmission device to further drive the valve core of the valve body to rotate so as to achieve the purpose of valve switching. The program control valve and the sample introduction gas circuit system can control the dead volume to be below 0.15 mu L.

Description

Electrically driven programmable valve with zero dead volume and sample injection gas circuit system
Technical Field
The invention belongs to the technical field of valves, and particularly relates to a zero dead volume electrically driven program control valve and a sample injection gas circuit system.
Background
The dead volume is large, which causes dead angles of gas path replacement, resulting in that the analysis equipment cannot obtain representative samples, and finally the analysis result is distorted. The dead volume of the zero dead volume programmable valve for analyzing international flow is controlled below 0.15 mu L.
At present, no electrically-driven programmable valve with zero dead volume suitable for a high-end online chromatograph exists in China, and the main technical problems are as follows: 1) the dead volume is large, typically greater than 100 μ L; 2) the sealing surface structure is unreasonable, a plane type or cylinder type sealing mode is almost adopted, and the leakage phenomenon can occur after long-term operation; 3) the continuous operation frequency of the valve is about tens of thousands of times, and the stability is not high.
Disclosure of Invention
The invention aims to provide an electrically-driven program control valve and a sample injection gas circuit system aiming at the problems, so that the dead volume is controlled to be less than 0.15 mu L, and the stability and the reliability of operation are improved.
The technical content of the invention is as follows:
a programmable valve driven electrically by zero dead volume comprises a valve body, a transmission device and a driving motor;
the valve body is provided with a gas inlet and outlet which is arranged in the valve body and used for introducing or discharging gas, the hardness of a metal material of the gas inlet and outlet is less than that of the material of the valve body, and a conical sealing surface is formed in a pressing mode after the matching surface between the valve body and the gas inlet and outlet reaches a certain degree of finish; the valve body is also internally provided with a valve core which is connected with the valve shaft and is made of high polymer materials for sealing, and the valve core and the gas inlet and outlet of the valve body form a sealing surface which can select different gas inlets and outlets to be communicated through an auxiliary mounting piece with an elastic telescopic function;
the transmission device comprises a valve rotor and a coupling device, one end of the valve rotor is connected with the valve shaft, the other end of the valve rotor is connected with the coupling device, the coupling device is matched with the driving motor, and the driving motor drives the valve shaft to rotate after rotating, so that the communication switching of different gas inlets and outlets is realized.
In some embodiments of the programmable valve of the invention, the smoothness of the pressing surface of the gas inlet and outlet and the valve body reaches Ra0.2 and below.
In some embodiments of the programmable valve of the present invention, the drive motor is driven in a relay isolated drive.
In some embodiments of the programmable valve of the present invention, the type of valve body comprises a six-way valve, an eight-way valve, or a ten-way valve.
The program control valve can control the dead volume to be less than 0.15 mu L, and the failure-free operation frequency is more than 20 ten thousand.
In some embodiments of the programmable valve of the present invention, the programmable valve is fixed on the chromatographic instrument by a mounting assembly, the mounting assembly includes a mounting collar, a collar sleeve and a mounting seat, the mounting collar is connected with the collar sleeve, the mounting seat is connected with the driving motor, the mounting collar is connected with the coupling device, and the mounting seat is provided with a mounting hole for fixing on the chromatographic instrument.
The invention also discloses a sample injection gas circuit system which comprises the program control valve and a gas circuit connected with the program control valve.
In some specific embodiments of the sample gas path system of the present invention, a filter is disposed at a gas inlet and outlet of each gas path entering the valve body, and the filtering precision of the filter is 0.01 to 1 μm.
In some embodiments of the sample injection gas path system of the present invention, the gas inlet and outlet of the programmable valve are connected to the gas path by a zero dead volume sealing joint, the gas path is designed with a small diameter of 0.5 to 1mm, and the tolerance of the outer diameter of the pipeline used for gas path connection is within ± 0.002 mm.
In some embodiments of the sample gas path system of the present invention, the dead volume of the sample gas path system is less than 0.15 μ L.
Due to the adoption of the technical scheme, the invention has the following technical effects: the invention develops the electrically driven programmable valve with zero dead volume of a high-end online chromatograph, can control the dead volume of the whole programmable valve to be less than 0.15 mu L, has excellent stability and reliability, can operate for more than 20 ten thousand times without faults, and does not leak after long-term operation; the zero dead volume electrically driven programmable valve provided by the invention is used for gas path sample injection, can realize optimal sampling, discharge and shunt of gas in a key process, and can provide better service for controlling the field of detection of ultra-pure and high-purity gas.
Drawings
FIG. 1 is an internal cross-sectional view of a zero dead volume electrically actuated programmable valve;
FIG. 2 is a schematic diagram of the components of a zero dead volume electrically driven programmable valve;
FIG. 3 is an assembled view of a zero dead volume electrically driven programmable valve;
FIG. 4 is a sampling plot of a zero dead volume electrically driven programmable valve;
FIG. 5 is a sample injection diagram of a zero dead volume electrically driven programmable valve;
FIG. 6 is a schematic view of the air intake arrangement when the programmable valve is a six-way valve;
fig. 7 is a schematic top view of the valve core structure when the programmable valve is a six-way valve.
Description of the drawings, 1-valve body; 2-a limit groove; 3-a valve rotor; 4-a transmission coupling; 5-driving the coupling; 6, mounting a lantern ring; 7-a snap ring sleeve; 8-driving a motor; 9-a control circuit; 10-a mounting seat; 11-a power line; 12-a ground line; 13-a relay; 14-two ends of the relay; 15-a driving control end, 16-a gas inlet and outlet, 17-a valve core, 18-a valve shaft, 19-an upper bearing, 20-a lower bearing, 21-a disc spring group, 22-a gasket, 23-a tetrafluoro gasket, 24-a limiting pin, 101-an upper valve body and 102-a lower valve body.
Detailed Description
All of the features disclosed in this specification, or all of the steps in any method or process so disclosed, may be combined in any combination, except combinations of features and/or steps that are mutually exclusive.
Any feature disclosed in this specification may be replaced by alternative features serving equivalent or similar purposes, unless expressly stated otherwise. That is, unless expressly stated otherwise, each feature is only an example of a generic series of equivalent or similar features.
As shown in fig. 1 to 3, a programmable valve driven by zero dead volume electricity comprises a valve body 1, a transmission device and a driving motor 8. The valve body 1 is provided with a gas inlet and outlet 16 which is arranged in the valve body and used for introducing or discharging gas, the hardness of the metal material of the gas inlet and outlet 16 is less than that of the material of the valve body, and a conical sealing surface is formed in a pressing mode after the matching surface between the gas inlet and outlet and the valve body reaches certain degree of finish. Specifically, the valve body may be integrally composed of an upper valve body 101 and a lower valve body 102. The material of the valve body 1 can be 304 or 316 stainless steel, the gas inlet and outlet 16 is installed on the upper valve body 101, the material can be copper and other metals or alloy materials, the hardness is required to be less than that of the valve body so as to be convenient for pressing, and the gas inlet and outlet 16 is in an inverted cone structure with a gas passing space from outside to inside; the smoothness of the mating surfaces of the gas inlet/outlet port 16 and the valve body 1 has an important influence on the sealing performance of the tapered mating surfaces, and the sealing performance is better when the surfaces are smoother, and this embodiment preferably controls the Ra of the contact surfaces to be less than 0.2, where Ra represents surface roughness, and the lower the value of Ra, the smoother the surface is. Finally, under a certain heating condition, the metal body of the gas inlet/outlet 16 is pressed into the valve body 1 to form a conical sealing surface. Compared with a planar or cylindrical sealing mode, the conical surface is easier to press and mount, the gas channel has continuity, and dead volume is hardly generated. The lower valve body 102 is internally provided with a cavity for installing the valve core 17, one end of the valve core 17 is connected with the valve shaft 18, the valve core 17 is made of a high polymer material for sealing, specifically, the high polymer material can be selected from modified Polyetheretherketone (PEEK), and the PEEK has high temperature resistance, mechanical properties, self-lubricating property and corrosion resistance, and is particularly suitable for valve core materials. The valve core 17 forms a sealing surface which can select different gas inlets and outlets to be communicated with the gas inlet and outlet 16 of the valve body through an auxiliary installation part with an elastic telescopic function. Specifically, as shown in fig. 1, the valve core 17 is installed by a disc spring set 21 having an upper bearing 19 and a lower bearing 20, the expansion and contraction performance of the disc spring set 21 ensures that the valve core 17 abuts against the bottom surface of the upper valve body 101 to form a sealing surface, and a gasket 22, a tetrafluoro gasket 23 and a limit pin 24 may be optionally arranged between the upper bearing 19 and the valve core 17 to improve the stability of the installation of the valve core 17.
The transmission device comprises a valve rotor 3 and a coupling device, one end of the valve rotor 3 is connected with the valve shaft 18, the other end of the valve rotor is connected with the coupling device, the coupling device is matched with the driving motor 8, and the driving motor 8 drives the valve shaft 18 to rotate after rotating, so that the communication switching of different gas inlets and outlets is realized. Specifically, as shown in fig. 2 to 3, the connecting end of the valve body 1 and the valve rotor 3 is provided with a limiting groove 2, the valve rotor 3 is installed in the limiting groove 2 and connected with the valve shaft 18, the other end of the valve rotor 3 is connected with a transmission coupler 4, the transmission coupler 4 is matched with the driving coupler 5, the other end of the driving coupler 5 is connected with the driving motor 8, and the driving motor 8 is controlled by the control circuit 9. The driving motor is connected with a power line 11, a grounding line 12 and a relay 13, and the relay 13 is connected with two relay ends 14 and a driving control end 15.
Further, the driving motor is driven in a relay isolation driving mode, after the driving motor is powered on, the driving motor 8 can control the valve to automatically reset, when the driving control end 15 is at a low level, the relay 13 is closed, the driving motor 8 rotates forwards, and the valve is in a sampling state, as shown in fig. 4; when the driving control end 15 is at a high level, the relay 13 is opened, the driving motor 8 rotates reversely, the valve is switched, and the valve is in a sample injection state, as shown in fig. 5.
In some embodiments of the programmable valve of the present embodiment, the type of valve body includes, but is not limited to, a six-way valve, an eight-way valve, or a ten-way valve. No matter how many passages of the valve body are, only the sealing surface between the valve core and the valve body needs to be adjusted. As shown in fig. 6 to 7, this embodiment discloses a structure of a six-way valve, in order to match with a device, a valve core of the six-way valve has three arc-shaped convex sealing surfaces at even intervals, and different gas inlets and outlets 16 in the upper valve body are communicated by rotation of the sealing surfaces, and the concept can be applied to other multi-channel valve paths.
This embodiment has still provided the installation scheme of programmable valve, and programmable valve passes through the installation component to be fixed on the chromatogram instrument, as shown in fig. 3, and the installation component includes the installation lantern ring 6, snap ring cover 7 and mount pad 10, and 6 one end of installation lantern ring is connected with drive coupling 5, and the other end is connected with snap ring cover 7, and snap ring cover 7 is connected with mount pad 10, and mount pad 10 is connected with driving motor 8, is provided with the mounting hole on the mount pad 10, can be used to the fixed on the chromatogram instrument. Therefore, the program control valve can be stably installed on the chromatographic instrument by adopting the installation scheme.
By adopting the program control valve of the embodiment, the dead volume of the whole program control valve can be controlled to be less than 0.15 mu L, and the failure-free operation frequency is more than 20 ten thousand. Dead volume is the portion of the gas path that cannot be displaced in the gas path that can affect the analysis of gas samples in the field of high purity gas, ultra high purity gas analysis. Zero dead volume generally refers to such a situation that does not affect the analysis. But usually there will always be a very small amount of such a space. Although no dead volume exists in the design, a tiny dead volume exists due to the influence of factors such as machining precision and the like, but the dead volume can be controlled to be below 0.15 mu L, so that the zero dead volume calling method is not contradictory to the possible dead volume in the industry. The program control valve of the embodiment is actually operated for more than 20 ten thousand times by adopting a testing method without any fault.
The embodiment also provides a sample injection gas circuit system, which comprises the program control valve and a gas circuit connected with the program control valve. The program control valve can be connected with a gas path of sample gas or carrier gas, and the sample gas path system can also comprise a quantitative device which is connected with the program control valve to determine the sample volume of the sample gas.
In some specific schemes of this embodiment, a filter is disposed at a gas inlet and outlet where each gas path enters the valve body, and the filtering precision of the filter is 0.01-1 μm. If gas with particles enters the valve body, the valve body can scratch fine lines on a sealing surface during operation, and the risk of air leakage, air leakage and dead volume formation of the valve can be caused. Through the filtering of the impurity thing of control filtering accuracy to probably existing in the entering gas, prevent that there is the granule to exist the destruction to each sealed face of valve body inside to promote the reliability of valve body use.
In some embodiments of this embodiment, the gas inlet/outlet of the programmable valve is connected to the gas path by a zero dead volume sealing joint, which is available in the prior art and commercially available, and is not limited herein. The gas circuit adopts 0.5 ~ 1 mm's little latus rectum design, and the gas circuit is connected the pipeline external diameter tolerance that uses and is within 0.002 mm. The drift diameter design of the gas path is reduced, and the pipe diameter tolerance at the gas path connection part is ensured to be smaller than a certain range, so that the dead volume possibly existing in the pipeline connection and the gas path is reduced. The small pipe diameter is used for realizing seamless compression sealing between the soft metal clamping sleeve and the conical surface of the valve body connecting hole and the conical surface of the connecting screw, thereby eliminating dead volume space; the small pipe diameter is easier to ensure the tight connection between the air inlet and outlet pipe and the vent hole, thereby reducing the dead volume.
By adopting the sample feeding gas circuit system of the embodiment, the dead volume of the whole system can be controlled to be less than 0.15 mu L. The gas sampling, discharging and shunting device can realize optimal sampling, discharging and shunting of gas in a key process, and can provide better service for controlling the field of ultra-pure and high-purity gas detection.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (9)

1. A zero dead volume electrically actuated programmable valve characterized by: comprises a valve body, a transmission device and a driving motor;
the valve body is provided with a gas inlet and outlet which is arranged in the valve body and used for introducing or discharging gas, the hardness of a metal material of the gas inlet and outlet is less than that of the material of the valve body, and a conical sealing surface is formed in a pressing mode after the matching surface between the valve body and the gas inlet and outlet reaches a certain degree of finish; the valve body is also internally provided with a valve core which is connected with the valve shaft and is made of high polymer materials for sealing, and the valve core and the gas inlet and outlet of the valve body form a sealing surface which can select different gas inlets and outlets to be communicated through an auxiliary mounting piece with an elastic telescopic function; the transmission device comprises a valve rotor and a coupling device, one end of the valve rotor is connected with the valve shaft, the other end of the valve rotor is connected with the coupling device, the coupling device is matched with the driving motor, and the driving motor drives the valve shaft to rotate after rotating so as to realize the switching of the communication of different gas inlets and outlets;
the smooth finish of the pressing surface of the gas inlet and outlet and the valve body reaches Ra0.2 or below.
2. The zero dead volume electrically actuated programmable valve of claim 1, wherein: the driving motor is driven in a relay isolation driving mode.
3. The zero dead volume electrically actuated programmable valve of claim 1, wherein: the valve body is in a six-way valve, eight-way valve or ten-way valve.
4. The zero dead volume electrically actuated programmable valve of claim 1, wherein: the program control valve is fixed on a chromatographic instrument through a mounting assembly, the mounting assembly comprises a mounting sleeve ring, a clamping ring sleeve and a mounting seat, the mounting sleeve ring is connected with the clamping ring sleeve, the mounting seat is connected with a driving motor, the mounting sleeve ring is connected with a coupling device, and a mounting hole is formed in the mounting seat and used for fixing the program control valve on the chromatographic instrument.
5. The zero dead volume electrically actuated programmable valve of claim 1, wherein: the dead volume of the program control valve is less than 0.15 mu L, and the program control valve operates for more than 20 ten thousand times without faults.
6. The utility model provides a kind gas circuit system that advances which characterized in that: comprising the programmable valve according to any of claims 1 to 5.
7. The sample gas path system of claim 6, wherein: and a filter is arranged at the gas inlet and outlet of each gas path entering the valve body, and the filtering precision of the filter is 0.01-1 mu m.
8. The sample gas path system of claim 6, wherein: the gas inlet and outlet of the program control valve are connected with the gas circuit through a zero dead volume sealing joint, the gas circuit is designed to have a small drift diameter of 0.5-1 mm, and the tolerance of the outer diameter of a pipeline used for gas circuit connection is +/-0.002 mm.
9. The sample injection gas circuit system according to any one of claims 6 to 8, characterized in that: the dead volume of the sample injection gas circuit system is less than 0.15 mu L.
CN202010540835.1A 2020-06-15 2020-06-15 Electrically driven programmable valve with zero dead volume and sample injection gas circuit system Active CN111650321B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112855991B (en) * 2021-01-08 2022-06-17 天华化工机械及自动化研究设计院有限公司苏州研究所 Chromatographic sample feeding switching valve for petrochemical industry

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CN202402669U (en) * 2011-12-26 2012-08-29 浙江蒙德克流体控制有限公司 Anti-scouring valve core of sequencing valve
CN104024847A (en) * 2011-12-26 2014-09-03 株式会社岛津制作所 Flow Path Switching Valve
CN105339789A (en) * 2013-03-11 2016-02-17 机械解析有限公司 Diaphragm valve with sealing assembly, chromatographic system including same and method of operation thereof
CN205877214U (en) * 2016-08-17 2017-01-11 重庆川仪调节阀有限公司 Compound seal structure's program control valve
CN206669084U (en) * 2017-03-31 2017-11-24 简阳市中原低温设备配套有限公司 Electromagnetism sequencing valve

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US9316324B2 (en) * 2008-10-29 2016-04-19 Agilent Technologies, Inc. Shear valve with silicon carbide member
JP5865403B2 (en) * 2014-02-12 2016-02-17 株式会社日立ハイテクノロジーズ Flow path switching valve and liquid chromatograph apparatus using the valve

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Publication number Priority date Publication date Assignee Title
CN202402669U (en) * 2011-12-26 2012-08-29 浙江蒙德克流体控制有限公司 Anti-scouring valve core of sequencing valve
CN104024847A (en) * 2011-12-26 2014-09-03 株式会社岛津制作所 Flow Path Switching Valve
CN105339789A (en) * 2013-03-11 2016-02-17 机械解析有限公司 Diaphragm valve with sealing assembly, chromatographic system including same and method of operation thereof
CN205877214U (en) * 2016-08-17 2017-01-11 重庆川仪调节阀有限公司 Compound seal structure's program control valve
CN206669084U (en) * 2017-03-31 2017-11-24 简阳市中原低温设备配套有限公司 Electromagnetism sequencing valve

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