Gravimetric method adsorption instrument based on magnetic suspension balance and control method of gravimetric method adsorption instrument
By using a magnetic levitation balance in the adsorbent, the atmosphere between the isolation circuit part and the sample chamber is solved, the existing adsorbent cannot withstand corrosive gases and high temperature and high pressure, and a wider application range is achieved.
Patent Information
- Application Number
- CN202411856920.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-12-17
- Publication Date
- 2025-03-28
AI Technical Summary
In the existing weight adsorbent, the balance cannot withstand corrosive gases and steam, and cannot withstand high temperatures, low temperatures and high pressures, limiting its application range.
A weight adsorption meter based on magnetic levitation balance is used to isolate the microbalance from the sample chamber through a magnetic levitation system to prevent partial contact of corrosive gases and steam from the circuit, and can withstand high temperatures, low temperatures and high pressures.
The adsorption test of corrosive gases, steams and flammable and explosive gases in high temperature, low temperature or high pressure states has been achieved, and the application range of adsorbent instruments has been expanded.
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Figure CN119715235A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of adsorption instruments, and specifically provides a gravimetric adsorption instrument based on a magnetic suspension balance and a control method thereof. Background Art
[0002] Gas molecules or steam molecules can be adsorbed by solid surfaces. If the adsorbate molecules bind to the solid surface, that is, they interact with each other by van der Waals forces, it is called physical adsorption. If the adsorbate molecules bind to the solid surface by chemical bonds, that is, a chemical reaction occurs, it is called chemical adsorption. Physical adsorption is widely used in determining the specific surface area and pore size distribution of materials, evaluating natural gas mineral reserves, and evaluating the performance of chemical catalysts and adsorbents. In this process, various types of tests and experiments are required, such as conventional gas / steam physical adsorption experiments, high temperature and high pressure physical adsorption experiments, corrosive gas / steam physical adsorption experiments, flammable and explosive gas physical adsorption experiments, and dynamic / static physical adsorption experiments. Among them, experiments under high temperature and high pressure also require accurate determination of the actual density of gas or supercritical fluid under high pressure. Chemical adsorption also has many applications in materials research, chemical industry and other fields.
[0003] In the existing gravimetric physical adsorption instrument, the balance is in the sample chamber and is in the test gas atmosphere together with the sample. Due to the material of the balance, the balance cannot tolerate corrosive gases and steam, and cannot withstand high temperature, low temperature and high pressure. In addition, due to the existence of circuits inside the balance, the balance cannot come into contact with flammable and explosive gases, which has many restrictions on the application scope of the physical adsorption instrument. Therefore, how to optimize the structure of the physical adsorption instrument to expand its application scope has become a technical problem that needs to be solved in this field. Similarly, there are similar problems in the field of chemical adsorption.
[0004] In view of this, the art needs a new gravimetric adsorption instrument based on a magnetic suspension balance and a control method thereof to solve the existing problems. Summary of the invention
[0005] The present invention aims to solve the above technical problem, that is, to solve the problem that the microbalance of the existing gravimetric adsorption instrument has many limitations on the application scope of the adsorption instrument.
[0006] In a first aspect, the present invention provides a gravimetric adsorption instrument based on a magnetic levitation balance, the adsorption instrument comprising a magnetic levitation balance, the magnetic levitation balance comprising a magnetic levitation system and a sample chamber for placing a sample, the magnetic levitation system comprising a first part arranged outside the sample chamber and a second part arranged inside the sample chamber, the first part comprising a microbalance and a first magnetic device, the first magnetic device being an electromagnetic force device, and the first magnetic device being connected to the microbalance of the magnetic levitation system, the second part comprising a second magnetic device, the second magnetic device being a permanent magnet and being connected to the sample in the sample chamber, the magnetic force generated by the first magnetic device after being energized can attract the second magnetic device and the sample and weigh them through the microbalance.
[0007] In a specific embodiment of the above-mentioned gravimetric adsorption instrument based on a magnetic suspension balance, a first connecting structure is arranged between the second magnetic device and the sample, the first connecting structure includes a connecting frame, a connecting frame bracket and a first connecting block arranged inside the connecting frame, the first connecting block is connected to the second magnetic device, and the connecting frame is connected to the sample. The first connecting block can be driven by the second magnetic device to move in the air for a distance in the connecting frame and then abut against the connecting frame, thereby driving the connecting frame and the sample to move to a suspended state separated from the connecting frame bracket.
[0008] In a specific embodiment of the above-mentioned gravimetric adsorption instrument based on a magnetic suspension balance, a sinker and a sinker bracket are further provided in the sample chamber, a second connecting structure is provided between the second magnetic device and the sinker, the second connecting structure is a second connecting block, and a corresponding connecting hole is provided on the sinker, the second connecting block is connected to the second magnetic device, and the second connecting block can be driven by the second magnetic device to move in the air for a distance and then abut against the connecting hole of the sinker, thereby driving the sinker to move to a suspended state separated from the sinker bracket.
[0009] In the above-mentioned specific embodiment of the gravimetric adsorption instrument based on the magnetic suspension balance, the adsorption instrument also includes a static air intake system, the static air intake system includes a static air intake pipeline, a static exhaust pipeline and a static air mixing pipeline connected end to end, the first end of the static air intake pipeline is connected to the air source, and the second end is connected to the static air mixing pipeline, the first end of the static exhaust pipeline is connected to the static air mixing pipeline, and the second end is connected to the exhaust port, the static air intake pipeline, the static exhaust pipeline and the static air mixing pipeline are respectively provided with a static air intake solenoid valve, a static exhaust solenoid valve and a static air mixing solenoid valve; the static air intake system also includes a static air supply pipeline and a static air return pipeline, and the corresponding The sample chamber includes an air supply port and an air return port. The first end of the static air supply pipeline is connected to the static air mixing pipeline, and the second end is connected to the air supply port. The first end of the static air return pipeline is connected to the air return port, and the second end is connected to the static air mixing pipeline. The static air supply pipeline and the static air return pipeline are respectively provided with a static air supply solenoid valve and a static air return solenoid valve; the static air intake system also includes a vacuum pump, which is connected to the static exhaust pipeline. The static air intake solenoid valve, the static exhaust solenoid valve, the static air mixing solenoid valve, the static air supply solenoid valve, the static air return solenoid valve and the vacuum pump are all communicatively connected to the controller of the adsorption instrument.
[0010] In the specific implementation of the above-mentioned gravimetric adsorption instrument based on a magnetic suspension balance, the static air intake pipeline includes a first static air intake pipeline, a second static air intake pipeline and a third static air intake pipeline, and the first static air intake pipeline, the second static air intake pipeline and the third static air intake pipeline are respectively provided with a first static air intake solenoid valve, a second static air intake solenoid valve and a third static air intake solenoid valve, and the first static air intake pipeline, the second static air intake solenoid valve and the third static air intake pipeline are all connected to the static air mixing pipeline; a mixing pump is also provided on the static air mixing pipeline, and a first static closed solenoid valve, a second static closed solenoid valve and a third static air mixing pipeline are also provided on the static air mixing pipeline in sequence. Valve and a third static closed solenoid valve and a first accommodating chamber, a second accommodating chamber and a third accommodating chamber, the third accommodating chamber is arranged between the third static closed solenoid valve and the second static closed solenoid valve, the second accommodating chamber is arranged between the second static closed solenoid valve and the first static closed solenoid valve, the first accommodating chamber is arranged between the first static closed solenoid valve and the static gas mixing solenoid valve, the gas mixing pump, the first static closed solenoid valve, the second static closed solenoid valve, the third static closed solenoid valve, the first static intake solenoid valve, the second static intake solenoid valve and the third static intake solenoid valve are all communicatively connected with the controller of the adsorption instrument.
[0011] In the specific embodiment of the above-mentioned gravimetric adsorption instrument based on a magnetic suspension balance, the adsorption instrument also includes a dynamic air intake system, the dynamic air intake system includes a dynamic air intake pipeline, the dynamic air intake pipeline is connected to an air source, the dynamic air intake pipeline includes a first dynamic air intake pipeline and at least one second dynamic air intake pipeline, the first dynamic air intake pipeline and the second dynamic air intake pipeline are respectively provided with a first mass flow controller, a first dynamic air intake solenoid valve, a second mass flow controller, and a second dynamic air intake solenoid valve; the dynamic air intake system also includes a dynamic exhaust pipeline, the dynamic exhaust pipeline is provided with a dynamic exhaust solenoid valve, the dynamic exhaust pipeline includes a dynamic high-pressure exhaust pipeline and a dynamic low-pressure exhaust pipeline, the dynamic high-pressure exhaust pipeline is provided with a dynamic high-pressure exhaust solenoid valve and a first back-pressure pressure controller, the dynamic low-pressure exhaust pipeline is provided with a dynamic low-pressure exhaust solenoid valve and a second back-pressure pressure controller; the dynamic The air intake system also includes a dynamic air supply pipeline and a dynamic air return pipeline, and the corresponding sample chamber includes an air supply port and an air return port. The first end of the dynamic air supply pipeline is connected to the dynamic air intake pipeline, and the second end is connected to the air supply port. The first end of the dynamic air return pipeline is connected to the air return port, and the second end is connected to the dynamic exhaust pipeline. The dynamic air supply pipeline and the dynamic air return pipeline are respectively provided with a dynamic air supply solenoid valve and a dynamic air return solenoid valve. The dynamic air intake system also includes a vacuum pump, which is connected to the dynamic exhaust pipeline. The first mass flow controller, the first dynamic air intake solenoid valve, the second mass flow controller, the second dynamic air intake solenoid valve, the dynamic exhaust solenoid valve, the dynamic high-pressure exhaust solenoid valve, the first back pressure pressure controller, the dynamic low-pressure exhaust solenoid valve, the second back pressure pressure controller and the vacuum pump are all communicatively connected to the controller of the adsorption instrument.
[0012] In the above-mentioned specific embodiment of the gravimetric adsorption instrument based on the magnetic suspension balance, the dynamic air intake system also includes an evaporator, which is arranged on the dynamic air intake pipeline, and the dynamic air intake system also includes a dynamic liquid inlet pipeline, which is connected to a liquid source, and the dynamic liquid inlet pipeline includes a first dynamic liquid inlet pipeline and at least one second dynamic liquid inlet pipeline, and the first dynamic liquid inlet pipeline and the second dynamic liquid inlet pipeline are respectively provided with a first high-pressure liquid pump, a first dynamic liquid inlet solenoid valve and a second high-pressure liquid pump, and a second dynamic liquid inlet solenoid valve, and the dynamic liquid inlet pipeline is connected to the evaporator; the dynamic air intake system also includes a cold trap, and the first end of the cold trap is connected to the dynamic exhaust pipeline after passing through the first cold trap solenoid valve, and the second end is connected to the dynamic exhaust pipeline after passing through the second cold trap solenoid valve, and the first high-pressure liquid pump, the first dynamic liquid inlet solenoid valve, the second high-pressure liquid pump, the second dynamic liquid inlet solenoid valve, the first cold trap solenoid valve and the second cold trap solenoid valve are all communicatively connected to the controller of the adsorption instrument.
[0013] In the above-mentioned specific embodiment of the gravimetric adsorption instrument based on the magnetic suspension balance, the dynamic air intake system also includes a connecting pipeline for connecting the dynamic air intake pipeline and the dynamic exhaust pipeline, and a connecting solenoid valve is provided on the connecting pipeline, and the connecting solenoid valve is communicatively connected to the controller of the adsorption instrument.
[0014] The present invention also provides a control method for a gravimetric adsorption instrument based on a magnetic levitation balance, wherein the gravimetric adsorption instrument is the gravimetric adsorption instrument described in the above-mentioned embodiment, and the adsorption instrument also includes an air intake system, wherein the air intake system includes a vacuum pump, and the vacuum pump is communicatively connected to the controller of the adsorption instrument, and the control method includes: controlling the magnetic levitation system to be reset; controlling the microbalance reading and obtaining the initial weight of the sample; controlling the vacuum pump to start and last for a first preset time; controlling the air intake system to intake air to adsorb the sample; controlling the microbalance reading and obtaining the weight of the sample after adsorption; obtaining the adsorption amount and adsorption speed of the sample based on the weight of the sample after adsorption and the initial weight; controlling the microbalance reading and obtaining the weight of the sedimentation plate after the system is aired; obtaining the weight change of the sedimentation plate and obtaining the fluid density based on the weight change of the sedimentation plate; and performing adsorption kinetics and adsorption isotherm analysis based on the obtained data.
[0015] In a specific implementation of the above-mentioned control method for a gravimetric adsorption instrument based on a magnetic suspension balance, the adsorption instrument also includes a static air intake system, the static air intake system includes a static air intake pipeline, a static exhaust pipeline and a static air mixing pipeline connected end to end, the first end of the static air intake pipeline is connected to an air source, and the second end is connected to the static air mixing pipeline, the first end of the static exhaust pipeline is connected to the static air mixing pipeline, and the second end is connected to an exhaust port, the static air intake pipeline, the static exhaust pipeline and the static air mixing pipeline are respectively provided with a static air intake solenoid valve, a static exhaust solenoid valve and a static air mixing solenoid valve; the static air intake system also includes a static air supply pipeline and a static air return pipeline, and the corresponding sample chamber includes an air supply pipeline. The static air intake system further comprises a vacuum pump, wherein the vacuum pump is connected to the static exhaust pipe, and the static air intake solenoid valve, the static exhaust solenoid valve, the static air mixing solenoid valve, the static air supply solenoid valve, the static air return solenoid valve and the vacuum pump are all connected to the controller of the adsorption instrument in a communication manner. The control method comprises: controlling the first magnetic device to be energized and Generate a first magnetic force, so that the first connecting block moves to a suspended state in the connecting frame driven by the second magnetic device, read the reading of the microbalance, and control the magnetic suspension system to reset; control the first magnetic device to be powered on and generate a second magnetic force, the first connecting block moves a certain distance in the connecting frame driven by the second magnetic device and then abuts against the connecting frame, and drives the connecting frame and the sample to move to a suspended state; control the reading of the microbalance and obtain the initial weight of the sample; control the static exhaust solenoid valve, the static mixing solenoid valve, the static air supply solenoid valve and the static air return solenoid valve to open, control the static air intake solenoid valve to close, and control the vacuum pump to start and lasts for a first preset time; controlling the static exhaust solenoid valve, the static air supply solenoid valve and the static air return solenoid valve to close, and controlling the static air intake solenoid valve to open so that the static air intake system reaches a target pressure; controlling the static air supply solenoid valve and the static air return solenoid valve to open so that the gas and the sample are adsorbed; controlling the first magnetic device to be energized and generate a second magnetic force, and the first connecting block moves a certain distance in the connecting frame driven by the second magnetic device and then abuts against the connecting frame, and drives the connecting frame and the sample to move to a suspended state, and then controlling the microbalance reading and obtaining the weight of the sample after adsorption; obtaining the adsorption amount and adsorption speed of the sample based on the weight of the sample after adsorption and the initial weight;The first magnetic device is controlled to be powered on and generate a third magnetic force. The second connecting block moves a certain distance driven by the second magnetic device and then abuts against the connecting hole of the sinker, and drives the sinker to move to a suspended state. Then the microbalance reading is controlled to obtain the weight of the sinker after the system is air-intaken; the weight change of the sinker is obtained and the fluid density is obtained based on the weight change of the sinker; adsorption kinetics and adsorption isotherm analysis are performed based on the obtained data. ;
[0016] In a specific implementation of the above-mentioned control method for a gravimetric adsorption instrument based on a magnetic suspension balance, the static air intake pipeline includes a first static air intake pipeline, a second static air intake pipeline and a third static air intake pipeline, and the first static air intake pipeline, the second static air intake pipeline and the third static air intake pipeline are respectively provided with a first static air intake solenoid valve, a second static air intake solenoid valve and a third static air intake solenoid valve, and the first static air intake pipeline, the second static air intake solenoid valve and the third static air intake pipeline are all connected to the static air mixing pipeline; a mixing pump is also provided on the static air mixing pipeline, and a first static closed solenoid valve, a second static closed solenoid valve and a third static air mixing pipeline are also provided on the static air mixing pipeline in sequence. The first static closed solenoid valve and the first accommodating chamber, the second accommodating chamber and the third accommodating chamber, the third accommodating chamber is arranged between the third static closed solenoid valve and the second static closed solenoid valve, the second accommodating chamber is arranged between the second static closed solenoid valve and the first static closed solenoid valve, the first accommodating chamber is arranged between the first static closed solenoid valve and the static gas mixing solenoid valve, the gas mixing pump, the first static closed solenoid valve, the second static closed solenoid valve, the third static closed solenoid valve, the first static air intake solenoid valve, the second static air intake solenoid valve and the third static air intake solenoid valve are all connected to the controller of the adsorption instrument in communication, and the step of "controlling the microbalance reading and obtaining the sample After the initial weight of the product, the following further includes: controlling the static exhaust solenoid valve, the static mixing solenoid valve, the static air supply solenoid valve, the static air return solenoid valve, the first static closed solenoid valve, the second static closed solenoid valve and the third static closed solenoid valve to open, controlling the first static intake solenoid valve, the second static intake solenoid valve and the third static intake solenoid valve to close, and then controlling the vacuum pump to open and continue for a first preset time; controlling the static exhaust solenoid valve, the static air supply solenoid valve, the static air return solenoid valve and the third static closed solenoid valve to close, and controlling the third static intake solenoid valve to open so that the third accommodating chamber reaches a third preset pressure; controlling the static exhaust solenoid valve valve, the static mixing solenoid valve and the first static closed solenoid valve are opened, the third static intake solenoid valve, the second static closed solenoid valve and the third static closed solenoid valve are controlled to be closed, and then the vacuum pump is controlled to be opened and maintained for a first preset time; the static exhaust solenoid valve is controlled to be closed, and the second static intake solenoid valve is controlled to be opened so that the second accommodating chamber reaches a second preset pressure; the static exhaust solenoid valve is controlled to be opened, and the second static intake solenoid valve and the first static closed solenoid valve are controlled to be closed, and then the vacuum pump is controlled to be opened and maintained for a first preset time; the static exhaust solenoid valve is controlled to be closed, and the first static intake solenoid valve is controlled to be opened so that the first accommodating chamber reaches a first preset pressure;Control the static gas mixing solenoid valve to close, control the static exhaust solenoid valve to open, and then control the vacuum pump to open and last for a first preset time; control the static gas mixing solenoid valve, the first static closed solenoid valve, the second static closed solenoid valve and the third static closed solenoid valve to open, control the gas mixing pump to open and last for a first preset time; control the static gas supply solenoid valve and the static gas return solenoid valve to open, so that the gas and the sample are adsorbed. ;
[0017] In a specific implementation of the above-mentioned control method for a gravimetric adsorption instrument based on a magnetic suspension balance, the adsorption instrument also includes a dynamic air intake system, the dynamic air intake system includes a dynamic air intake pipeline, the dynamic air intake pipeline is connected to an air source, the dynamic air intake pipeline includes a first dynamic air intake pipeline and at least one second dynamic air intake pipeline, the first dynamic air intake pipeline and the second dynamic air intake pipeline are respectively provided with a first mass flow controller, a first dynamic air intake solenoid valve and a second mass flow controller, and a second dynamic air intake solenoid valve; the dynamic air intake system also includes a dynamic exhaust pipeline, the dynamic exhaust pipeline is provided with a dynamic exhaust solenoid valve, and the dynamic exhaust pipeline includes a dynamic high-pressure exhaust. pipeline and a dynamic low-pressure exhaust pipeline, the dynamic high-pressure exhaust pipeline is provided with a dynamic high-pressure exhaust solenoid valve and a first back-pressure pressure controller, the dynamic low-pressure exhaust pipeline is provided with a dynamic low-pressure exhaust solenoid valve and a second back-pressure pressure controller; the dynamic intake system also includes a dynamic air supply pipeline and a dynamic air return pipeline, the corresponding sample chamber includes an air supply port and an air return port, the first end of the dynamic air supply pipeline is connected to the dynamic intake pipeline, and the second end is connected to the air supply port, the first end of the dynamic air return pipeline is connected to the air return port, and the second end is connected to the dynamic exhaust pipeline, the dynamic air supply pipeline and the dynamic air return pipeline are respectively provided with a dynamic air supply solenoid valve and a dynamic air return solenoid valve. valve, the dynamic air intake system also includes a vacuum pump, the vacuum pump is connected to the dynamic exhaust pipeline, the first mass flow controller, the first dynamic air intake solenoid valve, the second mass flow controller, the second dynamic air intake solenoid valve, the dynamic exhaust solenoid valve, the dynamic high-pressure exhaust solenoid valve, the first back pressure controller, the dynamic low-pressure exhaust solenoid valve, the second back pressure controller and the vacuum pump are all connected to the controller of the adsorption instrument in communication, and the control method includes: controlling the first magnetic device to be energized and generate a first magnetic force, so that the first connecting block moves to a suspended state in the connecting frame under the drive of the second magnetic device, and reading the trace sky The first magnetic device is energized to generate a second magnetic force, and the first connecting block moves a certain distance in the connecting frame driven by the second magnetic device and then abuts against the connecting frame, and drives the connecting frame and the sample to move to a suspended state, and then controls the microbalance reading and obtains the initial weight of the sample; the first dynamic air intake solenoid valve and the second dynamic air intake solenoid valve are controlled to be closed, and the dynamic exhaust solenoid valve, the dynamic high-pressure exhaust solenoid valve, the dynamic low-pressure exhaust solenoid valve, the dynamic air supply solenoid valve and the dynamic air return solenoid valve are controlled to be opened, and then the vacuum pump is controlled to be turned on and last for a first preset time;Control the first dynamic air intake solenoid valve and / or the second dynamic air intake solenoid valve to open, control the flow of the first dynamic air intake pipeline and / or the second dynamic air intake pipeline through the first mass flow controller and / or the second mass flow controller, and control the dynamic air supply solenoid valve and the dynamic air return solenoid valve to open so that the gas and the sample are adsorbed; control the dynamic high-pressure exhaust solenoid valve and / or the dynamic low-pressure exhaust solenoid valve to open, control the vacuum pump to open, and adjust the pressure of the dynamic air intake system through the first back pressure controller and / or the second back pressure controller; obtain the set pressure of the dynamic air intake system and compare the set pressure with the first preset pressure value; if the set pressure of the dynamic air intake system is higher than the first preset pressure value, control the dynamic high-pressure exhaust solenoid valve to open and the dynamic low-pressure exhaust solenoid valve to close, and adjust the pressure of the dynamic air intake system through the first back pressure controller; if the set pressure of the dynamic air intake system is not higher than the first preset pressure value, control the dynamic low pressure The exhaust solenoid valve is opened, the dynamic high-pressure exhaust solenoid valve is closed, and the vacuum pump is turned on, and the pressure of the dynamic air intake system is adjusted by the second back pressure controller; the first magnetic device is controlled to be energized and generate the second magnetic force, and the first connecting block moves a certain distance in the connecting frame driven by the second magnetic device and then abuts on the connecting frame, and drives the connecting frame and the sample to move to a suspended state; the microbalance reading is controlled and the weight of the sample after adsorption is obtained; the adsorption amount and adsorption speed of the sample are obtained based on the weight of the sample after adsorption and the initial weight; the first magnetic device is controlled to be energized and generate the third magnetic force, and the second connecting block moves a certain distance driven by the second magnetic device and then abuts on the connecting hole of the sinker, and drives the sinker to move to a suspended state; the microbalance reading is controlled and the weight of the sinker after the system is air-intaken; the weight change of the sinker is obtained and the fluid density is obtained based on the weight change of the sinker; adsorption kinetics and adsorption isotherm analysis are performed based on the obtained data. ;
[0018] In a specific implementation of the above-mentioned control method for a gravimetric adsorption instrument based on a magnetic suspension balance, the dynamic air intake system also includes an evaporator, and the evaporator is arranged on the dynamic air intake pipeline. The dynamic air intake system also includes a dynamic liquid inlet pipeline, and the dynamic liquid inlet pipeline is connected to a liquid source. The dynamic liquid inlet pipeline includes a first dynamic liquid inlet pipeline and at least one second dynamic liquid inlet pipeline. The first dynamic liquid inlet pipeline and the second dynamic liquid inlet pipeline are respectively provided with a first high-pressure liquid pump, a first dynamic liquid inlet solenoid valve and a second high-pressure liquid pump, and a second dynamic liquid inlet solenoid valve, and the dynamic liquid inlet pipeline is connected to the evaporator; the dynamic air intake system also includes a cold trap, and the first end of the cold trap passes through the first cold trap. The first end of the electromagnetic valve is connected to the dynamic exhaust pipeline, and the second end is connected to the dynamic exhaust pipeline after passing through the second cold trap electromagnetic valve. The first high-pressure liquid pump, the first dynamic liquid inlet electromagnetic valve, the second high-pressure liquid pump, the second dynamic liquid inlet electromagnetic valve, the first cold trap electromagnetic valve and the second cold trap electromagnetic valve are all connected to the controller of the adsorption instrument in communication. After the step of "controlling the microbalance reading and obtaining the initial weight of the sample", it also includes: controlling the first dynamic air inlet electromagnetic valve, the second dynamic air inlet electromagnetic valve, the first dynamic liquid inlet electromagnetic valve, the second dynamic liquid inlet electromagnetic valve, the first cold trap electromagnetic valve and the second cold trap electromagnetic valve to close, controlling the dynamic exhaust electromagnetic valve, the dynamic The high-pressure exhaust solenoid valve, the dynamic low-pressure exhaust solenoid valve, the dynamic air supply solenoid valve and the dynamic air return solenoid valve are opened; the vacuum pump is controlled to be turned on and last for a first preset time; the first dynamic liquid inlet solenoid valve and / or the second dynamic liquid inlet solenoid valve are controlled to be opened, and the liquid is pumped into the evaporator through the first high-pressure liquid pump and / or the second high-pressure liquid pump; the first dynamic air intake solenoid valve and / or the second dynamic air intake solenoid valve are controlled to be opened, and the flow of the first dynamic air intake pipeline and the second dynamic air intake pipeline is controlled through the first mass flow controller and the second mass flow controller, and the dynamic air supply solenoid valve and the dynamic air return solenoid valve are controlled to be opened so that the gas and the sample are released. adsorption; controlling the dynamic exhaust solenoid valve to close, and controlling the first cold trap solenoid valve and the second cold trap solenoid valve to open; obtaining the set pressure of the dynamic intake system; if the set pressure of the dynamic intake system is higher than the first preset pressure value, controlling the dynamic high-pressure exhaust solenoid valve to open, the dynamic low-pressure exhaust solenoid valve to close, and the vacuum pump to open, and adjusting the pressure of the dynamic intake system by the first back-pressure pressure controller; if the set pressure of the dynamic intake system is not higher than the first preset pressure value, controlling the dynamic low-pressure exhaust solenoid valve to open, the dynamic high-pressure exhaust solenoid valve to close, and the vacuum pump to open, and adjusting the pressure of the dynamic intake system by the second back-pressure pressure controller.
[0019] In a specific embodiment of the above-mentioned control method for a gravimetric adsorption instrument based on a magnetic suspension balance, the dynamic air intake system also includes a connecting pipeline for connecting the dynamic air intake pipeline and the dynamic exhaust pipeline, and a connecting solenoid valve is provided on the connecting pipeline, and the connecting solenoid valve is communicatively connected to the controller of the adsorption instrument. The control method also includes: controlling the first dynamic air intake solenoid valve, the second dynamic air intake solenoid valve, the first dynamic liquid inlet solenoid valve, the second dynamic liquid inlet solenoid valve, the first cold trap solenoid valve, the second cold trap solenoid valve, the dynamic air supply solenoid valve and the dynamic air return solenoid valve to close, controlling the dynamic exhaust solenoid valve, the dynamic high-pressure exhaust solenoid valve, the dynamic low-pressure exhaust solenoid valve and the connecting solenoid valve to open; controlling the vacuum pump to start and last for a first preset time.
[0020] In a specific embodiment of the above-mentioned control method for a gravimetric adsorption instrument based on a magnetic suspension balance, the adsorption instrument further includes a temperature acquisition device and a pressure acquisition device, and the temperature acquisition device and the pressure acquisition device are communicatively connected to the controller of the adsorption instrument, and the step of "performing adsorption kinetics and adsorption isotherm analysis based on the acquired data" further includes: controlling the temperature acquisition device to obtain the adsorption temperature of the sample; controlling the pressure acquisition device to obtain the adsorption pressure of the sample; performing adsorption kinetics analysis on the sample based on the adsorption temperature, adsorption pressure and adsorption rate of the sample; and performing adsorption isotherm analysis on the sample based on the adsorption amount of the sample and the fluid density of the gas after the adsorption is completed.
[0021] In a specific implementation of the above-mentioned control method for a gravimetric adsorption instrument based on a magnetic suspension balance, the adsorption instrument further includes a temperature acquisition device and a pressure acquisition device, and the temperature acquisition device and the pressure acquisition device are communicatively connected to the controller of the adsorption instrument, and the step of "obtaining the weight change of the sedimentation plate and obtaining the fluid density based on the weight change of the sedimentation plate" also includes: obtaining the proportion of various types of gas after adsorption is completed based on the fluid density, adsorption temperature, adsorption pressure and gas type of the gas after adsorption is completed; obtaining the set pressure of the static air intake system; obtaining the required air replenishment amount of various types of gas based on the set pressure of the static air intake system; replenishing the static air intake system based on the required air replenishment amount of various types of gas.
[0022] The technical effect of the present invention is as follows: the gravimetric adsorption instrument based on a magnetic levitation balance of the present invention improves the existing microbalance into a magnetic levitation balance, which includes a first part arranged outside the sample chamber and a second part arranged inside the sample chamber, and the first part and the second part are connected by magnetic force. On the basis of realizing accurate weighing of the sample in the sample chamber, it also avoids setting the circuit part of the microbalance inside the sample chamber, thereby isolating the circuit part of the microbalance from the complex atmosphere in the sample chamber, avoiding its contact with corrosive gases, steam and flammable and explosive gases, and also avoiding it from being subjected to high temperature, low temperature and high pressure. Therefore, the adsorption instrument of the present invention can realize the adsorption test of the sample on corrosive gases, steam and flammable and explosive gases under high temperature, low temperature or high pressure, greatly improving the application range of the adsorption instrument, and solving the problem that the microbalance of the existing gravimetric adsorption instrument has many limitations on the application range of the adsorption instrument. BRIEF DESCRIPTION OF THE DRAWINGS
[0023] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings, in which:
[0024] Figure 1 It is a structural schematic diagram of the magnetic suspension balance of the present invention when it is reset to zero;
[0025] Figure 2 It is a structural schematic diagram of the magnetic suspension balance of the present invention when measuring the weight of a sample;
[0026] Figure 3 It is a structural schematic diagram of the magnetic suspension balance of the present invention when measuring the weight of the sinker;
[0027] Figure 4 It is a connection relationship diagram of the static air intake system of the present invention, the sample tube and the magnetic suspension balance;
[0028] Figure 5 It is a connection relationship diagram of the dynamic air intake system of the present invention, the sample tube and the magnetic suspension balance;
[0029] Figure 6 This is the main flow chart of Embodiment 6 of the present invention;
[0030] Figure 7 is a flowchart of step S01 in embodiment 6 of the present invention;
[0031] Figure 8 is a flowchart of step S02 in embodiment 6 of the present invention;
[0032] Fig. 9 is a flowchart of step S03 in embodiment 6 of the present invention;
[0033] Fig.10 is a flowchart of step S04 in embodiment 6 of the present invention;
[0034] Fig.11 is a flowchart of step S05 in embodiment 6 of the present invention;
[0035] Fig.12 is a flowchart of step S07 in embodiment 6 of the present invention;
[0036] Fig.13 is a flowchart of step S09 in embodiment 6 of the present invention;
[0037] Fig.14 This is the main flow chart of Embodiment 7 of the present invention;
[0038] Fig.15 This is a flow chart after step S08 in the seventh embodiment of the present invention;
[0039] Fig.16 This is the main flow chart of Embodiment 8 of the present invention;
[0040] Fig.17 This is the main flow chart of Embodiment 9 of the present invention;
[0041] Fig.18 is a main flow chart of Embodiment 10 of the present invention;
[0042] Fig.19 It is a flowchart of step SN in embodiment eight of the present invention.
[0043] List of reference numerals:
[0044] 1-magnetic suspension system; 11-microbalance; 12-first magnetic device; 13-second magnetic device; 2-sample chamber; 21-crucible; 22-second connecting block; 23-sinking plate; 231-connecting hole; 232-sinking plate bracket; 24-connecting frame; 241-connecting frame bracket; 25-first connecting block; 26-air supply port; 27-air return port; 3-static air intake system; 31-first static air intake pipeline; 311-first static air intake solenoid valve; 32-second static air intake pipeline; 321-second static air intake solenoid valve; 33-third static Intake pipeline; 331-third static intake solenoid valve; 34-static mixing pipeline; 341-static mixing solenoid valve; 342-mixing pump; 343-first static closed solenoid valve; 344-second static closed solenoid valve; 345-third static closed solenoid valve; 346-first accommodating chamber; 347-second accommodating chamber; 348-third accommodating chamber; 35-static exhaust pipeline; 351-static exhaust solenoid valve; 36-static air supply pipeline; 361-static air supply solenoid valve; 37-static return air pipeline; 371-static return air solenoid valve; 4-dynamic Intake system; 41-first dynamic intake pipeline; 411-first mass flow controller; 412-first dynamic intake solenoid valve; 42-second dynamic intake pipeline; 421-second mass flow controller; 422-second dynamic intake solenoid valve; 43-dynamic exhaust pipeline; 431-dynamic exhaust solenoid valve; 432-dynamic high-pressure exhaust pipeline; 4321-dynamic high-pressure exhaust solenoid valve; 4322-first back pressure controller; 433-dynamic low-pressure exhaust pipeline; 4331-dynamic low-pressure exhaust solenoid valve; 4332-second back pressure controller device; 44-dynamic air supply pipeline; 441-dynamic air supply solenoid valve; 45-dynamic return air pipeline; 451-dynamic return air solenoid valve; 46-evaporator; 47-first dynamic liquid inlet pipeline; 471-first high-pressure liquid pump; 472-first dynamic liquid inlet solenoid valve; 48-second dynamic liquid inlet pipeline; 481-second high-pressure liquid pump; 482-second dynamic liquid inlet solenoid valve; 49-cold trap; 491-first cold trap solenoid valve; 492-second cold trap solenoid valve; 40-connecting pipeline; 401-connecting solenoid valve; 5-vacuum pump; 6-magnetic suspension balance. DETAILED DESCRIPTION
[0045] The preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only used to explain the technical principles of the present invention and are not intended to limit the scope of protection of the present invention. Those skilled in the art can make adjustments as needed to adapt to specific applications. In addition, the adsorption instrument mentioned in the present invention includes both a physical adsorption instrument and a chemical adsorption instrument.
[0046] It should be noted that in the description of the present invention, the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer" and the like indicating directions or positional relationships are based on the directions or positional relationships shown in the drawings, which are only for the convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed and operated in a specific orientation, and therefore cannot be understood as limiting the present invention. In addition, the terms "first", "second", and "third" are used for descriptive purposes only, and cannot be understood as indicating or implying relative importance.
[0047] In addition, it should be noted that in the description of the present invention, unless otherwise clearly specified and limited, the terms "installed", "connected", and "connected" should be understood in a broad sense, for example, it can be a fixed connection, a detachable connection, or an integral connection; it can be a mechanical connection or an electrical connection; it can be a direct connection, or it can be indirectly connected through an intermediate medium, or it can be the internal communication of two components. For those skilled in the art, the specific meanings of the above terms in the present invention can be understood according to specific circumstances.
[0048] Embodiment 1
[0049] like Figure 1-Figure 3 As shown, in order to solve the problem that the microbalance 11 of the existing gravimetric adsorption instrument has many limitations on the application scope of the adsorption instrument, the gravimetric adsorption instrument of the present invention includes a magnetic suspension balance 6, and the magnetic suspension balance 6 includes:
[0050] The sample chamber 2 includes a crucible 21 for placing a sample to be tested. The crucible 21 is connected to the second connecting block 22 at the top. The second connecting block 22 is provided with a sinker 23 at the bottom of the sinker 23. The second connecting block 22 will abut against the connecting hole 231 after moving upward for a distance. A sinker bracket 232 is provided near the sinker 23 for supporting the sinker 23 when the sinker 23 is not pulled up. Above the sedimentation plate 23 are a connecting frame 24 and a first connecting block 25. The first connecting block 25 is inside the connecting frame 24. The first connecting block 25 is connected to the second magnetic device 13. The connecting frame 24 is connected to the second connecting block 22 and the crucible 21. A connecting frame bracket 241 is also provided near the connecting frame 24. The first connecting block 25 can move up and down in the connecting frame 24 and abut against the upper edge of the connecting frame 24 after moving upward for a distance, or it can be in a suspended state in the connecting frame 24. The sample chamber 2 also includes an air supply port 26 and an air return port 27. The air supply port 26 is used to deliver test gas into the sample chamber 2, and the air return port 27 is used to discharge the test gas. The top of the sample chamber 2 is copper and the inside is gold-plated, and the other parts are made of stainless steel. Since copper is non-magnetic, it will not affect the first magnetic device 12 and the second magnetic device 13. The copper partition is resistant to corrosion after gold plating. At the same time, due to the high temperature resistance of metal materials such as copper, gold, and stainless steel, the entire sample chamber 2 can withstand high pressure, high temperature and corrosive gases.
[0051] The magnetic suspension system 1 includes a microbalance 11 and a first magnetic device 12 arranged outside the sample chamber 2. The first magnetic device 12 is an electromagnetic force device (generates magnetic force when powered on and disappears when powered off). The first magnetic device 12 is connected to the microbalance 11 of the magnetic suspension system 1 and also includes a second magnetic device 13 arranged inside the sample chamber 2 and connected to the sample.
[0052] In the case of adopting the above embodiment, before the adsorption test of the sample is performed, the magnetic suspension system 1 is firstly cleared and calibrated, the first magnetic device 12 is energized to generate magnetic force, and the second magnetic device 13 drives the first connection block 25 to move upward in the connection frame 24 to a suspended state under the action of the magnetic force. At this time, the magnetic suspension system 1 is controlled to be cleared, or the CAL weight built into the balance is used for calibration. After the clearing is completed, the magnetic force of the first magnetic device 12 is increased to make the first connection block 25 abut against the connection frame 24 (such as Figure 2As shown in the figure, the connection frame 24, the second connection block 22, the crucible 21 and the sample in the crucible 21 move upward to detach from the connection frame bracket 241 and hang in the air. At this time, the reading A1 of the microbalance 11 minus the weight of the connection frame 24, the second connection block 22 and the crucible 21 (the known quantity D measured before the test) can be used to obtain the initial weight M0 of the sample. Then, an adsorption test is performed on the sample. After the adsorption test, the first magnetic device 12 is energized. The first connection block 25 abuts against the connection frame 24 and drives the connection frame 24, the second connection block 22 and the crucible 21 to move upward to detach from the connection frame bracket 241 and hang in the air. At this time, the difference between the reading A2 of the microbalance 11 and the reading A1 of the aforementioned microbalance 11 is the adsorption weight of the sample (or A2 minus D can be used to obtain the weight M1 of the sample after adsorption, and M1 minus M0). Then, the magnetic force of the first magnetic device 12 is increased to make the first magnetic device 12 have a magnetic field. The two connecting blocks 22 abut against the sinker 23 and drive the sinker 23 to move to a suspended state. At this time, the difference between the readings A3 and A2 of the microbalance 11 is the weight of the sinker 23. Since the volume and weight of the sinker 23 are known quantities calibrated in advance, when the sinker 23 is in different fluid atmospheres (which can be gas, supercritical fluid, liquid, etc.), the measured weight change of the sinker 23 will change with the gas density in the atmosphere. Therefore, the fluid density of the adsorbed gas can be reversely calculated through the weight change of the sinker 23.
[0053] The advantage of the above embodiment is that the gravimetric adsorption instrument of the present invention improves the magnetic suspension system 1 to include a first part arranged outside the sample chamber 2 and a second part arranged inside the sample chamber 2, and the first part and the second part are connected by magnetic force. On the basis of achieving accurate weighing of the sample in the sample chamber 2, it also avoids setting the circuit part of the magnetic suspension system 1 inside the sample chamber 2, thereby isolating the circuit part of the magnetic suspension system 1 from the complex atmosphere in the sample chamber 2, avoiding its contact with corrosive gases, steam and flammable and explosive gases, and also avoiding it from being subjected to high temperature, low temperature and high pressure. Therefore, the adsorption instrument of the present invention can realize the adsorption test of samples on corrosive gases, steam and flammable and explosive gases under high temperature, low temperature or high pressure, greatly improving the application range of the adsorption instrument, and solving the problem that the magnetic suspension system 1 of the existing gravimetric adsorption instrument has many limitations on the application range of the adsorption instrument.
[0054] Embodiment 2
[0055] like Figure 1-Figure 4As shown, the adsorption instrument of the present invention also includes a static air intake system 3, which includes a static air intake pipeline (refer to the first static air intake pipeline 31), a static exhaust pipeline 35 and a static air mixing pipeline 34 connected end to end. The first end of the static air intake pipeline is connected to the air source, and the second end is connected to the static air mixing pipeline 34. The first end of the static exhaust pipeline 35 is connected to the static air mixing pipeline 34, and the second end is connected to the exhaust port. The static air intake pipeline, the static exhaust pipeline 35 and the static air mixing pipeline 34 are respectively provided with a static air intake solenoid valve, a static exhaust solenoid valve 351 and a static air mixing solenoid valve 341; the static air intake system 3 also includes a static air supply pipeline 36 and a static air return pipeline 37, and the corresponding sample chamber 2 It includes an air supply port 26 and an air return port 27. The first end of the static air supply pipeline 36 is connected to the static air mixing pipeline 34, and the second end is connected to the air supply port 26. The first end of the static air return pipeline 37 is connected to the air return port 27, and the second end is connected to the static air mixing pipeline 34. The static air supply pipeline 36 and the static air return pipeline 37 are respectively provided with a static air supply solenoid valve 361 and a static air return solenoid valve 371; the static air intake system 3 also includes a vacuum pump 5, which is connected to the static exhaust pipeline 35. The static air intake solenoid valve, the static exhaust solenoid valve 351, the static air mixing solenoid valve 341, the static air supply solenoid valve 361, the static air return solenoid valve 371 and the vacuum pump 5 are all connected to the controller of the adsorption instrument for communication.
[0056] Embodiment 3
[0057] Further, such as Figure 1-Figure 4As shown, the static air intake pipeline includes a first static air intake pipeline 31, a second static air intake pipeline 32 and a third static air intake pipeline 33, and the first static air intake pipeline 31, the second static air intake pipeline 32 and the third static air intake pipeline 33 are respectively provided with a first static air intake solenoid valve 311, a second static air intake solenoid valve 321 and a third static air intake solenoid valve 331, the first static air intake pipeline 31, the second static air intake pipeline 32 and the third static air intake pipeline 33 are all connected to a static air mixing pipeline 34, a mixing pump 342 is further provided on the static air mixing pipeline 34, and a first static closed solenoid valve 343, a second static closed solenoid valve 344 and a third static closed solenoid valve 345 are also sequentially provided on the static air mixing pipeline 34. As well as the first accommodating chamber 346, the second accommodating chamber 347 and the third accommodating chamber 348, the third accommodating chamber 348 is arranged between the third static closed solenoid valve 345 and the second static closed solenoid valve 344, the second accommodating chamber 347 is arranged between the second static closed solenoid valve 344 and the first static closed solenoid valve 343, the first accommodating chamber 346 is arranged between the first static closed solenoid valve 343 and the static gas mixing solenoid valve 341, the gas mixing pump 342, the first static closed solenoid valve 343, the second static closed solenoid valve 344, the third static closed solenoid valve 345, the first static air intake solenoid valve 311, the second static air intake solenoid valve 321 and the third static air intake solenoid valve 331 are all communicatively connected with the controller of the adsorption instrument.
[0058] Embodiment 4:
[0059] like Figure 1-Figure 3 , Figure 5As shown, the gravimetric adsorption instrument of the present invention also includes a dynamic air intake system 4, which includes a dynamic air intake pipeline, which is connected to an air source, and the dynamic air intake pipeline includes a first dynamic air intake pipeline 41 and at least one second dynamic air intake pipeline 42, and the first dynamic air intake pipeline 41 and the second dynamic air intake pipeline 42 are respectively provided with a first mass flow controller 411, a first dynamic air intake solenoid valve 412, a second mass flow controller 421, and a second dynamic air intake solenoid valve 422; the dynamic air intake system 4 also includes a dynamic exhaust pipeline 43, and the dynamic exhaust pipeline 43 is provided with a dynamic exhaust solenoid valve 431, and the dynamic exhaust pipeline 43 includes a dynamic high-pressure exhaust pipeline 432 and a dynamic low-pressure exhaust pipeline 433, and the dynamic high-pressure exhaust pipeline 432 is provided with a dynamic high-pressure exhaust solenoid valve 4321 and a first back-pressure pressure controller 4322, and the dynamic low-pressure exhaust pipeline 433 is provided with a dynamic low-pressure exhaust solenoid valve 4331 and a second back-pressure pressure controller 4332; The air intake system 4 also includes a dynamic air supply line 44 and a dynamic air return line 45. The corresponding sample chamber 2 includes an air supply port 26 and an air return port 27. The first end of the dynamic air supply line 44 is connected to the dynamic air intake line, and the second end is connected to the air supply port 26. The first end of the dynamic air return line 45 is connected to the air return port 27, and the second end is connected to the dynamic exhaust line 43. The dynamic air supply line 44 and the dynamic air return line 45 are respectively provided with a dynamic air supply solenoid valve 441 and a dynamic air return solenoid valve 451. The gas system 4 also includes a vacuum pump 5, which is connected to the dynamic exhaust pipeline 43. The first mass flow controller 411, the first dynamic air intake solenoid valve 412, the second mass flow controller 421, the second dynamic air intake solenoid valve 422, the dynamic exhaust solenoid valve 431, the dynamic high-pressure exhaust solenoid valve 4321, the first back-pressure pressure controller 4322, the dynamic low-pressure exhaust solenoid valve 4331, the second back-pressure pressure controller 4332 and the vacuum pump 5 are all communicatively connected to the controller of the adsorption instrument.
[0060] Embodiment 5
[0061] Further, such as Figure 5As shown, the dynamic air intake system 4 also includes an evaporator 46, which is arranged on the dynamic air intake pipeline. The dynamic air intake system 4 also includes a dynamic liquid inlet pipeline, which is connected to a liquid source. The dynamic liquid inlet pipeline includes a first dynamic liquid inlet pipeline 47 and at least one second dynamic liquid inlet pipeline 48. The first dynamic liquid inlet pipeline 47 and the second dynamic liquid inlet pipeline 48 are respectively provided with a first high-pressure liquid pump 471, a first dynamic liquid inlet solenoid valve 472, a second high-pressure liquid pump 481, and a second dynamic liquid inlet solenoid valve 482. The dynamic liquid inlet pipeline is connected to the evaporator 46; the dynamic air intake system 4 also includes a cold trap 49, a first end of the cold trap 49 is connected to the dynamic exhaust pipeline 43 after passing through a first cold trap solenoid valve 491, and a second end is connected to the dynamic exhaust pipeline 43 after passing through a second cold trap solenoid valve 492, a first high-pressure liquid pump 471, a first dynamic liquid inlet solenoid valve 472, a second high-pressure liquid pump 481, a second dynamic liquid inlet solenoid valve 482, a first cold trap solenoid valve 491 and a second cold trap solenoid valve 492 are all connected to the controller of the adsorption instrument for communication.
[0062] Furthermore, Figure 5 As shown, the dynamic intake system 4 also includes a connecting pipeline 40 for connecting the dynamic intake pipeline and the dynamic exhaust pipeline 43. A connecting solenoid valve 401 is provided on the connecting pipeline 40, and the connecting solenoid valve 401 is communicatively connected to the controller of the adsorption instrument.
[0063] In addition, regarding the static air intake system and the dynamic air intake system of the gravimetric adsorption instrument based on the magnetic suspension balance 6 of the present invention, those skilled in the art can understand that these two air intake systems enable various types of complex adsorption experiments to be carried out fully automatically and unattended; and users can carry out detailed and completely customized experimental processes to meet different testing requirements.
[0064] Embodiment 6
[0065] The present invention also provides a control method for a gravimetric adsorption instrument, wherein the gravimetric adsorption instrument is the gravimetric adsorption instrument in the above-mentioned embodiment 1 and embodiment 2, such as Figure 1-Figure 4 , Figure 6-Figure 12 As shown, the control method includes:
[0066] S01, control the magnetic suspension system 1 to reset;
[0067] S02, controlling the microbalance 11 to read and obtain the initial weight of the sample;
[0068] S03, controlling the vacuum pump 5 to start and continue for a first preset time;
[0069] S04, controlling the air intake of the air intake system to adsorb the sample;
[0070] S05, controlling the reading of the microbalance 11 and obtaining the weight of the sample after adsorption;
[0071] S06. Obtaining the adsorption amount and adsorption speed of the sample based on the weight of the sample after adsorption and the initial weight;
[0072] S07, controlling the reading of the microbalance 11 and obtaining the weight of the sinker 23 after the system is ventilated;
[0073] S08, obtaining a weight change of the sinker 23 and obtaining a fluid density based on the weight change of the sinker 23;
[0074] S09. Perform adsorption kinetics and adsorption isotherm analysis based on the acquired data.
[0075] In the above steps, step S01 further includes:
[0076] S011, control the first magnetic device 12 to be energized and generate a first magnetic force, so that the first connecting frame 25 is driven by the second magnetic device 13 to move to a suspended state in the connecting frame 24, read the reading of the microbalance 11, and control the magnetic suspension system 1 to be reset.
[0077] S02 further comprises:
[0078] S021, controlling the first magnetic device 12 to be energized and generate a second magnetic force, the first connecting frame 25 is driven by the second magnetic device 13 to move a certain distance in the connecting frame 24 and then abut against the connecting frame 24, and drives the connecting frame 24 and the sample to move to a suspended state;
[0079] S022. Control the microbalance 11 to read and obtain the initial weight of the sample.
[0080] Step S03 further includes:
[0081] S031, control the static exhaust solenoid valve 351, the static mixing solenoid valve 341, the static air supply solenoid valve 361 and the static air return solenoid valve 371 to open, control the static air intake solenoid valve to close, and control the vacuum pump 5 to open and continue for a first preset time.
[0082] Step S04 further includes:
[0083] S041, controlling the static exhaust solenoid valve 351, the static air supply solenoid valve 361 and the static air return solenoid valve 371 to close, and controlling the static air intake solenoid valve to open so that the static air intake system 3 reaches the target pressure;
[0084] S042, control the static gas supply solenoid valve 361 and the static gas return solenoid valve 371 to open so that the gas and the sample are adsorbed.
[0085] Step S05 further includes:
[0086] S051. Control the first magnetic device 12 to be energized and generate a second magnetic force. Driven by the second magnetic device 13, the first connecting frame 25 moves a certain distance in the connecting frame 24 and then abuts against the connecting frame 24, and drives the connecting frame 24 and the sample to move to a suspended state. Then, the microbalance 11 is controlled to read and obtain the weight of the sample after adsorption.
[0087] Step S07 further includes:
[0088] S071. Control the first magnetic device 12 to be energized and generate a third magnetic force. Driven by the second magnetic device 13, the second connecting block 22 moves a certain distance and then abuts against the connecting hole 231 of the sinker 23, and drives the sinker 23 to move to a suspended state. Then, control the reading of the microbalance 11 and obtain the weight of the sinker 23 after the system is ventilated.
[0089] In the case of adopting the above embodiment, firstly, the first magnetic device 12 is controlled to be powered on and generate the first magnetic force, the second magnetic device 13 moves upward under the attraction of the first magnetic force, and at the same time, the first connecting frame 25 is driven by the second magnetic device 13 to move to a suspended state in the connecting frame 24, the reading of the microbalance 11 is read, and the magnetic suspension system 1 is controlled to be reset, or the CAL weight built into the balance is used for calibration. After the balance is reset, the initial weight of the sample needs to be obtained, at this time, the first magnetic device 12 is controlled to be powered on and generate the second magnetic force, wherein the second magnetic force is greater than the first magnetic force, the first connecting frame 25 is driven by the second magnetic device 13 to move a distance in the connecting frame 24 and then abut on the connecting frame 24, and drive the connecting frame 24 and the sample to move to a suspended state, and the reading of the microbalance 11 is controlled, at this time, the reading A1 of the microbalance 11 minus the weight D of the connecting frame 24, the second connecting block 22 and the crucible 21 (known quantity measured before the test), and the initial weight M0 of the sample can be obtained.
[0090] Before injecting gas into the sample chamber 2, in order to ensure the accuracy of the adsorption test, it is also necessary to evacuate the entire static air intake system 3 and the sample chamber 2, control the static exhaust solenoid valve 351, the static mixing solenoid valve 341, the static air supply solenoid valve 361 and the static return air solenoid valve 371 to open, control the static air intake solenoid valve (with 311 as a reference) to close, and control the vacuum pump 5 to start and last for a first preset time (for example, 10 minutes or any other time). Since the vacuum pump 5 is connected to the static exhaust pipeline 35, the air in the static intake pipeline, the static exhaust pipeline 35, the static mixing pipeline 34 and the sample chamber 2 are all vacuumed out through the static exhaust pipeline 35, so that the entire static air intake system 3 and the sample chamber 2 are in a vacuum state. After the adsorption preparation stage is completed, the air intake system is controlled to intake air to adsorb the sample, the static exhaust solenoid valve 351, the static air supply solenoid valve 361 and the static air return solenoid valve 371 are controlled to be closed, and the static air intake solenoid valve is controlled to be opened, so that a specific type of gas enters the static mixing pipeline 34 from the static air intake pipeline, and at the same time, the gas in the static air intake system 3 reaches the target pressure, and then the static air supply solenoid valve 361 and the static air return solenoid valve 371 are controlled to open, so that the gas enters the sample chamber 2 and adsorbs the sample.
[0091] After the adsorption is completed, the first magnetic device 12 is controlled to be powered on and generate a second magnetic force. The first connecting frame 25 is driven by the second magnetic device 13 to move a distance in the connecting frame 24 and then abut against the connecting frame 24, and drive the connecting frame 24 and the sample to move to a suspended state, and then the reading of the microbalance 11 is controlled. At this time, the weight M1 of the sample after adsorption can be obtained by subtracting the weight D of the connecting frame 24, the second connecting block 22 and the crucible 21 from the reading A2 of the microbalance 11. The adsorption weight of the sample can be obtained based on the difference between the weight M1 after sample adsorption and the initial weight M0 (or the difference between A2 and A1 as described in Example 1), and the adsorption speed of the sample can be obtained in combination with the time of adsorption. Next, the fluid density of the gas is obtained by obtaining the weight change of the sedimentation plate 23. Specifically, the first magnetic device 12 is controlled to be energized and generate a third magnetic force, the third magnetic force is greater than the second magnetic force, the second connecting block 22 is driven by the second magnetic device 13 to move a distance and then abut against the connecting hole 231 of the sinker 23, and drive the sinker 23 to move to a suspended state, and then the microbalance 11 is controlled to read the reading. At this time, the difference between the readings A3 and A2 of the microbalance 11 is the weight of the sinker 23 after the system is air-intaken. Since the volume and weight of the sinker 23 are known quantities calibrated in advance, the weight change of the sinker 23 can be obtained based on the weight of the sinker 23 after the system is air-intaken and the calibrated weight of the sinker 23. When the sinker 23 is in different fluid atmospheres (which can be gas, supercritical fluid, liquid, etc.), the measured weight change of the sinker 23 will change with the gas density in the atmosphere. The fluid density can be obtained by reverse calculation (or table lookup) through the weight change of the sinker 23, and adsorption kinetics and adsorption isotherm analysis can be performed based on the acquired data.
[0092] In addition, to ensure the accuracy of the calculation results, the above steps of obtaining the weight of the sample after adsorption, obtaining the weight of the sedimentation plate 23 after the system is air-intaken, and subsequently calculating the adsorption amount, adsorption speed and fluid density of the sample are executed in a cycle for multiple times and the average is taken. The above steps S05, S06 and steps S07, S08 can be executed in sequence or simultaneously, which are all within the scope of protection of the present invention.
[0093] Further, such as Fig.13 As shown, the adsorption instrument of the present invention further includes a temperature acquisition device and a pressure acquisition device, and the temperature acquisition device and the pressure acquisition device are communicatively connected with the controller of the adsorption instrument. Step S09 further includes:
[0094] S091, controlling the temperature acquisition device to acquire the adsorption temperature of the sample;
[0095] S092, controlling the pressure acquisition device to acquire the adsorption pressure of the sample;
[0096] S093. Perform adsorption kinetics analysis on the sample based on the adsorption temperature, adsorption pressure and adsorption rate of the sample;
[0097] S094. Perform adsorption isotherm analysis on the sample based on the adsorption amount of the sample and the fluid density of the gas after the adsorption is completed.
[0098] By obtaining the adsorption temperature and adsorption pressure of the sample, combined with the above-obtained adsorption rate of the sample, the influence of factors such as temperature and pressure on the adsorption rate of the sample can be analyzed, thereby realizing the adsorption kinetics analysis of the sample. In addition, it is mentioned above that the fluid density of the mixed gas after adsorption can be obtained by reverse calculation (or table lookup) through the weight change of the sedimentation plate 23, and the adsorption isotherm analysis of the sample can be realized based on the adsorption amount of the sample and the fluid density of the gas after adsorption.
[0099] Embodiment 7
[0100] In this embodiment, the gravimetric adsorption instrument is the gravimetric adsorption instrument in the above-mentioned embodiment 1 and embodiment 3, such as Figure 1-Figure 4 , Figure 6-Figure 14 As shown, after step S022, the following steps are also included:
[0101] SA, control the static exhaust solenoid valve 351, the static mixing solenoid valve 341, the static air supply solenoid valve 361, the static air return solenoid valve 371, the first static closed solenoid valve 343, the second static closed solenoid valve 344 and the third static closed solenoid valve 345 to open, control the first static air intake solenoid valve 311, the second static air intake solenoid valve 321 and the third static air intake solenoid valve 331 to close, and then control the vacuum pump 5 to open and last for a first preset time;
[0102] SB, control the static exhaust solenoid valve 351, the static air supply solenoid valve 361, the static air return solenoid valve 371 and the third static closed solenoid valve 345 to be closed, and control the third static air intake solenoid valve 331 to be opened so that the third accommodating chamber 348 reaches a third preset pressure;
[0103] SC, control the static exhaust solenoid valve 351, the static mixing solenoid valve 341 and the first static closed solenoid valve 343 to open, control the third static intake solenoid valve 331, the second static closed solenoid valve 344 and the third static closed solenoid valve 345 to close, and then control the vacuum pump 5 to open and last for a first preset time;
[0104] SD, controlling the static exhaust solenoid valve 351 to close, and controlling the second static intake solenoid valve 321 to open so that the second accommodating chamber 347 reaches a second preset pressure;
[0105] SE, control the static exhaust solenoid valve 351 to open, control the second static intake solenoid valve 321 and the first static closed solenoid valve 343 to close, and then control the vacuum pump 5 to open and last for a first preset time;
[0106] SF, controlling the static exhaust solenoid valve 351 to close, and controlling the first static intake solenoid valve 311 to open so that the first accommodating chamber 346 reaches a first preset pressure;
[0107] SG, control the static gas mixing solenoid valve 341 to close, control the static exhaust solenoid valve 351 to open, and then control the vacuum pump 5 to start and continue for a first preset time;
[0108] SH, control the static gas mixing solenoid valve 341, the first static closed solenoid valve 343, the second static closed solenoid valve 344 and the third static closed solenoid valve 345 to open, and control the gas mixing pump 342 to open and last for a first preset time.
[0109] SX, controls the static gas supply solenoid valve 361 and the static gas return solenoid valve 371 to open, so that the gas and the sample are adsorbed.
[0110] The aforementioned embodiment six mentioned a single-component (i.e., only one gas is injected) static air intake system 3. In this embodiment, a multi-component static air intake system 3 is introduced, and a three-component static air intake system 3 is taken as an example. In the case of adopting this embodiment, after obtaining the initial weight of the sample and before injecting gas into the sample chamber 2, in order to ensure the accuracy of the adsorption test, it is also necessary to vacuum the entire static air intake system 3 and the sample chamber 2, control the static exhaust solenoid valve 351, the static mixing solenoid valve 341, the static air supply solenoid valve 361, the static return air solenoid valve 371, the first static closed solenoid valve 343, the second static closed solenoid valve 344 and the third static closed solenoid valve 345 to open, control the first static air intake solenoid valve 311, the second static air intake solenoid valve 321 and the third static air intake solenoid valve 331 to close, and then control the vacuum pump 5 to open and continue for a first preset time to vacuum the entire static air intake system 3 and the sample chamber 2, and then control the air intake of the air intake system. The static exhaust solenoid valve 351, the static air supply solenoid valve 361, the static air return solenoid valve 371 and the third static closed solenoid valve 345 are controlled to be closed, and the third static air intake solenoid valve 331 is controlled to be opened. At this time, the third gas enters the third accommodating chamber 348 from the third static air intake pipeline 33 through the static air mixing pipeline 34, the first accommodating chamber 346, and the second accommodating chamber 347, and makes the third accommodating chamber 348 reach the third preset pressure.
[0111] After the third gas is injected into the third containing chamber 348, the second gas is then injected into the second containing chamber 347. Specifically, the static exhaust solenoid valve 351, the static mixing solenoid valve 341 and the first static closed solenoid valve 343 are controlled to be opened, and the third static intake solenoid valve 331, the second static closed solenoid valve 344 and the third static closed solenoid valve 345 are controlled to be closed. Then, the vacuum pump 5 is controlled to be turned on and continuously evacuate the part except the third containing chamber 348 for the first preset time. After the vacuuming is completed, the static exhaust solenoid valve 351 is controlled to be closed, and the second static intake solenoid valve 321 is controlled to be opened. At this time, the second gas enters the second containing chamber 347 from the second static intake pipeline 32 through the static mixing pipeline 34 and the first containing chamber 346, and makes the second containing chamber 347 reach the second preset pressure.
[0112] Next, the part except the third accommodating chamber 348 and the second accommodating chamber 347 is evacuated, the static exhaust solenoid valve 351 is controlled to be opened, the second static intake solenoid valve 321 and the first static closed solenoid valve 343 are controlled to be closed, and then the vacuum pump 5 is controlled to be turned on and continuously for the first preset time to evacuate the part except the third accommodating chamber 348 and the second accommodating chamber 347. After the vacuuming is completed, the static exhaust solenoid valve 351 is controlled to be closed, and the first static intake solenoid valve 311 is controlled to be opened. At this time, the first gas enters the first accommodating chamber 346 from the first static intake pipeline 31 through the static mixing pipeline 34, and makes the first accommodating chamber 346 reach the first preset pressure. Then the static mixing solenoid valve 341 is controlled to be closed, the static exhaust solenoid valve 351 is controlled to be opened, and the vacuum pump 5 is controlled to be turned on and continuously for the first preset time to evacuate the part except the third accommodating chamber 348, the second accommodating chamber 347 and the first accommodating chamber 346.
[0113] Then, the static gas mixing solenoid valve 341, the first static closed solenoid valve 343, the second static closed solenoid valve 344 and the third static closed solenoid valve 345 are controlled to open, and the gas mixing pump 342 is controlled to open and last for a first preset time, so that the gas in the first accommodating chamber 346, the second accommodating chamber 347 and the third accommodating chamber 348 is released into the static gas mixing pipeline 34, and is evenly mixed in the static gas mixing pipeline 34 under the action of the gas mixing pump 342, and then the static gas supply solenoid valve 361 and the static gas return solenoid valve 371 are controlled to open, so that the gas is adsorbed with the sample, thereby realizing multi-component static adsorption.
[0114] Furthermore, the adsorption instrument further includes a temperature acquisition device and a pressure acquisition device, and the temperature acquisition device and the pressure acquisition device are communicatively connected with the controller of the adsorption instrument, such as Fig.15 As shown, after step S08, the following steps are also included:
[0115] S081. Obtaining the proportion of various types of gas after adsorption is completed based on the fluid density, adsorption temperature, adsorption pressure and gas type of the gas after adsorption is completed;
[0116] S082, obtaining a set pressure of the static intake system 3;
[0117] S083, obtaining the required air supply amount of various types of gas based on the set pressure of the static air intake system 3;
[0118] S084. Replenish air to the static air intake system 3 based on the required replenishment amounts of various types of gas.
[0119] After the multi-component static adsorption is completed, in the prior art, if it is necessary to perform the multi-component static adsorption again at a different set pressure, it is necessary to prepare again according to the process of the last multi-component static adsorption, which makes the operation process complicated. In the present embodiment, after the last multi-component static adsorption is completed, the fluid density of the mixed gas after adsorption can be obtained by the weight change of the sedimentation plate 23. Based on the fluid density of the mixed gas after adsorption, the adsorption temperature of the sample, the adsorption pressure and the type of gas, the proportion of each type of gas can be obtained by looking up the table, and then the set pressure of the static air intake system 3 is obtained again. When the first adsorption test is performed, a list of all pressures required to be set for the adsorption test will be input into the controller, and the next set pressure will be higher than the previous set pressure. Then, based on the next set pressure, the required air replenishment amount of each type of gas can be calculated, and then the static air intake system 3 can be replenished with air based on the required air replenishment amount of the type of gas to perform a new adsorption test. Therefore, the gravimetric adsorption instrument of the present invention can continuously perform multiple adsorption tests at different set pressures, and the operation process is automated to improve the user experience.
[0120] Embodiment 8
[0121] In this embodiment, the gravimetric adsorption instrument is the gravimetric adsorption instrument in the above-mentioned embodiment 1 and embodiment 4, such as Figure 1-Figure 3 , Figure 5 , Fig.16 , Fig.19 As shown, the control method includes:
[0122] SI, control the first magnetic device 12 to be energized and generate a first magnetic force, so that the first connecting frame 25 is driven by the second magnetic device 13 to move to a suspended state in the connecting frame 24, and read the reading of the microbalance 11, and control the magnetic suspension system 1 to be reset;
[0123] SJ, controlling the first magnetic device 12 to be energized and generate a second magnetic force, the first connecting frame 25 is driven by the second magnetic device 13 to move a certain distance in the connecting frame 24 and then abut against the connecting frame 24, and drives the connecting frame 24 and the sample to move to a suspended state;
[0124] SK, control the first magnetic device 12 to be energized and generate a second magnetic force, and the first connecting frame 25 is driven by the second magnetic device 13 to move a certain distance in the connecting frame 24 and then abut against the connecting frame 24, and drive the connecting frame 24 and the sample to move to a suspended state;
[0125] SW, control the microbalance 11 reading and obtain the initial weight of the sample;
[0126] SL, control the first dynamic air intake solenoid valve 412 and the second dynamic air intake solenoid valve 422 to close, control the dynamic exhaust solenoid valve 431, the dynamic high-pressure exhaust solenoid valve 4321, the dynamic low-pressure exhaust solenoid valve 4331, the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 to open, and then control the vacuum pump 5 to start and last for a first preset time;
[0127] SM, control the first dynamic air intake solenoid valve 412 and / or the second dynamic air intake solenoid valve 422 to open, control the flow of the first dynamic air intake pipeline 41 and / or the second dynamic air intake pipeline through the first mass flow controller 411 and / or the second mass flow controller 421, and control the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 to open so that the gas and the sample are adsorbed;
[0128] SN, control the dynamic high-pressure exhaust solenoid valve 4321 and / or the dynamic low-pressure exhaust solenoid valve 4331 to open, control the vacuum pump 5 to open, and adjust the pressure of the dynamic intake system 4 through the first back pressure controller 4322 and / or the second back pressure controller 4332;
[0129] SQ, control the first magnetic device 12 to be powered on and generate the second magnetic force, the first connecting frame 25 is driven by the second magnetic device 13 to move a distance in the connecting frame 24 and then abut against the connecting frame 24, and drive the connecting frame 24 and the sample to move to a suspended state, and then control the microbalance 11 to read and obtain the weight of the sample after adsorption;
[0130] SR, obtain the adsorption amount and adsorption rate of the sample based on the weight of the sample after adsorption and the initial weight;
[0131] SS, control the first magnetic device 12 to be energized and generate the third magnetic force, the second connecting block 22 is driven by the second magnetic device 13 to move a certain distance and then abut against the connecting hole 231 of the sinker 23, and drive the sinker 23 to move to a suspended state;
[0132] ST, control the reading of the microbalance 11 and obtain the weight of the sinker 23 after the system is ventilated;
[0133] SU, obtaining a weight change of the sinker 23 and obtaining a fluid density based on the weight change of the sinker 23;
[0134] SV, adsorption kinetics and adsorption isotherm analysis were performed based on the acquired data.
[0135] In the above steps, step SN further includes:
[0136] SN1. Obtaining a set pressure of the dynamic intake system 4 and comparing the set pressure with a first preset pressure value;
[0137] SN2. If the set pressure of the dynamic intake system 4 is higher than the first preset pressure value, the dynamic high-pressure exhaust solenoid valve 4321 is controlled to open, the dynamic low-pressure exhaust solenoid valve 4331 is controlled to close, and the vacuum pump 5 is turned on, and the pressure of the dynamic intake system 4 is adjusted by the first back pressure controller 4322;
[0138] SN3. If the set pressure of the dynamic intake system 4 is not higher than the first preset pressure value, the dynamic low-pressure exhaust solenoid valve 4331 is controlled to open, the dynamic high-pressure exhaust solenoid valve 4321 is controlled to close, and the vacuum pump 5 is turned on, and the pressure of the dynamic intake system 4 is adjusted by the second back pressure controller 4332;
[0139] In the case of adopting the above embodiment, the process of clearing the magnetic suspension system 1 and obtaining the initial weight M0 of the sample is consistent with the above-mentioned static adsorption method, which will not be repeated here. After obtaining the initial weight M0 of the sample, the first dynamic air intake solenoid valve 412 and the second dynamic air intake solenoid valve 422 are controlled to be closed, and the dynamic exhaust solenoid valve 431, the dynamic high-pressure exhaust solenoid valve 4321, the dynamic low-pressure exhaust solenoid valve 4331, the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 are controlled to be opened. Then the vacuum pump 5 is controlled to be turned on and continuously evacuates the entire dynamic air intake system 4 for a first preset time. After the vacuuming is completed, based on the requirements of the adsorption test, it is determined whether the component of the injected gas is a single component or a multi-component and the mixing ratio. The corresponding number of first dynamic air intake solenoid valves 412 and / or second dynamic air intake solenoid valves 422 are controlled to be opened accordingly. At the same time, the flow of the first dynamic air intake pipeline 41 and / or the second dynamic air intake pipeline is controlled by the first mass flow controller 411 and / or the second mass flow controller 421, and the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 are controlled to be opened so that the gas and the sample are adsorbed. At the same time, the high-pressure exhaust solenoid valve 4321 and / or the dynamic low-pressure exhaust solenoid valve 4331 are controlled to open, the vacuum pump 5 is controlled to open, and the pressure of the dynamic intake system 4 is adjusted by the first back pressure controller 4322 and / or the second back pressure controller 4332. It can be understood by those skilled in the art that during the gas injection process, the dynamic intake solenoid valve and the dynamic exhaust solenoid valve are opened at the same time, and the set intake flow and exhaust pressure are guaranteed at the same time. In the initial stage (when the actual pressure does not reach the set pressure), the back pressure sensor controls little or no exhaust, and the pressure in the system continues to rise. After the actual pressure in the system reaches the set pressure, the back pressure sensor controls the exhaust to increase until it is equal to the intake flow. At this time, the internal pressure of the system fluctuates only slightly above and below the set pressure, achieving a dynamic balance between intake and exhaust.
[0140] Furthermore, in order to avoid excessive pressure fluctuations in the system resulting in excessive deviation from the set pressure, while controlling the opening of the above-mentioned series of valves, the controller of the adsorption instrument also obtains the set pressure of the dynamic air intake system 4 and compares the set pressure with the first preset pressure value. If the set pressure of the dynamic air intake system 4 is higher than the first preset pressure value (the first preset pressure value can be 1.3 bar or other suitable values), the dynamic high-pressure exhaust solenoid valve 4321 is controlled to be opened, the dynamic low-pressure exhaust solenoid valve 4331 is controlled to be closed, and the vacuum pump 5 is turned on. The pressure of the dynamic air intake system 4 is adjusted in real time and automatically through the first back pressure controller 4322. If the set pressure of the dynamic air intake system 4 is not higher than the first preset pressure value, the dynamic low-pressure exhaust solenoid valve 4331 is controlled to be opened, the dynamic high-pressure exhaust solenoid valve 4321 is closed, and the vacuum pump 5 is turned on. The pressure of the dynamic air intake system 4 is adjusted in real time and automatically through the second back pressure controller 4332, so that the entire adsorption process of the sample is under the set flow and pressure, thereby ensuring the accuracy of the sample adsorption atmosphere.
[0141] After the adsorption is completed, the steps of weighing the sample after adsorption, obtaining the adsorption amount and adsorption rate of the sample, obtaining the weight of the sedimentation plate 23 in the system intake, obtaining the fluid density, and performing adsorption kinetics and adsorption isotherm analysis are consistent with the aforementioned static adsorption method and will not be repeated here.
[0142] Embodiment 9:
[0143] In this embodiment, the gravimetric adsorption instrument is the gravimetric adsorption instrument in the above-mentioned embodiment 1 and embodiment 5, such as Figure 1-Figure 5 , Fig.17 As shown, after step SW, the following steps are also included:
[0144] SY1, control the first dynamic air intake solenoid valve 412, the second dynamic air intake solenoid valve 422, the first dynamic liquid intake solenoid valve 472, the second dynamic liquid intake solenoid valve 482, the first cold trap solenoid valve 491 and the second cold trap solenoid valve 492 to close, and control the dynamic exhaust solenoid valve 431, the dynamic high-pressure exhaust solenoid valve 4321, the dynamic low-pressure exhaust solenoid valve 4331, the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 to open;
[0145] SY2, control the vacuum pump 5 to start and continue for a first preset time;
[0146] SY3, control the first dynamic liquid inlet solenoid valve 472 and / or the second dynamic liquid inlet solenoid valve 482 to open, and pump the liquid into the evaporator 46 through the first high-pressure liquid pump 471 and / or the second high-pressure liquid pump 481;
[0147] SY4, control the first dynamic air intake solenoid valve 412 and / or the second dynamic air intake solenoid valve 422 to open, control the flow of the first dynamic air intake pipeline 41 and the second dynamic air intake pipeline through the first mass flow controller 411 and the second mass flow controller 421, and control the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 to open so that the gas and the sample are adsorbed;
[0148] SY5, control the dynamic exhaust solenoid valve 431 to close, and control the first cold trap solenoid valve 491 and the second cold trap solenoid valve 492 to open;
[0149] SY6. Obtaining the set pressure of the dynamic intake system 4;
[0150] SY7. If the set pressure of the dynamic intake system 4 is higher than the first preset pressure value, the dynamic high-pressure exhaust solenoid valve 4321 is controlled to open and the dynamic low-pressure exhaust solenoid valve 4331 is controlled to close, and the pressure of the dynamic intake system 4 is adjusted by the first back pressure controller 4322;
[0151] SY8. If the set pressure of the dynamic intake system 4 is not higher than the first preset pressure value, the dynamic low-pressure exhaust solenoid valve 4331 is controlled to open, the dynamic high-pressure exhaust solenoid valve 4321 is closed, and the vacuum pump 5 is turned on, and the pressure of the dynamic intake system 4 is adjusted by the second back pressure controller 4332.
[0152] The difference between the present embodiment and the aforementioned ninth embodiment is that, in addition to the air intake pipeline, the present embodiment also includes a liquid intake pipeline. When the aforementioned embodiment is adopted, after obtaining the initial weight of the sample, the dynamic air intake system 4 and the sample chamber 2 are evacuated, the first dynamic air intake solenoid valve 412, the second dynamic air intake solenoid valve 422, the first dynamic liquid intake solenoid valve 472, the second dynamic liquid intake solenoid valve 482, the first cold trap solenoid valve 491 and the second cold trap solenoid valve 492 are controlled to be closed, the dynamic exhaust solenoid valve 431, the dynamic high-pressure exhaust solenoid valve 4321, the dynamic low-pressure exhaust solenoid valve 4331, the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 are controlled to be opened, and the vacuum pump 5 is controlled to be turned on and last for the first preset time.
[0153] After completing the vacuuming of the dynamic air intake system 4 and the sample chamber 2, determine whether the components of the injected gas and liquid are single-component or multi-component and the mixing ratio based on the requirements of the adsorption test, and control the first dynamic liquid inlet solenoid valve 472 and / or the second dynamic liquid inlet solenoid valve 482 to open accordingly, pump the liquid into the evaporator 46 through the first high-pressure liquid pump 471 and / or the second high-pressure liquid pump 481, and evaporate into steam in the evaporator 46. At the same time, control the first dynamic air intake solenoid valve 412 and / or the second dynamic air intake solenoid valve 422 to open, control the flow rate of the carrier gas in the first dynamic air intake pipeline 41 and the second dynamic air intake pipeline through the first mass flow controller 411 and the second mass flow controller 421, control the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 to open, and the carrier gas mixes with the steam and enters the sample chamber 2 to adsorb to the sample. At the same time, the dynamic exhaust solenoid valve 431 is controlled to be closed, and the first cold trap solenoid valve 491 and the second cold trap solenoid valve 492 are controlled to be opened. Since there is circulating cold water with a relatively low temperature in the cold trap 49, when the mixed gas of the carrier gas and the steam flows through the cold trap 49, the steam is condensed and remains in the cold trap 49, and the carrier gas flows into the subsequent gas path through the second cold trap solenoid valve 492. The control of the dynamic high-pressure exhaust solenoid valve 4321, the dynamic low-pressure exhaust solenoid valve 4331, the first back pressure controller 4322 and the second back pressure controller 4332 is consistent with that in the aforementioned embodiment 9, and will not be repeated here.
[0154] Embodiment 10
[0155] like Figure 5 , Fig.18 As shown, in this embodiment, the dynamic intake system 4 further includes a connecting pipeline 40 for connecting the dynamic intake pipeline and the dynamic exhaust pipeline 43, and a connecting solenoid valve is provided on the connecting pipeline 40, and the connecting solenoid valve is communicatively connected to the controller of the adsorption instrument, and the control method further includes:
[0156] SZ1, control the first dynamic air intake solenoid valve 412, the second dynamic air intake solenoid valve 422, the first dynamic liquid intake solenoid valve 472, the second dynamic liquid intake solenoid valve 482, the first cold trap solenoid valve 491, the second cold trap solenoid valve 492, the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 to be closed, and control the dynamic exhaust solenoid valve 431, the dynamic high-pressure exhaust solenoid valve 4321, the dynamic low-pressure exhaust solenoid valve 4331 and the connecting solenoid valve to be opened;
[0157] SZ2. Control the vacuum pump 5 to start and keep it on for a first preset time.
[0158] Since it is necessary to evacuate the dynamic air intake system 4 alone without evacuating the sample chamber 2 under certain circumstances, a connecting pipeline 40 is set between the dynamic air intake pipeline and the dynamic exhaust pipeline 43 in the present embodiment, and a connecting solenoid valve 401 is set on the connecting pipeline 40. When it is necessary to evacuate the dynamic air intake system 4 alone, the first dynamic air intake solenoid valve 412, the second dynamic air intake solenoid valve 422, the first dynamic liquid inlet solenoid valve 472, the second dynamic liquid inlet solenoid valve 482, the first cold trap solenoid valve 491, the second cold trap solenoid valve 492, the dynamic air supply solenoid valve 441 and the dynamic air return solenoid valve 451 are controlled to be closed, and the dynamic exhaust solenoid valve 431, the dynamic high-pressure exhaust solenoid valve 4321, the dynamic low-pressure exhaust solenoid valve 4331 and the connecting solenoid valve are controlled to be opened, and at the same time, the vacuum pump 5 is controlled to be turned on and last for the first preset time.
[0159] It should be noted that the above-mentioned implementation mode is only used to illustrate the principle of the present invention and is not intended to limit the scope of protection of the present invention. Without departing from the principle of the present invention, those skilled in the art can adjust the above-mentioned structure so that the present invention can be applied to more specific application scenarios.
[0160] Those skilled in the art can understand that the above-mentioned gravimetric adsorption instrument also includes some other well-known structures, such as a processor, a controller, a memory, etc., wherein the memory includes but is not limited to a random access memory, a flash memory, a read-only memory, a programmable read-only memory, a volatile memory, a non-volatile memory, a serial memory, a parallel memory or a register, etc., and the processor includes but is not limited to a CPLD / FPGA, a DSP, an ARM processor, a MIPS processor, etc. In order to unnecessarily obscure the embodiments of the present disclosure, these well-known structures are not shown in the drawings.
[0161] Although the various steps in the above embodiment are described in the above-mentioned order, those skilled in the art can understand that in order to achieve the effect of this embodiment, different steps do not have to be executed in such an order. They can be executed simultaneously (in parallel) or in a reverse order. These simple changes are within the scope of protection of the present invention.
[0162] So far, the technical solutions of the present invention have been described in conjunction with the preferred embodiments shown in the accompanying drawings. However, it is easy for those skilled in the art to understand that the protection scope of the present invention is obviously not limited to these specific embodiments. Without departing from the principle of the present invention, those skilled in the art can make equivalent changes or substitutions to the relevant technical features, and the technical solutions after these changes or substitutions will fall within the protection scope of the present invention.
Claims
1. A gravimetric adsorption instrument based on a magnetic suspension balance, characterized in that: The adsorption instrument includes a magnetic suspension balance, which includes a magnetic suspension system and a sample chamber for placing samples. The magnetic suspension system includes a first part arranged outside the sample chamber and a second part arranged inside the sample chamber. The first part includes a microbalance and a first magnetic device, which is an electromagnetic force device and is connected to the microbalance of the magnetic suspension system. The second part includes a second magnetic device, which is a permanent magnet and is connected to the sample in the sample chamber. The magnetic force generated by the first magnetic device after power is turned on can absorb the second magnetic device and the sample and weigh them through the microbalance.
2. The gravimetric adsorption instrument based on a magnetic suspension balance according to claim 1, characterized in that: A first connecting structure is arranged between the second magnetic device and the sample, and the first connecting structure includes a connecting frame, a connecting frame bracket and a first connecting block arranged inside the connecting frame, the first connecting block is connected to the second magnetic device, and the connecting frame is connected to the sample. The first connecting block can be driven by the second magnetic device to move in the air for a distance in the connecting frame and then abut against the connecting frame, thereby driving the connecting frame and the sample to move to a suspended state separated from the connecting frame bracket.
3. The gravimetric adsorption instrument based on a magnetic suspension balance according to claim 2, characterized in that: A sinker and a sinker bracket are also provided in the sample chamber, a second connecting structure is provided between the second magnetic device and the sinker, the second connecting structure is a second connecting block, and a corresponding connecting hole is provided on the sinker. The second connecting block is connected to the second magnetic device, and the second connecting block can be driven by the second magnetic device to move in the air for a distance and then abut against the connecting hole of the sinker, thereby driving the sinker to move to a suspended state separated from the sinker bracket.
4. The gravimetric adsorption instrument based on a magnetic suspension balance according to claim 3 is characterized in that: The adsorption instrument also includes a static air intake system, which includes a static air intake pipeline, a static exhaust pipeline and a static air mixing pipeline connected end to end. The first end of the static air intake pipeline is connected to the air source, and the second end is connected to the static air mixing pipeline. The first end of the static exhaust pipeline is connected to the static air mixing pipeline, and the second end is connected to the exhaust port. The static air intake pipeline, the static exhaust pipeline and the static air mixing pipeline are respectively provided with a static air intake solenoid valve, a static exhaust solenoid valve and a static air mixing solenoid valve; The static air intake system further includes a static air supply pipeline and a static air return pipeline, and the corresponding sample chamber includes an air supply port and an air return port. The first end of the static air supply pipeline is connected to the static air mixing pipeline, and the second end is connected to the air supply port. The first end of the static air return pipeline is connected to the air return port, and the second end is connected to the static air mixing pipeline. The static air supply pipeline and the static air return pipeline are respectively provided with a static air supply solenoid valve and a static air return solenoid valve; The static air intake system also includes a vacuum pump, which is connected to the static exhaust pipeline. The static air intake solenoid valve, the static exhaust solenoid valve, the static mixing solenoid valve, the static air supply solenoid valve, the static air return solenoid valve and the vacuum pump are all communicatively connected to the controller of the adsorption instrument.
5. The gravimetric adsorption instrument based on a magnetic suspension balance according to claim 4, characterized in that: The static air intake pipeline comprises a first static air intake pipeline, a second static air intake pipeline and a third static air intake pipeline, wherein the first static air intake pipeline, the second static air intake pipeline and the third static air intake pipeline are respectively provided with a first static air intake solenoid valve, a second static air intake solenoid valve and a third static air intake solenoid valve, and the first static air intake pipeline, the second static air intake solenoid valve and the third static air intake pipeline are all connected to the static air mixing pipeline; A mixing pump is also provided on the static gas mixing pipeline, and a first static closed solenoid valve, a second static closed solenoid valve and a third static closed solenoid valve and a first accommodating chamber, a second accommodating chamber and a third accommodating chamber are also sequentially provided on the static gas mixing pipeline, the third accommodating chamber is arranged between the third static closed solenoid valve and the second static closed solenoid valve, the second accommodating chamber is arranged between the second static closed solenoid valve and the first static closed solenoid valve, the first accommodating chamber is arranged between the first static closed solenoid valve and the static gas mixing solenoid valve, the mixing pump, the first static closed solenoid valve, the second static closed solenoid valve, the third static closed solenoid valve, the first static air intake solenoid valve, the second static air intake solenoid valve and the third static air intake solenoid valve are all communicatively connected with the controller of the adsorption instrument.
6. The gravimetric adsorption instrument based on a magnetic suspension balance according to claim 3, characterized in that: The adsorption instrument further includes a dynamic air intake system, the dynamic air intake system includes a dynamic air intake pipeline, the dynamic air intake pipeline is connected to an air source, the dynamic air intake pipeline includes a first dynamic air intake pipeline and at least one second dynamic air intake pipeline, and the first dynamic air intake pipeline and the second dynamic air intake pipeline are respectively provided with a first mass flow controller, a first dynamic air intake solenoid valve, a second mass flow controller, and a second dynamic air intake solenoid valve; The dynamic intake system further comprises a dynamic exhaust pipeline, a dynamic exhaust solenoid valve is arranged on the dynamic exhaust pipeline, the dynamic exhaust pipeline comprises a dynamic high-pressure exhaust pipeline and a dynamic low-pressure exhaust pipeline, a dynamic high-pressure exhaust solenoid valve and a first back-pressure pressure controller are arranged on the dynamic high-pressure exhaust pipeline, and a dynamic low-pressure exhaust solenoid valve and a second back-pressure pressure controller are arranged on the dynamic low-pressure exhaust pipeline; The dynamic air intake system also includes a dynamic air supply pipeline and a dynamic air return pipeline, and the corresponding sample chamber includes an air supply port and an air return port. The first end of the dynamic air supply pipeline is connected to the dynamic air intake pipeline, and the second end is connected to the air supply port. The first end of the dynamic air return pipeline is connected to the air return port, and the second end is connected to the dynamic exhaust pipeline. The dynamic air supply pipeline and the dynamic air return pipeline are respectively provided with a dynamic air supply solenoid valve and a dynamic air return solenoid valve. The dynamic air intake system also includes a vacuum pump, which is connected to the dynamic exhaust pipeline. The first mass flow controller, the first dynamic air intake solenoid valve, the second mass flow controller, the second dynamic air intake solenoid valve, the dynamic exhaust solenoid valve, the dynamic high-pressure exhaust solenoid valve, the first back pressure pressure controller, the dynamic low-pressure exhaust solenoid valve, the second back pressure pressure controller and the vacuum pump are all communicatively connected to the controller of the adsorption instrument.
7. The gravimetric adsorption instrument based on a magnetic suspension balance according to claim 6, characterized in that: The dynamic air intake system further includes an evaporator, which is arranged on the dynamic air intake pipeline. The dynamic air intake system further includes a dynamic liquid inlet pipeline, which is connected to a liquid source. The dynamic liquid inlet pipeline includes a first dynamic liquid inlet pipeline and at least one second dynamic liquid inlet pipeline. The first dynamic liquid inlet pipeline and the second dynamic liquid inlet pipeline are respectively provided with a first high-pressure liquid pump, a first dynamic liquid inlet solenoid valve, a second high-pressure liquid pump, and a second dynamic liquid inlet solenoid valve. The dynamic liquid inlet pipeline is connected to the evaporator. The dynamic air intake system also includes a cold trap, a first end of the cold trap is connected to the dynamic exhaust pipeline after passing through a first cold trap solenoid valve, and a second end of the cold trap is connected to the dynamic exhaust pipeline after passing through a second cold trap solenoid valve, and the first high-pressure liquid pump, the first dynamic liquid inlet solenoid valve, the second high-pressure liquid pump, the second dynamic liquid inlet solenoid valve, the first cold trap solenoid valve and the second cold trap solenoid valve are all communicatively connected to the controller of the adsorption instrument.
8. The gravimetric adsorption instrument based on a magnetic suspension balance according to claim 7, characterized in that: The dynamic air intake system further includes a connecting pipeline for connecting the dynamic air intake pipeline and the dynamic exhaust pipeline. A connecting solenoid valve is provided on the connecting pipeline. The connecting solenoid valve is communicatively connected to a controller of the adsorption instrument.
9. A control method for a gravimetric adsorption instrument based on a magnetic suspension balance, characterized in that: The gravimetric adsorption instrument is the gravimetric adsorption instrument described in claim 3, the adsorption instrument further comprises an air intake system, the air intake system comprises a vacuum pump, the vacuum pump is communicatively connected to a controller of the adsorption instrument, and the control method comprises: Controlling the magnetic suspension system to perform zeroing; Controlling the microbalance reading and obtaining the initial weight of the sample; Controlling the vacuum pump to start and continue for a first preset time; Control the air intake of the air intake system to adsorb the sample; Controlling the microbalance reading and obtaining the weight of the sample after adsorption; The adsorption amount and adsorption rate of the sample are obtained based on the weight of the sample after adsorption and the initial weight; Controlling the microbalance reading and obtaining the weight of the sinker after the system is ventilated; obtaining a weight change of the sinker and obtaining a fluid density based on the weight change of the sinker; Adsorption kinetics and adsorption isotherm analysis were performed based on the acquired data.
10. The control method for a gravimetric adsorption instrument based on a magnetic suspension balance according to claim 9, characterized in that: The adsorption instrument also includes a static air intake system, which includes a static air intake pipeline, a static exhaust pipeline and a static air mixing pipeline connected end to end. The first end of the static air intake pipeline is connected to the air source, and the second end is connected to the static air mixing pipeline. The first end of the static exhaust pipeline is connected to the static air mixing pipeline, and the second end is connected to the exhaust port. The static air intake pipeline, the static exhaust pipeline and the static air mixing pipeline are respectively provided with a static air intake solenoid valve, a static exhaust solenoid valve and a static air mixing solenoid valve; the static air intake system also includes a static air supply pipeline and a static air return pipeline, and the corresponding sample chamber includes an air supply port and an air return port. The first end of the air supply pipeline is communicated with the static air mixing pipeline, and the second end is communicated with the air supply port. The first end of the static air return pipeline is communicated with the air return port, and the second end is communicated with the static air mixing pipeline. The static air supply pipeline and the static air return pipeline are respectively provided with a static air supply solenoid valve and a static air return solenoid valve; the static air intake system also includes a vacuum pump, and the vacuum pump is communicated with the static exhaust pipeline. The static air intake solenoid valve, the static exhaust solenoid valve, the static air mixing solenoid valve, the static air supply solenoid valve, the static air return solenoid valve and the vacuum pump are all connected to the controller of the adsorption instrument in communication. The control method includes: Controlling the first magnetic device to be powered on and generate a first magnetic force, so that the first connecting block is driven by the second magnetic device to move to a suspended state in the connecting frame, reading the microbalance, and controlling the magnetic suspension system to be reset; Controlling the first magnetic device to be energized and generate a second magnetic force, the first connecting block is driven by the second magnetic device to move a certain distance in the connecting frame and then abut against the connecting frame, thereby driving the connecting frame and the sample to move to a suspended state; Controlling the microbalance reading and obtaining the initial weight of the sample; Control the static exhaust solenoid valve, the static mixing solenoid valve, the static air supply solenoid valve and the static air return solenoid valve to open, control the static air intake solenoid valve to close, and control the vacuum pump to start and last for a first preset time; Controlling the static exhaust solenoid valve, the static air supply solenoid valve and the static air return solenoid valve to close, and controlling the static air intake solenoid valve to open so that the static air intake system reaches a target pressure; Controlling the static gas supply solenoid valve and the static gas return solenoid valve to open so that the gas and the sample are adsorbed; The first magnetic device is controlled to be powered on and generate a second magnetic force, and the first connecting block is driven by the second magnetic device to move a certain distance in the connecting frame and then abut against the connecting frame, and drive the connecting frame and the sample to move to a suspended state, and then control the microbalance reading to obtain the weight of the sample after adsorption; The adsorption amount and adsorption rate of the sample are obtained based on the weight of the sample after adsorption and the initial weight; Controlling the first magnetic device to be energized and generate a third magnetic force, the second connecting block moves a certain distance driven by the second magnetic device and then abuts against the connecting hole of the sinker, and drives the sinker to move to a suspended state, and then controlling the microbalance reading to obtain the weight of the sinker after the system is air-intaken; obtaining a weight change of the sinker and obtaining a fluid density based on the weight change of the sinker; Adsorption kinetics and adsorption isotherm analysis were performed based on the acquired data.
11. The control method for a gravimetric adsorption instrument based on a magnetic suspension balance according to claim 10, characterized in that: The static air intake pipeline comprises a first static air intake pipeline, a second static air intake pipeline and a third static air intake pipeline, wherein the first static air intake pipeline, the second static air intake pipeline and the third static air intake pipeline are respectively provided with a first static air intake solenoid valve, a second static air intake solenoid valve and a third static air intake solenoid valve, and the first static air intake pipeline, the second static air intake solenoid valve and the third static air intake pipeline are all connected to the static air mixing pipeline; an air mixing pump is also provided on the static air mixing pipeline, and a first static closed solenoid valve, a second static closed solenoid valve and a third static closed solenoid valve as well as a first accommodating chamber, a second accommodating chamber and a third accommodating chamber are also provided on the static air mixing pipeline in sequence. The third accommodating chamber is arranged between the third static closed solenoid valve and the second static closed solenoid valve, the second accommodating chamber is arranged between the second static closed solenoid valve and the first static closed solenoid valve, the first accommodating chamber is arranged between the first static closed solenoid valve and the static gas mixing solenoid valve, the gas mixing pump, the first static closed solenoid valve, the second static closed solenoid valve, the third static closed solenoid valve, the first static air intake solenoid valve, the second static air intake solenoid valve and the third static air intake solenoid valve are all connected to the controller of the adsorption instrument in communication, and after the step of "controlling the microbalance reading and obtaining the initial weight of the sample", it also includes: Control the static exhaust solenoid valve, the static mixing solenoid valve, the static air supply solenoid valve, the static air return solenoid valve, the first static closed solenoid valve, the second static closed solenoid valve and the third static closed solenoid valve to open, control the first static intake solenoid valve, the second static intake solenoid valve and the third static intake solenoid valve to close, and then control the vacuum pump to open and last for a first preset time; Control the static exhaust solenoid valve, the static air supply solenoid valve, the static air return solenoid valve and the third static closed solenoid valve to be closed, and control the third static air intake solenoid valve to be opened so that the third accommodating chamber reaches a third preset pressure; Control the static exhaust solenoid valve, the static mixing solenoid valve and the first static closed solenoid valve to open, control the third static intake solenoid valve, the second static closed solenoid valve and the third static closed solenoid valve to close, and then control the vacuum pump to open and last for a first preset time; Controlling the static exhaust solenoid valve to close, and controlling the second static intake solenoid valve to open so that the second accommodating chamber reaches a second preset pressure; Controlling the static exhaust solenoid valve to open, controlling the second static intake solenoid valve and the first static closing solenoid valve to close, and then controlling the vacuum pump to turn on and last for a first preset time; Controlling the static exhaust solenoid valve to close, and controlling the first static intake solenoid valve to open so that the first accommodating chamber reaches a first preset pressure; Controlling the static gas mixing solenoid valve to close, controlling the static exhaust solenoid valve to open, and then controlling the vacuum pump to start and continue for a first preset time; Control the static gas mixing solenoid valve, the first static closed solenoid valve, the second static closed solenoid valve and the third static closed solenoid valve to open, and control the gas mixing pump to open and last for a first preset time; The static gas supply solenoid valve and the static gas return solenoid valve are controlled to open so that the gas and the sample are adsorbed.
12. The control method for a gravimetric adsorption instrument based on a magnetic suspension balance according to claim 9, characterized in that: The adsorption instrument also includes a dynamic air intake system, which includes a dynamic air intake pipeline, which is connected to an air source, and includes a first dynamic air intake pipeline and at least one second dynamic air intake pipeline, and the first dynamic air intake pipeline and the second dynamic air intake pipeline are respectively provided with a first mass flow controller, a first dynamic air intake solenoid valve, a second mass flow controller, and a second dynamic air intake solenoid valve; the dynamic air intake system also includes a dynamic exhaust pipeline, and the dynamic exhaust pipeline is provided with a dynamic exhaust solenoid valve, and the dynamic exhaust pipeline includes a dynamic high-pressure exhaust pipeline and a dynamic low-pressure exhaust pipeline, and the dynamic high-pressure exhaust pipeline is provided with a dynamic high-pressure exhaust solenoid valve and a first back-pressure pressure controller, and the dynamic low-pressure exhaust pipeline is provided with a dynamic low-pressure exhaust solenoid valve and a second back-pressure pressure controller; the dynamic air intake system also includes a dynamic air supply pipeline and a dynamic return pipeline. The air pipeline, the corresponding sample chamber includes an air supply port and an air return port, the first end of the dynamic air supply pipeline is connected to the dynamic air intake pipeline, and the second end is connected to the air supply port, the first end of the dynamic air return pipeline is connected to the air return port, and the second end is connected to the dynamic exhaust pipeline, the dynamic air supply pipeline and the dynamic air return pipeline are respectively provided with a dynamic air supply solenoid valve and a dynamic air return solenoid valve, the dynamic air intake system also includes a vacuum pump, the vacuum pump is connected to the dynamic exhaust pipeline, the first mass flow controller, the first dynamic air intake solenoid valve, the second mass flow controller, the second dynamic air intake solenoid valve, the dynamic exhaust solenoid valve, the dynamic high-pressure exhaust solenoid valve, the first back pressure pressure controller, the dynamic low-pressure exhaust solenoid valve, the second back pressure pressure controller and the vacuum pump are all connected to the controller of the adsorption instrument in communication, and the control method includes: Controlling the first magnetic device to be powered on and generate a first magnetic force, so that the first connecting block is driven by the second magnetic device to move to a suspended state in the connecting frame, reading the microbalance, and controlling the magnetic suspension system to be reset; Controlling the first magnetic device to be powered on and generate a second magnetic force, the first connecting block is driven by the second magnetic device to move a certain distance in the connecting frame and then abut against the connecting frame, and drives the connecting frame and the sample to move to a suspended state, and then controlling the microbalance reading to obtain the initial weight of the sample; Controlling the first dynamic air intake solenoid valve and the second dynamic air intake solenoid valve to close, controlling the dynamic exhaust solenoid valve, the dynamic high-pressure exhaust solenoid valve, the dynamic low-pressure exhaust solenoid valve, the dynamic air supply solenoid valve and the dynamic air return solenoid valve to open, and then controlling the vacuum pump to start and last for a first preset time; Control the first dynamic air intake solenoid valve and / or the second dynamic air intake solenoid valve to open, control the flow of the first dynamic air intake pipeline and / or the second dynamic air intake pipeline through the first mass flow controller and / or the second mass flow controller, and control the dynamic air supply solenoid valve and the dynamic air return solenoid valve to open so that the gas and the sample are adsorbed; Controlling the dynamic high-pressure exhaust solenoid valve and / or the dynamic low-pressure exhaust solenoid valve to open, controlling the vacuum pump to open, and adjusting the pressure of the dynamic intake system through the first back pressure controller and / or the second back pressure controller; Obtaining a set pressure of the dynamic air intake system and comparing the set pressure with a first preset pressure value; If the set pressure of the dynamic intake system is higher than a first preset pressure value, the dynamic high-pressure exhaust solenoid valve is controlled to open and the dynamic low-pressure exhaust solenoid valve is controlled to close, and the pressure of the dynamic intake system is adjusted by the first back pressure controller; If the set pressure of the dynamic intake system is not higher than the first preset pressure value, the dynamic low-pressure exhaust solenoid valve is controlled to open, the dynamic high-pressure exhaust solenoid valve is controlled to close, and the vacuum pump is controlled to open, and the pressure of the dynamic intake system is adjusted by the second back pressure controller; Controlling the first magnetic device to be energized and generate a second magnetic force, the first connecting block is driven by the second magnetic device to move a certain distance in the connecting frame and then abut against the connecting frame, thereby driving the connecting frame and the sample to move to a suspended state; Controlling the microbalance reading and obtaining the weight of the sample after adsorption; The adsorption amount and adsorption rate of the sample are obtained based on the weight of the sample after adsorption and the initial weight; Controlling the first magnetic device to be energized and generate a third magnetic force, the second connecting block moves a certain distance driven by the second magnetic device and then abuts against the connecting hole of the sinker, and drives the sinker to move to a suspended state; Controlling the microbalance reading and obtaining the weight of the sinker after the system is ventilated; obtaining a weight change of the sinker and obtaining a fluid density based on the weight change of the sinker; Adsorption kinetics and adsorption isotherm analysis were performed based on the acquired data.
13. The control method for a gravimetric adsorption instrument based on a magnetic suspension balance according to claim 12, characterized in that: The dynamic air intake system also includes an evaporator, which is arranged on the dynamic air intake pipeline. The dynamic air intake system also includes a dynamic liquid inlet pipeline, which is connected to a liquid source. The dynamic liquid inlet pipeline includes a first dynamic liquid inlet pipeline and at least one second dynamic liquid inlet pipeline. The first dynamic liquid inlet pipeline and the second dynamic liquid inlet pipeline are respectively provided with a first high-pressure liquid pump, a first dynamic liquid inlet solenoid valve, a second high-pressure liquid pump, and a second dynamic liquid inlet solenoid valve. The dynamic liquid inlet pipeline is connected to the evaporator; the dynamic air intake system also includes a cold trap, the first end of the cold trap is connected to the dynamic exhaust pipeline after passing through the first cold trap solenoid valve, and the second end is connected to the dynamic exhaust pipeline after passing through the second cold trap solenoid valve. The first high-pressure liquid pump, the first dynamic liquid inlet solenoid valve, the second high-pressure liquid pump, the second dynamic liquid inlet solenoid valve, the first cold trap solenoid valve, and the second cold trap solenoid valve are all connected to the controller of the adsorption instrument in communication. After the step of "controlling the microbalance reading and obtaining the initial weight of the sample", it also includes: Control the first dynamic air intake solenoid valve, the second dynamic air intake solenoid valve, the first dynamic liquid intake solenoid valve, the second dynamic liquid intake solenoid valve, the first cold trap solenoid valve and the second cold trap solenoid valve to be closed, and control the dynamic exhaust solenoid valve, the dynamic high-pressure exhaust solenoid valve, the dynamic low-pressure exhaust solenoid valve, the dynamic air supply solenoid valve and the dynamic air return solenoid valve to be opened; Controlling the vacuum pump to start and continue for a first preset time; Controlling the first dynamic liquid inlet solenoid valve and / or the second dynamic liquid inlet solenoid valve to open, and pumping liquid into the evaporator through the first high-pressure liquid pump and / or the second high-pressure liquid pump; Control the first dynamic air intake solenoid valve and / or the second dynamic air intake solenoid valve to open, control the flow of the first dynamic air intake pipeline and the second dynamic air intake pipeline through the first mass flow controller and the second mass flow controller, and control the dynamic air supply solenoid valve and the dynamic air return solenoid valve to open so that the gas is adsorbed by the sample; Controlling the dynamic exhaust solenoid valve to close, and controlling the first cold trap solenoid valve and the second cold trap solenoid valve to open; Obtaining a set pressure of the dynamic air intake system; If the set pressure of the dynamic intake system is higher than the first preset pressure value, the dynamic high-pressure exhaust solenoid valve is controlled to open, the dynamic low-pressure exhaust solenoid valve is controlled to close, and the vacuum pump is controlled to open, and the pressure of the dynamic intake system is adjusted by the first back pressure controller; If the set pressure of the dynamic intake system is not higher than the first preset pressure value, the dynamic low-pressure exhaust solenoid valve is controlled to open, the dynamic high-pressure exhaust solenoid valve is closed, and the vacuum pump is turned on, and the pressure of the dynamic intake system is adjusted by the second back pressure controller.
14. The control method for a gravimetric adsorption instrument based on a magnetic suspension balance according to claim 13, characterized in that: The dynamic air intake system further includes a connecting pipeline for connecting the dynamic air intake pipeline and the dynamic exhaust pipeline, a connecting solenoid valve is provided on the connecting pipeline, and the connecting solenoid valve is communicatively connected to the controller of the adsorption instrument, and the control method further includes: Control the first dynamic air intake solenoid valve, the second dynamic air intake solenoid valve, the first dynamic liquid intake solenoid valve, the second dynamic liquid intake solenoid valve, the first cold trap solenoid valve, the second cold trap solenoid valve, the dynamic air supply solenoid valve and the dynamic air return solenoid valve to be closed, and control the dynamic exhaust solenoid valve, the dynamic high-pressure exhaust solenoid valve, the dynamic low-pressure exhaust solenoid valve and the connecting solenoid valve to be opened; The vacuum pump is controlled to start and last for a first preset time.
15. The control method for a gravimetric adsorption instrument based on a magnetic suspension balance according to any one of claims 9 to 13, characterized in that: The adsorption instrument further includes a temperature acquisition device and a pressure acquisition device, and the temperature acquisition device and the pressure acquisition device are communicatively connected to the controller of the adsorption instrument. The step of "performing adsorption kinetics and adsorption isotherm analysis based on the acquired data" further includes: Controlling the temperature acquisition device to acquire the adsorption temperature of the sample; Controlling the pressure acquisition device to acquire the adsorption pressure of the sample; The adsorption kinetics of the samples were analyzed based on the adsorption temperature, adsorption pressure and adsorption rate of the samples; The adsorption isotherm analysis of the samples was performed based on the adsorption amount of the samples and the fluid density of the gas after the adsorption was completed.
16. The control method for a gravimetric adsorption instrument based on a magnetic suspension balance according to claim 11, characterized in that: The adsorption instrument further includes a temperature acquisition device and a pressure acquisition device, wherein the temperature acquisition device and the pressure acquisition device are communicatively connected to the controller of the adsorption instrument, and after the step of "obtaining the weight change of the sinker and obtaining the fluid density based on the weight change of the sinker", the following steps are further included: Based on the fluid density, adsorption temperature, adsorption pressure and gas type of the gas after adsorption, the proportion of each type of gas after adsorption is completed is obtained; Obtaining a set pressure of the static air intake system; Obtaining the required air supply volume of various types of gas based on the set pressure of the static air intake system; The static air intake system is supplemented with air based on the supplementary air amount required by various types of gas.
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