CN215375005U - Porous material specific surface area measuring device - Google Patents
Porous material specific surface area measuring device Download PDFInfo
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- CN215375005U CN215375005U CN202121728645.9U CN202121728645U CN215375005U CN 215375005 U CN215375005 U CN 215375005U CN 202121728645 U CN202121728645 U CN 202121728645U CN 215375005 U CN215375005 U CN 215375005U
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Abstract
The utility model discloses a porous substance specific surface area measuring device, which comprises an air source part, an adsorbate specific pressure control part and an adsorbate adsorption quantity measuring part; the gas source part comprises a nitrogen gas cylinder, a pressure stabilizing valve and a gas purifier; the adsorbate specific pressure control part comprises two mass flowmeters and an adsorbate saturator; the absorption quality and absorption quantity measuring part comprises two stop valves, a sample tube, a tube furnace, an isobaric meter and a vacuum pump. The device has the advantages of simple structure, convenient operation, accurate and stable control of all parameters, and capability of carrying out in-situ pretreatment on the porous substance, thereby improving the accuracy of the experimental result.
Description
Technical Field
The utility model belongs to the field of laboratory equipment, and particularly relates to an experimental device for determining the specific surface area of a porous substance by a flow adsorption method.
Background
The porous material is widely applied to the fields of energy, medicine, information, biology, electronics and the like. The specific surface area is one of the important indicators of porous materials. The accurate determination of the specific surface area of the porous material has guiding significance for material synthesis. The flow adsorption method for measuring the specific surface area of the porous substance is used as a comprehensive college physical and chemical experiment, can promote students to master basic theories such as gas adsorption and the like and basic operations such as gas flow rate control, correction and the like, and has important significance for culturing the comprehensive capacity of the students. At present, a device specially used for measuring the specific surface area of a porous substance by a flow adsorption method does not exist, the device used in the experiment is mainly formed by assembling an adsorption instrument, a constant-temperature water tank, a capillary flowmeter, a pressure stabilizing valve, a gas purification tube and the like, and the device can be divided into a gas source part, an adsorption mass specific pressure control part and an adsorption mass adsorption quantity measuring part. However, the assembly apparatus mainly has the following two problems: (1) the capillary tube flowmeter needs to observe and stabilize the height difference of liquid levels at two ends of the flowmeter in real time for controlling the gas flow rate, and the student has poor control capability, so that the gas flow error is large, and the accuracy of an experimental result is influenced; (2) the existing experimental device can not finish the 'in-situ pretreatment' of the porous substance, and can not exclude and avoid the adsorption of other impurities except the adsorbate on the porous substance in the experimental process, thereby causing the measurement error of the adsorbate adsorption quantity and influencing the accuracy of the experimental result. The above factors limit the popularization and spread of the physicochemical experiment. Therefore, the development and the utility model of an experimental device for measuring the specific surface area of the porous substance by the flow adsorption method have important practical significance.
Disclosure of Invention
The utility model aims to provide a device for measuring the specific surface area of a porous substance, which has the advantages of simple structure, convenient operation, accurate and stable control of all parameters and capability of carrying out in-situ pretreatment on the porous substance, thereby improving the accuracy of an experimental result.
The utility model provides a device for measuring the specific surface area of a porous substance, which comprises an air source part, an adsorbate specific pressure control part and an adsorbate adsorption quantity measuring part; the gas source part comprises a nitrogen gas cylinder, a pressure stabilizing valve and a gas purifier; the adsorbate specific pressure control part comprises two mass flowmeters and an adsorbate saturator; the absorption quality and absorption quantity measuring part comprises two stop valves, a sample tube, a tube furnace, an isobaric meter and a vacuum pump;
the device comprises a gas source part, a pressure stabilizing valve and a gas purifier are sequentially arranged on an outlet pipeline of a nitrogen gas cylinder, the outlet of the gas purifier is communicated with one gas inlet of a first three-way valve, the other two interfaces of the first three-way valve are gas outlets which are respectively communicated with the gas inlets of a first mass flow meter and a second mass flow meter, the gas outlet of the first mass flow meter is communicated with the inlet of an adsorption saturator, the outlet of the adsorption saturator and the outlet of the second mass flow meter are respectively communicated with the two gas inlets of a second three-way valve, the rest interfaces of the second three-way valve are gas outlets which are communicated with the gas inlet of a sample tube, and a first stop valve is arranged on a pipeline of the second three-way valve communicated with the sample tube; the sample tube is arranged in the tube furnace, the gas outlet of the sample tube is communicated with the third three-way valve, and a second stop valve is arranged on a pipeline for communicating the sample tube with the third three-way valve; and the other two interfaces of the third three-way valve are air outlets, one air outlet is sequentially connected with an isobaric meter and a vacuum pump, and the other air outlet is communicated with the atmosphere.
In the above apparatus for measuring the specific surface area of a porous material, the gas purifier in the gas source section is a tubular container filled with a molecular sieve.
The device for measuring the specific surface area of the porous substance further comprises an adsorbate specific pressure control part, wherein the adsorbate saturator consists of a stainless steel pipe with one closed end, a heating band wound on the outer wall of the stainless steel pipe, a thermocouple, a temperature display controller, an air inlet pipe and an air outlet pipe, the heating band is connected with the temperature display controller, one end of the thermocouple is inserted into the heating band, the other end of the thermocouple is connected with the temperature display controller, the air inlet pipe and the air outlet pipe are respectively inserted into the stainless steel pipe and fixed, and the air inlet pipe is inserted into the bottom of the stainless steel pipe. The adsorbate may be methanol or the like.
In the above device for measuring the specific surface area of the porous material, the sample tube is a U-shaped quartz tube; porous substances are placed in the middle of the U-shaped quartz tube, and the U-shaped tube is located in a constant-temperature area of the tube furnace. Two ends of the U-shaped quartz sample tube are connected with corresponding connecting pipelines through rubber tubes.
In the above apparatus for measuring a specific surface area of a porous substance, the tube furnace is a vertical tube furnace capable of temperature rise/fall by a program.
In the above porous substance specific surface area measuring apparatus, each connecting line is a stainless steel pipe.
The device for measuring the specific surface area of the porous substance can be further controlled by a PLC (programmable logic controller), wherein the mass flow meter, the two stop valves, the adsorbate saturator, the two three-way valves and the tube furnace are arranged on the tube furnace.
When the device provided by the utility model is used for measuring the specific surface area of the porous substance, the experimental process comprises the two steps of porous substance in-situ pretreatment and porous substance adsorption quantity measurement:
(1) in-situ pretreatment of porous material: firstly, closing a first stop valve and opening a second stop valve; adjusting the third three-way valve to enable the vacuum pump to be communicated with the U-shaped sample pipe, vacuumizing, and reading the system pressure by an isobaric meter; after the vacuumizing is finished, setting a temperature-raising program of the tube furnace to process the sample at a specific temperature for a certain time; the completion of the process completes the in-situ pretreatment process of the porous material.
(2) Measurement of the amount of adsorption of the porous substance: opening the first stop valve, and adjusting the third three-way valve to exhaust the gas at the outlet end of the U-shaped sample tube; during the experiment, the nitrogen from the nitrogen gas cylinder passes through a pressure stabilizing valve and then has stable gas flow, the stable nitrogen gas flow passes through a gas purifier to remove impurities and water vapor in the nitrogen, and then is divided into two paths of gas by a first three-way valve, and the flow of the two paths of gas is controlled by a first flowmeter and a second flowmeter respectively; wherein, the gas flow controlled by the first flowmeter passes through the adsorbate saturator to saturate the adsorbate with steam; the two paths of gas are converged through a second three-way valve, and at the moment, nitrogen and saturated steam of adsorbate flow into the U-shaped quartz sample tube; a porous substance in the U-shaped quartz sample tube adsorbs adsorbates in the airflow until the adsorbates are saturated; the adsorbed air flow is exhausted through a third three-way valve; the content of adsorbate adsorbed on the surface of the porous substance can be calculated by weighing the mass difference of the sample before and after adsorption.
Compared with the prior art, the utility model has the following beneficial effects:
1. the gas source part of the device adopts the mass flow meter to control the gas flow, the accuracy is high, and the problem of unstable gas flow caused by weak control capability of students is avoided.
2. The adsorbate specific pressure control part of the device introduces an adsorbate saturator, and compared with the conventional method for heating the adsorbate by controlling the temperature of a constant-temperature water bath, the device has simpler structure and operation.
3. The adsorption quantity measuring part of the device is additionally provided with a tubular furnace, a vacuum pump, an isobaric meter, a stop valve, a three-way valve and the like, so that the original pretreatment of porous substances can be realized, and the experimental accuracy is improved.
4. The device can be controlled by computer software, and the system integration level is high.
Drawings
FIG. 1 is a schematic view showing the overall structure of a specific surface area measuring apparatus for a porous substance according to the present invention;
FIG. 2 is a schematic view showing the structure of an adsorbate saturator of the apparatus for measuring specific surface area of a porous substance according to the present invention;
in the figure: the device comprises a nitrogen gas steel bottle 1-1, a pressure stabilizing valve 1-2, a gas purifier 1-3, a first three-way valve 1-4, a first mass flow meter 1-5, a second mass flow meter 1-6, an adsorbent saturator 1-7, a second three-way valve 1-8, a first stop valve 1-9, a tubular furnace 1-10, a sample tube 1-11, a second stop valve 1-12, a third three-way valve 1-13, an isobaric meter 1-14 and a vacuum pump 1-15, wherein the nitrogen gas steel bottle 1-2 is a nitrogen gas steel bottle; 2-1 is a stainless steel pipe; 2-2 is a heating belt; 2-3 is a thermocouple, and 2-4 is an air inlet pipe; 2-5 is an air outlet pipe; 2-6 are temperature display controllers.
Detailed Description
The specific surface area measuring apparatus of the present invention will be further described with reference to the accompanying drawings by way of examples.
Example 1
In this embodiment, an experimental apparatus for determining the specific surface area of a porous material by a flow adsorption method is shown in fig. 1, and includes an air source portion, an adsorbate specific pressure control portion, and an adsorbate adsorption amount determination portion; the gas source part comprises a nitrogen gas bottle 1-1, a pressure stabilizing valve 1-2 and a gas purifier 1-3; the adsorbate specific pressure control part comprises two mass flowmeters and an adsorbate saturator 1-7; the absorption quality and absorption quantity measuring part comprises two stop valves, a sample tube 1-11, a tube furnace 1-10, an isobaric meter 1-14 and a vacuum pump 1-15; the gas purifier in the gas source part is a tubular container filled with molecular sieves. The tube furnace is a vertical tube furnace capable of temperature programming/cooling.
A pressure stabilizing valve 1-2 and a gas purifier 1-3 are sequentially arranged on an outlet pipeline of the nitrogen gas bottle 1-1, an outlet of the gas purifier 1-3 is communicated with one gas inlet of a first three-way valve 1-4, the other two interfaces of the first three-way valve 1-4 are gas outlets which are respectively communicated with gas inlets of a first mass flow meter 1-5 and a second mass flow meter 1-6, the gas outlet of the first mass flow meter is communicated with an inlet of an adsorbate saturator 1-7, the outlet of the adsorbate saturator and the outlet of the second mass flow meter 1-6 are respectively communicated with two gas inlets of a second three-way valve 1-8, the rest interfaces of the second three-way valve are gas outlets, a pipeline which is communicated with the sample tube 1-11 is provided with a first stop valve 1-9; the sample tube is arranged in the tube furnace 1-10, the gas outlet of the sample tube is communicated with the third three-way valve 1-13, and a second stop valve 1-12 is arranged on a pipeline for communicating the sample tube with the third three-way valve; and the other two interfaces of the third three-way valve are air outlets, wherein one air outlet is sequentially connected with an isobaric meter 1-14 and a vacuum pump 1-15, and the two air outlets are communicated with the atmosphere. And each connecting pipeline adopts a stainless steel pipe.
Wherein, adsorbate specific pressure control part, adsorbate saturator comprises stainless steel pipe, the heating band of winding at stainless steel outer wall of tubes, thermocouple, temperature display controller, intake pipe, outlet duct that one end is confined, the heating band is connected with temperature display controller, during thermocouple one end inserts the heating band, the other end is connected with temperature display controller, intake pipe, outlet duct insert stainless steel pipe respectively and fixed, the nonrust steel pipe bottom of inserting of intake pipe. The adsorbate may be methanol or the like.
The sample tube adopts a U-shaped quartz sample tube; porous substances are placed in the middle of the U-shaped pipe, and the U-shaped pipe is located in a constant-temperature area of the tubular furnace. Two ends of the U-shaped quartz sample tube are connected with corresponding connecting pipelines through rubber tubes.
The mass flow meter, the two stop valves, the adsorbate saturator, the two three-way valves and the tube furnace are controlled by corresponding integrated computer system software.
In this embodiment, all the components can be purchased from the market.
The determination of the specific surface area of the porous material by the flow adsorption method is divided into an in-situ treatment part and an adsorbate adsorption quantity determination part of the porous material:
(1) in-situ pretreatment of the porous substance: closing the first stop valve 1-9, opening the second stop valve 1-12, and adjusting the third three-way valve 1-13 to communicate the U-shaped sample pipe with the isobaric meter and the vacuum pump; the purpose of communicating the sample tube with the vacuum pump is to process the impurity gas adsorbed on the surface of the porous substance by vacuumizing; the impurity gas adsorbed on the surface of the cleaning porous substance can be determined by observing the system pressure through an isobaric meter; in the in-situ treatment process of the porous substance, the temperature of the tubular furnace is set, so that the porous substance is heated, and the pretreatment process of the porous substance is accelerated; after the in-situ pretreatment process of the porous substance is finished, weighing the total weight of the U-shaped sample tube and the sample to be m1。
(2) And (3) measuring the adsorption quantity of the adsorbate: simultaneously opening the first stop valve and the second stop valve, and adjusting the third three-way valve to directly exhaust the gas at the outlet end of the U-shaped sample tube; in the measuring process of the adsorbate adsorption quantity, the temperature of an adsorbate saturator needs to be set so that adsorbate reaches corresponding saturated vapor pressure; in the testing process, nitrogen is divided into two paths after passing through a pressure stabilizing valve and a gas purifier, and the flow rates of the two paths of nitrogen are respectively controlled by a first mass flow meter and a second mass flow meter; the first path passes through a first mass flow meter and an adsorbate saturator, the second path passes through a second mass flow meter, and thenThe two paths of gas are converged by a second three-way valve; the gas converged by the second three-way valve enters the U-shaped sample tube through the first stop valve for adsorption, the adsorption process lasts for 30-40min, the porous substance is ensured to be adsorbed and saturated, and the adsorption is finished; the tail gas in the adsorption process is exhausted after passing through a second stop valve and a third three-way valve; after the adsorption is finished, taking out the U-shaped sample tube, and weighing the total weight of the sample tube and the porous substance to be m2(ii) a The adsorbate having an adsorption capacity equal to m2-m1(ii) a The adsorbate may be methanol or the like.
Completing the adsorption quantity measuring process of the adsorbate in the experiment to obtain the saturated adsorption quantity of the adsorbate on the surface of the porous substance; after the adsorption quantity of the adsorbate on the surface of the porous substance is obtained, the specific surface area of the porous substance can be calculated by a single-point BET method.
Claims (8)
1. A porous substance specific surface area measuring device is characterized by comprising an air source part, an adsorbate specific pressure control part and an adsorbate adsorption quantity measuring part; the gas source part comprises a nitrogen gas bottle (1-1), a pressure stabilizing valve (1-2) and a gas purifier (1-3); the adsorbate specific pressure control part comprises two mass flowmeters (1-5, 1-6) and an adsorbate saturator (1-7); the absorption quantity measuring part of the adsorbate comprises two stop valves (1-9, 1-12), a sample tube (1-11), a tube furnace (1-10), an isobaric meter (1-14) and a vacuum pump (1-15);
a pressure stabilizing valve and a gas purifier are sequentially arranged on an outlet pipeline of the nitrogen gas bottle, the outlet of the gas purifier is communicated with one gas inlet of a first three-way valve (1-4), the other two interfaces of the first three-way valve are gas outlets which are respectively communicated with the gas inlets of a first mass flow meter (1-5) and a second mass flow meter (1-6), the gas outlet of the first mass flow meter is communicated with the inlet of an adsorbate saturator, the outlet of the adsorbate saturator and the outlet of the second mass flow meter are respectively communicated with two gas inlets of a second three-way valve (1-8), the rest interfaces of the second three-way valve are gas outlets which are communicated with the gas inlet of the sample tube, and a first stop valve (1-9) is arranged on a pipeline for communicating the second three-way valve with the sample tube; the sample tube is placed in the tube furnace, the gas outlet of the sample tube is communicated with a third three-way valve (1-13), and a second stop valve (1-12) is arranged on a pipeline for communicating the sample tube with the third three-way valve; and the other two interfaces of the third three-way valve are air outlets, one air outlet is sequentially connected with an isobaric meter and a vacuum pump, and the other air outlet is communicated with the atmosphere.
2. The apparatus for measuring the specific surface area of a porous material according to claim 1, wherein the gas purifiers (1 to 3) in the gas source section are tubular vessels containing molecular sieves.
3. The device for measuring the specific surface area of the porous substance according to claim 1, wherein the adsorbate specific pressure control part comprises an adsorbate saturator (2-5) consisting of a stainless steel tube (2-1) with one end closed, a heating band (2-2) wound on the outer wall of the stainless steel tube, a thermocouple (2-3), a temperature display controller (2-6), an air inlet tube (2-4) and an air outlet tube, the heating band is connected with the temperature display controller, one end of the thermocouple is inserted into the heating band, the other end of the thermocouple is connected with the temperature display controller, the air inlet tube and the air outlet tube are respectively inserted into the stainless steel tube and fixed, and the air inlet tube is inserted into the bottom of the stainless steel tube.
4. The apparatus for measuring the specific surface area of a porous substance according to claim 1, wherein the sample tube is a U-shaped quartz tube; porous substances are placed in the middle of the U-shaped pipe, and the U-shaped pipe is located in a constant-temperature area of the tubular furnace.
5. The apparatus for measuring the specific surface area of a porous substance according to claim 4, wherein both ends of the U-shaped quartz tube are connected to the corresponding connecting lines through rubber tubes.
6. The apparatus for measuring the specific surface area of a porous substance according to claim 1, wherein the tube furnace is a vertical tube furnace capable of temperature rise/fall programming.
7. The apparatus for measuring the specific surface area of a porous substance according to claim 1, wherein each connecting line is a stainless steel pipe.
8. The apparatus for measuring the specific surface area of a porous substance according to claim 1, wherein the mass flow meter, the two stop valves, the adsorbent saturator, the two three-way valves, and the tube furnace are controlled by a PLC.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202121728645.9U CN215375005U (en) | 2021-07-28 | 2021-07-28 | Porous material specific surface area measuring device |
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| CN202121728645.9U CN215375005U (en) | 2021-07-28 | 2021-07-28 | Porous material specific surface area measuring device |
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Effective date of registration: 20230526 Address after: Room 2505, Building 1, No. 16 Yuning Road, Gulou District, Nanjing City, Jiangsu Province, 210037 Patentee after: Nanjing sang Li electronic equipment factory Address before: 610065, No. 24, south section of Ring Road, Sichuan, Chengdu Patentee before: SICHUAN University |