CN215866245U - Device for testing adsorption kinetics and adsorption heat - Google Patents
Device for testing adsorption kinetics and adsorption heat Download PDFInfo
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- CN215866245U CN215866245U CN202121723202.0U CN202121723202U CN215866245U CN 215866245 U CN215866245 U CN 215866245U CN 202121723202 U CN202121723202 U CN 202121723202U CN 215866245 U CN215866245 U CN 215866245U
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Abstract
本实用新型提供一种测试吸附动力学和吸附热的装置，所述装置包括：隔热箱体(1)、吸热件(2)、测温元件(3)、样品池(4)、测压元件(5)和吸附气体气源(6)；所述吸热件(2)设于所述隔热箱体(1)内，且所述吸热件(2)设有用于放置所述样品池(4)的样品槽；所述测温元件(3)用于实时检测所述吸热件(2)和所述样品池(4)的温度；所述吸附气体气源(6)通过第一气体通道与所述样品池(4)连通；所述第一气体通道上设有所述测压元件(5)，所述测压元件(5)用于实时检测压力。所述装置结构精巧，成本低，操作简便。
The utility model provides a device for testing adsorption kinetics and adsorption heat, the device comprising: a heat insulation box (1), a heat absorbing member (2), a temperature measuring element (3), a sample pool (4), a measuring a pressure element (5) and an adsorbed gas source (6); the heat absorbing member (2) is arranged in the heat insulation box (1), and the heat absorbing member (2) is provided with a the sample tank of the sample cell (4); the temperature measuring element (3) is used for real-time detection of the temperature of the heat absorbing member (2) and the sample cell (4); the adsorption gas source (6) passes through The first gas channel is in communication with the sample cell (4); the first gas channel is provided with the pressure measuring element (5), and the pressure measuring element (5) is used for real-time pressure detection. The device has compact structure, low cost and simple operation.
Description
Technical Field
The utility model relates to a testing device, in particular to a device for testing adsorption kinetics and adsorption heat.
Background
With the use of fossil energy such as coal and petroleum, the carbon dioxide content in the atmosphere is increasing, resulting in greenhouse effect. Natural gas, whose main component is methane, a relatively clean fossil energy source, produces CO with the same calorific value255 percent lower than coal and 28 percent lower than petroleum, and has low nitrogen and sulfur content and is cleaner. However, the low energy density is a bottleneck limiting the wide application, and it is a current challenge to improve the energy density without affecting the mass transfer rate.
Metal-Organic Frameworks (MOFs) are a novel ordered porous material, and have an ultra-high specific surface area and porosity, so that they have been widely studied in the field of gas storage. The energy density of 9.2MJ/L (263 cm) determined by the United states department of energy to adsorbed natural gas in 2012 can be theoretically achieved at present3/cm3) And 12MJ/kg (0.5g/g) of MOFs materials are available, such as MOF-205, MUF-7a, ST-2, etc. However, in practice, these particulate materials are packed. By adopting multi-stage particle size stacking, higher stacking density can be obtained to improve the actual adsorption amount, but as the stacking density is improved, whether the mass transfer rate of methane is greatly influenced or not is not clear.
In the prior art, equipment for testing high-pressure adsorption kinetics is expensive, the equipment for testing high-pressure adsorption heat is difficult to avoid contacting with air when preparing a sample, and the equipment for testing high-pressure adsorption kinetics can not test adsorption heat while testing adsorption kinetics.
SUMMERY OF THE UTILITY MODEL
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide a device for testing adsorption kinetics and heat of adsorption, which is used for solving the problems that the equipment for testing high-pressure adsorption kinetics in the prior art is expensive, and the adsorption heat and the adsorption kinetics cannot be simultaneously tested.
To achieve the above objects and other related objects, the present invention includes the following technical solutions.
The present invention provides an apparatus for testing adsorption kinetics and heat of adsorption, the apparatus comprising: the device comprises a heat insulation box body, a heat absorbing piece, a temperature measuring element, a sample cell, a pressure measuring element and an adsorbed gas source; the heat absorbing piece is arranged in the heat insulation box body and is provided with a sample groove for placing the sample cell; the temperature measuring element is used for detecting the temperatures of the heat absorbing piece and the sample pool in real time; the adsorption gas source is communicated with the sample cell through a first gas channel; the first gas channel is provided with the load cell, and the load cell is used for detecting pressure in real time.
Preferably, a first valve is arranged on the first gas channel.
Preferably, a pressure reducing valve is further disposed upstream of the first valve in the flowing direction of the gas in the adsorbed gas source.
Preferably, the apparatus further comprises a vacuum pump, the vacuum pump being in communication with the first gas channel via a second gas channel.
Preferably, a second valve is arranged on the second gas channel.
Preferably, a spiral section is arranged at the end of the first gas channel connected with the sample cell, and the spiral section is arranged in the sample groove of the heat absorbing member.
Preferably, the heat insulation box body is also provided with a box door.
Preferably, the temperature measuring element is a thermocouple.
Preferably, the weight of the sample to be detected is 0.5-1.5 g.
Preferably, the temperature change of the heat absorbing member due to the heat of adsorption is within 1 ℃.
In order to achieve a temperature variation of the heat absorbing member of only within 1 ℃, in a preferred embodiment the weight of the heat absorbing member is 1.5-2.5 kg and the weight of the sample cell is 0.4-0.6 kg.
The adsorption material is expected to be inflated and deflated quickly by those skilled in the art, so that the use is more convenient and time-saving, and therefore, the gas adsorption kinetics test of the material under the actual filling condition is important. At the same time, however, the adsorbent is accompanied by an exothermic phenomenon during the adsorption of the gas. If the adsorbent is too much heat released during the adsorption process and is not easily discharged, the overall storage capacity is reduced, and the adsorbent itself is damaged to some extent. Therefore, in the process of selecting a proper adsorbent, the characterization of the adsorption heat of the adsorbent is also important.
The technical scheme has the following beneficial effects:
the method can not only test the high-pressure adsorption kinetics of a large-scale actual filling sample, but also test the adsorption heat of the sample while testing the adsorption kinetics; during testing, the sample cell can be operated in a glove box, so that the sample is prevented from contacting with air. The test equipment subassembly that forms from this is less, and the structure is exquisite, and equipment cost is low, easy and simple to handle during the test.
Drawings
FIG. 1 is a schematic diagram showing the structure of the apparatus for testing adsorption kinetics and heat of adsorption of the present invention.
The reference numerals in fig. 1 are as follows:
1 is a heat insulation box body, 2 is a heat absorbing piece, 3 is a temperature measuring element, 4 is a sample cell, 5 is a pressure measuring element, 6 is an adsorbed gas source, 7 is a vacuum pump, 8 is a first valve, 9 is a second valve, 10 is a spiral section, 11 is a box door, and 12 is a pressure reducing valve.
Detailed Description
The following description of the embodiments of the present invention is provided for illustrative purposes, and other advantages and effects of the present invention will become apparent to those skilled in the art from the present disclosure.
Please refer to fig. 1. It should be understood that the structures, ratios, sizes, and the like shown in the drawings and described in the specification are only used for matching with the disclosure of the specification, so as to be understood and read by those skilled in the art, and are not used to limit the conditions under which the present invention can be implemented, so that the present invention has no technical significance, and any structural modification, ratio relationship change, or size adjustment should still fall within the scope of the present invention without affecting the efficacy and the achievable purpose of the present invention. In addition, the terms "upper", "lower", "left", "right", "middle" and "one" used in the present specification are for clarity of description, and are not intended to limit the scope of the present invention, and the relative relationship between the terms and the terms is not to be construed as a scope of the present invention.
As shown in figure 1, the utility model firstly provides a device for testing adsorption kinetics and adsorption heat, which comprises a heat insulation box body 1, a heat absorbing piece 2, a temperature measuring element 3, a sample cell 4, a load cell 5 and an adsorbed gas source 6;
the heat absorbing piece 2 is arranged in the heat insulation box body 1, and the heat absorbing piece 2 is provided with a sample groove for placing the sample cell 4;
the temperature measuring element 3 is used for detecting the temperatures of the heat absorbing member 2 and the sample cell 4 in real time;
the adsorption gas source 6 is communicated with the sample cell 4 through a first gas channel;
the first gas channel is provided with the load cell 5, and the load cell 5 is used for detecting pressure in real time.
In the present application, the heat absorbing member is used to dilute the heat generated by adsorption so that the temperature does not rise too high to eliminate the influence of temperature on the adsorption kinetics.
In a specific embodiment of the present application, the heat absorbing member 2 is made of a material with good thermal conductivity, such as a copper material, and further specifically, a simple substance of copper.
In one embodiment of the present invention, the sample cell 4 may be made of stainless steel because of its mechanical strength.
In a preferred embodiment, the sample chamber is arranged in the vicinity of the middle of the heat absorbing member 2, as shown in fig. 1.
In a more preferred embodiment, as shown in fig. 1, a first valve 8 is provided in the first gas passage. The first valve 8 may control the admission of the adsorption gas and may also control the rate of admission of the adsorption gas. The first valve 8 is a ball valve.
In a more preferred embodiment, a pressure reducing valve 12 is further provided upstream of the first valve 8 in the flow direction of the gas from the adsorbed gas source 6. More specifically, when the source 6 of the adsorption gas is a high-pressure gas cylinder, the pressure reducing valve 12 is used for reducing the pressure of the high-pressure adsorption gas in the high-pressure gas cylinder to a pressure required for testing.
In a preferred embodiment, the apparatus further comprises a vacuum pump 7, the vacuum pump 7 being in communication with the first gas channel via a second gas channel. The vacuum pump 7 can be combined with a load cell to check whether the gas channel leaks gas or not, and the gas pressure and the vacuum degree in the gas channel can be adjusted according to the actual test requirement.
In a preferred embodiment, a second valve 9 is provided on the second gas passage. In a more specific embodiment, the second valve 9 is a needle valve, which allows a finer adjustment of the flow rate.
In a more preferred embodiment, the load cells 5 include a low range load cell 51 and a high range load cell 52. Specifically, the load cell is a pressure gauge.
In a preferred embodiment, the first gas channel is made of a material with relatively poor heat conduction. Such as stainless steel tubing.
In a preferred embodiment, the end of the first gas channel connected to the sample cell 4 is provided with a spiral section 10, and the spiral section 10 is arranged in the sample groove of the heat absorbing member 2.
In a more specific embodiment, the spiral section 10 is in cooperative communication with the sample cell via a detachable structure. Such as removable communication via a threaded arrangement or the like.
In a specific embodiment of the present application, the heat insulation box body is a sealed heat insulation box, and the inner wall of the heat insulation box body is in contact fit with the heat absorbing member 2 to prevent heat dissipation in the heat absorbing member 2. In a preferred embodiment, the insulated cabinet 1 is further provided with a door 11.
In a specific embodiment of the present application, the temperature measuring element 3 is a thermocouple. In a specific embodiment as shown in fig. 1, a plurality of temperature measuring elements 3 are arranged and distributed on a plurality of positions of the outer walls of the heat absorbing member 2 and the sample cell 4 respectively. More specifically, the temperature measuring elements 3 are multiple, and the multiple temperature measuring elements 3 are used for measuring the temperatures of several places on the outer walls of the heat absorbing member 2 and the sample cell 4, so that the temperatures and temperature changes of the several places in the heat absorbing member 2 and the sample cell 4 can be detected in real time at multiple points, and the average value of the final temperature values at the multiple points is used as the temperature value of the heat absorbing member 2 and the sample cell 4 after adsorption in the adsorption heat calculation.
In a specific embodiment of the present application, the lower portion of the sample cell 4 is not in direct contact with the upper bottom surface of the heat insulation box 1, but is spaced apart from the upper bottom surface, so that heat is dissipated in a direction around the periphery of the sample cell 4, thereby allowing the temperature measuring element 3 to measure more accurately.
The device in the above scheme of this application: the weight of the sample to be detected is 0.5-1.5 g, such as 1 g; the temperature change of the heat absorbing member caused by the heat of adsorption is within 1 ℃. In order to achieve a temperature variation of only within 1 ℃, in a preferred embodiment the heat absorbing member has a weight of 1.5 to 2.5kg and the sample cell has a weight of 0.4 to 0.6 kg. In the embodiment shown in fig. 1, the heat absorbing member is 2 kg.
When the device described above in the present application is used for testing the adsorption kinetics and heat of adsorption of a porous material, the following steps are included:
1) putting a sample to be detected into a sample cell, and connecting the sample to be detected with each gas channel but not communicating the gas channels;
2) firstly, slowly opening a valve 9 for vacuumizing until the pressure does not drop, and observing the pressure change condition on a first gas channel displayed on a pressure measuring element within a period of time after the vacuumizing is stopped so as to judge whether gas leaks; if the air is leaked, checking and reinstalling the air channel to the air leakage-free device; if no air leakage occurs, the following steps are carried out;
3) and opening the valve 8, introducing a certain amount of adsorbed gas, closing the valve, observing and waiting for the numerical values displayed by the load cell 5 and the temperature measuring element 3 to tend to be balanced, and recording the pressure change curve and the temperature change value of the load cell 5 and the temperature measuring element 3 before and after introducing the adsorbed gas along with the time.
4) Calculating the heat released by the sample to be detected after adsorption according to the temperature change before and after adsorption, namely obtaining the adsorption heat; and obtaining an adsorption kinetics curve according to the change of the pressure before and after adsorption along with the time, thereby obtaining the adsorption rate.
Heat of adsorption Q ═ cm. DELTA.T ═ cm (T)t-T0) (ii) a Wherein c is the specific heat capacity, m is the mass, T0Temperature before adsorption, TtThe temperature at which equilibrium is reached after adsorption. When the temperature tends to be balanced after adsorption, the temperature difference of each temperature test point is not large or tends to be consistent. The temperature changes of the sample cell and the heat absorbing member are substantially uniform during the processes before and after the adsorption.
In the present application, the total heat of adsorption can be determined for more accurate determination of the heat of adsorption, which is the total heat of the heat absorbing member 2 and the sample cell 4.
In conclusion, the device has few components and a compact structure, not only can test the high-pressure adsorption kinetics of the sample to be tested, but also can test the adsorption heat of the sample to be tested, and greatly reduces the equipment cost for testing the high-pressure adsorption kinetics in the prior art. Therefore, the utility model effectively overcomes various defects in the prior art and has high industrial utilization value.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the utility model. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (9)
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| Application Number | Priority Date | Filing Date | Title |
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| CN202121723202.0U CN215866245U (en) | 2021-07-27 | 2021-07-27 | Device for testing adsorption kinetics and adsorption heat |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202121723202.0U CN215866245U (en) | 2021-07-27 | 2021-07-27 | Device for testing adsorption kinetics and adsorption heat |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113433029A (en) * | 2021-07-27 | 2021-09-24 | 上海科技大学 | Device and method for testing adsorption kinetics and adsorption heat |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113433029A (en) * | 2021-07-27 | 2021-09-24 | 上海科技大学 | Device and method for testing adsorption kinetics and adsorption heat |
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