CN109142136B - Device and method for measuring loading depth of functional group on surface of pore channel of modified porous material - Google Patents
Device and method for measuring loading depth of functional group on surface of pore channel of modified porous material Download PDFInfo
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Abstract
The invention relates to a device and a method for measuring the loading depth of functional groups on the surface of a pore channel of a modified porous material, wherein the device comprises a gas mixing chamber, a filling column for filling the modified porous material to be measured and a gas analyzer for analyzing the concentration of gas which are sequentially connected, the inlet of the gas mixing chamber is connected with a high-purity nitrogen generator and a gas generator to be measured, two ends of the filling column are blocked and are inserted into a guide pipe for ventilation or exhaust, the filling column is connected with a bypass pipe in parallel, the gas inlet pipe of the filling column is provided with a valve, and a third flow regulator is arranged in front of the gas mixing chamber and the filling column. Compared with the prior art, the method has the advantages of common required instruments, simple operation steps, greatly reduced measurement time and cost consumption, less restriction requirements on the porous material and the modified functional group, and suitability for measurement characterization of most surface functional group modified porous materials.
Description
Technical Field
The invention relates to the field of development of air purification environment-friendly materials, in particular to a device and a method for measuring the loading depth of functional groups on the surface of a pore channel of a modified porous material.
Background
Porous materials have rapidly attracted much attention from many scholars since their invention, with their unique pore structure. The commonly used porous materials comprise activated carbon, activated carbon fibers, carbon nanotubes, zeolite, molecular sieves, macroporous adsorption resin and the like, and have the advantages of large specific surface area, high porosity, rich pore diameters and the like, so the porous materials are widely applied to the fields of adsorption, catalysis, chromatography, gas separation, energy storage and the like. Surface functional group modification is an important means for improving the application performance of porous materials. By loading or grafting different types of chemical functional groups on the surface of the pore channel of the porous material, the chemical properties of the surface of the porous material, such as polarity, acidity and alkalinity, hydrophilicity/hydrophobicity and the like, can be changed so as to adapt to different application purposes.
The loading rate of the modified functional groups on the surfaces of the pores of the porous material is the most common index for evaluating the modification result of the porous material, because the loading rate directly reflects the number of the modified functional groups in the pores. Various influencing factors influencing the loading rate of the chemical functional groups on the surfaces of the pore canals are also studied in detail by a plurality of scholars at home and abroad. However, in addition to the loading rate, the loading depth and distribution of the modified functional groups on the surfaces of the pore channels are also important indexes influencing the modification result of the porous material. The chemical functional groups on the surface of the pore channels of the porous material are required to exert a modification effect, and the first premise is that the chemical functional groups can be contacted with a target substance. For example, in the field of gas adsorption separation, a target gas can be chemisorbed by loading a specific chemical functional group on the surface of a pore channel of a porous material so as to improve the adsorption separation capacity of the target gas. However, chemisorption can be performed smoothly only when the adsorbed gas molecules can come into contact with the modified functional groups on the surfaces of the pores. If the loading depth of the modified functional group on the surface of the pore channel is far greater than the depth which can be reached by adsorbed gas, the modified functional group is wasted; if the modified functional group only gathers and loads at the outer port of the pore channel, on one hand, adsorbed gas molecules can be prevented from entering the pore channel of the porous material, and meanwhile, the utilization rate of the modified functional group is low. Therefore, the distribution and the loading depth of the modified functional groups in the porous material pore channels are effectively represented, and the method has great significance for optimizing modification experimental parameters and improving the modification effect of the porous material.
At present, methods capable of measuring and characterizing the distribution and loading depth of the modified functional groups in the pore channels of the porous material are limited, and the most used technology reported in the literature is a confocal laser scanning microscope and fluorescent probe combined technology. But the method has obvious defects that firstly, the instrument is expensive and the operation is complex; secondly, the restriction conditions on the porous material and the modified functional group are multiple, and the porous material is required to be penetrated by confocal laser, and the modified functional group is required to have a 1:1 chemical reaction with the fluorescent probe. Therefore, the method for measuring the loading depth of the functional group on the surface of the pore channel of the modified porous material by using the gas adsorption method can quickly and accurately represent the loading depth of the modified functional group on the surface of the pore channel of the porous material, effectively evaluate the modification result of the functional group on the surface of the porous material and provide scientific basis for further optimizing modification.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a device and a method for measuring the loading depth of functional groups on the surface of pore channels of a modified porous material
The purpose of the invention can be realized by the following technical scheme: the device comprises a gas mixing chamber, a filling column and a gas analyzer, wherein the gas mixing chamber, the filling column and the gas analyzer are sequentially connected, the filling column is used for filling modified porous materials to be detected, the gas analyzer is used for analyzing gas concentration, an inlet of the gas mixing chamber is connected with a high-purity nitrogen generator and the gas generator to be detected, two ends of the filling column are closed, a guide pipe is inserted into the filling column for ventilation or exhaust, the filling column is connected with a bypass pipe in parallel, a valve is arranged in a gas inlet pipe of the filling column, and a third flow regulator is arranged in front of the gas mixing chamber and the filling column.
And a first flow regulator and a second flow regulator are respectively arranged on connecting pipelines of the high-purity nitrogen generator, the gas generator to be detected and the gas mixing chamber.
The ends of the packed column are closed by a plug of silanized glass wool and inserted into a catheter for venting or venting.
The packed column is placed in the temperature control box, and the influence of the temperature on adsorption is large, so that the adsorption capacity of the modified porous material to be detected at different temperatures can be measured by the arrangement.
A method for measuring the loading depth of functional groups on the surfaces of the pore channels of a modified porous material by using the device comprises the following steps:
(1) filling the modified porous material to be detected in the packed column, blocking the two ends of the packed column,
(2) opening the high-purity nitrogen generator, and exhausting impurities adsorbed in the device and the pore channel of the modified porous material to be detected;
(3) opening a gas generator to be detected, adjusting the concentration of the gas to be detected and the high-purity nitrogen, closing a valve of a gas inlet pipe of the packed column, opening a bypass pipe, and determining the concentration of the gas to be detected in the initial gas through a gas analyzer;
(4) closing the bypass pipe, opening a valve of a gas inlet pipe of the packed column, recording the concentration of the gas to be detected in real time through a gas analyzer until the modified porous material to be detected is saturated in adsorption, recording the time required by the saturation in adsorption, and calculating the adsorption quantity by utilizing an adsorption penetration curve, wherein the calculation method of the adsorption quantity Q comprises the following steps:
wherein: f is the flow rate of the gas to be measured, C is the initial concentration of the gas to be measured, m is the mass of the modified porous material to be measured in the packed column, and taIs the integration time used for the adsorption process. t is taThe calculation method of (2) is as follows:
wherein: c is the initial concentration of the gas to be measured, C1The real-time concentration of the gas to be measured at the downstream of the packed column. (ii) a
(5) And (5) repeating the steps (2) to (4), changing the flow of the gas introduced into the packed column through the third flow regulator, ensuring that the first flow regulator and the second flow regulator are not changed and the concentration of the gas to be detected is not changed at the moment, obtaining the adsorption capacity under different flow rates, and then calculating to obtain the loading depth of the functional group on the surface of the pore channel of the modified porous material.
The method for judging whether the modified porous material is saturated or not in the step (4) is that the concentration of the gas to be detected in the real-time gas measured by a gas analyzer is equal to 95% of the concentration of the gas to be detected in the initial gas, the adsorbed gas is selected to be the gas which can be chemically grafted with the surface functional groups of the modified porous material in a ratio of 1:1, the concentration of the adsorbed gas is a certain value between 100ppm and 200ppm, and the adsorbed gas is kept unchanged in the whole testing process.
And (5) gradually reducing the gas flow in the step (5), wherein the reduction amount is 5-50 mL/min each time. The amount of each reduction at the early stage may be larger. The later, the smaller the reduction amount is, so that the time when the adsorption amount is kept unchanged can be accurately obtained, and the accurate t can be obtained.
And when the adsorption amounts of two adjacent tests are the same, obtaining the time t required by the penultimate adsorption saturation.
The method for calculating the loading depth d of the functional group on the surface of the pore channel of the modified porous material comprises the following steps:
wherein D is the diffusion coefficient of the modified porous material to be detected, C is the concentration of the gas to be detected, X is the diffusion direction of the gas to be detected,
is the concentration gradient of the gas to be measured, indicates that the diffusion direction is the opposite direction of the concentration gradient, and rho is the density of the gas to be measured.
The above-mentioned
The solution of (2) is the concentration of the gas to be measured divided by the unit length.
Compared with the prior art, the beneficial effects of the invention are embodied in the following aspects:
(1) the method related by the invention not only can describe the loading condition of the modified functional group on the surface of the pore channel of the porous material macroscopically, but also can quantitatively calculate the loading depth and the distribution condition of the modified functional group in the pore channel from a microscopic angle.
(2) The method provided by the invention has the advantages of common required instruments, simple operation steps and capability of greatly reducing the measurement time and cost consumption.
(3) The method has less restriction requirements on the porous material and the modified functional group, and is suitable for measurement and characterization of most of the surface functional group modified porous materials.
Drawings
FIG. 1 is a schematic diagram of the connection of the present invention.
The system comprises a gas generator to be tested, a high-purity nitrogen generator, a pressure reducing valve, a first flow regulator, a second flow regulator, a first three-way valve, a gas mixing chamber, a second three-way valve, an exhaust valve, a third flow regulator, a third three-way valve, a filling column, a temperature control box, a bypass pipe, a fourth three-way valve and a gas analyzer, wherein the gas generator is 1, the high-purity nitrogen generator is 2, the pressure reducing valve is 3, the first flow regulator is 4, the second flow regulator is 5, the first three-way valve is 6, the gas mixing chamber is 7, the second three-way.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
A device for measuring the loading depth of functional groups on the surface of a pore channel of a modified porous material is structurally shown in figure 1 and comprises a gas mixing chamber 7, a filling column 13 for filling the modified porous material to be measured and a gas analyzer 17 for analyzing the concentration of gas which are sequentially connected, wherein the inlet of the gas mixing chamber 6 is connected with a high-purity nitrogen generator 2 and the gas generator 1 to be measured, the outlet of the gas generator 1 to be measured is provided with a pressure reducing valve 3, a first flow regulator 4 is arranged on a pipeline and finally led into one inlet of a first three-way valve 6, the outlet of the high-purity nitrogen generator 2 is provided with a pressure reducing valve 3, a second flow regulator 5 is arranged on the pipeline and finally led into the other inlet of the first three-way valve 6, and the outlet of the first three-way valve 6 is connected with the gas mixing chamber 7. An outlet of the gas mixing chamber 7 is connected with an inlet of a second three-way valve 8, one outlet of the second three-way valve 8 is connected with the tail gas treatment unit through an exhaust valve 9, and the other outlet of the second three-way valve 8 is connected with an inlet of a third three-way valve 11 through a third flow regulator 10. One outlet of the third three-way valve 11 is connected with the inlet of the packing column 13 through a valve 12, the other outlet of the third three-way valve 11 is connected with a bypass pipe 15, and the bypass pipe 15 is provided with a valve. The outlet of the packed column 13 and the outlet of the bypass pipe 15 are connected to two inlets of a fourth three-way valve 16, and the outlet of the fourth three-way valve 16 is connected to a gas analyzer.
Both ends of the packed column 13 were closed by silanized glass wool and a catheter was inserted for aeration or deaeration, and the packed column 13 was placed in a temperature control box 14.
The device is used for testing, and the specific method is as follows:
0.5g of the sulfonic acid group-modified porous material was placed in a packed column having a length of 0.5cm and an inner diameter of 0.7 cm. The two ends of the packed column are plugged with silanized glass wool and placed in a constant temperature control box. The upstream of the packed column is connected with a gas mixing box, and two gas inlets of the gas mixing box are respectively connected with high-purity nitrogen and 100ppm NH3A gas. The downstream of the packed column is connected with NH3Gas analyzer for real-time on-line monitoring of NH3The concentration of (c). By carrying out NH3Before the adsorption experiment, high-purity nitrogen is introduced into the packed column at the flow rate of 300mL/min for 1 hour under the condition of 80 ℃ so as to fully remove impurities adsorbed by the sulfonic modified porous material. After introducing high-purity nitrogen gas for 1 hour, NH was introduced into the pack at a flow rate of 400mL/min at 25 ℃3Gas, according to NH downstream of the packed column3Reading of a gas analyzer, and calculating NH of the sulfonic modified porous material3Adsorption quantity, denoted as Q1Then replacing the sulfonic acid modified porous material with new NH3The flow rate of the gas is reduced to 350mL/min, and the above steps are repeated, at this time, NH is added3The adsorption capacity is recorded as Q2. Up to Qn-1＝QnWhen the reaction is stopped (n is the number of adsorption experiments), NH is stopped3Adsorption experiment, at this time NH3Flow rate of gas Fd. According to NH3The diffusion flux J can be obtained from the diffusion coefficient D of the gas in the sulfonic acid group modified porous material under the conditions of 25 ℃ and 100ppm, and the loading depth D of the sulfonic acid group in the pore channel of the porous material can be obtained according to a formula. The specific experimental results are as follows:
TABLE 1 NH3Results of adsorption experiment (25 ℃, 100ppm)
| NH3Flow (F, mL/min) | Adsorption saturation time (t, s) | NH3Adsorption capacity (Q, mg/g) |
| 500 | 108 | 20.87 |
| 450 | 201 | 22.94 |
| 400 | 286 | 24.61 |
| 350 | 349 | 26.01 |
| 300 | 401 | 27.88 |
| 250 | 430 | 28.25 |
| 225 | 437 | 28.33 |
| 200 | 438 | 28.34 |
As can be seen from the above table, Fd＝300mL/min；
Known NH3Diffusion coefficient D of 0.8e-5cm at 25 deg.C2/s；ρ＝7.59e-8g/cm3；
t＝430s；
C＝100ppm＝7.59e-8g/cm3。
According to the formula:
the depth d of the sulfonic acid group supported in the pores of the porous material was calculated to be 15.01 μm.
Example 2
The same apparatus as in example 1 was used, and the operation was as follows:
0.5g of the amino-modified porous material was placed in a packed column having a length of 0.5cm and an inner diameter of 0.7 cm. The two ends of the packed column are plugged with silanized glass wool and placed in a constant temperature control box. The upstream of the packed column is connected with a gas mixing box, and two gas inlets of the gas mixing box are respectively connected with high-purity nitrogen and 100ppm SO2A gas. Packed column downstream connection SO2Gas analyzer for real-time on-line monitoring of SO2The concentration of (c). Carrying out SO2Before the adsorption experiment, high-purity nitrogen is introduced into the packed column at the flow rate of 300mL/min for 1 hour under the condition of 80 ℃ so as to fully remove impurities adsorbed by the amino modified porous material. After introducing high-purity nitrogen gas for 1 hour, SO was introduced into the pack at a flow rate of 400mL/min at 25 ℃2Gas, according to SO downstream of the packed column2Reading by a gas analyzer, and calculating the SO of the amino modified porous material2Adsorption quantity, denoted as Q1Then replacing the amino modified porous material with new one, and adding SO2The flow rate of the gas is reduced to 350mL/min, and the above steps are repeated, at this timeSO2The adsorption capacity is recorded as Q2. Up to Qn-1＝QnWhen (n is the number of adsorption experiments), the SO is stopped2Adsorption experiment, at this time SO2Flow rate of gas Fd. According to SO2The diffusion flux J can be obtained by the diffusion coefficient D of the gas in the amino modified porous material under the conditions of 25 ℃ and 100ppm, and the loading depth D of the amino in the pore channel of the porous material can be obtained according to a formula. The specific experimental results are as follows:
TABLE 2 SO2Results of adsorption experiment (25 ℃, 100ppm)
| SO2Flow (F, mL/min) | Adsorption saturation time (t, s) | SO2Adsorption capacity (Q, mg/g) |
| 500 | 378 | 40.21 |
| 450 | 498 | 44.09 |
| 400 | 582 | 46.59 |
| 350 | 689 | 50.10 |
| 300 | 753 | 54.89 |
| 250 | 789 | 56.34 |
| 225 | 807 | 57.80 |
| 200 | 812 | 57.89 |
| 175 | 813 | 57.90 |
As can be seen from the above table, Fd＝200mL/min；
Known SO2Diffusion coefficient D of 1.1e-5cm at 25 deg.C2/s；ρ＝2.86e-7g/cm3；
t＝812s；
C＝100ppm＝2.86e-7g/cm3。
According to the formula:
the depth d of the sulfonic acid group supported in the pores of the porous material was calculated to be 29.81 μm.
Claims (8)
1. The device is characterized by comprising a gas mixing chamber, a filling column and a gas analyzer, wherein the gas mixing chamber, the filling column and the gas analyzer are sequentially connected, the filling column is used for filling a modified porous material to be detected, the gas analyzer is used for analyzing gas concentration, an inlet of the gas mixing chamber is connected with a high-purity nitrogen generator and a gas generator to be detected, two ends of the filling column are closed, a guide pipe is inserted into the filling column for ventilation or exhaust, the filling column is connected with a bypass pipe in parallel, a valve is arranged in an air inlet pipe of the filling column, and a third flow regulator is arranged in front of the gas mixing chamber and the filling column.
2. The apparatus according to claim 1, wherein the first flow regulator and the second flow regulator are respectively disposed on the connecting lines of the high-purity nitrogen generator, the gas generator to be measured and the gas mixing chamber.
3. The device for determining the loading depth of the functional groups on the surfaces of the pore channels of the modified porous material as claimed in claim 1, wherein the two ends of the packed column are plugged by silanized glass wool and inserted into a catheter for ventilation or air exhaust.
4. The apparatus for determining the loading depth of the functional groups on the surfaces of the pore channels of the modified porous material according to claim 1, wherein the packed column is placed in a temperature control box.
5. A method for measuring the loading depth of functional groups on the surfaces of the pore channels of a modified porous material by using the device as claimed in any one of claims 1 to 4, which is characterized by comprising the following steps:
(1) filling the modified porous material to be detected in the packed column, blocking the two ends of the packed column,
(2) opening the high-purity nitrogen generator, and exhausting impurities adsorbed in the device and the pore channel of the modified porous material to be detected;
(3) opening a gas generator to be detected, adjusting the concentration of the gas to be detected and the high-purity nitrogen, closing a valve of a gas inlet pipe of the packed column, opening a bypass pipe, and determining the concentration of the gas to be detected in the initial gas through a gas analyzer;
(4) closing the bypass pipe, opening a valve of a gas inlet pipe of the packed column, recording the concentration of the gas to be detected in real time through a gas analyzer until the modified porous material to be detected is saturated in adsorption, recording the time required by the saturation in adsorption, and calculating the adsorption capacity by using an adsorption penetration curve;
(5) repeating the step (2) to the step (4), changing the flow of gas introduced into the packed column through a third flow regulator to obtain the adsorption capacity under different flow rates, and then calculating to obtain the loading depth of the functional group on the surface of the pore channel of the modified porous material;
the method for calculating the loading depth d of the functional group on the surface of the pore channel of the modified porous material comprises the following steps:
wherein D is the diffusion coefficient of the modified porous material to be detected, C is the concentration of the gas to be detected, X is the diffusion direction of the gas to be detected,
the concentration gradient of the gas to be measured, represents that the diffusion direction is the opposite direction of the concentration gradient, and rho is the density of the gas to be measured;
the above-mentioned
The solution of (2) is the concentration of the gas to be measured divided by the unit length.
6. The method for determining the loading depth of the functional group on the surface of the pore channel of the modified porous material as claimed in claim 5, wherein the method for determining whether the adsorption of the modified porous material is saturated in step (4) is that the concentration of the gas to be measured in the real-time gas measured by the gas analyzer is equal to 95% of the concentration of the gas to be measured in the initial gas.
7. The method for determining the loading depth of the functional groups on the surfaces of the pores of the modified porous material as claimed in claim 5, wherein the gas flow rate in step (5) is gradually reduced by 5-50 mL/min.
8. The method for determining the loading depth of the functional groups on the surfaces of the pore channels of the modified porous material as claimed in claim 7, wherein the time t required for the penultimate adsorption saturation is obtained when the adsorption amounts of two adjacent tests are the same.
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