CN115651258A - Co-BPDC/MXene composite material, preparation method and application - Google Patents
Co-BPDC/MXene composite material, preparation method and application Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000000463 material Substances 0.000 claims abstract description 33
- 239000012855 volatile organic compound Substances 0.000 claims abstract description 18
- 238000001514 detection method Methods 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 47
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 44
- 239000000243 solution Substances 0.000 claims description 20
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 16
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 15
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 12
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 235000011837 pasties Nutrition 0.000 claims description 3
- 238000001338 self-assembly Methods 0.000 claims description 3
- 238000001179 sorption measurement Methods 0.000 claims description 3
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- 238000002156 mixing Methods 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 230000004044 response Effects 0.000 abstract description 37
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 61
- 238000003756 stirring Methods 0.000 description 7
- 239000012621 metal-organic framework Substances 0.000 description 5
- 230000008569 process Effects 0.000 description 5
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- 230000001070 adhesive effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
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- 238000009210 therapy by ultrasound Methods 0.000 description 2
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- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
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- 238000002474 experimental method Methods 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 239000012212 insulator Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000012924 metal-organic framework composite Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- -1 polytetrafluoroethylene Polymers 0.000 description 1
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 1
- 239000004810 polytetrafluoroethylene Substances 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 230000002335 preservative effect Effects 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000007790 scraping Methods 0.000 description 1
- 239000007784 solid electrolyte Substances 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- CCEKAJIANROZEO-UHFFFAOYSA-N sulfluramid Chemical group CCNS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F CCEKAJIANROZEO-UHFFFAOYSA-N 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a Co-BPDC/MXene composite material, a preparation method and application thereof, and belongs to the field of gas sensitive materials. The Co-BPDC/MXene composite material-based gas sensor has a high response value to a target gas at 110 ℃, and due to the high specific surface area and rich porous structure of the Co-BPDC/MXene material, the VOCs sensor made of the Co-BPDC/MXene composite material can remarkably improve the response value and sensitivity to VOC gas. On the other hand, the sensor has obvious linear relation between the response value and the concentration in the range of the acetone gas concentration of 10ppm to 50ppm, and also shows high response value in the acetone gas of 100ppm and above. This shows that the sensor has better detection lower limit and range, and better meets the market requirement.
Description
Technical Field
The invention belongs to the field of gas-sensitive materials, and particularly relates to a Co-BPDC/MXene composite material, a preparation method and application thereof.
Background
Volatile Organic Compounds (VOCs) are volatile organic substances with melting points below room temperature and boiling points between 50-260 c, which are found everywhere in the productive life of people. The discharge of excessive VOCs into the atmosphere can cause great harm to human bodies and the environment, for example, VOCs are often the precursors of chemical smog, and human bodies can cause diseases and even die after being excessively inhaled or exposed to the gas environment of VOCs for a long time. The gas sensor is widely concerned and researched by people as a quick, convenient and low-cost method for detecting VOCs. With the development of society and technology, gas sensors which can only detect single VOC gas and have poor performance cannot meet the requirements of more and more abundant production and living of people in the past. In order to promote the further development of gas sensors, research on gas sensors in recent years focuses on the aspects of materials, algorithms, devices, mechanisms and the like, so as to develop VOCs sensors with better performance, lower cost and more convenient carrying. Among them, the development of high-performance gas-sensitive materials is one of the most important aspects for improving the performance of sensors. Metal organic framework Materials (MOFs) are a new class of organic-inorganic hybrid materials, which have the advantages of high specific surface area, various structures, good stability, etc., and these characteristics have attracted people's interest in applying them to the field of gas sensing. However, the conventional MOF materials exhibit insulator properties due to their structural characteristics, which severely hampers the application of MOFs to gas sensors.
The optical gas sensor for detecting the VOC gas has the excellent performances of high accuracy and short response time, but the optical sensor has the defects of complex structure, high manufacturing cost and higher subsequent maintenance cost. The electrical gas sensor can be divided into a semiconductor type, a solid electrolyte type, an electrochemical type and the like, and the most common semiconductor type sensor has the defects of poor selectivity, high working temperature, high energy consumption, easy environmental influence and the like. Therefore, the preparation of the gas sensitive material with high sensitivity, interference resistance, good selectivity and low working temperature is still an important direction for the development of the electrical gas sensor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a Co-BPDC/MXene composite material, a preparation method and application.
In order to achieve the purpose, the invention adopts the following technical scheme to realize the purpose:
a preparation method of a Co-BPDC/MXene composite material comprises the following operations:
mixing MXene and Co (NO) 3 ) 2 ·6H 2 Dispersing O in N, N-dimethylformamide, and carrying out electrostatic adsorption self-assembly to obtain a mixed solution;
dispersing a terephthalic acid solution with DMF as a solvent in the mixed solution, and then sequentially adding ethanol and water to form a precursor solution;
transferring the precursor solution into a reaction kettle, filling Ar gas, reacting for 12 hours at 140 ℃, centrifuging for multiple times after the reaction is finished, and collecting precipitates to obtain the Co-BPDC/MXene composite material.
Further, 0.035g of MXene and 0.2328g of Co (NO) were dispersed in 15ml of N, N-dimethylformamide in the mixed solution 3 ) 2 ·6H 2 O；
0.1938g of terephthalic acid was dispersed in 10ml of DMF solution.
Further, 0.1938g of terephthalic acid was added to 15ml of N, N-dimethylformamide in the mixed solution.
Further, 2ml of ethanol and 2ml of water were added to 15ml of N, N-dimethylformamide in the precursor solution.
The Co-BPDC/MXene composite material is prepared according to the preparation method provided by the invention.
Further, the gas sensitive material is used for detecting the concentration of VOCs.
Further, grinding the Co-BPDC/MXene, and adding ethanol for multiple times in the grinding process to finally obtain pasty liquid;
and coating the paste liquid on a counter electrode, and obtaining the Co-BPDC/MXene gas sensitive element after ethanol volatilizes.
Further, the working temperature during detection is 110 ℃.
Further, the detection gas is acetone, methanol, n-propanol, toluene, ethanol and formaldehyde.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the Co-BPDC/MXene composite material provided by the invention is simple and can be implemented, and the Co-BPDC/MXene composite material is prepared by compounding materials by a hydrothermal method.
According to the Co-BPDC/MXene composite material and the application thereof, the gas sensor based on the Co-BPDC/MXene composite material has a high response value to the target gas at 110 ℃, and due to the high specific surface area and rich porous structure of the Co-BPDC/MXene material, the response value and the sensitivity to the VOC gas can be remarkably improved by the VOCs sensor made of the material. On the other hand, the sensor has obvious linear relation between the response value and the concentration in the range of the acetone gas concentration of 10ppm to 50ppm, and also shows high response value in the acetone gas of 100ppm and above. This shows that the sensor has better detection lower limit and range, and better meets the market requirement. Finally, the MXene/MOF composite material effectively overcomes the defects of instability of the MXene material and poor conductivity of the MOF material.
Drawings
FIG. 1 is a graph showing the relationship between the sensitivity of a Co-BPDC/MXene gas sensor to 100ppm acetone gas and the operating temperature;
FIG. 2 is a graph showing the dynamic response of a Co-BPDC/MXene gas sensor to acetone gas of different concentrations at a working temperature of 110 ℃;
FIG. 3 shows the response values of the Co-BPDC/MXene gas sensor to five different VOC gases at the working temperature of 110 ℃.
Detailed Description
In order to make those skilled in the art better understand the technical solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used is interchangeable under appropriate circumstances such that the embodiments of the invention described herein are capable of operation in sequences other than those illustrated or described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
The invention is described in further detail below with reference to the accompanying drawings:
the invention provides a method for manufacturing a VOCs gas sensor based on a Co-BPDC/MXene composite material. The Co-BPDC/MXene material is synthesized according to the following process, and the obtained material is uniformly coated on an electrode to finally prepare the tiny indirectly heated gas sensitive element. A series of tests were performed on the performance of the sensor. For example, the optimum operating temperature of the sensor for 100ppm acetone gas; dynamic response to acetone gas of different concentrations and comparison of response values for multiple VOC gases at optimum operating temperatures. The experimental result shows that the sensor has good sensitivity and detection limit, and has the potential of being made into a flexible wearable gas sensor.
Examples
(1) Synthesis of MXene materials
Firstly, measuring 20ml 12mol/L HCl, transferring the HCl into a centrifugal tube for standby, then, weighing 1.2g LiF (99%) into HCl, placing the solution into an oil bath pan to enable the liquid temperature to reach 40 ℃, and then stirring for 20min (18 r). Weighing 1.0g MAX (Ti) with balance 3 AlC 2 ) Solid, added to the above system in small portions over ten minutes. After the raw material is added, ar gas is filled into the centrifugal tube, andsealing with a preservative film, covering tightly with a cover, placing in a 40 ℃ water bath kettle, and stirring at the rotating speed of 18r for reaction for 48h. After the reaction is finished, taking out the centrifugal tubes, averagely transferring the liquid in the centrifugal tubes into another two new centrifugal tubes, respectively adding a small amount of water, then putting the centrifugal tubes into a centrifugal machine, setting the rotating speed of the centrifugal machine to 3000r, centrifuging the liquid for 2min to make the liquid sticky, pouring out the upper layer liquid, adding water to 45ml, then putting the centrifugal machine into the centrifugal machine again to centrifuge for 5min at the rotating speed of 3500r, centrifuging for four times to precipitate sticky, and testing that the pH of the upper layer liquid is close to neutral. And stirring and shaking the clay-like precipitate uniformly, adding water to mix into uniform liquid, transferring the liquid into a round-bottom flask, and carrying out ice bath ultrasound for 4 hours while stirring. After the ultrasonic treatment, the mixture was centrifuged at 3500r for 1 hour in a centrifuge, and the supernatant liquid was collected. Pre-freezing the collected liquid, freeze-drying, and collecting MXene (Ti) 3 C 2 ) And (5) performing vacuum freezing storage.
(2) Synthetic Co-BPDC/MXene composite material
0.035g MXene sample was weighed, the solid was transferred to 15ml N, N-Dimethylformamide (DMF) solution and dispersed evenly by ultrasound in ice bath for 20 min. Then 0.2328g of Co (NO) was added 3 ) 2 ·6H 2 And adding the O sample into MXene dispersion liquid, performing ultrasonic treatment for 15min, and performing electrostatic adsorption self-assembly. 0.1938g of terephthalic acid (BPDC) solid was dissolved in 10ml of DMF solution and sonicated for 15min to fully dissolve. The prepared BPDC solution was poured into MXene dispersion in which cobalt ions were dissolved with stirring, and then 2ml of ethanol and 2ml of water were rapidly added in this order, followed by stirring at room temperature for 30min. After stirring uniformly, transferring the solution into a 100ml polytetrafluoroethylene reaction kettle, charging Ar gas, and placing the reaction kettle in a muffle furnace to maintain at the high temperature of 140 ℃ for 12 hours. And after the temperature of the solution is reduced to room temperature, centrifuging the solution by using a centrifuge, alternately centrifuging the solution by using DMF (dimethyl formamide) and ethanol reagents for three times, pouring off supernatant, and collecting final precipitate. And pre-freezing the product, performing freeze drying, and collecting for later use.
(3) Preparation of Co-BPDC/MXene gas-sensitive element
Carefully scraping the frozen Co-BPDC/MXene sample from the bottom of a glass dish, collecting the scraped solid particles into a sealed bag, putting the sealed bag into a mortar, adding an adhesive ethanol for multiple times in the grinding process to keep the sample uniformly dispersed in the reagent, and finally preparing the sample into uniform pasty liquid. The adjusted paste sample was applied to both pairs of gold electrodes with a brush pen to ensure uniform and complete coverage of the electrodes and failure to apply to the heater electrodes. And obtaining the Co-BPDC/MXene gas-sensitive element after the adhesive is completely volatilized.
(4) Testing of Material Properties
The Co-BPDC/MXene gas sensor was tested for various properties for acetone gas using a related instrument. The response of the Co-BDC/MXene material to acetone gas at 100ppm concentration at five different temperatures (80 deg.C, 100 deg.C, 110 deg.C, 120 deg.C and 140 deg.C) was first tested by an instrument and finally the optimum working temperature of the material was found to be 110 deg.C. The dynamic response of the Co-BPDC/MXene material to acetone gas with different concentrations at the optimal working temperature is tested, and the material is found to have a good linear relation between the response value of the sensor and the concentration of the acetone gas in the range of 10ppm to 50ppm, when the concentration of the acetone gas is more than or equal to 100ppm, the response value of the sensor can reach more than 25, and the increase of the response value can be slowed down until the response value is smooth. Finally, response values of the Co-BPDC/MXene composite material to six different organic volatile compounds (acetone, methanol, n-propanol, toluene, ethanol and formaldehyde respectively) with concentrations of 100ppm at a working temperature of 110 ℃ are tested, and the response value of the Co-BPDC/MXene composite material to acetone gas is higher than that of the other five gases, but the response values to the n-propanol, the toluene and the ethanol are higher and cannot be obviously distinguished from the acetone gas.
The response values of the Co-BPDC/MXene composite material to 100ppm acetone gas at different temperatures are tested, and as can be seen from FIG. 1, the response value of the material to the target gas shows a movement trend of increasing firstly and then decreasing with the increase of the temperature, the whole material shows a volcano shape, the response value of the material to the acetone gas reaches a maximum of about 26 at the temperature of 110 ℃, the response value shows a very good response value of the Co-BPDC/MXene material to the acetone gas, and the optimal working temperature of 110 ℃ is far lower than that of a common metal oxide semiconductor material-based sensor. Secondly, the dynamic response of the Co-BPDC/MXene material at the temperature of 110 ℃ in the atmosphere of acetone with different concentrations is tested, the test range is 10ppm-300ppm, and the test result is shown in figure 2. The experimental results show that in the range of 30-200ppm, there is an almost linear relationship between the sensor response value and the acetone gas concentration, and the sensor response value increases with the increase of the acetone gas concentration. When the acetone gas is higher than 200ppm, the response value of the sensor is increased and slowed down, and the response value of the sensor at 10ppm to the acetone gas is still about 2, so that the Co-BPDC/MXene material-based sensor has a satisfactory detection lower limit and a satisfactory detection range. Finally, we tested the response of the Co-BPDC/MXene material to six different kinds of organic volatile gases (acetone, methanol, n-propanol, toluene, ethanol and formaldehyde) at the optimum working temperature (110 ℃), with the test gas concentrations all being 100ppm. The results of the experiment (see fig. 3) show that the response values of the materials to them are 26, 3.8, 23, 20, 22 and 4.2 in sequence. The sensor has a response value of 26 at most to acetone gas, shows good response performance to the acetone gas, and has response values of about 20 to n-propanol, toluene and ethanol.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (9)
1. The preparation method of the Co-BPDC/MXene composite material is characterized by comprising the following operations:
mixing MXene and Co (NO) 3 ) 2 ·6H 2 Dispersing O in N, N-dimethylformamide, and carrying out electrostatic adsorption self-assembly to obtain a mixed solution;
dispersing a terephthalic acid solution with DMF as a solvent in the mixed solution, and then sequentially adding ethanol and water to form a precursor solution;
transferring the precursor solution into a reaction kettle, filling Ar gas, reacting for 12 hours at 140 ℃, centrifuging for many times after the reaction is finished, and collecting precipitates to obtain the Co-BPDC/MXene composite material.
2. The method of claim 1, wherein 0.035g MXene and 0.2328g Co (NO) are dispersed in 15ml N, N-dimethylformamide in the mixture 3 ) 2 ·6H 2 O；
0.1938g of terephthalic acid was dispersed in 10ml of DMF solution.
3. The method of claim 2, wherein 0.1938g of terephthalic acid is added to 15ml of N, N-dimethylformamide in the mixed solution.
4. The method of claim 2, wherein 2ml ethanol and 2ml water are added to 1 ml N, N-dimethylformamide in the precursor solution.
5. A Co-BPDC/MXene composite characterized by being prepared according to the preparation method of any one of claims 1-4.
6. The use of the Co-BPDC/MXene composite of claim 5 as a gas sensitive material for detecting the concentration of VOCs.
7. The application of the Co-BPDC/MXene composite material according to claim 6, wherein the Co-BPDC/MXene is ground, ethanol is added for multiple times during grinding, and finally pasty liquid is obtained;
and coating the paste liquid on a counter electrode, and obtaining the Co-BPDC/MXene gas sensor after ethanol volatilizes.
8. The use of the Co-BPDC/MXene composite according to claim 6, characterized in that the working temperature at the time of detection is 110 ℃.
9. The use of the Co-BPDC/MXene composite of claim 6, wherein the detection gas is acetone, methanol, n-propanol, toluene, ethanol and formaldehyde.
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| CN116106379A (en) * | 2023-02-27 | 2023-05-12 | 中国医学科学院药用植物研究所 | Composite material, preparation method thereof and application thereof in electrochemical detection of tanshinol |
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| CN116106379A (en) * | 2023-02-27 | 2023-05-12 | 中国医学科学院药用植物研究所 | Composite material, preparation method thereof and application thereof in electrochemical detection of tanshinol |
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