CN108421541B - Preparation method and application of Zn-carbide-based MOFs extraction coating - Google Patents
Preparation method and application of Zn-carbide-based MOFs extraction coating Download PDFInfo
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- CN108421541B CN108421541B CN201810216394.2A CN201810216394A CN108421541B CN 108421541 B CN108421541 B CN 108421541B CN 201810216394 A CN201810216394 A CN 201810216394A CN 108421541 B CN108421541 B CN 108421541B
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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Abstract
The invention discloses a preparation method and application of a Zn carbide-based MOFs extraction coating, wherein the preparation method comprises the following steps: synthesizing ZIF-8 coating and carbonizing; the application is as follows: the method for analyzing the aromatic smelly pollutants in the water body is established, and specifically comprises the following steps: the extraction experiment is carried out on the carbonized Zn-based MOFs extraction coating material under the conditions of extraction temperature of 20-50 ℃, extraction time of 20-80min, desorption time of 0.5-4min, desorption temperature of 200-270 ℃ and salt concentration of 0-37%, the extraction effect difference of the extraction coating and the commercial fiber coating before and after carbonization is compared, and the thermal stability and the chemical stability of the synthesized coating are researched. The material of the invention has simple preparation, convenient operation, low cost and good reproducibility of the establishing method. Therefore, the method is used for detecting the aromatic smelly substances in the polluted water body, and has good economic and environmental benefits.
Description
Technical Field
The invention relates to the technical field of inorganic materials and water treatment, in particular to a preparation method and application of a carbonized Zn-based MOFs (metal-organic frameworks) carbonized coating.
Background
The basic principle of the solid-phase microextraction technology is to immobilize the coating material with extraction function on the surface of a certain substrate by a physical or chemical method. The coating is directly or indirectly contacted with the sample to enrich and concentrate the target analyte, and then the coating is directly placed at a sample inlet for thermal desorption and is combined with a sample injection device or is injected after solvent desorption, so that the target in the sample is accurately analyzed. To date, the most widely used is fibrous solid phase microextraction. The method comprises two steps of extraction and desorption: (1) and (3) extraction process: inserting the solid phase microextraction stainless steel protective sheath into the sample bottle, pushing out the coating part to extract the sample, and withdrawing the extraction coating into the stainless steel needle tube after a period of time, thus finishing the extraction process. (2) And (3) desorption process: the gas chromatographic analysis adopts thermal desorption to desorb the target substance on the coating, namely, the extraction fiber which has finished the extraction process is inserted into a gasification chamber of a gas chromatographic sample inlet, a handle is pressed down to expose the extraction coating in high-temperature carrier gas, and the extract is desorbed and directly enters the gas chromatographic analysis.
At present, commercial solid-phase micro-extraction fibers are successfully applied to the determination of smelly substances in various environmental media. However, commercial solid phase microextraction fibers suffer from several disadvantages during the extraction process, such as instability at high temperatures, etc.
Metal Organic Frameworks (MOFs) are highly ordered porous materials with tunable pore structure and chemical function. Can be used for hydrogen storage, gas separation, catalysis, sensor technology, imaging and the like. In addition, MOFs have shown great potential applications in gas/vapor and liquid phase adsorption to remove harmful substances, etc., such as SCC, NCC, dyes, PPCPs, phenols, SOx, NOx, VOCs, etc. At present, the MOFs carbonized materials gradually draw more and more attention due to their higher specific surface area, adjustable pore structure, higher thermal stability and chemical stability.
Disclosure of Invention
Aiming at the technical problems, the invention provides a preparation method of a Zn-based MOFs carbonized coating, which is simple to prepare and low in cost; the invention solves another technical problem of providing an application of a carbonized Zn-based MOFs carbonized coating, which comprises the following specific steps: a method for analyzing aromatic smelly substances in a water body by using the Zn-based MOFs carbonized coating is established.
In order to solve the first technical problem, the technical scheme of the invention is as follows: a preparation method of a Zn-based MOFs carbonized coating comprises the following steps:
the method comprises the following steps: synthetic ZIF-8 coatings
1) Respectively carrying out ultrasonic treatment on the stainless steel 304 steel wire substrate for 30min by using 1M HCl, methanol and deionized water;
2) 2.868g of zinc nitrate hexahydrate and 0.72g of dimethylimidazole were weighed and dissolved in 216 ml of N-N-2-methylformamide (DMF);
3) transferring the solution and the matrix into a high-pressure reaction kettle, and heating to 140 ℃ for 24 hours; transferring the solution into a microwave reaction kettle, and carrying out microwave treatment for 3-5min by using microwaves with the frequency of 500-3000MHz and the power of 5-8 kW;
4) separating the crystal and the mother liquor to obtain a light yellow crystal material;
5) adding the obtained yellow crystal and a matrix into 20mL of chloroform solution for immersion washing; the temperature is kept between 25 and 28 ℃ during immersion cleaning;
6) rinsing with DMF solution;
7) drying the obtained material in a fume hood for 24h to obtain a ZIF-8 coating;
step two: carbonizing
1) Placing the synthesized ZIF-8 coating in a tube furnace;
2) setting a temperature-raising program to keep the temperature at 250 ℃ for 6h, and then raising the temperature at 700-1000 ℃ for 8h to obtain the carbonized MOFs coating.
Further, the carbonization temperature in the second step is respectively increased to 700 ℃, 800, 900 and 1000 ℃ and kept for 8 hours; the carbonization rate can be effectively improved by adopting medium and high temperature carbonization, and the medium and high temperature does not influence the carbonization effect reaching ZIF-8.
In order to solve the second technical problem, the technical solution of the present invention is: establishing an analysis method of the Zn-based MOFs carbonized coating on aromatic smelly substances in the water body.
Further, main factors influencing SPME extraction efficiency in the SPME coating extraction process are researched, including extraction time, extraction temperature, desorption time, desorption temperature and salt concentration, and L is established16(45) And (3) performing a positive crossing experiment, quantitatively analyzing the influence degree of each factor on an experiment result by adopting an Analysis of Variance (ANOVA) method, and determining the experiment factor with significant influence.
Further, determining optimized extraction conditions, comparing the extraction effects of the Zn-based MOFs carbonized coating and the commercial fiber coating, and considering the influence of humic acid on the extraction conditions.
Further, the Zn-based MOFs carbonized coating is respectively treated by acid, alkali, a polar solvent and a non-polar solvent, the chemical stability of the coating is researched, and thermogravimetric analysis is carried out on the material to research the thermal stability of the material.
Further, in the above scheme, the preparation method of the Zn-based MOFs carbonized coating comprises:
1) synthesizing a ZIF-8 coating by a hydrothermal method;
2) then placed in N2And roasting the obtained product in a tubular furnace under protection at 700 ℃, 800, 900 and 1000 ℃ to obtain the MOFs carbonized coating.
The invention has the beneficial effects that: the invention overcomes the defect that the traditional commercial fiber is unstable under the high-temperature condition, and establishes a method for analyzing aromatic smelly substances in water by using a Zn-based MOFs carbonized coating. In addition, the material of the invention has the advantages of simple preparation, convenient operation, low cost, and higher thermal stability and chemical stability. Therefore, the method is used for detecting aromatic smelly substances, and has the advantages of good reproducibility and wide linear range.
Detailed Description
Example 1:
preparing a carbonized ZIF-8 coating:
1) respectively carrying out ultrasonic treatment on the stainless steel 304 steel wire substrate for 30min by using 1M HCl, methanol and deionized water;
2) 2.868g of zinc nitrate hexahydrate and 0.72g of dimethylimidazole were weighed and dissolved in 216 ml of N-N-2-methylformamide (DMF), and the mixture was mixed by a glass rod;
3) transferring the solution and the matrix into a high-pressure reaction kettle, and heating to 140 ℃ for 24 hours; transferring the solution into a microwave reaction kettle, and carrying out microwave treatment for 3min by using microwaves with the frequency of 500MHz and the power of 5-8 kW;
4) separating the crystal and the mother liquor to obtain a light yellow crystal material;
5) adding the obtained yellow crystal and a matrix into 20mL of chloroform solution for immersion washing; the temperature is kept at 25 ℃ during immersion cleaning;
6) rinsing with DMF solution;
7) and (3) drying the obtained material in a fume hood for 24 hours to obtain the ZIF-8 coating.
8) Placing the obtained material in a tube furnace; in N2Under protection, setting a temperature raising program to keep at 250 ℃ for 6h, and raising the temperature to 700 ℃ for 8h to obtain the carbonized coating material.
Selecting an extraction temperature of 20 ℃, an extraction time of 20min, a desorption time of 0.5min, a desorption temperature of 200 ℃, a salt concentration of 0, puncturing a bottle cap with polytetrafluoroethylene during extraction, placing a part extending out of a coating layer into a water phase for extraction, drawing the extraction coating layer back into a stainless steel protective sheath after extraction is finished, immediately inserting the extraction coating layer into a GC-MS sample inlet, extending out of the coating layer, and carrying out thermal desorption at the sample inlet. Selecting C700Coating layer the analytical methods for 2,4, 6-trichlorophenoxy ether (TCA) and 2-methoxy-3-Isobutylpyrazine (IBMP) were established, with standard deviations (RSD) of 5.69% and 7.61% for the two contaminants under the established methods, respectively (n ═ 8). The linear correlation coefficient of 2 aromatic smelly pollutants measured by the method exceeds 0.990. The linear range is wide, spanning three orders of magnitude. The detection limit is as low as 0.05 mu g/L.
Example 2:
preparing a carbonized ZIF-8 coating:
1) respectively carrying out ultrasonic treatment on the stainless steel 304 steel wire substrate for 30min by using 1M HCl, methanol and deionized water;
2) 2.868g of zinc nitrate hexahydrate and 0.72g of dimethylimidazole were weighed and dissolved in 216 ml of N-N-2-methylformamide (DMF), and the mixture was mixed by a glass rod;
3) transferring the solution and the matrix into a high-pressure reaction kettle, and heating to 140 ℃ for 24 hours; transferring the solution into a microwave reaction kettle, and carrying out microwave treatment for 3min by using microwaves with the frequency of 500MHz and the power of 5-8 kW;
4) separating the crystal and the mother liquor to obtain a light yellow crystal material;
5) adding the obtained yellow crystal and a matrix into 20mL of chloroform solution for immersion washing; the temperature is kept at 25 ℃ during immersion cleaning;
6) rinsing with DMF solution;
7) and (3) drying the obtained material in a fume hood for 24 hours to obtain the ZIF-8 coating.
8) Placing the obtained material in a tube furnace; under the protection of N2, setting a temperature raising program to keep at 250 ℃ for 6h, and raising the temperature to 800 ℃ for 8h to obtain the carbonized coating material.
Selecting an extraction temperature of 30 ℃, an extraction time of 40min, a desorption time of 1min, a desorption temperature of 230 ℃, a salt concentration of 10%, puncturing a bottle cap with polytetrafluoroethylene during extraction, placing a part extending out of a coating layer in a water phase for extraction, drawing the extraction coating layer back into a stainless steel protective sheath after extraction is finished, immediately inserting the extraction coating layer into a GC-MS sample inlet, extending out of the coating layer, and carrying out thermal desorption at the sample inlet. Selecting C800The coating was analyzed for TCA and IBMP with standard deviations of 7.53% and 6.69% for the two contaminants (n-8) under the established method. The linear correlation coefficient of 2 aromatic smelly pollutants measured by the method exceeds 0.990. The linear range is wide, spanning four orders of magnitude. The detection limit is as low as 0.01 mu g/L.
Example 3:
preparing a carbonized ZIF-8 coating:
1) respectively carrying out ultrasonic treatment on the stainless steel 304 steel wire substrate for 30min by using 1M HCl, methanol and deionized water;
2) 2.868g of zinc nitrate hexahydrate and 0.72g of dimethylimidazole were weighed and dissolved in 216 ml of N-N-2-methylformamide (DMF), and the mixture was mixed by a glass rod;
3) transferring the solution and the matrix into a high-pressure reaction kettle, and heating to 140 ℃ for 24 hours; transferring the solution into a microwave reaction kettle, and carrying out microwave treatment for 3min by using microwaves with the frequency of 500MHz and the power of 5-8 kW;
4) separating the crystal and the mother liquor to obtain a light yellow crystal material;
5) adding the obtained yellow crystal and a matrix into 20mL of chloroform solution for immersion washing; the temperature is kept at 25 ℃ during immersion cleaning;
6) rinsing with DMF solution;
7) and (3) drying the obtained material in a fume hood for 24 hours to obtain the ZIF-8 coating.
8) Placing the obtained material in a tube furnace; in N2Under protection, setting a temperature raising program to maintain at 250 ℃ for 6h, and raising the temperature to 900 ℃ for 8h to obtain carbonizationAnd (3) coating materials.
Selecting an extraction temperature of 40 ℃, an extraction time of 60min, a desorption time of 2min, a desorption temperature of 250 ℃, a salt concentration of 20%, puncturing a bottle cap with polytetrafluoroethylene during extraction, placing a part extending out of a coating layer in a water phase for extraction, drawing the extraction coating layer back into a stainless steel protective sheath after extraction is finished, immediately inserting the extraction coating layer into a GC-MS sample inlet, extending out of the coating layer, and carrying out thermal desorption at the sample inlet. Selecting C900The coating was analyzed for TCA and IBMP with standard deviations RSD of 9.32% and 5.12% for the two contaminants (n ═ 8), respectively. The linear correlation coefficient of 2 aromatic smelly pollutants measured by the method exceeds 0.992. The linear range is wide, spanning four orders of magnitude. The detection limit is as low as 0.008 mu g/L.
Example 4
Preparing a carbonized ZIF-8 coating:
1) respectively carrying out ultrasonic treatment on the stainless steel 304 steel wire substrate for 30min by using 1M HCl, methanol and deionized water;
2) 2.868g of zinc nitrate hexahydrate and 0.72g of dimethylimidazole were weighed and dissolved in 216 ml of N-N-2-methylformamide (DMF), and the mixture was mixed by a glass rod;
3) transferring the solution and the matrix into a high-pressure reaction kettle, and heating to 140 ℃ for 24 hours; transferring the solution into a microwave reaction kettle, and carrying out microwave treatment for 3min by using microwaves with the frequency of 500MHz and the power of 5-8 kW;
4) separating the crystal and the mother liquor to obtain a light yellow crystal material;
5) adding the obtained yellow crystal and a matrix into 20mL of chloroform solution for immersion washing; the temperature is kept at 25 ℃ during immersion cleaning;
6) rinsing with DMF solution;
7) and (3) drying the obtained material in a fume hood for 24 hours to obtain the ZIF-8 coating.
8) Placing the obtained material in a tube furnace; in N2Under protection, setting a temperature raising program to keep at 250 ℃ for 6h, and raising the temperature to 1000 ℃ for 8h to obtain the carbonized coating material.
Selecting the extraction temperature of 50 ℃, the extraction time of 80min, the desorption time of 4min, the desorption temperature of 270 ℃, and the salt concentration of 37%And during extraction, a bottle cap with polytetrafluoroethylene is punctured, the part extending out of the coating is placed in a water phase for extraction, after extraction is finished, the extraction coating is drawn back into a stainless steel protective sheath, and is immediately inserted into a GC-MS sample inlet, the coating extends out, and thermal analysis is carried out at the sample inlet. Selecting C1000The coatings were analyzed for TCA and IBMP with standard deviations RSD of 3.62% and 4.97% for the two contaminants (n ═ 8), respectively. The linear correlation coefficient of 2 aromatic smelly pollutants measured by the method exceeds 0.993. The linear range is wide, spanning five orders of magnitude. The detection limit is as low as 0.005 mu g/L.
Comparative example 1
Preparation of ZIF-8 coating:
1) respectively carrying out ultrasonic treatment on the stainless steel 304 steel wire substrate for 30min by using 1M HCl, methanol and deionized water;
2) 2.868g of zinc nitrate hexahydrate and 0.72g of dimethylimidazole were weighed and dissolved in 216 ml of N-N-2-methylformamide (DMF), and the mixture was mixed by a glass rod;
3) transferring the solution and the matrix into a high-pressure reaction kettle, and heating to 140 ℃ for 24 hours; transferring the solution into a microwave reaction kettle, and carrying out microwave treatment for 3min by using microwaves with the frequency of 500MHz and the power of 5-8 kW;
4) separating the crystal and the mother liquor to obtain a light yellow crystal material;
5) adding the obtained yellow crystal and a matrix into 20mL of chloroform solution for immersion washing; the temperature is kept at 25 ℃ during immersion cleaning;
6) rinsing with DMF solution;
7) and (3) drying the obtained material in a fume hood for 24 hours to obtain the ZIF-8 coating.
The extraction temperature is 20 ℃, the extraction time is 20min, the desorption time is 0.5min, the desorption temperature is 200 ℃, the salt concentration is 0, a ZIF-8 coating is selected to establish an analysis method for TCA and IBMP, and the standard deviation of the two pollutants under the established method is 9.63% and 9.19% (n is 8) respectively. The linear correlation coefficient of 2 aromatic smelly pollutants measured by the method exceeds 0.98. The linear range is wide, spanning three orders of magnitude. The detection limit is as low as 0.5 mu g/L.
Comparative example 2
The extraction temperature is 20 ℃, the extraction time is 20min, the desorption time is 0.5min, the desorption temperature is 200 ℃ and the salt concentration is 0, a commercial fiber coating is selected to establish an analysis method for TCA and IBMP, and the standard deviation of the two pollutants under the established method is 10.36 percent and 11.29 percent respectively (n is 8). The linear correlation coefficient of 2 aromatic smelly pollutants measured by the method exceeds 0.95. The linear range is wide, spanning two orders of magnitude. The detection limit is as low as 0.1 mu g/L.
Finally, it should be noted that: the above examples are only used to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some of the technical features may be equivalently replaced; such modifications and substitutions do not substantially depart from the spirit and scope of the embodiments of the present invention.
Claims (1)
1. A method for detecting and analyzing aromatic smelly substances by using a carbonized MOF-8 coating is characterized by mainly comprising the following steps of:
s1 preparation of carbonized MOF-8 coating
S11 synthetic ZIF-8 coating
S111, respectively carrying out ultrasonic treatment on the stainless steel 304 steel wire substrate for 30min by using 1M HCl, methanol and deionized water;
s112, weighing 2.868g of zinc nitrate hexahydrate and 0.72g of dimethyl imidazole, and dissolving in 216 ml of N, N-Dimethylformamide (DMF);
s113, transferring the solution and the matrix into a high-pressure reaction kettle, and heating at 140 ℃ for 24 hours; then transferring the solution into a microwave reaction kettle, and carrying out microwave treatment for 3-5min by using microwaves with the frequency of 500-3000MHz and the power of 5-8 kW;
s114, separating crystals and mother liquor to obtain a light yellow crystal material;
s115, adding the obtained yellow crystal and a matrix into 20mL of chloroform solution for immersion cleaning, wherein the temperature is kept at 25-28 ℃ during immersion cleaning;
s116, rinsing with a DMF solution;
s117, drying the obtained material in a fume hood for 24 hours to obtain a ZIF-8 coating;
s12, ZIF-8 carbide coating
Putting the synthesized ZIF-8 coating in a tube furnace, setting a temperature rise program to keep the temperature at 250 ℃ for 6 hours, and then keeping the temperature at 700-1000 ℃ for 8 hours to obtain a carbonized ZIF-8 coating;
s2 detection and analysis of aromatic odorants using carbonized MOF-8 coating
S21, carrying out extraction experiments on the carbonized MOF-8 coating under the conditions of extraction temperature of 20-50 ℃, extraction time of 20-80min, desorption time of 0.5-4min, desorption temperature of 200-270 ℃ and salt concentration of 0-37%;
s22, puncturing a bottle cap with polytetrafluoroethylene during extraction, and placing the part of the extended carbonized MOF-8 coating in a water phase for extraction; after extraction is finished, the carbonized MOF-8 coating is drawn back to a stainless steel protective sheath, and is immediately inserted into a GC-MS sample inlet for thermal analysis;
s23, selecting the carbonized MOF-8 coating to establish an analysis method for TCA and IBMP, and obtaining the standard deviation RSD, the linear correlation coefficient, the linear range width and the minimum detection limit value of the aromatic smelling substances.
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