CN115490869A - Method for rapidly synthesizing metal organic framework material on paper chip assisted by circular furnace - Google Patents
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Abstract
The invention discloses a method for rapidly synthesizing a metal organic framework material on a paper chip assisted by a ring furnace. The paper chip with a special structure is designed to be placed on a ring furnace, a metal precursor solution and an organic ligand precursor solution are dripped into a sample injection area in the center of the paper chip, liquid is diffused to a heating area of the ring furnace due to the siphoning effect of the paper chip, the liquid is rapidly changed into steam in a proper temperature environment of the area, and after the liquid is rapidly cooled, a metal organic framework material is deposited in the heating area on the surface of the paper chip. The method realizes the synthesis of the metal organic frame material in a specific area on the paper chip, the synthesis can be completed within 1 hour, and the cost is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of material synthesis methods, and particularly relates to a method for rapidly synthesizing a metal organic framework material on a paper chip with the assistance of a circular furnace.
Background
The metal organic framework Materials (MOFs) are crystal materials with periodic grid structures formed by self-assembling and connecting metal ions and organic ligands, have the characteristics of large specific surface area, large porosity, diversified structures and metal unsaturated coordination, and have great development potential and attractive development prospects in the fields of gas adsorption, luminescence, catalysis, sensing detection and the like. In recent years, due to the demand for the device formation of MOFs, researchers have loaded MOFs on a microchip to realize the sensing application thereof. Ameloot et al first reported a vapor-based MOFs deposition strategy that employs a combination of atomic layer deposition and vapor-assisted conversion to effect the conversion of metal oxides on a microchip to crystalline MOFs. The method has high deposition efficiency, uniformity and controllable thickness, and can complete the deposition of MOFs in an extremely tiny size.
To further develop the applications of MOFs, supporting rigid structured MOFs on flexible substrates can impart new properties to the MOFs. The paper chip has the characteristics of low cost, simplicity, easiness in operation and throw-away property, and is widely applied to the fields of biological analysis, medical diagnosis, environmental monitoring and the like as a flexible substrate. Therefore, the MOFs loaded on the paper chip has certain application prospect. However, at present, the MOFs are loaded on the paper substrate by a direct growth method, a secondary growth method and a liquid phase epitaxy method, which generally take a long time, and contact with a solution for a long time may damage a paper fiber structure, and especially, the MOFs are difficult to assemble on a specific position of a substrate with a tiny size by a solution-based synthesis method.
The ring furnace technology is firstly proposed by austria analytical chemist weizi in 1954, and is applied as a microanalysis method in the early stage, a sample to be detected which is dripped into the center of a paper substrate is continuously and radially diffused under the driving of flushing liquid, when the sample reaches a heating ring of the ring furnace, the flushing liquid is rapidly evaporated under the heating, and an object to be detected is concentrated in the heating ring of the ring furnace to form a ring for detection.
Disclosure of Invention
The invention aims to overcome the problems of the paper substrate MOFs loading method, provides a method for synthesizing MOFs on a paper chip in situ by using a ring furnace, and realizes low-cost, high-efficiency and rapid in-situ synthesis of MOFs in a specific area of the paper chip.
Aiming at the purposes, the technical scheme adopted by the invention is as follows: spreading a paper chip on the ring furnace, wherein the paper chip consists of a sample injection area at the center, 2-24 MOFs synthesis areas, a liquid flow channel connecting the sample injection area and the MOFs synthesis areas, and an outermost ring of waste liquid area, the diameter of the paper chip is not less than the outer diameter of a heating ring of the ring furnace, the diameter of the sample injection area is less than the inner diameter of the heating ring of the ring furnace, and the diameter of the MOFs synthesis area is not more than the ring width of the heating ring of the ring furnace; sealing an MOFs synthesis area of the paper chip by using a polyethylene film, adjusting a circular furnace to a reaction temperature, sequentially dripping a metal precursor solution and an organic ligand precursor solution into a sample injection area of the paper chip for 10-60 seconds respectively, adding an ice bag on the polyethylene film for cooling, after reacting for 10-60 minutes, pushing the paper chip downwards to enable a waste liquid area to be located on a heating ring of the circular furnace, cleaning the MOFs synthesis area by using a cleaning liquid, cleaning unbound sites in the waste liquid area of the paper chip, and finally performing vacuum drying.
The paper chip is cut by a paper substrate, and the paper substrate is preferably Whatman No. 1 filter paper or Whatman No. 3 filter paper.
The invention further preferably performs carboxymethylation treatment on the paper chip, and the specific treatment method comprises the following steps: soaking the paper chip in an aqueous solution containing 1-1.5 mol/L of sodium chloroacetate and 4-6 wt.% of NaOH for 40-60 minutes, taking out, cleaning and air-drying.
In the above synthesis method, the number of the MOFs synthesis regions is preferably 8 to 16.
The metal precursor solution is any one of an N, N-dimethylformamide solution of copper nitrate, an ethanol-water solution of copper acetate, an N, N-dimethylformamide solution of zinc nitrate, an N, N-dimethylformamide solution of cobalt nitrate, etc., the organic ligand precursor solution is any one of an N, N-dimethylformamide-methanol solution of 2, 5-dihydroxyterephthalic acid, an N, N-dimethylformamide-nitric acid solution of 1,3, 5-tris (4-carboxyphenyl) benzene, an N, N-dimethylformamide solution of 1,3, 5-benzenetricarboxylic acid, an N, N-dimethylformamide solution of 1, 4-terephthalic acid, etc., and the rinse is N, N-dimethylformamide or a mixed solution of N, N-dimethylformamide and ethanol or a mixed solution of N, N-dimethylformamide, ethanol, and water. The reaction temperature is 80-110 ℃. In addition, the invention can also select corresponding metal precursor and organic ligand according to the metal organic framework material to be synthesized, and the reaction temperature can also be adjusted according to the metal organic framework material to be synthesized.
In the above synthesis method, it is preferable to sequentially drop the metal precursor solution and the organic ligand precursor solution into the sample injection region of the paper chip at a rate of 200 to 800. Mu.L/min using a flow syringe pump.
In the synthesis method, the loading capacity of the metal organic framework material in the MOFs synthesis area is 0.1-1 mg/cm 3 。
The invention has the following beneficial effects:
the invention can realize the in-situ synthesis of the metal organic framework material in the fixed-point area of the paper chip by utilizing the functions of heating, enriching and washing in the edge area of the ring furnace. The paper chip with a special structure is designed to be placed on a ring furnace, a metal precursor solution and an organic ligand precursor solution are dripped into a sample injection area in the center of the paper chip, liquid is diffused to a heating area of the ring furnace due to the siphoning effect of the paper chip, the liquid is rapidly changed into steam in a proper temperature environment of the area, and after the liquid is rapidly cooled, a metal organic framework material is deposited in the heating area on the surface of the paper chip. The method realizes the synthesis of the metal organic framework material in a specific area on the paper chip, has controllable synthesis amount, can complete the synthesis within 1 hour, greatly reduces the cost, has simple operation and strong universality, and is suitable for synthesizing different types of metal organic framework materials on the paper chip.
Drawings
Fig. 1 is a schematic structural diagram of a paper chip in the embodiment.
FIG. 2 is a schematic diagram of the method for rapidly synthesizing the metal organic frame material on the paper chip assisted by the ring furnace in the embodiment.
FIG. 3 is a scanning electron microscope image of the Cu-MOF-74@ paper chip prepared in example 1.
FIG. 4 is an X-ray diffraction pattern of Cu-MOF-74, paper chip and Cu-MOF-74@ paper chip prepared in example 1.
FIG. 5 is an infrared spectrum of Cu-MOF-74, paper chip and Cu-MOF-74@ paper chip prepared in example 1.
FIG. 6 is an X-ray photoelectron spectrum of a Cu-MOF-74@ paper chip prepared in example 1.
FIG. 7 is a scanning electron microscope image of the Cu-BTB @ paper chip prepared in example 2.
FIG. 8 is a scanning electron microscope image of the Cu-BTC @ paper chip prepared in example 3.
Detailed Description
The present invention will be described in further detail with reference to the drawings and examples, but the scope of the present invention is not limited to these examples.
The annular furnace adopted in the following embodiment is a single-hole metal annular furnace, the outer part is a heat preservation iron box, the heating body in the annular furnace is a copper cylinder with the outer diameter of 60mm, the inner diameter of 22mm and the height of 35mm, the cylindrical surface of the cylinder is wound with an electric heating wire, asbestos and mica sheets are wrapped around the cylinder for heat preservation, the temperature of the heating body is controlled by a voltage regulating transformer, and the heating range is 0-200 ℃.
The structure of the paper chip in the following embodiment is shown in fig. 1, and is formed by cutting Whatman No. 1 filter paper, wherein the paper chip consists of a sample injection area at the center, 12 MOFs synthesis areas, a liquid flow channel connecting the sample injection area and the MOFs synthesis areas, and an outermost ring of waste liquid area, the diameter of the paper chip is 80mm, the diameter of the sample injection area is 10mm, the diameter of the MOFs synthesis areas is 6mm, and the distance between the centers of the two MOFs synthesis areas on the same straight line is 60mm; and soaking the paper chip in an aqueous solution containing 1mol/L of sodium chloroacetate and 5wt.% of NaOH for 1h, taking out, cleaning and air-drying to obtain the carboxymethylated paper chip.
Example 1
As shown in fig. 2, the paper chip subjected to carboxymethylation is laid on a circular furnace, the MOFs synthesis area of the paper chip is sealed by a polyethylene film, and the circular furnace is adjusted to 100 ℃; weighing 0.0299g of copper nitrate trihydrate to be dissolved in 10mL of N, N-dimethylformamide to obtain a 15mmol/L copper nitrate solution; weighing 0.0731g of 2, 5-dihydroxyterephthalic acid, and dissolving in 10mL of a mixed solution of N, N-dimethylformamide and methanol in a volume ratio of 9; dropping a copper nitrate solution for 30s in a sample injection area at the center of the paper chip at a speed of 400 mu L/min by using a flow injection pump, then dropping a 2, 5-dihydroxy terephthalic acid solution for 30s, adding an ice bag on a polyethylene film for cooling, after the reaction for 30min, pushing the paper chip downwards to enable a waste liquid area to be positioned on a heating ring of a circular furnace, cleaning an MOFs synthesis area by using N, N-dimethylformamide, cleaning unbound sites in the waste liquid area at the outermost circle of the paper chip, and finally drying in vacuum at 50 ℃ to obtain the Cu-MOF-74@ paper chip.
As can be seen from figure 3, the Cu-MOF-74 on the paper chip is in a unidirectional flower bunch shape, and the Cu-MOF-74 is covalently bonded on the surface of the paper base along fibers. As can be seen from fig. 4, the X-ray diffraction pattern of Cu-MOF-74 on the paper chip has both the characteristic diffraction peak of the paper chip at 2 θ =24.5 ° and the characteristic diffraction peaks of Cu-MOF-74 at 2 θ =6.7 ° and 11.8 °, corresponding to the (210) and (300) crystal planes, respectively. As can be seen from FIG. 5, the infrared spectrum of Cu-MOF-74 on the paper chip has Cu-MOF-74 located at 1558cm -1 、1430cm -1 、1250cm -1 、1191cm -1 、1043cm -1 、598cm -1 The absorption peak of (A), and the paper chip is 2870cm -1 、3325cm -1 the-OH stretching vibration peak at (C). As can be seen from FIG. 6, the presence of C, O and Cu elements is also clearly shown in the broad scanning spectrum of X-ray photoelectron spectroscopy of Cu-MOF-74 on a paper chip, wherein the characteristic peaks of Cu element appear mainly at the binding energies 954.9 and 935.0, corresponding to Cu 2p 1/2 、Cu 2p 3/2 。
Example 2
As shown in fig. 2, the paper chip subjected to carboxymethylation is flatly laid on a circular furnace, the MOFs synthesis area of the paper chip is sealed by a polyethylene film, and the circular furnace is adjusted to 100 ℃; 0.0241g of copper nitrate trihydrate is weighed and dissolved in 10mL of N, N-dimethylformamide to obtain 10mmol/L copper nitrate solution; 0.0246g of 1,3, 5-tris (4-carboxyphenyl) benzene is weighed and dissolved in 10mL of a mixed solution of N, N-dimethylformamide and nitric acid in a volume ratio of 3; dropping a copper nitrate solution for 30s in a sample injection area at the center of the paper chip at a speed of 400 mu L/min by using a flow injection pump, then dropping a 1,3, 5-tris (4-carboxyphenyl) benzene solution for 30s, adding an ice bag on a polyethylene film for cooling, after reacting for 30min, pushing the paper chip downwards to enable a waste liquid area to be positioned on a heating ring of a circular furnace, cleaning an MOFs synthesis area by using N, N-dimethylformamide, cleaning an unbonded site in the waste liquid area at the outermost circle of the paper chip, and finally drying in vacuum at 50 ℃ to obtain the Cu-BTB @ paper chip. As can be seen from FIG. 7, the Cu-BTB on the paper chip is hexahedron-shaped, and the Cu-BTB is bonded on the surface of the paper chip along the fiber covalent bond.
Example 3
As shown in fig. 2, the paper chip subjected to carboxymethylation is laid on a circular furnace, the MOFs synthesis area of the paper chip is sealed by a polyethylene film, and the circular furnace is adjusted to 100 ℃; weighing 0.0241g of copper acetate, dissolving in 10mL of mixed solution of ethanol and water in a volume ratio of 1; weighing 0.0630g of 1,3, 5-benzenetricarboxylic acid to dissolve in 5mL of N, N-dimethylformamide to obtain a 30 mmol/L1, 3, 5-benzenetricarboxylic acid solution; dropping a copper acetate solution for 30s in a sample injection area at the center of the paper chip at a speed of 400 mu L/min by using a flow injection pump, then dropping a 1,3, 5-benzenetricarboxylic acid solution for 30s, adding an ice bag on a polyethylene film for cooling, after reacting for 30min, pushing the paper chip downwards to enable a waste liquid area to be positioned on a circular furnace heating ring, cleaning an MOFs synthesis area by using a mixed solution of N, N-dimethylformamide, ethanol and water in a volume ratio of 1. As can be seen from FIG. 5, the Cu-BTC on the paper chip is in a regular octahedron shape, and the Cu-BTC is bonded to the surface of the paper base along the fiber covalent bond.
Example 4
As shown in fig. 2, the paper chip subjected to carboxymethylation is laid on a circular furnace, the MOFs synthesis area of the paper chip is sealed by a polyethylene film, and the circular furnace is adjusted to 110 ℃; 0.0297g of zinc nitrate hexahydrate is weighed and dissolved in 10mL of N, N-dimethylformamide to obtain 10mmol/L of copper nitrate solution; 0.0630g of 1, 4-terephthalic acid is weighed and dissolved in 10mL of N, N-dimethylformamide to obtain a 1, 4-terephthalic acid solution with the concentration of 5 mmol/L; dropping a zinc nitrate solution for 30s in a sample injection area at the center of a paper chip at a speed of 400 mu L/min by using a flow injection pump, then dropping a 1, 4-terephthalic acid solution for 30s, adding an ice bag on a polyethylene film for cooling, after the mixture reacts for 30min, pushing the paper chip downwards to enable a waste liquid area to be positioned on a heating ring of a circular furnace, cleaning an MOFs synthesis area by using a mixed solution of N, N-dimethylformamide and ethanol with a volume ratio of 1.
Claims (9)
1. A method for rapidly synthesizing a metal organic framework material on a paper chip assisted by a circular furnace is characterized by comprising the following steps: spreading a paper chip on the ring furnace, wherein the paper chip consists of a sample injection area at the center, 2-24 MOFs synthesis areas, a liquid flow channel connecting the sample injection area and the MOFs synthesis areas, and an outermost ring of waste liquid area, the diameter of the paper chip is not less than the outer diameter of a heating ring of the ring furnace, the diameter of the sample injection area is less than the inner diameter of the heating ring of the ring furnace, and the diameter of the MOFs synthesis area is not more than the ring width of the heating ring of the ring furnace; sealing an MOFs synthesis area of the paper chip by using a polyethylene film, adjusting a ring furnace to a reaction temperature, sequentially dropwise adding a metal precursor solution and an organic ligand precursor solution into a sample injection area of the paper chip for 10-60 seconds respectively, adding an ice bag on the polyethylene film to cool, reacting for 10-60 minutes, pushing the paper chip downwards to enable a waste liquid area to be located on a heating ring of the ring furnace, cleaning the MOFs synthesis area by using a cleaning liquid, cleaning an unbonded site in the waste liquid area of the paper chip, and finally performing vacuum drying.
2. The method for rapidly synthesizing the metal organic framework material on the paper chip assisted by the circular furnace as claimed in claim 1 is characterized in that: the paper chip is formed by cutting a paper substrate, and carboxymethylation treatment is carried out on the paper chip, and the specific treatment method comprises the following steps: soaking the paper chip in an aqueous solution containing 1-1.5 mol/L of sodium chloroacetate and 4-6 wt.% of NaOH for 40-60 minutes, taking out, cleaning and air-drying.
3. The method for rapidly synthesizing the metal organic framework material on the paper chip assisted by the circular furnace as claimed in claim 2, characterized in that: the paper substrate is Whatman No. 1 filter paper or Whatman No. 3 filter paper.
4. The method for rapidly synthesizing the metal organic framework material on the paper chip assisted by the circular furnace as claimed in claim 1 is characterized in that: the number of the MOFs synthetic regions is 8-16.
5. The method for rapidly synthesizing the metal organic framework material on the paper chip assisted by the ring furnace according to claim 1, is characterized in that: the metal precursor solution is any one of an N, N-dimethylformamide solution of copper nitrate, an ethanol-water solution of copper acetate, an N, N-dimethylformamide solution of zinc nitrate and an N, N-dimethylformamide solution of cobalt nitrate, and the organic ligand precursor solution is any one of an N, N-dimethylformamide-methanol solution of 2, 5-dihydroxyterephthalic acid, an N, N-dimethylformamide-nitric acid solution of 1,3, 5-tris (4-carboxyphenyl) benzene, an N, N-dimethylformamide solution of 1,3, 5-benzenetricarboxylic acid and an N, N-dimethylformamide solution of 1, 4-terephthalic acid.
6. The method for rapidly synthesizing the metal organic framework material on the paper chip assisted by the ring furnace as claimed in claim 5, wherein the method comprises the following steps: the flushing fluid is N, N-dimethylformamide or a mixed solution of N, N-dimethylformamide and ethanol or a mixed solution of N, N-dimethylformamide, ethanol and water.
7. The method for rapidly synthesizing the metal organic framework material on the paper chip assisted by the ring furnace as claimed in claim 5, wherein the method comprises the following steps: the reaction temperature is 80-110 ℃.
8. The method for rapidly synthesizing the metal organic framework material on the paper chip assisted by the ring furnace according to claim 1, is characterized in that: and (3) sequentially dripping a metal precursor solution and an organic ligand precursor solution into the sample injection area of the paper chip at the speed of 200-800 mu L/min by using a flow injection pump.
9. The method for rapidly synthesizing the metal organic framework material on the paper chip assisted by the ring furnace according to claim 1, is characterized in that: the load capacity of the metal organic framework material in the MOFs synthetic region is 0.1-1 mg/cm 3 。
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