CN113861434A - Novel magnesium-based MOF material and solution processing method of MOF material - Google Patents
Novel magnesium-based MOF material and solution processing method of MOF material Download PDFInfo
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Abstract
A novel magnesium-based MOF material with a chemical formula of Mg2(TCPE)(DMA)(CH3OH)(H2O). The synthesis method comprises the following steps: the organic ligand 1,1,2, 2-tetra (4-carboxylphenyl) ethylene (H)4TCPE) and magnesium nitrate hexahydrate (Mg (NO)3)2‧6H2O) to N, N-Dimethylacetamide (DMA), methanol (CH)3OH) and water (H)2O) in a mixed solvent; and (3) reacting the mixed solution in a solvothermal mode to obtain colorless blocky single crystals, and washing and drying to obtain the magnesium-based MOF. A method of solution processing a MOF material: using water as componentPowders, a series of metal-organic framework materials as dispersoids; the dispersion system can be used for solution processing, realizes different applications of crystalline materials, can be processed into water-based fluorescent ink, and is used for the field of fluorescence anti-counterfeiting. The novel magnesium-based MOF solid shows good fluorescence property, so that the material can be prepared into aqueous fluorescent ink. The solution processing method of the MOF material is simple to operate, has excellent effect and can be suitable for various magnesium-based metal-organic framework materials.
Description
The technical field is as follows:
the invention relates to the field of materials, in particular to a novel magnesium-based MOF material and a solution processing method of the MOF material.
(II) background technology:
Metal-Organic Framework (MOF) materials are a new type of inorganic-Organic hybrid porous materials obtained by coordination self-assembly of Metal ions or clusters and Organic ligands, have rich pore channel structures and high porosity and specific surface area, have wide application prospects in catalysis, adsorption separation, and numerous fields of optics, electrics, magnetics and the like, and have become a hot research direction of chemistry and materials science. However, poor solubility/dispersibility of MOF materials makes them difficult to solution process.
In order to further expand the application range of MOF materials and fully develop their functional advantages, it is necessary to solve the problem of poor solubility/dispersibility of MOF materials. In general, nano-scale particles enable simple and fast dispersion. Therefore, based on the characteristic of poor stability of coordination bonds, the external stimulus is utilized to promote the dissociation of the framework part, so that highly dispersed nano particles can be obtained, and the method has important significance for improving the solubility/dispersibility of the MOF material.
(III) the invention content:
the invention aims to provide a novel magnesium-based MOF material and a solution processing method of the MOF material.
The technical scheme of the invention is as follows: novel magnesium-based MOF material, characterized in that it has the chemical formula Mg2(TCPE)(DMA)(CH3OH)(H2O), wherein TCPE4-Is 1,1,2, 2-tetra (4-carboxystyrene) ethylene quadrivalent anion, and DMA is N, N-dimethylacetamide.
The crystal of the novel magnesium-based MOF material belongs to an orthorhombic system, a Cmce space group and unit cell parameters are as follows:
α ═ β ═ γ ═ 90 °; the mg (ii) ions in the framework adopt a hexacoordinated mode, comprising four carboxyl O atoms, one O atom from water and one O atom from methanol or DMA, with adjacent mg (ii) ions linked into a tetranuclear Secondary Building Unit (SBU).
The synthesis method of the novel magnesium-based MOF material is characterized by comprising the following steps:
(1) the organic ligand 1,1,2, 2-tetra (4-carboxylphenyl) ethylene (H)4TCPE) and magnesium nitrate hexahydrate (Mg (NO)3)2·6H2O) to N, N-Dimethylacetamide (DMA), methanol (CH)3OH) and water (H)2O) in a mixed solvent;
(2) carrying out solvothermal reaction on the mixed solution obtained in the step (1) to obtain colorless blocky single crystals, and washing and drying to obtain magnesium-based MOF (metal organic framework), namely Mg)2(TCPE)(DMA)(CH3OH)(H2O)。
The molar ratio of the 1,1,2, 2-tetra (4-carboxystyrene) ethylene to the magnesium nitrate hexahydrate is 1: 1.
The volume ratio of the N, N-dimethylacetamide to the methanol to the water is 2:2: 1.
The solvothermal condition is that the reaction is carried out for 4-6 days at the constant temperature of 75-85 ℃, and the reaction is naturally cooled to the room temperature.
A method of solution processing a MOF material comprising the steps of:
(1) water is used as a dispersant, and a metal-organic framework material is used as a dispersoid; adding 0.002g-0.01g of MOF material into each 10-50mL of ultrapure water;
(2) and (3) performing ultrasonic treatment in an ultrasonic instrument until the solid is completely dispersed, wherein the solution is clear and transparent, has a Tyndall effect under the irradiation of laser, and is dispersed into particles of 1-200 nm.
The metal-organic framework material employs a novel magnesium-based MOF, i.e., Mg2(TCPE)(DMA)(CH3OH)(H2O); or the following magnesium-based MOFs materials are adopted:
the water-based anti-counterfeiting fluorescent ink containing the novel magnesium-based MOF material is characterized in that 100mL of ink contains 0.01-3.0g of novel magnesium-based MOF, 10-20mL of ethanol, 8-12mL of glycerol, 0.05-0.15g of OP-10 emulsifier, 0.05-0.15g of ultraviolet absorbent UV-320, 0.25-0.75g of phenol and the balance of water.
The preparation method of the aqueous anti-counterfeiting fluorescent ink containing the novel magnesium-based MOF material is characterized by comprising the following steps:
(1) 0.01-3.0g of novel magnesium-based MOF is required to be weighed and taken as a dye to be dispersed in 40-50mL of water;
(2) adding 10-20mL of ethanol, 8-12mL of glycerol, 0.05-0.15g of OP-10 emulsifier, 0.05-0.15g of ultraviolet absorbent UV-320 and 0.25-0.75g of phenol;
(3) and finally adding water to 100mL to obtain 100mL of the aqueous anti-counterfeiting fluorescent ink for the ink-jet printer.
The invention has the advantages that: 1. the novel magnesium-based MOF of the invention, namely Mg2(TCPE)(DMA)(CH3OH)(H2O), the magnesium-based MOF solid shows good fluorescence performance, the magnesium-based MOF can be uniformly dispersed by using the solution processing method, and a dispersion system has a Tyndall effect and no fluorescence; however, since the solid precipitated from the dispersion is fluorescent, the material can be prepared into an aqueous fluorescent ink. 2. The invention discloses a solution processing method of a Metal Organic Framework (MOF) material, namely a method for promoting the partial dissociation of the MOF material by utilizing external stimulation based on the characteristic of poor coordinate bond stability to obtain highly dispersed nano particles, thereby realizing the simple and rapid MOF materialDispersion of (2). The method has important significance for overcoming the problems that the MOF material is poor in solubility or dispersibility and difficult to process solution. Currently, many applications require the use of nano-sized crystalline materials to be achieved, and thus, increasing the solubility/dispersibility of MOF materials is critical to advance the practical process of MOF materials. 3. The solution processing method of the MOF material is very suitable for solution processing, and the method is favorable for expanding the application field of crystalline MOF materials, such as processing into aqueous fluorescent anti-counterfeiting ink, preparing MOF thin films, 3D printing of MOF materials and the like. 4. The solution processing method of the MOF material is simple to operate, has excellent effect and can be suitable for various magnesium-based metal-organic framework materials.
(IV) description of the drawings:
FIG. 1 is a crystal structure diagram of a novel magnesium-based MOF material according to the present invention.
FIGS. 2-1 and 2-2 are examples of the application of the solution processing method for the novel magnesium-based MOF material of the invention: the effect graph of the printed content under visible light and ultraviolet light is obtained by using the novel magnesium-based MOF as the fluorescent dye to prepare the fluorescent anti-counterfeiting ink for the ink-jet printer.
FIG. 3 is a powder X-ray diffraction pattern of precipitated solids from three magnesium-based MOFs and their aqueous dispersions.
(V) specific embodiment:
example (b): a novel magnesium-based MOF material (shown in figure 1) is characterized in that the chemical formula of the material is Mg2(TCPE)(DMA)(CH3OH)(H2O), wherein TCPE4-Is 1,1,2, 2-tetra (4-carboxystyrene) ethylene quadrivalent anion, and DMA is N, N-dimethylacetamide.
The crystal of the novel magnesium-based MOF material belongs to an orthorhombic system, a Pbcn space group, and unit cell parameters are as follows:
α ═ β ═ γ ═ 90 °; the Mg (II) ion in the framework adopts a hexacoordinate mode, comprising four carboxyl O atoms, one O atom from water and one O atom from methanol or DMAThe adjacent Mg (II) ions are linked to form a tetranuclear Secondary Building Unit (SBU).
The synthesis method of the novel magnesium-based MOF material is characterized by comprising the following steps:
(1) the organic ligand 1,1,2, 2-tetra (4-carboxylphenyl) ethylene (H)4TCPE) and magnesium nitrate hexahydrate (Mg (NO)3)2·6H2O) to N, N-Dimethylacetamide (DMA), methanol (CH)3OH) and water (H)2O) in a mixed solvent;
(2) carrying out solvothermal reaction on the mixed solution obtained in the step (1) to obtain colorless blocky single crystals, and washing and drying to obtain magnesium-based MOF (metal organic framework), namely Mg)2(TCPE)(DMA)(CH3OH)(H2O)。
The molar ratio of the 1,1,2, 2-tetra (4-carboxystyrene) ethylene to the magnesium nitrate hexahydrate is 1: 1.
The volume ratio of the N, N-dimethylacetamide to the methanol to the water is 2:2: 1.
The solvothermal condition is that the reaction is carried out for 5 days at the constant temperature of 80 ℃ and the reaction is naturally cooled to the room temperature.
A method of solution processing a MOF material comprising the steps of:
(1) water is used as a dispersant, and a metal-organic framework material is used as a dispersoid; 0.006g of MOF material per 30mL of ultrapure water;
(2) and (3) performing ultrasonic treatment in an ultrasonic instrument until the solid is completely dispersed, wherein the solution is clear and transparent, has a Tyndall effect under the irradiation of laser, and is dispersed into particles of 1-200 nm.
The metal-organic framework material employs a novel magnesium-based MOF, i.e.
Mg2(TCPE)(DMA)(CH3OH)(H2O)；
Or the following magnesium-based MOFs materials are adopted:
the water-based anti-counterfeiting fluorescent ink containing the novel magnesium-based MOF material is characterized in that 100mL of the ink contains 1.5g of the novel magnesium-based MOF, 16mL of ethanol, 10mL of glycerol, 0.1g of OP-10 emulsifier, 0.1g of ultraviolet absorbent UV-320, 0.5g of phenol and the balance of water.
The preparation method of the aqueous anti-counterfeiting fluorescent ink containing the novel magnesium-based MOF material is characterized by comprising the following steps:
(1) 1.5g of novel magnesium-based MOF is required to be weighed and taken as a dye to be dispersed in 45mL of water;
(2) adding 16mL of ethanol, 10mL of glycerol, 0.1g of OP-10 emulsifier, 0.1g of ultraviolet absorbent UV-320 and 0.5g of phenol;
(3) and finally adding water to 100mL to obtain 100mL of the aqueous anti-counterfeiting fluorescent ink for the ink-jet printer.
The invention carries out Tyndall effect detection on the dispersed sample and confirms the dispersion state; and confirming the crystalline state of the dispersible magnesium-based MOF material after being dispersed and separated out again; in addition, the fluorescence state of the dispersible magnesium-based MOF material before, after, and after precipitation was confirmed.
The magnesium-based MOF materials in the invention can be dispersed in water, and the re-precipitated sample still has good crystallinity, but is different from the original structure, and can be confirmed from powder X-ray diffraction Pattern (PXRD). Meanwhile, the fluorescence properties of the magnesium-based MOF material before and after dispersion and re-precipitated samples are different, and the fluorescence properties can be obviously distinguished under an ultraviolet lamp of 365nm, and the characteristics are shown in the following table:
Claims (10)
1. a novel magnesium-based MOF material is characterized in that the chemical formula is Mg2(TCPE)(DMA)(CH3OH)(H2O), wherein TCPE4-Is 1,1,2, 2-tetrakis (4-carboxy)Benzene) ethylene tetravalent anion, DMA is N, N-dimethylacetamide.
2. A novel magnesium-based MOF material according to claim 1, wherein the crystals of said novel magnesium-based MOF material belong to the orthorhombic system, Cmce space group, unit cell parameters:
α ═ β ═ γ ═ 90 °; the mg (ii) ions in the framework adopt a hexacoordinated mode, comprising four carboxyl O atoms, one O atom from water and one O atom from methanol or DMA, with adjacent mg (ii) ions linked into a tetranuclear Secondary Building Unit (SBU).
3. A method for synthesizing a novel magnesium-based MOF material according to claim 1, comprising the following steps:
(1) the organic ligand 1,1,2, 2-tetra (4-carboxylphenyl) ethylene (H)4TCPE) and magnesium nitrate hexahydrate (Mg (NO)3)2·6H2O) to N, N-Dimethylacetamide (DMA), methanol (CH)3OH) and water (H)2O) in a mixed solvent;
(2) carrying out solvothermal reaction on the mixed solution obtained in the step (1) to obtain colorless blocky single crystals, and washing and drying to obtain magnesium-based MOF (metal organic framework), namely Mg)2(TCPE)(DMA)(CH3OH)(H2O)。
4. The method of synthesizing a novel magnesium-based MOF material according to claim 3, wherein the molar ratio of 1,1,2, 2-tetrakis (4-carboxystyrene) ethylene to magnesium nitrate hexahydrate is 1: 1.
5. The method for synthesizing the novel magnesium-based MOF material according to claim 3, wherein the volume ratio of the N, N-dimethylacetamide to the methanol to the water is 2:2: 1.
6. The synthesis method of the novel magnesium-based MOF material according to claim 3, wherein the solvothermal condition is that the reaction is carried out at a constant temperature of 75-85 ℃ for 4-6 days, and the reaction is naturally cooled to room temperature.
7. A method of solution processing a MOF material comprising the steps of:
(1) water is used as a dispersant, and a metal-organic framework material is used as a dispersoid; adding 0.002g-0.01g of MOF material into each 10-50mL of ultrapure water;
(2) and (3) performing ultrasonic treatment in an ultrasonic instrument until the solid is completely dispersed, wherein the solution is clear and transparent, has a Tyndall effect under the irradiation of laser, and is dispersed into particles of 1-200 nm.
8. A method of solution processing of MOF material according to claim 7, characterized in that the metal-organic framework material uses new magnesium-based MOFs, Mg2(TCPE)(DMA)(CH3OH)(H2O)；
Or the following magnesium-based MOFs materials are adopted:
9. an aqueous anti-counterfeiting fluorescent ink containing the novel magnesium-based MOF material as claimed in claim 1, wherein 100mL of the ink contains 0.01-3.0g of the novel magnesium-based MOF, 10-20mL of ethanol, 8-12mL of glycerol, 0.05-0.15g of OP-10 emulsifier, 0.05-0.15g of ultraviolet absorbent UV-320, 0.25-0.75g of phenol, and the balance of water.
10. A method for preparing the aqueous anti-counterfeiting fluorescent ink containing the novel magnesium-based MOF material, according to claim 9, which is characterized by comprising the following steps:
(1) 0.01-3.0g of novel magnesium-based MOF is required to be weighed and taken as a dye to be dispersed in 40-50mL of water;
(2) adding 10-20mL of ethanol, 8-12mL of glycerol, 0.05-0.15g of OP-10 emulsifier, 0.05-0.15g of ultraviolet absorbent UV-320 and 0.25-0.75g of phenol;
(3) and finally adding water to 100mL to obtain 100mL of the aqueous anti-counterfeiting fluorescent ink for the ink-jet printer.
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| CN115449083A (en) * | 2022-08-23 | 2022-12-09 | 南开大学 | Erasable inkless printing material with high cycle performance and preparation method and application thereof |
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| CN115449083B (en) * | 2022-08-23 | 2023-07-04 | 南开大学 | Erasable inkless printing material with high cycle performance and preparation method and application thereof |
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