CN112110822A - Manganese-containing inorganic-organic hybrid material and preparation and application thereof - Google Patents
Manganese-containing inorganic-organic hybrid material and preparation and application thereof Download PDFInfo
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Abstract
The invention relates to a manganese-containing inorganic-organic hybrid material and a preparation method thereof. The manganese-containing inorganic-organic hybrid material is MnBr4(TPA)2TPA is tetrapropylammonium ion with chemical formula C24H56Br4MnN2The formula weight is 747.28, the crystal space group is C2/C, the unit cell parameters are a ═ 32.9036(18), b ═ 14.2967(8), C ═ 14.8159(8), α ═ 90, β ═ 109.898(5), and γ ═ 90. The preparation method comprises the steps of respectively dissolving tetrapropyl ammonium bromide and manganese bromide in isopropanol, and mixing the tetrapropyl ammonium bromide and the manganese bromide under stirring to react to obtain MnBr4(TPA)2And (3) obtaining a powder product. Dissolving the powder product in ethanol for recrystallization to obtain MnBr4(TPA)2And (3) crystallizing the product. The preparation method has simple operation and short time consumption, and the product can emit light at 512nm under the excitation of 361nm ultraviolet lightGreen fluorescence, and has high quantum yield and stability.
Description
Technical Field
The invention relates to the technical field of inorganic and organic materials, in particular to a manganese-containing inorganic and organic hybrid material and a preparation method thereof.
Background
Inorganic-organic hybrid materials are widely used in many fields of electricity, optics, energy storage, catalysis and sensing due to their mild synthetic methods and superior properties. Among them, metal-halogen inorganic-organic hybrid materials have been receiving attention in recent years due to their superior optical and electrical properties. Although there is currently a great deal of research on photoluminescent metal-halogen inorganic-organic hybrid materials, most of these research is based on lead-halogen hybrid perovskites or copper (i) -halogen perovskites. The biotoxicity of lead and the instability of copper (i) limit the practical application of these two metal-halogen perovskites. The manganese-halogen-based inorganic-organic hybrid material is low in biological toxicity and good in stability, so that the manganese-halogen-based inorganic-organic hybrid material can possibly replace the two metal-halogen inorganic-organic hybrid optical materials. However, there are few reports on the manganese-halogen hybrid photoluminescent material, and the preparation method of the manganese-halogen hybrid photoluminescent material is time-consuming.
Disclosure of Invention
Aiming at the problems, the invention provides a manganese-containing inorganic-organic hybrid material and a preparation method thereof. The method comprises the steps of mixing and stirring tetrapropylammonium bromide and manganese bromide in isopropanol, and filtering to obtain green fluorescent MnBr under the excitation of 361nm ultraviolet light4(TPA)2Inorganic-organic hybrid materials. The preparation method is simple and convenient to operate, short in time consumption, and the prepared MnBr4(TPA)2The inorganic-organic hybrid material has high quantum yield.
Manganese-containing inorganic-organic hybrid material MnBr4(TPA)2TPA is tetrapropylammonium ion, MnBr4(TPA)2TPA is tetrapropylammonium ion with chemical formula C24H56Br4MnN2The formula weight is 747.28, the crystal space group is C2/C, the unit cell parameters are a ═ 32.9036(18), b ═ 14.2967(8), C ═ 14.8159(8), α ═ 90, β ═ 109.898(5), γ ═ 90; it emits green fluorescence at 512nm under the excitation of 361nm ultraviolet light;
TABLE 1 MnBr4(TPA)2Crystal data
A manganese-containing inorganic-organic hybrid material and a preparation method thereof are realized by the following technical scheme:
weighing tetrapropylammonium bromide, adding the tetrapropylammonium bromide into a reaction bottle, adding isopropanol, and carrying out ultrasonic treatment for 0.1-10 minutes to dissolve the tetrapropylammonium bromide to obtain a solution 1; weighing manganese bromide, adding the manganese bromide into a reaction bottle, adding isopropanol, and carrying out ultrasonic treatment for 0.1-10 minutes to dissolve the manganese bromide to obtain a solution 2; dropwise adding the solution 1 into the solution 2 or dropwise adding the solution 2 into the solution 1 or simultaneously adding the two into an empty container under the condition that the stirring speed is 100-2500 rpm, and continuously stirring for reaction, wherein the stirring speed is 100-2500 rpm, and the stirring temperature is 0-160 ℃. Obtaining suspension after reaction, and filtering the suspension at normal pressure by using filter paper as a filter layer to obtain a solid powder product. Washing the solid product with 0.1-20mL of isopropanol for 1-5 times, and naturally drying at room temperature for 0.1-72 hours to obtain MnBr4(TPA)2A solid powder product; to MnBr4(TPA)2Recrystallizing the solid powder product to obtain green blocky MnBr4(TPA)2A crystal product having a crystal size of
The concentration of the tetrapropylammonium bromide in the isopropanol is 0.001-20 mol/L; the concentration of the manganese bromide in the isopropanol is 0.001-20 mol/L; the molar ratio of tetraethyl ammonium bromide to manganese bromide is as follows: 1:10-10: 1; the volume of the solution 1 is 0.1-100 mL; the volume of the solution 2 is 0.1-100 mL.
The pair of MnBr4(TPA)2The recrystallization step of the solid powder product is as follows: weighing MnBr4(TPA)2Adding ethanol into the solid powder product, performing ultrasonic treatment for 0.1-10 min to dissolve the solid powder product to obtain a solution 3, and filtering at normal pressure by using filter paper as a filter layer to obtain a filtrate. Standing the filtrate in natural room temperature environment for 0.1-72 hr, volatilizing solvent to separate out green blocky crystal, i.e. MnBr4(TPA)2And (3) crystallizing the product.
The pair of MnBr4(TPA)2Subjecting the solid powder product to a recrystallization step, MnBr4(TPA)2The concentration of the solid powder product in ethanol is 0.001-20 mol/L; the volume of the solution 3 is 0.1-100 mL.
The invention has the following technical characteristics and beneficial effects:
1. the MnBr thus claimed4(TPA)2The hybrid material has good stability and high fluorescence quantum yield;
2. the MnBr thus claimed4(TPA)2The preparation method of the hybrid material is simple and convenient, short in time consumption and low in cost;
drawings
FIG. 1.MnBr4(TPA)2Schematic structure of inorganic-organic hybrid.
FIG. 2 is MnBr4(TPA)2An inorganic-organic hybrid infrared spectrum;
FIG. 3 is MnBr4(TPA)2Simulating a powder diffraction pattern obtained by an inorganic-organic hybrid experiment and crystal data to obtain a comparison pattern of data;
FIG. 4.MnBr4(TPA)2Photoluminescence spectra of inorganic-organic hybrids. Solid line (right): emission spectrum (excitation wavelength 361 nm); dotted line (left): excitation spectroscopy.
FIG. 5.MnBr4(TPA)2Ultraviolet absorption spectrum of inorganic-organic hybrid; solvent: and (3) acetonitrile.
FIG. 6.MnBr4(TPA)2Thermogram of inorganic organic hybrid.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the present invention is limited to the examples, and any technologies implemented based on the present invention should be considered as the scope of the present invention.
Example 1
Weighing 0.266 of tetrapropylammonium bromide, adding the weighed tetrapropylammonium bromide into a 25mL reaction bottle, adding 10mL of isopropanol, and carrying out ultrasonic treatment for 5 minutes to dissolve the mixture to obtain a solution 1; weighing 0.214g of manganese bromide, adding the manganese bromide into a 25mL reaction bottle, adding 5mL of isopropanol, and carrying out ultrasonic treatment for 5 minutes to dissolve the manganese bromide to obtain a solution 2; the solution is stirred at 1500rpmDropwise adding the solution 1 into the solution 2, and continuously stirring and reacting at the same stirring speed for 0.5 hour at the stirring temperature of 25 ℃. Obtaining suspension after reaction, and filtering the suspension at normal pressure by using filter paper as a filter layer to obtain a solid powder product. Washing the solid product with 5mL of isopropanol for 3 times, and naturally drying at room temperature for 12 hours to obtain MnBr4(TPA)2Solid powder product. To MnBr4(TPA)2The solid powder product was recrystallized: weighing MnBr4(TPA)2Adding 0.3g of solid powder product into 15mL of ethanol, performing ultrasonic treatment for 5 minutes to dissolve the solid powder product to obtain a solution 3, and performing normal-pressure filtration by using filter paper as a filter layer to obtain a filtrate. Standing the filtrate in natural room temperature environment for 72 hr, volatilizing the solvent to separate out green blocky crystal, i.e. MnBr4(TPA)2And (3) crystallizing the product.
Is selected to have a size of
The obtained MnBr4(TPA)2Single crystal diffraction analysis of the crystal at low temperature 100K gave the crystal structure data C2/C point group, a 32.9036(18), b 14.2967(8), C14.8159 (8), α 90, β 109.898(5), and γ 90, as shown in fig. 1. Testing the prepared MnBr4(TPA)2The infrared spectrum (as shown in figure 2) and the powder diffraction spectrum (as shown in figure 3) of the product show that the obtained crystals have higher purity from figures 2 and 3. Measuring MnBr4(TPA)2The steady state spectrum of the solid powder and the obtained excitation and luminescence spectrum are shown in FIG. 4, under 361nm excitation, the solid powder has an emission peak at 512nm, and the photoluminescence quantum yield is 89%, which is higher than the quantum yield of some manganese-containing inorganic-organic hybrid materials (such as (Pyrrolidinium) MnBr)3The quantum yield was 28.5%; (pyrrolidium) MnCl3Quantum yield 56%). Weighing MnBr4(TPA)2The UV absorption spectrum of 0.1g solid powder dissolved in 5mL acetonitrile was measured, and the data are shown in FIG. 5, which shows distinct absorption peaks at 277nm, 287nm, 305nm, 361nm, 375nm, 435nm and 451nm, corresponding to (MnBr)4)2-Seven characteristic absorption peaks of, furtherThe prepared product is the manganese-containing inorganic-organic hybrid material. To MnBr4(TPA)2Thermogravimetric analysis is carried out on the solid powder product, the test condition is nitrogen atmosphere, the temperature is raised at the speed of 10 ℃/min, the measurement temperature range is 40-800 ℃, the obtained data is shown in figure 6, and the initial decomposition temperature is about 273 ℃, which shows that the solid powder product has higher thermal stability.
Example 2
Weighing 0.133 of tetrapropylammonium bromide, adding the tetrapropylammonium bromide into a 25mL reaction bottle, adding 10mL of isopropanol, and carrying out ultrasonic treatment for 5 minutes to dissolve the tetrapropylammonium bromide to obtain a solution 1; weighing 0.157g of manganese bromide, adding the manganese bromide into a 25mL reaction bottle, adding 5mL of isopropanol, and carrying out ultrasonic treatment for 5 minutes to dissolve the manganese bromide to obtain a solution 2; dropwise adding the solution 1 into the solution 2 under the condition of a stirring speed of 1500rpm, and continuously stirring and reacting at the same stirring speed for 1 hour at a stirring temperature of 45 ℃. Obtaining suspension after reaction, and filtering the suspension at normal pressure by using filter paper as a filter layer to obtain a solid powder product. Washing the solid product with 5mL of isopropanol for 3 times, and naturally drying at room temperature for 16 hours to obtain MnBr4(TPA)2Solid powder product. To MnBr4(TPA)2The solid powder product was recrystallized: weighing MnBr4(TPA)2Adding 0.2g of solid powder product into 25mL of ethanol, and carrying out ultrasonic treatment for 5 minutes to dissolve the solid powder product to obtain a solution 3, and filtering the solution at normal pressure by using filter paper as a filter layer to obtain a filtrate. Standing the filtrate in natural room temperature environment for 36 hr, volatilizing the solvent to separate out green blocky crystal, i.e. MnBr4(TPA)2And (3) crystallizing the product.
Example 3
Weighing 0.266 of tetrapropylammonium bromide, adding the weighed tetrapropylammonium bromide into a 25mL reaction bottle, adding 15mL of isopropanol, and carrying out ultrasonic treatment for 10 minutes to dissolve the mixture to obtain a solution 1; weighing 0.157g of manganese bromide, adding the manganese bromide into a 25mL reaction bottle, adding 5mL of isopropanol, and carrying out ultrasonic treatment for 5 minutes to dissolve the manganese bromide to obtain a solution 2; the solution 2 is dropwise added into the solution 1 under the condition of the stirring speed of 1200rpm, the stirring reaction is continued under the same stirring speed, the stirring reaction time is 1 hour, and the stirring temperature is 85 ℃. Obtaining suspension after reaction, taking filter paper as a filter layer, and filtering at normal pressure to obtain the suspensionTo a solid powder product. Washing the solid product with 5mL of isopropanol for 3 times, and naturally drying at room temperature for 12 hours to obtain MnBr4(TPA)2Solid powder product. To MnBr4(TPA)2The solid powder product was recrystallized: weighing MnBr4(TPA)2Adding 0.05g of solid powder product into 10mL of ethanol, and carrying out ultrasonic treatment for 10 minutes to dissolve the solid powder product to obtain a solution 3, and filtering the solution at normal pressure by using filter paper as a filter layer to obtain a filtrate. Standing the filtrate in natural room temperature environment for 72 hr, volatilizing the solvent to separate out green blocky crystal, i.e. MnBr4(TPA)2And (3) crystallizing the product.
Example 4
Weighing 0.266 of tetrapropylammonium bromide, adding the weighed tetrapropylammonium bromide into a 25mL reaction bottle, adding 10mL of isopropanol, and carrying out ultrasonic treatment for 10 minutes to dissolve the mixture to obtain a solution 1; weighing 0.214g of manganese bromide, adding the manganese bromide into a 25mL reaction bottle, adding 10mL of isopropanol, and carrying out ultrasonic treatment for 10 minutes to dissolve the manganese bromide to obtain a solution 2; the solution 2 is dropwise added into the solution 1 under the condition of the stirring speed of 500rpm, the stirring reaction is continued under the same stirring speed, the stirring reaction time is 1 hour, and the stirring temperature is 120 ℃. Obtaining suspension after reaction, and filtering the suspension at normal pressure by using filter paper as a filter layer to obtain a solid powder product. Washing the solid product with 10mL of isopropanol for 3 times, and naturally drying at room temperature for 24 hours to obtain MnBr4(TPA)2Solid powder product. To MnBr4(TPA)2The solid powder product was recrystallized: weighing MnBr4(TPA)2Adding 0.10g of solid powder product into 15mL of ethanol, and carrying out ultrasonic treatment for 10 minutes to dissolve the solid powder product to obtain a solution 3, and filtering the solution at normal pressure by using filter paper as a filter layer to obtain a filtrate. Standing the filtrate in natural room temperature environment for 72 hr, volatilizing the solvent to separate out green blocky crystal, i.e. MnBr4(TPA)2And (3) crystallizing the product.
Claims (8)
1. A manganese-containing inorganic-organic hybrid material is characterized in that: MnBr4(TPA)2TPA is tetrapropylammonium ion with chemical formula C24H56Br4MnN2Chemical formula weight of 747.28, crystal space group is C2/C, unit cell parameters are a ═ 32.9036(18), b ═ 14.2967(8), C ═ 14.8159(8), α ═ 90, β ═ 109.898(5), γ ═ 90.
2. The manganese-containing inorganic-organic hybrid material according to claim 1, wherein: it emits green fluorescence at 512nm under the excitation of 361nm ultraviolet light; green blocky MnBr4(TPA)2Crystals of size of
3. A preparation method of the manganese-containing inorganic-organic hybrid material as claimed in claim 1 or 2, which is characterized by comprising the following specific steps:
weighing tetrapropylammonium bromide, adding the tetrapropylammonium bromide into a reaction bottle, adding isopropanol, and carrying out ultrasonic treatment for 0.1-10 minutes to dissolve the tetrapropylammonium bromide to obtain a solution 1;
weighing manganese bromide, adding the manganese bromide into a reaction bottle, adding isopropanol, and carrying out ultrasonic treatment for 0.1-10 minutes to dissolve the manganese bromide to obtain a solution 2;
dropwise adding the solution 1 into the solution 2, or dropwise adding the solution 2 into the solution 1, or simultaneously adding the solution 1 and the solution 2 into an empty container under the condition of a stirring speed of 100-2500 rpm, and continuously stirring for reaction, wherein the stirring speed is 100-2500 rpm, and the stirring temperature is 0-160 ℃; obtaining suspension after reaction, and filtering the suspension at normal pressure by using filter paper as a filter layer to obtain a solid powder product; washing the solid product with isopropanol for 1-5 times, and naturally drying at room temperature for 0.1-72 hr to obtain MnBr4(TPA)2A solid powder product; to MnBr4(TPA)2Recrystallizing the solid powder product to obtain green blocky MnBr4(TPA)2And (3) crystallizing the product.
4. The production method according to claim 3, characterized in that: the concentration of tetrapropylammonium bromide in isopropanol is 0.001-20 mol/L; the concentration of the manganese bromide in the isopropanol is 0.001-20 mol/L; the molar ratio of tetrapropylammonium bromide to manganese bromide is as follows: 1:10-10: 1; the volume of the solution 1 is 0.1-100 mL; the volume of the solution 2 is 0.1-100 mL; the solid product was washed with 0.1-20mL of isopropanol.
5. The production method according to claim 3 or 4, characterized in that: to MnBr4(TPA)2The recrystallization step of the solid powder product is as follows: weighing MnBr4(TPA)2Adding ethanol into the solid powder product, performing ultrasonic treatment for 0.1-10 min to dissolve the solid powder product to obtain a solution 3, and filtering at normal pressure by using filter paper as a filter layer to obtain a filtrate; standing the filtrate in natural room temperature environment for 0.1-72 hr, volatilizing solvent to separate out green blocky crystal, i.e. MnBr4(TPA)2And (3) crystallizing the product.
6. The method of claim 5, wherein: MnBr4(TPA)2The concentration of the solid powder product in ethanol is 0.001-20 mol/L.
7. The method of claim 5, wherein: the volume of the solution 3 is 0.1-100 mL.
8. Use of the manganese-containing inorganic-organic hybrid material according to claim 1 or 2, wherein: the manganese-containing inorganic-organic hybrid material is applied as a photoluminescence material.
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Cited By (3)
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| CN113943225A (en) * | 2021-09-26 | 2022-01-18 | 华中科技大学 | Zero-dimensional organic manganese-based metal halide beta-ray scintillator and preparation method thereof |
| CN114656364A (en) * | 2022-03-09 | 2022-06-24 | 北京科技大学 | Mn-based organic-inorganic hybrid metal halide luminescent material and preparation method thereof |
| CN115651019A (en) * | 2022-09-16 | 2023-01-31 | 南开大学 | Self-recoverable elastic force luminous organic-inorganic hybrid metal halide crystal and synthetic method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113943225A (en) * | 2021-09-26 | 2022-01-18 | 华中科技大学 | Zero-dimensional organic manganese-based metal halide beta-ray scintillator and preparation method thereof |
| CN113943225B (en) * | 2021-09-26 | 2022-11-11 | 华中科技大学 | Zero-dimensional organic manganese-based metal halide beta-ray scintillator and preparation method thereof |
| CN114656364A (en) * | 2022-03-09 | 2022-06-24 | 北京科技大学 | Mn-based organic-inorganic hybrid metal halide luminescent material and preparation method thereof |
| CN115651019A (en) * | 2022-09-16 | 2023-01-31 | 南开大学 | Self-recoverable elastic force luminous organic-inorganic hybrid metal halide crystal and synthetic method and application thereof |
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