CN114873642B - Doughnut-shaped strontium molybdate nano material and preparation method thereof - Google Patents
Doughnut-shaped strontium molybdate nano material and preparation method thereof Download PDFInfo
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- CN114873642B CN114873642B CN202210354488.2A CN202210354488A CN114873642B CN 114873642 B CN114873642 B CN 114873642B CN 202210354488 A CN202210354488 A CN 202210354488A CN 114873642 B CN114873642 B CN 114873642B
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Abstract
The invention belongs to the field of inorganic material synthesis, and discloses a doughnut-shaped strontium molybdate nano material and a preparation method thereof. The preparation method comprises the following steps: dissolving a certain amount of phenanthrene in chloroform solventThe solute of the carrier of the corollary is stirred vigorously to obtain a liquid film containing the carrier; soaking the treated clean egg membrane in the liquid membrane to form a free biological membrane supported liquid membrane; preparation of Sr (NO) 3 ) 2 Solutions and Na containing specific additives 2 MoO 4 A solution; the two solutions are separated into two vertical solution systems by using a free biological film supported liquid film to form a free biological film supported liquid film synthesis system which is divided into an upper side and a lower side, wherein the upper side solution is Na containing a specific additive 2 MoO 4 Solution, the lower solution is Sr (NO 3 ) 2 A solution; after the reaction was completed at normal temperature and pressure, the product in the upper solution was collected. The doughnut-shaped strontium molybdate nano material synthesized by the method has novel structure, the preparation method is green and mild, is simple and efficient, and has wide application prospect in the optical field.
Description
Technical Field
The invention belongs to the field of inorganic material synthesis, and particularly relates to a doughnut-shaped strontium molybdate nano material and a preparation method thereof.
Background
SrMoO 4 Is a wide forbidden band semiconductor and has important application in the fields of luminescence, laser, photocatalysis and the like. Research shows that SrMoO 4 The physicochemical properties of (2) can be adjusted by different synthesis techniques and experimental conditions. Heretofore, there have been many syntheses of SrMoO 4 Nanostructure methods such as microwave irradiation, electrochemical, hydrothermal, sol-gel, and the like. By these methods, various SrMoO has been obtained 4 The nanometer structure comprises rice grain shape, elliptic rod, nanometer wire, flower structure, dumbbell shape, etc. The control of the structure is expected to improve the specific surface, reduce the forbidden bandwidth, introduce active defects and the like, and the structure has positive effects on improving the performance.
On the other hand, the existing synthesis methods often require additional energy, such as high temperature and high pressure, electric energy, etc., not only waste energy, but also may pollute the environment or reduce the quality of the product due to volatilization of reactants. For the reaction carried out at normal temperature and normal pressure, it is often difficult to obtain a material with uniform structure and better performance. Therefore, the novel synthesis method is provided, not only can be performed in green and efficient manner, but also can regulate and control the morphology and structure of the material, and has positive and important significance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a doughnut-shaped strontium molybdate nano material with uniform size, novel structure and improved performance and a preparation method thereof. The doughnut-shaped strontium molybdate nano material has a structure similar to a biconcave disc structure of erythrocytes in a human body, and the shape can increase the ratio of the surface area to the volume, accelerate the exchange rate of substances and improve the stacking density; the preparation method is green and mild, and is simple and efficient.
In order to achieve the above purpose, the present invention provides the following technical solutions:
a doughnut-shaped strontium molybdate nanomaterial characterized by: the nanomaterial has a doughnut-like structure, and has circular grooves on the upper and lower surfaces, grooves in the middle, and rough surfaces, and has a diameter of 5 μm, a height of 2.5 μm, and grooves on the upper and lower surfaces of 1.5 μm.
The invention also provides a preparation method of the doughnut-shaped strontium molybdate nano material, which comprises the following specific steps:
(1) Dissolving phenanthroline carrier solute in chloroform solvent, and stirring vigorously for a certain time to obtain carrier-containing liquid film.
(2) Soaking the treated clean egg membrane in the liquid membrane in the step (1) for a certain time to form a free biological membrane supported liquid membrane.
(3) Preparation of Sr (NO) 3 ) 2 Solutions and Na containing specific additives 2 MoO 4 A solution.
(4) Separating the two solutions in the step (3) into two vertical solution systems by using the free biofilm supported liquid film in the step (2) to form a free biofilm supported liquid film synthesis system; the free biological film supported liquid film synthesizing system is divided intoThe upper solution is Na containing specific additive 2 MoO 4 Solution, the lower solution is Sr (NO 3 ) 2 The solutions at the upper side and the lower side are separated by a free biomembrane supported liquid film.
(5) After the reaction is finished at normal temperature and normal pressure for a certain time, the product in the upper solution is centrifugally separated and cleaned to obtain the final product.
Wherein, the specific additive in the step (3) is citric acid, which plays a role in controlling the shape and size of the material.
Preferably, in the step (1), the dosage of the chloroform solvent is 80mL, the dosage of the phenanthroline carrier solute is 0.2g, the stirring speed is 3000rpm, and the stirring time is 15min; the soaking time in the step (2) is 48 hours; the step (3) contains Na with specific additive 2 MoO 4 The solution dosage is 20mL, sr (NO) 3 ) 2 The dosage of the solution is 20mL; the reaction in the step (5) is carried out at normal temperature and pressure for 24 hours.
Preferably, reactant Na as described in step (3) 2 MoO 4 The concentration of the solution is 0.005-0.02mol/L, sr (NO) 3 ) 2 The concentration of the solution is 0.005-0.02mol/L, and the dosage of citric acid is 0.002-0.005g.
Preferably, in the steps (3) and (4), 20mL of Na containing 0.004g of citric acid and 0.01mol/L 2 MoO 4 Solution and 0.01mol/L concentration of Sr (NO) in 20mL volume 3 ) 2 The solution is respectively added to the upper side and the lower side of the free biological film supported liquid film synthesizing system.
In the invention, the constructed free biomembrane supported liquid film synthesis system is the key for synthesizing the doughnut-shaped strontium molybdate structure. After the synthesis reaction starts, sr in solution at the lower side of the supported liquid film 2+ Complexing with the phenanthroline carrier dissolved in the supported liquid film at the interface. When the complex ions diffuse to the interface between the upper solution of the supported liquid film and the supported liquid film, moO in the upper solution 4 2- Will abstract Sr from complex ions 2+ Under the induction of double templates of eggshell membrane and additive, the egg shell membrane is shaped by crystal nucleation, growth and assemblySrMoO formation 4 Is a doughnut structure.
In the synthesis process, the free biomembrane supported liquid film synthesis system has multiple functions of regulating and controlling crystal nucleation, growth and assembly:
(1) Transmission function of the "K-Na" pump of the free biofilm supported liquid film: due to SrMoO 4 Precipitation of Sr 2+ Can be transported by phenanthroline selectivity and even reverse concentration gradient, and the transport process of the ions can control the reaction kinetics.
(2) Eggshell membrane promotes precipitation: the egg membrane is rich in various organic matters, wherein part of the components can reduce SrMoO 4 And promote its precipitation.
(3) Double induction of eggshell membrane and additives: the additive cooperates with eggshell membrane to realize stronger adsorption and space limiting effect, thereby inducing SrMoO 4 Growing and assembling along a specific direction. SrMoO 4 The crystal nucleus should grow along two-dimensional directions to form a sheet shape, and the sheet structures are mutually piled to form a shape of a 'drum', but under the combined action of the multiple effects, obvious lattice defects appear in the crystal growth process, the middle part of the 'drum' is deleted, and finally the shape of the doughnut is formed.
If any factor such as free biofilm, carrier-containing liquid film, citric acid additive is missing from the synthesis system, such a structure is completely unavailable.
Compared with the prior art, the invention has the following advantages:
1. the free biomembrane supported liquid film synthesizing system constructed by the invention can synthesize the doughnut-shaped strontium molybdate nano material at normal temperature and normal pressure, and the method is green and mild, simple and efficient.
2. The invention synthesizes the doughnut-shaped strontium molybdate nano material for the first time, the material has novel structure and uniform size, and the rough assembly structure can lead to higher specific surface area and favorable defects, thereby bringing improved performance and having wide prospect in the optical field.
Drawings
Fig. 1 is an SEM photograph of the doughnut-shaped strontium molybdate nanomaterial obtained in example 1 at a magnification of 5 um.
Fig. 2 is an SEM photograph of the doughnut-shaped strontium molybdate nanomaterial obtained in example 1 at a magnification of 1 um.
Fig. 3 is an XRD pattern of the doughnut-shaped strontium molybdate nanomaterial obtained in example 1.
FIG. 4 is a schematic diagram of a free biofilm supported liquid membrane synthesis system.
Detailed Description
The technical scheme of the doughnut-shaped strontium molybdate nano material and the preparation method thereof provided by the invention are further described below with reference to specific examples and attached drawings. The advantages and features of the present invention will become more apparent in conjunction with the following description.
It should be noted that the embodiments of the present invention are preferred embodiments, and are not intended to limit the present invention in any way. The technical features or combinations of technical features described in the embodiments of the present invention should not be regarded as isolated, and they may be combined with each other to achieve a better technical effect. Additional implementations are also included within the scope of the preferred embodiments of the present invention and should be understood by those skilled in the art to which the embodiments of the present invention pertain.
Techniques, methods, and apparatus known to one of ordinary skill in the relevant art may not be discussed in detail, but should be considered part of the specification where appropriate. In all examples shown and discussed herein, any specific values should be construed as merely illustrative and not limitative. Thus, other examples of the exemplary embodiments may have different values.
The drawings of the invention are in a very simplified form and are not to scale precisely, but are for the purpose of illustrating embodiments of the invention conveniently and clearly, and are not intended to limit the scope of the invention. Any structural modification, proportional change or size adjustment should fall within the scope of the technical disclosure without affecting the effects and the achieved objects of the present invention. And the same reference numerals appearing in the drawings of the present invention denote the same features or elements, and may be used in different embodiments.
Example 1
(1) 0.2g of phenanthroline carrier solute was dissolved in 80mL of chloroform solvent, and stirred at a stirring speed of 3000rpm for 15 minutes to obtain a carrier-containing liquid film.
(2) Soaking the treated egg membrane in the liquid membrane for 48h to form a free biological membrane supported liquid membrane.
(3) 20mL of Na containing 0.004g of citric acid at 0.01mol/L was prepared 2 MoO 4 Solution and 0.01mol/L concentration of Sr (NO) in 20mL volume 3 ) 2 A solution;
(4) Separating the two solutions in the step (3) into two vertical solution systems by using a free biofilm supported liquid film to form a free biofilm supported liquid film synthesis system; the free biomembrane supported liquid film synthesizing system is divided into upper and lower sides, and the upper solution is Na containing citric acid 2 MoO 4 Solution, the lower solution is Sr (NO 3 ) 2 The solutions at the upper side and the lower side are separated by a free biomembrane supported liquid film. As shown in fig. 4.
(5) And after the reaction is carried out for 24 hours at normal temperature and normal pressure, centrifugally separating and cleaning the product in the upper solution to obtain a final product.
Fig. 1 is an SEM photograph of the doughnut-shaped strontium molybdate nanomaterial obtained in example 1 at a magnification of 5 um. It can be seen from the figure that it has a doughnut-like structure and is uniform in size.
Fig. 2 is an SEM photograph of the doughnut-shaped strontium molybdate nanomaterial obtained in example 1 at a magnification of 1 um. As can be seen, the strontium molybdate doughnut structure has circular grooves on the upper and lower surfaces, grooves in the middle and has a rough surface, the diameter of which is 5 μm, the height of which is 2.5 μm, and the diameter of the grooves on the upper and lower surfaces is 1.5. Mu.m.
Fig. 3 is an XRD pattern of the doughnut-shaped strontium molybdate nanomaterial obtained in example 1. As can be seen from the figure, the prepared product is consistent with the standard JCPDS card (No. 85-0586) and is of tetragonal scheelite strontium molybdate structure.
Example 2
(1) 0.2g of phenanthroline carrier solute was dissolved in 80mL of chloroform solvent, and stirred at a stirring speed of 3000rpm for 15 minutes to obtain a carrier-containing liquid film.
(2) Soaking the treated egg membrane in the liquid membrane for 48h to form a free biological membrane supported liquid membrane.
(3) 20mL of 0.005mol/L Na containing 0.004g of citric acid was prepared 2 MoO 4 Solution and 20mL volume of 0.005mol/L Sr (NO) 3 ) 2 A solution.
(4) Separating the two solutions in the step (3) into two vertical solution systems by using a free biofilm supported liquid film to form a free biofilm supported liquid film synthesis system; the free biomembrane supported liquid film synthesizing system is divided into upper and lower sides, and the upper solution is Na containing citric acid 2 MoO 4 Solution, the lower solution is Sr (NO 3 ) 2 The solutions at the upper side and the lower side are separated by a free biomembrane supported liquid film.
(5) And after the reaction is carried out for 24 hours at normal temperature and normal pressure, centrifugally separating and cleaning the product in the upper solution to obtain a final product.
Example 3
(1) 0.2g of phenanthroline carrier solute was dissolved in 80mL of chloroform solvent, and stirred at a stirring speed of 3000rpm for 15 minutes to obtain a carrier-containing liquid film.
(2) Soaking the treated egg membrane in the liquid membrane for 48h to form a free biological membrane supported liquid membrane.
(3) 20mL of Na containing 0.002g of citric acid at 0.02mol/L was prepared 2 MoO 4 Solution and 0.02mol/L concentration of Sr (NO) in 20mL volume 3 ) 2 A solution.
(4) Separating the two solutions in the step (3) into two vertical solution systems by using a free biofilm supported liquid film to form a free biofilm supported liquid film synthesis system; the free biomembrane supported liquid film synthesizing system is divided into upper and lower sides, and the upper solution is Na containing citric acid 2 MoO 4 Solution, the lower solution is Sr (NO 3 ) 2 The solutions at the upper side and the lower side are separated by a free biomembrane supported liquid film.
(5) And after the reaction is carried out for 24 hours at normal temperature and normal pressure, centrifugally separating and cleaning the product in the upper solution to obtain a final product.
The reagents adopted by the invention are purchased from national drug group chemical reagent limited company: wherein, chloroform, AR (Shanghai test) purity is more than or equal to 99%; phenanthroline, AR (Shanghai test), purity not less than 99%; sodium molybdate, AR (Shanghai test), purity not less than 99%; strontium nitrate, AR (Shanghai test), purity not less than 99.5%; citric acid, AR (Shanghai test), purity not less than 99.5%. The instrument adopted by the invention is a conventional chemical reagent.
The above description is only illustrative of the preferred embodiments of the invention and is not intended to limit the scope of the invention in any way. Any alterations or modifications of the invention, which are obvious to those skilled in the art based on the teachings disclosed above, are intended to be equally effective embodiments, and are intended to be within the scope of the appended claims.
Claims (3)
1. The preparation method of the doughnut-shaped strontium molybdate nano material is characterized by comprising the following specific steps of:
(1) Dissolving a phenanthroline carrier solute in a chloroform solvent, and stirring to obtain a carrier-containing liquid film;
(2) Soaking the treated egg membrane in the liquid membrane to form a free biological membrane supported liquid membrane;
(3) Preparation of Sr (NO) 3 ) 2 Solutions and Na containing specific additives 2 MoO 4 A solution;
(4) Separating the two solutions in the step (3) into two vertical solution systems by using the free biofilm supported liquid film in the step (2) to form a free biofilm supported liquid film synthesis system; the free biomembrane supported liquid film synthesizing system is divided into upper and lower sides, and the upper solution is Na containing specific additive 2 MoO 4 Solution, the lower solution is Sr (NO 3 ) 2 The solutions at the upper side and the lower side are separated by a free biomembrane supported liquid film;
(5) After the reaction is finished at normal temperature and normal pressure, centrifugally separating and cleaning the product in the upper solution to obtain a final product;
the chloroform solvent dosage is 80mL, the phenanthroline carrier solute dosage is 0.2g, the stirring speed is 3000rpm, and the stirring time is 15min;
the soaking time in the step (2) is 48 hours;
the step (3) contains Na with specific additive 2 MoO 4 The solution dosage is 20mL, sr (NO) 3 ) 2 The dosage of the solution is 20mL;
the reaction is carried out for 24 hours at normal temperature and pressure in the step (5);
the specific additive in the step (3) is citric acid;
na in the step (3) 2 MoO 4 The concentration of the solution is 0.005-0.02mol/L, sr (NO) 3 ) 2 The concentration of the solution is 0.005-0.02mol/L, and the dosage of citric acid is 0.002-0.005g;
the steps (3) and (4) contain 0.004g of 0.01mol/L Na of citric acid 2 MoO 4 Solution and Sr (NO) with concentration of 0.01mol/L 3 ) 2 The solution is respectively added to the upper side and the lower side of the free biological film supported liquid film synthesizing system.
2. A doughnut-shaped strontium molybdate nano material is characterized in that the nano material has a doughnut-like structure, and the upper and lower surfaces of the nano material contain circular grooves, the middle of the nano material contains grooves and the surface of the nano material is rough.
3. A doughnut-shaped strontium molybdate nanomaterial according to claim 2 wherein: the nanomaterial has a doughnut-like structure, and has circular grooves on the upper and lower surfaces, grooves in the middle, and rough surfaces, and has a diameter of 5 μm, a height of 2.5 μm, and grooves on the upper and lower surfaces of 1.5 μm.
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