CN112079379B - ZnTiO compound 3 Material and method for producing same - Google Patents

ZnTiO compound 3 Material and method for producing same Download PDF

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CN112079379B
CN112079379B CN202010972183.9A CN202010972183A CN112079379B CN 112079379 B CN112079379 B CN 112079379B CN 202010972183 A CN202010972183 A CN 202010972183A CN 112079379 B CN112079379 B CN 112079379B
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陈龙
赵屹
陈思凡
郑玉船
潘乐
朱旭宏
王俊波
李良清
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Huangshan University
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Abstract

The invention relates to the field of photocatalytic materials, in particular to ZnTiO 3 Materials and methods for their preparation. The preparation method of the invention takes zinc acetate dihydrate as a zinc source and butyl titanate as a titanium source, utilizes the mixed reaction of a zinc acetate ethanol solution and a butyl titanate ethanol solution, dries the generated white precipitate and then calcines the white precipitate to prepare ZnTiO 3 A material; organic micromolecule triethylamine is added into a reaction system to be used as a soft template to ZnTiO 3 The shape and the structure are regulated and controlled, and the ZnTiO with higher purity and more uniform particle size distribution is prepared 3 A material. Taking malachite green as a target degradation product, and investigating ZnTiO under the irradiation of a xenon-mercury lamp 3 The photocatalytic performance of the material proves that ZnTiO prepared by adding triethylamine 3 The material has better photocatalysis effect.

Description

ZnTiO compound 3 Material and method for producing same
Technical Field
The invention relates to the field of photocatalytic materials, in particular to ZnTiO 3 Materials and methods for their preparation.
Background
Zinc titanate is a perovskite structure complex oxide, which can be expressed as ABO 3 The ionic radius and electronegativity of the elements A and B influence the photocatalytic performance of the elements A and B, and the zinc titanate is stable in property, non-toxic, harmless, high in catalytic efficiency, good in semiconductor property and optical and electrical property, and is one of the best candidate materials as a photocatalyst. Therefore, the regulation and control of the preparation of the zinc titanate have important significance in the aspects of environmental protection, photocatalytic utilization rate and the like. The zinc titanate has a stable perovskite structure, and the unique forbidden band width of the zinc titanate enables the zinc titanate to have photocatalytic performanceThe mask has advantages. Meanwhile, the forbidden bandwidth is large, so that the utilization rate of the zinc titanate to sunlight is low, and the wide application of the zinc titanate is limited. Therefore, the modification of the zinc titanate and the improvement of the light utilization rate are significant.
The coprecipitation method is a uniform precipitation method in which when a solution contains two or more kinds of cations and the ions exist in a uniform phase, various components can be obtained through precipitation reaction after a precipitant is added. The method is an important method for preparing the composite oxide superfine powder containing two or more metal elements. The coprecipitation method has the advantages that the obtained nano powder material has uniform chemical components, smaller particles and uniform particle size distribution. ZnTiO prepared by coprecipitation method in prior art 3 The material has the problems of low purity, large particle size and poor photocatalytic performance.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provides ZnTiO 3 A method for preparing the material.
The invention aims to solve another technical problem and provide a ZnTiO preparation for overcoming the defects in the prior art 3 A material.
In order to solve the technical problem of the invention, the technical scheme is that the ZnTiO modified ZnTiO material 3 The preparation method of the material comprises the following steps:
s1, preparing a zinc acetate ethanol solution and a butyl titanate ethanol solution, wherein the concentrations of the two solutions are the same and are 0.01-0.03mol/L, measuring the two solutions with the same volume, slowly adding the butyl titanate ethanol solution into the zinc acetate ethanol solution, uniformly stirring to obtain a mixed solution, then slowly dropwise adding triethylamine, wherein each 1mL of the butyl titanate ethanol solution corresponds to 0.10-0.15mL of triethylamine, and uniformly stirring to obtain a reaction solution;
s2, filling the reaction liquid into a reagent tube, carrying out centrifugal separation until the reaction liquid is layered, removing a supernatant, adding absolute ethyl alcohol into a lower-layer precipitate for washing, carrying out centrifugal separation to remove the supernatant, repeating the step of adding absolute ethyl alcohol until the supernatant is removed for 2-3 times, and drying the lower-layer precipitate in a drying oven at 70-90 ℃ for 3-8 hours to obtain a dried precipitate;
s3, grinding the dried precipitate, calcining at 700-900 ℃ for 3-5h, cooling to room temperature, and taking out to obtain ZnTiO 3 A material.
As the above ZnTiO compound 3 The material preparation method is further improved as follows:
preferably, the preparation method of the zinc acetate ethanol solution comprises the steps of weighing 0.09-0.27g of zinc acetate dihydrate solid powder, adding the zinc acetate dihydrate solid powder into 40mL of absolute ethanol, and stirring at room temperature until the zinc acetate dihydrate solid powder is completely dissolved.
Preferably, the preparation method of the butyl titanate ethanol solution comprises the steps of measuring 0.14-0.42mL of butyl titanate, adding the butyl titanate into 40mL of anhydrous ethanol, and stirring until the butyl titanate is completely dissolved.
In order to solve another technical problem of the invention, the technical scheme adopted is that the ZnTiO prepared by any one of the preparation methods is 3 A material.
As the above ZnTiO 3 Further improvement of the material:
preferably, the ZnTiO compound is 3 When the material is used for degrading malachite green, the method comprises the following steps: weighing malachite green, adding into water to obtain malachite green solution of 8-20mg/L, and adding ZnTiO 3 Adding the material into malachite green solution at an addition amount of 0.5-1.0g/L, irradiating with mercury xenon lamp, and stirring at 28-42 deg.C with magnetic stirrer until the malachite green is completely degraded.
Compared with the prior art, the invention has the beneficial effects that:
1) The method adopts a coprecipitation method, takes zinc acetate dihydrate as a zinc source and butyl titanate as a titanium source, and carries out multiple groups of experimental regulation and control to prepare ZnTiO under different experimental conditions 3 . The butyl titanate reacts violently with water to form Ti (OH) 4 Precipitation, hydrolysis of butyl titanate in ethanol environment, reaction equation as
Ti(OC 4 H 9 ) 4 +4H 2 O＝Ti(OH) 4 +4CH 3 (CH 2 ) 3 OH。
The ethanol added in the experimental process is mainly used as a solvent of the butyl titanate, so that the butyl titanate is fully filled in the ethanolThe dispersion can slow down the hydrolysis speed of the butyl titanate, and no violent reaction can occur. Triethylamine (C) 2 H 5 ) 3 N is a symmetrical structure, wherein the N atom has partial negative charge, and can attract Zn in the reaction process 2+ Equipositively charged ions or radicals, on ZnTiO 3 The generation process of the material precursor and the final product has a regulation function.
2) Part of added triethylamine is combined into the product, and because the triethylamine is volatile at high temperature, the triethylamine in the deep calcination is volatilized, so that the final ZnTiO prepared 3 Has a porous structure, thereby having higher specific surface area and photocatalytic performance.
3) ZnTiO of perovskite structure under the condition of illumination 3 After absorbing energy, the organic material is excited to generate electrons and holes, and strong oxidizing radicals are generated to oxidize organic materials, thereby achieving the fading effect.
Drawings
FIG. 1 is a general ZnTiO compound prepared in example 1 3 Wherein 1b is an enlarged view of 1 a;
FIG. 2 is a view of the general ZnTiO compound prepared in example 1 3 XRD pattern of (a);
FIG. 3 is the triethylamine mediated ZnTiO preparation of example 2 3 Wherein 3b is an enlarged view of 3 a;
FIG. 4 is the triethylamine-modulated ZnTiO prepared in example 2 3 XRD pattern of (a);
FIG. 5 shows the ZnTiO compound prepared in example 1 3 Ultraviolet spectrum test chart of the powder;
FIG. 6 is the triethylamine-modulated ZnTiO prepared in example 2 3 Ultraviolet spectrum test pattern of the powder.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments, and all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without creative efforts belong to the protection scope of the present invention.
The reagents used primarily in this experiment are shown in table 1 below.
TABLE 1 Main test reagents
Figure BDA0002684487640000031
Figure BDA0002684487640000041
The apparatus used mainly in this experiment is shown in table 2 below.
TABLE 2 instruments required for the experiment
Figure BDA0002684487640000042
Example 1
S1, preparation of solution
(1) Preparation of 0.02mol/L zinc acetate ethanol solution
Opening an analytical balance and preheating for half an hour, and weighing 0.1790g of zinc acetate dihydrate solid powder by using weighing paper; the weighed powder was put into a beaker, 40mL of absolute ethanol was added to the beaker, stirred at room temperature using a magnetic stirrer, and stirred until completely dissolved.
(2) Preparation of 0.02mol/L butyl titanate ethanol solution
40mL of the absolute ethanol solution was weighed using a 50mL graduated cylinder and poured into a beaker. The beaker was placed on a constant temperature heating magnetic stirrer for stirring, 0.272mL (272. Mu.L) of butyl titanate was quickly and accurately measured using a pipette gun, and the weighed butyl titanate was dropped into an absolute ethanol solution. The reaction was stirred at room temperature by heating the magnetic stirrer at constant temperature until complete dissolution.
S2, measuring 40mL of zinc acetate ethanol solution by using a 50mL measuring cylinder, transferring the measured zinc acetate ethanol solution into a beaker, placing the beaker on a constant-temperature heating magnetic stirrer for stirring, and measuring 40mL of tetrabutyl titanate ethanol solution by using a 50mL measuring cylinder. Slowly adding 40mL of butyl titanate ethanol solution into zinc acetate ethanol solutionThe solution was added to a beaker with stirring, and the resulting mixed solution was designated as solution 1. After the reaction is finished, shaking the obtained mixed solution 1 evenly, respectively filling the mixed solution into a plurality of 5mL plastic centrifuge tubes, symmetrically placing the centrifuge tubes into a centrifuge, washing the centrifuge tubes by using absolute ethyl alcohol and centrifuging the centrifuge tubes twice, putting the final solid product obtained by centrifuging the centrifuge tubes into an electrothermal blowing constant-temperature drying oven, drying the product at 75 ℃, grinding the dried product, pouring the product into a crucible, putting the crucible into a box-type high-temperature furnace, calcining the product at 800 ℃ for 5 hours, cooling the product to room temperature, and taking out the crucible to obtain the common ZnTiO 3 。
Example 2
The difference between this example and example 1 is that in step S2, "40 mL of butyl titanate ethanol solution was slowly added to a beaker of zinc acetate ethanol solution, and after" addition with stirring "4.8 mL of triethylamine was measured with a dropper and slowly added to the stirred beaker, and stirring was continued until the reaction was completed after the dropwise addition, and the other conditions were the same as in example 1, and ZnTiO adjusted and controlled by triethylamine was obtained 3 。
Performance testing
1. XRD and SEM testing
(1) The general ZnTiO prepared in example 1 3 SEM and XRD tests are respectively carried out, and the test results are shown in figure 1 and figure 2, wherein figure 1b is an enlarged view of figure 1 a;
as can be seen from FIG. 1, ordinary ZnTiO 3 The particle size distribution of (A) is several micrometers to dozens of micrometers, and the enlarged view is mostly honeycomb-like small particles and a small amount of blocky particles;
as can be seen from FIG. 2, when 2 θ is 24.04 °, 32.9 °, 35.44 °, 40.58 °, 49.06 °, 53.56 °, 56.9 °, 61.9 °, 63.52 °, respectively, corresponding to orthorhombic ZnTiO crystals 3 Diffraction peaks of (110), (121), (110), (120), (220), (231), (332), (130), (211) crystal plane (JCPDS card number: 85-0547); when the 2 theta is 27.58 degrees, 36.18 degrees and 54.44 degrees, the crystal corresponds to simple cubic crystal TiO 2 Crystal face (JCPDS card number: 88-1175) of (110), (101), (211). The plain ZnTiO produced in example 1 was considered by comparison with PDF card 3 For doping simple cubic TiO 2 ZnTiO of orthorhombic crystal type 3 A mixture of (a).
(2) ZnTiO modulated by Triethylamine prepared in example 2 3 SEM and XRD tests were performed, respectively, and the results are shown in fig. 3 and 4, in which fig. 3b is an enlarged view of fig. 3 a;
as can be seen from FIG. 3, znTiO modulated by triethylamine 3 Has a particle size distribution of several microns to several tens of microns, compared with that of the common ZnTiO 3 ZnTiO regulated by triethylamine 3 The particle size of (2) is smaller and the dispersibility is better.
ZnTiO regulated by triethylamine in FIG. 4 3 The XRD pattern shows that when the 2 theta is 24 degrees, 32.88 degrees, 35.4 degrees, 40.54 degrees, 49.02 degrees, 53.52 degrees, 61.92 degrees and 63.52 degrees, the ZnTiO with the corresponding orthorhombic crystal form corresponds to the orthorhombic crystal form 3 The diffraction peaks of (110), (121), (110), (120), (231), (130) and (211) (JCPDS card number: 85-0547) of the crystal face (JCPDS) correspond to TiO of simple cubic crystal form when the 2 theta is 27.54 DEG 2 The diffraction peak of (110) crystal face (JCPDS card number: 88-1175) is compared with that of PDF card to determine that the calcined triethylamine regulates ZnTiO 3 Mainly doped with trace TiO 2 ZnTiO of orthorhombic crystal type 3 The purity of the mixture of (1) is higher.
2. Ultraviolet spectrum test
Respectively weighing 40mg of the final 1 and 2 sample powders obtained in the steps by using an analytical balance, measuring 60mL of 10mg/L malachite green solution by using a 100mL measuring cylinder, pouring the solution into a 100mL beaker, respectively dispersing the weighed powders into the equivalent malachite green solution, rapidly stirring at room temperature until the solution is completely mixed, respectively sucking the equivalent mixed solution by using a suction pipe, putting the same mixed solution into a 5mL plastic centrifuge tube for comparison, and respectively marking the mixed solution as 1 and 2. Turning on a xenon-mercury lamp light source, after preheating, focusing the light source on a beaker filled with reactants in a stirrer, adjusting the temperature of the stirrer to 30 ℃, taking one sample every 10 minutes for storage, marking, and carrying out ultraviolet spectrum test on each group of samples, wherein the results are respectively shown in fig. 5 and fig. 6.
FIG. 5 shows a general ZnTiO compound 3 An ultraviolet spectrogram of the malachite green through photocatalytic degradation; FIG. 6 is ZnTiO modulated by triethylamine 3 An ultraviolet spectrogram of the malachite green through photocatalytic degradation; the two groups of malachite green have different coursesAnd (3) degradation, wherein the degradation degree of the graph 6 is the highest, and the photocatalytic degradation of the malachite green within 50min is more than 90%. Thus obtaining the reaction of the butyl titanate and the zinc acetate in the ethanol system and adding the triethylamine for regulation and control to prepare the product doped with trace TiO 2 ZnTiO of 3 Has better photocatalytic activity.
It should be understood by those skilled in the art that the foregoing is only illustrative of several embodiments of the invention, and not of all embodiments. It should be noted that many variations and modifications are possible to those skilled in the art, and all variations and modifications that do not depart from the gist of the invention are intended to be within the scope of the invention as defined in the appended claims.

Claims (5)

1. ZnTiO compound 3 The preparation method of the material is characterized by comprising the following steps:
s1, preparing a zinc acetate ethanol solution and a butyl titanate ethanol solution, wherein the concentrations of the two solutions are the same and are 0.01-0.03mol/L, measuring the two solutions with the same volume, slowly adding the butyl titanate ethanol solution into the zinc acetate ethanol solution, uniformly stirring to obtain a mixed solution, then slowly dropwise adding triethylamine, wherein each 1mL of the butyl titanate ethanol solution corresponds to 0.10-0.15mL of triethylamine, and uniformly stirring to obtain a reaction solution;
s2, filling the reaction liquid into a reagent tube, carrying out centrifugal separation until the reaction liquid is layered, removing a supernatant, adding absolute ethyl alcohol into a lower-layer precipitate for washing, carrying out centrifugal separation to remove the supernatant, repeating the step of adding absolute ethyl alcohol until the supernatant is removed for 2-3 times, and drying the lower-layer precipitate in a drying oven at 70-90 ℃ for 3-8 hours to obtain a dried precipitate;
s3, grinding the dried precipitate, calcining at 700-900 ℃ for 3-5h, cooling to room temperature, and taking out to obtain ZnTiO 3 A material.
2. The ZnTiO of claim 1 3 The preparation method of the material is characterized in that the preparation method of the zinc acetate ethanol solution comprises the steps of weighing 0.09-0.27g of zinc acetate dihydrate solid powder, adding the zinc acetate dihydrate solid powder into 40mL of absolute ethyl alcohol, and stirring at room temperature until the zinc acetate dihydrate solid powder is completely stirredAnd (4) completely dissolving.
3. The ZnTiO of claim 1 3 The preparation method of the material is characterized in that the preparation method of the butyl titanate ethanol solution is that 0.14-0.42mL of butyl titanate is measured and added into 40mL of absolute ethanol, and the mixture is stirred until the butyl titanate is completely dissolved.
4. ZnTiO obtainable by a process according to any one of claims 1 to 3 3 A material.
5. ZnTiO according to claim 4 3 The material is characterized in that the ZnTiO compound 3 When the material is used for degrading malachite green, the method comprises the following steps: weighing malachite green, adding into water to obtain malachite green solution of 8-20mg/L, and adding ZnTiO 3 Adding the material into malachite green solution at an addition amount of 0.5-1.0g/L, irradiating with mercury xenon lamp, and stirring at 28-42 deg.C with magnetic stirrer until the malachite green is completely degraded.
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