CN109499495B - Zinc oxide/zinc hydroxide aerogel and preparation method thereof - Google Patents
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Abstract
A zinc oxide/zinc hydroxide aerogel and a preparation method thereof, belonging to the technical field of aerogel preparation. According to the invention, a hydrothermal method is adopted, soluble zinc salt and an alkaline slow-release agent are used as raw materials, zinc oxide/zinc hydroxide nanosheets with uniform appearance are formed under the influence of an anionic surfactant and hydroxyl ions, and then an ice template method is adopted to prepare the loose and porous zinc oxide/zinc hydroxide aerogel by utilizing the acting force between water molecules and lamella. The method aims to explore a simple and feasible method for preparing the zinc oxide/zinc hydroxide aerogel, which is beneficial to large-scale popularization and application. The preparation method of the zinc oxide/zinc hydroxide aerogel provided by the invention has the characteristics of easy reaction, simple operation, low production information and time cost and high yield, and the prepared zinc oxide/zinc hydroxide aerogel has the advantages of uniform structure, low density, higher specific surface area and higher porosity.
Description
Technical Field
The invention belongs to the technical field of aerogel preparation, and particularly relates to a method for preparing zinc oxide/zinc hydroxide aerogel by self-assembly of ice template-induced nanosheets.
Background
The photocatalytic water splitting hydrogen production is considered as a very promising method for obtaining clean energy, thereby relieving the energy crisis caused by the gradual shortage of fossil energy. The method can convert nearly unlimited solar energy into clean and storable chemical energy. In the technology, the introduction of the semiconductor photocatalyst can obviously improve the solar energy conversion efficiency. Therefore, inexpensive, efficient, stable semiconductor materials are considered to be highly potential photocatalyst materials. Some semiconductor materials, e.g. TiO2、ZnO、Fe2O3、WO3And the like are widely applied to the field of hydrogen preparation by photocatalytic water splitting. These materials may beAn environmentally friendly photocatalyst is simply and economically prepared by a hydrothermal growth method or an electrodeposition method. However, the solar-hydrogen energy conversion efficiency of these catalysts is limited by factors such as low conductivity, short diffusion length, poor charge conductivity between the reagents and the photocatalyst, low light energy utilization rate, and poor surface precipitation kinetics. In order to avoid the defects, besides changing the substance composition of the catalyst material, the structure of the existing catalyst can be improved, for example, the material is endowed with special structures, and the catalytic performance of the material is further improved through the synergistic effect of the structures and the material. The special structures can enlarge the contact interface of the catalyst, reduce the carrier recombination, and improve the charge transfer rate and the light energy utilization rate, thereby showing good performance in the field of photocatalysis application.
The zinc oxide is used as a transition metal oxide, has the characteristics of abundant resources, low price, environmental friendliness, wider working voltage window, good electrochemical performance and the like, and is a favorite in the fields of photoelectric materials and electrode materials all the time. In addition, zinc oxide has good ion exchange and molecular adsorption properties, has a wide prospect in the fields of molecular sieves, catalyst materials and the like, and has attracted wide attention in recent years. It is known that the crystal form, size, morphology and dimension of the nanoparticles affect the optical, electrical and magnetic properties of the nanomaterial to different degrees. The existing research shows that the size, the morphology, the specific surface area and the pore size distribution of zinc oxide particles determine the diffusion distance of ions and the maximum contact surface between a solid electrode and a solution interface, and have important significance for improving the electrochemical performance and the catalytic performance. Therefore, the control of the size, the composition, the crystal structure and even the assembly structure of the zinc oxide nano material has important significance for deeply researching the relationship between the structural characteristics and the physical and chemical properties of the zinc oxide nano material and finally improving the performance of the nano material.
Since the discovery of graphene, a large number of two-dimensional materials, such as nitrides, sulfides, selenides, tellurides, and the like, have been produced. How to mass-produce high quality layered materials is an important step in the development of 2D materials. At present, one method for preparing mesoporous zinc oxide with higher cost benefit is to decompose layered zinc hydroxide at high temperature. However, the layered structure is destroyed after calcination, and the photocatalytic performance is similar to that of nano zinc oxide. Therefore, how to further exert the advantages of the two-dimensional material and the zinc oxide to prepare the zinc oxide material similar to the two-dimensional material is a significant research hotspot. Also in nanotechnology, nanomaterial units with specific properties on the microscopic scale need to be assembled in order to obtain macroscopically novel structures and functions. Aerogel is a light porous solid material with controllable structure, which is formed by the mutual coalescence of colloidal particles or high polymer molecules. The micro-network structure in the aerogel has abundant holes, provides a large specific surface area, has a wide application prospect, and has been used for acoustic impedance coupling materials, catalysts or catalyst carriers, adsorbents, filter materials, high-temperature heat insulation materials and high-performance reversible battery materials. Therefore, the control of the size, the composition, the crystal structure and even the assembly structure of the zinc oxide nano material has important significance for deeply researching the relationship between the structural characteristics and the physical and chemical properties of the zinc oxide nano material and finally improving the performance of the nano material.
In the past case of aerogel production, scientists have mainly used sol-gel and template-guided methods. The former can be synthesized in batch, but has poor controllability; the latter can produce ordered structures, but depending on the size and fine structure of the template, are difficult to prepare in large quantities. Preparation of zinc oxide aerogels reported so far typically produces a wet zinc oxide gel, which is then subjected to a supercritical drying process to produce the aerogel. However, there are very limited reports of studies on zinc oxide wet gels, mainly due to the weak interaction of crystalline particles in the zinc oxide material in the aerogel structure. So far, there are few reports on zinc oxide aerogels. The kohlrabi takes zinc salt, polyacrylic acid and propylene oxide as precursors, and zinc oxide aerogel (Mianyang academy of academic Press 2012, 31 and 28) is prepared by supercritical drying and high-temperature annealing treatment in a protective atmosphere. The authors carried out a detailed analysis of the crystal structure of the zinc oxide of the aerogel by means of X-ray diffraction and found that the crystal system of the zinc oxide varies between triclinic and monoclinic at different annealing temperatures. Sebastian Polarz prepared zinc oxide aerogel by sol-gel action of organic zinc salts and hydrolysis of organic zinc salts using organic zinc salts (methyl zinc and zinc alkoxide) as precursors (chem. mater.2010,22,5129). Djamel Djouadi et al systematically investigated the solvent effect of the aerogel formation process by using the effect of the solvent on the sol-gel process (eur. phys.j.appl.phys.2014, 66, 10402). Because of the self crystal structure limitation of the zinc oxide, the zinc oxide aerogel is simpler to construct by adopting a hybridization mode. The zinc oxide/reduced graphene oxide hybrid aerogel is prepared by taking graphene as a framework and zinc oxide nanoparticles as active ingredients (patent application number: 201610086811.7); pozeshu et al prepared hybrid aerogels by infiltrating a sol containing zinc oxide and germanium oxide into inorganic fibers, gel aging, and supercritical drying (patent application No. 201610067340.5). Duyi et al use natural cellulose as a skeleton structure, and prepare flaky nano zinc oxide on the skeleton structure through low-temperature water bath reaction, thereby constructing the zinc oxide aerogel (patent application number: 201710366441.7). The zinc oxide aerogel prepared by the methods grows on the surface of other materials capable of forming the aerogel, and the method for preparing the zinc oxide aerogel reported at present generally has the problem of residual zinc oxide reactant precursors, template materials or organic modification molecules, so that the wide application of the zinc oxide aerogel is limited. Therefore, a method for preparing the zinc oxide aerogel, which has low cost, simple operation and easy production and amplification, needs to be developed.
Disclosure of Invention
The invention aims to provide a zinc oxide/zinc hydroxide aerogel and a preparation method thereof. Compared with the traditional supercritical drying method, the vacuum freeze drying method used in the invention has the advantages of simple operation, mild conditions, low cost and easy process amplification. The zinc oxide/zinc hydroxide aerogel prepared by the invention is formed by self-assembling wurtzite zinc oxide/zinc hydroxide nanosheets, has good crystal form purity, and solves the problem of production complexity in the currently reported preparation method of the zinc oxide aerogel. The aerogel prepared by the method has the characteristics of high specific surface area and high porosity, so that the aerogel has a good application prospect in the field of surface catalysis.
The invention starts from preparing zinc oxide/zinc hydroxide nano-sheet dispersion liquid, induces the self-assembly of the nano-sheets through an ice crystal template during freezing, and then carries out vacuum freeze drying to conveniently and quickly prepare the low-density zinc oxide/zinc hydroxide aerogel. The zinc oxide/zinc hydroxide aerogel prepared by the invention can be widely applied to the fields of batteries, sensing, catalysis and the like.
The invention relates to a method for preparing zinc oxide/zinc hydroxide aerogel, which comprises the following steps:
1) preparation of zinc oxide/zinc hydroxide nanosheet
Adding 1-4 mL of 200-300 mM surfactant aqueous solution, 4-8 mL of 100-200 mM alkaline slow-release agent aqueous solution and 4-8 mL of 100-200 mM soluble zinc salt aqueous solution into deionized water to make the total volume 100mL, adding 10-20 mg of alkali solid into the mixed solution to adjust the pH value of the solution, fully dissolving and uniformly mixing, then placing at 90-110 ℃ to react for 1-3 h, fully stirring during the reaction, finally obtaining a suspension rich in zinc oxide/zinc hydroxide nanosheet, centrifuging at 3000-7000 rpm for 3-10 min, separating out a precipitate part, and obtaining the zinc oxide/zinc hydroxide nanosheet;
2) preparation of zinc oxide/zinc hydroxide nanosheet dispersion
Repeatedly cleaning the zinc oxide/zinc hydroxide nanosheet precipitate prepared in the step 1) with deionized water for purification, then adding the purified precipitate into deionized water, standing the obtained suspension for more than 12h to enable the zinc oxide/zinc hydroxide nanosheet to naturally settle in water to be flocculent, and removing the supernatant to obtain a zinc oxide/zinc hydroxide nanosheet dispersion liquid;
3) preparation of Zinc oxide/Zinc hydroxide aerogels
And (3) freezing the zinc oxide/zinc hydroxide nanosheet dispersion liquid prepared in the step 2) at a low temperature, and after the zinc oxide/zinc hydroxide nanosheet dispersion liquid is completely solidified, carrying out vacuum freeze drying to prepare the zinc oxide/zinc hydroxide aerogel.
The surfactant used in the step 1) is one or a mixture of more of sodium dodecyl sulfate, sodium n-decyl sulfate, potassium dodecyl sulfate, sodium tetradecyl sulfate, sodium dodecyl polyoxyethylene ether sulfate and ammonium dodecyl sulfate.
The alkaline slow-release agent is hexamethylenetetramine or urea.
The soluble zinc salt is one of zinc nitrate, zinc bromide, zinc chloride, zinc acetate or zinc sulfate.
It is worth noting that the molar ratio of the added alkaline slow-release agent and the soluble zinc salt should be kept between 1: 1.
the alkali solid for adjusting the pH value of the mother liquor can be sodium hydroxide, sodium carbonate or potassium hydroxide; the stirring speed is 150-300 rpm.
The concentration of the zinc oxide/zinc hydroxide nanosheet suspension prepared in the step 1) is 0.1-0.2 mg/mL.
The concentration of the zinc oxide/zinc hydroxide nanosheet dispersion prepared after purification in the step 2) is 1-2 mg/mL.
The freezing temperature in the step 3) is-20 ℃ to-80 ℃, and the time is 12-24 hours.
The vacuum freeze drying temperature in the step 3) is-50 ℃ to-80 ℃, and the time is 24-48 hours.
The method for preparing the zinc oxide/zinc hydroxide aerogel has the advantages of simple equipment, mild conditions and cheap and easily-obtained chemical reagents. The density of the aerogel can be conveniently fine-tuned by varying the concentration of the zinc oxide/hydroxide dispersion when frozen. The prepared zinc oxide/zinc hydroxide aerogel has a microscopic three-dimensional porous structure, micropores separated by curled and interconnected zinc oxide/zinc hydroxide nanosheets (with the thickness of less than 100 nm) are abundant, and the micropores are communicated with one another. In addition, the volume and shape of the aerogel can be conveniently and effectively adjusted by the volume of the flocculent dispersion liquid during freezing and the shape of a vessel used during freezing, for example, the zinc oxide/zinc hydroxide nanosheet dispersion liquid is concentrated to 4mL and then placed in a 5mL beaker for freeze drying to obtain the aerogel with the volume of 2.25cm3Cylindrical zinc oxide/hydroxide aerogels. Oxidation prepared by the inventionThe zinc/zinc hydroxide aerogel has quite large specific surface area and lower density, and has wide application prospect in the fields of capacitors, catalysis, biosensors, lithium ion batteries and the like.
Drawings
FIG. 1: optical photographs of different volumes of cylindrical zinc oxide/zinc hydroxide aerogels prepared in example 1;
FIG. 2: scanning electron micrographs of the zinc oxide/zinc hydroxide aerogel prepared in example 1;
FIG. 3: the X-ray diffraction pattern of the zinc oxide/zinc hydroxide aerogel prepared in example 1;
FIG. 4: example 1 experimental results of the zinc oxide/zinc hydroxide aerogel prepared in example 1 for photocatalytic degradation of organic dye (rhodamine);
FIG. 5: scanning electron micrographs and optical micrographs (inset) of the zinc oxide/zinc hydroxide aerogel prepared in example 2.
Detailed Description
The technical solution of the present invention is described in more detail with the following specific examples, but the examples are not to be construed as limiting the present invention.
Example 1
1) Preparing zinc oxide/zinc hydroxide nanosheets:
adding 1mL of 200mM sodium dodecyl sulfate solution, 4mL of 100mM hexamethylenetetramine solution and 4mL of 100mM zinc nitrate solution into 91mL deionized water, adding 10mg NaOH solid to adjust the pH value of the solution, uniformly mixing, placing at 90 ℃ for reaction for 2h, fully stirring during the reaction, wherein the stirring speed is 200rpm, and finally obtaining the suspension rich in zinc oxide/zinc hydroxide nanosheets. Taking out, airing at room temperature, cooling, centrifuging the suspension at the rotating speed of 3000rpm, taking out the precipitate, repeatedly washing with deionized water for 5 times, finally dispersing into 10mL of deionized water, standing, removing supernatant, and then remaining 5mL of flocculent zinc oxide/zinc hydroxide nanosheet dispersion. The dispersion was placed in a 5mL beaker and frozen in a freezer at-20 ℃ for 12h, and then dried in a vacuum freeze dryer at-50 ℃ for 24h to give a volume of about 2 each.7cm3、2.3cm3、3.6cm3、2.2cm3Zinc oxide/hydroxide aerogels. Accurately weighing their masses respectively 17.9mg, 14.8mg, 19.1mg and 12.6mg with a precision balance to obtain aerogel with density of 6.6mg/cm3、6.4mg/cm3、5.3mg/cm3、5.7mg/cm3。
FIG. 1 is an optical photograph of the resulting zinc oxide/zinc hydroxide aerogel in various shapes and volumes.
FIG. 2 is a scanning electron micrograph of the resulting zinc oxide/zinc hydroxide aerogel. As shown in the figure, the material has a three-dimensional loose porous structure in a large range, the zinc oxide/zinc hydroxide nano-sheets are curled and connected to form abundant cavities, the sizes of the cavities are mostly below 30 mu m, the shapes are fluffy and uniform, and the thickness of the zinc oxide/zinc hydroxide nano-sheets in the figure is below 0.1 mu m.
FIG. 3 is an X-ray diffraction pattern of the obtained zinc oxide/zinc hydroxide aerogel. As shown in the figure, diffraction characteristic peaks of (100), (002), (101), (102), (110), (103) and (112) of wurtzite zinc oxide are clearly visible, which indicates that the zinc oxide component in the prepared aerogel is in a wurtzite crystal form. Meanwhile, the diffraction peaks (distinguished by adding and zinc oxide) of (004), (005), (006) and (007) of the zinc hydroxide are sharp, which indicates that the material contains a certain amount of zinc hydroxide.
FIG. 4 is a graph showing the absorption of organic dye (rhodamine used to simulate organic pollutants in water) degraded by photocatalysis in the obtained zinc oxide/zinc hydroxide aerogel. As shown in the figure, the obtained zinc oxide aerogel completely catalyzes and degrades rhodamine within 3 hours, which shows that the prepared zinc oxide/zinc hydroxide aerogel has good performance in the aspect of photocatalytic degradation of organic pollutants.
Example 2
The procedure of example 1 was followed, and a 300mM sodium dodecyl sulfate solution (4 mL), a 200mM hexamethylenetetramine solution (8 mL) and a 200mM zinc nitrate solution (8 mL) were added to 80mL deionized water, followed by adjusting the pH with 20mg sodium hydroxide solid to obtain a zinc oxide/zinc hydroxide nanosheet precipitate having a mass of about 40mg. Further preparing zinc oxide/zinc hydroxide aerogel by the same method, wherein the prepared zinc oxide/zinc hydroxide aerogel is cylindrical and has a volume of 4.8cm3The density was 7.7mg/cm3。
FIG. 5 shows scanning electron micrographs and optical photographs (inset) of the zinc oxide/zinc hydroxide aerogel obtained in this example. As shown in the figure, the three-dimensional porous structure is shown in a large range, the pore walls are formed by curling and connecting zinc oxide/zinc hydroxide nano sheets, and the thickness of the sheet layer is below 0.1 mu m.
Example 3
The procedure is as in example 1, using potassium lauryl sulfate; the same method was further used to prepare zinc oxide/zinc hydroxide aerogels. The prepared zinc oxide/zinc hydroxide aerogel is cylindrical and has a volume of 3.0cm3Mass 19.5mg, density 6.5mg/cm3。
Example 4
The procedure of example 1 was followed, with zinc oxide/zinc hydroxide nanoplates dispersed in 20mL of deionized water at a concentration of about 0.5 mg/mL; the same method was further used to prepare zinc oxide/zinc hydroxide aerogels. The obtained zinc oxide/zinc hydroxide aerogel is cylindrical and has a volume of 3.7cm3The mass is 16.2mg, and the density is 4.4mg/cm3。
Example 5
The same procedure as in example 1 was followed, with the freezing temperature being-80 ℃ and the freezing time being 24 hours, to prepare a zinc oxide/zinc hydroxide aerogel. The zinc oxide/hydroxide aerogel prepared was cylindrical and had a volume of 3.1cm3The density was 5.3mg/cm3And the micropores are abundant.
Example 6
The same procedure as in example 1 was followed, except that the vacuum freeze-drying temperature was-80 ℃ and the freeze-drying time was 48 hours, to prepare a zinc oxide/zinc hydroxide aerogel. The prepared zinc oxide/zinc hydroxide aerogel is cylindrical and has a volume of 3.3cm3The density was 6.0mg/cm3The zinc oxide/zinc hydroxide nano-sheets are tightly connected and have abundant cavities.
Example 7
The same procedure as in example 1 was followed, except that the reaction temperature was 110 ℃, to prepare a zinc oxide/zinc hydroxide aerogel. The prepared zinc oxide/zinc hydroxide aerogel is cylindrical and has a volume of 3.3cm3The density was 6.6mg/cm3。
It should be understood that the above description of the preferred embodiments is given for clarity and not for any purpose of limitation, and that various alternatives, modifications and combinations will be apparent to those skilled in the art without departing from the scope of the invention as defined in the appended claims.
Claims (10)
1. A method for preparing a zinc oxide/hydroxide aerogel comprising the steps of:
1) preparation of zinc oxide/zinc hydroxide nanosheet
Adding 1-4 mL of 200-300 mM surfactant aqueous solution, 4-8 mL of 100-200 mM alkaline slow-release agent aqueous solution and 4-8 mL of 100-200 mM soluble zinc salt aqueous solution into deionized water to make the total volume 100mL, adding 10-20 mg of alkali solid into the mixed solution to adjust the pH value of the solution, fully dissolving and uniformly mixing, then placing at 90-110 ℃ to react for 1-3 h, fully stirring during the reaction, finally obtaining a suspension rich in zinc oxide/zinc hydroxide nanosheet, centrifuging at 3000-7000 rpm for 3-10 min, separating out a precipitate part, and obtaining the zinc oxide/zinc hydroxide nanosheet;
2) preparation of zinc oxide/zinc hydroxide nanosheet dispersion
Repeatedly cleaning the zinc oxide/zinc hydroxide nanosheet precipitate prepared in the step 1) with deionized water for purification, then adding the purified precipitate into deionized water, standing the obtained suspension for more than 12h to enable the zinc oxide/zinc hydroxide nanosheet to naturally settle in water to be flocculent, and removing the supernatant to obtain a zinc oxide/zinc hydroxide nanosheet dispersion liquid;
3) preparation of Zinc oxide/Zinc hydroxide aerogels
And (3) freezing the zinc oxide/zinc hydroxide nanosheet dispersion liquid prepared in the step 2) at a low temperature, and after the zinc oxide/zinc hydroxide nanosheet dispersion liquid is completely solidified, carrying out vacuum freeze drying to prepare the zinc oxide/zinc hydroxide aerogel.
2. A method of preparing a zinc oxide/hydroxide aerogel as claimed in claim 1, wherein: the surfactant used in the step 1) is one or a mixture of more of sodium dodecyl sulfate, sodium n-decyl sulfate, potassium dodecyl sulfate, sodium tetradecyl sulfate, sodium dodecyl polyoxyethylene ether sulfate and ammonium dodecyl sulfate.
3. A method of preparing a zinc oxide/hydroxide aerogel as claimed in claim 1, wherein: the alkaline slow-release agent used in the step 1) is hexamethylenetetramine or urea.
4. A method of preparing a zinc oxide/hydroxide aerogel as claimed in claim 1, wherein: the soluble zinc salt in the step 1) is one of zinc nitrate, zinc bromide, zinc chloride, zinc acetate or zinc sulfate.
5. A method of preparing a zinc oxide/hydroxide aerogel as claimed in claim 1, wherein: the molar ratio of the alkaline slow-release agent to the soluble zinc salt added in the step 1) is 1: 1.
6. a method of preparing a zinc oxide/hydroxide aerogel as claimed in claim 1, wherein: the alkali solid in the step 1) is sodium hydroxide, sodium carbonate or potassium hydroxide.
7. A method of preparing a zinc oxide/hydroxide aerogel as claimed in claim 1, wherein: the stirring speed in the step 1) is 150-300 rpm, and the concentration of the obtained zinc oxide/zinc hydroxide nanosheet suspension is 0.1-0.2 mg/mL.
8. A method of preparing a zinc oxide/hydroxide aerogel as claimed in claim 1, wherein: the concentration of the zinc oxide/zinc hydroxide nanosheet dispersion prepared after purification in the step 2) is 1-2 mg/mL.
9. A method of preparing a zinc oxide/hydroxide aerogel as claimed in claim 1, wherein: the freezing temperature in the step 3) is-20 ℃ to-80 ℃, and the time is 12-24 hours; the vacuum freeze drying temperature is-50 ℃ to-80 ℃, and the time is 24-48 hours.
10. A zinc oxide/zinc hydroxide aerogel is characterized in that: is prepared by the method of any one of claims 1 to 9.
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