CN113145091A - Nano composite photocatalytic material and preparation method thereof - Google Patents
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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Abstract
The invention relates to a nano composite photocatalytic material, which is mainly of a block structure formed by stacking a large number of spherical titanium dioxide particles; the spherical titanium dioxide particles comprise spherical titanium dioxide and a graphene coating layer coated on the surface of the spherical titanium dioxide; when the spherical titanium dioxide particles are stacked, a large number of internally and externally connected hole structures are formed; the spherical titanium dioxide particles are bonded together through the hanging bonds on the surface of the graphene. The invention aims to provide a nano composite photocatalytic material and a preparation method thereof, which have higher specific surface area, improve photocatalytic degradation efficiency and increase actual load capacity.
Description
Technical Field
The invention belongs to the technical field of nano composite materials and photocatalysis, and particularly relates to a nano composite photocatalytic material and a preparation method thereof.
Background
The photocatalytic material is an electron (e) on the valence band under the action of a certain light source-) A transition to the conduction band, a corresponding hole (h) being generated in the valence band+) Generated by havingSuperoxide ion free radical, hydroxyl free radical and superoxide hydroxyl free radical with extremely strong oxidation effect can oxidize and decompose toxic and harmful gas pollutants such as formaldehyde, benzene, toluene, xylene, ammonia, VOC, odor, bacteria and the like into harmless CO2And H2O, and has high-efficiency broad-spectrum disinfection performance, and has good inhibition and killing effects on various common pathogenic bacteria.
However, the photocatalytic material in the conventional sense has high quantum conversion efficiency only in the nanometer size, and the smaller the size of the nanomaterial is, the higher the photocatalytic efficiency is. For example, the degradation efficiency of P5 (average particle size of about 5nm) particles in solution for methyl blue is much better than that of P25 (average particle size of about 21nm, in mixed crystal form, anatase and rutile). However, the photocatalytic particles of P5 or smaller have no way of being used directly in air, they are suspended in air, and there is no way of blowing wind. Meanwhile, the traditional photocatalytic material is difficult to bond with other materials, has small reactive sites, increases the recombination probability of holes and electrons, has short service life and can only utilize ultraviolet light.
Graphene has a two-dimensional honeycomb-like crystal structure formed by close packing of single-layer carbon atoms. The unique and perfect structure of graphene enables the graphene to have excellent electrical, mechanical, thermal and optical properties. Because the surface of the graphene has a plurality of dangling bonds which can be well bonded with the photocatalytic material, the graphene has large specific surface area and high electron mobility, active points of reaction are increased, the combination of electrons and holes is reduced, the photocatalytic efficiency is improved, the band gap of the titanium dioxide photocatalytic material is narrowed due to the existence of the graphene, and the utilization rate of sunlight is increased. Therefore, the photocatalytic efficiency can be improved by effectively compounding the graphene and titanium dioxide photocatalytic materials. However, the specific surface area of the graphene and titanium dioxide composite photocatalytic material disclosed at present is limited, and in the practical application of air purification, the composite photocatalytic material needs to be loaded on a substrate for use, the load capacity of the substrate is limited, the contact area and the contact time of the air passing through the purification device once and the composite photocatalytic material on the substrate are limited, and the composite photocatalytic material cannot completely and rapidly degrade harmful substances such as bacteria and viruses in the air. Therefore, in order to widen the practical application of the composite photocatalytic material, a graphene and titanium dioxide composite photocatalytic material with a large specific surface area and higher photocatalytic efficiency still needs to be developed.
Disclosure of Invention
The invention aims to provide a nano composite photocatalytic material and a preparation method thereof, which have higher specific surface area, improve photocatalytic degradation efficiency and increase actual load capacity.
The purpose of the invention is realized by the following technical scheme:
a nano composite photocatalytic material is mainly a block structure formed by stacking a large number of spherical titanium dioxide particles; the spherical titanium dioxide particles comprise spherical titanium dioxide and a graphene coating layer coated on the surface of the spherical titanium dioxide; when the spherical titanium dioxide particles are stacked, a large number of internally and externally connected hole structures are formed; the spherical titanium dioxide particles are bonded together through the hanging bonds on the surface of the graphene.
Compared with the prior art, the invention has the advantages that:
(1) according to the nano composite photocatalytic material, the spherical titanium dioxide particles coated with the graphene on the surface are bonded and stacked to form a hole structure in a block structure, so that the composite photocatalytic material has a higher specific surface area. And because the shapes of the spherical titanium dioxide particles are not fixed and the sizes of the spherical titanium dioxide particles are different, more hole structures can be formed during stacking.
(2) In the practical application of air purification, the block structure and the high specific surface area of the nano composite photocatalytic material can effectively increase the load capacity of the nano composite photocatalytic material on the substrate, and meanwhile, the hole structure in the block structure enables air and ultraviolet light to enter the block structure, so that titanium dioxide particles can contact with more harmful substances such as bacteria and viruses in the air and kill the harmful substances in the air during photocatalytic air purification, and the photocatalytic efficiency is greatly improved. Verified by a third authority detection mechanism, the air purification system prepared by the nano composite photocatalytic material provided by the invention has a virus removal rate of 93.2% in 5 minutes and 99.94% in 10 minutes. The nano composite photocatalytic material provided by the invention is proved to have ultrahigh photocatalytic degradation efficiency, and the photocatalytic degradation efficiency of air passing through a purification device once is effectively improved, so that the application range of the composite photocatalytic material is further widened.
(3) The surfaces of the spherical titanium dioxide particles of the nano composite photocatalytic material are coated with a layer of graphene, so that the titanium dioxide particles can be stacked together through bonding, the bulk composite material with a proper size can be selected according to different practical application scenes, and meanwhile, the stability of the bulk structure formed by stacking the spherical titanium dioxide particles is effectively improved by the graphene.
Drawings
FIG. 1 is a schematic flow chart of a method for preparing a nano composite photocatalytic material according to the present invention.
FIG. 2 is an SEM photograph of the nano composite photocatalytic material provided by the present invention.
FIG. 3 is a schematic structural diagram of spherical titanium dioxide particles coated with graphene on the surface of the nano-composite photocatalytic material provided by the present invention.
Detailed Description
A nano composite photocatalytic material is mainly a block structure formed by stacking a large number of spherical titanium dioxide particles; the spherical titanium dioxide particles comprise spherical titanium dioxide and a graphene coating layer coated on the surface of the spherical titanium dioxide; when the spherical titanium dioxide particles are stacked, a large number of internally and externally connected hole structures are formed; the spherical titanium dioxide particles are bonded together through the hanging bonds on the surface of the graphene.
The shape and size of the spherical titanium dioxide particles are not fixed.
A process for preparing the nano-class composite photocatalytic material includes such steps as,
A. preparing a nitric acid solution;
B. preparing a butyl titanate solution;
C. preparing a graphene dispersion liquid;
D. preparing colloidal titanium dioxide solid by using the nitric acid solution prepared in the step A and the butyl titanate solution prepared in the step B;
E. d, placing the colloidal titanium dioxide solid prepared in the step D into an oil bath pot for heating, and adding the graphene dispersion liquid prepared in the step C to prepare spherical titanium dioxide particles;
F. and E, sintering the spherical titanium dioxide particles prepared in the step E at a high temperature to form a block structure.
The specific method of the step A comprises the steps of pouring pure water and absolute ethyl alcohol into a reaction container, mixing and stirring for 30-60min, adding nitric acid, and continuing mixing and stirring for 30-60 min.
The volume ratio of the pure water to the absolute ethyl alcohol is 1: (1-2); the volume ratio of the nitric acid to the absolute ethyl alcohol is 1: (8-10).
The concrete method of the step B is that the butyl titanate and the absolute ethyl alcohol are mixed and continuously stirred for 30-60 min; the volume ratio of the butyl titanate to the absolute ethyl alcohol is 1: (0.5-1).
The specific method of the step C comprises the steps of firstly putting absolute ethyl alcohol into a container, then adding graphene, and then putting the container into an ultrasonic cleaning machine for ultrasonic dispersion for 30-60 min;
0.02-0.03g of graphene is added into each 100ml of absolute ethyl alcohol.
The concrete method of the step D is that the butyl titanate solution prepared in the step B is slowly added into the reaction vessel containing the nitric acid solution prepared in the step A at the adding speed of 150-250ml/min, and the stirring is continued to ensure that the color of the mixed solution is gradually changed from transparent color to light blue color so as to form the colloidal titanium dioxide solid.
And E, heating the reaction vessel containing the colloidal titanium dioxide solid prepared in the step D at the temperature of 100-120 ℃ in an oil bath to dissolve the colloidal titanium dioxide solid to obtain milky white liquid, adding the graphene dispersion liquid prepared in the step C, stirring by a stirrer to uniformly disperse the graphene into the milky white liquid, and continuously heating and stirring until the solution in the reaction vessel is completely evaporated to obtain spherical titanium dioxide particle powder with the surface coated with a layer of graphene.
And F, putting the spherical titanium dioxide particle powder into a high-temperature muffle furnace to be sintered for 2-4h at the temperature of 410-430 ℃, and bonding and stacking the spherical titanium dioxide particles together by utilizing the suspension bond of the graphene under the action of the graphene to form a block structure with a large number of internally and externally connected hole structures. The forming mechanism of the nano composite photocatalytic material provided by the invention is as follows: 1) in the process of preparing the nitric acid solution, the absolute ethyl alcohol is added into the pure water, so that the decomposition rate of the butyl titanate in the adding process is effectively inhibited; 2) the butyl titanate is slowly hydrolyzed under the combined action of the absolute ethyl alcohol and the nitric acid to form titanium dioxide spherical particles. The nitric acid effectively suppresses the rate of hydrolysis of the butyl titanate while also promoting the formation of spherical titanium dioxide particles. 3) In the high-temperature sintering process, spherical titanium dioxide particles are bonded and stacked together by utilizing a dangling bond on the surface of graphene, so that the nano composite photocatalytic material with a block structure, wherein the interior of the nano composite photocatalytic material contains a plurality of spherical titanium dioxide particles with the surface coated with graphene and a plurality of internal and external connected hole structures, is formed.
The invention is described in detail below with reference to the drawings and examples of the specification:
fig. 1 to fig. 3 are schematic diagrams of an embodiment of a nano composite photocatalytic material and a preparation method thereof provided by the invention.
The invention provides a nano composite photocatalytic material, as shown in figures 2 and 3, a block structure 1 is formed by stacking a plurality of spherical titanium dioxide particles 11 with surfaces coated with graphene; the block structure 1 also comprises a plurality of internally and externally connected hole structures 12 formed by mutually stacking spherical titanium dioxide particles 11 with surfaces coated with graphene; the spherical titanium dioxide particles 11 with the surfaces coated with the graphene comprise inner-layer spherical titanium dioxide 11-2 and outer-layer graphene coating layers 11-1; the shape of the spherical titanium dioxide particles 11 coated with the graphene on the surface is not fixed, the spherical titanium dioxide particles 11 coated with the graphene on the surface are different in size, and the spherical titanium dioxide particles 11 coated with the graphene on the surface are bonded together through the hanging bonds on the surface of the graphene 11-1.
As shown in FIG. 1, the preparation process of the nano composite photocatalytic material provided by the invention comprises the following steps:
s01, preparing a nitric acid solution
Pouring 250ml of pure water and 250ml of absolute ethyl alcohol into a reactor, stirring for 30min, uniformly mixing, adding 30ml of nitric acid, and continuously mixing and stirring for 30min to obtain a nitric acid solution.
S02, preparing butyl titanate solution
500ml of butyl titanate and 250ml of absolute ethanol were mixed and stirred continuously for 30min to obtain a butyl titanate solution.
S03, preparing graphene dispersion liquid
Firstly, 100ml of absolute ethyl alcohol is put into a beaker, then 0.0254g of graphene is added, and finally the beaker is put into an ultrasonic cleaning machine for ultrasonic dispersion for 30min to obtain graphene dispersion liquid.
S04, preparing colloidal titanium dioxide solid
Slowly adding the butyl titanate solution prepared in the step S02 into the nitric acid solution in the reactor at the adding speed of 200ml/min, continuously stirring to gradually change the color of the mixed solution from transparent to light blue, slowly hydrolyzing the butyl titanate under the combined action of the absolute ethyl alcohol and the nitric acid, and forming colloidal titanium dioxide solid;
s05, preparing spherical titanium dioxide particles
Heating the reactor in an oil bath at 110 ℃ to dissolve colloidal titanium dioxide solids to obtain milky white liquid, adding the graphene dispersion liquid prepared in the step S03, stirring the mixture by a stirrer to uniformly disperse the graphene into the milky white liquid, and continuously heating and stirring until the solution in the reactor is completely evaporated to obtain spherical titanium dioxide particle powder with the surface coated with a layer of graphene;
s06, high-temperature sintering, wherein spherical titanium dioxide particles are stacked to form a block structure;
and (4) placing the spherical titanium dioxide particle powder prepared in the step (S05) into a high-temperature muffle furnace, sintering at the temperature of 420 ℃ for 2h, and bonding and stacking the spherical titanium dioxide particles together by utilizing the dangling bonds of the graphene under the action of the graphene to form the composite photocatalytic material with a block structure with a plurality of internally and externally connected holes.
The photocatalytic efficiency detection and practical application conditions of the nano composite photocatalytic material are as follows:
the nano composite photocatalytic material provided by the invention is adhered and loaded on a plastic substrate through glue to form a photocatalytic module, the photocatalytic module and an ultraviolet lamp are combined to form a photocatalytic module, the photocatalytic module is installed in an air purifier case to assemble an air purification system, the air purification system is sent to a third party authoritative detection mechanism to carry out killing efficiency detection on bacteria, viruses and the like, and the detection results are shown in the following table 1:
table 1:
the above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (11)
1. A nano composite photocatalytic material is characterized in that: it is mainly a block structure formed by stacking a large number of spherical titanium dioxide particles; the spherical titanium dioxide particles comprise spherical titanium dioxide and a graphene coating layer coated on the surface of the spherical titanium dioxide; when the spherical titanium dioxide particles are stacked, a large number of internally and externally connected hole structures are formed; the spherical titanium dioxide particles are bonded together through the hanging bonds on the surface of the graphene.
2. The nano-composite photocatalytic material according to claim 1, characterized in that: the shape and size of the spherical titanium dioxide particles are not fixed.
3. A method for preparing the nano composite photocatalytic material as recited in claim 1 or 2, wherein: the steps of the method are as follows,
A. preparing a nitric acid solution;
B. preparing a butyl titanate solution;
C. preparing a graphene dispersion liquid;
D. preparing colloidal titanium dioxide solid by using the nitric acid solution prepared in the step A and the butyl titanate solution prepared in the step B;
E. d, placing the colloidal titanium dioxide solid prepared in the step D into an oil bath pot for heating, and adding the graphene dispersion liquid prepared in the step C to prepare spherical titanium dioxide particles;
F. and E, sintering the spherical titanium dioxide particles prepared in the step E at a high temperature to form a block structure.
4. The method for preparing the nano composite photocatalytic material according to claim 3, wherein the method comprises the following steps: the specific method of the step A comprises the steps of pouring pure water and absolute ethyl alcohol into a reaction container, mixing and stirring for 30-60min, adding nitric acid, and continuing mixing and stirring for 30-60 min.
5. The method for preparing the nano composite photocatalytic material according to claim 4, wherein the method comprises the following steps: the volume ratio of the pure water to the absolute ethyl alcohol is 1: (1-2); the volume ratio of the nitric acid to the absolute ethyl alcohol is 1: (8-10).
6. The method for preparing the nano composite photocatalytic material according to claim 3, wherein the method comprises the following steps: the concrete method of the step B is that the butyl titanate and the absolute ethyl alcohol are mixed and continuously stirred for 30-60 min; the volume ratio of the butyl titanate to the absolute ethyl alcohol is 1: (0.5-1).
7. The method for preparing the nano composite photocatalytic material according to claim 3, wherein the method comprises the following steps: and C, putting absolute ethyl alcohol into a container, adding graphene, and putting the container into an ultrasonic cleaning machine for ultrasonic dispersion for 30-60 min.
8. The method for preparing the nano composite photocatalytic material according to claim 7, wherein the method comprises the following steps: 0.02-0.03g of graphene is added into each 100ml of absolute ethyl alcohol.
9. The method for preparing the nano composite photocatalytic material according to claim 3, wherein the method comprises the following steps: the concrete method of the step D is that the butyl titanate solution prepared in the step B is slowly added into the reaction vessel containing the nitric acid solution prepared in the step A at the adding speed of 150-250ml/min, and the stirring is continued to ensure that the color of the mixed solution is gradually changed from transparent color to light blue color so as to form the colloidal titanium dioxide solid.
10. The method for preparing the nano composite photocatalytic material according to claim 3, wherein the method comprises the following steps: and F, putting the spherical titanium dioxide particle powder into a high-temperature muffle furnace to be sintered for 2-4h at the temperature of 410-430 ℃, and bonding and stacking the spherical titanium dioxide particles together by utilizing the suspension bond of the graphene under the action of the graphene to form a block structure with a large number of internally and externally connected hole structures.
11. The method for preparing a nano composite photocatalytic material according to any one of claims 3 to 10, wherein: and E, heating the reaction vessel containing the colloidal titanium dioxide solid prepared in the step D at the temperature of 100-120 ℃ in an oil bath to dissolve the colloidal titanium dioxide solid to obtain milky white liquid, adding the graphene dispersion liquid prepared in the step C, stirring by a stirrer to uniformly disperse the graphene into the milky white liquid, and continuously heating and stirring until the solution in the reaction vessel is completely evaporated to obtain spherical titanium dioxide particle powder with the surface coated with a layer of graphene.
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| CN114618466A (en) * | 2020-12-08 | 2022-06-14 | 福建新峰二维材料科技有限公司 | Nano composite photocatalytic material and preparation method thereof |
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