CN111013582A - Nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde and preparation method thereof - Google Patents
Nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde and preparation method thereof Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/48—Silver or gold
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/34—Chemical or biological purification of waste gases
- B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
- B01D53/86—Catalytic processes
- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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- B01D2255/802—Photocatalytic
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention discloses a nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde and a preparation method thereof, belonging to the field of nano materials and the field of photocatalysis. The invention uses titanium sulfate (Ti (SO)4)2) And sodium hydroxide (NaOH) is used as a raw material, titanium dioxide nano particles with the size of about 10nm are prepared by a gradual coprecipitation method, nano graphene is compounded, and the proportion of titanium dioxide, graphene and auxiliary materials is adjusted, fully mixed and quantified to form the nano titanium dioxide-graphene composite photocatalyst. The photocatalyst has high photocatalytic activity and shows excellent air purification and formaldehyde photocatalytic degradation capabilities.
Description
Technical Field
The invention belongs to the technical field of nano materials and photocatalytic materials, and particularly relates to a nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde and a preparation method thereof.
Background
With the social development and the improvement of the living standard of human beings, environmental pollution is more and more concerned by people. The results of World Health Organization (WHO) surveys indicate that harmful gases are found in 30% of new building structures in the world, and that these toxic indoor air have resulted in an increase in worldwide population morbidity and mortality, and that indoor air pollution is therefore one of the five environmental factors that endanger public health.
Formaldehyde is an organic substance with stronger volatility, has higher toxicity, is one of main air pollutants in an indoor closed environment, and is mainly derived from wood materials, floor materials, coatings and the like. The formaldehyde has pungent odor, can be smelled at low concentration, and the olfaction threshold of human on the formaldehyde is usually 0.06-0.07 mg/m3. Formaldehyde is classified as teratogenic and carcinogenic substance by the world health organization, has strong stimulation effect on eyes, respiratory tract and skin, can be combined with amino acid in protein to denature the protein, and can react with ionic chloride in the air to generate a carcinogenic substance, namely dichloroformaldehyde ether. People who have formaldehyde in contact with formaldehyde for a long time can cause cancers of nasal cavities, oral cavities, nasopharynx, throats, skins and digestive tracts, and have a greater toxic effect on newborns, infants and old people.
The formaldehyde has low price and good chemical reaction activity, so the formaldehyde is widely used in industrial production. Formaldehyde is mainly used as a binder in the process of industrial synthesis of urea-formaldehyde resin, melamine-formaldehyde resin, phenolic resin and the like. Therefore, formaldehyde is always used and released in the link of using a large amount of adhesive. Common formaldehyde removal methods include physical adsorption, biological methods, ozone oxidation, plant degradation, catalytic oxidation and the like, and in contrast, the ozone oxidation method easily causes secondary pollution and has a limited removal effect.
The photocatalytic technology is the air purification technology with the greatest application prospect due to the outstanding characteristics of simple operation, mild conditions, low energy consumption, no secondary pollution and the like, wherein the nanometer titanium dioxide semiconductor becomes a research hotspot of many photocatalysts due to the advantages of good chemical stability, corrosion resistance, high activity, low price, no toxicity, no secondary pollution and the like. However, the band gap of titanium dioxide is wide, and only a small amount of ultraviolet light can be absorbed and utilized, so that the application prospect of titanium dioxide is limited.
The invention patent (application number 201010240649) and the invention patent (200910303193) propose that tetrabutyl titanate is used as a titanium source, and a sol-gel method is adopted to prepare the nano titanium dioxide, but the reaction conditions are complex, the difficulty of the production and preparation process is increased, the generated waste is difficult to treat, and the industrial production is difficult to realize. The invention patent (application No. 201210262371) provides a method for preparing titanium dioxide particles with a particle size of about 10nm by adding oleylamine as a surfactant in a solvothermal system. But the whole process has various raw materials, complex process and higher cost.
The invention mainly takes titanium sulfate and sodium hydroxide as raw materials, prepares titanium dioxide nano particles with the size of about 10nm by a gradual coprecipitation method, and has the advantages of few raw materials and simple operation flow. Through the compounding of the nano titanium dioxide and the graphene, the absorption capacity of visible light is increased, and the utilization rate of active ingredients to natural light can be improved. The auxiliary material contains a penetrating agent and noble metal Ag+The adhesive bonding capability of the photocatalyst and the wood material can be obviously enhanced, and the sterilization effect is improved.
Disclosure of Invention
The invention mainly provides a nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde and a preparation method thereof. The method is simple to operate, low in cost and suitable for large-scale production. The produced nano titanium dioxide-graphene composite photocatalyst has high catalytic degradation activity on indoor air pollutants (formaldehyde).
The purpose of the invention is realized by the following technical scheme:
a nano titanium dioxide-graphene composite photocatalyst for efficiently degrading formaldehyde mainly comprises an active material, an auxiliary material and deionized water, wherein the main active material is a nano titanium dioxide-graphene composite material.
A preparation method of a nano titanium dioxide-graphene composite photocatalyst for efficiently degrading formaldehyde comprises the following specific steps:
s1, preparing nano titanium dioxide, preparing a titanium sulfate solution and a sodium hydroxide solution with proper concentrations, dropwise adding the titanium sulfate solution into the sodium hydroxide solution at a corresponding temperature, violently stirring to obtain a white flocculent product F1, adjusting the pH value of the white flocculent F1 to be neutral (pH is 7) through the titanium sulfate solution or the sodium hydroxide solution, standing, layering, washing by a suction filtration method until sulfate ions are cleaned, and washing to obtain the nano titanium dioxide F2;
s2, compounding nano titanium dioxide and graphene, compounding the nano titanium dioxide F2 obtained in the step S1 and the graphene, and adding deionized water to prepare an active ingredient stock solution Y1;
s3, preparing a photocatalyst stock solution Y2, and proportioning the active ingredient stock solution Y1 obtained in the step S2 and auxiliary materials to obtain the photocatalyst stock solution Y2;
s4, preparing the nano titanium dioxide-graphene composite photocatalyst, and proportioning the photocatalyst stock solution Y2 obtained in the step S3 and deionized water to obtain the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde.
Preferably, the concentration of the titanium sulfate solution in the step S1 is 2.4-96 g/L, the concentration of the sodium hydroxide solution is 0.4-16 g/L, and the temperature in the synthesis process is-30-60 ℃.
Preferably, in step S1, the supernatant of the solution washed by the suction filtration method is subjected to barium nitrate solution to detect whether sulfate ions are washed.
Preferably, the graphene in step S2 includes graphene, graphene oxide, and graphene oxide-reduced.
Preferably, in the step S2, the composite mass ratio of the nano titanium dioxide F2 to the graphene is 1: 0.1-0.001, and the addition amount of the deionized water is 10 mL-11 mL.
Preferably, the auxiliary materials in step S3 mainly include plant extract essence, penetrant, and noble metal Ag + solution.
Preferably, the volume ratio of the active ingredient stock solution Y1 to the auxiliary materials in the step S3 is as follows: the active ingredient stock solution Y1, the plant extract essence, the penetrating agent and the noble metal Ag + solution are respectively 1: 0.00001-0.1: 0.00001-1: 0.01.
Preferably, the volume ratio of the photocatalyst stock solution Y2 to the deionized water in the step S4 is 1: 1-1000.
Compared with the prior art, the nano titanium dioxide-graphene composite photocatalyst for efficiently degrading formaldehyde and the preparation method thereof have the following beneficial effects:
1. the invention uses titanium sulfate and sodium hydroxide as raw materials, prepares titanium dioxide nano particles with the size of about 10nm by a gradual coprecipitation method, and has simple and effective operation method.
2. According to the invention, through the compounding of the nano titanium dioxide and the graphene, the absorption capacity of visible light is increased, and the utilization rate of active ingredients to natural light can be improved.
3. The auxiliary materials of the invention comprise a penetrating agent and noble metal Ag+The adhesive bonding capability of the photocatalyst and the wood material can be obviously enhanced, and the sterilization effect is improved.
4. The invention mainly utilizes the high-efficiency photocatalytic reaction of the active components of the photocatalyst to effectively convert indoor harmful gas pollutants (such as formaldehyde, benzene and the like), the active components have certain visible light absorption capacity, can effectively utilize natural light to carry out the photocatalytic reaction, and are different from main formaldehyde removal products (such as activated carbon and the like) in the market in essence in removing formaldehyde through adsorption.
Drawings
FIG. 1 is an SEM photograph of nano titanium dioxide;
FIG. 2 is a TEM photograph of nano-titania;
fig. 3 is a TEM photograph of the nano titanium dioxide-graphene composite.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the scope of the present invention is not limited thereto.
A nanometer titanium dioxide-graphene composite photocatalyst for efficiently degrading formaldehyde mainly comprises an active material, auxiliary materials and deionized water, wherein the main active material is the nanometer titanium dioxide-graphene composite material, and the nanometer titanium dioxide-graphene composite photocatalyst is mainly used for air purification and organic pollutant degradation in closed spaces such as indoor spaces, vehicle interiors and the like, and is especially used for degrading formaldehyde.
Specifically, the invention relates to a nano titanium dioxide-graphene composite photocatalyst for efficiently degrading formaldehyde, which utilizes the high-efficiency photocatalytic reaction of the active ingredients of the photocatalyst to effectively convert indoor harmful gas pollutants (such as formaldehyde, benzene and the like), the active ingredients have certain visible light absorption capacity, can effectively utilize natural light to carry out photocatalytic reaction, and are different from main formaldehyde removal products (such as activated carbon and the like) in the market in essence in removing formaldehyde through adsorption.
A preparation method of a nano titanium dioxide-graphene composite photocatalyst for efficiently degrading formaldehyde comprises the following specific steps:
s1, preparing nano titanium dioxide, preparing a titanium sulfate solution with the concentration of 2.4-96 g/L and a sodium hydroxide solution with the concentration of 0.4-16 g/L, dropwise adding the titanium sulfate solution into the sodium hydroxide solution at the temperature of-30-60 ℃, vigorously stirring to obtain a white flocculent product F1, adjusting the pH value of the white flocculent F1 to be neutral (pH is 7) through the titanium sulfate solution or the sodium hydroxide solution, standing for layering, washing by a suction filtration method until sulfate ions are washed (taking supernatant to detect through a barium nitrate solution), and washing to obtain the nano titanium dioxide F2;
s2, compounding nano titanium dioxide and graphene, compounding the nano titanium dioxide F2 obtained in the step S1 and the graphene in a compounding mass ratio of 1: 0.1-0.001, and adding 10-11 mL of deionized water to prepare an active ingredient stock solution Y1;
s3, preparing a photocatalyst stock solution Y2, and proportioning the active ingredient stock solution Y1 obtained in the step S2 and auxiliary materials, wherein the auxiliary materials mainly comprise plant extraction essence, a penetrating agent and a precious metal Ag + solution, and the volume ratio of the active ingredient stock solution Y1 to the auxiliary materials is as follows: the active ingredient stock solution Y1, the plant extract essence, the penetrating agent and the noble metal Ag + solution are respectively 1: 0.00001-0.1: 0.00001-1: 0.01, and finally the photocatalyst stock solution Y2 is obtained;
s4, preparing the nano titanium dioxide-graphene composite photocatalyst, and mixing the photocatalyst stock solution Y2 obtained in the step S3 with deionized water according to the volume ratio of 1: 1-1000 to obtain the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde.
Specifically, the graphene in step S2 includes graphene, graphene oxide, and graphene oxide. Specifically, the photocatalyst is prepared by adjusting the concentration of a titanium sulfate solution, the concentration of a sodium hydroxide solution, the temperature of a synthesis process, the proportion of each component and the total concentration through the examples, and is specifically shown in the following table. And testing the formaldehyde removal performance according to GB// T16129.
Table 1 examples 1-7: the concentration of titanium sulfate and sodium hydroxide and the temperature in the synthesis process are adjusted to prepare the nano titanium dioxide. (the ratio of the redox graphene is 0.01, the ratio of the plant extract essence is 0.0001, the ratio of the penetrating agent is 0.0001, and the noble metal Ag is+Ratio 0.1, deionized water ratio 100)
| Example sample | Ti(SO4)2Solution g/L | NaOH solution g/L | Synthesis temperature (. degree.C.) | Formaldehyde degradation rate (%) |
| Example 1 | 2.4 | 0.4 | 10 | 93％ |
| Example 2 | 12 | 2 | -20 | 96％ |
| Example 3 | 12 | 2 | 10 | 98％ |
| Example 4 | 12 | 2 | 60 | 91％ |
| Example 5 | 24 | 4 | 10 | 88％ |
| Example 6 | 48 | 8 | 10 | 86％ |
| Example 7 | 96 | 16 | 10 | 86％ |
Table 2 examples 8-11: on the basis of example 3, the type of graphene and the ratio of nano titanium dioxide to graphene are adjusted. (plant extract essence ratio is 0.0001)Penetrant ratio of 0.0001, noble metal Ag+Ratio 0.1, deionized water ratio 100)
Table 3 examples 12-20: on the basis of example 3, the composition ratio was adjusted.
| Example sample | Plant extract essence | Penetrant | Noble metal Ag+ | Deionized water | Formaldehyde degradation rate (%) |
| Example 12 | 0.0001 | 0.01 | 0.01 | 100 | 95％ |
| Example 13 | 0.0001 | 0.1 | 0.01 | 100 | 92％ |
| Example 14 | 0.00001 | 0.001 | 0.1 | 100 | 97％ |
| Example 15 | 0.001 | 0.0001 | 0.1 | 100 | 97％ |
| Example 16 | 0.0001 | 0.0001 | 1 | 100 | 96％ |
| Example 17 | 0.0001 | 0.0001 | 0.01 | 100 | 96％ |
| Example 18 | 0.0001 | 0.0001 | 0.1 | 1 | 55％ |
| Example 19 | 0.0001 | 0.0001 | 0.1 | 10 | 70％ |
| Example 20 | 0.0001 | 0.0001 | 0.1 | 1000 | 73％ |
| Example 3 | 0.0001 | 0.0001 | 0.1 | 100 | 98％ |
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (9)
1. A nanometer titanium dioxide-graphene composite photocatalyst for efficiently degrading formaldehyde is characterized in that: the composite material mainly comprises an active material, an auxiliary material and deionized water, wherein the main active material is a nano titanium dioxide-graphene composite material.
2. A preparation method of a nano titanium dioxide-graphene composite photocatalyst for efficiently degrading formaldehyde is characterized by comprising the following steps: the method comprises the following specific steps:
s1, preparing nano titanium dioxide, preparing a titanium sulfate solution and a sodium hydroxide solution with proper concentrations, dropwise adding the titanium sulfate solution into the sodium hydroxide solution at a corresponding temperature, violently stirring to obtain a white flocculent product F1, adjusting the pH value of the white flocculent F1 to be neutral (pH is 7) through the titanium sulfate solution or the sodium hydroxide solution, standing, layering, washing by a suction filtration method until sulfate ions are cleaned, and washing to obtain the nano titanium dioxide F2;
s2, compounding nano titanium dioxide and graphene, compounding the nano titanium dioxide F2 obtained in the step S1 and the graphene, and adding deionized water to prepare an active ingredient stock solution Y1;
s3, preparing a photocatalyst stock solution Y2, and proportioning the active ingredient stock solution Y1 obtained in the step S2 and auxiliary materials to obtain the photocatalyst stock solution Y2;
s4, preparing the nano titanium dioxide-graphene composite photocatalyst, and proportioning the photocatalyst stock solution Y2 obtained in the step S3 and deionized water to obtain the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde.
3. The preparation method of the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde according to claim 2, which is characterized by comprising the following steps: in the step S1, the concentration of the titanium sulfate solution is 2.4-96 g/L, the concentration of the sodium hydroxide solution is 0.4-16 g/L, and the temperature in the synthesis process is-30-60 ℃.
4. The preparation method of the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde according to claim 2, which is characterized by comprising the following steps: in step S1, the supernatant of the solution washed by the suction filtration method is collected and washed with barium nitrate solution to detect whether sulfate ions are washed.
5. The preparation method of the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde according to claim 2, which is characterized by comprising the following steps: in the step S2, the graphene includes graphene, graphene oxide, and graphene oxide-reduced.
6. The preparation method of the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde according to claim 2, which is characterized by comprising the following steps: in the step S2, the composite mass ratio of the nano titanium dioxide F2 to the graphene is 1: 0.1-0.001, and the addition amount of deionized water is 10-11 mL.
7. The preparation method of the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde according to claim 2, which is characterized by comprising the following steps: in the step S3, the auxiliary materials mainly comprise plant extract essence, penetrant and noble metal Ag + solution.
8. The method for preparing the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde according to claim 7, is characterized by comprising the following steps: the volume ratio of the active ingredient stock solution Y1 to the auxiliary materials in the step S3 is 1: 0.00001-0.1: 0.00001-1: 0.01.
9. The preparation method of the nano titanium dioxide-graphene composite photocatalyst capable of efficiently degrading formaldehyde according to claim 2, which is characterized by comprising the following steps: in step S4, the volume ratio of the photocatalyst stock solution Y2 to deionized water is 1: 1-1000.
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