CN111359582A - Graphene composite aerogel formaldehyde-removing material and preparation method thereof - Google Patents
Graphene composite aerogel formaldehyde-removing material and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 139
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 134
- 239000002131 composite material Substances 0.000 title claims abstract description 79
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- YONPGGFAJWQGJC-UHFFFAOYSA-K titanium(iii) chloride Chemical compound Cl[Ti](Cl)Cl YONPGGFAJWQGJC-UHFFFAOYSA-K 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims description 52
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- 239000000243 solution Substances 0.000 claims description 35
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- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims description 11
- 239000002244 precipitate Substances 0.000 claims description 11
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 claims description 10
- 238000000464 low-speed centrifugation Methods 0.000 claims description 10
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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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
- B01D53/02—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 by adsorption, e.g. preparative gas chromatography
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Abstract
The invention relates to the field of purification, and particularly relates to a graphene composite aerogel formaldehyde-removing material and a preparation method thereof. Preparing graphene oxide, preparing a graphene oxide aqueous solution, adding nano silver-titanium dioxide composite microspheres prepared by taking nano silver and titanium trichloride as raw materials, adding a reducing agent, uniformly mixing, pouring into a mould, freeze-drying, and removing water by freeze-drying to obtain the graphene composite aerogel formaldehyde-removing material. According to the method, the nano-silver-titanium dioxide composite microspheres and the graphene aerogel have synergistic effects, the graphene aerogel is excellent in adsorption performance, the nano-silver-titanium dioxide composite microspheres can completely degrade adsorbed formaldehyde under the photocatalysis effect, the defects that the graphene material is low in adsorption capacity and cannot completely degrade organic pollutants and the like are fundamentally overcome, and meanwhile, the production process is simple, the air purification efficiency is high, and the application prospect is good.
Description
Technical Field
The invention relates to the field of purification, in particular to a preparation method of a formaldehyde removing material, and especially relates to a graphene composite aerogel formaldehyde removing material and a preparation method thereof.
Background
In recent years, the problem of air pollution is always a problem to be solved urgently by governments. The flue gas released by burning fossil fuel (coal, petroleum, natural gas, etc.) in energy, chemical, metallurgy, traffic, etc. industries contains a great deal of SO2And NOxCausing serious pollution to the atmosphere. In addition, various dusts generated by human activities, solid suspended particles such as sand dust caused by climate deterioration, and the like pollute the ambient air, and volatile organic pollutants from various decorative materials and oral chemicals increasingly enter residences and public buildings, so that the degree of pollution of human living environment is increased sharply.
In order to meet the requirements of people on air quality, various types of air purifiers appear in the market, most of the air purifiers adopt porous materials such as activated carbon and the like to adsorb harmful gases in the air, but the adsorption capacity of the activated carbon of an adsorption material is limited, and a pollutant penetration phenomenon can occur after the adsorption is saturated. The photocatalytic technology is also used for degrading organic matters such as formaldehyde in the air, or a negative ion generator is used for generating negative oxygen ions to improve the air quality. However, these products are either costly or have poor air purification. Graphene is a two-dimensional sp2The hybrid carbon material and the graphene material have a large specific surface area, good mechanical strength and other excellent properties. The graphene material can be mixed with organic dirtThe dye produces strong complex reaction, plays a good role in adsorption, can directly kill bacteria, and fundamentally treats air pollution, so that the air purification technology combining the unique structure and chemical property of graphene with the filtering technology also becomes a new king brand for air treatment.
Chinese patent application No. 201810078703.4 discloses a graphene-based indoor air purifier filter screen and a preparation method thereof. The graphene-based indoor air purifier filter screen comprises an activated carbon fiber filter screen, a glass fiber net layer, a nylon net layer, a graphene coating metal net and a filter screen supporting frame, wherein the nylon net layer is arranged on the filter screen supporting frame, the glass fiber net layer is arranged on the nylon net layer, the activated carbon fiber net layer is arranged on the glass fiber net layer, the graphene coating metal net is arranged on the activated carbon fiber net layer, and a graphene layer is sprayed on the graphene coating metal net.
The Chinese patent application No. 201310304050.4 discloses a macroscopic preparation method of a macroscopic three-dimensional graphene aerogel adsorption material for indoor air purification, and belongs to the technical field of indoor air purification. According to the invention, polyethyleneimine and graphite oxide are used as raw materials, the polyethyleneimine is used for guiding the assembly of graphene, and a freeze-drying method is adopted to obtain the three-dimensional graphene aerogel. The invention adopts a mild solution method, and the synthesis method has the advantages of low cost, environmental protection, simplicity and feasibility, easy control, capability of macro preparation and the like, and is suitable for industrial large-scale production.
The Chinese patent application No. 201810068814.7 discloses a preparation method of a graphene aerogel air purification filter screen, wherein a graphene oxide solution is diluted by a solvent; adding a reducing agent into the obtained graphene oxide solution, adding the reducing agent according to the mass ratio of the graphene oxide to the reducing agent of 10: 1-1: 100, and then stirring for 10-600 min or performing ultrasonic treatment for 10-600 min until the mixture is uniformly mixed; quantitatively adding the obtained mixed solution into a mold, then putting the mold into a water bath kettle, heating to 50-100 ℃, and preserving heat for 1-6 hours to obtain graphene hydrogel; and removing water contained in the graphene hydrogel by a freeze drying method to obtain the porous graphene aerogel air purification filter screen.
The Chinese patent application No. 201810423105.6 discloses a porous graphene-based air purifying agent, which is prepared from the following components, by weight, 3-12 parts of organic titanate, 0.1-1 part of soluble metal salt, 1-3 parts of a silane coupling agent, 5-8 parts of graphene oxide, 3-8 parts of oxometallate, 1-12 parts of melamine, 1-5 parts of a foaming agent, 80-150 parts of polypropylene resin, 2-10 parts of inorganic acid and 10-50 parts of a solvent.
According to the above, the graphene composite material for air purification in the existing scheme has the defects of small filtration capacity, capability of adsorbing organic volatile gases such as formaldehyde and the like, incapability of thoroughly degrading organic pollutants and the like.
Disclosure of Invention
Aiming at the defects that the existing graphene air purification material with wider application is low in filtering capacity and can not thoroughly degrade organic pollutants such as formaldehyde, the invention provides the graphene composite aerogel formaldehyde removal material and the preparation method, so that the adsorption performance and the catalytic degradation capability of the graphene air purification material are effectively improved.
In order to achieve the purpose, the invention relates to the following specific technical scheme:
a preparation method of a graphene composite aerogel formaldehyde-removing material comprises the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 0.5-1 h in an ice water bath, heating to 50-60 ℃, stirring and reacting for 12-13 h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 15-20%, mixing and stirring under a light-shielding condition, then transferring to a hydrothermal reaction kettle, heating to perform hydrothermal reaction, performing low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres;
(4) and (3) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring into a mold, and freeze-drying to remove moisture to prepare the graphene composite aerogel formaldehyde-removing material.
The concentrated sulfuric acid is a sulfuric acid solution with the mass fraction of more than or equal to 70%; ice water refers to a mixture of ice and water at 0 ℃ (zero degrees centigrade) at one standard atmosphere.
Preferably, in the step (1), 8-10 parts by weight of natural graphite, 10-15 parts by weight of concentrated sulfuric acid, 2-3 parts by weight of phosphoric acid, 25-30 parts by weight of potassium permanganate, 35-50 parts by weight of ice water and 5-7 parts by weight of hydrogen peroxide.
Preferably, in the step (2), 20-40 parts by weight of graphene oxide and 60-80 parts by weight of deionized water.
Preferably, the rotation speed of the mixing and stirring under the dark condition in the step (3) is 200-300 r/min, and the time is 20-30 min.
Preferably, the temperature of the hydrothermal reaction in the step (3) is 180-190 ℃ and the time is 24-25 h.
Preferably, in the step (3), 8-14 parts by weight of nano silver, 31-42 parts by weight of deionized water and 50-55 parts by weight of a titanium trichloride solution.
Preferably, the reducing agent in step (4) is hydrazine hydrate.
Preferably, the temperature of the freeze drying in the step (4) is-60 to-50 ℃, and the time is 20 to 22 hours.
Preferably, in the step (4), 30-40 parts by weight of nano silver-titanium dioxide composite microspheres, 3-5 parts by weight of reducing agent and 55-67 parts by weight of graphene oxide aqueous solution.
The invention also provides the graphene composite aerogel formaldehyde-removing material prepared by the preparation method. Firstly, preparing graphene oxide, and adding deionized water to form a graphene oxide aqueous solution. Uniformly dispersing a certain amount of nano silver into deionized water, adding a titanium trichloride solution, stirring under the condition of keeping out of the sun, transferring to a hydrothermal reaction kettle for reaction, centrifuging the precipitate at a low speed, washing, and drying to obtain nano silver-titanium dioxide composite microspheres; and finally, adding the nano silver-titanium dioxide composite microspheres into a graphene oxide aqueous solution, adding a reducing agent hydrazine hydrate, pouring the mixture into a mold, and removing moisture through freeze drying to obtain the product.
The invention provides a graphene composite aerogel formaldehyde-removing material and a preparation method thereof, and compared with the prior art, the graphene composite aerogel formaldehyde-removing material has the outstanding characteristics and excellent effects that:
1. a method for preparing a graphene composite aerogel formaldehyde-removing material by compounding nano silver-titanium dioxide composite microspheres and graphene is provided.
2. The prepared and synthesized nano silver-titanium dioxide composite microspheres have the characteristics of good dispersity and uniform size, and simultaneously have good catalytic degradation performance and bactericidal performance.
3. The prepared graphene aerogel has a porous structure, can have strong adsorption reaction with organic matters such as formaldehyde and the like, and has good adsorption performance.
4. In the formaldehyde removal material prepared by the invention, the nano silver-titanium dioxide composite microspheres can completely degrade adsorbed organic matters under the photocatalysis effect, thereby fundamentally solving the defects that the graphene material has low adsorption capacity and can not completely degrade organic pollutants and the like.
5. The invention has simple production process, high air purification efficiency of the obtained product and good application prospect.
Drawings
FIG. 1: the invention relates to a preparation process flow chart of a graphene composite aerogel formaldehyde removal material.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but it should not be construed that the scope of the present invention is limited to the following examples. Various substitutions and alterations can be made by those skilled in the art and by conventional means without departing from the spirit of the method of the invention described above.
Example 1
The preparation process comprises the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 0.5h in an ice water bath, heating to 56 ℃, stirring and reacting for 12.5h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide; wherein, 9 parts of natural graphite, 13 parts of concentrated sulfuric acid, 2 parts of phosphoric acid, 27 parts of potassium permanganate, 43 parts of ice water and 6 parts of hydrogen peroxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution; 28 parts of graphene oxide and 72 parts of deionized water;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 17%, mixing and stirring under the condition of keeping out of the sun, then transferring to a hydrothermal reaction kettle, heating to carry out hydrothermal reaction, carrying out low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres; the rotation speed of mixing and stirring under the condition of keeping out of the sun is 260r/min, and the time is 24 min; the temperature of the hydrothermal reaction is 186 ℃, and the time is 24.5 h; wherein, 11 parts of nano silver, 36 parts of deionized water and 53 parts of titanium trichloride solution;
(4) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring the mixture into a mold, and freeze-drying the mixture to remove moisture to prepare a graphene composite aerogel formaldehyde-removing material; the reducing agent is hydrazine hydrate; the temperature of freeze drying is-56 ℃, and the time is 21 h; the composite material comprises, by weight, 34 parts of nano silver-titanium dioxide composite microspheres, 4 parts of a reducing agent and 62 parts of a graphene oxide aqueous solution.
Example 2
The preparation process comprises the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 0.5h in an ice water bath, heating to 52 ℃, stirring and reacting for 13h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide; wherein, 9 parts of natural graphite, 11 parts of concentrated sulfuric acid, 2 parts of phosphoric acid, 27 parts of potassium permanganate, 46 parts of ice water and 5 parts of hydrogen peroxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution; 25 parts of graphene oxide and 75 parts of deionized water;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 17%, mixing and stirring under the condition of keeping out of the sun, then transferring to a hydrothermal reaction kettle, heating to carry out hydrothermal reaction, carrying out low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres; the mixing and stirring speed is 220r/min under the condition of keeping out of the sun, and the time is 28 min; the temperature of the hydrothermal reaction is 182 ℃, and the time is 25 h; wherein, the silver nanoparticle comprises 10 weight parts of nano silver, 38 weight parts of deionized water and 52 weight parts of titanium trichloride solution;
(4) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring the mixture into a mold, and freeze-drying the mixture to remove moisture to prepare a graphene composite aerogel formaldehyde-removing material; the reducing agent is hydrazine hydrate; the temperature of freeze drying is-52 ℃ and the time is 22 h; the composite material comprises, by weight, 32 parts of nano silver-titanium dioxide composite microspheres, 3 parts of a reducing agent and 65 parts of a graphene oxide aqueous solution.
Example 3
The preparation process comprises the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 1h in an ice water bath, heating to 56 ℃, stirring and reacting for 12h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide; wherein, the natural graphite comprises 10 parts by weight of natural graphite, 14 parts by weight of concentrated sulfuric acid, 3 parts by weight of phosphoric acid, 28 parts by weight of potassium permanganate, 39 parts by weight of ice water and 6 parts by weight of hydrogen peroxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution; wherein, 35 parts by weight of graphene oxide and 65 parts by weight of deionized water;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 19%, mixing and stirring under the condition of keeping out of the sun, then transferring to a hydrothermal reaction kettle, heating to carry out hydrothermal reaction, carrying out low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres; the rotation speed of mixing and stirring under the condition of keeping out of the sun is 280r/min, and the time is 22 min; the temperature of the hydrothermal reaction is 188 ℃, and the time is 24 h; wherein, 12 parts of nano silver, 35 parts of deionized water and 53 parts of titanium trichloride solution;
(4) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring the mixture into a mold, and freeze-drying the mixture to remove moisture to prepare a graphene composite aerogel formaldehyde-removing material; the reducing agent is hydrazine hydrate; the temperature of freeze drying is-58 ℃ and the time is 20.5 h; the composite material comprises, by weight, 37 parts of nano silver-titanium dioxide composite microspheres, 5 parts of a reducing agent and 58 parts of a graphene oxide aqueous solution.
Example 4
The preparation process comprises the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 0.5h in an ice water bath, heating to 50 ℃, stirring and reacting for 13h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide; wherein, 8 parts by weight of natural graphite, 10 parts by weight of concentrated sulfuric acid, 2 parts by weight of phosphoric acid, 25 parts by weight of potassium permanganate, 50 parts by weight of ice water and 5 parts by weight of hydrogen peroxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution; wherein, the graphene oxide comprises 20 parts by weight of graphene oxide and 80 parts by weight of deionized water;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 15%, mixing and stirring under the condition of keeping out of the sun, then transferring to a hydrothermal reaction kettle, heating to carry out hydrothermal reaction, carrying out low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres; the rotation speed of mixing and stirring under the condition of keeping out of the sun is 200r/min, and the time is 30 min; the temperature of the hydrothermal reaction is 180 ℃ and the time is 25 h; wherein, 8 weight parts of nano silver, 42 weight parts of deionized water and 50 weight parts of titanium trichloride solution;
(4) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring the mixture into a mold, and freeze-drying the mixture to remove moisture to prepare a graphene composite aerogel formaldehyde-removing material; the reducing agent is hydrazine hydrate; the temperature of freeze drying is-60 ℃, and the time is 20 h; the composite material comprises, by weight, 30 parts of nano silver-titanium dioxide composite microspheres, 3 parts of a reducing agent and 67 parts of a graphene oxide aqueous solution.
Example 5
The preparation process comprises the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 1h in an ice water bath, heating to 60 ℃, stirring and reacting for 12h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide; wherein, the natural graphite comprises 10 parts by weight of natural graphite, 15 parts by weight of concentrated sulfuric acid, 3 parts by weight of phosphoric acid, 30 parts by weight of potassium permanganate, 35 parts by weight of ice water and 7 parts by weight of hydrogen peroxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution; 40 parts of graphene oxide and 60 parts of deionized water;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 20%, mixing and stirring under the condition of keeping out of the sun, then transferring to a hydrothermal reaction kettle, heating to carry out hydrothermal reaction, carrying out low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres; the rotation speed of mixing and stirring under the condition of keeping out of the sun is 300r/min, and the time is 20 min; the temperature of the hydrothermal reaction is 190 ℃ and the time is 24 h; wherein, 14 parts by weight of nano silver, 31 parts by weight of deionized water and 55 parts by weight of titanium trichloride solution;
(4) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring the mixture into a mold, and freeze-drying the mixture to remove moisture to prepare a graphene composite aerogel formaldehyde-removing material; the reducing agent is hydrazine hydrate; the temperature of freeze drying is-50 ℃ and the time is 22 h; the composite material comprises, by weight, 40 parts of nano silver-titanium dioxide composite microspheres, 5 parts of a reducing agent and 55 parts of a graphene oxide aqueous solution.
Example 6
The preparation process comprises the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 1h in an ice water bath, heating to 55 ℃, stirring and reacting for 12.5h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide; wherein, 9 parts by weight of natural graphite, 12 parts by weight of concentrated sulfuric acid, 3 parts by weight of phosphoric acid, 28 parts by weight of potassium permanganate, 42 parts by weight of ice water and 6 parts by weight of hydrogen peroxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution; wherein, 30 parts by weight of graphene oxide and 70 parts by weight of deionized water;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 18%, mixing and stirring under the condition of keeping out of the sun, then transferring to a hydrothermal reaction kettle, heating to carry out hydrothermal reaction, carrying out low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres; the rotation speed of mixing and stirring under the condition of keeping out of the sun is 250r/min, and the time is 25 min; the temperature of the hydrothermal reaction is 185 ℃, and the time is 24.5 h; wherein, 11 parts by weight of nano silver, 37 parts by weight of deionized water and 52 parts by weight of titanium trichloride solution;
(4) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring the mixture into a mold, and freeze-drying the mixture to remove moisture to prepare a graphene composite aerogel formaldehyde-removing material; the reducing agent is hydrazine hydrate; the temperature of freeze drying is-55 ℃, and the time is 21 h; the composite material comprises, by weight, 35 parts of nano silver-titanium dioxide composite microspheres, 4 parts of a reducing agent and 61 parts of a graphene oxide aqueous solution.
Comparative example 1
The preparation process comprises the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 1h in an ice water bath, heating to 55 ℃, stirring and reacting for 12.5h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide; wherein, 9 parts by weight of natural graphite, 12 parts by weight of concentrated sulfuric acid, 3 parts by weight of phosphoric acid, 28 parts by weight of potassium permanganate, 42 parts by weight of ice water and 6 parts by weight of hydrogen peroxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution; wherein, 30 parts by weight of graphene oxide and 70 parts by weight of deionized water;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 18%, mixing and stirring under the condition of keeping out of the sun, then transferring to a hydrothermal reaction kettle, heating to carry out hydrothermal reaction, carrying out low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres; the rotation speed of mixing and stirring under the condition of keeping out of the sun is 250r/min, and the time is 25 min; the temperature of the hydrothermal reaction is 185 ℃, and the time is 24.5 h; wherein, 11 parts by weight of nano silver, 37 parts by weight of deionized water and 52 parts by weight of titanium trichloride solution;
(4) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring the mixture into a mold, and freeze-drying the mixture to remove moisture to prepare a graphene composite aerogel formaldehyde-removing material; the reducing agent is hydrazine hydrate; the temperature of freeze drying is-55 ℃, and the time is 21 h; the composite material comprises, by weight, 35 parts of nano silver-titanium dioxide composite microspheres, 4 parts of a reducing agent and 20 parts of a graphene oxide aqueous solution.
Comparative example 1 the amount of the aqueous solution of graphene oxide was greatly reduced, so that the mesh was reduced.
Comparative example 2
The preparation process comprises the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 0.5h in an ice water bath, heating to 56 ℃, stirring and reacting for 12.5h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide; wherein, 9 parts of natural graphite, 13 parts of concentrated sulfuric acid, 2 parts of phosphoric acid, 27 parts of potassium permanganate, 43 parts of ice water and 6 parts of hydrogen peroxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution; 28 parts of graphene oxide and 72 parts of deionized water;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 17%, mixing and stirring under the condition of keeping out of the sun, then transferring to a hydrothermal reaction kettle, heating to carry out hydrothermal reaction, carrying out low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres; the rotation speed of mixing and stirring under the condition of keeping out of the sun is 260r/min, and the time is 24 min; the temperature of the hydrothermal reaction is 186 ℃, and the time is 24.5 h; wherein, 11 parts of nano silver, 36 parts of deionized water and 53 parts of titanium trichloride solution;
(4) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring the mixture into a mold, and heating and drying the mixture to remove moisture to prepare a graphene composite aerogel formaldehyde-removing material; the reducing agent is hydrazine hydrate; the composite material comprises, by weight, 34 parts of nano silver-titanium dioxide composite microspheres, 4 parts of a reducing agent and 62 parts of a graphene oxide aqueous solution.
Comparative example 2 no freeze-drying was used, and micropores formed by graphene decreased, affecting the adsorption of formaldehyde.
At 3m2Cutting the materials prepared in examples 1-6 and comparative example 1 into 30 × 30cm, placing the square with the thickness of 3mm in a test room, testing by adopting a British PPM-htV-m formaldehyde tester under the conditions of normal temperature and normal pressure, irradiating by adopting a lamp with the wavelength of 400-760 nm and the power of 100W, and respectively testing the formaldehyde concentration for 0.5h, 1h and 2 h.
The formaldehyde concentrations of the air cleaning filters measured by the above method in the formaldehyde removal test are shown in table 1.
Table 1:
through tests, the graphene is subjected to porous treatment, so that the adsorption of formaldehyde is greatly accelerated, and the purification of the formaldehyde is accelerated. The reference sample (comparative example 1) reduces the amount of graphene, so that the adsorption pores are reduced, and the adsorption and purification of formaldehyde are affected. If freeze drying is not adopted, micropores of the graphene can be greatly reduced, and the adsorption and purification of the formaldehyde are also influenced.
Claims (10)
1. A preparation method of a graphene composite aerogel formaldehyde-removing material is characterized by comprising the following steps:
(1) mixing natural graphite, concentrated sulfuric acid and phosphoric acid uniformly, adding potassium permanganate, stirring and reacting for 0.5-1 h in an ice water bath, heating to 50-60 ℃, stirring and reacting for 12-13 h, transferring into ice water after the reaction is finished, adding hydrogen peroxide in a stirring state until the color of the solution becomes golden yellow, filtering, washing and drying to obtain graphene oxide;
(2) adding the graphene oxide prepared in the step (1) into deionized water, and uniformly dispersing by ultrasonic to prepare a graphene oxide aqueous solution;
(3) adding nano silver into deionized water, uniformly dispersing, then adding a titanium trichloride solution with the mass concentration of 15-20%, mixing and stirring under a light-shielding condition, then transferring to a hydrothermal reaction kettle, heating to perform hydrothermal reaction, performing low-speed centrifugation on the precipitate after the hydrothermal reaction is finished, washing, and drying to obtain nano silver-titanium dioxide composite microspheres;
(4) and (3) adding the nano silver-titanium dioxide composite microspheres prepared in the step (3) and a reducing agent into the graphene oxide aqueous solution prepared in the step (2), uniformly mixing, pouring into a mold, and freeze-drying to remove moisture to prepare the graphene composite aerogel formaldehyde-removing material.
2. The preparation method of the graphene composite aerogel formaldehyde-removing material according to claim 1, characterized by comprising the following steps: in the step (1), 8-10 parts by weight of natural graphite, 10-15 parts by weight of concentrated sulfuric acid, 2-3 parts by weight of phosphoric acid, 25-30 parts by weight of potassium permanganate, 35-50 parts by weight of ice water and 5-7 parts by weight of hydrogen peroxide.
3. The preparation method of the graphene composite aerogel formaldehyde-removing material according to claim 1, characterized by comprising the following steps: in the step (2), 20-40 parts by weight of graphene oxide and 60-80 parts by weight of deionized water.
4. The preparation method of the graphene composite aerogel formaldehyde-removing material according to claim 1, characterized by comprising the following steps: and (4) mixing and stirring under the dark condition in the step (3) at the rotating speed of 200-300 r/min for 20-30 min.
5. The preparation method of the graphene composite aerogel formaldehyde-removing material according to claim 1, characterized by comprising the following steps: the temperature of the hydrothermal reaction in the step (3) is 180-190 ℃, and the time is 24-25 h.
6. The preparation method of the graphene composite aerogel formaldehyde-removing material according to claim 1, characterized by comprising the following steps: in the step (3), 8-14 parts by weight of nano silver, 31-42 parts by weight of deionized water and 50-55 parts by weight of a titanium trichloride solution.
7. The preparation method of the graphene composite aerogel formaldehyde-removing material according to claim 1, characterized by comprising the following steps: and (4) the reducing agent in the step (4) is hydrazine hydrate.
8. The preparation method of the graphene composite aerogel formaldehyde-removing material according to claim 1, characterized by comprising the following steps: and (4) carrying out freeze drying at the temperature of-60 to-50 ℃ for 20 to 22 hours.
9. The preparation method of the graphene composite aerogel formaldehyde-removing material according to claim 1, characterized by comprising the following steps: in the step (4), 30-40 parts by weight of nano silver-titanium dioxide composite microspheres, 3-5 parts by weight of reducing agent and 55-67 parts by weight of graphene oxide aqueous solution.
10. The graphene composite aerogel formaldehyde-removing material prepared by the preparation method of any one of claims 1 to 9.
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