CN113860293A - Preparation method of graphene oxide sponge with formaldehyde decomposition function - Google Patents
Preparation method of graphene oxide sponge with formaldehyde decomposition function Download PDFInfo
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- CN113860293A CN113860293A CN202111167105.2A CN202111167105A CN113860293A CN 113860293 A CN113860293 A CN 113860293A CN 202111167105 A CN202111167105 A CN 202111167105A CN 113860293 A CN113860293 A CN 113860293A
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- graphene oxide
- aqueous solution
- formaldehyde
- sponge
- titanium dioxide
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 114
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 46
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000007864 aqueous solution Substances 0.000 claims abstract description 37
- 239000000243 solution Substances 0.000 claims abstract description 19
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 238000004108 freeze drying Methods 0.000 claims abstract description 8
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 6
- 239000001301 oxygen Substances 0.000 claims abstract description 6
- 239000011347 resin Substances 0.000 claims abstract description 6
- 229920005989 resin Polymers 0.000 claims abstract description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 230000003213 activating effect Effects 0.000 claims abstract description 4
- 238000001354 calcination Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000011049 filling Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 13
- 238000003837 high-temperature calcination Methods 0.000 claims description 3
- 238000003980 solgel method Methods 0.000 claims description 3
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 claims description 2
- 239000002994 raw material Substances 0.000 claims description 2
- 239000000126 substance Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 abstract description 2
- 238000004064 recycling Methods 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 description 5
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000004887 air purification Methods 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 231100000357 carcinogen Toxicity 0.000 description 1
- 239000003183 carcinogenic agent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 208000032839 leukemia Diseases 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 208000017520 skin disease Diseases 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J21/00—Catalysts comprising the elements, oxides, or hydroxides of magnesium, boron, aluminium, carbon, silicon, titanium, zirconium, or hafnium
- B01J21/06—Silicon, titanium, zirconium or hafnium; Oxides or hydroxides thereof
- B01J21/063—Titanium; Oxides or hydroxides thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/312—Preparation
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
- C01G23/08—Drying; Calcining ; After treatment of titanium oxide
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Nanotechnology (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
The invention provides a preparation method of a graphene oxide sponge with a formaldehyde decomposition function, which comprises the following steps: preparing a graphene oxide aqueous solution, wherein the oxygen content in the aqueous solution is 10-55%; preparing a nano titanium dioxide aqueous solution, wherein the concentration of the aqueous solution is 0.1-10%; mixing the graphene oxide aqueous solution and the nano titanium dioxide aqueous solution by the volume percentage of 10:1, slowly adding the nano titanium dioxide aqueous solution while stirring the graphene oxide aqueous solution, and stirring for 15-30 minutes to obtain a mixture solution; adding water-based resin into the mixture solution, stirring for a period of time, performing ultrasonic dispersion, and filling into a specific mold for freeze drying; and (3) calcining and activating the mixture obtained by freeze drying at high temperature to obtain the graphene oxide sponge with the function of decomposing formaldehyde. The graphene oxide sponge has the advantages of no powder falling, strong formaldehyde decomposition capability and recycling.
Description
Technical Field
The invention relates to the field of air purification, and particularly relates to a preparation method of a graphene oxide sponge with a formaldehyde decomposition function.
Background
Formaldehyde, as a carcinogen, is widely present in decorative materials, and is easily caused to leukemia, skin diseases and even cancers after being exposed to formaldehyde environment for a long time. In particular, the release of formaldehyde is a long slow process, some even more than 10 years, and the removal of formaldehyde is imminent.
The graphene oxide is a two-dimensional material with a single atom thickness and rich functional groups, has a large specific surface area and the possibility of a composite material, is stably dispersed in an aqueous solution for a long time, and has good loading performance.
Disclosure of Invention
The invention provides a preparation method of a graphene oxide sponge with formaldehyde decomposition performance, and aims to obtain a functionalized graphene oxide sponge for adsorbing formaldehyde in air, and prepare the graphene oxide sponge which has high adsorption capacity, can be recycled, is efficient and has no pollution by combining a formaldehyde decomposition catalyst.
Therefore, the invention adopts the following technical scheme:
a preparation method of graphene oxide sponge with formaldehyde decomposition function comprises the following steps:
1) preparing a graphene oxide aqueous solution, wherein the oxygen content of the graphene oxide aqueous solution is 10% -55%;
2) preparing a nano titanium dioxide aqueous solution, wherein the concentration of the nano titanium dioxide aqueous solution is 0.1-10%;
3) mixing the graphene oxide aqueous solution and the nano titanium dioxide aqueous solution by the volume percentage of 10:1, slowly adding the nano titanium dioxide aqueous solution while stirring the graphene oxide aqueous solution, and stirring for 15-30 minutes to obtain a mixture solution;
4) adding water-based resin into the mixture solution, stirring for a period of time, performing ultrasonic dispersion, and filling into a specific mold for freeze drying;
5) and (3) calcining and activating the mixture obtained by freeze drying at high temperature to obtain the graphene oxide sponge with the function of decomposing formaldehyde.
Preferably, the graphene oxide solution is prepared by a chemical method, including a hummers method and a modified hummers method.
Preferably, the oxygen content in the graphene oxide aqueous solution is 35% -55%.
Preferably, the nano titanium dioxide aqueous solution is prepared by a sol-gel method, and is synthesized by taking tetrabutyl titanate as a raw material.
Preferably, the aqueous resin is added into the mixture solution, the stirring time is 1-2 hours, and the ultrasonic dispersion time is 15-60 minutes.
Preferably, the high-temperature calcination is carried out at 600-1000 ℃ for 20-40 minutes.
The graphite oxide sponge of the invention needs high-temperature calcination, can effectively improve the specific surface area of the sponge, and simultaneously converts titanium dioxide into anatase type to activate the catalyst. Meanwhile, the adsorption capacity of the sponge to formaldehyde is enhanced by utilizing the characteristic that the specific surface area of graphene oxide is large, and the capacity of decomposing formaldehyde into water and carbon dioxide is enhanced by combining the composite nano titanium dioxide nanosheet and ultraviolet illumination. The graphene oxide sponge with the formaldehyde decomposition function has the advantages of strong adsorption capacity, high decomposition capacity, simple and feasible preparation method, no powder falling, formaldehyde decomposition and recycling compared with the traditional carbon particle formaldehyde adsorbent.
Drawings
Fig. 1 is a schematic flow chart of a preparation method of the graphene oxide sponge with a formaldehyde decomposition function according to the present invention.
Fig. 2 is a schematic diagram of a graphene oxide sponge sample prepared in the embodiment of the present invention.
FIG. 3 shows the results of the specific surface area test of the sample according to the embodiment of the present invention.
FIG. 4 shows the results of the test of formaldehyde adsorption capacity of the sample according to the embodiment of the present invention.
FIG. 5 shows the results of the formaldehyde decomposition test of the sample according to the embodiment of the present invention.
Detailed Description
In order that the objects, features and advantages of the invention will be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings, which are illustrated in detail in order to provide a thorough understanding of the invention, but which may be carried out in other ways than those described. Accordingly, the invention is not limited by the specific implementations disclosed below.
According to the preparation method of the graphene oxide sponge with the formaldehyde decomposition function, the specific implementation is described as follows:
a preparation method of graphene oxide sponge with formaldehyde decomposition function comprises the following steps:
1) preparing a graphene oxide aqueous solution by adopting a modified hummers method, wherein the oxygen content in the graphene oxide aqueous solution is 45%;
2) preparing a nano titanium dioxide aqueous solution by adopting a sol-gel method, wherein the concentration of the nano titanium dioxide aqueous solution is 1%;
3) mixing the graphene oxide aqueous solution and the nano titanium dioxide aqueous solution by the volume percentage of 10:1, slowly adding the nano titanium dioxide aqueous solution while stirring the graphene oxide aqueous solution, and stirring for 30 minutes to obtain a mixture solution;
4) adding water-based resin into the mixture solution, stirring for 2 hours, performing ultrasonic dispersion for 30 minutes, and putting into a glass culture dish for freeze drying;
5) and (3) calcining and activating the mixture obtained by freeze drying at a high temperature of 800 ℃ for 30 minutes to obtain the graphene oxide sponge with the function of decomposing formaldehyde, as shown in figure 2.
The graphene oxide sponge obtained by the invention is characterized, and the specific surface area test result is as follows: 647.968m2(ii)/g, as shown in FIG. 3; formaldehyde adsorption capacity test results: after 4 hours, the formaldehyde content is reduced from 8ppm to 3ppm, as shown in FIG. 4; formaldehyde decomposition capability test results: taking out a part of the sponge after absorbing the formaldehyde, adding a formaldehyde absorbing solution, and after 30 minutes, adding a color developing agent, wherein the solution is changed into light yellow from colorless and transparent; taking out a part of the sponge after absorbing the formaldehyde, putting a formaldehyde absorbing solution after the sponge is illuminated by an ultraviolet lamp, putting a color developing agent into the formaldehyde absorbing solution after 30 minutes, wherein the solution is still a colorless transparent solution, and the result shows that the formaldehyde absorbed by the sponge is effectively dividedThe solution is shown in fig. 5.
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 (6)
1. A preparation method of graphene oxide sponge with formaldehyde decomposition function is characterized by comprising the following steps:
1) preparing a graphene oxide aqueous solution, wherein the oxygen content of the graphene oxide aqueous solution is 10% -55%;
2) preparing a nano titanium dioxide aqueous solution, wherein the concentration of the nano titanium dioxide aqueous solution is 0.1-10%;
3) mixing the graphene oxide aqueous solution and the nano titanium dioxide aqueous solution by the volume percentage of 10:1, slowly adding the nano titanium dioxide aqueous solution while stirring the graphene oxide aqueous solution, and stirring for 15-30 minutes to obtain a mixture solution;
4) adding water-based resin into the mixture solution, stirring for a period of time, performing ultrasonic dispersion, and filling into a specific mold for freeze drying;
5) and (3) calcining and activating the mixture obtained by freeze drying at high temperature to obtain the graphene oxide sponge with the function of decomposing formaldehyde.
2. The method for preparing the graphene oxide sponge with the function of decomposing formaldehyde according to claim 1, wherein the graphene oxide solution is prepared by a chemical method, including hummers method and modified hummers method.
3. The method for preparing graphene oxide sponge with formaldehyde decomposition function according to claim 1, wherein the oxygen content in the graphene oxide aqueous solution is 35% -55%.
4. The method for preparing graphene oxide sponge with formaldehyde decomposition function according to claim 1, wherein the nano titanium dioxide aqueous solution is prepared by a sol-gel method and synthesized by using tetrabutyl titanate as a raw material.
5. The method for preparing graphene oxide sponge with formaldehyde decomposition function according to claim 1, wherein the aqueous resin is added into the mixture solution, the stirring time is 1-2 hours, and the ultrasonic dispersion time is 15-60 minutes.
6. The method for preparing graphene oxide sponge with formaldehyde decomposing function as claimed in claim 1, wherein the high temperature calcination temperature is 600-1000 ℃ and the time is 20-40 minutes.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111167105.2A CN113860293A (en) | 2021-10-02 | 2021-10-02 | Preparation method of graphene oxide sponge with formaldehyde decomposition function |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111167105.2A CN113860293A (en) | 2021-10-02 | 2021-10-02 | Preparation method of graphene oxide sponge with formaldehyde decomposition function |
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|---|---|---|---|---|
| GB754553A (en) * | 1953-06-24 | 1956-08-08 | Wingfoot Corp | Reinforced latex foam rubber sponge |
| EP2463233A1 (en) * | 2010-12-08 | 2012-06-13 | Taiwan Textile Research Institute | Graphene/nano-titanium dioxide composites and methods for preparing the same |
| KR20130045996A (en) * | 2011-10-27 | 2013-05-07 | 한국과학기술원 | Method for manufacturing graphene-oxide sponge, graphene-oxide sponge manufactured by the same and absorption material for organic material comprising the same |
| CN104874347A (en) * | 2015-04-02 | 2015-09-02 | 浙江工业大学 | TiO2-loaded nitrogen-doped graphene sponge preparation method and application thereof |
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| CN107051380A (en) * | 2017-04-14 | 2017-08-18 | 杭州高烯科技有限公司 | A kind of preparation method of graphene/activated carbon/titanium dioxide composite porous microspheres |
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| CN108906006A (en) * | 2018-07-13 | 2018-11-30 | 北京欧美中科学技术研究院 | It is a kind of can efficient absorption formaldehyde modified graphene sponge preparation method |
| CN110127697A (en) * | 2019-05-23 | 2019-08-16 | 东南大学 | A method of can be prepared on a large scale modified activated carbon |
| CN113120890A (en) * | 2021-03-10 | 2021-07-16 | 苏州兴华高新材料科技有限公司 | Preparation method and application of graphene and titanium oxide nanocomposite |
-
2021
- 2021-10-02 CN CN202111167105.2A patent/CN113860293A/en active Pending
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| GB754553A (en) * | 1953-06-24 | 1956-08-08 | Wingfoot Corp | Reinforced latex foam rubber sponge |
| EP2463233A1 (en) * | 2010-12-08 | 2012-06-13 | Taiwan Textile Research Institute | Graphene/nano-titanium dioxide composites and methods for preparing the same |
| KR20130045996A (en) * | 2011-10-27 | 2013-05-07 | 한국과학기술원 | Method for manufacturing graphene-oxide sponge, graphene-oxide sponge manufactured by the same and absorption material for organic material comprising the same |
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| CN104874347A (en) * | 2015-04-02 | 2015-09-02 | 浙江工业大学 | TiO2-loaded nitrogen-doped graphene sponge preparation method and application thereof |
| CN107051380A (en) * | 2017-04-14 | 2017-08-18 | 杭州高烯科技有限公司 | A kind of preparation method of graphene/activated carbon/titanium dioxide composite porous microspheres |
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Application publication date: 20211231 |