CN113996277A - Preparation method of Schiff base sensitized graphene composite titanium dioxide photocatalyst - Google Patents
Preparation method of Schiff base sensitized graphene composite titanium dioxide photocatalyst Download PDFInfo
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- CN113996277A CN113996277A CN202111290765.XA CN202111290765A CN113996277A CN 113996277 A CN113996277 A CN 113996277A CN 202111290765 A CN202111290765 A CN 202111290765A CN 113996277 A CN113996277 A CN 113996277A
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 102
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 46
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 43
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 33
- 150000004753 Schiff bases Chemical class 0.000 title claims abstract description 26
- 239000002262 Schiff base Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 16
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims abstract description 15
- 239000007864 aqueous solution Substances 0.000 claims abstract description 12
- KUCOHFSKRZZVRO-UHFFFAOYSA-N terephthalaldehyde Chemical compound O=CC1=CC=C(C=O)C=C1 KUCOHFSKRZZVRO-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000000725 suspension Substances 0.000 claims description 27
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000000843 powder Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000000243 solution Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 5
- 230000001804 emulsifying effect Effects 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 abstract description 42
- 239000000126 substance Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 4
- 238000002474 experimental method Methods 0.000 abstract description 4
- 239000011521 glass Substances 0.000 abstract description 3
- 230000006872 improvement Effects 0.000 abstract description 3
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000002516 radical scavenger Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 description 1
- 239000000809 air pollutant Substances 0.000 description 1
- 231100001243 air pollutant Toxicity 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003995 emulsifying agent Substances 0.000 description 1
- 229910000037 hydrogen sulfide Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002466 imines Chemical class 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- VUZPPFZMUPKLLV-UHFFFAOYSA-N methane;hydrate Chemical compound C.O VUZPPFZMUPKLLV-UHFFFAOYSA-N 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/26—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24
- B01J31/38—Catalysts comprising hydrides, coordination complexes or organic compounds containing in addition, inorganic metal compounds not provided for in groups B01J31/02 - B01J31/24 of titanium, zirconium or hafnium
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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
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- B01D53/8668—Removing organic compounds not provided for in B01D53/8603 - B01D53/8665
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Abstract
The invention discloses a preparation method of Schiff base sensitized graphene composite titanium dioxide photocatalyst, wherein nanometer TiO2 and nanometer graphene oxide are modified by a silane coupling agent, Schiff base is formed by terephthalaldehyde and amino, TiO2 and graphene oxide are linked through Schiff base groups, and further chemical bond linkage of graphene, dye and TiO2 is realized, so that the Schiff base sensitized graphene composite titanium dioxide photocatalyst is obtained. The photocatalyst synthesized by the method is sprayed into a glass box closed space with a certain volume, a certain amount of formaldehyde aqueous solution is added to volatilize the photocatalyst, then the photocatalyst is irradiated for 48 hours under a fluorescent lamp, and then the concentration of formaldehyde is tested. This experiment proves, the synthetic photocatalyst of this patent has obvious improvement to gaseous formaldehyde's clearance effect, and the clearance efficiency to formaldehyde is 89% in 48 h.
Description
Technical Field
The invention belongs to the technical field of indoor odor removal, and particularly relates to a preparation method of a Schiff base sensitized graphene composite titanium dioxide photocatalyst.
Background
The photocatalytic oxidation method is mainly characterized in that after the photocatalyst receives illumination, active oxygen substances such as hydroxyl radicals and oxygen radicals are generated on the surface of the photocatalyst, and the strong oxidizing substances can directly oxidize formaldehyde and finally oxidize the formaldehyde into nontoxic and harmless carbon dioxide and water. The method becomes a research hotspot for treating air pollutants. Among them, semiconductor photocatalytic technology has attracted much attention. Namely the photocatalyst technology which we commonly call. nano-TiO 2 is commonly used for semiconductors. And the dye-sensitized TiO2 photocatalytic system solves the problem of weak visible light response of TiO 2.
Although graphene is an excellent photocatalyst material, graphene is a material with zero bandwidth, and the application of graphene in the field of photocatalysis is weakened. Therefore, researchers often modify organic dye molecules on the surface of graphene, and on one hand, the excellent hydrophilicity of the graphene can be utilized to improve the dispersibility of the dye molecules in an aqueous solution; on the other hand, the photoresponse range of the graphene can be widened by using organic dye molecules.
In the dye-sensitized TiO2 photocatalytic system, TiO2 is often regarded as a base material, and its bonding with dye molecules is strong and weak, directly affecting the electron transport properties. Meanwhile, the crystal form, size, morphology and the like of the TiO2 also have influence on dye-sensitized TiO2 photocatalysis.
Schiff base, also known as Schiff base, Schiff base. Schiff base mainly refers to a class of organic compounds containing imine or azomethine characteristic groups (-RC ═ N-), and generally, Schiff base is formed by condensation of amine and active carbonyl, is an important dye chromophore and has photoresponse.
The traditional dye-sensitized photocatalyst deposits a dye on the surface of nano TiO2 in a physical doping mode, and the dye and nano TiO2 particles are not connected by chemical bonds, so that the dye and the nano TiO2 particles are not tightly combined, and the injection of electrons to a semiconductor conduction band is not fast enough.
Disclosure of Invention
The invention aims to provide a preparation method of a Schiff base sensitized graphene composite titanium dioxide photocatalyst, and aims to solve the problems in the background technology. In order to realize the purpose, the invention adopts the technical scheme that:
according to the preparation method, the silane coupling agent is used for modifying the nano TiO2 and the nano graphene oxide, Schiff base is formed by terephthalaldehyde and amino, the TiO2 and the graphene oxide are linked through Schiff base groups, and further the chemical bond linkage of the graphene, the dye and the TiO2 is realized.
The method specifically comprises the following steps:
a preparation method of Schiff base sensitized graphene composite titanium dioxide photocatalyst comprises the following specific steps:
s1: selecting Degussa P25 as nano TiO2 powder, mixing the nano TiO2 powder with deionized water, and dispersing at high speed for 0.5-1.5h by using an emulsifying machine to prepare 5-10% suspension;
s2: adjusting the pH value of the suspension of S1 to 4-6 by using acetic acid, adding a silane coupling agent KH550 accounting for 5-15% of the mass of the nano TiO2 powder, and reacting at 80-100 ℃ for 1-3h to obtain a nano TiO2 suspension;
s3: preparing a graphene oxide suspension by a Hummers method, and obtaining a stable graphene oxide aqueous dispersion with the concentration of 5mg/mL through ultrasonic treatment in deionized water;
s4: adding 20mL of GO aqueous solution and 1g of silane coupling agent KH550 into absolute ethyl alcohol, stirring to dissolve, adding into GOs aqueous solution, performing ultrasonic treatment for 30min, and stirring for 10 min;
s5: adjusting the pH value of the solution in the S4 to 4-5 by using acetic acid, then reacting in a water bath at 50 ℃ for 0.5-1h, heating to 70 ℃, and continuing to react for 0.5-1h to obtain a graphene oxide suspension;
s6: mixing the nano TiO2 suspension of S2 and the graphene oxide suspension of S5 according to the weight ratio of 1: 1, slowly dripping 50 percent of ethanol solution of terephthalaldehyde in mass fraction, and reacting for 1-2 hours at the temperature of 60-80 ℃ to obtain the Schiff base sensitized graphene composite titanium dioxide photocatalyst.
Preferably, the dispersion time of the emulsifying machine in the S1 is 1h, and the mass fraction of the suspension is preferably 7%.
Preferably, the pH of the suspension in the S2 is 5, the adding amount of the silane coupling agent KH550 is 10% of the mass of the nano TiO2 powder, and the reaction is carried out for 2 hours at 90 ℃.
Preferably, the GO aqueous solution in S4 is reacted with a silane coupling agent for 1h at 50 ℃ or 1h at 70 ℃.
Preferably, the reaction with terephthalaldehyde in S6 is carried out at 70 ℃ for 1.5 h.
The invention has the beneficial effects that:
according to the preparation method, a silane coupling agent is used for modifying nano TiO2 and nano graphene oxide, Schiff base is formed by terephthalaldehyde and amino, TiO2 and graphene oxide are linked through Schiff base groups, and further chemical bond linkage of graphene, dye and TiO2 is achieved;
the photocatalyst synthesized by the method is sprayed into a glass box closed space with a certain volume, a certain amount of formaldehyde aqueous solution is added to volatilize the photocatalyst, then the photocatalyst is irradiated for 48 hours under a fluorescent lamp, and then the concentration of formaldehyde is tested. The experiment proves that the photocatalyst synthesized by the patent has obvious improvement on the removing effect of gaseous formaldehyde. The formaldehyde removal efficiency in 48h was 89%.
Drawings
Fig. 1 is a schematic diagram of a product generation process provided in an embodiment of the present invention.
Detailed Description
To facilitate an understanding of the invention, the invention will now be described more fully with reference to the accompanying drawings. Preferred embodiments of the present invention are shown in the drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
It will be understood that when an element is referred to as being "secured to" another element, it can be directly on the other element or intervening elements may also be present. When an element is referred to as being "connected" to another element, it can be directly connected to the other element or intervening elements may also be present. In contrast, when an element is referred to as being "directly on" another element, there are no intervening elements present. As used herein, the terms "vertical," "horizontal," "left," "right," and the like are for illustrative purposes only and do not represent the only embodiments, and as used herein, the terms "upper," "lower," "left," "right," "front," "rear," and the like are used in a positional relationship with reference to the drawings.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The technical solution of the present patent will be described in further detail with reference to the following embodiments.
As shown in fig. 1, an embodiment of the present invention provides a preparation method of a schiff base-sensitized graphene composite titanium dioxide photocatalyst, which specifically includes the following steps:
s1: selecting Degussa P25 as nano TiO2 powder, mixing the nano TiO2 powder with deionized water, and dispersing at high speed for 0.5-1.5h by using an emulsifying machine to prepare 5-10% suspension;
s2: adjusting the pH value of the S1 suspension to 4-6 by using acetic acid, adding a silane coupling agent KH550 accounting for 5-15% of the mass of the nano TiO2 powder, and reacting at 80-100 ℃ for 1-3h to obtain a nano TiO2 suspension;
s3: preparing a graphene oxide suspension by a Hummers method, and obtaining a stable graphene oxide aqueous dispersion with the concentration of 5mg/mL through ultrasonic treatment in deionized water;
s4: adding 20mL of GO aqueous solution and 1g of silane coupling agent KH550 into absolute ethyl alcohol, stirring to dissolve, adding into GOs aqueous solution, performing ultrasonic treatment for 30min, and stirring for 10 min;
s5: adjusting the pH value of the solution in the S4 to 4-5 by using acetic acid, then reacting in a water bath at 50 ℃ for 0.5-1h, heating to 70 ℃, and continuing to react for 0.5-1h to obtain a graphene oxide suspension;
s6: mixing the nano TiO2 suspension of S2 and the graphene oxide suspension of S5 according to the weight ratio of 1: 1, slowly dripping 50 percent of ethanol solution of terephthalaldehyde in mass fraction, and reacting for 1-2 hours at the temperature of 60-80 ℃ to obtain the Schiff base sensitized graphene composite titanium dioxide photocatalyst.
In this embodiment, the emulsifier dispersion time in S1 is 1 hour, and the mass fraction of the suspension is preferably 7%.
In the present embodiment, the pH of the suspension in S2 is preferably 5, the amount of the silane coupling agent KH550 added is 10% of the mass of the nano TiO2 powder, and the reaction is carried out for 2h at 90 ℃.
In this particular example, the aqueous GO solution in S4 was reacted with the silane coupling agent for 1 hour at 50 deg.C or 1 hour at 70 deg.C.
In this embodiment, the reaction with terephthalaldehyde in S6 was carried out at 70 ℃ for 1.5 h.
The odor scavenger prepared by the embodiment is adopted to remove odor, the odor scavenger with the same amount of commercial Evonik TEGO A30 is adopted as a control group, formaldehyde, hydrogen sulfide and ammonia gas are respectively removed for experiments, and after the odor scavenger is removed for 45min, the effects are shown in the following table:
the photocatalyst synthesized by the method is sprayed into a glass box closed space with a certain volume, a certain amount of formaldehyde aqueous solution is added to volatilize the photocatalyst, then the photocatalyst is irradiated for 48 hours under a fluorescent lamp, and then the concentration of formaldehyde is tested. The experiment proves that the photocatalyst synthesized by the patent has obvious improvement on the removing effect of gaseous formaldehyde. The formaldehyde removal efficiency in 48h was 89%. The method comprises the following specific steps:
the above embodiments are only for illustrating the invention and are not to be construed as limiting the invention, and those skilled in the art can make various changes and modifications without departing from the spirit and scope of the invention, therefore, all equivalent technical solutions also belong to the scope of the invention, and the scope of the invention is defined by the claims.
Claims (5)
1. A preparation method of Schiff base sensitized graphene composite titanium dioxide photocatalyst is characterized by comprising the following steps: the method comprises the following specific steps:
s1: selecting Degussa P25 as nano TiO2 powder, mixing the nano TiO2 powder with deionized water, and dispersing at high speed for 0.5-1.5h by using an emulsifying machine to prepare 5-10% suspension;
s2: adjusting the pH value of the suspension of S1 to 4-6 by using acetic acid, adding a silane coupling agent KH550 accounting for 5-15% of the mass of the nano TiO2 powder, and reacting at 80-100 ℃ for 1-3h to obtain a nano TiO2 suspension;
s3: preparing a graphene oxide suspension by a Hummers method, and obtaining a stable graphene oxide aqueous dispersion with the concentration of 5mg/mL through ultrasonic treatment in deionized water;
s4: adding 20mL of GO aqueous solution and 1g of silane coupling agent KH550 into absolute ethyl alcohol, stirring to dissolve, adding into GOs aqueous solution, performing ultrasonic treatment for 30min, and stirring for 10 min;
s5: adjusting the pH value of the solution in the S4 to 4-5 by using acetic acid, then reacting in a water bath at 50 ℃ for 0.5-1h, heating to 70 ℃, and continuing to react for 0.5-1h to obtain a graphene oxide suspension;
s6: mixing the nano TiO2 suspension of S2 and the graphene oxide suspension of S5 according to the weight ratio of 1: 1, slowly dripping 50 percent of ethanol solution of terephthalaldehyde in mass fraction, and reacting for 1-2 hours at the temperature of 60-80 ℃ to obtain the Schiff base sensitized graphene composite titanium dioxide photocatalyst.
2. The method for preparing the Schiff base sensitized graphene composite titanium dioxide photocatalyst according to claim 1, which is characterized in that: the dispersing time of the emulsifying machine in the S1 is 1h, and the mass fraction of the suspension is 7%.
3. The method for preparing the Schiff base sensitized graphene composite titanium dioxide photocatalyst according to claim 1, which is characterized in that: the pH of the suspension in the S2 is preferably 5, the adding amount of the silane coupling agent KH550 is 10 percent of the mass of the nano TiO2 powder, and the reaction is carried out for 2 hours at 90 ℃.
4. The method for preparing the Schiff base sensitized graphene composite titanium dioxide photocatalyst according to claim 1, which is characterized in that: and the GO aqueous solution in the S4 reacts with a silane coupling agent for 1h at 50 ℃ or 1h at 70 ℃.
5. The method for preparing the Schiff base sensitized graphene composite titanium dioxide photocatalyst according to claim 1, which is characterized in that: the reaction with terephthalaldehyde in S6 was carried out at 70 ℃ for 1.5 h.
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| CN117143529A (en) * | 2023-08-23 | 2023-12-01 | 派乐玛光学薄膜(东莞)有限公司 | Blue light resistant optical adhesive, OCA optical adhesive and preparation method and application thereof |
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