CN116371443A - Preparation method of carbon nitride composite photocatalyst, and product and application thereof - Google Patents
Preparation method of carbon nitride composite photocatalyst, and product and application thereof Download PDFInfo
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- CN116371443A CN116371443A CN202310311543.4A CN202310311543A CN116371443A CN 116371443 A CN116371443 A CN 116371443A CN 202310311543 A CN202310311543 A CN 202310311543A CN 116371443 A CN116371443 A CN 116371443A
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 43
- 239000002131 composite material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 63
- 239000010445 mica Substances 0.000 claims abstract description 22
- 229910052618 mica group Inorganic materials 0.000 claims abstract description 22
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims abstract description 18
- 238000001035 drying Methods 0.000 claims abstract description 18
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims abstract description 13
- 239000004575 stone Substances 0.000 claims abstract description 13
- 238000010438 heat treatment Methods 0.000 claims abstract description 12
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 11
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000002156 mixing Methods 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 7
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000004202 carbamide Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000000034 method Methods 0.000 claims description 13
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 5
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 239000002904 solvent Substances 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 8
- 238000006731 degradation reaction Methods 0.000 abstract description 8
- 238000009776 industrial production Methods 0.000 abstract description 4
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000005034 decoration Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 239000002002 slurry Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000001680 brushing effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- -1 density board Substances 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000002655 kraft paper Substances 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000011120 plywood Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000009827 uniform distribution Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- 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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- 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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/70—Organic compounds not provided for in groups B01D2257/00 - B01D2257/602
- B01D2257/704—Solvents not covered by groups B01D2257/702 - B01D2257/7027
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2259/00—Type of treatment
- B01D2259/45—Gas separation or purification devices adapted for specific applications
- B01D2259/4508—Gas separation or purification devices adapted for specific applications for cleaning air in buildings
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Abstract
The invention discloses a preparation method of a carbon nitride composite photocatalyst, a product and application thereof, and relates to the technical field of indoor formaldehyde treatment, wherein the preparation method comprises the following steps: s1, preparing graphite-phase carbon nitride by taking urea or melamine as a raw material; s2, uniformly mixing graphite-phase carbon nitride and mica stone with a calcium hydroxide solution and calcium sulfate in water, and heating and stirring to react; and S3, after the reaction is finished, cooling and filtering, and drying filter residues to obtain the composite photocatalyst. The preparation process is simple, the preparation cost is low, the environment pollution is avoided, the large-scale industrial production is facilitated, and the degradation efficiency of formaldehyde can be greatly improved by the prepared carbon nitride composite photocatalyst.
Description
Technical Field
The invention relates to the technical field of indoor formaldehyde treatment, in particular to a preparation method of a carbon nitride composite photocatalyst, namely a porous mica stone supported porous carbon nitride oxide photocatalyst, a product thereof and application of the product in photocatalytic degradation of formaldehyde.
Background
Formaldehyde is one of the typical indoor pollutants, and the main sources are plywood, density board, paint and the like in the decoration materials, and the volatilization of formaldehyde in the home decoration materials is a very long process, which has serious harm to human health. Currently, the photocatalytic technology can completely degrade formaldehyde into CO 2 And H 2 O is widely studied; and ink phase carbon nitride (g-C) 3 N 4 ) The catalyst is widely applied in the field of photocatalysis due to the characteristics of low cost, good chemical property and high stability. However, conventional single graphite phase carbon nitride photocatalytic technology, while exhibiting photocatalytic activity under visible light driving, has low efficiency preventing further performance and industrial application.
In the prior art, researches on a carbon nitride composite photocatalyst are related, such as a preparation method of a two-dimensional and three-dimensional carrier reinforced carbon nitride photocatalytic material in patent application CN106582768A, and the like, which can utilize a two-dimensional flaky mica, a three-dimensional glass powder and other visible light carriers to reinforce the carbon nitride photocatalytic material, but most of the prior art is complicated in operation, dust, corrosive waste liquid and the like are easy to generate in the whole process, environmental pollution is easy to cause, the carbon nitride composite photocatalyst is not suitable for large-scale industrial production, meanwhile, the specific surface area of the carbon nitride composite photocatalyst prepared by the prior art is still general, and the degradation efficiency of formaldehyde is still limited finally.
For this reason, a new technical solution is needed to solve the above technical problems.
Disclosure of Invention
The invention aims to provide a preparation method of a carbon nitride composite photocatalyst, a product and application thereof, which are used for solving the technical problems that most of the prior art provided by the background technology are complex in operation, easy to pollute the environment and unsuitable for large-scale industrial production, and meanwhile, the specific surface area of the carbon nitride composite photocatalyst prepared by the prior art is still general, and finally the degradation efficiency of formaldehyde is still limited.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
in a first aspect, the present invention provides a method for preparing a carbon nitride composite photocatalyst, comprising the steps of:
s1, preparing graphite-phase carbon nitride by taking urea or melamine as a raw material, specifically calcining the urea or melamine in a nitrogen atmosphere, cooling after calcining, grinding, washing with absolute ethyl alcohol, centrifuging and drying to obtain the graphite-phase carbon nitride;
s2, uniformly mixing graphite-phase carbon nitride and mica with calcium hydroxide solution and calcium sulfate in water through a magnetic stirrer, heating and stirring to enable the mixture to react, wherein the mass ratio of the graphite-phase carbon nitride to the mica is 3:1, 2:1, 1:1, 1:2 or 1:3, the mass ratio of the total mass of the graphite-phase carbon nitride and the mica to the calcium hydroxide solution is 1:5-4:5, the mass ratio of the total mass of the graphite-phase carbon nitride and the mica to the calcium sulfate is 1:4-4:5, the calcium hydroxide solution is saturated calcium hydroxide solution, the heating temperature is not lower than 90 ℃, and the stirring time is not less than 8 hours;
and S3, after the reaction is finished, cooling and filtering, and drying filter residues to obtain the composite photocatalyst, wherein the drying temperature is not lower than 105 ℃, and the drying time is not less than 2 hours.
In a second aspect, the invention provides the carbon nitride composite photocatalyst obtained by the preparation method.
In a third aspect, the invention provides an application of the carbon nitride composite photocatalyst obtained by the preparation method in photocatalytic degradation of formaldehyde.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the invention, after the preparation of graphite-phase carbon nitride is completed, only graphite-phase carbon nitride and mica stone are used as raw materials, and calcium hydroxide solution and calcium sulfate are added, so that a porous photocatalyst of mica stone-loaded carbon nitride oxide, namely a carbon nitride composite photocatalyst, can be obtained through heating reaction, the whole preparation process is simple, the preparation cost is low, environmental pollution is avoided, and the preparation method is beneficial to large-scale industrial production;
2. the carbon nitride oxide has small size and uniform distribution, and is tightly combined with the interface of the mica stone, so that the transmission efficiency of the photo-generated carrier is improved, the absorption of light is enhanced, and compared with the pure carbon nitride oxide, the efficiency of degrading formaldehyde is greatly improved;
3. the addition of the mica stone can prevent the collapse of porous oxidized carbon nitride, so that the mechanical stability of the composite photocatalyst is improved, and finally, the efficiency of degrading formaldehyde by photocatalysis is further and indirectly ensured.
Drawings
FIG. 1 is a SEM image of a photocatalyst of the present invention;
FIG. 2 is a SEM image of a photocatalyst of the present invention;
FIG. 3 is a graph showing the degradation of formaldehyde by the photocatalyst of the present invention.
Detailed Description
The present invention will be described in further detail with reference to the following embodiments.
Example 1
Preparation of carbon nitride composite photocatalyst:
s1, weighing 5g of melamine in an alumina crucible, placing the melamine in a tube furnace, heating to 550 ℃ at a speed of 5 ℃/min under a nitrogen atmosphere, keeping for 4 hours, cooling, taking out, grinding, washing with absolute ethyl alcohol, centrifugally separating, and drying at 80 ℃ to obtain graphite-phase carbon nitride;
s2, weighing 0.75g of graphite-phase carbon nitride and 0.25g of mica stone in a conical flask, adding 5g of saturated calcium hydroxide solution and 4g of calcium sulfate, adding 20mL of water, mixing and stirring uniformly on a magnetic stirrer, heating to enable the reaction temperature to be 90 ℃, cooling and filtering after stirring for 8 hours, drying filter residues in a drying box at 105 ℃ for 2 hours, and taking out the filter residues to finally obtain porous mica stone-loaded porous carbon nitride oxide powder, namely the carbon nitride composite photocatalyst.
Example 2
Preparation of carbon nitride composite photocatalyst:
s1, weighing 20g of melamine in an alumina crucible, placing the melamine in a tube furnace, heating to 550 ℃ at a speed of 5 ℃/min under a nitrogen atmosphere, keeping for 4 hours, cooling, taking out, grinding, washing with absolute ethyl alcohol, centrifugally separating, and drying at 80 ℃ to obtain graphite-phase carbon nitride;
s2, weighing 2g of graphite-phase carbon nitride and 6g of mica stone in a conical flask, adding 10g of saturated calcium hydroxide solution and 10g of calcium sulfate, adding 40mL of water, mixing and stirring uniformly on a magnetic stirrer, heating to enable the reaction temperature to be 90 ℃, cooling and filtering after stirring for 8 hours, drying filter residues in a drying box at 105 ℃ for 2 hours, and taking out the filter residues to finally obtain porous mica stone loaded porous carbon nitride oxide powder, namely the carbon nitride composite photocatalyst.
Example 3
Preparation of carbon nitride composite photocatalyst:
s1, weighing 10g of melamine in an alumina crucible, placing the melamine in a tube furnace, heating to 550 ℃ at a speed of 5 ℃/min under a nitrogen atmosphere, keeping for 4 hours, cooling, taking out, grinding, washing with absolute ethyl alcohol, centrifugally separating, and drying at 80 ℃ to obtain graphite-phase carbon nitride;
s2, weighing 1g of graphite-phase carbon nitride and 1g of mica stone in a conical flask, adding 6g of saturated calcium hydroxide solution and 6g of calcium sulfate, adding 30mL of water, mixing and stirring uniformly on a magnetic stirrer, heating to enable the reaction temperature to be 90 ℃, cooling and filtering after stirring for 8 hours, drying filter residues in a drying box at 105 ℃ for 2 hours, and taking out the filter residues to finally obtain porous mica stone-loaded porous carbon nitride oxide powder, namely the carbon nitride composite photocatalyst.
Both fig. 1 and fig. 2 are scanning electron microscope images of the carbon nitride composite photocatalyst prepared in example 1 of the present invention (examples 2 to 3 are similar to the scanning electron microscope images of example 1 and are not listed), and fig. 2 is an enlarged view of fig. 1, and it can be seen from fig. 1 and fig. 2 that carbon nitride oxide is tightly combined with mica, and the surface is in an irregular hole shape, which can increase the specific surface area and expose more active sites, thereby improving the degradation performance to formaldehyde.
In order to further observe the application effect of the prepared carbon nitride composite photocatalyst in photocatalytic degradation of formaldehyde, taking example 2 as an example, experiments of photocatalytic degradation of formaldehyde are performed on the carbon nitride composite photocatalyst prepared in example 2, and the specific experimental process is as follows:
firstly, weighing 1g of the carbon nitride composite photocatalyst prepared in the embodiment 2, adding 0.2ml of absolute ethyl alcohol and 0.2ml of deionized water, uniformly mixing to form slurry, uniformly brushing the slurry on a kraft paper coated organic glass cylinder with the diameter of 40 mm and the length of 200 mm, and naturally airing; then, putting the organic glass cylinder into a small intelligent environmental climate chamber containing formaldehyde with the initial concentration of 110ppm, turning on a xenon lamp, filtering light waves smaller than 420nm by using a light filter to obtain a visible light source, and starting a photocatalytic degradation experiment; finally, in the process of the photocatalytic degradation experiment, sampling is carried out once every 4min, testing is carried out by using a formaldehyde tester, and the testing result is recorded.
The final formaldehyde degradation result is shown in fig. 3, and as can be seen from fig. 3, the degradation rate of formaldehyde reaches more than 90% within 5min, and the degradation efficiency of formaldehyde is very high under visible light.
Claims (10)
1. The preparation method of the carbon nitride composite photocatalyst is characterized by comprising the following steps of:
s1, preparing graphite-phase carbon nitride by taking urea or melamine as a raw material;
s2, uniformly mixing graphite-phase carbon nitride and mica stone with a calcium hydroxide solution and calcium sulfate in water, and heating and stirring to react;
and S3, after the reaction is finished, cooling and filtering, and drying filter residues to obtain the composite photocatalyst.
2. The method for preparing a carbon nitride composite photocatalyst according to claim 1, wherein the specific operation procedure of step S1 is as follows: calcining urea or melamine in nitrogen atmosphere, cooling after calcining, grinding, washing, centrifugally separating and drying to obtain graphite-phase carbon nitride.
3. The method for preparing a carbon nitride composite photocatalyst according to claim 2, wherein the washed solvent is absolute ethanol.
4. The method for preparing a carbon nitride composite photocatalyst according to claim 1, wherein in step S2, the mass ratio of graphite-phase carbon nitride to mica is 3:1, 2:1, 1:1, 1:2 or 1:3.
5. The method for preparing a carbon nitride composite photocatalyst according to claim 1, wherein in step S2, the mass ratio of the total mass of graphite-phase carbon nitride and mica to the calcium hydroxide solution is 1:5-4:5, and the mass ratio of the total mass of graphite-phase carbon nitride and mica to calcium sulfate is 1:4-4:5.
6. The method for preparing a carbon nitride composite photocatalyst according to claim 1, wherein in step S2, the calcium hydroxide solution is a saturated calcium hydroxide solution.
7. The method for preparing a carbon nitride composite photocatalyst according to claim 1, wherein in step S2, the mixture is uniformly mixed by a magnetic stirrer.
8. The method for preparing a carbon nitride composite photocatalyst according to claim 1, wherein in step S2, the heating temperature is not lower than 90 ℃, and the stirring time is not less than 8 hours; in the step S3, the drying temperature is not lower than 105 ℃, and the drying time is not less than 2 hours.
9. A carbon nitride composite photocatalyst obtained by the production method according to any one of claims 1 to 8.
10. Use of the carbon nitride composite photocatalyst obtained by the preparation method of any one of claims 1 to 8 in photocatalytic degradation of formaldehyde.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202310311543.4A CN116371443A (en) | 2023-03-28 | 2023-03-28 | Preparation method of carbon nitride composite photocatalyst, and product and application thereof |
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| CN202310311543.4A CN116371443A (en) | 2023-03-28 | 2023-03-28 | Preparation method of carbon nitride composite photocatalyst, and product and application thereof |
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| CN106111174A (en) * | 2016-06-17 | 2016-11-16 | 中国矿业大学(北京) | G C3N4/ kaolinite composite photo-catalyst and preparation method thereof |
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