CN111320228A - Self-cleaning carbon nitride gel and preparation method thereof - Google Patents
Self-cleaning carbon nitride gel and preparation method thereof Download PDFInfo
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- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 69
- 238000004140 cleaning Methods 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000001879 gelation Methods 0.000 title description 2
- 239000000178 monomer Substances 0.000 claims abstract description 14
- 229920002643 polyglutamic acid Polymers 0.000 claims abstract description 13
- 229920000642 polymer Polymers 0.000 claims abstract description 12
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 9
- 239000000243 solution Substances 0.000 claims description 24
- 239000007864 aqueous solution Substances 0.000 claims description 21
- 238000000034 method Methods 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 6
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 4
- 238000004108 freeze drying Methods 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 238000001354 calcination Methods 0.000 claims description 3
- 239000004202 carbamide Substances 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- PQDJYEQOELDLCP-UHFFFAOYSA-N trimethylsilane Chemical group C[SiH](C)C PQDJYEQOELDLCP-UHFFFAOYSA-N 0.000 claims description 2
- 239000004964 aerogel Substances 0.000 abstract description 31
- 239000000499 gel Substances 0.000 abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 12
- 239000000463 material Substances 0.000 abstract description 7
- YUYCVXFAYWRXLS-UHFFFAOYSA-N trimethoxysilane Chemical compound CO[SiH](OC)OC YUYCVXFAYWRXLS-UHFFFAOYSA-N 0.000 abstract description 6
- 239000004065 semiconductor Substances 0.000 abstract description 4
- 238000010521 absorption reaction Methods 0.000 abstract description 3
- 239000000017 hydrogel Substances 0.000 abstract description 2
- 239000006185 dispersion Substances 0.000 abstract 1
- 230000005284 excitation Effects 0.000 abstract 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract 1
- 238000005286 illumination Methods 0.000 abstract 1
- 230000014759 maintenance of location Effects 0.000 abstract 1
- 238000006116 polymerization reaction Methods 0.000 abstract 1
- 150000001720 carbohydrates Chemical class 0.000 description 14
- 239000000975 dye Substances 0.000 description 14
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 12
- 229940043267 rhodamine b Drugs 0.000 description 12
- 230000000694 effects Effects 0.000 description 8
- 230000015556 catabolic process Effects 0.000 description 6
- 238000006731 degradation reaction Methods 0.000 description 6
- 239000011651 chromium Substances 0.000 description 5
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 5
- 230000000593 degrading effect Effects 0.000 description 4
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 229910002804 graphite Inorganic materials 0.000 description 3
- 239000010439 graphite Substances 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910001430 chromium ion Inorganic materials 0.000 description 2
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000002798 spectrophotometry method Methods 0.000 description 2
- 239000004966 Carbon aerogel Substances 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 239000000982 direct dye Substances 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000011664 nicotinic acid Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000005067 remediation Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0052—Preparation of gels
- B01J13/0056—Preparation of gels containing inorganic material and water
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
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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
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- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
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- 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
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F1/70—Treatment of water, waste water, or sewage by reduction
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
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Abstract
The invention discloses a self-cleaning carbon nitride gel and a preparation method thereof. The gel is prepared by high-dispersion thin-layer carbon nitride, polymer monomer y-polyglutamic acid and cross-linking agent trimethoxy silane, under the excitation of visible light, photo-generated electrons and holes generated by the semiconductor carbon nitride material react with water to generate a large amount of hydroxyl free radicals, and the semiconductor carbon nitride material generates carbon nitride hydrogel or carbon nitride aerogel through the polymerization of the monomer and the cross-linking agent. The carbon nitride aerogel has good water absorption and moisture retention capacity, can degrade an adsorbed dye solution under illumination, and has good self-cleaning capacity.
Description
Technical Field
The invention relates to a nitrided carbohydrate aerogel and carbon nitride aerogel material, and a preparation method and application thereof, and belongs to the field of application of nano materials.
Background
The environmental pollution is always a main factor influencing the living environment of human beings, wherein the treatment modes of dye pollution and heavy metal pollution mainly comprise an adsorption method, an extraction method, a membrane separation method, a coagulation sedimentation method, a catalytic oxidation method, an electrochemical method and a biological method. However, most of these methods cause secondary pollution, so that a treatment method with good biocompatibility is a problem to be solved. Photocatalytic technology has emerged in recent years with great potential in environmental remediation. Graphite phase carbon nitride (g-C)3N4) As a novel polymer semiconductor material, the photocatalyst can absorb visible light, has better stability, and is known as a novel environment-friendly photocatalytic semiconductor material with development potential. The prior art uses g-C3N4There is a certain effect of direct dye degradation of the powder, but on g-C3N4Post-processing and recycling do not have a good solution.
Disclosure of Invention
The invention aims to provide a carbon nitride gel material and a preparation method thereof.
The technical solution for realizing the purpose of the invention is as follows: a self-cleaning carbon nitride gel is prepared by the following steps:
the first step, carbon nitride is uniformly dispersed in an aqueous solution;
a second step of uniformly dispersing the polymer monomer in an aqueous solution;
thirdly, dripping the carbon nitride aqueous solution obtained in the first step into the polymer monomer aqueous solution obtained in the second step;
step four, dripping a cross-linking agent into the mixed solution obtained in the step three, and stirring and dispersing uniformly;
and fifthly, transferring the uniformly dispersed solution into a mold and drying.
Preferably, in the first step, the carbon nitride is obtained by calcining a nitrogen-rich precursor, and the specific preparation steps are as follows: and (3) putting the urea into a crucible with a cover, placing the crucible in a tube furnace, raising the temperature to 500-550 ℃ by a program, and preserving the heat for 2-4h to obtain solid powder, namely the carbon nitride.
Preferably, in the second step, the polymer monomer is gamma-polyglutamic acid.
Preferably, in the third step, the mass ratio of the carbon nitride to the polymer monomer is 1:10-1: 40.
Preferably, in the fourth step, the crosslinking agent is trimethylsilane, and the mass ratio of the polymer monomer to the crosslinking agent is 1:1-4: 1.
Preferably, in the fifth step, the drying is drying at 35-40 ℃, or freeze drying.
Compared with the prior art, the invention has the advantages that: (1) the carbon nitride obtained by calcining urea as a precursor is lighter, the band gap can properly show better photocatalytic performance, and the carbon nitride prepared by the method is easy to disperse in an aqueous solution; (2) the raw materials of the y-polyglutamic acid and the carbon nitride for preparing the carbon nitride gel have good biocompatibility, are harmless to the environment and the human body, and are hopeful to be applied to the research of bionic materials. (3) The prepared carbon nitride aerogel has small density, light weight, good water absorption and self-cleaning capability. (4) The carbon nitride gel is utilized to carry out dye degradation and heavy metal reduction, and the post-treatment is convenient.
Drawings
FIG. 1 is a digital photograph of the nitrogenated carbohydrate gel prepared in example 1.
FIG. 2 is a scanning electron micrograph of the nitrogenated carbohydrate gel prepared in example 1.
FIG. 3 is a scanning electron micrograph of the carbon nitride aerogel prepared in example 2.
Fig. 4 is an X-ray diffraction pattern of graphite phase carbon nitride powder and the carbon nitride aerogel prepared in example 2.
FIG. 5 is a Fourier infrared spectrum of a graphite phase carbon nitride powder, a carbon nitride aerogel prepared in example 1, and a carbon nitride aerogel prepared in example 2.
FIG. 6 is a graph showing the effect of reducing hexavalent chromium ions by the nitrogenated carbohydrate gel prepared in example 3.
FIG. 7 is a graph showing the effect of the carbon nitride aerogel prepared in example 4 on degrading rhodamine B dye solution.
FIG. 8 is a diagram of the process of degrading rhodamine B dye solution by the carbon nitride aerogel prepared in example 4.
Detailed Description
The carbon nitride hydrogel and the carbon nitride aerogel prepared by the method have outstanding degradation effect on dye pollutants, have obvious reduction effect on heavy metal Cr (VI), and have a self-cleaning function.
The nitrided carbohydrate aerogel and the nitrided carbon aerogel are prepared by the following steps:
a first step of uniformly dispersing a monomer (gamma-polyglutamic acid, 0.5-2 g) in an aqueous solution;
secondly, uniformly dispersing graphite-phase carbon nitride powder (0.05-0.1 g) in an aqueous solution;
thirdly, dropwise adding the uniformly dispersed carbon nitride aqueous solution into the uniformly dispersed monomer solution;
fourthly, dripping a cross-linking agent (trimethoxy silane, 0.5-1 g) into the mixed solution obtained in the third step, and uniformly stirring and dispersing;
fifthly, transferring the uniformly dispersed solution into a die and drying.
Example 1:
firstly, uniformly dispersing 0.5g of gamma-polyglutamic acid in 10mL of water, and stirring for 1 h;
step two, uniformly dispersing 0.05g of carbon nitride in 10mL of water, and stirring for 2 hours;
thirdly, dropwise adding the uniformly dispersed carbon nitride aqueous solution into the uniformly dispersed gamma-polyglutamic acid aqueous solution;
step four, dripping 1g of trimethoxy silane into the mixed solution in the step three, and stirring for 3 hours;
and fifthly, transferring the uniformly dispersed solution into a mold, and drying in a vacuum oven at 38 ℃ for 12h to obtain the nitrogenated carbohydrate gel.
Sixthly, the prepared nitrogenated carbohydrate gel is characterized, wherein figure 1 is a digital photo of the nitrogenated carbohydrate gel, figure 2 is a scanning electron microscope image of the nitrogenated carbohydrate gel, and figure 5 is a Fourier infrared spectrum of the nitrogenated carbohydrate gel.
Example 2:
firstly, uniformly dispersing 0.5g of gamma-polyglutamic acid in 10mL of water, and stirring for 1 h;
step two, uniformly dispersing 0.05g of carbon nitride in 10mL of water, and stirring for 2 hours;
thirdly, dropwise adding the uniformly dispersed carbon nitride aqueous solution into the uniformly dispersed gamma-polyglutamic acid aqueous solution;
step four, dripping 1g of trimethoxy silane into the mixed solution in the step three, and stirring for 3 hours;
and fifthly, transferring the uniformly dispersed solution into a mold, and freeze-drying and dehydrating to obtain the carbon nitride aerogel.
And sixthly, characterizing the prepared carbon nitride aerogel, wherein fig. 3 is a scanning electron microscope image of the carbon nitride aerogel, fig. 4 is an X-ray diffraction spectrum of the carbon nitride aerogel, and fig. 5 is a Fourier infrared spectrum of the carbon nitride aerogel.
Example 3:
firstly, uniformly dispersing 0.5g of gamma-polyglutamic acid in 10mL of water, and stirring for 1 h;
step two, uniformly dispersing 0.05g of carbon nitride in 10mL of water, and stirring for 2 hours;
thirdly, dropwise adding the uniformly dispersed carbon nitride aqueous solution into the uniformly dispersed gamma-polyglutamic acid aqueous solution;
step four, dripping 1g of trimethoxy silane into the mixed solution in the step three, and stirring for 3 hours;
and fifthly, transferring the uniformly dispersed solution into a mold, and drying in a vacuum oven at 38 ℃ for 12h to obtain the nitrogenated carbohydrate gel. (ii) a
Sixthly, placing the prepared nitrogenated carbohydrate gel into a beaker filled with 50mL of 50ppm Cr (VI) solution, and placing a xenon lamp light source 25cm above the beaker to perform an experiment of photocatalytic reduction of heavy metal ions. Taking 1mL of solution every 20min for measuring by an ultraviolet spectrophotometer, wherein the measured result is the concentration of Cr (VI) in the solution.
The effect of reducing hexavalent chromium ions by the nitrided carbohydrate gel prepared in example 3 is shown in fig. 6. The results of UV spectrophotometric measurements showed that 0.5g of nitrogenated carbohydrate gel completely reduced Cr (VI) ions in 50mL of 50ppm Cr (VI) solution within 80 min.
Example 4:
firstly, uniformly dispersing 0.5g of gamma-polyglutamic acid in 10mL of water, and stirring for 1 h;
step two, uniformly dispersing 0.05g of carbon nitride in 10mL of water, and stirring for 2 hours;
thirdly, dropwise adding the uniformly dispersed carbon nitride aqueous solution into the uniformly dispersed y-polyglutamic acid aqueous solution;
step four, dripping 1g of trimethoxy silane into the mixed solution in the step three, and stirring for 3 hours;
fifthly, transferring the uniformly dispersed solution into a mold, and freeze-drying and dehydrating to obtain carbon nitride aerogel;
sixthly, placing the prepared carbon nitride aerogel in a beaker filled with 50mL of 50ppm rhodamine B solution, and placing a xenon lamp light source 25cm above the beaker to perform a dye photocatalytic degradation experiment;
seventhly, after standing for half an hour, the carbon nitride aerogel completely adsorbs 50mL of 50ppm rhodamine B solution, and shows the color of rhodamine B dye in external light, which shows that the dye solution is only adsorbed;
and eighthly, after the xenon lamp light source is turned on, the color of the carbon nitride aerogel is completely faded after 20min of photocatalytic degradation, which shows that the rhodamine B dye is successfully degraded.
And ninthly, detecting the aqueous solution in the degraded aerogel by using an ultraviolet spectrophotometry in a physical extrusion mode, and comparing test results before and after degradation to successfully verify the degradation of the carbon nitride aerogel on the rhodamine B dye.
The effect of the carbon nitride aerogel prepared in example 4 on degrading rhodamine B dye solution is shown in fig. 7. The result of ultraviolet spectrophotometer measurement shows that after 20min of photocatalytic degradation, the carbon nitride aerogel has obvious degradation effect on 50mL of 50ppm rhodamine B solution, thereby showing that the prepared carbon nitride aerogel has good self-cleaning capability.
FIG. 8 is a diagram of the process of degrading rhodamine B dye solution by the carbon nitride aerogel prepared in example 4. Placing carbon nitride aerogel in rhodamine B dye solution for adsorption; b shows that 50mL of rhodamine B dye solution is completely adsorbed by the carbon nitride aerogel after 30min of adsorption, which also shows that the prepared carbon nitride aerogel has good water absorption; c is a schematic diagram of a device for performing photocatalytic degradation by a xenon lamp; d is a digital photograph of the gel after photocatalytic degradation.
Claims (8)
1. A preparation method of self-cleaning carbon nitride gel is characterized by comprising the following steps:
the first step, carbon nitride is uniformly dispersed in an aqueous solution;
a second step of uniformly dispersing the polymer monomer in an aqueous solution;
thirdly, dripping the carbon nitride aqueous solution obtained in the first step into the polymer monomer aqueous solution obtained in the second step;
step four, dripping a cross-linking agent into the mixed solution obtained in the step three, and stirring and dispersing uniformly;
and fifthly, transferring the uniformly dispersed solution into a mold and drying.
2. The method of claim 1, wherein in the first step the carbon nitride is obtained by calcining a nitrogen-rich precursor, and is prepared by: and (3) putting the urea into a crucible with a cover, placing the crucible in a tube furnace, raising the temperature to 500-550 ℃ by a program, and preserving the heat for 2-4h to obtain solid powder, namely the carbon nitride.
3. The method of claim 1, wherein in the second step, the polymer monomer is gamma-polyglutamic acid.
4. The method according to claim 1, wherein in the third step, the mass ratio of the carbon nitride to the polymer monomer is 1:10 to 1: 40.
5. The method of claim 1, wherein in the fourth step, the crosslinking agent is trimethylsilane and the mass ratio of the polymer monomer to the crosslinking agent is from 1:1 to 4: 1.
6. The method of claim 1, wherein in the fifth step, the drying is drying at 35-40 ℃.
7. The method of claim 1, wherein said drying is freeze drying.
8. A self-cleanable carbon nitride gel prepared by the method of any one of claims 1-7.
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