CN108714431B - Nano-cellulose reinforced composite photocatalyst and preparation method and application thereof - Google Patents
Nano-cellulose reinforced composite photocatalyst and preparation method and application thereof Download PDFInfo
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 30
- 239000001913 cellulose Substances 0.000 title claims abstract description 30
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 23
- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical compound [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 15
- 239000000725 suspension Substances 0.000 claims abstract description 15
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 239000002243 precursor Substances 0.000 claims abstract description 12
- 229910001961 silver nitrate Inorganic materials 0.000 claims abstract description 12
- 230000015556 catabolic process Effects 0.000 claims abstract description 11
- 238000006731 degradation reaction Methods 0.000 claims abstract description 11
- 230000001699 photocatalysis Effects 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 229920001046 Nanocellulose Polymers 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 9
- 230000003197 catalytic effect Effects 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 7
- 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
- 239000002134 carbon nanofiber Substances 0.000 claims description 11
- 230000008569 process Effects 0.000 claims description 4
- 238000004519 manufacturing process Methods 0.000 claims description 3
- GDOPTJXRTPNYNR-UHFFFAOYSA-N methyl-cyclopentane Natural products CC1CCCC1 GDOPTJXRTPNYNR-UHFFFAOYSA-N 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000005416 organic matter Substances 0.000 claims 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 27
- 230000000694 effects Effects 0.000 abstract description 14
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 14
- 229910052799 carbon Inorganic materials 0.000 abstract description 6
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 abstract description 5
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 5
- 238000004804 winding Methods 0.000 abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 description 13
- 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 11
- 229940043267 rhodamine b Drugs 0.000 description 11
- 230000000052 comparative effect Effects 0.000 description 10
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 3
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- 239000000969 carrier Substances 0.000 description 3
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- 230000000593 degrading effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 229910052755 nonmetal Inorganic materials 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 230000001678 irradiating effect Effects 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
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- 229910001316 Ag alloy Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
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- 238000005530 etching Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 150000002843 nonmetals Chemical class 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- OGFYIDCVDSATDC-UHFFFAOYSA-N silver silver Chemical compound [Ag].[Ag] OGFYIDCVDSATDC-UHFFFAOYSA-N 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000011800 void material Substances 0.000 description 1
- 238000005406 washing Methods 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
- 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
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/082—Decomposition and pyrolysis
- B01J37/084—Decomposition of carbon-containing compounds into carbon
-
- 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
-
- 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
-
- 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
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a preparation method of a nano-cellulose reinforced composite photocatalyst, which comprises the following steps: (1) dissolving silver nitrate and urea in a suspension of nano-cellulose, and then drying to obtain a precursor substance; (2) calcining the precursor substance at the temperature of 450-600 ℃ in the oxygen or air atmosphere to obtain the nano-cellulose reinforced composite photocatalytic material. The invention also discloses the nano-cellulose reinforced composite photocatalyst prepared by the method and application thereof. The invention innovatively utilizes rich carboxyl and hydroxyl on a nano cellulose chain and a network structure formed by winding the carboxyl and the hydroxyl around each other to couple Ag+Has strong chemical adsorption and physical winding effects, and can adsorb Ag+Fixing on the surface of carbonized nitrogen to reduce Ag+The carbon doping is realized, and the carbon and the Ag synergistically promote the catalytic degradation efficiency of the carbonized nitrogen.
Description
Technical Field
The invention belongs to the field of material chemistry, and particularly relates to a nano-cellulose enhanced composite photocatalyst Ag/CNFs/g-C3N4And a preparation method and application thereof.
Background
Increasingly serious environmental pollution and energy shortage become two major problems restricting the development of human society, and the search for clean energy and the effective improvement of environmental pollution are important problems to be solved at present. Solar energy is considered the first choice for replacing fossil energy because of its non-pollution, low cost, huge reserves, etc. The semiconductor catalyst can effectively convert solar energy into chemical energy, and can be used for catalyzing and degrading pollutants in water, producing hydrogen by photocatalysis and the like.
Non-metal semiconductor catalyst carbonized nitrogen (g-C)3N4) Has response to visible light, and is used for preparing clean energy by catalysis and degrading organic pollutants by photocatalysis. However, the nitrogen carbide catalyst has the defects of low catalytic efficiency, low specific surface area, easy recombination of photon-generated carriers and the like, and the photocatalytic performance of the nitrogen carbide catalyst is seriously influenced. Researchers at home and abroad widely adopt ways such as structure and chemical regulation, void structure modification, element doping and the like to improve g-C3N4The semiconductor catalyst has obvious element doping modification effect on the photocatalysis performance. In the element doping modification process, nonmetal elements (C, N, P, S and the like) or metal elements (Ag, K and Co) are usually adopted to improve the effect, and particularly, the metal element Ag is adopted to realize remarkable modification effect. But commonly used Ag-doped modified g-C3N4The preparation process of the composite catalyst is complex, and Ag is easy to lose in the high-temperature calcination process, so that the modification effect is greatly limited, and the single non-metal element doping or metal element doping is difficult to achieve the synergistic promotion effect.
Disclosure of Invention
The invention aims to solve the technical problem of overcoming the defects and shortcomings in the background technology and providing a nano-cellulose reinforced composite photocatalyst Ag/CNFs/g-C3N4And a preparation method and application thereof.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of a nano-cellulose reinforced composite photocatalyst comprises the following steps:
(1) dissolving silver nitrate and urea in a suspension of nano-cellulose, and then drying to obtain a precursor substance;
(2) at 450 ℃ and 650 DEG CCalcining the precursor substance in the atmosphere of oxygen or air to obtain the nano-cellulose reinforced composite photocatalytic material Ag/CNFs/g-C3N4. The catalyst is calcined in oxygen or air, and the carbonized nitrogen is etched by the oxygen or the air, so that abundant pores are generated on the surface of the carbonized nitrogen, and the specific surface area is large, thereby increasing the active sites of the catalyst and obviously improving the catalytic degradation activity of the catalyst on organic matters.
In the above preparation method, preferably, the nanocellulose suspension is an oxidized nanocellulose suspension.
In the preparation method, the suspension of the nano-cellulose is preferably a suspension of TEMPO oxidized nano-cellulose. The surface of the nano-cellulose is rich in carboxyl and hydroxyl, has extremely high length-diameter ratio and can be used for treating Ag+Form chemical adsorption and physical winding effects, and can fix Ag+Reduction of Ag+The loss in the preparation process can promote the catalytic degradation capability of the composite catalyst to organic matters.
In the preparation method, preferably, the aspect ratio of the nanocellulose in the nanocellulose suspension is 200-1000.
In the above production method, the silver nitrate is preferably present in an amount of 0.2% by mass or less based on the mass of urea. The applicant finds that the loss of Ag in the calcining process can be effectively reduced due to the introduction of the nano-cellulose, and a remarkable improvement effect can be achieved only by a small amount of silver nitrate; meanwhile, if the addition amount of silver nitrate is too large, Ag agglomeration may be caused, and the effect is not good.
In the preparation method, the solid content of the cellulose nanofibrils in the nano-cellulose suspension is preferably 0.002-0.05 wt%, and the mass ratio of the urea to the nano-cellulose suspension is 1: 1-2: 1. The main function of adding the nano-cellulose in the invention is to fix Ag in g-C3N4Meanwhile, C doping is realized. The applicant found through research that if the addition amount of the nanocellulose is small, the fixing effect on Ag cannot be realized, and if the addition amount of the nanocellulose is too large, too much C doping is generated, and too much C doping causes too much C dopingBecomes a center of recombination of photogenerated carriers, thereby inhibiting photocatalysis. Therefore, only a proper amount of C doping is beneficial to the separation of photon-generated carriers, thereby improving the photocatalysis.
In the above production method, preferably, in the step (2), the calcination time is 3 to 8 hours.
In the preparation method, preferably, the drying is air-blast drying, the drying temperature is 60-70 ℃, and the drying time is 8-12 h.
As a general inventive concept, the present invention also provides a photocatalyst, which is obtained by the above preparation method, and has a large number of mesopores distributed therein and a large specific surface area.
As a general inventive concept, the invention also provides an application of the photocatalyst in catalyzing and degrading organic matters.
Compared with the prior art, the invention has the advantages that:
(1) the preparation method of the invention is to prepare the porous and high-activity carbonized nitrogen nano catalyst by one-step calcination; the method utilizes the etching of air or oxygen to the carbonized nitrogen at the temperature of 450-600 ℃, particularly 550 ℃, so as to generate rich pores on the surface of the carbonized nitrogen, increase the active sites of the catalyst and obviously improve the catalytic degradation activity of the catalyst to organic matters.
(2) The invention innovatively utilizes rich carboxyl and hydroxyl on a nano cellulose chain and a network structure formed by winding the carboxyl and the hydroxyl around each other to couple Ag+Has strong chemical adsorption and physical winding effects, and can adsorb Ag+Fixing on the surface of carbonized nitrogen to reduce Ag+The loss of the carbon is realized, and the carbon and the Ag synergistically promote the catalytic degradation efficiency of the carbonized nitrogen.
(3) The composite photocatalyst has excellent degradation performance on organic matters under visible light and has excellent stability.
(4) The composite photocatalyst can be repeatedly recycled.
Drawings
Fig. 1 is an XRD chart of the photocatalysts prepared in comparative examples 1-2 and example 1 of the present invention.
FIG. 2 is an SEM image of photocatalysts prepared in comparative examples 1-2 and example 1 according to the present invention.
FIG. 3 shows the degradation rate of rhodamine B under xenon lamp irradiation (not less than 420nm) of the photocatalysts prepared in comparative examples 1-2 and example 1 of the invention.
Detailed Description
In order to facilitate an understanding of the invention, the invention will be described more fully and in detail below with reference to the accompanying drawings and preferred embodiments, but the scope of the invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Comparative example 1:
the preparation method of the photocatalyst of the comparative example includes the following steps:
(1) dissolving 20g of urea in 20mL of deionized water to obtain a urea solution;
(2) putting the urea solution into a forced air drying oven, and drying for 12h at 70 ℃ to obtain a precursor substance;
(3) covering the crucible containing the precursor substance with a cover, wrapping a layer of tin foil paper, calcining for 4h in a muffle furnace at 550 ℃ under the air atmosphere, wherein the heating rate is 15 ℃/min, and naturally cooling to obtain the g-C3N4The XRD pattern and SEM photograph of the catalytic material are shown in figure 1 and figure 2(a: g-C)3N4) As shown.
And (3) putting 50mg of the carbonized nitrogen catalyst prepared in the comparative example into 100mL of 20mg/L rhodamine B solution, carrying out dark reaction for 30min, irradiating for 30min under visible light with lambda being more than or equal to 420nm, and measuring the concentration of the rhodamine B in supernatant after centrifugation. The test result shows that the degradation rate of RhB after 30min of illumination is 96%.
Comparative example 2:
the preparation method of the photocatalyst of the comparative example includes the following steps:
(1) taking 0.04g of silver nitrate, and fully stirring to dissolve the silver nitrate into 20g of deionized water to obtain a silver nitrate solution;
(2) dissolving 20g of urea in the silver nitrate solution obtained in the step (1), and fully stirring and dissolving;
(3) placing the mixed solution prepared in the step (2) in a forced air drying oven, and drying at 70 ℃ for 12h to obtain a precursor substance;
(4) covering the crucible containing the precursor substance with a cover, wrapping a layer of tin foil paper, placing the crucible in a muffle furnace, calcining at 550 ℃ for 4h in air atmosphere at a heating rate of 15 ℃/min, and naturally cooling to obtain Ag/g-C3N4The XRD pattern and SEM picture of the composite photocatalytic material are respectively shown in figure 1 and figure 2(b: Ag/g-C)3N4) As shown.
50mg of Ag/g-C prepared in this comparative example was taken3N4The composite photocatalytic material is put into 100mL of 20mg/L rhodamine B solution, after dark reaction for 30min, the solution is irradiated for 30min under visible light with lambda being more than or equal to 420nm, and the concentration of rhodamine B in supernatant liquid is measured after centrifugation. The test result shows that the degradation rate of RhB after 30min of illumination is 100%.
Example 1:
the preparation method of the nano-cellulose reinforced composite photocatalyst comprises the following steps:
(1) taking 20g of TEMPO oxidized nano-cellulose suspension (CNFs, the solid content of the cellulose nano-fibrils is 0.01 wt%, and the length-diameter ratio of the nano-fibers is about 300-600) and 0.04g of silver nitrate, and stirring to fully dissolve the nano-cellulose suspension;
(2) dissolving 20g of urea in the mixed solution, and fully stirring and dissolving;
(3) placing the mixed solution obtained in the step (2) in a forced air drying oven, and drying at 70 ℃ for 12h to obtain a precursor substance;
(4) covering a crucible containing the precursor substance with a cover, wrapping a layer of tin foil paper, placing the crucible in a muffle furnace, calcining at 550 ℃ for 4h in air atmosphere at a heating rate of 15 ℃/min, and naturally cooling to obtain the nano-gradeCellulose reinforced composite photocatalyst Ag/CNFs/g-C3N4The XRD pattern and SEM photograph are shown in figure 1 and figure 2 (C: Ag/CNFs/g-C)3N4) As shown. As can be seen from the SEM image of FIG. 2, g-C prepared in this example and comparative example3N4All have a fluffy pore structure. As can be seen from FIG. 1, the addition of Ag/CNFs/g-C3N4The XRD curve of the silver-silver alloy can obviously detect the characteristic peak of Ag, and Ag/g-C3N4The characteristic peak of Ag is not detected, which indicates that the invention adds CNFs to fix more Ag at g-C3N4The above. Moreover, the g-C is realized while adding CNFs3N4The synergistic effect of C and Ag obviously improves the g-C3N4The photocatalytic degradation of (a) is shown in fig. 3.
50mg of the nano-cellulose reinforced composite photocatalyst Ag/CNFs/g-C prepared in the embodiment3N4The method is characterized by adding the rhodamine B (RhB) solution into 100mL and 20mg/L, after dark reaction for 30min, irradiating the solution for 30min under visible light with lambda being more than or equal to 420nm, and measuring the concentration of the rhodamine B in supernatant after centrifugation, wherein test results show that the degradation rate of RhB is 100% after 21min of illumination.
The nanocellulose-reinforced composite photocatalyst prepared in the embodiment is subjected to photocatalytic reaction, then is subjected to centrifugal washing, and after drying, is recycled for 5 times, and then has unchanged photocatalytic degradation performance.
Claims (6)
1. A preparation method of a nano-cellulose reinforced composite photocatalyst is characterized by comprising the following steps:
(1) dissolving silver nitrate and urea in a suspension of TEMPO oxidized nano-cellulose, and then drying to obtain a precursor substance; the mass of the silver nitrate accounts for less than 0.2% of the mass of the urea; the solid content of cellulose nanofibrils in the nano-cellulose suspension is 0.002 wt% -0.05 wt%, and the mass ratio of urea to the nano-cellulose suspension is 1: 1-2: 1;
(2) calcining the precursor substance at the temperature of 450-600 ℃ in the atmosphere of oxygen or air to obtain the nano-cellulose reinforced composite photocatalytic material Ag/CNFs/g-C3N4。
2. The method of claim 1, wherein the nanocellulose suspension has an aspect ratio of 200-1000.
3. The method according to claim 1, wherein in the step (2), the calcination time is 3 to 8 hours.
4. The process according to any one of claims 1 to 3, wherein the drying is air-blast drying, the drying temperature is 60 to 70 ℃ and the drying time is 8 to 12 hours.
5. A photocatalyst obtained by the production method according to any one of claims 1 to 4.
6. Use of the photocatalyst of claim 5 in the catalytic degradation of organic matter.
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| CN114988515A (en) * | 2022-04-21 | 2022-09-02 | 南京林业大学 | Method for removing Cr (VI) and g-C adopted by same 3 N 4 Composite foam/cellulose/GO |
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