CN111530459B - Preparation method and application of 0D/2D composite material based on AlOOH nanosheets - Google Patents
Preparation method and application of 0D/2D composite material based on AlOOH nanosheets Download PDFInfo
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- 229910002706 AlOOH Inorganic materials 0.000 title claims abstract description 52
- 239000002135 nanosheet Substances 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 239000002131 composite material Substances 0.000 title claims abstract description 12
- 239000002114 nanocomposite Substances 0.000 claims abstract description 31
- 238000006243 chemical reaction Methods 0.000 claims abstract description 28
- 239000000463 material Substances 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- JGDITNMASUZKPW-UHFFFAOYSA-K aluminium trichloride hexahydrate Chemical compound O.O.O.O.O.O.Cl[Al](Cl)Cl JGDITNMASUZKPW-UHFFFAOYSA-K 0.000 claims abstract description 15
- 229940009861 aluminum chloride hexahydrate Drugs 0.000 claims abstract description 14
- 238000001035 drying Methods 0.000 claims abstract description 14
- BTJIUGUIPKRLHP-UHFFFAOYSA-N 4-nitrophenol Chemical compound OC1=CC=C([N+]([O-])=O)C=C1 BTJIUGUIPKRLHP-UHFFFAOYSA-N 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 13
- MPTQRFCYZCXJFQ-UHFFFAOYSA-L copper(II) chloride dihydrate Chemical compound O.O.[Cl-].[Cl-].[Cu+2] MPTQRFCYZCXJFQ-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000004202 carbamide Substances 0.000 claims abstract description 8
- 239000012716 precipitator Substances 0.000 claims abstract description 6
- 239000002904 solvent Substances 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 12
- 239000002243 precursor Substances 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 238000003756 stirring Methods 0.000 claims description 9
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims description 6
- -1 polytetrafluoroethylene Polymers 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- 239000007787 solid Substances 0.000 claims description 6
- 229910001220 stainless steel Inorganic materials 0.000 claims description 6
- 239000010935 stainless steel Substances 0.000 claims description 6
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 6
- 238000004108 freeze drying Methods 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
- 150000001879 copper Chemical class 0.000 claims description 4
- 231100000252 nontoxic Toxicity 0.000 claims description 4
- 230000003000 nontoxic effect Effects 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- 150000003839 salts Chemical class 0.000 claims description 2
- 229910021591 Copper(I) chloride Inorganic materials 0.000 claims 1
- OXBLHERUFWYNTN-UHFFFAOYSA-M copper(I) chloride Chemical compound [Cu]Cl OXBLHERUFWYNTN-UHFFFAOYSA-M 0.000 claims 1
- 239000002086 nanomaterial Substances 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 9
- 230000008901 benefit Effects 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 5
- 229910000033 sodium borohydride Inorganic materials 0.000 abstract description 5
- 239000012279 sodium borohydride Substances 0.000 abstract description 5
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 229910001593 boehmite Inorganic materials 0.000 abstract description 2
- 238000005984 hydrogenation reaction Methods 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052802 copper Inorganic materials 0.000 abstract 1
- 239000010949 copper Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 11
- 239000002105 nanoparticle Substances 0.000 description 10
- 239000006185 dispersion Substances 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 6
- 239000003054 catalyst Substances 0.000 description 5
- 238000006722 reduction reaction Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 238000011065 in-situ storage Methods 0.000 description 3
- 239000002055 nanoplate Substances 0.000 description 3
- 229910052757 nitrogen Inorganic materials 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000006228 supernatant Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- ORTQZVOHEJQUHG-UHFFFAOYSA-L copper(II) chloride Chemical compound Cl[Cu]Cl ORTQZVOHEJQUHG-UHFFFAOYSA-L 0.000 description 2
- 238000013461 design Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000010531 catalytic reduction reaction Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 229960003280 cupric chloride Drugs 0.000 description 1
- 238000002408 directed self-assembly Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000007306 functionalization reaction Methods 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical compound O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011112 process operation Methods 0.000 description 1
- 239000002096 quantum dot Substances 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000012876 topography Methods 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- B01J35/393—
-
- B01J35/394—
-
- 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
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C213/00—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton
- C07C213/02—Preparation of compounds containing amino and hydroxy, amino and etherified hydroxy or amino and esterified hydroxy groups bound to the same carbon skeleton by reactions involving the formation of amino groups from compounds containing hydroxy groups or etherified or esterified hydroxy groups
Abstract
The invention belongs to the technical field of preparation of nano materials, and discloses a preparation method of a 0D/2D composite material based on AlOOH nanosheets, wherein a hydrothermal method is utilized to prepare a sea urchin-shaped copper oxide-boehmite (CuO/AlOOH) nano composite material; copper chloride dihydrate and aluminum chloride hexahydrate are used as raw materials, urea is used as a precipitator, deionized water is used as a solvent, a constant-temperature reaction is carried out under the condition of a specific temperature, and the sea urchin-shaped CuO/AlOOH nano material is prepared through centrifugal separation, sample washing and drying. The 0D/2D nano composite material prepared by the invention efficiently catalyzes sodium borohydride to reduce p-nitrophenol through two processes of adsorption and hydrogenation. The preparation method has the advantages of simple preparation process, short period, low cost, large-scale industrial production and good economic benefit and environmental benefit.
Description
Technical Field
The invention belongs to the technical field of nano material preparation, and particularly relates to a preparation method and application of a 0D/2D composite material based on AlOOH nanosheets.
Background
The zero-dimensional (0D) nano material is also called as quantum dot, and is a catalyst with wide application prospect due to the superfine size (< 10 nm), large surface area, high charge transfer rate, unique optical characteristics and excellent catalytic performance. However, achieving good dispersion of the zero-dimensional (0D) nanomaterial to avoid its intrinsic aggregation is still a great challenge, which also limits the practical application of the zero-dimensional (0D) nanomaterial in the field of catalysis. Therefore, an effective supporting material is searched and compounded with the composite material, so that the large surface area and the excellent characteristics of the 0D nano material can be kept, the problems can be solved, and the composite material becomes a current research hotspot.
Ultra-thin two-dimensional (2D) nanomaterials, which have a thickness of only one or a few atoms (typically less than 5 nm), exhibit unusual mechanical, optical and electronic properties, and are both ideal low-dimensional systems for fundamental research and fundamental building blocks for design assembly. The ultrathin two-dimensional (2D) nano material can also realize the directional self-assembly with heterogeneous materials and the precise regulation and control of molecular level, so the ultrathin two-dimensional (2D) nano material is an effective support structure of a 0D nano material. Boehmite (AlOOH), a classic 2D material, is attracting attention for its good properties such as high thermal and chemical stability, environmental friendliness, low cost and low toxicity, and has important applications in many fields including adsorbents, composites and catalysts. Therefore, alOOH is selected as a carrier of the 0D nano-particles.
The recombination of 0D/2D nano-materials has proved to be an effective strategy, and the most reported recombination method at present is as follows: loading 0D nanoparticles on the basis of 2D nanomaterials remains a challenge to prepare highly dispersed 0D/2D nanocomposites because 0D nanoparticles are prone to agglomeration in solvents. Therefore, the design of the preparation method which has simple process and can synchronously synthesize the high-dispersion 0D/2D nano material in situ has important significance.
Disclosure of Invention
The invention aims to provide a green synthesis method for synchronously preparing a high-dispersion 0D/2D nano composite material in situ, which has a simple process and aims at solving the problems of the existing preparation method of the 0D/2D nano composite material and insufficient dispersibility of nano particles. The CuO/AlOOH nano composite material with uniform appearance, controllable size and highly dispersed nano particles is formed by self-assembly through one-step hydrothermal synthesis. The prepared CuO/AlOOH nano composite material has excellent catalytic performance, low cost and simple method, provides a preparation method with controllable shape and size, has good economic benefit and environmental benefit, and can be produced and applied on a large scale.
In order to realize the purpose, the invention adopts the following technical scheme:
a preparation method of a 0D/2D composite material based on AlOOH nanosheets comprises the following raw materials: cupric chloride dihydrate (CuCl) 2 ·2H 2 O), aluminum chloride hexahydrate (AlCl) 3 ·6H 2 O), urea (CH) 4 N 2 O)。
A preparation method of a 0D/2D composite material based on AlOOH nanosheets comprises the following steps: mixing and dissolving copper chloride dihydrate, aluminum chloride hexahydrate and precipitator urea in deionized water to prepare uniformly dispersed reaction precursor liquid; then transferring the reaction precursor liquid into a stainless steel high-pressure autoclave with a polytetrafluoroethylene lining, and carrying out constant-temperature reaction in a drying oven; after the reaction is finished, cooling, centrifugally separating, washing and drying until the water is completely volatilized, and the white solid powdery CuO/AlOOH nano composite material with uniform size and high dispersion is obtained.
The CuO/AlOOH nano composite material with uniform size and high dispersion specifically comprises the following steps:
(1) Adding a divalent copper salt, a trivalent aluminum salt and a precipitator into deionized water, and fully mixing and dissolving to prepare uniformly dispersed reaction precursor liquid;
(2) Then transferring the reaction precursor liquid into a stainless steel high-pressure autoclave with a polytetrafluoroethylene lining, and carrying out constant-temperature reaction in a drying oven;
(3) After the reaction is finished, cooling, centrifugally separating, washing and drying until the water is completely volatilized to obtain a white solid powdery 0D/2D-CuO/AlOOH nano composite material.
Further, the cupric salt in the step (1) is nontoxic copper chloride dihydrate CuCl 2 ·2H 2 O; the trivalent aluminum salt is nontoxic aluminum chloride hexahydrate AlCl 3 ·6H 2 O; the precipitator is urea CH 4 N 2 O。
Further, in the step (1), the molar ratio of the divalent copper salt to the trivalent aluminum salt to the precipitant is 0.3.
Further, the mixing and dissolving in the step (1) specifically comprises: ultrasonic dispersion and magnetic stirring are carried out, and the ultrasonic dispersion time is 10min; the stirring speed is 500rpm; the stirring time was 10min.
Further, the isothermal reaction in the step (2) is specifically as follows: the reaction is carried out for 24h at a constant temperature of 120 ℃.
Further, the cooling in the step (3) is specifically as follows: and cooling the mixture along with the furnace to room temperature.
Further, the washing solvent in the step (3) is deionized water, and the washing times are 3 times.
Further, the drying mode in the step (3) is vacuum-53 ℃ freeze drying, and the drying time is 12h.
Wherein the particle size of the CuO nanoparticles is in the range of
Uniformly dispersed on acicular AlOOH nanosheets, which were about 2um long and about 500nm wide, as shown in FIG. 5.
The invention has the beneficial effects that:
(1) The invention adopts a one-step hydrothermal synthesis method, and synchronously generates the CuO/AlOOH nano composite material with uniform and high dispersion in situ. Enriches the method for compounding zero-dimensional and two-dimensional nano materials and provides a new idea for directional assembly and functionalization of nano particles.
(2) According to the CuO/AlOOH nano composite material prepared by the invention, a synergistic effect is caused by lattice matching between nano particles and nano sheets, the surface area is increased, the charge transfer rate is increased, and sodium borohydride is efficiently catalyzed to reduce p-nitrophenol through two processes of adsorption and hydrogenation.
(3) The preparation method has the advantages of easily obtained equipment and materials, simple process operation, concise process conditions, low cost, safety and high efficiency, and can be used for large-scale industrial production; compared with other noble metal elements, the material has less environmental pollution, is an ecological environment-friendly material, and has good popularization and application values.
Drawings
FIG. 1 is an X-ray diffraction (XRD) pattern of a CuO/AlOOH nanocomposite prepared in example 1 of the present invention and AlOOH nanoplates prepared in comparative example 1;
FIG. 2 is a micro-morphology and an EDS energy spectrum of a CuO/AlOOH nanocomposite prepared in example 1 of the present invention;
FIG. 3 is a microstructure of AlOOH nanoplates made by comparative example 1 of the present invention;
FIG. 4 is a micro-topography and EDS energy spectra of a 0.2CuO/AlOOH nanocomposite prepared according to comparative example 2 of the present invention;
FIG. 5 is a transmission electron microscope image of a CuO/AlOOH nanocomposite prepared in example 1 of the present invention;
FIG. 6 is a transmission electron microscope image of an AlOOH nanocomposite prepared in example 1 of the present invention;
FIG. 7 is a BET plot of CuO/AlOOH nanocomposites made with example 1 of the invention and AlOOH nanoplates made with comparative example 1;
FIG. 8 is a graph comparing the performance of CuO/AlOOH nanocomposites made with example 1 of the present invention, alOOH nanosheets made with comparative example 1, and 0.2CuO/AlOOH nanocomposites made with comparative example 2;
FIG. 9 is a graph of the cycle performance of the CuO/AlOOH nanocomposite prepared in example 1 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail below with reference to the accompanying drawings, which are examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined as long as they do not conflict with each other.
Example 1
Preparing a CuO/AlOOH nano composite material:
(1) 0.0507g of copper chloride dihydrate (CuCl) was weighed using an electronic balance 2 ·2H 2 O), 0.24g of aluminum chloride hexahydrate (AlCl) 3 ·6H 2 O), adding copper chloride dihydrate and aluminum chloride hexahydrate according to the molar ratio of 0.3 to 1 into 50mL of deionized water, and performing ultrasonic dispersion for 10 minutes to obtain a solution A;
(2) 0.24g of urea (CH) is weighed out with an electronic balance 4 N 2 O), adding the mixture into the solution A, and magnetically stirring for 10min at the stirring speed of 500rpm to prepare uniformly dispersed reaction precursor solution;
(3) Then transferring the reaction precursor liquid into a stainless steel autoclave with a polytetrafluoroethylene lining, carrying out constant-temperature reaction for 24 hours in a drying oven at 120 ℃, and cooling to room temperature along with the oven after the reaction is finished;
(4) Centrifuging the sample by using a centrifugal machine to obtain white solid powder, wherein the rotating speed is 10000rpm; and washing with deionized water for three times;
(5) And freeze-drying overnight until the water is completely volatilized to obtain the CuO/AlOOH nano composite material. As can be seen from fig. 4, the CuO nanoparticles are lattice-matched with the AlOOH nanosheets, and the CuO nanoparticles are uniform in size and highly dispersed on the AlOOH nanosheets.
Comparative example 1
Preparing an AlOOH nano sheet:
(1) 0.24g of aluminium chloride hexahydrate (AlCl) was weighed out on an electronic balance 3 ·6H 2 O) and 0.24g of urea (CH) 4 N 2 O), adding the mixture into 50ml of deionized water, and stirring for 10 minutes to react with the precursor solution;
(2) Then transferring the reaction precursor liquid into a stainless steel autoclave with a polytetrafluoroethylene lining, carrying out constant-temperature reaction for 24 hours in a drying oven at 120 ℃, and cooling to room temperature along with the oven after the reaction is finished;
(3) Centrifuging the sample by using a centrifugal machine to obtain white solid powder, wherein the rotating speed is 10000rpm; and washing with deionized water for three times;
(4) And (4) freeze-drying overnight until the moisture is completely volatilized, so as to obtain the AlOOH nano composite material with uniform size and high dispersion.
Comparative example 2
0.2 preparation of CuO/AlOOH nano sheet:
(1) 0.0341g of copper chloride dihydrate (CuCl) was weighed out on an electronic balance 2 ·2H 2 O), 0.24g of aluminum chloride hexahydrate (AlCl) 3 ·6H 2 O), adding copper chloride dihydrate and aluminum chloride hexahydrate in a molar ratio of 0.2 to 1 in 50mL of deionized water, and performing ultrasonic dispersion for 10 minutes to obtain a solution A;
(2) 0.24g of urea (CH) was weighed out with an electronic balance 4 N 2 O), adding the mixture into the solution A, and magnetically stirring for 10min at the stirring speed of 500rpm to prepare uniformly dispersed reaction precursor solution;
(3) Then transferring the reaction precursor liquid into a stainless steel autoclave with a polytetrafluoroethylene lining, carrying out constant-temperature reaction for 24 hours in a drying oven at 120 ℃, and cooling to room temperature along with the oven after the reaction is finished;
(4) Centrifuging the sample by using a centrifugal machine to obtain white solid powder, wherein the rotating speed is 10000rpm; and washing with deionized water for three times;
(5) Through freeze drying overnight until the water is completely volatilized, 0.2CuO/AlOOH nano composite material is obtained.
P-nitrophenol reduction experiment
Application example 1
The CuO/AlOOH nano composite material obtained in the example 1 is used for p-nitrophenol reduction, and the specific steps are as follows:
(1) Taking 50ml of p-nitrophenol in a beaker, adding 80mg of sodium borohydride, introducing nitrogen for 10 minutes, and continuing the next step until the color of the solution is kept yellow all the time;
(2) Adding 10mg of CuO/AlOOH catalyst, and starting timing;
(3) Taking supernatant with needle tube at 1min, 3min, 5min, 10min, and 15min, filtering with filter head, and performing liquid ultraviolet test.
Application example 2
The AlOOH nanosheet obtained in the comparative example 1 is used for p-nitrophenol reduction, and the specific steps are as follows:
(1) Taking 50ml of p-nitrophenol in a beaker, adding 80mg of sodium borohydride, introducing nitrogen for 10 minutes, and continuing the next step until the color of the solution is kept yellow all the time;
(2) Adding 10mg of AlOOH catalyst, and starting timing;
(3) Taking supernatant with needle tube at 1min, 3min, 5min, 10min, and 15min, filtering with filter head, and performing liquid ultraviolet test.
Application example 3
The 0.2CuO/AlOOH nanosheet obtained in the comparative example 2 is used for p-nitrophenol reduction, and the specific steps are as follows:
(1) Taking 50ml of p-nitrophenol in a beaker, adding 80mg of sodium borohydride, introducing nitrogen for 10 minutes, and continuing the next step until the color of the solution is kept yellow all the time;
(2) Adding 10mg of 0.2CuO/AlOOH catalyst, and starting timing;
(3) Taking supernatant with needle tube at 1min, 3min, 5min, 10min, and 15min, filtering with filter head, and performing liquid ultraviolet test.
Fig. 7 is BET diagrams of the CuO/AlOOH nanocomposite prepared in example 1 of the present invention and the AlOOH nanosheet prepared in comparative example 1, and it can be seen that the CuO/AlOOH nanocomposite has a large specific surface area, which is advantageous for its catalytic performance, and it can be verified from the performance comparison diagram of fig. 8. The CuO/AlOOH nano composite material can catalyze and reduce 95% of p-nitrophenol in 1 minute, can catalyze and reduce 100% of p-nitrophenol in three minutes, and has performance far superior to that of AlOOH nano sheets and 0.2CuO/AlOOH composite materials. As can be seen from FIG. 9, the CuO/AlOOH nanocomposite prepared by the invention has excellent cycle performance, and still maintains excellent catalytic reduction performance on p-nitrophenol after 6 cycles.
It will be understood by those skilled in the art that the foregoing is merely a preferred embodiment of the invention, and is not intended to limit the invention, and that any modification, equivalent replacement or improvement made within the spirit and principle of the invention should be included within the scope of protection of the invention.
Claims (5)
1. An application of 0D/2D composite material based on AlOOH nano-sheets in catalyzing reduction of p-nitrophenol is characterized in that: the preparation method of the composite material comprises the following steps:
(1) Adding a divalent copper salt, a trivalent aluminum salt and a precipitator into deionized water, and fully mixing and dissolving to prepare uniformly dispersed reaction precursor liquid;
(2) Then transferring the reaction precursor liquid into a stainless steel high-pressure autoclave with a polytetrafluoroethylene lining, and carrying out constant-temperature reaction in a drying oven;
(3) After the reaction is finished, cooling, centrifugally separating, washing and drying until the moisture is completely volatilized to obtain a white solid powdery 0D/2D-CuO/AlOOH nano composite material;
the cupric salt in the step (1) is nontoxic copper chloride dihydrate CuCl 2 ·2H 2 O; the trivalent aluminum salt is nontoxic aluminum chloride hexahydrate AlCl 3 ·6H 2 O; the precipitator is urea CH 4 N 2 O；
In the step (1), the molar ratio of the divalent copper salt to the trivalent aluminum salt to the precipitant is 0.3;
the drying mode in the step (3) is vacuum-53 ℃ freeze drying, and the drying time is 12h.
2. Use according to claim 1, characterized in that: the mixing and dissolving in the step (1) are specifically as follows: ultrasonic dispersion and magnetic stirring are carried out, and the ultrasonic dispersion time is 10min; the stirring speed is 500rpm; the stirring time was 10min.
3. Use according to claim 1, characterized in that: the constant-temperature reaction in the step (2) is specifically as follows: the reaction is carried out at 120 ℃ under constant temperature for 24h.
4. Use according to claim 1, characterized in that: the cooling in the step (3) is specifically as follows: and cooling the mixture along with the furnace to room temperature.
5. Use according to claim 1, characterized in that: and (4) the washing solvent in the step (3) is deionized water, and the washing times are 3.
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| CN107252690A (en) * | 2017-05-09 | 2017-10-17 | 北京化工大学 | A kind of base catalyst of supported copper oxide containing auxiliary agent and preparation method thereof |
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| CN110882702A (en) * | 2019-12-16 | 2020-03-17 | 生态环境部环境规划院 | Preparation method and application of catalytic material based on magnetic layered double hydroxide |
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| CN110227509A (en) * | 2019-06-24 | 2019-09-13 | 中北大学 | A kind of carbon dots/copper oxide/mesoporous hydroxyapatite catalysis material preparation method of efficient reduction p-nitrophenol |
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