CN113546659B - Highly dispersed CeCN-urea-N by coordination method 2 Material, preparation method and application thereof - Google Patents

Highly dispersed CeCN-urea-N by coordination method 2 Material, preparation method and application thereof Download PDF

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CN113546659B
CN113546659B CN202110673560.3A CN202110673560A CN113546659B CN 113546659 B CN113546659 B CN 113546659B CN 202110673560 A CN202110673560 A CN 202110673560A CN 113546659 B CN113546659 B CN 113546659B
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urea
cecn
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CN113546659A (en
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董林
李婉芹
濮钰
邹伟欣
魏小倩
朱成章
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Nanjing University
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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
    • 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
    • B01D53/46—Removing components of defined structure
    • B01D53/62—Carbon oxides
    • 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
    • B01D53/8671—Removing components of defined structure not provided for in B01D53/8603 - B01D53/8668
    • B01J35/39—
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
    • C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/50—Carbon oxides
    • B01D2257/504—Carbon dioxide
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2527/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
    • C07C2527/24—Nitrogen compounds

Abstract

The invention discloses a CeCN-urea-N treated by a coordination method 2 A material, a preparation method and application thereof, belonging to the field of material preparation and photocatalytic reduction of CO 2 The technical field of resource utilization. The method comprises (1) reacting Ce (NO) 3 ) 3 ·6H 2 And respectively adding O and urea into absolute ethyl alcohol to obtain dispersion liquid A and dispersion liquid B, slowly dropwise adding the dispersion liquid A into the dispersion liquid B, and uniformly stirring to obtain a solution C. (2) G to C 3 N 4 Adding into anhydrous ethanol to obtain dispersion solution D, adding dropwise solution C into dispersion solution D, and heating in water bath to obtain solid; (3) The solid is placed in a tube furnace at N 2 Calcining, cooling to obtain CeCN-urea-N 2 . The invention adopts a coordination method to obtain the high-dispersion heterojunction material, the preparation process is simple and convenient, and the raw materials are cheap; the material has strong practicability and high environmental stability, and can be used for reducing CO in photocatalysis 2 Has potential application prospect in the aspect.

Description

Highly dispersed CeCN-urea-N by coordination method 2 Material, preparation method and application thereof
Technical Field
The invention belongs to material preparation and photocatalytic reduction of CO 2 The technical field of resource utilization, in particular to a high-dispersion CeCN-urea-N adopting a coordination method 2 A material and a preparation method and application thereof.
Background
In recent years, various methods have been proposed to solve the problems of rapid consumption of fossil fuels and global warmingAnd carbon emission is reduced. Wherein CO is reduced in sustainable solar energy 2 Discharging or converting CO 2 Solutions for conversion to valuable carbon derivatives (e.g. methane, formic acid, methanol, etc.) are receiving a lot of attention. In recent years, photocatalytic CO 2 Abatement is one of the most mature solutions today due to its sustainability, environmental friendliness and high efficiency. At present, many photocatalysts have the problems of large size, easy agglomeration of particles and the like, so that the reaction center is reduced, and the photocatalytic performance is influenced. In recent years, a monatomic catalyst in which metal atoms are highly dispersed on a carrier has attracted much attention in the field of catalysis, and methods for synthesizing the monatomic catalyst have been increasing. Atomic Layer Deposition (ALD) and mass selective soft landing techniques are the two most effective methods for achieving precise and controlled synthesis of monatomic catalysts. However, the high cost and low yield of the synthesis equipment prevent the large-scale production of the monatomic catalyst. Therefore, from the practical application point of view, the application of the wet chemical method with the advantages of simple operation and mass production in the synthesis of the monatomic catalyst is explored and developed. In wet chemical methods, dispersion of synthetic precursors and prevention of migration and aggregation of monoatomic atoms are very important, and there are some reported strategies such as building suitable defects on the surface of the support, controlling the design of coordinatively unsaturated sites to enhance interactions with metal atoms, sterically confining the metal atoms in molecular cages of framework materials, i.e. zeolites, MOFs and COFs, introducing site-anchoring metal precursors, etc.
Wherein graphene carbon nitride (g-C) 3 N 4 ) The graphene carbon nitride (g-C) with a two-dimensional layered structure has an advantageous structure that N atoms on a triazine ring have lone pair electrons 3 N 4 ) Is a ligand suitable for anchoring and coordinating isolated metal atoms. CeO (CeO) 2 As rare earth oxide, the rare earth oxide has the characteristics of rich oxygen vacancy, good oxidation-reduction capability, alkaline surface and the like, and is beneficial to CO in the photocatalysis process 2 Adsorption and activation. In the past work on CeO 2 Photo-reduction of CO 2 Some studies have been carried out to find that oxygen vacancies and surface functional groups can act as Lewis acidic and basic sites, respectively, both of which contribute to CO 2 Adsorption of (2)And activating. However, no preparation at g-C by chelation of urea and cerium salt precursors has been achieved so far by complexation 3 N 4 Ce species with high dispersibility (denoted as CeCN-urea-N) 2 ) Preparation method of (1) and photocatalytic CO 2 Reduction applications are reported.
Disclosure of Invention
In view of the problems in the prior art, one technical problem to be solved by the present invention is to provide a highly dispersed CeCN-urea-N using coordination method 2 A method for preparing the material. Another technical problem to be solved by the present invention is to provide a highly dispersed CeCN-urea-N using a coordination method 2 A material. The invention also provides a highly dispersed CeCN-urea-N using coordination method 2 Photocatalytic reduction of CO in materials 2 The use of (1).
In order to solve the problems, the technical scheme adopted by the invention is as follows:
highly dispersed CeCN-urea-N by coordination method 2 The preparation method of the material specifically comprises the following steps:
(1) Solid Ce (NO) 3 ) 3 ·6H 2 Respectively putting O and urea into absolute ethyl alcohol to respectively obtain dispersion liquid A and dispersion liquid B, after completely dissolving, slowly dropwise adding the dispersion liquid A into the dispersion liquid B, and uniformly stirring to obtain a solution C;
(2) The solid g to C 3 N 4 Adding into anhydrous ethanol, stirring to obtain dispersion solution D, slowly dropwise adding the solution C into the dispersion solution D, heating in water bath, and stirring to obtain solid;
(3) The solids were placed in a porcelain boat and the boat was placed in a tube furnace in N 2 Calcining in the atmosphere, cooling to room temperature to obtain the catalyst CeCN-urea-N 2 。
The high-dispersion CeCN-urea-N adopting the coordination method 2 Method for preparing material, solid g-C 3 N 4 The preparation of (1): putting urea in a muffle furnace, heating to 550-600 ℃, calcining for 4-6 h, and obtaining g-C 3 N 4 (ii) a The heating rate is 2-3 ℃/min.
The high-dispersion CeCN-urea-N adopting the coordination method 2 The preparation method of the material comprises the following steps of 1-4 g/L of dispersion liquid A, 3-10 g/L of dispersion liquid B and 17-20 g/L of dispersion liquid D; the ultrasonic dispersion time is 0.5-1 h when preparing the dispersion solution.
The high-dispersion CeCN-urea-N adopting the coordination method 2 Method for preparing material, solid Ce (NO) 3 ) 3 ·6H 2 O, urea and solids g-C 3 N 4 The mass ratio of (1).
The high-dispersion CeCN-urea-N adopting the coordination method 2 The preparation method of the material, in the step (2), the water bath heating temperature is 100 ℃.
The high-dispersion CeCN-urea-N adopting the coordination method 2 The preparation method of the material comprises the following steps of calcining the material at the temperature of 450-550 ℃; n is a radical of 2 The gas flow rate is 150-250 mL/min.
The high-dispersion CeCN-urea-N prepared by the method 2 A material.
The high-dispersion CeCN-urea-N 2 Photocatalytic reduction of CO in materials 2 The use of (1).
Has the advantages that: compared with the prior art, the invention has the advantages that:
(1) High dispersion CeCN-urea-N of coordination method of the invention 2 The preparation process of the material is green and simple, the cost is low, the practicability is high, the material has excellent environmental stability, and the problem of solving CO is solved 2 Has potential application prospect in the aspect of environmental problems such as greenhouse effect and the like.
(2) The invention relates to a coordination method of high-dispersion CeCN-urea-N 2 Ce particles are highly dispersed on the material, not forming CeO 2 The particles are agglomerated in g-C 3 N 4 A surface. Highly dispersed Ce species with g-C 3 N 4 Interface interaction is enhanced, the transfer of photogenerated electrons is promoted, and the Ce species is taken as Lewis base sites to be beneficial to CO 2 Adsorption and activation. In addition, in CeCN-urea-N 2 More CO formed thereon 2 H in which the free radicals are surface-enriched 2 O/OH proton attack in favor of CH 4 The selectivity of (a); is composed ofDesigning a highly efficient photocatalyst provides a simple method.
Drawings
FIG. 1 is XRD, STEM-HAADF and STEM-EDX mapping spectra of the prepared sample, wherein FIG. 1A is XRD map, FIG. 1B is STEM-HAADF map, and FIGS. 1C-1F are STEM-EDX mapping spectra;
FIG. 2 is N1s XPS (FIG. 2A) and DFT (FIG. 2B) of the prepared samples;
FIG. 3 is the ESR (FIG. 3A) and water contact angle (FIGS. 3B and 3C) of the prepared samples;
FIG. 4 is a graph of O1s XPS (FIG. 4A) and O of the prepared sample 2 -TPD (fig. 4B) diagram;
FIG. 5 is a graph of the prepared samples under full spectrum illumination for CO 2 And (5) reducing the effect graph.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with examples are described in detail below.
Example 1
Highly dispersed CeCN-urea-N by coordination method 2 The preparation method of the material comprises the following steps:
(1) Preparation of solid g-C 3 N 4 Photocatalyst: weighing 15g of urea, putting the urea into a crucible, covering the crucible with a crucible cover, horizontally placing the urea into a muffle furnace, calcining in air atmosphere, raising the temperature to 560 ℃, reacting for 4 hours at the temperature, and cooling to room temperature after calcination to obtain solid g-C 3 N 4 ；
(2) 0.2g of solid Ce (NO) 3 ) 3 ·6H 2 Adding O into 50mL of absolute ethyl alcohol, performing ultrasonic dispersion for 1h, and fully stirring and uniformly mixing to obtain a dispersion liquid A; adding 0.3g of urea into 50mL of absolute ethyl alcohol, performing ultrasonic dispersion for 1h, and fully stirring and uniformly mixing to obtain a dispersion liquid B; slowly dripping the dispersion liquid A into the dispersion liquid B, and uniformly stirring to obtain a solution C;
(3) 0.93g of solid g-C 3 N 4 Adding the mixture into 50mL of absolute ethyl alcohol, performing ultrasonic dispersion for 1h, and fully stirring and uniformly mixing to obtain a dispersion liquid D; slowly dropwise adding the solution C into the dispersion liquid DHeating the mixture to 100 ℃ in a water bath in a fume hood, and uniformly stirring to obtain a solid;
(4) The collected solid powder was placed in a porcelain boat and the porcelain boat was placed in a tube furnace in N 2 Calcining to 520 ℃ for 5h at the heating rate of 2 ℃/min, cooling to room temperature after the reaction is finished, and obtaining the catalyst CeCN-urea-N 2 。
Preparation of CeCN-N 2 A material comprising the steps of:
(1) Preparation of g-C 3 N 4 Photocatalyst: weighing 15g of urea, putting the urea into a crucible, covering the crucible with a crucible cover, horizontally placing the crucible into a muffle furnace, calcining in an air atmosphere, raising the temperature to 560 ℃, reacting for 4 hours at the temperature, and cooling to room temperature after calcination to obtain g-C 3 N 4 A photocatalyst;
(2) 10g of Ce (NO) 3 ) 3 ·6H 2 Calcining O in a muffle furnace at 560 ℃ for 4h (the temperature rise rate is 2 ℃/min) to prepare CeO 2 。
(3) 0.06g of urea was added to 50mLH 2 In O, ultrasonically dispersing for 1h, and fully stirring and uniformly mixing to obtain a dispersion liquid A;
(4) 0.94g of-C 3 N 4 Adding into 50mLH 2 In O, ultrasonically dispersing for 1h, fully stirring and uniformly mixing to obtain a dispersion liquid B;
(5) Slowly dripping the dispersion liquid A into the dispersion liquid B, and uniformly stirring to obtain a solution C;
(6) Heating the solution C in a fume hood by water bath to 100 ℃, and uniformly stirring to obtain a solid; the collected solid powder was placed in a porcelain boat and the boat was placed in a tube furnace in N 2 Calcining to 520 deg.C for 5h at a heating rate of 2 deg.C/min, cooling to room temperature to obtain catalyst named CeCN-N 2 。
FIG. 1 is CeCN-urea-N 2 ，CeCN-N 2 And g-C 3 N 4 An X-ray diffraction pattern (XRD) of the sample, wherein FIG. 1A is an XRD pattern, FIG. 1B is a STEM-HAADF pattern, and FIGS. 1C-1F are STEM-EDX mapping patterns. As can be seen from FIG. 1A, sample CeCN-urea-N 2 Only the peak at 27.3 ℃ appears, which is attributed to g-C 3 N 4 (002)) Kneading; the peaks not appearing at 28.7 °,33.3 °, 47.8 ° and 56.8 ° were CeO, respectively 2 (111) Characteristic peaks of (200), (220) and (311) crystal planes. FIGS. 1B and 1C-1F are CeCN-urea-N 2 STEM-HAADF and STEM-EDX mapping of (1). As can be seen from FIGS. 1B and 1C-1F, the Ce species are highly dispersed in g-C 3 N 4 Instead of forming CeO 2 The particles are agglomerated in g-C 3 N 4 A surface.
FIG. 2 is CeCN-urea-N 2 ，CeCN-N 2 And g-C 3 N 4 N1s XPS (FIG. 2A) and DFT (FIG. 2B) of the sample, from which it can be observed that a large number of electrons are concentrated at the N atom (g-C) 3 N 4 ) The number of Ce electrons decreased, indicating that electrons were transferred from Ce to g-C 3 N 4 On N of (C) to result in CeCN-urea-N 2 A strong built-in electric field is formed, consistent with the XPS results.
FIG. 3 is CeCN-urea-N 2 And CeCN-N 2 Fig. 3A shows ESR (fig. 3A) and water contact angle (fig. 3B and fig. 3C) of the sample, and signals at g =2.03 and g =1.96 correspond to superoxide radical and Ce, respectively 3+ Species of the species. By comparison of the intensities of the two peaks (I) 1 /I 2 ) Found CeCN-urea-N 2 Ce of 3+ Species ratio CeCN-N 2 Poly of (A) to (B), ce 3+ The species are the hydroxyl groups and the lewis basic sites to which the water molecules adsorb. On the basis of the above, ceCN-urea-N 2 Has good Ce species dispersibility, ce and g-C 3 N 4 Has strong built-in electron field among N atoms, more surface adsorbs hydroxyl and water molecules, and catalyzes CO 2 Photochemical Properties of reduction and CH 4 The selectivity has a positive influence. As can be seen from FIG. 3B, the results of water contact angles (FIGS. 3B and 3C) show that CeCN-urea-N 2 Has a lower contact angle, which indicates better hydrophilicity and more oxygen-containing substances adsorbed on the CeCN-urea-N 2 On the surface.
FIG. 4 is CeCN-urea-N 2 ，CeCN-N 2 And g-C 3 N 4 O1s XPS plot (FIG. 4A) and O of sample 2 TPD plot (FIG. 4B), from FIG. 4A it can be seen that the broad peak consists of two peaks at the binding energy, each belonging to lattice oxygen (O) L ) And adsorbing oxygen (O) C ) 530 and 532.6eV, respectively. Generally, the species of surface oxygen include surface hydroxyl groups and adsorbed water molecules. According to the calculated A C /A( C+L ) Peak area value, ceCN-urea-N 2 More water molecules and hydroxyl are adsorbed on the surface. As shown in fig. 4B, the width between 100-200 c is due to desorption of chemically adsorbed oxygen at the surface. Wherein, ceCN-urea-N 2 The peak intensity of (A) is greater and moves slightly to higher temperatures, indicating that CeCN-urea-N 2 The adsorption interaction of surface oxygen is stronger. In combination with the results of O1s XPS, the surface adsorbed oxygen species are strongly attributed to hydroxyl groups and water molecules. Thus, ceCN-urea-N 2 The surface has more hydroxyl groups and water molecules to adsorb.
Example 2
Application of the photocatalyst prepared in example 1 to CO 2 In the reduction, the experimental steps are as follows:
CO 2 the photoreduction reaction of (2) was carried out in a 100ml autoclave, and CO was tested 2 Photoreductive property. 20mg of the sample was weighed and placed in a quartz glass sand reactor. 1ml of distilled water was dropped on the catalyst surface to soak the catalyst. After degassing, 4bar of high purity CO was added 2 The autoclave was charged and the xenon lamp was turned on for 8h and the resulting gas was detected by gas chromatography. The used samples were washed several times with distilled water and then dried in an oven at 80 ℃. FIG. 5 is a graph of the prepared samples under full spectrum illumination for CO 2 And (5) reducing the effect graph.
As can be seen from FIG. 5, g-C was observed after 8 hours of light irradiation 3 N 4 Only CO was detected, whereas CO and CH were detected on both CeCN catalysts 4 The activity is all compared with g-C 3 N 4 Is improved. Wherein, ceCN-urea-N 2 The CO yield of the sample was CeCN-N 2 About 2 times of the sample, CH 4 The yield is CeCN-N 2 More than 10 times of the sample shows that the sample is CeCN-urea-N 2 CH of sample 4 The selectivity is greatly improved.

Claims (1)

1. High dispersion CeCN-urea-N 2 Photocatalytic reduction of CO in materials 2 The use of (A) in (B), characterized byPreparation of highly dispersed CeCN-urea-N by coordination 2 The material specifically comprises the following steps:
(1) Solid Ce (NO) 3 ) 3 ·6H 2 Respectively putting O and urea into absolute ethyl alcohol to respectively obtain dispersion liquid A and dispersion liquid B; after the dispersion liquid A is completely dissolved, slowly dropwise adding the dispersion liquid A into the dispersion liquid B, and uniformly stirring to obtain a solution C;
(2) The solid g-C 3 N 4 Adding into anhydrous ethanol, stirring to obtain dispersion solution D, slowly dropwise adding the solution C into the dispersion solution D, heating in water bath, and stirring to obtain solid;
(3) The solids were placed in a porcelain boat and the boat placed in a tube furnace under N 2 Calcining in atmosphere, cooling to room temperature to obtain catalyst CeCN-urea-N 2 ；
Wherein the solids g to C 3 N 4 The preparation of (1): putting urea into a muffle furnace, heating to 550-600 ℃, calcining for 4-6 h, and obtaining g-C 3 N 4 (ii) a The heating rate is 2-3 ℃/min;
the concentration of the dispersion liquid A is 1-4 g/L, the concentration of the dispersion liquid B is 3-10 g/L, and the concentration of the dispersion liquid D is 17-20 g/L; the ultrasonic dispersion time is 0.5-1 h when preparing the dispersion solution;
solid Ce (NO) 3 ) 3 ·6H 2 O, urea and solid g-C 3 N 4 The mass ratio of (1);
in the step (2), the water bath heating temperature is 100 ℃;
the calcination temperature is 450-550 ℃; n is a radical of hydrogen 2 The gas flow rate is 150-250 mL/min.
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