CN111569792A - Aerogel composite material and preparation method and application thereof - Google Patents

Aerogel composite material and preparation method and application thereof Download PDF

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CN111569792A
CN111569792A CN202010383167.6A CN202010383167A CN111569792A CN 111569792 A CN111569792 A CN 111569792A CN 202010383167 A CN202010383167 A CN 202010383167A CN 111569792 A CN111569792 A CN 111569792A
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aerogel composite
carbon nitride
composite material
aerogel
graphene oxide
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丁萍
何亚菲
陈翠梅
李晶
开天翰
黄瑞雪
伍翩
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Central South University
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    • 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
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
    • B01J20/28009—Magnetic properties
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    • B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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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
    • 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
    • C02F1/48—Treatment of water, waste water, or sewage with magnetic or electric fields
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • B01J2220/00—Aspects relating to sorbent materials
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    • B01J2220/00—Aspects relating to sorbent materials
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    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • 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 an aerogel composite material and a preparation method and application thereof, wherein the aerogel composite material comprises carbon nitride, reduced graphene oxide aerogel and a magnetic material, and the preparation method comprises the following steps: (1) dispersing carbon nitride and a magnetic material in a solvent, uniformly mixing to obtain a suspension, and removing the solvent to obtain mixed powder; (2) and dispersing the mixed powder and graphene oxide in a solvent, reacting for 8-16 h, and then carrying out freeze drying in a vacuum environment to obtain the aerogel composite material. The aerogel composite material can be used as a photocatalyst to be applied to degradation of microcystins, has excellent physicochemical properties, has the advantages of wide absorption range of visible light, good degradation effect of microcystins, and capability of simultaneously performing magnetic separation and photocatalytic degradation.

Description

Aerogel composite material and preparation method and application thereof
Technical Field
The invention belongs to the field of photocatalysis, and particularly relates to an aerogel composite material as well as a preparation method and application thereof.
Background
Microcystins (MCs) are monocyclic heptapeptides with multiple isomers, and the most abundant, most widely present, and most harmful is microcystin-LR (MC-LR). The main target organ of microcystin-LR is the liver, which has a wide range of toxic effects including genetic toxicity, neurotoxicity, immunotoxicity and potential tumor-promoting properties, and can also cause abnormal development of the tested organism. These toxins are present in water bodies, or are concentrated in fish or shellfish and accumulate in the human body through the food chain, and many toxic deaths of humans and animals have occurred worldwide. The drinking water recommendation standard of the World Health Organization (WHO) and the sanitary Standard of Drinking Water issued in 2006 (GB 5749-. The microcystin-LR is easy to dissolve in water, the cyclic structure and the interval double bonds in the molecule enable the microcystin-LR to have quite high stability, the toxin cannot be damaged when the microcystin-LR is heated and boiled, the natural degradation process is very slow, and the microcystin-LR is difficult to remove by a conventional water treatment process.
At present, the removal technology of microcystin-LR in water mainly comprises coagulating sedimentation, activated carbon adsorption, membrane separation, biodegradation, oxidation reduction and the like. However, they have various disadvantages, such as essentially failing to completely remove microcystin-LR, only spatially transferring microcystin-LR, environmental limitation, and easy occurrence of secondary pollution. Therefore, the photocatalytic oxidation technology is convenient to operate, environment-friendly, free of secondary pollution, wide in development prospect and application space, popular with researchers, and considered to be one of ideal technologies for energy conversion, environmental remediation and organic synthesis. However, the existing photocatalyst has the problems of difficult recovery, narrow light absorption range, low light utilization rate, unstable chemical property and the like, and limits the industrialization and the expansion of the photocatalytic removal of microcystin-LR.
Disclosure of Invention
The invention aims to solve the technical problems that the defects and the defects mentioned in the background technology are overcome, and the aerogel composite material and the preparation method and the application thereof are provided.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
an aerogel composite comprising carbon nitride, reduced graphene oxide aerogel, and a magnetic material.
The technical scheme has the design idea that the magnetic material is dispersed in pores of the aerogel by preparing the aerogel composite material containing the magnetic material, so that the problems that the composite material is difficult to recover and reuse and brings impurities to a catalytic system when being used as a catalyst can be solved; in addition, the non-metal semiconductor photocatalyst carbon nitride has obvious advantages compared with other metal photocatalysts, has stable physicochemical properties, can keep stable performance in strong acid, strong alkali and high temperature environments, and has the advantages of safety, no toxicity, environmental friendliness and no secondary pollution; in addition, the three-dimensional aerogel taking the reduced graphene oxide as the framework is taken as the carrier of the carbon nitride, so that the problem of possible agglomeration of two-dimensional powder can be avoided, charge separation is promoted, and electron-hole recombination is inhibited, so that the problem of high photoproduction electron-hole recombination rate of graphite-phase carbon nitride is solved; meanwhile, due to the fact that the carbon nitride is fixed on the reduced graphene oxide aerogel, the separation and recycling process of the carbon nitride can be greatly simplified in practical application.
Preferably, in the above aspect, the carbon nitride is graphite phase carbon nitride. The carbon nitride in the graphite phase form is selected because the forbidden band width of the graphite phase carbon nitride is 2.70eV, the absorption sideband is about 460nm, and the visible light in sunlight can be absorbed at normal temperature and normal pressure to play a photocatalysis role, so that the carbon nitride has great potential in the field of photocatalysis.
Preferably, in the above technical solution, the magnetic material is Fe3O4And (3) powder. The ferroferric oxide is selected as the magnetic material, so that the recovery process of the aerogel composite material as a catalyst can be simplified, the visible light absorption range of the graphite-phase carbon nitride can be expanded when the aerogel composite material is compounded with the graphite-phase carbon nitride for use, and the utilization rate of the aerogel composite material to visible light is improved.
Preferably, the aerogel composite material is prepared from the following raw materials in parts by mass: 5-17 parts of carbon nitride, 1.2-18 parts of reduced graphene oxide and 1 part of magnetic material.
Based on the same technical concept, the invention also provides a preparation method of the aerogel composite material in the technical scheme, which comprises the following steps:
(1) dispersing carbon nitride and a magnetic material in a solvent, uniformly mixing to obtain a suspension, and removing the solvent to obtain mixed powder;
(2) and dispersing the mixed powder and graphene oxide in a solvent, reacting for 8-16 h, and freeze-drying in a vacuum environment to obtain the aerogel composite material.
The technical scheme has the design idea that the aerogel composite material is synthesized by a solution method, so that the preparation condition is simple, the raw material toxicity is low, the reaction steps are simple and convenient, and the method is suitable for large-scale industrialized production.
Preferably, the carbon nitride calcination is carried out in two times, and the first calcination is carried out for 2-6 h in a closed environment at the temperature of 525-575 ℃; and the second calcination is carried out for 1-3 h in an open environment at the temperature of 475-525 ℃. The method has the advantages that the blocky carbon nitride can be generated by calcining thiourea once, and the carbon nitride is converted into the carbon nitride nanosheets by calcining twice.
Preferably, the temperature rise rate of the first calcination is 22-2.4 ℃/min, and the temperature rise rate of the second calcination is 4.8-5.2 ℃/min.
Preferably, in the step (2), the reaction condition of the mixed powder and the graphene oxide is heating or adding ammonia water.
Based on the same technical concept, the invention also provides an application of the aerogel composite material, and the aerogel composite material is used as a photocatalyst to be applied to degradation of microcystins.
As a preferred aspect of the above technical solution, the application of the aerogel composite specifically includes the following steps: adding the aerogel composite material into a microcystin-LR solution to obtain a mixed solution, placing the mixed solution into a photochemical reactor for dark adsorption balance, and irradiating by using visible light.
Compared with the prior art, the invention has the beneficial effects that:
(1) the aerogel composite material is a three-dimensional reticular reduced graphene oxide aerogel, has large specific surface area, rich pores and high electron mobility, is added with a magnetic material, is convenient to recycle and utilize, and is a high polymer material with excellent physicochemical properties;
(2) the preparation method of the aerogel has the advantages of simple preparation conditions, low raw material toxicity, simple and convenient reaction steps, and reaction in a solution phase, and is a cheap and environment-friendly green synthesis method.
(3) The aerogel disclosed by the invention can be used as photocatalysis and applied to degradation of microcystins, has a wide absorption range on visible light and a good degradation effect on the microcystins, has the advantages of a magnetic material and a photocatalytic material, and can realize the functions of magnetic separation and photocatalytic degradation at the same time.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a scanning electron micrograph of an aerogel composite of example 1;
FIG. 2 is a mapping plot of element C, N, O, Fe of the aerogel composite of example 1;
FIG. 3 is an X-ray diffraction pattern of the aerogel composite of example 1;
FIG. 4 is a graph of the photocatalytic degradation of microcystin by the aerogel composite of example 1.
FIG. 5 is a UV-visible diffuse reflectance spectrum of the aerogel composite of example 1.
Detailed Description
In order to facilitate understanding of the invention, the invention will be described more fully and in detail 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.
Example 1:
the aerogel composite material of the embodiment is prepared from graphite phase carbon nitride and Fe3O4Powder and reduced graphene oxide aerogel composition, whichIn the preparation of the aerogel composite material of the present example, the raw materials in parts by mass were 6.032 parts of graphite-phase carbon nitride and 0.757 parts of Fe3O4Powder and 3.395 parts of reduced graphene oxide.
The preparation method of the aerogel composite material of the embodiment comprises the following steps:
(1) 20g of thiourea is put in a ceramic crucible with a cover and is put in a muffle furnace, the temperature is raised to 550 ℃ at the speed of 2.2 ℃/min, the 550 ℃ is kept for reaction for 4h, then the thiourea is naturally cooled to the room temperature, the temperature is raised to 500 ℃ in an open environment at the speed of 5 ℃/min, the 500 ℃ is kept for reaction for 2h, and the graphite-phase carbon nitride powder is prepared for standby after the thiourea is naturally cooled to the room temperature and ground.
(2) Taking 6.032g of graphite phase carbon nitride in a 1L beaker, adding 800mL of 25% ethanol, and carrying out ultrasonic treatment for 2h to obtain a uniformly dispersed graphite phase carbon nitride suspension. 1.082g ferric chloride and 0.398g ferrous chloride were dissolved in 15mL deionized water and added to the graphite phase carbon nitride suspension, respectively. Placing the mixture in a heating stirrer, stirring at 80 ℃ for 1h, then injecting 15mL of 25% ammonia water into the mixture, stirring again for 1h, separating the solvent to obtain a solid product, repeatedly washing with deionized water and absolute ethyl alcohol for several times, drying at 60 ℃, and grinding to obtain a mixed powder for later use.
(3) And (3) taking 60mg of the mixed powder in the step (2) and 30mg of graphene oxide in a 22mL glass bottle, adding 15mL of deionized water, and performing ultrasonic dispersion for 2h until the mixture is uniformly mixed. And (2) placing the glass bottle filled with the mixed solution into a polytetrafluoroethylene high-pressure reaction kettle, reacting for 12 hours at 200 ℃, naturally cooling to room temperature, washing away surface residues with deionized water, adding 5mL of 20% ethanol, placing the mixture on a water bath kettle, heating in a water bath at 60 ℃ for 6 hours, and drying for 6 hours by using a vacuum freeze-drying instrument to obtain the aerogel composite material.
A scanning electron microscope image of the aerogel composite material or the aerogel composite material prepared by the method of the present embodiment is shown in fig. 1, and it can be seen from the image that the surface of the aerogel has a plurality of graphene folds, and the graphene sheets are connected to form a three-dimensional porous honeycomb structure; the mapping diagram of element C, N, O, Fe of the aerogel composite material is shown in fig. 2, and it can be seen that graphite phase carbon nitride and ferroferric oxide are uniformly distributed in the aerogel structure; the X-ray diffraction pattern of the aerogel composite is shown in fig. 3, and the raw material composition of the aerogel composite can be determined by comparing the characteristic peaks of the aerogel composite with the characteristic peaks of the raw material components.
The UV-visible diffuse reflectance spectrum of the aerogel composite of this example is shown in FIG. 5, which is shown in the graph, g-C3N4Comparing the monomers, the aerogel composite of this example added Fe3O4Then, the light absorption side band is red-shifted, and the visible light absorption range is increased.
Placing the aerogel composite material into 5mL of 8 mu g/mLMC-LR solution, placing the solution in a photochemical reactor for dark adsorption equilibrium, and placing the solution in a reactor for light adsorption>Irradiating with visible light of 500W xenon lamp under 420nm filter, sampling at 30min intervals, centrifuging at 13500r/min for 20min, and separating supernatant to determine MC-LR concentration by high performance liquid chromatograph; wherein the high performance liquid chromatograph adopts C18The column (4.6 × 150mm,5 μm, Agilent, USA) was used for separation with a detection wavelength of 238nm, a column temperature of 40 deg.C, and a mobile phase of 57% methanol + 43% water + 0.05% trifluoroacetic acid at a flow rate of 0.8mL/min and a sample volume of 10 μ L.
Fig. 4 shows a photocatalytic degradation curve of the aerogel composite material or the aerogel composite material prepared by the method of this embodiment on microcystin, and it can be seen that the content of the microcystin-LR blank tube is substantially unchanged under the illumination condition, the aerogel composite material of this embodiment has the maximum adsorption and degradation rate, and 90% of microcystin-LR can be removed by catalytic degradation within 2 hours.
Example 2:
the aerogel composite material of the embodiment is prepared from graphite phase carbon nitride and Fe3O4Powder and reduced graphene oxide aerogel, wherein the raw materials for preparing the aerogel composite material of the present embodiment comprise, by mass, 6.451 parts of graphite-phase carbon nitride and 0.832 parts of Fe3O4Powder and 4.370 parts of reduced graphene oxide.
The preparation method of the aerogel composite material of the embodiment comprises the following steps:
(1) 20g of thiourea is put in a ceramic crucible with a cover and is put in a muffle furnace, the temperature is raised to 550 ℃ at the speed of 2.2 ℃/min, the thiourea reacts for 4 hours at 550 ℃, the thiourea is naturally cooled to the room temperature, the temperature is raised to 500 ℃ in an open environment at the speed of 5 ℃/min, the thiourea is kept at 500 ℃ and reacts for 2 hours, and the thiourea is naturally cooled to the room temperature and is ground to prepare the graphite-phase carbon nitride powder for later use.
(2) 6.451g of graphite-phase carbon nitride is taken in a 1L beaker, 800mL of 25% ethanol is added, and the mixture is subjected to ultrasonic treatment for 2 hours to obtain a uniformly dispersed graphite-phase carbon nitride suspension. 1.198g of ferric chloride and 0.432g of ferrous chloride were dissolved in 15mL of deionized water and added to the graphite phase carbon nitride suspension. Placing the mixture in a heating stirrer, stirring at 80 ℃ for 1h, then injecting 15mL of 25% ammonia water into the mixture, stirring again for 1h, separating the solvent to obtain a solid product, repeatedly washing with deionized water and absolute ethyl alcohol for several times, drying at 60 ℃, and grinding to obtain a mixed powder for later use.
(3) And (3) putting 50mg of the mixed powder obtained in the step (2) and 30mg of graphene oxide into a 22mL glass bottle, adding 15mL of deionized water, performing ultrasonic dispersion for 2h until the mixture is uniformly mixed, and adding 2mL of 25% ammonia water. And (2) placing the glass bottle filled with the mixed solution into a polytetrafluoroethylene high-pressure reaction kettle, reacting for 12 hours at 200 ℃, naturally cooling to room temperature, washing away surface residues with deionized water, adding 5mL of 20% ethanol, placing the mixture on a water bath kettle, heating in a water bath at 60 ℃ for 6 hours, and drying for 6 hours by using a vacuum freeze-drying instrument to obtain the aerogel composite material.

Claims (10)

1. An aerogel composite comprising the following components: carbon nitride, reduced graphene oxide aerogel and magnetic materials.
2. The aerogel composite of claim 1, wherein the magnetic material is Fe3O4And (3) powder.
3. The aerogel composite of claim 1, wherein the carbon nitride is a graphite phase carbon nitride.
4. The aerogel composite of any of claims 1-3, prepared from the following raw materials in parts by mass: 5-17 parts of carbon nitride, 1.2-18 parts of reduced graphene oxide and 1 part of magnetic material.
5. A method of preparing an aerogel composite as described in any of claims 1-4, comprising the steps of:
(1) dispersing carbon nitride and a magnetic material in a solvent, uniformly mixing to obtain a suspension, and removing the solvent to obtain mixed powder;
(2) and dispersing the mixed powder and graphene oxide in a solvent, reacting for 8-16 h, and freeze-drying to obtain the aerogel composite material.
6. The method of claim 5, wherein the carbon nitride is prepared by calcining thiourea; calcining the thiourea twice, wherein the first calcining is carried out for 2-6 h in a closed environment at the temperature of 525-575 ℃; and the second calcination is carried out for 1-3 h in an open environment at the temperature of 475-525 ℃.
7. The method according to claim 6, wherein the temperature increase rate in the first calcination is 2 to 2.4 ℃/min, and the temperature increase rate in the second calcination is 4.8 to 5.2 ℃/min.
8. The method according to claim 5, wherein the reaction condition of the mixed powder and the graphene oxide in the step (2) is heating or addition of ammonia water.
9. Use of the aerogel composite of any of claims 1 to 4 as a photocatalyst for the degradation of microcystins.
10. Use of an aerogel composite as claimed in claim 9, comprising the following steps: adding the aerogel composite material into a microcystin-LR solution to obtain a mixed solution, placing the mixed solution into a photochemical reactor for dark adsorption balance, and irradiating the mixed solution by using visible light.
CN202010383167.6A 2020-05-08 2020-05-08 Aerogel composite material and preparation method and application thereof Pending CN111569792A (en)

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