CN115282925A - Three-dimensional graphene/clay composite aerogel for water treatment - Google Patents
Three-dimensional graphene/clay composite aerogel for water treatment Download PDFInfo
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- CN115282925A CN115282925A CN202210837740.5A CN202210837740A CN115282925A CN 115282925 A CN115282925 A CN 115282925A CN 202210837740 A CN202210837740 A CN 202210837740A CN 115282925 A CN115282925 A CN 115282925A
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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
- 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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- 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
- 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
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- 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
- B01J20/28014—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 form
- B01J20/28047—Gels
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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
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/14—Treatment of water, waste water, or sewage by heating by distillation or evaporation using solar energy
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/208—Off-grid powered water treatment
- Y02A20/212—Solar-powered wastewater sewage treatment, e.g. spray evaporation
Abstract
The invention relates to the technical field of water treatment, in particular to a water treatment device prepared from three-dimensional graphene/clay composite aerogel. The mechanical property of the composite aerogel can be enhanced by adding the clay into the aerogel, and the hydrophilicity and hydrophobicity of the composite aerogel can be adjusted. After the graphene/clay aerogel in the device is compressed to 90% strain for 20 cycles, the graphene/clay aerogel shows excellent fatigue resistance, can be completely recovered to the original height, and shows super-strong mechanical properties.
Description
Technical Field
The invention relates to the technical field of water treatment, in particular to three-dimensional graphene/clay composite aerogel and application thereof in preparation of a water treatment device.
Background
At present, fresh water resources are deficient, and a new water purification technology needs to be developed. Among them, solar evaporation of water is the current research focus. However, for practical use, the water evaporation device needs to consider manufacturing cost, evaporation efficiency, reusability, durability under severe environments, and the like. The photothermal conversion material should remain structurally stable under many severe conditions (e.g., organic, strong caustic acid and/or alkaline conditions). The graphene aerogel is a 3D porous network structure assembled by graphene. Has excellent photo-thermal conversion performance and can be applied to various severe environments (high and low temperature, strong acid and the like). Graphene aerogels are therefore candidates for evaporating water. However, the graphene has strong hydrophobicity, so that the graphene aerogel cannot be directly used as a high-efficiency water evaporation device. In addition, the graphene is relatively high in cost, so that the graphene aerogel is limited from being used for large-scale solar water evaporation.
Clays (attapulgite (ATP), montmorillonite (MMT) and Laponite (LAP)) are abundant industrial minerals. Has the advantages of low cost, good filling performance and rich pore structure, and can be used as an adsorbent and a filler. The powder or the membrane material prepared by the combination of the interaction of hydrogen bond, electrostatic force and the like and graphene has good application prospect in the fields of composite reinforcement, pollution treatment, biocatalysis and the like.
Good mechanical strength is critical to maintaining structural stability of solar evaporation devices under long-term solar desalination conditions. Particularly for low-density graphene aerogel, under actual working conditions, the structure is fragile due to dynamic flow and extrusion of seawater.
Due to the strong binding force between the salt crystals and the evaporation interface, the deposited crystalline salt will partially separate under the influence of gravity when the evaporation rate is slow or the water content at the interface increases. Therefore, how to collect the salt conveniently and timely is a difficult problem. In addition, if the deposited salt is not collected in time, the effective evaporation area is inevitably reduced, and the solar evaporation rate is reduced. Therefore, it remains a great challenge to produce an ideal solar desalination system with high-speed stable evaporation, no salt deposition and convenient salt collection.
Disclosure of Invention
Aiming at the technical problem, the invention provides a three-dimensional graphene/clay composite aerogel and application thereof in preparing a water treatment device. Specifically, the graphene/clay composite aerogel with a special structure is prepared by utilizing the excellent processability of Melamine (MF) foam, and can be used in the fields of long-term sustainable desalination, organic solvent adsorption and the like.
The invention concretely comprises the following technical scheme:
firstly, the invention provides a three-dimensional graphene/clay composite aerogel for water treatment, and specifically, the three-dimensional aerogel comprises a hollow quadrangular pyramid, a hollow triangular pyramid and a hollow cuboid.
Further, the aerogel comprises graphene/Attapulgite (ATP) aerogel, graphene/montmorillonite (MMT) aerogel, graphene/Laponite (LAP) aerogel.
Further, the three-dimensional aerogel is prepared by taking melamine foam with a specific shape as a template.
Further, the three-dimensional aerogel obtaining comprises the following steps:
(1) Mixing the clay suspension and the Graphene Oxide (GO) suspension according to the mass ratio of solid content to obtain uniform mixed suspension;
(2) Adding ascorbic acid into the mixed suspension obtained in the step 1, and absorbing the ascorbic acid by using Melamine Foam (MF) with a specific shape to obtain graphene/clay/MF composite hydrogel;
(3) Placing the composite hydrogel in hydroiodic acid at the temperature of 90-100 ℃ for 2-10 hours, and removing the MF template to obtain the graphene/clay composite hydrogel with a specific shape;
(4) And (3) repeatedly replacing the composite hydrogel in deionized water, and then freezing and drying to obtain the graphene/clay composite aerogel.
Further, the clay in step 1 includes attapulgite ATP, montmorillonite MMT and laponite LAP.
Further, the mass ratio of the graphene oxide and the clay in the step 1 can be controlled within a range of 1:1 to 10.
Further, the specific process of Melamine Foam (MF) absorption in step 2 is as follows: immersing MF template with special shape into the mixed suspension liquid, and repeatedly squeezing and sucking.
Further, the specific shape in step 3 is a hollow quadrangular pyramid, a hollow triangular pyramid, or a hollow rectangular parallelepiped; preferably a hollow triangular pyramid and a hollow rectangular parallelepiped.
The invention further provides an application of the three-dimensional graphene/ATP composite aerogel in a solar efficient desalting system, and particularly relates to a long-term efficient solar desalting device.
Further, the device comprises the following components: the three-dimensional graphene/ATP aerogel with a specific shape is used as a solar evaporation component, an aerogel fixing device and a water container below the aerogel fixing device.
Further, the specific shape is a hollow quadrangular pyramid or a hollow triangular pyramid.
Furthermore, MF foam can be placed above the three-dimensional aerogel, and the MF has a hole with the same size as the inner wall of the three-dimensional aerogel. The holes do not influence the passing of sunlight, and in the solar evaporation process, the MF foam placed on the holes can adsorb salt under the driving of the salt concentration gradient (as can be obviously seen from the schematic diagram of figure 3), and the aim of long-term and efficient desalination can be achieved by replacing the MF foam placed on the holes.
Further, the whole solar desalination device can be placed in a transparent sealed space, and steam is condensed on the surface of the transparent plate to form fresh water, so that the fresh water can flow into a container to collect the fresh water (the specific structural layout is shown in fig. 4).
In addition, the invention also provides an application of the three-dimensional graphene/MMT aerogel or the three-dimensional graphene/LAP aerogel in solvent adsorption, and specifically, a mixture of an organic solvent and water is poured into the cubic cup aerogel, so that the organic solvent can be quickly adsorbed, and can be completely separated within a few seconds. The composite aerogel adsorbed with the solvent can be removed by burning, and the organic solvent can be removed by repeatedly extruding due to the excellent mechanical property of the composite aerogel, so that the composite aerogel can be repeatedly used.
Compared with the prior art, the invention has the following advantages:
firstly, the invention provides the three-dimensional graphene/clay composite aerogel, and the mechanical property of the composite aerogel can be enhanced by adding the clay, and the hydrophilicity and hydrophobicity of the composite aerogel can be adjusted. After the graphene/clay aerogel is compressed to 90% and strained for 20 cycles, the graphene/clay aerogel shows excellent fatigue resistance, can be completely recovered to the original height, and shows super-strong mechanical properties.
Secondly, the invention provides a preparation method of the graphene/clay composite aerogel, the mass ratio of graphene to clay can be as high as 1:1, and the preparation cost is greatly reduced. The graphene/clay composite aerogel in various shapes can be prepared by using Melamine Foam (MF) as a template.
In addition, the invention utilizes the excellent processability of MF foam to prepare the three-dimensional aerogel with a special structure, and can realize long-term sustainable desalination and solvent/water separation.
Drawings
FIG. 1 is a schematic diagram of the application of a quadrangular pyramid shaped three-dimensional aerogel in a solar desalination system.
FIG. 2 is a schematic diagram of application of a triangular pyramid-shaped three-dimensional aerogel in a solar desalination system.
FIG. 3 is a schematic diagram of the application of a triangular pyramid-shaped three-dimensional aerogel (top loaded with a foam MF) in a solar desalination system.
Fig. 4 is a schematic diagram of a portable small evaporator based on a triangular pyramid-shaped three-dimensional aerogel design.
FIG. 5 is a schematic diagram of the application of cubic cup-shaped three-dimensional aerogel in solvent adsorption.
Detailed Description
The present application is described in further detail below by way of examples to enable those skilled in the art to practice the present application. It is to be understood that other embodiments may be utilized and that changes may be made without departing from the spirit or scope of the present application. To avoid detail not necessary to enable those skilled in the art to practice the application, the description may omit certain information known to those skilled in the art. The following detailed description is, therefore, not to be taken in a limiting sense, and the scope of the present invention is defined only by the appended claims. The following examples facilitate a better understanding of the present application and are not intended to limit the scope of the present application. The materials used in the practice of the present invention are all commercially available products that do not provide a method of preparation.
Example 1
Adding a certain mass of ATP into water, performing ultrasonic treatment to obtain an ATP aqueous suspension, and obtaining an graphene oxide aqueous suspension according to a Hummers method. And mixing the water suspensions of the two materials according to the mass ratio of the solid contents of 1:1, adding ascorbic acid with twice the solid content of graphene, and absorbing the ascorbic acid by using MF with a specific shape to obtain the graphene/ATP/MF composite hydrogel. And (3) placing the composite hydrogel in hydroiodic acid at 90-100 ℃ for 2-10 hours, removing the MF template, and performing water replacement and freeze drying to obtain the graphene/ATP composite aerogel with a specific shape. The aerogel has hydrophilic performance, can be tested by xenon lamp light source equipment for evaporation performance, and has an evaporation rate of 4.10 kg m under sunlight -2 h -1 Na in the obtained fresh water + 、Ca + 、Mg + 、K + The concentrations of (1) were 0.42,0.24,0.13,0.21mg L -1 ) Far below the drinking water standard of the World Health Organization (WHO) (water hardness is 50-200 mg L in terms of calcium carbonate content) -1 ）。
Example 2
Adding a certain mass of LAP into water, performing ultrasonic treatment to obtain an aqueous suspension of the LAP, and obtaining an aqueous suspension of graphene oxide according to a hummers method. And mixing the water suspensions of the two materials according to the mass ratio of the solid contents of 1:1, adding ascorbic acid with twice the solid content of graphene, and absorbing the ascorbic acid by using MF with a specific shape to obtain the graphene/LAP/MF composite hydrogel. And (3) placing the composite hydrogel in hydroiodic acid at the temperature of 90-100 ℃ for 2-10 hours, removing the MF template, and performing water replacement and freeze drying to obtain the cubic cup-shaped graphene/LAP composite aerogel. The composite aerogel has hydrophobicity, can be used for treating substances such as oil, solvents and the like in sewage, and the cubic cup-shaped shape greatly simplifies the adsorption process. And the organic solvent can be removed in a repeated extrusion mode due to the excellent mechanical property of the composite aerogel, and the composite aerogel can be repeatedly used for many times.
Example 3
A mass of MMT was added to water and sonicated to obtain an aqueous suspension of MMT, which was obtained according to hummers method. And mixing the water suspensions of the graphene and the graphene according to the mass ratio of 1:1 of solid contents, then adding ascorbic acid with twice the solid content of the graphene, and absorbing the ascorbic acid by using MF with a specific shape to obtain the graphene/MMT/MF composite hydrogel. And (3) placing the composite hydrogel in hydroiodic acid at the temperature of 90-100 ℃ for 2-10 hours, removing the MF template, and performing water replacement and freeze drying to obtain the cubic cup-shaped graphene/MMT composite aerogel. The composite aerogel has hydrophobicity and can be used for treating substances such as oil, solvents and the like in sewage. And the processability of MF is utilized, so that the adsorption process is greatly simplified. And the organic solvent can be removed in a repeated extrusion mode due to the excellent mechanical property of the composite aerogel, and the composite aerogel can be repeatedly used for many times.
Test for desalting application
The three-dimensional graphene/ATP aerogel prepared by the invention is used for a solar seawater desalination test, and specifically, a hollow square body is arranged above the three-dimensional graphene/ATP aerogel, and a quadrangular pyramid is arranged below the three-dimensional graphene/ATP aerogel. In the continuous desalination of 15 hours under one sun, salt is accumulated on the upper surface of the cube, no salt is deposited on the bottom and the wall (fig. 1 a), and when the sun is increased to 3 sun lights, salt is gradually accumulated on the cup wall due to the flow of salt water along the cup wall except for the salt deposited on the upper surface, so that the effective evaporation area and the evaporation rate are reduced (fig. 1 b), and the evaporation performance is influenced.
To solve the problem of salt deposition on the walls of the cups, the aerogel is shaped as a triangular pyramid so that salt accumulates only on the upper surface and does not accumulate on the walls of the cups (fig. 2).
In order to solve the problems of salt deposition and salt concentration, an MF plate filled with water is placed on the upper surface of the three-dimensional graphene/ATP aerogel, the MF plate is provided with a hole with the same size as the inner wall of the 3D aerogel, and the passing of sunlight is not influenced, so that in the solar evaporation process, the MF plate placed on the MF plate can adsorb salt under the driving of a salt concentration gradient (the MF plate can be obviously seen through the schematic diagram of fig. 3), and the aim of long-term efficient desalination can be achieved by replacing the MF plate placed on the MF plate.
Based on the structure, the invention also designs and prepares a portable small evaporator (figure 4), the triangular pyramid type graphene/ATP composite aerogel (on which the MF foam is placed) floats on saline water in a 2 x 2 array, then the whole device is sealed in a transparent acrylic plate like a house, and steam is condensed on the transparent acrylic plate to form fresh water, namely the fresh water can flow into a container to collect the fresh water.
The three-dimensional graphene/MMT aerogel prepared by the present invention was used for solvent adsorption test, and the mixture of organic solvent (dyed with sudan iii) and water was poured into the cubic cup-shaped aerogel structure, so that the organic solvent was rapidly adsorbed and completely separated within a few seconds (fig. 5). The composite aerogel adsorbed with the solvent can be removed by burning, and the organic solvent can be removed by repeatedly extruding due to the excellent mechanical property of the composite aerogel, so that the composite aerogel can be repeatedly used.
Claims (10)
1. The three-dimensional graphene/clay composite aerogel for water treatment is characterized in that the shape of the three-dimensional aerogel comprises a hollow quadrangular pyramid, a hollow triangular pyramid and a hollow cuboid.
2. The aerogel of claim 1, comprising a graphene/attapulgite aerogel, a graphene/montmorillonite aerogel, a graphene/laponite aerogel.
3. Aerogel according to claim 1, characterized in that the obtaining of said three-dimensional aerogel comprises the following steps:
(1) Mixing the clay suspension and the graphene oxide suspension according to a certain proportion to obtain a uniform mixed suspension;
(2) Adding ascorbic acid into the mixed suspension obtained in the step (1), and absorbing the ascorbic acid by using Melamine (MF) foam with a specific shape to obtain graphene/clay/MF composite hydrogel;
(3) Placing the composite hydrogel in hydroiodic acid at the temperature of 90-100 ℃ for 2-10 hours, and removing the MF template to obtain the graphene/clay composite hydrogel with a specific shape;
(4) And (3) repeatedly replacing the composite hydrogel in deionized water, and then freezing and drying to obtain the graphene/clay composite aerogel.
4. The aerogel of claim 2, wherein the clay in step 1 comprises attapulgite ATP, montmorillonite MMT, and laponite LAP.
5. The aerogel of claim 2, wherein the ratio of graphene oxide and clay in step 1 can be controlled within the range of 1:1 to 10.
6. The application of the three-dimensional graphene/clay aerogel in a solar efficient desalting system is characterized in that the application is to prepare a long-term efficient solar desalting device.
7. Use according to claim 6, characterized in that the device comprises the following components: the three-dimensional graphene/clay aerogel with a specific shape is used as a solar evaporation component, an aerogel fixing device and a water container below the aerogel fixing device.
8. The use according to claim 6, wherein further, there is placed above the three-dimensional aerogel a MF foam, wherein the MF foam has a hole with the same size as the inner wall of the three-dimensional aerogel.
9. The use according to any one of claims 6 to 8, wherein the entire desalination apparatus is placed in a transparent sealed space, and the steam is condensed on the surface of the transparent plate to form fresh water, which can be flowed into a container to collect the fresh water.
10. The application of the three-dimensional graphene/clay aerogel in solvent adsorption is characterized in that the aerogel is graphene/MMT aerogel or graphene/LAP aerogel.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107281982A (en) * | 2016-04-05 | 2017-10-24 | 中国科学院化学研究所 | A kind of adjustable graphene of hydrophilic and hydrophobic/clay composite elastic aeroge and preparation method thereof |
| CN110127670A (en) * | 2019-05-16 | 2019-08-16 | 宿迁南航新材料与装备制造研究院有限公司 | A kind of graphene three-dimensional structure aeroge hydrophobic material |
| CN110581026A (en) * | 2019-09-03 | 2019-12-17 | 滨州学院 | Transition metal selenide/ordered porous graphene aerogel composite electrode material and preparation method thereof |
| CN113908780A (en) * | 2021-11-01 | 2022-01-11 | 山东第一医科大学(山东省医学科学院) | Graphene-attapulgite composite elastic aerogel and application thereof in seawater desalination |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107281982A (en) * | 2016-04-05 | 2017-10-24 | 中国科学院化学研究所 | A kind of adjustable graphene of hydrophilic and hydrophobic/clay composite elastic aeroge and preparation method thereof |
| CN110127670A (en) * | 2019-05-16 | 2019-08-16 | 宿迁南航新材料与装备制造研究院有限公司 | A kind of graphene three-dimensional structure aeroge hydrophobic material |
| CN110581026A (en) * | 2019-09-03 | 2019-12-17 | 滨州学院 | Transition metal selenide/ordered porous graphene aerogel composite electrode material and preparation method thereof |
| CN113908780A (en) * | 2021-11-01 | 2022-01-11 | 山东第一医科大学(山东省医学科学院) | Graphene-attapulgite composite elastic aerogel and application thereof in seawater desalination |
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