CN111760466A - Preparation method and application of lithium aluminum-layered double hydroxide two-dimensional nanosheet film based on AAO template - Google Patents
Preparation method and application of lithium aluminum-layered double hydroxide two-dimensional nanosheet film based on AAO template Download PDFInfo
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- CN111760466A CN111760466A CN202010644284.3A CN202010644284A CN111760466A CN 111760466 A CN111760466 A CN 111760466A CN 202010644284 A CN202010644284 A CN 202010644284A CN 111760466 A CN111760466 A CN 111760466A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/02—Inorganic material
- B01D71/024—Oxides
- B01D71/025—Aluminium oxide
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0044—Inorganic membrane manufacture by chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
Abstract
The invention discloses a preparation method of an AAO template-based LiAl-LDHs ion filtering membrane, which is characterized by comprising the following steps: and putting the AAO template into a LiOH aqueous solution, and reacting for 1-4 h to obtain the AAO template-based LiAl-LDHs ion filtering membrane. The method is simple, the experimental steps are greatly reduced, the process is easy to control, and the obtained filtering membrane has a very stable structure.
Description
Technical Field
The invention belongs to the technical field of seawater filtration, and particularly relates to a preparation method of a lithium aluminum-layered double hydroxide two-dimensional nanosheet film based on an AAO template.
Background
The shortage of fresh water resources is a big problem faced by human beings, while the content of seawater on the earth reaches about 71 percent, if the seawater can be desalinated by a certain technical means, the problem of the shortage of fresh water resources can be obviously solved. At present, more and more researchers are engaged in the research, and the ion filtering membrane is a very promising research direction and achieves a remarkable effect. In recent decades, research on two-dimensional materials has been promoted, and due to their unique structures and their easy-to-process properties, ion filtration membranes are mostly prepared on the surfaces of some porous substrates (such as PES, PVDF, AAO, etc.) by vacuum filtration methods from a plurality of two-dimensional materials, such as graphene, graphene oxide, and transition group metal chalcogen compounds represented by MoS2, and the membranes prepared from these two-dimensional materials have many excellent properties compared with some conventional ion filtration membranes.
For two-dimensional material ion filtration membranes, the currently common methods are: the two-dimensional material nanosheet is obtained by stripping through a certain method, and then the membrane is prepared on the surface of the AAO plate or other porous materials through a vacuum filtration method.
Disclosure of Invention
The invention aims to prepare a novel two-dimensional material ion filtering membrane based on an AAO template, so as to solve the problem of shortage of fresh water resources.
In order to achieve the above object, the present invention provides a method for preparing a lithium aluminum-layered double hydroxide (LiAl-LDHs) ion filtration membrane based on an AAO (anodic alumina) template, comprising: placing the AAO template into a LiOH aqueous solution, standing at room temperature for 1-4 h for reaction, and obtaining a LiAl-LDHs ion filtering membrane based on the AAO template;
preferably, the AAO template has a specification of: a diameter of 25mm, an effective pore diameter of 350nm and a thickness of 50 μm.
Preferably, the concentration of LiOH in the LiOH aqueous solution is 5 mmol/L.
Preferably, the standing reaction time at room temperature is 1.5 h.
The invention also provides an application of the AAO template-based LiAl-LDHs ion filter membrane prepared by the method in seawater desalination treatment.
Compared with the prior art, the invention has the beneficial effects that:
the invention adopts a preparation method completely different from vacuum filtration film forming which is researched more at present, and the preparation method is based on an AAO template, the AAO template is put into LiOH aqueous solution with a certain concentration, the AAO template and the LiOH aqueous solution react spontaneously at room temperature for a certain time to generate a lithium aluminum-layered double hydroxide (LiAl-LDHs) nanosheet film taking the AAO template as a framework, wherein the LiAl-LDHs is a two-dimensional material. The two-dimensional material is obtained through research, because of the structural characteristics of the two-dimensional material, certain interlayer distances exist among layers, and the interlayer distances can enable water molecules with smaller sizes to pass through, prevent salt ions with larger ion sizes, and have the effect of ion filtration, so that the two-dimensional material can be applied to the field of ion filtration, and therefore the two-dimensional material nanosheet film prepared by the method is applied to the field of ion filtration and is subjected to ion filtration test, and better experimental results are obtained.
The two-dimensional material ion filtering membrane of the LiAl-LDHs based on the AAO template is directly prepared by a one-step method, and compared with the general method for preparing the two-dimensional material ion filtering membrane by vacuum filtration, the method disclosed by the invention is simple, greatly reduces the experimental steps, is easy to control the process, and has a very stable structure.
Drawings
FIG. 1 is a process flow diagram of an AAO template-based lithium aluminum-layered double hydroxide (LiAl-LDHs) ion filtration membrane prepared in accordance with the present invention;
FIG. 2 is a test apparatus for ion filtration performance of an AAO template-based lithium aluminum-layered double hydroxide (LiAl-LDHs) ion filtration membrane;
FIG. 3 is a Scanning Electron Microscope (SEM) image of an AAO template-based LiAl-LDHs ion filtration membrane prepared according to the present invention; wherein FIG. 3a is a cross-sectional view of an AAO template LiAl-LDHs ion filtration membrane, FIG. 3b is a surface topography of the filtration membrane, and FIG. 3c is a film internal topography;
FIG. 4 is a test curve of the rejection performance of the LiAl-LDHs ion filter membrane prepared based on the AAO template to Na + in 1M NaCl solution;
FIG. 5 is a test curve of ion filtration performance of the prepared LiAl-LDHs ion filtration membrane based on the AAO template versus the prepared artificial simulated seawater;
FIG. 6 is an SEM image of an AAO template-based LiAl-LDHs ion filtration membrane prepared by the invention after 6H filtration;
FIG. 7 is water permeation test data for AAO template based LiAl-LDHs ion filtration membranes made in accordance with the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
The invention provides a preparation method of an AAO template-based LiAl-LDHs ion filtering membrane, which comprises the following specific steps:
as shown in FIG. 1, a piece of AAO template with the diameter of 25mm, the effective pore diameter of 350nm and the thickness of 50 μm is added into 0.005mol/L LiOH aqueous solution, and the mixture is stood still for reaction for 1.5 hours at room temperature to obtain the AAO template-based lithium aluminum-layered double hydroxide (LiAl-LDHs) ion filtration membrane filtering membrane.
Ion filtration performance and water permeability testing of AAO template based lithium aluminum-layered double hydroxide (LiAl-LDHs) ion filtration membranes:
ion permeation was measured using a custom H-type device (fig. 2). One side of the device is added with 10ml NaCl solution with concentration of 1M or artificial seawater (with composition of 0.469M NaCl, 0.1M KCl, 0.1M CaCl)2、0.1M MgCl2) As feed side, the other side was charged with an equal volume of deionized water as permeate side, and the prepared filtration membrane was located in the middle of both sides. Under the action of osmotic pressure, ions automatically diffused from the high concentration side (feed side) to the low concentration side (permeate side), and in order to minimize the influence of the concentration gradient, magnetic stirring was continued for 200r/min on both the feed side and the permeate side until the end of the experiment.
From the beginning of the reaction, 20. mu.L of the permeate was measured from the permeate at regular intervals, and then 20ml of deionized water was added to dilute the permeate to serve as a test solution, and samples were taken several times until the end of the reaction. And respectively measuring the corresponding ion concentration in the solution of the permeation edge in different time periods by using an inductively coupled plasma emission spectrometer (ICP-OES).
The performance of the inventive ion filtration membrane was characterized using the ion exclusion Rate (Salt Rejection Rate), which was calculated by the following formula: ion rejection ratio (%) ═ 1-Cp/CFWhere Cp is the corresponding ion concentration in the permeate side after a specific reaction time, CFIs the corresponding remaining initial ion concentration at the feed side.
Meanwhile, in order to test the durability of the filtration membrane of our invention, the reaction time was extended from 3h to 24h, and then the ion concentration in the solution at the permeate side was measured using an inductively coupled plasma emission spectrometer (ICP-OES).
As shown in fig. 4, the filtration membrane has a filtration rate of 97% or more for ions within 3 hours, and the effect is very satisfactory, and even if the reaction time is prolonged to 24H, the filtration rate for Na + is still about 87%, indicating the excellent stability of the filtration membrane of our invention.
The filter membrane pair Na was tested as shown in FIG. 5+、K+、Ca2+、Mg2+The filtering performance of four ions mainly existing in seawater, the filtering rate of a filtering membrane to different ions is different due to different concentrations of the ions in a solution, self-hydrated ion radiuses and the like, but the filtering membrane of the invention has higher filtering performance to the four ions, and after 24H reaction, except K+The filtration rate to other three ions is above 97%, and k is+The filtration rate of (2) is also 93% or more. This shows that our ion filtering membrane can have excellent ion filtering performance for real seawater.
As shown in FIG. 6, in the SEM image of the AAO template-based LiAl-LDHs ion filtration membrane after 6H filtration, the appearance of the membrane is not obviously changed before reaction, which illustrates the stability of the filtration membrane.
For the water penetration test, the method of the water vapor penetration test was employed. The method comprises the following steps: deionized water with the same mass is filled in the two glass beakers, a blank AAO template and the LiAl-layered double hydroxide filtering membrane based on the AAO template are respectively covered on the surfaces of the glass beakers, and vaseline is coated on the surfaces of the beakers to ensure the tightness in the test, so that the blank AAO template and the LiAl-layered double hydroxide filtering membrane based on the AAO template are tightly sealed with the surfaces of the beakers, and the water vapor is ensured to completely pass through the surfaces of the two templates. The initial mass of the two test units was recorded and then placed on a heating plate at 40 c to measure the mass change of the two units at different times, and since the AAO template is a porous structure and has excellent water permeability, the water permeability of the AAO template-based LiAl-layered double hydroxide filtration membrane prepared by us was evaluated by comparison with a blank AAO template.
As shown in fig. 7, the water vapor reduction mass corresponding to our inventive filter membrane was very close to that of the blank AAO template within 50h of the test time. The AAO template has a low water permeation hindering effect due to the porous structure, and water vapor can smoothly pass through the AAO template, and the reduction amount of the water vapor of the LiAl-layered double hydroxide filtering membrane based on the AAO template is close to that of a blank AAO template, so that the filtering membrane prepared by the LiAl-layered double hydroxide filtering membrane has good water permeability.
In conclusion, the AAO template-based LiAl-LDHs two-dimensional material ion filtering membrane is directly prepared and obtained through a one-step method, and compared with a general vacuum filtration preparation method of the two-dimensional material ion filtering membrane, the method is simple, the experimental steps are greatly reduced, the process is easy to control, and the obtained filtering membrane is very stable in structure.
Claims (5)
1. A preparation method of an AAO template-based LiAl-LDHs ion filter membrane is characterized by comprising the following steps: and putting the AAO template into a LiOH aqueous solution, and reacting for 1-4 h to obtain the AAO template-based LiAl-LDHs ion filtering membrane.
2. The preparation method of the AAO template-based LiAl-LDHs ion filtration membrane of claim 1, wherein the AAO template has a specification: a diameter of 25mm, an effective pore diameter of 350nm and a thickness of 50 μm.
3. The preparation method of the AAO template-based LiAl-LDHs ion-filtration membrane of claim 1, wherein the LiOH concentration of the LiOH aqueous solution is 5 mmol/L.
4. The preparation method of the AAO template-based LiAl-LDHs ion filtration membrane according to claim 1, wherein the reaction time of standing at room temperature is 1.5 h.
5. Use of the AAO template-based LiAl-LDHs ion filtration membrane prepared by the method of any one of claims 1 to 4 in seawater desalination treatment.
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| CN202010644284.3A CN111760466A (en) | 2020-07-07 | 2020-07-07 | Preparation method and application of lithium aluminum-layered double hydroxide two-dimensional nanosheet film based on AAO template |
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| CN202010644284.3A CN111760466A (en) | 2020-07-07 | 2020-07-07 | Preparation method and application of lithium aluminum-layered double hydroxide two-dimensional nanosheet film based on AAO template |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113758977A (en) * | 2021-08-20 | 2021-12-07 | 浙江大学 | Method for detecting ion concentration of nutrient solution based on LDHs anion selective membrane |
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| US20030047505A1 (en) * | 2001-09-13 | 2003-03-13 | Grimes Craig A. | Tubular filter with branched nanoporous membrane integrated with a support and method of producing same |
| CN102976278A (en) * | 2012-12-19 | 2013-03-20 | 青岛科技大学 | Laminar bimetal hydroxide and preparation method thereof |
| CN105502477A (en) * | 2016-01-08 | 2016-04-20 | 西北大学 | Preparation method of morphology-controllable large-area nanometer platy zinc-aluminum type hydrotalcite |
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2020
- 2020-07-07 CN CN202010644284.3A patent/CN111760466A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US20030047505A1 (en) * | 2001-09-13 | 2003-03-13 | Grimes Craig A. | Tubular filter with branched nanoporous membrane integrated with a support and method of producing same |
| CN102976278A (en) * | 2012-12-19 | 2013-03-20 | 青岛科技大学 | Laminar bimetal hydroxide and preparation method thereof |
| CN105502477A (en) * | 2016-01-08 | 2016-04-20 | 西北大学 | Preparation method of morphology-controllable large-area nanometer platy zinc-aluminum type hydrotalcite |
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| SHAN-LI WANG等: "Synthesis of Li/Al LDH using aluminum and LiOH", 《APPLIED CLAY SCIENCE》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113758977A (en) * | 2021-08-20 | 2021-12-07 | 浙江大学 | Method for detecting ion concentration of nutrient solution based on LDHs anion selective membrane |
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