Method for preparing mesoporous ceramic membrane based on novel two-dimensional material

A two-dimensional material, ceramic membrane technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problem of inability to obtain separation precision mesoporous ceramic membrane, ultra-fine sol particles easily infiltrated into the support, affecting the membrane. Integrity permeation flux and other issues, to avoid cracking defects, reduce capillary suction, and improve water permeation flux

Active Publication Date: 2018-06-01
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in the process of sol-gel membrane preparation, nanoscale ultrafine sol particles can easily penetrate into the macropore defects of the support, which will directly affect the integrity of the membrane and the permeation flux of the membrane, which restricts the mesoporous ceramic membrane. to promote
Secondly, when the sol is coated on the macroporous support to obtain the loaded mesoporous membrane, the interfacial stress is not uniform. Therefore, in the drying process and sintering process of the sol-to-gel process, the uneven stress distribution of the membrane layer is easy to cause Cracking, unable to obtain complete mesoporous ceramic membrane with high separation precision
In CN 103360080 A, it is proposed to add nanoparticles of a certain particle size to the sol to modify the macropore defects on the surface of the support and play a role in toughening the gel, which improves the toughness and rigidity of the gel material. Reactive sol requires the size of nanoparticles to match the pore size of the support to a certain extent, which has certain limitations for the selection of the pore size of the support.

Method used

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  • Method for preparing mesoporous ceramic membrane based on novel two-dimensional material
  • Method for preparing mesoporous ceramic membrane based on novel two-dimensional material
  • Method for preparing mesoporous ceramic membrane based on novel two-dimensional material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add MXene nanosheets with an average particle size of 300nm into the aqueous sol with a titanium content of 0.1mol / L and a sol particle size of 15nm, and disperse it uniformly in the sol to make a coating solution, wherein the MXene nanosheets are in the coating film The content in the liquid is 0.1g / L. Using the prepared coating solution on the sheet-type α-Al with an average pore diameter of 100 nm 2 o 3 The film was coated on the support by the spin coating method, dried in an oven at 40°C, and then calcined in a muffle furnace at 400°C for 4 hours at a heating rate of 0.5°C / min. A pore size of 10 nm can be obtained by one sintering. Pure water flux is 9.9L / (m 2 h bar) TiO 2 @MXene mesoporous ceramic membrane. figure 1 In a is calcined TiO 2 @MXene sheet membrane, b is a sheet support; figure 2 It is the SEM figure of MXene nanosheet in embodiment 1; image 3 It is the AFM figure of MXene nanosheet in embodiment 1; Figure 4 Middle b is TiO after calcination...

Embodiment 2

[0031] Add MXene nanosheets with an average particle size of 300nm into the aqueous sol with a titanium content of 0.1mol / L and a sol particle size of 15nm, and disperse it uniformly in the sol to make a coating solution, wherein the MXene nanosheets are in the coating film The content in the liquid is 0.05g / L. The hollow fiber α-Al with the average pore size of 300nm 2 o 3A film was coated on the support by the dipping and pulling method, dried in an oven at 40°C, and then calcined in a muffle furnace at 400°C for 4 hours at a heating rate of 0.5°C / min. One-time sintering can obtain pore diameters of 6.07nm and pure water flux of 94L / (m 2 h bar) TiO 2 @MXene mesoporous ceramic membrane. figure 1 In c is calcined TiO 2 @MXene hollow fiber membrane, d is the hollow fiber support; Figure 5 is the cut-off curve of the membrane to dextran after calcination; it can be seen from the figure that the molecular weight cut-off of the prepared membrane to dextran is 18566Da, and t...

Embodiment 3

[0033] Add MXene nanosheets with an average particle size of 400nm into the acidic sol with a titanium content of 1.5mol / L and a sol particle size of 6nm, and disperse it uniformly in the sol to make a coating solution, wherein the MXene nanosheets are in the coating film The content in the liquid is 0.15g / L. Using the prepared coating solution on the sheet-type α-Al with an average pore diameter of 100 nm 2 o 3 Spin-coat the film on the support, dry it in an oven at 60°C, and then calcinate it at 400°C for 4 hours at a heating rate of 0.5°C / min in a muffle furnace. A pore size of 2.8nm can be obtained by one sintering. , The molecular weight cut-off to PEG is 2836Da, and the pure water flux is 3.5L / (m 2 h bar) TiO 2 @MXene mesoporous ceramic membrane.

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Abstract

The invention relates to a method for preparing a mesoporous ceramic membrane based on a novel two-dimensional material. The method comprises the following steps: introducing the novel two-dimensionalmaterial into sol and carrying out uniform dispersion to prepare coating liquid; and coating a support body with the prepared coating liquid in a one-shot coating manner so as to prepare the mesoporous ceramic membrane with bore diameters of 2 to 10 nm. According to the invention, the novel two-dimensional flaky material and sol particles or a sol polymer are assembled to form a brick structure so as to reduce capillary pulp suction effect and modify macroporous defects on the surface of the support body, so inward infiltration of sol is effectively prevented, and water permeation flux is increased; and gel toughening effect is obtained, and the cracking defect of the membrane is effectively avoided. The preparation method provided by the invention is simple in process, short in preparation period, good in repeatability and high in permeation flux; and the method can realize high-efficiency preparation of the mesoporous ceramic membrane and is suitable for mass production.

Description

technical field [0001] The invention relates to a method for preparing a mesoporous ceramic membrane based on a new two-dimensional material, in particular a method for assembling a new two-dimensional material with sol particles or polymers to form a brick structure, and a method for efficiently preparing a mesoporous ceramic membrane by one-time coating , suitable for large-scale production. Background technique [0002] Mesoporous ceramic membranes with a pore size of 2-10 nm have been widely studied and applied in the fields of energy storage, food, medicine and water purification due to their high thermal and chemical stability, high flux and low cost. , so the large-scale production of highly efficient and energy-saving mesoporous ceramic membranes has become a research hotspot in recent years. [0003] The sol-gel method has become the most commonly used method for preparing mesoporous ceramic membranes in industry due to its advantages of easy process control, low p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01D71/02B01D69/10B01D67/00
CPCB01D67/0039B01D69/10B01D71/024B01D71/025
Inventor 景文珩孙雨晴夏成胜徐志邢卫红
Owner NANJING UNIV OF TECH
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