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Method for preparation of ceramic nanofiltration membrane by improved sol-gel technique

A technology of ceramic nanofiltration membrane and gel method, which is applied in the field of preparation of ceramic nanofiltration membrane, can solve the problems of increasing equipment investment cost and production cost, being unsuitable for preparation of ceramic nanofiltration membrane, etc. Loss modulus, reduction of internal seepage, effect of hindering stress propagation

Active Publication Date: 2013-10-23
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In CN1443597A, by coupling the powder method prepared by the wet chemical method with the solid particle sintering method, the method can be preferably used in the preparation of ultrafiltration membranes, but the method is not suitable for the preparation of ceramic nanofiltration membranes with smaller apertures
These methods require precise control of the temperature and humidity in the production process, resulting in a substantial increase in equipment investment costs and production costs

Method used

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  • Method for preparation of ceramic nanofiltration membrane by improved sol-gel technique
  • Method for preparation of ceramic nanofiltration membrane by improved sol-gel technique
  • Method for preparation of ceramic nanofiltration membrane by improved sol-gel technique

Examples

Experimental program
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Effect test

Embodiment 1

[0026] When the average particle size of the sol is 8nm and the titanium content is 1mol L -1 TiO with an average particle size of 21nm was added to the acidic sol 2 Nanoparticles get a stable coating solution, TiO 2 The particle content is 0.5g / L. Use the prepared coating solution on a porous sheet support (surface structure is 100nm Al 2 o 3 Ceramic film) was coated by spin coating method, dried in an oven at 40°C, heated at 1°C / min, and calcined at 400°C for 4 hours to obtain a titanium dioxide ceramic film with a pore diameter of 7 nm and a porosity of 40%. . figure 1 It is the surface electron micrograph of the film after the calcining of Example 1; figure 2 It is a cross-sectional electron microscope image of the calcined film in Example 1; it can be seen from the figure that the film layer prepared by this method is uniform without cracks, and there is almost no infiltration phenomenon during film coating.

Embodiment 2

[0028] When the average particle size of the sol is 2nm and the titanium content is 1mol L -1 TiO with an average particle size of 25nm was added to the alkaline sol 2 Nanoparticles get a stable coating solution, TiO 2 The particle content was 0.2 g / L. Use the prepared coating solution on a porous sheet support (surface structure is 100nm Al 2 o 3 Ceramic membrane) was coated by dip coating, dried in an oven at 70°C, heated at 1°C / min, and calcined at 300°C for 3 hours to obtain a ceramic membrane with a pore size of 8nm. Then, when the titanium content is 0.2mol·L -1 Add 10nm TiO to titanium sol 2 Nanoparticles (0.05g / L) obtained a stable coating solution and repeated coating drying and sintering to obtain a titanium dioxide nanofiltration membrane with a pore size of 2.1nm and a porosity of 50%. Figure 3A It is the cut-off curve of the ceramic membrane to dextran after calcined in Example 2; it can be seen from the figure that the dextran molecular weight cut-off of t...

Embodiment 3

[0030] The average particle size of the sol is 3nm, and the titanium content is 1.5mol L -1 Add TiO with an average particle size of 5nm in the acidic sol 2 Nanoparticles get a stable coating solution, TiO 2 The particle content was 0.2 g / L. Using the prepared coating solution on the tubular ZrO 2The ultrafiltration membrane (pore size is 50nm, single tube 10cm long) is coated with dip coating method, dried in a constant temperature and humidity box at 65°C and 70%RH, and heated at 2°C / min, at 600°C Calcined at ℃ for 3 hours to obtain a titanium dioxide ceramic membrane with a pore diameter of 4.5 nm and a porosity of 45%. Figure 4 It is the relationship diagram of the storage modulus and temperature before and after adding particles of the gel material, Figure 5 It is the relationship diagram of loss modulus and temperature before and after adding particles of the gel material. It can be seen from the figure that after doping particles, the storage modulus and loss mod...

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Abstract

The invention relates to a method for preparation of a ceramic nanofiltration membrane by an improved sol-gel technique. The method includes: adding nano-particles with certain particle size into sol to prepare a film coating solution, conducting film coating on a porous supporting body by the prepared film coating solution, airing and drying a wet film, and then carrying out direct calcinations, thus obtaining the nanofiltration membrane. In the invention, the nano-particles with a size of 3-50nm are employed to modify the supporting body surface macropore defect, and also can achieve the purpose of toughening gel and increasing its strength, thus effectively avoiding the problem of film cracking during drying. On a sheet, single tube or multi-channel supporting body with a pore diameter of 50-200nm, the ceramic membrane that is intact, crack-free, defect-free and has a pore diameter of 1-10nm can be prepared. The ceramic nanofiltration membrane prepared by the method has the advantages of narrow pore diameter distribution, simple process and good repeatability, and is suitable for large scale ceramic nanofiltration membrane production.

Description

technical field [0001] The invention relates to a method for preparing ceramic nanofiltration membranes, in particular to a method for preparing ceramic nanofiltration membranes by an improved sol-gel method; The membrane filtration method is suitable for large-scale preparation of high-performance ceramic nanofiltration membranes. Background technique [0002] Nanofiltration is a separation process developed in the late 1980s. It is a new pressure-driven membrane separation process between reverse osmosis and ultrafiltration. Due to the characteristics of good chemical stability, strong anti-biological ability, high mechanical strength, non-toxic and high temperature resistance, ceramic nanofiltration membranes are widely used in the fields of biology, food, chemical industry and environment. [0003] The preparation methods of inorganic ceramic membranes mainly include solid particle sintering method and sol-gel method. Among them, the solid particle sintering method is ...

Claims

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Application Information

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IPC IPC(8): C04B35/624
Inventor 景文珩李丹王慧陈涛涛邢卫红范益群徐南平
Owner NANJING UNIV OF TECH
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