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Method for preparing aluminum oxide-based ceramic hollow fibrous membrane

An alumina, fiber membrane technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of reduced gas permeability, unable to meet the requirements of practical applications, low mechanical properties, etc., and achieve mechanical strength. improved effect

Active Publication Date: 2010-12-08
NANJING UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] However, for ceramic hollow fiber membranes, the main problem at present is poor mechanical strength (Smid et al, J.Membr.Sci.1996, 112, 85; Sun et al, J.Membr.Sci.2006, 278, 162 ), which is caused by the morphological structure of the membrane
Kingsbury et al. (Kingsbury et al, J.Membr.Sci.2009, 328, 134) studied the effect of the amount of non-solvent in the spinning solution on the microstructure of alumina hollow fiber membranes, and found that the introduction of an appropriate amount of non-solvent can completely eliminate The finger-like macropores in the membrane greatly improve the mechanical strength of the membrane, but the gas permeability of the membrane is significantly reduced
Li et al. (Li et al, J.Membr.Sci.2005, 256, 1) used the reaction bonding technology in the ceramic process, adding aluminum powder to the spinning solution, through the nano-scale alumina generated in situ during the sintering process The ceramic microstructure is obviously improved, and the mechanical strength is 129% higher than that of the film made of pure alumina. However, compared with most reported values ​​in the literature, the mechanical properties of the film are still low and cannot meet the requirements of practical applications.

Method used

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  • Method for preparing aluminum oxide-based ceramic hollow fibrous membrane
  • Method for preparing aluminum oxide-based ceramic hollow fibrous membrane

Examples

Experimental program
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Effect test

Embodiment 1

[0021] According to the following steps: (1) mixing of main membrane material and reinforcing agent, (2) preparation of spinning solution, (3) spinning of membrane green body and sintering treatment to prepare reinforced alumina-based hollow fiber membrane, wherein:

[0022] (1) Mixing of main membrane material and reinforcing agent 350g main membrane material alumina powder (d 50 =5μm) and 150g enhancer magnesium oxide (d 50 = 100nm) for mixing, wet ball milling and mixing for 12 hours, then dry and grind through a 200-mesh sieve.

[0023] (2) Preparation of spinning solution Add 100g polysulfone to 400g N, N-dimethylacetamide to form a polymer solution, then add 500g of mixed ceramic powder prepared in the previous step and stir for 24 hours to obtain uniform dispersion spinning solution.

[0024] (3) Textile membrane green body and sintering treatment Spinning solution is extruded from the spinneret after degassing treatment, enters the external coagulation bath at 30°C t...

Embodiment 2

[0027] According to the steps in Example 1, the film-making solution is prepared and processed by spinning and sintering, but the difference is that aluminum oxide adopts d 50 = 0.5μm powder, enhancer is d 50=10nm magnesium oxide (mass fraction in the mixed ceramic powder is 5%), the mixed powder was wet ball milled for 24 hours, and dried and ground through a 300-mesh sieve. The polymer is cellulose acetate, its mass fraction in the polymer solution is 10%, and the organic solvent is dimethyl sulfoxide. The mixed ceramic powder (the mass fraction in the spinning solution is 30%) was added into the polymer solution and stirred for 48 hours to obtain a spinning solution. The dry spinning distance of spinning is 20cm, the temperature of the external coagulation bath and the core liquid are both 10°C, and the solidification time of the green film is 10 hours. The green film was soaked in tap water at 10°C for 48 hours. During the sintering process, the temperature was raised t...

Embodiment 3

[0029] According to the steps in Example 1, the film-making solution is prepared and processed by spinning and sintering, but the difference is that aluminum oxide adopts d 50 = 20μm powder, enhancer is d 50 =50nm silicon carbide (mass fraction in the mixed ceramic powder is 50%), the mixed powder was wet ball milled for 20 hours, dried and ground and sieved. The polymer is a mixture of polyethersulfone and cellulose acetate, the mass ratio of the two is 3:1, and its mass fraction in the polymer solution is 40%; the organic solvent is N, N-dimethylacetamide and N- A mixture of methyl-2-pyrrolidone, the mass ratio of the two is 1:1. The mixed ceramic powder (the mass fraction in the spinning solution is 80%) was added into the polymer solution and stirred for 30 hours to obtain a spinning solution. The dry spinning distance of spinning is 10 cm, the temperature of the external coagulation bath and the core liquid are both 20° C., and the solidification time of the green film ...

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Abstract

The invention relates to a method for preparing an enhanced aluminum oxide-based ceramic hollow fibrous membrane. The method comprises the following steps: performing ball milling and mixing a main membrane material aluminum oxide powder and a reinforcing agent, and then drying, grinding and sieving; preparing a polymer solution, adding the evenly mixed ceramic powder in the polymer solution and evenly dispersing to obtain a spinning solution with proper viscosity; after the spinning solution is subjected to deaeration treatment, extruding the spinning solution via a spinning jet, enabling the extruded spinning solution to enter into external coagulated bath by passing through a certain dry spinning procedure, and generating a phase separation process at the moment while forming a hollow fibrous membrane green body; soaking the membrane green body in the external coagulated bath to replace out residual organic solvents; and after naturally drying, processing the green body via a sintering technology to obtain the ceramic hollow fibrous membrane. The invention has simple and convenient technology and no expensive devices, the prepared aluminum oxide-based ceramic hollow fibrous membrane has favorable mechanical property, and the mechanical strength thereof is remarkably improved compared with the hollow fibrous membrane produced by pure aluminum oxide powder.

Description

technical field [0001] The invention relates to a preparation method of a ceramic separation membrane, in particular to a preparation method of a reinforced alumina-based ceramic hollow fiber membrane. Background technique [0002] Ceramic membranes based on inorganic materials have outstanding characteristics such as good chemical stability, high mechanical strength, anti-biological pollution, and high temperature resistance, and are widely used in fluid separation, fuel cells, and membrane reactors. At present, the commercialized ceramic membranes are mainly tubular and multi-channel membranes, which have the advantages of convenient installation, easy maintenance and high filtration efficiency. However, the asymmetric structure of this type of ceramic membrane determines its long preparation period and high cost. Compared with organic membranes, the competitive advantage is not obvious. The hollow fiber configuration is a common structural form in polymer membranes. Its ...

Claims

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Application Information

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IPC IPC(8): B01D71/02B01D69/08B01D67/00
Inventor 金万勤戚律刘正堃董学良徐南平
Owner NANJING UNIV OF TECH
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