Method for sintering of porous ceramic support and in-situ hydrothermal synthesis of molecular sieve membrane by molecular sieve
A porous ceramic, in-situ hydrothermal technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc. The effect of less waste, good separation selectivity and permeability, and easy operation
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Embodiment 1
[0040] (1) Preparation of porous alumina hollow fiber support containing NaA molecular sieve conversion
[0041] Step A. Configure the alumina hollow fiber spinning solution containing NaA molecular sieve
[0042] According to the composition mass ratio NMP:PES:(Al 2 o 3 +NaA):PVP=40.2:8.5:50.8:0.5 to prepare hollow fiber spinning solution, wherein NaA:(Al 2 o 3 +NaA) was 10% by mass. The mixing step is: add PES into NMP, stir for 2 hours to fully dissolve, then add NaA molecular sieve and stir for 12 hours. Added NaA molecular sieves such as figure 1 As shown, it has a typical cubic shape. Then, under continuous stirring, the Al 2 o 3 The powder is added in batches and the PVP is added at the end. The obtained white hollow fiber spinning solution still needs to be continuously stirred for more than 2 days.
[0043] Step B. Spinning to obtain the hollow fiber precursor and sintering at high temperature
[0044] Under the action of nitrogen, the spinning solution is...
Embodiment 2
[0048] (1) Preparation of porous alumina hollow fiber support containing NaA molecular sieve conversion
[0049] Step A. Configure the alumina hollow fiber spinning solution containing NaA molecular sieve
[0050] According to the composition mass ratio NMP:PES:(Al 2 o 3 +NaA):PVP=40.2:8.5:50.8:0.5 to prepare hollow fiber spinning solution, wherein NaA:(Al 2 o 3 +NaA) was 20% by mass. The mixing step is: add PES into NMP, stir for 2 hours to fully dissolve, then add NaA molecular sieve powder and stir for 12 hours. Then, under continuous stirring, the Al 2 o 3 The powder is added in batches and the PVP is added last. The obtained white hollow fiber spinning solution still needs to be continuously stirred for more than 2 days.
[0051] Step B. Spinning to obtain the hollow fiber precursor and sintering at high temperature
[0052] Under the action of nitrogen, the spinning solution is extruded from the spinning head, firstly contacts the inner coagulation bath (water),...
Embodiment 3
[0056] (1) Preparation of porous alumina hollow fiber support containing NaA molecular sieve conversion
[0057] With embodiment 1.
[0058] (2) In situ hydrothermal synthesis of NaA molecular sieve membrane
[0059] According to molar ratio Na 2 O:SiO 2 :Al 2 o 3 :H 2O=41.9:4.4:1:833.3 Prepare the synthesis solution for synthesizing molecular sieve membranes. Weigh 4.34g of water glass (solid content 55%) and 19.15g of sodium hydroxide into 54.86g of deionized water, and stir at room temperature for 15 minutes to completely dissolve it; simultaneously weigh 1.20g of sodium aluminate and add to 36.20g of In deionized water, stir at room temperature for 15 minutes to dissolve completely. Then pour the sodium aluminate solution into the constantly stirring sodium silicate solution. After the end, the synthetic solution was continuously stirred at room temperature for 1 hour to complete the aging. The support was inserted into the synthesis solution, and after static in-s...
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