Method for preparing high-performance Silicalite-1 molecular sieve membrane in super-dilute synthetic fluid
A dilute synthetic liquid and molecular sieve technology, applied in chemical instruments and methods, membrane technology, semi-permeable membrane separation, etc., can solve the problems of unseen literature reports, synthetic membrane performance reports, and inability to realize industrialization, so as to improve flux and selectivity, content reduction, and preparation cost reduction
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Embodiment 1
[0040] Synthesis of embodiment 1 Silicalite-1 molecular sieve crystal
[0041] Take a certain amount of TPAOH aqueous solution and flaky NaOH dissolved in deionized water, stir to dissolve and cool to room temperature, then continue to add a certain amount of silica sol to the above solution, and finally the composition (molar ratio) of each component in the solution is SiO 2 : 0.3TPAOH : 0.15NaOH : 45H 2 O, then aging at room temperature, after aging for 24 hours, put it into a stainless steel reactor, and put the stainless steel reactor into an oven at 130°C for 30 hours to synthesize. The synthesized crystals were washed with deionized water until neutral and then dried. After drying, they were placed in a muffle furnace and calcined at 550° C. for 12 hours to remove the template agent (such as figure 1 ). Calcined crystals are detected by XRD (X-ray diffraction) and show to be Silicalite-1 crystals (such as figure 2 ), and the molecular sieve crystals are in the shape ...
Embodiment 2
[0042] Embodiment 2 Preparation of Silicalite-1 molecular sieve membrane
[0043] The carrier used in this experiment is the tubular mullite produced by Japan Nikkato Co., Ltd. (the composition of mullite is 67wt.%Al 2 o 3 and 33wt.% SiO 2 ) as a carrier for synthesizing Silicalite-1 membrane, the inner diameter and outer diameter of the carrier are 9mm and 12mm respectively, the length is 100mm, the porosity is about 43%, and the average pore diameter is about 1 μm. Ultrasonic cleaning in deionized water and drying for later use. The dried carrier is coated with self-made Silicalite-1 molecular sieve.
[0044] Weigh a certain amount of TPAOH and deionized water and stir evenly to make it a uniform solution, then add a certain amount of TEOS to the above solution and continue stirring and aging at room temperature until it becomes a clear and transparent solution at room temperature. The composition (molar ratio) of each component in the solution is TEOS: 0.3TPAOH: 500H 2...
Embodiment 3
[0049] Embodiment 3 Preparation of Silicalite-1 molecular sieve membrane
[0050] The synthetic liquid raw material and operation that adopt are as embodiment 2, just the proportioning of the synthetic liquid that forms is TEOS: 0.3TPAOH: 600H 2 O, other preparation steps are identical with embodiment 2. After calcination, the Silicalite-1 molecular sieve membrane was used for pervaporation experiments and characterizations. The results of the pervaporation experiments are shown in S-3 and S-4 in Table 2.
[0051] Table 2 Pervaporation separation performance of Silicalite-1 molecular sieve membrane on mullite carrier (60℃)
[0052]
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