A kind of molecular sieve membrane, membrane reactor and its application in the preparation of p-tert-butylphenol
A technology of p-tert-butylphenol and membrane reactor, which is applied in the direction of molecular sieve catalysts, preparation of organic compounds, membranes, etc., and can solve problems such as difficult product separation
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Embodiment 1
[0060] (1) Prepare the low-temperature synthesis mother liquor of MCM-22 molecular sieve:
[0061] Add 5400g water and 72g NaOH to the container successively, and stir for 30min; then add 33.7g alumina, stir 1830g silica sol (30wt% silica concentration) for 2h, and finally add 350g CTAB and stir for 3h to obtain a gel. The gel was transferred to a reaction kettle, and crystallized at a low temperature of 100° C. for 8 hours to prepare a low-temperature synthesis mother liquor of MCM-22 molecular sieve. In the synthesis mother liquor, the molar ratio of each component is: SiO 2 :Al 2 o 3 :Na + :CTAB=9.14:0.33:1.8:0.96.
[0062] (2) Preparation of molecular sieve membrane:
[0063] Prepare a cylindrical steel mesh with a diameter of 20 cm and a height of 30 cm (aperture 1 μm), and coat a layer of Al on the inside of the steel mesh 2 o 3 Adhesive, coated with a thickness of about 1mm, placed in a high-temperature baking furnace at 600°C for 4 hours to make α-Al 2 o 3 Ine...
Embodiment 2
[0067] (1) Prepare the low-temperature synthesis mother liquor of ZSM-5 molecular sieve:
[0068] Weigh 400g NaOH, add it to 1600g deionized water, stir until completely dissolved, then add 15290g 25% TPAOH solution and stir for 20min; then, slowly drop 14120g 34% silica sol solution into the above solution, stir for 4h; add 695g TPAOH solution Aluminum, stirred for 4 hours to obtain a gel; transfer the above gel to a stainless steel hydrothermal kettle, carry out the first stage of crystallization reaction in an oven at 100°C, and quench the crystallized mother liquor under cold water at 20°C after 8 hours Cool to obtain the first section of crystallization solution; under the condition of 20°C water bath, add 3530g 34% silica sol and 1300g water to the first section of crystallization solution, stir for 20min, and put it into the stainless steel crystallization kettle again, at 180 The second-stage crystallization reaction is carried out at ℃, and the second-stage crystalliz...
Embodiment 3
[0076] [Example 3] Preparation of p-tert-butylphenol by membrane reactor MR-1
[0077] Using phenol and isobutylene as raw materials, under the action of HMCM-22 molecular sieve catalyst, the membrane reactor MR-1 reacts continuously. Wherein, the catalyst loading accounts for 50% of the reactor volume in the membrane, the molar feed ratio of phenol and isobutylene is 10:1, the reaction temperature is 120°C, the reaction pressure inside the membrane is set at 50KPaG, and the external pressure of the membrane is 5KPaG. The reaction liquid is sent to a rectification tower, the unreacted phenol is recovered at the top of the tower, and p-tert-butylphenol is obtained at the bottom of the tower (product purity 99.77%). In this example, the conversion rate of isobutene is 99.92%, and the selectivity to p-tert-butylphenol is 99.92%.
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