Process for continuously producing isopropanolamine
A propylene oxide and loop reactor technology, applied in the field of continuous process, can solve the problems of improper control of propylene oxide concentration, poor selectivity of monoisopropanolamine, easy occurrence of temperature flying, etc. Eliminate the effects of many side reactions and long service life
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[0056] Preparation of immobilized heteropolyacid catalyst:
[0057] 1. Experimental raw materials
[0058] Phosphotungstic acid (H 3 [P(W 3 o 10 ) 4 ]·12H 2 O), silicotungstic acid (H 3 [Si(W 3 o 10 ) 4 ]·12H 2 O), phosphomolybdic acid (H 3 [P(Mo 3 o 10 ) 4 ]·12H 2 O): analytically pure, Sigma-Aldrich (Shanghai) Trading Co., Ltd.,
[0059] Bentonite, MCM-41, methanol: analytically pure, Sinopharm Chemical Reagent Co., Ltd.
[0060] 2. Preparation example
preparation example 1
[0062] Catalyst A: Immobilized phosphotungstic acid catalyst
[0063] Add 1.5g of phosphotungstic acid and 12.55g of bentonite into a three-necked flask, then add 70ml of methanol to dissolve completely, and stir at room temperature for 5h. After that, the solvent was removed under reduced pressure, and the product was dried in a vacuum oven at 110°C for 6 hours. After drying, it was roasted in a muffle furnace at 300°C for 8 hours to prepare a solid-supported heteropolyacid with a loading capacity of phosphotungstic acid of about 10%. catalyst. By adjusting the amount of phosphotungstic acid and bentonite, it is possible to prepare immobilized phosphotungstic acid catalysts with loadings of 20%, 30%, 40%, 50%, and 60%.
preparation example 2
[0065] Catalyst B: Immobilized phosphomolybdic acid catalyst
[0066] Add 1.5g of phosphomolybdic acid and 3.13g of MCM-41 into a three-necked flask, then add 30ml of methanol to dissolve completely, and stir at room temperature for 5h. Afterwards, the solvent was removed under reduced pressure, and the product was dried in a vacuum oven at 120°C for 4 hours. After drying, it was activated in a muffle furnace at 250°C for 10 hours to prepare a solid-supported heteropolyacid with a loading capacity of phosphomolybdic acid of about 30%. catalyst. By adjusting the amount of phosphomolybdic acid and MCM-41, the immobilized phosphomolybdic acid catalysts with loadings of 10%, 20%, 40%, 50% and 60% can be prepared.
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