Method of recovering and utilizing oligomer of polymer catalyst for catalyzing aldol condensation
A technology for catalyzing aldols and catalysts, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc., can solve the problem of low preparation yield and no catalytic aldol condensation activity , inactivity and other problems, to achieve the effect of improving the preparation yield, uniform molecular weight distribution and reducing costs
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Embodiment 1
[0027] (1) Monomer I and monomer II are copolymerized to prepare PNL
[0028] Add 4.70g of monomer I, 1.17g of monomer II, 0.09g of initiator AIBN and 10.0mL of solvent DMF to a 50mL thick-walled pressure-resistant bottle with a side branch (Beijing Shinwell Glass Instrument Co., Ltd.), and remove water and oxygen After that, the reaction was stirred at 75°C for 8h. Carry out the following post-treatment operations in a glove box (with oxygen below 1ppm and water below 10ppm): 100g of anhydrous ether is used as a precipitating agent to precipitate the product, and the clear liquid and precipitate are obtained after pouring. The clear solution was simply desolvated to obtain 11.0 g of a DMF solution of PN radicals, which was used in the second step of PN oligomer polymerization to prepare PNL. The precipitate was dried at a vacuum degree of -0.095 MPa at 50° C. for 8 hours to obtain 4.37 g of catalyst PNL with a preparation yield of 74.4%.
[0029] (2) PN oligomer polymerizat...
Embodiment 2
[0032] Add 11.30 g of PN free radical DMF solution (PN free radical content 11.5 wt%), 0.40 g of monomer II and 0.03 g of initiator AIBN into a 50 mL thick-walled pressure-resistant bottle with side branch, stir to dissolve, and remove oxygen. The reaction was stirred at 75°C for 8 hours. After the reaction, 200 g of anhydrous ether was used as a precipitant to precipitate the product and centrifuged. The precipitate was dried at a vacuum of -0.080MPa at 80°C for 10 hours to obtain 1.52g of catalyst PNL-II with a preparation yield of 89.4%, which effectively increased the PNL preparation yield by 22.8%, and the average molecular weight was 70000, where a:b=7: 1.
Embodiment 3
[0034] Add 11.80 g of PN free radical DMF solution (PN free radical content 15.2 wt%), 0.10 g of monomer II and 0.05 g of initiator AIBN into a 50 mL thick-walled pressure-resistant bottle with a side branch in sequence, stir to dissolve, and remove oxygen. The reaction was stirred at 75°C for 8 hours. After the reaction, 300 g of anhydrous ether was used as a precipitant to precipitate the product and centrifuged. The precipitate was dried at a vacuum of -0.05MPa at 30°C for 12h to obtain 1.52g of catalyst PNL-III, with a preparation yield of 80.4%, which effectively increased the PNL preparation yield by 19.7%, and the average molecular weight was 45000, where a:b=36: 1.
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