Preparation method and application of heterogeneous epoxy catalyst
A technology of oxidation catalyst and phase ring, which is applied in physical/chemical process catalysts, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., to achieve simple preparation process, stable reuse performance, and convenient catalyst recovery. Effect
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Embodiment 1
[0029] (1) PS-[MoO 2 (H 2 Preparation of FSAP)DMF]:
[0030] ① Ligand H 2 Synthesis of FSAP: 1.66g (10mmol) of 3-formyl salicylic acid and 1.09g (10mmol) of o-aminophenol were mixed and dissolved in 30mL of absolute ethanol, stirred for 6h under reflux to produce orange-red precipitate, filtered and dried , recrystallized in boiling alcohol, filtered and dried to obtain the pure ligand H 2 FSAP.
[0031] ②PS-H 2 Synthesis of FSAP: 1g PS (equivalent to 4.69mmol Cl) microspheres were added to a 100mL three-necked flask, swelled in 10mL DMF for 2h, and 3.6g H 2 A 15 mL DMF solution of FSAP (14 mmol, 1:3 amount of microspheres and ligand) was added to the suspension solution, followed by a 100 mL ethyl acetate solution of 4.5 g triethylamine. React for 15 hours under mechanical stirring at 90°C, filter after cooling down to room temperature, wash with hot DMF and methanol several times, and dry in an oven at 120°C to obtain purple-red PS-H 2 FSAP microspheres.
[0032] ③PS...
Embodiment 2
[0035] (1) PS-[MoO 2 (H 2 FSAP) DMF] preparation: same as Example 1.
[0036] (2) Synthesis of epoxy fatty acid methyl ester: 10g of refined fatty acid methyl ester, 0.5gPS-[MoO 2 (H 2 FSAP)DMF], 10mL of 1,2-dichloroethane were added to a 100mL three-necked flask, ozone was introduced into the reaction system at a flow rate of 0.50mg / min, and the epoxidation reaction was carried out at 80°C. After the reaction, the reaction mixture was depressurized Epoxy fatty acid methyl esters are obtained after distillation. The catalyst can be reused 4 times.
Embodiment 3
[0038] (1) PS-MP-[MoO 2 (H 2 Preparation of FSAP)DMF]:
[0039] ① Ligand H 2 Synthesis of FSAP: same as Example 1.
[0040] ②PS-MP-H 2 Synthesis of FSAP: 1g PS-MP (equivalent to 3.5mmol Cl) was added to a 100mL three-neck flask, swelled in 10mL DMF for 2h, 2.69g H 2 A 15 mL DMF solution of FSAP (10.5 mmol, 1:3 amount of microspheres and ligand) was added to the suspension solution, followed by a 100 mL ethyl acetate solution of 4.5 g triethylamine. React for 15 hours under mechanical stirring at 90°C, filter after cooling down to room temperature, wash with hot DMF and methanol several times, and dry in an oven at 120°C to obtain orange PS-MP-H 2 FSAP microspheres.
[0041] ③PS-MP-[MoO 2 (H 2 FSAP) DMF] synthesis: add 1gPS-MP-H in 100mL there-necked flask 2 FSAP (equivalent to 1.17mmol Schiff base ligand), swell in 15mlDMF for 2h, 0.77gMoO 2 (acac) 2 (2.34mmol, 1:2 the amount of Schiff base ligand and metal) was added to the above suspended state, reacted in an oil ...
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