Method for fixing homogeneous catalyst and catalyst material
A technology of homogeneous catalysts and catalytic materials, applied in the direction of catalyst carriers, molecular sieve catalysts, chemical instruments and methods, etc., can solve the problems of limited separation, fine crystals are not stable enough, and hinder
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Embodiment 3
[0035] 2.0g of mesoporous MFI type zeolite was mixed with 1.0g of Mn(CH 3 COO) 2 4H 2 The aqueous solution of O was ion-exchanged at room temperature for 24 h. After filtration and drying, the zeolitic material was suspended in CH 2 Cl 2 / methanol (1:1). To this slurry was added 0.10 ml of diaminocyclohexane. The mixture was stirred for 24h. After addition of 200 mg of 3,5-bis(tert-butyl)salicylaldehyde and 100 mg of LiCl, the mixture was stirred in air for another 48 h.
[0036] The resulting light brown material, Jacobsen's catalyst immobilized in a mesoporous MFI type zeolite, was filtered and washed with CH 2 Cl 2 Wash several times and dry in air at 50°C.
Embodiment 4
[0038] 2.0g of mesoporous MFI type zeolite was mixed with 0.50g of Co(CH 3 COO) 2 4H 2 O and 0.98gMn(CH 3 COO) 2 4H 2 An aqueous solution of O (molar ratio Co:Mn 1:2) was ion-exchanged at 65°C for 4h. After filtration and drying, the zeolitic material was suspended in glacial acetic acid (18 ml). To the slurry was added pyridine (3.6ml), NaBr (0.60g) and H 2 o 2 (35%, 7.7ml). The mixture was stirred at room temperature while passing air flow through the solution for 2h.
[0039] In the product, the catalyst of Chavan et al. immobilized in a mesoporous MFI type zeolite, after filtration, with CH 3 COOH washed and dried in vacuo.
[0040] The catalyst of Comparative Example 1 had a metal loading of 1315 ppm Mn. The catalyst of Example 3 had a metal loading of 5970 ppm Mn.
[0041] The IR spectra of the two catalysts were indistinguishable from each other and compared with the unsupported Jacobsen catalyst N,N'-bis(3,5-di-tert-butyl-salicylidene)-1,2-cyclohexane-diami...
Embodiment 5
[0046] Sodium hypochlorite aqueous solution and Na 2 HPO 4 The solution was mixed and the pH was adjusted to 11.3. The catalyst from Comparative Example 1 (908 mg) or from Example 3 (200 mg, providing the same amount of Mn for both catalysts) was added to the cooled solution (0°C). A solution of 10 mmoles of styrene in 10 ml of dichloromethane was then added with stirring. The biphasic mixture was stirred at room temperature for a total of 5 h. Stir intermittently every 20min, and take samples from the separated organic phase, wash with water, in Na 2 SO 4 dried and analyzed by GC-MS. The mesoporous catalyst from Example 3 shows faster conversion of styrene to styrene oxide than the non-mesoporous catalyst from Comparative Example 1 .
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