A kind of framework vanadium mcm-41 molecular sieve and its preparation method and application
A technology of MCM-41 and molecular sieve, applied in the field of molecular sieve, can solve the problems of blocking molecular sieve channels, increasing side reactions, catalyst deactivation, etc., and achieving the effects of easy industrial application, reduction of production cost, and simple preparation method.
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Embodiment 1
[0047] Under the condition of 30°C, 10g of cetyltrimethylammonium bromide (CTAB) and 85.7g of deionized water were successively added into the reactor, stirred evenly, and then 1.89g of ammonium metavanadate and 2.5g of oxalic acid were added, Stir well until the blue clear solution is obtained, then add 6.6g of tartaric acid, continue to stir, slowly add 11g of tetraethyl orthosilicate (TEOS) dropwise, and finally add 10.8g of NaOH to adjust the pH of the solution to 11-13. The ratio is SiO 2 :90H 2 O:0.5R:0.3V:5OH - , the mixture was transferred to a crystallization kettle, heated to 110° C., and crystallized at a constant temperature for 72 hours. After the crystallization is complete, when the temperature drops to room temperature, the reacted mixture is separated, washed, and dried at 100°C, and the dried sample is calcined at 550°C for 6 hours to obtain V -MCM-41 molecular sieve raw powder. The obtained samples were analyzed by XRF and BET, and the results are shown ...
Embodiment 2
[0050] Same as Example 1, the difference is that cetyltrimethylammonium bromide is changed into cetyltrimethylammonium chloride (CTAC), consumption is changed into 6.9g, and the amount of deionized water is changed into is 63.4g, the amount of ammonium metavanadate is changed into 1g, the amount of oxalic acid is changed into 1.1g, the amount of tartaric acid is changed into 6.27g, the amount of TEOS is changed into 9.1g, the amount of NaOH is changed into 10.4g, the obtained mixture The molar ratio is SiO 2 :80H 2 O:0.6R:0.2V:6OH - , the crystallization temperature was 120°C, the crystallization time was 80h, and the other components and synthesis conditions were unchanged, and the raw powder of V-MCM-41 molecular sieve was obtained. The obtained samples were analyzed by XRF and BET, and the results are shown in Table 1.
[0051] The obtained molecular sieve was used for the hydroxylation of benzene to prepare phenol. The conditions of the hydroxylation reaction were the s...
Embodiment 3
[0053] Same as Example 1, the difference is that the amount of CTAB is changed into 8g, the amount of deionized water is changed into 56.5g, ammonium metavanadate is changed into sodium orthovanadate, consumption is 1.7g, and the amount of oxalic acid is changed into For 1.2g, tartaric acid is changed to citric acid, and the dosage is 13.3g, and TOES is changed to sodium silicate, and the dosage is 9.0g, and the amount of NaOH is changed to 6.3g, and the molar ratio of the obtained mixture is SiO 2 :100H 2 O:0.7R:0.3V:5OH - , the crystallization temperature was 130°C, the crystallization time was 50h, and the other components and synthesis conditions were unchanged, and the raw powder of V-MCM-41 molecular sieve was obtained. The obtained samples were analyzed by XRF and BET, and the results are shown in Table 1.
[0054] The obtained molecular sieve was used for the hydroxylation of benzene to prepare phenol. The conditions of the hydroxylation reaction were the same as tho...
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