Oxidation desulfuration method based on modified MCM-41 anchored heteropolyacid catalyst
A MCM-41, oxidative desulfurization technology, applied in the direction of molecular sieve catalysts, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of catalysts being difficult to recycle, restricting industrial production applications, and large consumption of oxidants, etc., to achieve easy Recycling and reuse, saving oxidant usage, and improving desulfurization efficiency
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Embodiment 1
[0019] Embodiment 1: the synthesis of catalyst
[0020] (1) Preparation of amino-modified MCM-41: 1.0 MCM-41, 50 mL of absolute ethanol and 1.5 g of γ-aminopropyltriethoxysilane were placed in a 100 mL three-necked flask. in N 2 Under protection, the mixture was reacted for 12 h under the condition of reflux and stirring in a water bath at 70° C., and filtered by suction to obtain a white solid. The white solid was subjected to Soxhlet extraction with absolute ethanol as a solvent, the temperature was 180°C, the extraction time was 4 hours, and finally dried in an infrared dryer for 1 hour to obtain MCM-41 / amine.
[0021] (2)MCM-41 / amine / PW 12 o 40 Preparation: Dissolve 3.5g MCM-41 / amine in 40mL deionized water and stir at room temperature for 1h. 4.0g HPW 12 o 40 Dissolve it in 20mL deionized water, make it into a solvent, add it dropwise to the above MCM-41 / amine solution, stir vigorously at room temperature for 12 hours, and filter with suction to obtain a white solid...
Embodiment 2
[0022] Embodiment 2: the synthesis of catalyst
[0023] Except following difference, other is with embodiment 1: by changing heteropolyacid (H 3 PW 12 o 40 、H 3 PMo 12 o 40 、H 4 SiW 12 o 40 、H 4 PMo 11 V 1 o 40 、H 5 PMo 10 V 2 o 40 and H 6 PMo 9 V 3 o 40 ), the synthesized modified MCM-41 anchored heteropolyacid compound has 6 kinds, which are: MCM-41 / amine / PW 12 o 40 、MCM-41 / amine / PMo 12 o 40 、MCM-41 / amine / SiW 12 o 40 、MCM-41 / amine / PMo 11 V 1 o 40 、MCM-41 / amine / PMo 10 V 2 o 40 、MCM-41 / amine / PMo 9 V 3 o40 .
Embodiment 3
[0024] Embodiment 3: the simulation system of dibenzothiophene (DBT)-n-octane
[0025] Taking dibenzothiophene (DBT), which is difficult to remove in hydrodesulfurization, as a representative, a certain amount of DBT was dissolved in 60ml of n-octane to prepare a simulated system with a sulfur content of 500ppm, and 60ml of acetonitrile was added and heated with magnetic stirring to 60°C. Calculate H by O / S (molar ratio) = 10 2 o 2 Adding amount, calculated by 1% n-octane mass MCM-41 / amine / PW 12 o 40 The amount of catalyst added, the H 2 o 2 With MCM-41 / amine / PW 12 o 40 After pre-contacting for 10 minutes, it was added into the above simulation system. After 240 minutes of reaction, the conversion rate of DBT in n-octane reached 72.97%.
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