Fuel oil desulfurizer and preparation thereof
A desulfurizer and fuel oil technology, which is applied in the petroleum industry, refined hydrocarbon oil, etc., can solve the problems of slow diffusion, affecting the removal effect of thiophene sulfur, and the hydrothermal stability needs to be improved, and achieve the effect of improving the desulfurization rate.
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[0021] The present invention provides the preparation method of above-mentioned desulfurizer, and this method comprises the following steps:
[0022] (1) preparing a crosslinking liquid by one or more soluble compounds selected from zirconium, silicon, and aluminum;
[0023] (2) Mix the clay suspension whose pH value has been adjusted between 0.5-5.0 with the cross-linking liquid described in step (1), while stirring continuously and raising the temperature to 50-90°C, to carry out cross-linking treatment on the clay ;
[0024] (3) washing, centrifuging and heat-treating the clay obtained in step (2) cross-linking treatment to obtain cross-linking clay;
[0025] (4) Add the cross-linked clay obtained in step (3) into the aqueous solution of the soluble compound of rare earth metal and / or transition metal, carry out impregnation treatment, then carry out centrifugation, drying, drying and roasting to obtain fuel oil desulfurizer .
[0026] In the above preparation method, th...
Embodiment 1
[0046] (1) Add 7.5g of zirconium oxychloride to 100ml of water to make an aqueous solution of zirconium oxychloride, adjust the pH to 1.1 with 1:10 ammonia water, raise the temperature of the solution to 80°C, stir for 6 hours, then cool down to room temperature, Prepared into zirconium cross-linking solution;
[0047] (2) 400ml of calcium-based montmorillonite suspension with a solid content of 4.0% was added dropwise to the zirconium crosslinking solution described in (1), and the crosslinking reaction was carried out at 80° C. for 12 hours, naturally cooled to room temperature and left standing. Wash with deionized water until no chloride ions can be detected with 0.1M silver nitrate solution. The obtained sample was dried at 100°C, placed in a muffle furnace and raised to 400°C at a heating rate of 10°C / min, kept for 2 hours, and then naturally cooled to room temperature. The obtained cross-linked clay sample number is A 0 ;
Embodiment 2
[0058] (1) 15.2g of zirconium oxychloride and 11.6g of aluminum nitrate are added to 412ml of water, the pH value is adjusted to 1.5 with ammonia water, and the mixed cross-linking liquid of zirconium and aluminum is prepared;
[0059] (2) 1500ml of calcium-based montmorillonite suspension with a solid content of 12.5% was adjusted to pH 1.5 with 0.5M hydrochloric acid solution;
[0060] (3) Quickly mix the mixed cross-linking solution of zirconium and aluminum with the calcium-based montmorillonite suspension, stir and raise the temperature to 90°C. After 8 hours of cross-linking reaction, cool down to room temperature and wash with deionized water to 0.1M No chloride ions can be detected in the silver nitrate solution, and it is dried at 120°C and crushed to below 40 mesh to obtain cross-linked clay. The obtained cross-linked clay sample number is B 0 ;
[0061] (4) 5.4g lanthanum nitrate, 1.8g zinc nitrate and 2.6g ferric nitrate are added to 160ml water to be mixed wit...
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