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采用十六烷基三甲基氯化铵、磷钼酸和乙醇为原料,制备磷钼杂多酸盐催化剂,然后对其脱硫性能进行考察。实验过程中考察了催化剂制备条件对催化剂催化脱硫性能的影响。从而确定了催化剂最佳制备条件:十六烷基三甲基氯化铵与磷钼酸的摩尔比为1∶1;制备温度为60℃;反应时间为2h;干燥活化时间为10h。在上述的实验条件下,精制的磷钼杂多酸季铵盐在焦化柴油脱硫实验中具有很高的催化活性。结果表明,以三氟乙酸为氧化剂,以制备的磷钼杂多酸盐为催化剂,反应温度为60℃,反应时间为70min的条件下,经糠醛多级萃取和氧化铝吸附后柴油的硫含量可从1052μg/g降至48.2μg/g,脱硫率为95.4%,柴油的收率为92.5%,达到了欧Ⅲ标准对硫含量的要求。
Using cetyltrimethylammonium chloride, phosphomolybdic acid and ethanol as raw materials, the phosphomolybdic heteropolyacid salt catalyst was prepared, and then the desulfurization performance was investigated. During the experiment, the effect of catalyst preparation conditions on catalytic performance of catalyst was investigated. The optimum conditions were as follows: the molar ratio of cetyl trimethyl ammonium chloride to phosphomolybdic acid was 1: 1; the preparation temperature was 60 ℃; the reaction time was 2h; the drying activation time was 10h. Under the above experimental conditions, refined phosphomolybdic heteropolyacid quaternary ammonium salt has high catalytic activity in coking diesel desulfurization experiments. The results showed that under the conditions of trifluoroacetic acid as oxidant, prepared molybdophosphoric acid heteropolyacid salt as catalyst, the reaction temperature was 60 ℃ and the reaction time was 70min, the sulfur content of diesel oil after multi-stage extraction with furfural and alumina adsorption From 1052μg / g down to 48.2μg / g, the desulfurization rate was 95.4%, the yield of diesel was 92.5%, reached the European Ⅲ standard sulfur content requirements.