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以三氧化二钒为钒源,在体系中引入氧化剂和水夹带剂,合成了乙酰丙酮氧钒,实现了乙酰丙酮氧钒的绿色连续合成。探讨了空气、过氧化氢和氧气3种氧化剂对乙酰丙酮氧钒合成的影响,对产物进行表征并与商业乙酰丙酮氧钒对比。结果表明,引入氧化剂后,乙酰丙酮氧钒的产率显著提高,3种氧化剂制得的乙酰丙酮氧钒产率均可达到80%以上,其中氧气氧化效果最好,当氧气流量为200 mL/min,回流2 h时,乙酰丙酮氧钒产率可达90%。XRD、FTIR和TG结果显示,该文合成的乙酰丙酮氧钒与商业乙酰丙酮氧钒纯度相当。
With vanadium trioxide as vanadium source, oxidant and water entrainer were introduced into the system to synthesize vanadyl acetylacetonate, which achieved the green continuous synthesis of vanadyl acetylacetonate. The effects of three oxidants, air, hydrogen peroxide and oxygen, on vanadyl acetylacetonate synthesis were investigated. The products were characterized and compared with commercial vanadyl acetylacetonate. The results showed that the yield of vanadyl acetylacetonate increased remarkably with the introduction of oxidant. The yield of vanadyl acetylacetonate obtained by three oxidants can all reach more than 80%. The oxygen oxidation effect is the best. When the oxygen flow rate is 200 mL / min, refluxed 2 h, vanadyl acetylacetonate yield of up to 90%. The results of XRD, FTIR and TG show that vanadyl acetylacetonate synthesized in this paper has the same purity as commercial vanadyl acetylacetonate.