湿法冶金
濕法冶金
습법야금
HYDROMETALLURGY OF CHINA
2014年
4期
292-296
,共5页
于林华%黎铉海%李林艳%曾中贤%范闽光%徐盛明%王学军%刘欣
于林華%黎鉉海%李林豔%曾中賢%範閩光%徐盛明%王學軍%劉訢
우림화%려현해%리림염%증중현%범민광%서성명%왕학군%류흔
2-羟基-5-特辛基苯乙酮肟%铜萃取剂%Fries重排%合成
2-羥基-5-特辛基苯乙酮肟%銅萃取劑%Fries重排%閤成
2-간기-5-특신기분을동우%동췌취제%Fries중배%합성
2-hydroxy-5-t-octylacetophenone oxime%copper%extractant%Fries rearrangement%synthesis
研究了用4-特辛基酚、乙酰氯、三氯化铝、盐酸羟胺、异辛酸为原料,用四氯乙烷为溶剂,经3步反应合成2-羟基-5-特辛基苯乙酮肟。在AlCl3作用下,乙酸-(4-特辛基)-苯酯经过Fries重排合成2-羟基-5-特辛基苯乙酮,其优化的合成条件为:以四氯乙烷为溶剂,n(AlCl3)∶ n(4-特辛基酚)=1.2∶1,反应温度120℃,反应时间6 h。该条件下,2-羟基-5-特辛基苯乙酮的合成产率为90.8%(以辛基酚计),液相色谱纯度为89.2%。产物经IR、1 H-NM R表征确认。由于特辛基的位阻比壬基的高,相同条件下合成的2-羟基-5-特辛基苯乙酮肟的纯度明显比2-羟基-5-壬基苯乙酮肟高;此外,由于高位阻基团的存在,有望提高其对铜的反萃取性能。
研究瞭用4-特辛基酚、乙酰氯、三氯化鋁、鹽痠羥胺、異辛痠為原料,用四氯乙烷為溶劑,經3步反應閤成2-羥基-5-特辛基苯乙酮肟。在AlCl3作用下,乙痠-(4-特辛基)-苯酯經過Fries重排閤成2-羥基-5-特辛基苯乙酮,其優化的閤成條件為:以四氯乙烷為溶劑,n(AlCl3)∶ n(4-特辛基酚)=1.2∶1,反應溫度120℃,反應時間6 h。該條件下,2-羥基-5-特辛基苯乙酮的閤成產率為90.8%(以辛基酚計),液相色譜純度為89.2%。產物經IR、1 H-NM R錶徵確認。由于特辛基的位阻比壬基的高,相同條件下閤成的2-羥基-5-特辛基苯乙酮肟的純度明顯比2-羥基-5-壬基苯乙酮肟高;此外,由于高位阻基糰的存在,有望提高其對銅的反萃取性能。
연구료용4-특신기분、을선록、삼록화려、염산간알、이신산위원료,용사록을완위용제,경3보반응합성2-간기-5-특신기분을동우。재AlCl3작용하,을산-(4-특신기)-분지경과Fries중배합성2-간기-5-특신기분을동,기우화적합성조건위:이사록을완위용제,n(AlCl3)∶ n(4-특신기분)=1.2∶1,반응온도120℃,반응시간6 h。해조건하,2-간기-5-특신기분을동적합성산솔위90.8%(이신기분계),액상색보순도위89.2%。산물경IR、1 H-NM R표정학인。유우특신기적위조비임기적고,상동조건하합성적2-간기-5-특신기분을동우적순도명현비2-간기-5-임기분을동우고;차외,유우고위조기단적존재,유망제고기대동적반췌취성능。
Using 4-tert-octylphenol ,CH3COCl ,AlCl3 ,NH2 OH · HCl ,2-ethylhexanoic acid as reactants and tetrachlor-ethane as solvent ,2-hydroxy-5-t-octylacetophenone oxime is synthesized through three steps of reaction .The key step is the Fries of 4-tert-octylphenyl acetate under the catalysis of AlCl3 . The optimal synthesis conditions which affords 2-hydroxy-5-t-octylacetophenone of 90 .8% yields and 89 .2% purities are as follows :n(AlCl3 )∶ n(4-tert-octylpheno)= 1 .2∶1 ,θ= 120 ℃ ,t= 6 h .The structure of the product is identified by IR and 1 H-NMR . The purity of 2-hydroxy-5-t-octylacetophenone oxime is obviously higher than the nonyl-product under the same synthesis conditions presumably due to the high steric hindrance of tert-octyl .T he produce is hopeful to improve the striping performance as copper extractant .