化工进展
化工進展
화공진전
CHEMICAL INDUSTRY AND ENGINEERING PROGRESS
2014年
11期
3053-3056,3081
,共5页
1,4-二氯蒽醌%合成%氯转羟基%机理
1,4-二氯蒽醌%閤成%氯轉羥基%機理
1,4-이록은곤%합성%록전간기%궤리
1,4-dihydroxyanthraquinone%synthesis%chlorine hydroxylation%mechanism
以廉价的对二氯苯和邻苯二甲酸酐为原料制得1,4-二氯蒽醌,经硼酸催化水解得到1,4-二羟基蒽醌。系统地考察了反应温度、硫酸浓度、原料摩尔比和反应时间对氯转羟基反应的影响。确定了氯转羟基反应制备1,4-二羟基蒽醌的优化实验条件为:以95%浓硫酸为溶剂,在反应温度为220℃、硫酸∶1,4-二氯蒽醌∶硼酸(摩尔比)为37.5∶1.0∶1.4、反应时间为60min的条件下,以1,4-二氯蒽醌计的产物收率为71.0%。探讨和解释了硼酸催化作用下氯代蒽醌转换成羟基蒽醌可能的机理。
以廉價的對二氯苯和鄰苯二甲痠酐為原料製得1,4-二氯蒽醌,經硼痠催化水解得到1,4-二羥基蒽醌。繫統地攷察瞭反應溫度、硫痠濃度、原料摩爾比和反應時間對氯轉羥基反應的影響。確定瞭氯轉羥基反應製備1,4-二羥基蒽醌的優化實驗條件為:以95%濃硫痠為溶劑,在反應溫度為220℃、硫痠∶1,4-二氯蒽醌∶硼痠(摩爾比)為37.5∶1.0∶1.4、反應時間為60min的條件下,以1,4-二氯蒽醌計的產物收率為71.0%。探討和解釋瞭硼痠催化作用下氯代蒽醌轉換成羥基蒽醌可能的機理。
이렴개적대이록분화린분이갑산항위원료제득1,4-이록은곤,경붕산최화수해득도1,4-이간기은곤。계통지고찰료반응온도、류산농도、원료마이비화반응시간대록전간기반응적영향。학정료록전간기반응제비1,4-이간기은곤적우화실험조건위:이95%농류산위용제,재반응온도위220℃、류산∶1,4-이록은곤∶붕산(마이비)위37.5∶1.0∶1.4、반응시간위60min적조건하,이1,4-이록은곤계적산물수솔위71.0%。탐토화해석료붕산최화작용하록대은곤전환성간기은곤가능적궤리。
1,4-dihydroxyanthraquinone was obtained by boric acid catalytic hydrolysis of 1,4-dichloroanthraquinone , which was synthesized by using commercial phthalic anhydride and p-dichlorobenzene as raw materials. The effect of reaction temperature,sulfuric acid concentration (mass concentration),molar ratio of reactants and reaction time on the chlorine hydroxylation reaction was investigated,and optimal experimental conditions were obtained as follows,temperature 220℃, sulfuric acid concentration 95%,molar ratio of sulfuric acid/1,4-dichloroanthraquinone/boric acid 37.5 ∶ 1.0 ∶ 1.4 , reaction time 60min. Under above conditions , the yield of 1,4-dihydroxyanthraquinone was 71.0%. The possible mechanism of chlorine hydroxylation with the catalytic effect of boric acid was discussed.