化工技术与开发
化工技術與開髮
화공기술여개발
TECHNOLOGY & DVELOPMENT OF CHEMICAL INDUSTRY
2014年
6期
22-24
,共3页
2,4-二氯-1,3,5-三硝基苯%硝化%合成工艺
2,4-二氯-1,3,5-三硝基苯%硝化%閤成工藝
2,4-이록-1,3,5-삼초기분%초화%합성공예
2,4-dichloro-1,3,5-trinitrobenzene%nitration%synthetic process
采用2,4-二氯硝基苯为原料，以硝硫混酸为硝化试剂，经硝化反应得到2,4-二氯-1,3,5-三硝基苯。研究了硝化体系的比例、反应温度和反应时间对硝化反应的影响，确定了合成工艺条件为：发烟硫酸与发烟硝酸的体积比为5∶1、反应温度为150℃，反应时间为8 h，产品得率达64%以上。对产物样品进行熔点测定，熔点为127~128℃。用薄层色谱和高效液相色谱分析了样品的纯度，用红外和核磁共振表征了样品的结构。
採用2,4-二氯硝基苯為原料，以硝硫混痠為硝化試劑，經硝化反應得到2,4-二氯-1,3,5-三硝基苯。研究瞭硝化體繫的比例、反應溫度和反應時間對硝化反應的影響，確定瞭閤成工藝條件為：髮煙硫痠與髮煙硝痠的體積比為5∶1、反應溫度為150℃，反應時間為8 h，產品得率達64%以上。對產物樣品進行鎔點測定，鎔點為127~128℃。用薄層色譜和高效液相色譜分析瞭樣品的純度，用紅外和覈磁共振錶徵瞭樣品的結構。
채용2,4-이록초기분위원료，이초류혼산위초화시제，경초화반응득도2,4-이록-1,3,5-삼초기분。연구료초화체계적비례、반응온도화반응시간대초화반응적영향，학정료합성공예조건위：발연류산여발연초산적체적비위5∶1、반응온도위150℃，반응시간위8 h，산품득솔체64%이상。대산물양품진행용점측정，용점위127~128℃。용박층색보화고효액상색보분석료양품적순도，용홍외화핵자공진표정료양품적결구。
The 2,4-dichloro-1,3,5-trinitrobenzene was obtained by nitration starting from 2,4-dichloronitrobenzene, with fuming nitric acid and fuming sulfuric acid as nitration reagent. Effect of nitration reagent ratio, reaction temperature and reaction time on the yield of product was observed. The synthesis conditions were obtained: the volume ratio of fuming sulfuric acid to fuming nitric acid was 5:1, the reaction temperature was 150℃, the reaction time was 8 hours. The yield of product was above 64%. The melting test showed that the melting point of sample was 127~128℃. The sample was analyzed by TLC and HTLC, and the structure was characterized by IR and1HNMR.
