豆渣制取草酸工艺研究
Process of preparing oxalic acid from soybean dregs
  
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中文关键词:  豆渣  制取工艺  草酸
英文关键词:soybean dreg  preparation  oxalic acid
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WANG Qiao, YAN Zongguang  
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中文摘要:
      以豆渣为原料制取二水合草酸,研究了硫酸质量分数、干豆渣浸泡时间、硝酸用量、反应时间、反应温度及催化剂五氧化二矾-三氯化铁(质量比1∶?1)用量对草酸收率的影响,并对产品进行了质量测定。结果表明,豆渣制取草酸的最佳工艺条件为:硫酸质量分数70%,干豆渣浸泡时间3 h,硝酸、干豆渣、催化剂质量比2.1∶?1∶?0.002,反应时间5~6 h,反应温度65~70?℃。在最佳工艺条件下,采用母液套用的方法连续操作9批物料,二水合草酸收率平均可达76.5%,纯度99.5%。产品经红外光谱确定为草酸,熔点101.5?℃,铁盐和硫酸盐含量分别为0.002%和0.04%,850?℃灼烧残渣为0.07%。
英文摘要:
      Dihydrate oxalic acid was prepared from soybean dregs. The effects of mass fraction of sulphuric acid, immersion time of dry soybean dregs, dosage of nitric acid, reaction time, reaction temperature and dosage of catalyst(mass ratio of antimony pentoxide to ferric chloride 1∶?1) on the yield of oxalic acid were studied. The product quality was also determined.The results showed that the optimal conditions were obtained as follows: mass fraction of sulphuric acid 70%, immersion time of dry soybean dregs 3 h, mass ratio of nitric acid to dry soybean dregs to catalyst 2.1∶?1∶?0.002, reaction temperature 65-70?℃, and reaction time 5-6 h. Under these conditions, nine batches of materials were continuously operated by mother liquid recycle, and the yield and purity of oxalic acid dihydrate were 76.5% and 99.5%, respectively. The product was determined as oxalic acid by IR, and its melting point, iron salt and sulfate contents, and buring residule content at 850?℃ were 1015?℃, 0.002%, 0.04% and 0.07%, respectively.
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