Effect of water and impurity accumulation in reclaimed solvent on crystallization of carbazole from crude anthracene

YE Cuiping; WU Tingting; LI Wenying; ZHENG Huan; FENG Jie

doi:10.3969/j.issn.0438-1157.2014.09.027

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Effect of water and impurity accumulation in reclaimed solvent on crystallization of carbazole from crude anthracene

更新时间：2025-12-10

- Effect of water and impurity accumulation in reclaimed solvent on crystallization of carbazole from crude anthracene
- CIESC Journal Issue 9, Pages: 3505-3511(2014)
- 作者机构：
  
  太原理工大学煤科学与技术教育部与山西省重点实验室, 省部共建国家重点实验室培育基地,山西,太原,030024
- 作者简介：
- 基金信息：
- DOI：10.3969/j.issn.0438-1157.2014.09.027
  CLC： Q522.64
- Online First：05 September 2014，
  
  Published：05 September 2014
- 稿件说明：
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YE Cuiping, WU Tingting, LI Wenying, et al. Effect of water and impurity accumulation in reclaimed solvent on crystallization of carbazole from crude anthracene[J]. CIESC Journal, 2014, (9): 3505-3511.
DOI：

YE Cuiping, WU Tingting, LI Wenying, et al. Effect of water and impurity accumulation in reclaimed solvent on crystallization of carbazole from crude anthracene[J]. CIESC Journal, 2014, (9): 3505-3511. DOI： 10.3969/j.issn.0438-1157.2014.09.027.

摘要

考察了粗蒽结晶分离过程在溶剂循环使用时二甲苯中杂质和乙醇中水的积累对精制咔唑的影响。结果表明，随着二甲苯循环次数的增加，原料中的主要杂质萘、菲和芴在回收二甲苯中逐渐积累，其中萘的浓度最高可达0.35 mg·ml-1，滤饼中咔唑的含量降低2.77%（质量）左右，收率降低高达7.05%（质量）。同时，母液中杂质的积累使溶剂回收困难，二甲苯的损失率随着循环次数增加而增加，由单程实验的44.75%（体积）增加到循环3次时的79.17%（体积）。原料中的水分随着溶剂循环在回收溶剂中逐渐积累，循环使用3次后，乙醇的含水量高达6.65%（体积）。乙醇含水量在0～12%（体积）之间时，咔唑纯度在98%（质量）以上。含水量在0～6%（体积）时，咔唑的相对结晶度随含水量增加从45.67 %降到40.79 %；含水量为9%和12%时，相对结晶度分别为48.85% 和48.52%。

Abstract

To investigate the effect of water and other impurities in solvents on crystallization of carbazole from crude anthracene

the accumulation amount of impurities in xylene and water in ethanol in the solvent recycling were studied. Results showed that with the increase of xylene recycling

the main impurities in mother solution gradually accumulated in xylene

with the concentration of naphthalene up to 0.35 mg·ml-1 after recycling twice

and the carbazole content in the corresponding filter cake was reduced about 2.77% (mass) and the yield decreased 7.05% (mass). At the same time

the accumulation of impurities makes solvent recovery difficult

and the loss ratio of xylene increased from 44.75% (vol) to 79.17% (vol) after recycling three times. Water was gradually accumulated to 6.65% (vol) in ethanol. The purity of carbazole was higher than 98% (mass) when the water content added was between 0 to 12% (vol). The relative crystallinity of carbazole decreased from 45.67% to 40.79% when added water content is between 0 and 6% (vol) in ethanol; with the added water content of 9% (vol) and 12% (vol) in ethanol

it increased to 48.85% and 48.52%

respectively.

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