精蒽蒽含量测定方法的改进

ＨＧ２－１４００－８０精蒽蒽含量测定过程中滴定终点不明显，结果偏差大，经研究实验，在加指示剂滴定前加适量溶剂，可使滴定终点更明显，与原方法比较蒽含量结果相同，平行样结果更接近。     

精蒽蒽含量测定方法的改进

针对 HG2— 140 0— 80精蒽蒽含量测定过程中滴定终点不明显 ,结果偏差大 ,经研究实验 ,在加指示剂滴定前加适量溶剂 ,可使滴定终点明显。与原方法比较 ,蒽含量结果相同 ,平行样结果更接近。     

蒽烷基化和烷基转移合成2-戊基蒽工艺研究

2-戊基蒽是氧化法合成2-戊基蒽醌工艺的关键原料。以蒽和叔戊醇为原料经Friedel-Crafts烷基化合成了2-戊基蒽,由核磁共振氢谱(1H NMR)表征其结构,并考察催化剂、溶剂、反应物的量比、温度和时间对反应的影响。以烷基化的主要副产物二戊基蒽为原料,经烷基转移反应合成了2-戊基蒽,考察了催化剂、溶剂、温度、时间和反应物的量比对反应的影响。结果表明,AlCl3在烷基化和烷基转移反应中均具有良好的低温催化活性。在最佳烷基化反应条件下,蒽的转化率为92.8%,2-戊基蒽的收率为76.3%;在最佳烷基转移反应条件下,二戊基蒽的转化率为85.0%,2-戊基蒽的收率为68.9%。     

以精饼为原料合成吡唑蒽酮

用生产１－氨基蒽醌时的副产物精饼为原料，合成了吡唑蒽酮，含量达９３％以上。     

液膜结晶法制备精蒽的研究

实验研究了乳化结晶法制备精蒽的新工艺,考察了乳化剂用量、水/溶剂质量比以及助剂加入量等因素对精蒽质量的影响。实验结果表明,以苯乙酮作溶剂,采用十二烷基苯磺酸钠(SDBS)和Span20复合型乳化剂,经一次乳化结晶所得精蒽纯度大于95%,符合国家一级精蒽标准。     

从蒽油中提取精蒽和精咔唑的新工艺

介绍了从蒽油中提取精蒽和精咔唑的新工艺，分析了设备安装及生产中需要注意的问题。     

9-蒽硼酸的合成研究

蒽衍生物被认为是很有开发前景和实用价值的一类发光材料,9-蒽硼酸是合成其他蒽衍生物重要的中间体。本文以蒽为原料,经溴化得到9-溴蒽,再采用丁基锂法得到9-蒽硼酸。并对影响反应的重要因素进行了考察和讨论。反应需要在低于-70℃下进行,得到的收率达到79.8%。本文采用的工艺路线合理,反应时间短,产品收率高。     

精蒽提纯溶剂的选择和应用

精蒽作为生产蒽醌的原料随蒽醌用量的增加显得极为重要。本文论述了精蒽提纯溶剂选择的理论根据和试验依据,研究了以DMF及溶剂A为溶剂提高精蒽收率的方法。通过生产应用试验证明了小试及中试成果,可获得良好的经济及社会效益。     

焦油中精蒽／咔唑提取工艺的评述

介绍了近年来从焦油中提取精蒽和咔唑产品工艺的现状,并对两种常用工艺从工艺方案合理性、技术先进性及经济技术三方面做了较详尽的比较分析和综合评述。提出结晶－蒸馏法是目前提取精蒽／咔唑技术先进、工艺合理、有发展前途的工艺。同时提出了对现有溶剂洗涤法制取精蒽和咔唑工艺状况的改进设想。     

提高粗蒽质量的改进措施

1 存在问题 本钢焦化厂焦油车间主要生产粗蒽、工业萘、沥青等,粗蒽生产系统是以蒸馏工段的Ⅰ葸油为原料,在结晶机内强冷和自然冷却后,形成粗蒽结晶颗粒,经过真空分离脱去油和水,生产粗蒽产品.该工艺操作复杂,质量影响因素多.     

新型复合工艺制取蒽系产品的研究

研究了用复合工艺制取蒽系产品的新方法,该法可同时得到纯度９９．１４％的蒽、９６ ２８％的菲和９６．８８％的咔唑,具有流程简单、投资低和无环境污染等特点。     

用紫外吸收光谱法测定粗蒽中菲、蒽的含量

用紫外吸收光谱法同时测定粗蒽中菲、蒽的含量,结果表明,采用环已烷作溶剂,吸收波长分别为293nm和357nm,在0.004～0.04g/L范围内,菲、蒽符合线性关系。该方法操作简单、测定迅速、结果准确。     

Separation of Anthracene from Crude Anthracene Using Gas Antisolvent Recrystallization

Abstract

Pure anthracene is mostly used for conversion to anthraquinone, an intermediate for the synthesis of very powerful vat dyestuffs. A coal tar distillate, crude anthracene, which contains 30% anthracene, 25% phenanthrane, 15% carbazole, and other impurities, was used as the model mixture. In this study, 90% by weight purity anthracene was obtained using gas antisolvent (GAS) recrystallization. The GAS process induces the separation of solids by introducing an antisolvent, carbon dioxide (or the supercritical fluid), into acetone which was used as the liquid solvent. The dissolution of the compressed gas into the solute-laden solution selectively lowers the solubilities of solid solutes and salts them out. The results showed that high purity anthracene was obtained at a high feed concentration and high pressure conditions. The separation factor of anthracene versus phenanthrene is close to 30.07.     

Recovery of Anthracene from Coal Tar by Solvent Extraction

Abstract

A method of anthracene purification by extraction of impurities with a methanol-benzene solvent mixture is proposed. In the first stage the anthracene cake is dissolved in the solvent mixture at the boiling temperature of the system. Subsequently the precipitation of the great part of anthracene takes place by cooling the system to room temperature. The solid phase is removed by filtration while the liquid phase is arranged in the last stage by stripping. After this operation the solvent can be reused in the anthracene recovery process. In this paper the results obtained on the recovery of anthracene from anthracene cake are reported. The influence of solvent mixture composition, solvent mixture volume/anthracene cake weight ratio, and operation time are studied. According to the experimental results, 90% of the anthracene from the anthracene cake can be recovered. The anthracene purity attained is close to 90%.     

蒽、菲、咔唑的分离提纯方法

综述了蒽、菲、咔唑分离提纯的各种方法．如溶剂萃取法、精馏-溶剂法、乳化液膜法等，并讨论了它们各自的特点以及应用情况。     

溶剂结晶法制取精芴的研究

以工业芴为原料、甲苯为溶剂,研究了溶剂结晶法制取精芴的工艺过程和最佳操作条件,精芴的纯度可达９９％以上,收率达９０％。     

Liquid-phase oxidation of anthracene in acetic acid with an oxygen/Nitric acid system

Oxidation of anthracene in acetic acid by the oxygen/nitric acid system has been studied and an attempt has been made to ascertain a practical limit of the amount of solvent keeping the commercial prospects in view. The effects of other reaction parameters such as flow rate, amount of nitric acid and water, residence time, etc., have been investigated. While opting for a solvent/substrate ratio of 10, the optimum conversion of anthracene to anthraquinone free from nitro-compounds has been found to be 91% with purity of 98.7%, acceptable to dye-stuff industries.