从粗蒽中分离精制蒽、菲、咔唑

<正>前言 粗蒽是从煤焦油分级蒸馏时所得的300—360℃的蒽油馏分经过结晶过滤后分出来的固体产物,是一种炼焦副产品。 通常粗蒽中含蒽量约为10—35%,咔唑则为蒽的一半左右,其余为菲、芴、（艹屈）、甲基蒽等,我们进行试验的鞍钢,石景山原料粗蒽的主要成分列于表1。     

蒽油馏分深加工工艺现状及研究进展

介绍了蒽油馏分深加工的2种工艺、蒽油精制分离提取精蒽、菲、咔唑工艺的现状及研究进展,阐述了蒽油馏分加氢生产轻质燃料油工艺研究进展、工艺原理、工艺流程等。对山西焦化集团有限公司未来建设蒽油深加工项目提出了建议。     

煤焦油中蒽、菲、咔唑分离技术进展

综述了煤焦油中蒽、菲、咔唑的分离技术进展,系统总结了传统工艺一些新的改进,并重点介绍了一些新的分离方法在煤焦油中蒽、菲、咔唑的分离上的应用.     

煤焦油中蒽、菲、咔唑的精制技术

主要介绍了煤焦油中蒽、菲和咔唑的精制方法,系统地总结了溶剂洗涤法、精馏-溶剂法、结晶-精馏法、乳化液膜法、区域熔融法、溶剂萃取-恒沸蒸馏-升华法和化学分离法、新型分离法等精制蒽、菲及咔唑的工艺原理,对各种方法所具有的优势及不足之处进行了评述。     

咔唑化学的进展及其在颜料工业中的应用

咔唑是一种含氮杂环化合物,是煤焦油中的重要组份。它与蒽和菲共同存在于高温焦油馏份中,含量与蒽相当。过去,在回收蒽的时候把咔唑等其它组份都烧掉了,如果能将咔唑也回收利用,不仅提供了一种重要的有机原料,同时也将使蒽的成本降低。目前,煤化学的研究方兴未艾,我国已经考虑同时回收蒽和咔唑,因此咔唑的利用将成为一个重要的研究课题。     

Ⅰ蒽油分离中的相平衡研究

从Ⅰ蒽油中提取蒽菲咔唑具有十分重要的应用价值。通过固液平衡的研究，利用ＵＮＩＱＵＡＣ，ＵＮＩＦＡＣ模型关联实验数据，可以为工程开发提供一定的依据。     

I蒽油分离中的相平衡研究

从Ｉ蒽油中提取蒽菲咔唑具有十分重要的应用价值。通过固液平衡的研究，利用ＵＮＩＱＵＡＣ，ＵＮＩＦＡＣ模型关联实验数据，可以为工程开发提供一定的依据。     

用毛细管柱气相色谱法分析煤焦油高馏分产物中菲,蒽及咔唑的含量

采用气相色谱法，在长２５ｍ、内径０．２ｍｍ的ＯＶ－１０１交联弹性石英毛细管柱和２５０℃柱温下，对煤焦油高馏分产物中菲、蒽及咔唑含量进行了定量分析。     

提高酚提取率的措施

1 影响酚提取率的因素 我厂的煤焦油蒸馏为两塔工艺,在蒽、洗塔中分别切取二蒽油、一蒽油、重质洗油、酚萘洗三混馏分和轻油馏分.三混馏分和工业萘初馏塔顶采出的酚油一起在洗涤器中进行两次间歇洗涤, 所得的中性酚盐用直接蒸汽蒸吹出中性油,精制酚盐用焦炉烟道废气中的CO2分解得粗酚.几年来,我厂纯酚提取率一直低于60%.为此, 通过对粗酚生产各环节的考察和分析,认为影响酚提取率的因素有以下几方面.     

蒸馏和溶剂结合法制取精蒽

一、前言精蒽是重要的化工原料之一,有广泛的用途。目前,我国主要用于制取染料工业急需的中间体——蒽醌,蒽仅存在于煤焦油中,含量0.6～1.4％。将煤焦油蒸馏,可得到含蒽4～7％的蒽油馏份,其成份很复杂,(大致见下表)。蒽油用结晶和离心分离法处理,可制得约     

Analysis by GC-MS of Polycyclic Aromatic Hydrocarbons in a Cream Containing Coal Tar

Qualitative and quantitative PAHs composition of a cream containing coal tar (5%), used in cutaneous diseases treatment, was studied. Eleven PAHs were analysed in pure coal tar and in the cream by GC-MS, after ultrasonic extraction by pyridine. Ten PAHs were found in pure coal tar: naphthalene, biphenyl, acenaphthylene, fluorene, phenanthrene, anthracene, carbazole, fluoranthene, pyrene and benzo[a]pyrene. No traces of 2,3-benzofluorene were detected. Seven PAHs were identified in the cream: naphthalene, biphenyl, acenaphthylene, fluorene, phenanthrene, fluoranthene and pyrene. 2,3-benzofluorene was also absent in the cream. Anthracene, carbazole and benzo[a]pyrene (one of the most toxic) were present in coal tar and not detected in the cream.

The seven PAHs found in the cream and in coal tar were quantified. Hydrocarbons concentrations were between 0.107 ± 0.0038 mg.g^?1 (for biphenyl) and 0.734 ± 0.0438 mg.g^?1 (for phenanthrene) in the cream and between 4.31 ± 0.23 mg.g^?1 (for biphenyl) and 21.9 ± 0.57 mg.g^?1 (for fluorene) in coal tar.     

咔唑生产技术浅谈

对蒸馏-溶剂法、溶剂-蒸馏法和双溶剂法生产咔唑的3种实用工艺进行了评述。结果表明,双溶剂法工艺的咔唑得率高、劳动强度小、投资少,可以充分利用煤焦油中的咔唑资源。该工艺适用于50万t/a以下的煤焦油加工厂,经济效益好。     

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.     

Separation of high-purity phenanthrene and anthracene from the anthracene fraction of coal tar

The separation of high-purity phenanthrene and anthracene from mixtures obtained in the rectification of the first anthracene fraction from coal tar is considered. The method employed is selective deposition from an aqueous solution of the anthracene-phenanthrene mixture with organic solvent.     

超临界乙醇萃取咔唑的实验研究

以乙醇为超临界萃取基剂,采用恒容升温法研究了超临界乙醇对煤焦油蒽油组分咔唑的萃取效果,探讨了温度和压力对萃取效果的影响。结果表明,在萃取温度为270-280℃、萃取压力为12MPa左右时,咔唑的溶解度较大、萃取率较高,萃取效果明显;温度和压力对超临界乙醇萃取咔唑影响显著;超临界乙醇萃取单组分咔唑效果较好。     

从煤焦油分离提纯蒽和咔唑工艺改进探讨

溶剂结晶-精馏法是目前从煤焦油中分离提纯蒽和咔唑的比较先进成熟的已工业化工艺,其杂质的脱除主要在溶剂结晶部分,操作步骤多,但杂质分离效果还不是很理想,最终影响产品纯度。通过实验研究,发现结晶物中高杂质母液的滞留是该工艺杂质分离效果难以提高的关键因素。提出了溶剂结晶结合抽滤-精馏法新工艺,给结晶箱组合气液分离器,实现结晶同步抽滤功能,降低结晶物的母液滞留量,可提高分离效果,减少溶剂循环量,提高产品纯度和回收率,降低装置能耗,增加产能,有较好的经济性。     

粗蒽加工工艺的研究现状和进展

依据精细化工的发展和炼焦工业的现状，精蒽、精咔唑的供应紧张状况仍将持续。借鉴国外焦油加工工艺，开发符合国情的粗蒽分离新工艺是当条之急。本文主要介绍了粗蒽加工的生产工艺和发展趋势，提出了利用分子工程的研究方法进行了焦油加工基础研究的问题，对减少粗蒽加工成本、合理利用煤焦油资源有一定的启示。     

Separation of Phenantrene from Anthracene Oil using Supercritical Carbon Dioxide

Supercritical fluid extraction (SFE) is a relatively new separation technique that has received much attention in recent years. This process is an alternative to distillation or liquid extraction. Its main advantage over the conventional ones is that the dissolved extract may be completely separated from the supercritical fluid simply by decreasing the pressure. In recent years considerable effort has been devoted to the measurement of equilibrium solubility data for solids in supercritical fluids. A coal tar distillate, anthracene oil, which contains 34.46 mass‐% phenanthrene, 33.8 mass‐% anthracene, 13.89 mass‐% carbazole and other impurities, was used as the model mixture. In this study, an experimental flow‐type apparatus has been designed to determine solubility data for the main components of anthracene oil (phenanthrene, anthracene, and carbazole) as a binary, quaternary, and multi component mixture in supercritical carbon dioxide. The equilibrium solubilities were measured at 45 °C isotherm, over a pressure range of 98–200 bar. The separation of phenanthrene from anthracene oil has been also studied by supercritical carbon dioxide at different temperatures and pressure in an extracting vessel containing 27 sieve trays.     

Effects of model coal tar components on adhesion strength of polyurethane coating on steel plate

In order to study the effects of coal tar components on the adhesion strength of a heavy duty anticorrosive coating formed with tar-urethane resin on a steel plate, polyurethane coatings that were compounded with 15 kinds of polycyclic aromatic compounds as model coal tar components were prepared. In the model coal tar components, naphthalene, quinoline, 2-naphthol, and phenanthrene showed good compatibility with polyurethane. To test their heavy duty anticorrosive properties, tensile adhesion strength of the cured coatings prepared with the compatible model coal tar components was measured, and the change in tensile adhesion strength as a function of time during salt-water spray treatment was measured. We found that the systems compounded with naphthalene, 2-naphthol, and phenanthrene showed good properties in an ordinary state for adhesion strength. However, only the system with 2-naphthol was found to have good properties in the change of tensile adhesion strength as a function of time during salt-water spray treatment. The curing time of the system with 2-naphthol was slower than that of the others, i.e., we found an inverse proportion between curing speed and adhesion durability. We also measured the dynamic viscoelasticity of cured coatings. We found that a tan δ curve of the system with 2-naphthol shifted towards a low temperature side and the tan δ at the temperature at which adhesion strength was measured was larger than that of the others. We hypothesized that the reason for the tan δ shift was a result of the decrease in crosslinking density because 2-naphthol partially capped the isocyanate group. Considering these results, we hypothesized that one of the reasons why the adhesion properties of the system with 2-naphthol had improved was due to the increase of tan δ. Presented at the 32nd Adhesion Symposium of the Adhesion Society of Japan, Tokyo Japan, June 27–28, 1994.     

中低温煤焦油加氢转化路径

以中低温煤焦油360℃的馏分油为原料,Ni-Mo/γ-Al2O3为催化剂,在小型固定床单管加氢反应器上进行加氢实验。在压力13 MPa、空速0.4 h-1、氢油体积比1 700∶1和反应温度370℃工艺条件下进行催化加氢反应,通过对原料油和加氢产物的GC-MS的检测结果分析,确定了酚类、萘类、联苯类和菲类化合物的加氢转化路径,得到煤焦油馏分油中主要化合物的加氢反应网络。