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     

煤焦油中蒽、菲、咔唑的精制及利用

蒽、菲、咔唑是煤焦油中的重要组分 ,主要富集在煤焦油初馏时蒽油馏分中。本文综述了从煤焦油蒽油馏分中分离精制蒽、菲、咔唑的原理、方法及技术发展状况 ;并对蒽、菲、咔唑及其衍生物的应用作了系统介绍     

蒽油的深加工

兖矿集团公司和济宁煤化公司采用闪蒸、结晶、蒸馏、氧化等技术生产氧化蒽醌,联产咔唑,副产脱晶蒽油和萘油。该工艺技术先进,自动化程度高,三废排放少,符合环保要求,所得产品质量好,收率高。其中蒽的收率大于70％,蒽醌纯度达99％以上,咔唑收率大于60％,纯度达95％-98％。产品在市场上都具有较强的竞争力。     

提高粗蒽质量的生产经验

我厂焦油蒸馏装置采用两塔式切取混合馏分工艺，从蒽塔切取Ｉ蒽油，经结晶和真空过滤后，滤饼在立式离心机中离心分离得产品粗蒽。由于我厂的过滤机和离心机设备陈旧，近几年来粗蒽的质量难以达到国家标准，含蒽量仅在３３％左右。为此，我们在分析影响粗蒽质量和收率各因素的基础上，对生产工艺进行了适当的调整，取得了很好的效果。１影响粗蒽质量和收率的因素（１）Ｉ蒽油对粗蒽质量的影响。控制Ｉ蒽油的主要质量指标是３００℃和３６０℃前馏出量。３６０℃前馏出量直接影响Ｉ蒽油的粘度，同时也代表了Ｉ蒽油的含蒽量。对于３６０℃前馏…     

结晶温度对粗蒽产量与质量的影响

几年来,我公司生产的粗蒽中的油含量和水分指标均能达到国家标准,只是含蒽量的波动较大,低时不足２５％,高时可达４４％,严重影响粗蒽深加工产品的质量和生产成本。在粗蒽生产中,我们一直采用一段结晶法,提高粗蒽含蒽量的关键是提高Ｉ蒽油的质量和控制适宜的结晶温度。为此,我们在实验室条件下,进行了不同结晶温度对粗蒽含蒽量影响的对比试验。１试验情况１．１Ｉ蒽油的组成表１列出了用毛细管气相色谱法分析的Ｉ蒽油组成。１．２试验步骤将４００g左右的Ｉ蒽油倒人６００ｍＬ烧杯中,在超级恒温水浴中升温至Ｉ蒽油全部熔化,此时…     

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。     

从Ⅰ蒽油中连续提取粗蒽的工艺研究

文章针对传统的粗蒽制取工艺中制取粗蒽质量不稳定,结晶机设备多,效率低下,生产周期长等问题,提出了从Ⅰ蒽油中连续提取粗蒽的新工艺路线,简化了生产设备和工艺路线,通过严格控制Ⅰ蒽油原料质量、降温结晶条件和离心操作等真正实现了粗蒽的连续化生产,缩短了生产周期,提高了粗蒽的产率和蒽含量,同时降低了粗蒽中的油含量和水含量,保证了产品达到一级品95%以上。     

蒽醌生产方法及其催化剂研究进展

论述了国内外制备蒽醌的方法及其催化剂,并简单介绍了国内蒽醌生产方法的应用。通过比较,认为蒽气相氧化法具有原料充足、环境友好、操作简便等优点,符合目前环境对蒽醌生产行业的要求,是较为理想的蒽醌生产方法。催化剂是以Al2O3为载体的V2O5为主体的复合催化剂。国内近年大量上马一批蒽气相氧化项目,但多引进国外技术,研究和开发国产催化剂和设备已成为蒽醌生产行业的迫切任务。     

凝华器喷嘴对蒽醌堆密度的影响

蒽醌生产工艺主要由氧化反应和凝华包装2部分组成。蒽醌生产工艺见图1,液体精蒽通过过滤器后,用过热蒸汽把液体精蒽汽化,然后在催化剂的作用下与氧反应将精蒽氧化为蒽醌,在凝华器中将蒽醌凝华．最后过滤得到产品蒽醌。     

从I蒽油中提取工业蒽的生产经验

从I蒽油中提取工业蒽的生产经验表明，影响工业蒽产质量的主要因素是原料含蒽量和结晶冷却温度，还可利用结晶装置生产60％工业芴和96％工业苊。     

MECHANISM AND FACTORS AFFECTED ON THE PAIRED ELECTRO-OXIDATION OF ANTHRACENE TO ANTHRAQUINONE

Anodic oxidation and paired electrochemical oxidation of anthracene to anthraquinone in an undivided cell were carried out. The factors affected on the paired electrochemical oxidation of anthracene to anthraquinone were explored. The results revealed that oxygen flow rate, concentration of sulfuric acid and agitation rate were the major factors, and concentration of mediator, temperature, and current density were the minor factors. The reaction mechanism of paired electro-oxidation of anthracene was proposed. Oxygen was cathodically reduced to generate H₂O₂ which chemically reacted with V⁴⁺ to produce both OH free radical and V⁵⁺. Which then oxidized anthracene to anthraquinone. The results also showed that the total current efficiency of anthraquinone was higher than 100%.     

Oxidation of anthracene to anthraquinone in liquid-phase with an air/oxygen/nitric acid system

Oxidation of anthracene to anthraquinone by air/oxygen in the presence of small amounts of nitric acid was studied in the liquid phase. The effects of various process variables (e.g. temperature, flow rate, amount of nitric acid and solvent substrate ratio) were investigated. An attempt was made to minimise the amount of nitric acid. The optimum conversions of anthracene into anthraquinone free from nitro compounds, using air and oxygen was found to be 81.7 and 96.2% respectively with corresponding purities of 98.5% and 99.6%.     

Oxidation kinetics of anthracene with nitrogen dioxide in acetic acid

Kinetics of liquid-phase oxidation of anthracene to anthraquinone with nitrogen dioxide in acetic acid as solvent has been studied. The reaction takes place through the anthrone as intermediate compound. The first and second reactions are first order with respect to anthracene and anthrone concentration, respectively. The values of the rate constants in the temperature range 60–95°C have been reported. According to the reaction system developed, an industrial process for the manufacture of anthraquinone of high purity has been proposed.     

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。     

微波辐射条件下H2O2氧化蒽合成蒽醌的研究

研究了微波辐射条件下H2O2氧化蒽的反应，考察了时间、H2O2用量、催化剂和溶剂对葸醌收率的影响。结果表明．CH3COOH浓度对蒽醌的收率影响很大，以适量的(CH3COO)3Fe作为催化剂可以增加蒽醌的收率和缩短反应时间。     

Paired electro-oxidation Part II: Production of anthraquinone in an undivided cell

Oxidation of anthracene to anthraquinone by the anodically generated oxidant V⁵⁺ and both V⁵⁺ and · OH free radicals generated cathodically was carried out simultaneously in an undivided cell. Both the yield and selectivity of anthraquinone by paired electro-oxidation are higher than that by anodic oxidation only. The maximum total current efficiency for anthraquinone production in the paired electro-oxidation was 151%. A process for anthraquinone production using an undivided cell electrolyser is proposed.     

高效化学发光材料9，10－二苯乙炔基蒽的合成

以苯乙炔和蒽醌为原料，采用非氨基锂路线，合成了高效化学发光材料９，１０－二苯乙炔基蒽以质谱和荧光光谱鉴定了结构。     

高效化学发光材料9，10－二苯乙炔基蒽的合成

以苯乙炔和蒽醌为原料，采用非氨基锂路线，合成了高效化学发光材料９，１０－二苯乙炔基蒽以质谱和荧光光谱鉴定了结构。     

Precursors to aromatic units in coal

Previous oxidation experiments with bituminous coal have produced fluorenone, benzophenone and anthraquinone carboxylic acids. Precursors to these acids were speculated to be fluorene, diphenylmethane, anthracene and 9,10-dihydroanthracene derivatives. Oxidation experiments suggested that polymethylene bridges between aromatic units may also act as precursors to these acids.