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对焦化纯苯进行脱硫精制的研究

Study on Desulphurization from Benzene Product from Coking Production

【作者】 范明霞

【导师】 童仕唐;

【作者基本信息】 武汉科技大学 , 化学工艺, 2004, 硕士

【摘要】 本文通过分析比较各种方法之后,提出了采用吸附法脱除焦化纯苯中CS2、采用反应—精馏法脱除噻吩的工艺方法。吸附法具有能耗低,精制深度高,操作方便,不产生二次废物等优点;而反应—精馏法与常用的磺化法相比,耗酸量少,操作容易,精制深度高。 分光光度法测定苯中CS2和噻吩是有效的,该法操作简便、快速、测量精度高。所建立的标准曲线相关系数达0.99以上。 本课题采用比表面积较大、空隙率较高的粒状活性炭进行吸附试验。低温有利于吸附进行,在静态吸附试验中,对CS2浓度为0.001g/100mL的苯—CS2溶液,在22℃时,活性炭对CS2的吸附率可达74%以上,吸附后苯中CS2的质量含量小于3×10-6g/g。该吸附实验的Freundlich吸附等温式为q=0.047c0.3853,吸附热为597.9J/mol,属典型的物理吸附范围。在动态吸附实验中,在26℃、进料流率为2.12×10-4m3/m2s、床层高度为25cm时,饱和吸附量为0.07536mg/g吸附剂。活性炭对CS2的吸附动力学行为可用Elovich方程进行描述,进料流速为2.12×10-4m3/m2s时传质系数最大。吸附后的活性炭可以通过热N2吹扫再生,再生温度400℃,再生时间1h,经过三个周期的吸附—再生,活性炭的动态饱和吸附量仍可达最初的90%以上。 在酸洗试验中,对100mL浓度为0.030g/100mL的苯—噻吩溶液,共用48mL浓硫酸时,噻吩的脱除率为100%。在反应—精馏试验中,对400mL苯—噻吩溶液,采用玻璃多圈柱状填料,填料层高度为40cm,硫酸用量为80mL,采用人工控制回流情况,噻吩脱除率可达94%以上,苯中噻吩的质量含量小于2×10-5g/g。对处理相同质量的苯—噻吩溶液,实际上节省硫酸58.33%,在实际生产过程中,耗酸量的显著减少,大大降低了生产成本;而且,每次试验过程中的溶液量减少,所需塔釜热负荷降低,减少了能耗。硫酸用量的减少,产生的废酸量也相应减少,从而降低了废酸的处理量,降低了后续工作难度,也符合环保要求。

【Abstract】 Carbon disulfide in benzene product from coking production is removed by adsorption and thiophene is removed by .reaction and distillation in this thesis after evaluating various methods for removal of carbon disulfide and thiophene in benzene product from coking production. Low energy consumption, deep refinement and convenient operation as well as no waste characterize adsorption. Distillation is characterized by less quantity of sulphur acid and easy operation as well as high refine extent.It is effective for carbon disulfide and thiophene in benzene to be measured by spectrophotometer. Operation of the experiment is easy, high-speed, and the precision is high.Correlative coefficient of standard curve can reach above 0.99.Granule activiated carbon, which has larger surface area and lacuna radio has been adopt to adsorb carbon disulfide. The result shows that low temperature favors the adsorption process. In the static adsorption experiment, as to 0.001g/100mL carbon disulfide-benzene solution, at 22 C, adsorption ratio can reach above 74%. After adsorption, the residual amount of carbon disulfide occurring in benzene is less than 3 10-6g/g. Freundlich adsorption formula of the adsorption experiment is q = 0.047c0.3853 The adsorption neat is 597.9J/mol, which prove the adsorption belongs to typical physics adsorption. In the dynamic adsorption experiment, at 26 C, on the condition of flow ratio 2. 12 10-4m3/m2s, bed height 25cm, saturation adsorption quantity is 0.07536mg/g. Adsorption kinetics can be described by Elovich equation, and mass transfer coefficient is the largest at the flow ratio of 2. 12 X 10-4m3/m2s. Activiated carbon after adsorption can be regenerated by hot N2. At the temperature of 400 C and time of 1h, after three period of adsorption regeneration, dynamic saturation adsorption quantity of activiated carbon can reach above 90% of which of initial activiated carbon.In the reaction and distillation experiment, as to 400mL benzene product from coking production (containing thiophene 0.030g/100mL), at the conditions of height of glass column packing 40cm, 80mL sulphuric acid and reflux controlled by manual work, the removal ratio of thiophene can be up to 94%, and the quality content of thiophene in benzene product from coking production is less than 2 10-5g/g. As to the same quantity benzene product from coking production, 58.33% sulphuric acid has been saved. In the production, the quantity of sulphuric acid is reduced obviously, so the cost of production is reduced greatly. Moreover, heat burden in the bottom of tower and energy consumption is reduced too. In addition, along with the quantity of sulphuric acid is reduced, the quantity of waste acid is reduced correspondly, and the difficulty of disposed work and enviroment protection is shortened.

  • 【分类号】TQ522
  • 【被引频次】6
  • 【下载频次】254
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