本文關鍵詞：減壓間歇精餾回收廢液中甲苯的應用研究　出處：《蘇州科技學院》2015年碩士論文　論文類型：學位論文

  更多相關文章： 減壓間歇精餾 實驗室廢液 甲苯回收 ChemCAD模擬

【摘要】：石油、化工、機械、涂料、纖維、油脂、橡膠、醫藥和電子等行業中甲苯被大量地用作有機溶劑,并最終形成大量的甲苯廢液。甲苯易揮發、有刺激性和毒性,對人體健康和生態環境均能造成嚴重的危害,但同時也具有一定的經濟價值。目前,國內外高濃度甲苯廢液以焚燒法處理為主,但焚燒過程中產生的一氧化碳、氮氧化物、硫氧化物、二VA英和飛灰等有害物質引起了社會的普遍擔憂。因此,研究開發新型高濃度甲苯廢液處理工藝和處理裝置是環境、安全、資源和經濟等多方面的迫切需要。本論文首次采用了減壓間歇精餾工藝,通過自主設計的減壓間歇精餾裝置,從實驗室生產廢液中成功得到了分析純規格的甲苯,實現了實驗室生產廢液向再生有機溶劑的轉變。本論文研究對象為實驗室小規模生產共混添加劑過程中產生的廢液。經真空抽濾、飽和食鹽水洗滌、分液等簡單預處理后,采用色譜-質譜分析方法測試了廢液的組分和組成,得到了廢液主要組分為甲苯、乙醇和水,三者質量分數分別為89.8%,8.2%和1.0%；在對廢液組成特點分析和減壓間歇精餾原理充分理解的基礎上,確定了采用減壓間歇精餾技術回收廢液中高濃度的甲苯；自行設計安裝和測試了減壓間歇精餾實驗的實驗裝置,得到了填料精餾塔的理論板數N=11,填料精餾塔正常操作塔壓降為400 Pa；考察了操作壓力、精餾時間、回流比、廢液組成等參數對減壓間歇精餾過程的影響,發現：(1)隨著壓力的降低,甲苯純度逐漸增加,甲苯回收率總體呈下降的趨勢；(2)間歇精餾塔塔釜溫度隨時間變化平緩,塔頂溫度的變化和塔頂組成的變化存在時間上的相關性。本回收實驗通過觀察記錄塔頂溫度的變化間接判斷塔頂組成的變化；(3)隨著回流比的增大,甲苯純度和甲苯回收率均呈現出增大的趨勢；(4)本回收實驗操作條件：操作壓力為30.4 kPa,120 min為區分前餾分段和產品段時間點,前餾分段回流比為7,產品段回流比為5的條件下,典型廢液的回收產品中甲苯質量分數為99.7%,單程甲苯回收率為70.5%,二次精餾甲苯總回收率為92.2%；(5)隨著乙醇／水質量比的增加,甲苯回收率總體上呈現上升的趨勢。在精餾實際廢液前需要采取干燥等措施降低廢液中水的含量；(6)在模擬廢液中水質量分數保持在2%的前提下,甲苯／乙醇質量比低于1,減壓間歇精餾實驗分別無法進行,低于4時獲得低回收率甲苯,高于9時獲得高回收率甲苯。在精餾實際廢液前需要采取飽和實驗水洗滌等措施降低廢液中乙醇的含量；依據相關的國家標準,減壓間歇精餾實驗所得產品經檢測為分析純甲苯試劑；采用了ChemCAD軟件對整個減壓間歇精餾過程進行了模擬,模擬結果與實驗數據吻合較好,為實驗規模的擴大化奠定了基礎；進行了減壓間歇精餾實驗的經濟效益分析,結果表明實驗經濟效益顯著。
[Abstract]:Toluene is widely used as an organic solvent in petroleum, chemical industry, machinery, coatings, fiber, oil, rubber, medicine and electronics industries, and finally a large amount of toluene waste liquid is formed. Toluene is volatile, irritant and toxic, and can cause serious harm to human health and ecological environment, but it also has a certain economic value. At present, high concentration toluene waste water is mainly incineration, but carbon monoxide, nitrogen oxides, sulfur oxides, two VA, fly ash and other harmful substances caused widespread concern in the society. Therefore, the research and development of new high concentration toluene waste liquid treatment process and treatment device is the urgent need of environment, safety, resources and economy and so on. For the first time, the vacuum batch distillation process has been used for the first time, and the pure toluene has been successfully obtained from the laboratory waste liquid by the self designed decompression batch distillation unit, and the transformation from laboratory waste liquid to regenerated organic solvent has been realized. The research object of this paper is the waste liquid produced in the process of small scale production of blending additives in the laboratory. The vacuum and saturated salt water, washing liquid after simple pretreatment, using gas chromatography-mass spectrometry analysis method of waste liquid component and the composition of the test, the waste is mainly composed of toluene, ethanol and water, the three mass fraction were 89.8%, 8.2% and 1%; understanding on waste composition analysis of the characteristics and principle of vacuum batch distillation, a high concentration of toluene were determined by vacuum batch distillation technology in recycling of waste liquid; self-designed experimental device installation and vacuum batch distillation experiment test, the number of theoretical plates N=11 packed distillation column, packed distillation column normal operation of the tower drop to 400 Pa; the effects of operation pressure, distillation time, reflux ratio, liquid composition and other parameters on the vacuum batch distillation process, found that: (1) as the pressure decreases, the purity of toluene increased gradually, the recovery rate of total body is under toluene The trend of the reduction is: (2) the temperature of the batch distillation tower is slow with time, and the change of the top temperature of the tower and the change of the composition of the top of the tower has the correlation of time. The recovery experiment by observing the changes of the temperature at the top of the record to determine changes in composition of the indirect overhead; (3) when the reflux ratio increased, and the purity of toluene toluene recovery rate showed increasing trend; (4) the recovery experiment of operating pressure of 30.4 kPa and 120 min to distinguish the fraction and product segments the point in time, before the fraction reflux ratio is 7, the product section of reflux ratio is 5, the mass fraction of toluene recovery in 99.7% typical waste products, one-way toluene recovery rate was 70.5%, two times the total recovery of toluene distillation rate was 92.2%; (5) with the increase of ethanol / water mass ratio, toluene recovery the rate of overall upward trend. In the actual wastewater before distillation need to take measures to reduce the water content of dry waste; (6) in the simulated waste water content maintained at 2% under the premise of toluene / ethanol ratio less than 1, vacuum batch distillation experiments were not less than 4, low recovery rate of toluene was higher than 9, to obtain high recovery rate toluene. In the actual wastewater need to be taken before the distillation experiment of water washing and other measures to reduce the saturated alcohol content in liquor; according to relevant national standards, vacuum batch distillation experiment for product testing by the analysis of pure toluene reagent; by vacuum batch distillation process on the whole have undergone ChemCAD simulation software, the simulation results agree well with the experimental data, which the foundation for the expansion of the scale; analyzes the vacuum batch distillation experiment results show that the economic benefits, economic benefits.
【學位授予單位】：蘇州科技學院
【學位級別】：碩士
【學位授予年份】：2015
【分類號】：X703

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