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從阻聚劑生產(chǎn)廢液中回收N,N-二甲基乙酰胺研究

發(fā)布時間:2018-01-21 00:57

  本文關(guān)鍵詞: N N-二甲基乙酰胺 精餾 熱力學(xué) 提純 ProⅡ 出處:《華東理工大學(xué)》2017年碩士論文 論文類型:學(xué)位論文


【摘要】:N,N-二甲基乙酰胺(簡稱DMAC)作為一種具有高沸點、強極性的質(zhì)子化有機溶劑,對于多種有機物都有極強的溶劑性能,同時因其具有穩(wěn)定性好、揮發(fā)性低、不易水解和腐蝕性低等特點,廣泛應(yīng)用于樹脂、橡膠、石油化工及其他有機合成等領(lǐng)域。隨著國內(nèi)腈綸、氨綸行業(yè)的需求增長和化工行業(yè)的發(fā)展,DMAC將會擁有更為廣闊的發(fā)展和應(yīng)用前景。論文探討了從阻聚劑生產(chǎn)廢液中回收N,N-二甲基乙酰胺的方法。針對廢液中的酸性組分,首先研究了中和法處理廢液的方法,使用堿液與廢液中的酸性組分進行反應(yīng),考察了直接中和后分離的可行性。結(jié)果表明,直接中和分離法操作復(fù)雜,分離困難,不具備可行性。之后,研究了采用反應(yīng)法處理廢液,在廢液中通入二甲胺,使二甲胺與廢液中的酸性組分進行反應(yīng),一方面使廢液中的酸性組分濃度降低,另一方面使廢液中的DMAC濃度提高。使用Benson基團貢獻法估算DMAC等組分的熱力學(xué)參數(shù),并對二甲胺與乙酸和乙酸酐反應(yīng)進行熱力學(xué)分析,研究了反應(yīng)的可行性和最優(yōu)進行條件。在熱力學(xué)研究的基礎(chǔ)上,通過二甲胺與廢液中的乙酸和乙酸酐的反應(yīng),考察了催化劑種類、催化劑用量、二甲胺與酸性組分摩爾配比、反應(yīng)溫度和反應(yīng)時間等因素對提高廢液中DMAC濃度的影響。在最優(yōu)條件組下進行反應(yīng),可以有效提升廢液中DMAC含量,廢液中DMAC的含量由原廢液的57.07%提高到83.77%,酸性組分含量由26.44%降低到1.54%,大大降低了后續(xù)精餾分離的難度。論文還使用ProII模擬軟件對反應(yīng)終液的精餾分離流程進行模擬分析。在一定分離條件下通過簡捷法獲取塔參數(shù),并使用嚴格法檢驗相關(guān)塔參數(shù)。分析理論塔板數(shù)、進料板位置、最小回流比、再沸器熱負荷和冷凝器熱負荷等參數(shù)對分離結(jié)果的影響,并對塔參數(shù)進行優(yōu)化。最終分離得到合格的DMAC產(chǎn)品,為工廠的可持續(xù)處理流程奠定了實驗室基礎(chǔ)。該工藝流程可以同時處理廢液中的乙酸和乙酸酐等雙重酸性組分,且流程簡單、反應(yīng)成本低,同時使用軟件模擬可以獲得高純度的DMAC產(chǎn)品。通過分析和模擬,獲取了工藝流程的優(yōu)化參數(shù),降低了廢液對環(huán)境的污染,節(jié)省了資源,并為企業(yè)創(chuàng)造了一定的經(jīng)濟效益。
[Abstract]:As a kind of proton organic solvent with high boiling point and strong polarity, N- N- dimethyl acetamide (DMAC) has very strong solvent properties for many kinds of organic matter, at the same time, it has good stability. It is widely used in many fields such as resin, rubber, petrochemical and other organic synthesis. With the increasing demand of domestic acrylic and spandex industry and the development of chemical industry. DMAC will have a wider prospect of development and application. This paper discusses the method of recovering N- N- dimethyl acetamide from the waste liquor of polymerization inhibitor production, aiming at the acid component in the waste liquid. Firstly, the neutralization method was studied, and the feasibility of direct neutralization separation was investigated by reaction of alkali solution with acid component. The results showed that the direct neutralization separation method was complicated. The separation is difficult and not feasible. After that, the reaction method is used to treat the waste liquid, and the dimethylamine is added into the waste liquid to make the dimethylamine react with the acid component in the waste liquid. On the one hand, the concentration of acid component in waste liquid is decreased, on the other hand, the concentration of DMAC in waste liquid is increased. The thermodynamic parameters of DMAC and other components are estimated by Benson group contribution method. The thermodynamic analysis of the reaction of dimethylamine with acetic acid and acetic anhydride was carried out, and the feasibility and optimum conditions of the reaction were studied. On the basis of thermodynamic study, the reaction of dimethylamine with acetic acid and acetic anhydride in waste liquid was carried out. The effects of catalyst type, amount of catalyst, molar ratio of dimethylamine to acid component, reaction temperature and reaction time on the concentration of DMAC in waste liquor were investigated. The content of DMAC in waste liquid increased from 57.07% to 83.77, and the content of acid component decreased from 26.44% to 1.54%. The difficulty of subsequent distillation separation is greatly reduced. ProII simulation software is also used to simulate and analyze the distillation separation process of the final reaction liquid. Under certain separation conditions, the column parameters are obtained by the simplified method. The influence of theoretical tray number, feed plate position, minimum reflux ratio, reboiler heat load and condenser thermal load on the separation results was analyzed. The parameters of the tower were optimized. Finally, the qualified DMAC product was obtained. This process can simultaneously treat the acid components such as acetic acid and acetic anhydride in the waste liquor, and the process is simple, and the reaction cost is low. At the same time, high purity DMAC products can be obtained by software simulation. Through analysis and simulation, the optimization parameters of process flow are obtained, which can reduce the pollution of waste liquid to the environment and save resources. And for the enterprise to create certain economic benefits.
【學(xué)位授予單位】:華東理工大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2017
【分類號】:X78;TQ413.26

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