本文選題：草銨膦　切入點(diǎn)：廢溶劑　出處：《南京師范大學(xué)》2015年碩士論文　論文類型：學(xué)位論文

【摘要】：草銨膦是重要的除草劑,其生產(chǎn)量近年來增長迅速,草銨膦生產(chǎn)過程中需要用到多種溶劑,相關(guān)企業(yè)面臨著大量的廢溶劑回收再利用問題。本文系統(tǒng)地總結(jié)了當(dāng)前國內(nèi)外草銨膦的生產(chǎn)現(xiàn)狀以及生產(chǎn)過程中產(chǎn)生混合廢溶劑的種類和處理辦法。由于生產(chǎn)流程的差異,草銨膦生產(chǎn)過程中主要產(chǎn)生兩種混合廢溶劑,經(jīng)企業(yè)初步處理后,其組成分別為：廢溶劑A(四氫呋喃35.0 wt%、甲基亞磷酸二乙酯15.0 wt%、亞磷酸三乙酯2.0 wt%及三甲苯48.0 wt%)以及廢溶劑B(四氫呋喃38.0 wt%、二溴乙烷14.0 wt%、亞磷酸三乙酯4.0 wt%、三甲苯44.0 wt%)。其中主要成分四氫呋喃、甲基亞磷酸二乙酯、二溴乙烷、亞磷酸三乙酯、三甲苯都是重要化工原料,必須采用合適的工藝路線回收這些物料,使其能夠循環(huán)利用,同時(shí)降低企業(yè)的環(huán)保壓力。針對廢溶劑A,設(shè)計(jì)了三種工藝流程用以回收其中的四氫呋喃、甲基亞磷酸二乙酯、亞磷酸三乙酯、三甲苯等有用組分。這三種流程分別為常壓三塔串聯(lián)連續(xù)精餾、單塔側(cè)線出料精餾后接單塔連續(xù)精餾和單塔雙側(cè)線出料精餾,通過Aspen Plus化工流程模擬軟件模擬計(jì)算,以產(chǎn)品的純度、收率、能耗及設(shè)備造價(jià)為指標(biāo),考察分析確定單塔側(cè)線出料精餾后接單塔連續(xù)精餾為最佳的工藝方案,并進(jìn)一步通過單因素實(shí)驗(yàn)結(jié)合正交實(shí)驗(yàn)設(shè)計(jì)的方法考察了塔板數(shù)、進(jìn)料位置、回流比以及側(cè)線出料位置等工藝參數(shù)對回收結(jié)果的影響。在模擬計(jì)算基礎(chǔ)上,設(shè)計(jì)了單塔側(cè)線出料精餾實(shí)驗(yàn)裝置并進(jìn)行了實(shí)驗(yàn)研究,實(shí)驗(yàn)結(jié)果表明,在優(yōu)化的工藝條件下,所回收的四氫呋喃純度達(dá)到99.7%、收率為99.1%,甲基亞磷酸二乙酯純度達(dá)到98.6%、收率為98.0%,亞磷酸三乙酯純度達(dá)到95.1%、收率為94.2%,三甲苯的純度達(dá)到98.1%、收率為97.5%1所回收產(chǎn)品的純度均達(dá)到企業(yè)循環(huán)利用的標(biāo)準(zhǔn)。針對廢溶劑B,同樣設(shè)計(jì)了三種工藝流程用以回收其中的四氫呋喃、二溴乙烷、亞磷酸三乙酯、三甲苯等有用組分。這三種流程分別為常壓三塔串聯(lián)連續(xù)精餾、單塔側(cè)線出料精餾后接連續(xù)萃取精餾和單塔雙側(cè)線出料精餾,通過AspenPlus化工流程模擬軟件模擬計(jì)算,以產(chǎn)品的純度、收率、能耗及設(shè)備造價(jià)為指標(biāo),考察分析確定單塔側(cè)線出料精餾后接連續(xù)萃取精餾為最佳的工藝方案,并進(jìn)一步通過單因素實(shí)驗(yàn)結(jié)合正交實(shí)驗(yàn)設(shè)計(jì)的方法考察了塔板數(shù)、原料進(jìn)料位置、萃取劑進(jìn)料位置、回流比、側(cè)線出料位置以及溶劑比等工藝參數(shù)對回收結(jié)果的影響。在模擬計(jì)算基礎(chǔ)上,設(shè)計(jì)了單塔側(cè)線出料精餾實(shí)驗(yàn)裝置、萃取精餾實(shí)驗(yàn)裝置并進(jìn)行了實(shí)驗(yàn)研究,實(shí)驗(yàn)結(jié)果表明,在優(yōu)化的工藝條件下,所回收的四氫呋喃純度為99.0%、收率為98.6%,二溴乙烷純度為96.5%、收率為89.9%,亞磷酸三乙酯純度為99.0%、收率為93.2%,三甲苯的純度為99.0%、收率為98.5%；所回收產(chǎn)品的純度均達(dá)到企業(yè)循環(huán)利用的標(biāo)準(zhǔn)。本文所做工作為草銨磷生產(chǎn)中廢溶劑的回收循環(huán)利用提供了新的解決方案。
[Abstract]:Phosphine oxalate is an important herbicide, and its production has been increasing rapidly in recent years. The related enterprises are faced with a large number of waste solvent recovery and reuse problems. This paper systematically summarizes the current production situation of ammonium phosphine at home and abroad, and the types and treatment methods of mixed waste solvents in the production process. Two kinds of mixed waste solvents are mainly produced in the production process of ammonium phosphine. After preliminary treatment by enterprises, The composition of the waste solvent A (tetrahydrofuran 35.0 wtand methyl diethyl phosphite 15.0 wtt, triethyl phosphite 2.0 wt% and trimethylbenzene 48.0 wtt respectively) and the waste solvent B (tetrahydrofuran 38.0 wtt, dibromoethane 14.0 wtth, triethyl phosphite 4.0 wt, trimethylbenzene). 44.0 wts. the main component of tetrahydrofuran is tetrahydrofuran, the main component of which is tetrahydrofuran. Diethyl methyl phosphite, dibromoethane, triethyl phosphite and trimethylbenzene are all important chemical raw materials. At the same time, the environmental pressure of the enterprise was reduced. For the waste solvent A, three processes were designed to recover the tetrahydrofuran, methyl diethyl phosphite and triethyl phosphite. The three processes are series continuous distillation under atmospheric pressure, continuous distillation with single column side line and single column with double side line distillation. The simulation calculation is carried out by Aspen Plus chemical process simulation software. Taking the purity, yield, energy consumption and equipment cost of the product as the index, the best process scheme was determined by investigating and analyzing the single column side line discharge rectification followed by single column continuous distillation. The effects of the process parameters, such as plate number, feed position, reflux ratio and side line discharge position, on the recovery results were investigated by single factor experiment and orthogonal design. The experimental equipment of single column side line discharge distillation is designed and studied. The experimental results show that, under the optimized technological conditions, The purity of the recovered tetrahydrofuran is 99.7, the yield is 99.1, the purity of diethyl methyl phosphite is 98.6, the yield is 98.0, the purity of triethyl phosphite is 95.1 percent, the yield is 94.2 percent, the purity of trimethylbenzene is 98.1 and the purity of the recovered product is 97.51. For waste solvent B, three processes were also designed to recover tetrahydrofuran. The three useful components, such as dibromoethane, triethyl phosphite and trimethylbenzene, are serially rectified in series with three columns under atmospheric pressure, followed by continuous extraction distillation in a single side line and a double side line extraction distillation in a single column. Through the simulation calculation of AspenPlus chemical process simulation software, taking the purity, yield, energy consumption and equipment cost of the product as the index, the optimum technological scheme was determined by investigating and analyzing the single column side line discharge rectification followed by continuous extractive distillation. Furthermore, the number of trays, the feed position of raw materials, the feed position of extractant and the ratio of reflux were investigated by single factor experiment and orthogonal design. On the basis of simulation calculation, a single column side line extraction distillation experimental device and an experimental device for extractive distillation are designed and studied. The experimental results show that the recovery results are affected by the side line discharge position and solvent ratio. Under the optimized technological conditions, The purity of the recovered tetrahydrofuran is 99.0, the yield is 98.6um, the purity of dibromoethane is 96.55.The yield is 89.9. the purity of triethyl phosphite is 99.0, the purity of triethyl phosphite is 99.0, the purity of trimethylbenzene is 99.0, and the purity of trimethylbenzene is 98.5.The purity of the recovered products reaches the enterprise recycling profit. The work in this paper provides a new solution for recycling waste solvent in ammonium oxalate production.
【學(xué)位授予單位】：南京師范大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2015
【分類號】：X786

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