螺旋盤管反應(yīng)器強化液-液混合及應(yīng)用研究
發(fā)布時間：2018-07-29 13:50
【摘要】：混合過程在化學(xué)工業(yè)中具有重要地位,涉及均相混合與非均相混合過程。反應(yīng)器的混合性能對產(chǎn)物分布、產(chǎn)品質(zhì)量等有重要影響,是化工過程強化研究中的重要課題。螺旋盤管反應(yīng)器(英文Helical Tube Reactor,簡稱HTR)作為一種典型的被動式混合設(shè)備,具有結(jié)構(gòu)緊湊、耐壓、軸向返混少、體系溫度易控制等優(yōu)點,已應(yīng)用于硝化反應(yīng)、氧化反應(yīng)、鹵化反應(yīng)、結(jié)晶、乳液聚合、生物柴油制備、萃取、納米材料制備等過程。上述應(yīng)用研究中涉及快速復(fù)雜反應(yīng)過程和液-液非均相混合過程。然而對上述兩類過程起到至關(guān)重要作用的HTR微觀混合和液-液分散性能的基礎(chǔ)研究卻相對薄弱。本論文首先針對快速復(fù)雜反應(yīng)過程,鑒于預(yù)混性能對反應(yīng)過程具有重要影響,設(shè)計了預(yù)混式HTR,通過CFD模擬及實驗研究的方法對預(yù)混組件進行類型優(yōu)選,并對預(yù)混式HTR微觀混合性能進行實驗研究,進一步通過預(yù)混組件結(jié)構(gòu)優(yōu)化實現(xiàn)了對HTR微觀混合性能的調(diào)變,初步探索了預(yù)混性能優(yōu)化與HTR微觀混合性能強化之間的定量關(guān)系。針對液-液非均相混合過程,鑒于分散相初始微元尺寸對分散特性有重要影響,設(shè)計了預(yù)分散式HTR,利用預(yù)分散組件調(diào)控分散相初始微元尺寸,采用乳化體系對預(yù)分散式HTR壓降及液-液分散性能展開研究。最后,將預(yù)分散式HTR應(yīng)用于連續(xù)濕法磷酸的萃取過程。主要研究結(jié)論如下:1、針對快速復(fù)雜反應(yīng)體系,設(shè)計了預(yù)混式HTR,由預(yù)混組件和螺旋盤管兩部分組成,其中預(yù)混組件用于改變HTR預(yù)混性能。根據(jù)管內(nèi)兩股液體接觸方式的不同,將預(yù)混組件分為同軸環(huán)管型(CCM)和錯流剪切型(CRM)。CFD模擬結(jié)果表明,CRM比CCM具備更好的預(yù)混性能,從而可以預(yù)測裝配CRM的HTR (CRM-HTR)的微觀混合性能優(yōu)于裝配CCM的HTR (CCM-HTR)的微觀混合性能。通過CFD模擬預(yù)測結(jié)果與微觀混合實驗結(jié)果的一致性討論優(yōu)選出CRM,并利用碘化物-碘酸鹽體系對CRM-HTR微觀混合性能進行實驗研究。2、針對CRM-HTR,本課題提出兩種結(jié)構(gòu)優(yōu)化方案,即切向進料和螺旋擾流的方式優(yōu)化CRM-HTR的預(yù)混性能。CFD模擬結(jié)果表明兩種優(yōu)化方案均可以改變預(yù)混組件內(nèi)的流體流動狀態(tài)、強化湍流動能和改善預(yù)混性能。進一步,利用碘化物-碘酸鹽體系研究了不同優(yōu)化結(jié)構(gòu)CRM-HTR微觀混合性能,研究結(jié)果表明通過預(yù)混組件預(yù)混性能優(yōu)化來調(diào)變CRM-HTR的微觀混合性能是可行的�；贑FD模擬結(jié)果及微觀混合實驗結(jié)果,定義了無量綱參數(shù)RPM,用于表示預(yù)混性能優(yōu)化與CRM-HTR微觀混合性能強化的定量關(guān)系,不同結(jié)構(gòu)的CRM-HTR的RPM值在0.3-0.5之間。利用團聚模型計算得到不同預(yù)混結(jié)構(gòu)CRM-HTR的微觀混合時間。3、針對液-液非均相混合體系,設(shè)計了預(yù)分散式HTR,由預(yù)分散組件和螺旋盤管兩部分組成,其中預(yù)分散組件用于調(diào)控分散相初始微元尺寸。利用環(huán)己烷-Tween 80-水體系考察了預(yù)分散組件中泡沫鎳單元個數(shù)、孔徑及體積流量比、螺旋盤管曲率對壓降和液-液分散性能的影響。液-液分散性能研究結(jié)果表明,當(dāng)泡沫鎳單元個數(shù)為2-6、體積流量比為6-15、總體積流量為960-1730 ml/min時,得到的乳液粒徑為30-65 μm,且粒徑分布均勻。根據(jù)實驗結(jié)果得到了如下的粒徑無因次關(guān)聯(lián)式:d_(32)/D_m = 0.80We_c~(-0.32)De~(-0.24)n_e~(-0.15)ψ~(0.68)計算值與實驗值偏差均在±20%以內(nèi),吻合較好。4、將預(yù)分散式HTR應(yīng)用于濕法磷酸萃取過程,研究了相比、磷酸質(zhì)量分?jǐn)?shù)、螺旋盤管曲率、匝數(shù)對磷酸萃取效率的影響。當(dāng)相比為1-3、磷酸質(zhì)量分?jǐn)?shù)30%-70%、螺旋盤管曲率為7.5-15、匝數(shù)為25-50、螺距為10 mm時,預(yù)分散式HTR的萃取效率為33%-59%。與其他萃取設(shè)備相比,預(yù)分散式HTR萃取效率與轉(zhuǎn)盤塔萃取能力相當(dāng)。
[Abstract]:The mixing process plays an important role in the chemical industry, involving a homogeneous and heterogeneous mixing process. The mixing performance of the reactor has an important influence on the product distribution and product quality. It is an important subject in the study of chemical process strengthening. The spiral coil reactor (Helical Tube Reactor, referred to as HTR) is a typical passive formula. The hybrid equipment has the advantages of compact structure, pressure resistance, less axial backmixing and easy control of the system temperature. It has been applied to the process of nitrification, oxidation, halogenation, crystallization, emulsion polymerization, biodiesel preparation, extraction, and nanomaterial preparation. The above application involves the rapid complex reaction process and liquid liquid heterogeneous mixing process. The basic research on the HTR micro mixing and liquid liquid dispersion performance which plays an important role in the above two kinds of processes is relatively weak. Firstly, in view of the rapid and complex reaction process, the premixed HTR is designed in view of the important influence of premixing performance on the reaction process. The premixed component is carried out by the method of CFD simulation and experimental research. Type optimization was selected and the micro mixing performance of premixed HTR was experimentally studied. The microstructure of HTR was adjusted by the optimization of premixed component structure. The quantitative relationship between the optimization of pre mixing performance and the micro mixing performance of HTR was preliminarily explored. Size has an important influence on dispersion characteristics. Pre dispersed HTR is designed and pre dispersed component is used to regulate the initial microelement size of dispersed phase. The emulsification system is used to study the pre dispersed HTR pressure drop and liquid liquid dispersion. Finally, the pre dispersed HTR is applied to the extraction process of continuous wet process phosphoric acid. The main conclusions are as follows: 1 The premixed HTR is designed, which consists of two parts: premixed component and spiral coil, in which the premixed component is used to change the premixing performance of HTR. According to the different contact modes of two strands of liquid in the tube, the premixed module is divided into coaxial loop tube (CCM) and CRM.CFD simulation results, and CRM is better premixed than CCM. The micro mixing performance of HTR (CRM-HTR) in assembly CRM is better than that of HTR (CCM-HTR) with assembly CCM. CRM is optimized by the agreement between the prediction results of CFD simulation and the results of micro mixing experiment, and the micro mixing performance of CRM-HTR is experimentally studied by iodide iodate system for.2, for C. RM-HTR, in this subject, two structural optimization schemes are proposed, that is, the optimization of the premixing performance of CRM-HTR by tangential feed and spiral spoiler. The results of.CFD simulation show that the two optimization schemes can all change the flow state in the premixed component, strengthen the turbulent kinetic energy and improve the premixing performance. The micro mixing performance of the optimized structure CRM-HTR shows that it is feasible to adjust the micro mixing performance of CRM-HTR by premixing performance optimization. Based on the results of CFD simulation and micro mixing experiment, the dimensionless parameter RPM is defined, which is used to express the quantitative correlation between pre mixing performance optimization and the micro mixing performance enhancement of CRM-HTR. The RPM value of different structures of CRM-HTR is between 0.3-0.5. The micro mixing time of different premixed structure CRM-HTR is calculated by the agglomeration model, and the pre dispersed HTR is designed for the liquid liquid heterogeneous mixture system. The pre dispersed component and the spiral coil are composed of two parts. The pre dispersed component in the mixture is used to control the initial microelement ruler of the dispersed phase. By using cyclohexane -Tween 80- water system, the number of nickel foam units, pore size and volume flow ratio, and the effect of the curvature of the spiral coil on the pressure drop and liquid liquid dispersion are investigated. The results of liquid liquid dispersion study show that when the number of nickel foam units is 2-6, the volume flow ratio is 6-15, the total volume flow rate is 960-1730 ml/min The particle size of the emulsion is 30-65 m, and the particle size distribution is uniform. According to the experimental results, the following correlations are obtained: d_ (32) /D_m = 0.80We_c~ (-0.32) De~ (-0.24) n_e~ (-0.15) n_e~ (-0.15) and experimental values are both within + 20%, and are in good agreement with.4, and the pre dispersion HTR is applied to the process of wet process phosphoric acid extraction. Compared with the effect of phosphoric acid mass fraction, spiral coil curvature and turn number on the efficiency of phosphoric acid extraction, the extraction efficiency of pre dispersed HTR is 33%-59%. compared with other extraction equipment when compared to 1-3, 7.5-15 of phosphoric acid mass fraction 30%-70%, spiral coil curvature of 25-50, and 10 mm of pitch, pre dispersed HTR extraction efficiency and turntable extraction The ability is equal.
【學(xué)位授予單位】：北京化工大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2017
【分類號】：TQ027.1
本文編號：2152876
[Abstract]:The mixing process plays an important role in the chemical industry, involving a homogeneous and heterogeneous mixing process. The mixing performance of the reactor has an important influence on the product distribution and product quality. It is an important subject in the study of chemical process strengthening. The spiral coil reactor (Helical Tube Reactor, referred to as HTR) is a typical passive formula. The hybrid equipment has the advantages of compact structure, pressure resistance, less axial backmixing and easy control of the system temperature. It has been applied to the process of nitrification, oxidation, halogenation, crystallization, emulsion polymerization, biodiesel preparation, extraction, and nanomaterial preparation. The above application involves the rapid complex reaction process and liquid liquid heterogeneous mixing process. The basic research on the HTR micro mixing and liquid liquid dispersion performance which plays an important role in the above two kinds of processes is relatively weak. Firstly, in view of the rapid and complex reaction process, the premixed HTR is designed in view of the important influence of premixing performance on the reaction process. The premixed component is carried out by the method of CFD simulation and experimental research. Type optimization was selected and the micro mixing performance of premixed HTR was experimentally studied. The microstructure of HTR was adjusted by the optimization of premixed component structure. The quantitative relationship between the optimization of pre mixing performance and the micro mixing performance of HTR was preliminarily explored. Size has an important influence on dispersion characteristics. Pre dispersed HTR is designed and pre dispersed component is used to regulate the initial microelement size of dispersed phase. The emulsification system is used to study the pre dispersed HTR pressure drop and liquid liquid dispersion. Finally, the pre dispersed HTR is applied to the extraction process of continuous wet process phosphoric acid. The main conclusions are as follows: 1 The premixed HTR is designed, which consists of two parts: premixed component and spiral coil, in which the premixed component is used to change the premixing performance of HTR. According to the different contact modes of two strands of liquid in the tube, the premixed module is divided into coaxial loop tube (CCM) and CRM.CFD simulation results, and CRM is better premixed than CCM. The micro mixing performance of HTR (CRM-HTR) in assembly CRM is better than that of HTR (CCM-HTR) with assembly CCM. CRM is optimized by the agreement between the prediction results of CFD simulation and the results of micro mixing experiment, and the micro mixing performance of CRM-HTR is experimentally studied by iodide iodate system for.2, for C. RM-HTR, in this subject, two structural optimization schemes are proposed, that is, the optimization of the premixing performance of CRM-HTR by tangential feed and spiral spoiler. The results of.CFD simulation show that the two optimization schemes can all change the flow state in the premixed component, strengthen the turbulent kinetic energy and improve the premixing performance. The micro mixing performance of the optimized structure CRM-HTR shows that it is feasible to adjust the micro mixing performance of CRM-HTR by premixing performance optimization. Based on the results of CFD simulation and micro mixing experiment, the dimensionless parameter RPM is defined, which is used to express the quantitative correlation between pre mixing performance optimization and the micro mixing performance enhancement of CRM-HTR. The RPM value of different structures of CRM-HTR is between 0.3-0.5. The micro mixing time of different premixed structure CRM-HTR is calculated by the agglomeration model, and the pre dispersed HTR is designed for the liquid liquid heterogeneous mixture system. The pre dispersed component and the spiral coil are composed of two parts. The pre dispersed component in the mixture is used to control the initial microelement ruler of the dispersed phase. By using cyclohexane -Tween 80- water system, the number of nickel foam units, pore size and volume flow ratio, and the effect of the curvature of the spiral coil on the pressure drop and liquid liquid dispersion are investigated. The results of liquid liquid dispersion study show that when the number of nickel foam units is 2-6, the volume flow ratio is 6-15, the total volume flow rate is 960-1730 ml/min The particle size of the emulsion is 30-65 m, and the particle size distribution is uniform. According to the experimental results, the following correlations are obtained: d_ (32) /D_m = 0.80We_c~ (-0.32) De~ (-0.24) n_e~ (-0.15) n_e~ (-0.15) and experimental values are both within + 20%, and are in good agreement with.4, and the pre dispersion HTR is applied to the process of wet process phosphoric acid extraction. Compared with the effect of phosphoric acid mass fraction, spiral coil curvature and turn number on the efficiency of phosphoric acid extraction, the extraction efficiency of pre dispersed HTR is 33%-59%. compared with other extraction equipment when compared to 1-3, 7.5-15 of phosphoric acid mass fraction 30%-70%, spiral coil curvature of 25-50, and 10 mm of pitch, pre dispersed HTR extraction efficiency and turntable extraction The ability is equal.
【學(xué)位授予單位】：北京化工大學(xué)
【學(xué)位級別】：博士
【學(xué)位授予年份】：2017
【分類號】：TQ027.1
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