發(fā)布時(shí)間：2018-07-02 10:44

  本文選題：折流式旋轉(zhuǎn)床 + RZB��； 參考：《浙江工業(yè)大學(xué)》2017年碩士論文

【摘要】：作為最受關(guān)注的過(guò)程強(qiáng)化技術(shù)之一,超重力技術(shù)已經(jīng)成為化學(xué)工程學(xué)科研究的前沿和熱點(diǎn)方向之一。與普通的旋轉(zhuǎn)填料床相比,折流式旋轉(zhuǎn)床具有諸多優(yōu)點(diǎn)。其中,獨(dú)特的動(dòng)靜轉(zhuǎn)子結(jié)構(gòu)有利于改善液體進(jìn)口處的“端效應(yīng)區(qū)”,使得折流式旋轉(zhuǎn)床具有更優(yōu)異的微觀混合性能和液-液傳質(zhì)強(qiáng)化性能,使其在“受傳質(zhì)和分子混合限制”的化學(xué)反應(yīng)制備化學(xué)品的應(yīng)用領(lǐng)域具有巨大潛力。本文從折流式旋轉(zhuǎn)床的微觀混合和液-液傳質(zhì)強(qiáng)化兩個(gè)特性研究出發(fā),開(kāi)展實(shí)驗(yàn)研究,并且第一次將其應(yīng)用于羥醛縮合制備化學(xué)品的過(guò)程強(qiáng)化中。主要工作和研究結(jié)果如下:1、采用碘化物-碘酸鹽平行競(jìng)爭(zhēng)反應(yīng)體系,對(duì)折流式旋轉(zhuǎn)床(RZB)的微觀混合性能進(jìn)行研究,分別考察了超重力因子β、液體入口總流量uin、H+濃度、反應(yīng)物體積流量比VA/VB對(duì)RZB反應(yīng)器離集指數(shù)Xs的影響;并與三通混合裝置、旋轉(zhuǎn)填料床(RPB)對(duì)離集指數(shù)Xs的影響進(jìn)行對(duì)比。實(shí)驗(yàn)結(jié)果表明:在本實(shí)驗(yàn)范圍內(nèi),折流式旋轉(zhuǎn)床實(shí)驗(yàn)所得到的離集指數(shù)XS在0.01~0.05之間,顯示出了較三通混合裝置優(yōu)越的微觀混合性能;另外,由實(shí)驗(yàn)結(jié)果可知RZB反應(yīng)器的微觀混合性能略優(yōu)于RPB反應(yīng)器。2、以大豆油-異丙醇-水為實(shí)驗(yàn)體系,研究了折流式旋轉(zhuǎn)床(RZB)強(qiáng)化物理萃取傳質(zhì)的性能�？疾炝顺亓σ蜃应�、液體入口總流量uin和水油兩相體積流量比?等主要操作參數(shù)對(duì)萃取級(jí)效率η影響;并在相同操作條件下,進(jìn)一步探究了折流式旋轉(zhuǎn)床(RZB)萃取傳質(zhì)性能與微觀混合性能之間的定量關(guān)系。實(shí)驗(yàn)結(jié)果表明:對(duì)比于傳統(tǒng)攪拌萃取裝置,折流式旋轉(zhuǎn)床萃取性能更加優(yōu)異。它能夠使液滴粒徑瞬間達(dá)到微米級(jí)水平,具有優(yōu)異的微觀混合特性,能有效的強(qiáng)化物理萃取傳質(zhì)過(guò)程。在折流式旋轉(zhuǎn)床(RZB)反應(yīng)器內(nèi),萃取傳質(zhì)性能與微觀混合性能密切相關(guān)。在實(shí)驗(yàn)操作條件下,超重力因子β逐漸增加到263時(shí),離集指數(shù)Xs減小為0.020,對(duì)應(yīng)的萃取級(jí)效率η逐漸增加到94.2%,萃取級(jí)效率η隨離集指數(shù)Xs的減小而逐漸增加,說(shuō)明隨RZB著反應(yīng)器微觀混合效果的提高,萃取傳質(zhì)效果也逐漸提高,但兩者并不呈線性關(guān)系。3、采用異戊醛和丙酮進(jìn)行羥醛縮合反應(yīng)制備甲基庚烯酮的生產(chǎn)工藝,將折流式旋轉(zhuǎn)床反應(yīng)器用于強(qiáng)化反應(yīng)過(guò)程�？疾炝顺亓σ蜃应�、反應(yīng)溫度T、堿濃度?和異戊醛與丙酮物質(zhì)的量比?等操作條件對(duì)異戊醛轉(zhuǎn)化率X、甲基庚烯酮選擇性S和收率Y的影響,并對(duì)目的產(chǎn)物甲基庚烯酮(MHK)進(jìn)行了核磁共振氫譜(1H-NMR)、核磁共振碳譜(13 CNMR)和GC-MS的表征,以確定其分子結(jié)構(gòu)。實(shí)驗(yàn)結(jié)果表明:RZB反應(yīng)器可以有效強(qiáng)化異戊醛和丙酮羥醛縮合反應(yīng),當(dāng)堿性催化劑用量為物料的40%,循環(huán)流量為150L/h時(shí),控制適當(dāng)溫度和異戊醛丙酮物質(zhì)的量比,堿性催化劑濃度為4.2%,超重力因子為263時(shí),異戊醛轉(zhuǎn)化率為88.6%,甲基庚烯酮的選擇性和收率分別達(dá)到93.3%和82.7%。相同操作條件下,與機(jī)械攪拌裝置強(qiáng)化效果對(duì)比,RZB反應(yīng)器強(qiáng)化下的異戊醛轉(zhuǎn)化率提高了20%,選擇性提高了30%。
[Abstract]:As one of the most concerned process strengthening techniques, supergravity technology has become one of the frontiers and hot topics in the research of chemical engineering. Compared with the ordinary rotating packed bed, the baffled rotary bed has many advantages. The rotary bed has a more excellent micro mixing performance and liquid liquid mass transfer enhancement. It has great potential in the application field of chemical reaction preparation of "mass transfer and molecular mixing restriction". In this paper, two characteristics of micro mixing and liquid to liquid mass transfer enhancement in a baffled rotating bed are studied, and the experimental study is carried out. The main work and research results are as follows: 1, the micro mixing properties of the RZB are studied by the iodide iodate parallel competitive reaction system, and the supergravity factor beta, the total flow rate UIN, H+ concentration and the reaction object are investigated. The effect of VA/VB on the off set index Xs of the RZB reactor and the effect of the three pass mixing device and the rotating packed bed (RPB) on the off set index Xs are compared. The experimental results show that in the experimental range, the off set index XS obtained by the baffle rotary bed experiment is between 0.01~0.05, which shows the superior microstructure of the three pass mixing device. In addition, the experimental results show that the micro mixing performance of the RZB reactor is slightly better than that of the RPB reactor.2. With the soybean oil isopropanol water as the experimental system, the properties of the mass transfer in the physical extraction of the baffled rotating bed (RZB) are studied. The supergravity factor beta, the total flow rate UIN of the liquid inlet and the volume flow ratio of the water and oil two phase are investigated. The effect of the operating parameters on the extraction efficiency was investigated. The quantitative relationship between the mass transfer performance and the micro mixing performance of the RZB was further investigated under the same operating conditions. The experimental results showed that the performance of the baffled rotary bed was better than that of the traditional stirred extraction device. At the micron level, with excellent micro mixing characteristics, it can effectively strengthen the mass transfer process of physical extraction. In a baffled rotary bed (RZB) reactor, the mass transfer performance is closely related to the micro mixing performance. Under the experimental operating conditions, the supergravity factor beta is gradually increased to 263, the off set index Xs is reduced to 0.020, the corresponding extraction grade The efficiency ETA gradually increased to 94.2%, the extraction efficiency was gradually increased with the decrease of the separation index Xs, indicating that the mass transfer effect of the extraction was gradually increased with the increase of the micro mixing effect of the RZB reactor, but they did not have a linear relationship.3. The production process of methyl heptanone by isovalaraldehyde and acetone was used to prepare methyl heptanone. The flow type rotating bed reactor was used to strengthen the reaction process. The effects of the supergravity factor beta, the reaction temperature T, the concentration of the alkali and the ratio of the isovalaraldehyde to acetone were investigated, such as the conversion of isovaleral X, the selective S of methyl hepenone and the yield Y, and the nuclear magnetic resonance hydrogen spectrum (1H-NMR) was carried out for the target product of methyl heptanone (MHK). The molecular structure of the magnetic resonance carbon spectrum (13 CNMR) and GC-MS is determined. The experimental results show that the RZB reactor can effectively strengthen the condensation reaction of Isoamyl aldehyde and acetone hydroxyaldehyde. When the amount of the basic catalyst is 40% of the material and the circulation flow is 150L/h, the ratio of the appropriate temperature to the isovalaraldehyde acetone is controlled, and the concentration of the alkaline catalyst is 4.2%, When the supergravity factor was 263, the conversion rate of isovaleral was 88.6%. The selectivity and yield of methyl hepenone were 93.3% and 82.7%., respectively, under the same operating conditions, compared with the mechanical agitator, the conversion of isovaleral under the RZB reactor was increased by 20%, and 30%. was selectively raised.
【學(xué)位授予單位】：浙江工業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2017
【分類號(hào)】：TQ051.1

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本文編號(hào)：2089866