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1、乙醇-水精餾塔實(shí)驗(yàn)、實(shí)驗(yàn)?zāi)康?1. 了解板式精餾塔的結(jié)構(gòu)和操作。2. 學(xué)習(xí)精餾塔性能參數(shù)的測量方法,并掌握其影響因素。二、實(shí)驗(yàn)內(nèi)容:1. 測定精餾塔在全回流條件下,穩(wěn)定操作后的全塔理論塔板數(shù)和總板效率。2. 測定精餾塔在部分回流條件下,穩(wěn)定操作后的全塔理論塔板數(shù)和總板效率三、實(shí)驗(yàn)原理:對于二元物系,如已知其汽液平衡數(shù)據(jù),則根據(jù)精餾塔的原料液組成,進(jìn)料熱狀況,操作回流比及塔頂餾出液組成,塔底釜液組成可以求出該塔的理論板數(shù)Nr.按照式1可以得到總板效率Et,其中NP為實(shí)際塔板數(shù)(1)Et 二100 %N P部分回流時,進(jìn)料熱狀況參數(shù)的計(jì)算式為Cpm(tBP -七卩)rm(2)rm式中:t F 進(jìn)料
2、溫度,C 。t BP 進(jìn)料的泡點(diǎn)溫度,C 。Cpm 進(jìn)料液體在平均溫度(th t p) /2下的比熱,kJ/ (kmol? C)r m 進(jìn)料液體在其組成和泡點(diǎn)溫度下的汽化潛熱,kJ/kmolCpm - C p 1 M 1 X1C p2M 2X2 kJ/ (kmol? C)(3)(4)r = r1 M 1 x1r2M 2x2 kJ/kmol式中:CP1,CP2 分別為純組份1和組份2在平均溫度下的比熱,kJ/ (kg? C) r 1,r 2 分別為純組份1和組份2在泡點(diǎn)溫度下的汽化潛熱,kJ/kg。M, M分別為純組份1和組份2的摩爾質(zhì)量,kJ/kmol。X1,X2分別為純組份1和組份2在進(jìn)料中
3、的摩爾分率。四、實(shí)驗(yàn)裝置基本情況:1 實(shí)驗(yàn)設(shè)備流程圖(如圖1所示):圖1精餾實(shí)驗(yàn)裝置流程圖1-儲料罐;2-進(jìn)料泵;3-放料閥;4-加熱器;5-直接進(jìn)料閥;6-間接進(jìn)料閥;7-進(jìn)料流量計(jì);8-高位槽;9-玻璃觀察段;10-精餾塔;11-塔釜取樣閥;12- 釜液放空閥;13-塔頂冷凝器;14-回流比流量計(jì);15-塔頂取樣閥;16-塔頂液 回收罐;17-放空閥;18-冷卻水流量計(jì);19-塔釜儲料罐;20-塔釜冷凝器;21- 第8塊板進(jìn)料閥;22-第9塊板進(jìn)料閥;23-第10塊板進(jìn)料閥;24-液位計(jì);25- 料液循環(huán)閥;26-釜?dú)堃撼隽祥y;27-進(jìn)料入口閥;28-指針壓力表2.實(shí)驗(yàn)設(shè)備主要技術(shù)參數(shù):精
4、餾塔實(shí)驗(yàn)裝置結(jié)構(gòu)參數(shù)見表1: 表1精餾塔結(jié)構(gòu)參數(shù)名稱直徑(mm高度(mm板間距(mr)板數(shù)(塊)板型、孔徑(mr)i材質(zhì)塔體 76X 3.510010011篩板2.0不銹鋼塔釜 220X 2400不銹鋼塔頂冷凝器 89X 3.5600不銹鋼塔釜 冷凝器 57X 3.5300不銹鋼表2乙醇一水t-x-y 關(guān)系(以乙醇摩爾分率表示,x-液相,y-氣相)摩爾分?jǐn)?shù)x摩爾分?jǐn)?shù)yt/C0.0000.0001000.0500.31090.60.1000.43086.40.2000.52083.20.3000.57581.70.4000.61480.70.5000.65779.90.6000.69879.10
5、.7000.75578.70.8000.82078.40.8940.89478.150.9500.94278.31.0001.00078.3乙醇沸點(diǎn):78.3 C ; 水沸點(diǎn):100.0 C .3 實(shí)驗(yàn)儀器及試劑:(1) 實(shí)驗(yàn)物系:乙醇一水(本試驗(yàn)也可用乙醇 -正丙醇物系);(2) 實(shí)驗(yàn)物系純度要求:化學(xué)純或分析純;(3) 實(shí)驗(yàn)物系平衡關(guān)系見表2;(4) 實(shí)驗(yàn)物系濃度要求:15-25 % (乙醇質(zhì)量百分?jǐn)?shù)),濃度分析使用酒精計(jì), 酒精計(jì)為體積分?jǐn)?shù), 通過查酒精體積分?jǐn)?shù)、質(zhì)量分?jǐn)?shù)、密度對照表可得酒 精的質(zhì)量分?jǐn)?shù)W通過質(zhì)量分率求出摩爾分率(X A),公式如下:乙醇分子量M A =46;水分子量M
6、b= 18嚴(yán))X( Ma)aWa 口-網(wǎng) M/Mb3 實(shí)驗(yàn)設(shè)備面板圖(如圖2所示):1-塔頂溫度( A第勿夬板溫度代) 辦執(zhí)塊板溫度(匸:1- 第&塊板溫度2)2- 第9塊板溫度(匸3- 第山塊板溫即匸塔釜溫度(口回流庚溫底匸)迸糾溫席(-C)加哋壓(V)總電源進(jìn)料泵加熱O OO 進(jìn)料 加熟圖2精餾設(shè)備儀表面板圖五、實(shí)驗(yàn)方法及步驟:1. 實(shí)驗(yàn)前檢查準(zhǔn)備工作:配制一定濃度(質(zhì)量濃度20 %左右)的乙醇一水混合液(總?cè)萘?5升左右),倒 入儲料罐中。打開進(jìn)料入口閥 27,其余閥門關(guān)閉,啟動進(jìn)料泵 2,打開料液循 環(huán)閥25,使料液混合均勻,混合均勻后將料液循環(huán)閥 25打至半開,將直接進(jìn)料 閥全開,放
7、空閥12全開,進(jìn)行進(jìn)料,一般在塔釜總高 2/3處。然后關(guān)閉進(jìn)料閥門和進(jìn)料泵2. 實(shí)驗(yàn)操作:(1)全回流操作: 打開塔頂冷凝器進(jìn)水閥門 , 保證冷卻水足量( 160L/h 即可)。 記錄室溫。接通總電源開關(guān)( 220V)。 調(diào)節(jié)加熱電壓約為150伏,待塔板上建立液層后再適當(dāng)加大電壓至 170V,使 塔內(nèi)維持正常操作。 當(dāng)各塊塔板上鼓泡均勻后 , 保持加熱釜電壓不變 , 在全回流情況下穩(wěn)定20 分鐘左右。期間要隨時觀察塔內(nèi)傳質(zhì)情況直至操作穩(wěn)定。然后分別在塔頂、 塔釜取樣口用100ml量筒同時取樣,通過酒精計(jì)分析樣品濃度。(2)部分回流操作: 打開間接進(jìn)料閥門和進(jìn)料泵,調(diào)節(jié)轉(zhuǎn)子流量計(jì) ,以3.0-4
8、.0( L/h)的流量向塔內(nèi)加料, 打開進(jìn)料加熱開關(guān), 調(diào)節(jié)到合適的進(jìn)料溫度, 用回流比流量計(jì)調(diào)節(jié)回 流比為R = 3,餾出液收集在塔頂液回收罐中。 塔釜產(chǎn)品經(jīng)冷卻后由溢流管流出 , 收集在容器內(nèi)。 待操作穩(wěn)定后 , 觀察塔板上傳質(zhì)狀況 , 記下加熱電壓、 塔頂溫度, 塔釜壓力等有 關(guān)數(shù)據(jù), 整個操作中維持進(jìn)料流量計(jì)讀數(shù)不變 , 分別在塔頂、塔釜和進(jìn)料三處取樣 用酒精計(jì)其濃度并記錄下進(jìn)塔原料液的溫度。(3)實(shí)驗(yàn)結(jié)束 取好實(shí)驗(yàn)數(shù)據(jù)并檢查無誤后可停止實(shí)驗(yàn), 此時關(guān)閉進(jìn)料閥門和加熱開關(guān), 關(guān)閉 回流比流量計(jì)閥門。 停止加熱后 10 分鐘再關(guān)閉冷卻水 , 一切復(fù)原。 根據(jù)物系的 t-x-y 關(guān)系, 確
9、定部分回流條件下進(jìn)料的泡點(diǎn)溫度, 并進(jìn)行數(shù)據(jù)處 理。六、實(shí)驗(yàn)注意事項(xiàng):1. 由于實(shí)驗(yàn)所用物系屬易燃物品,所以實(shí)驗(yàn)中要特別注意安全 ,操作過程中避免 灑落以免發(fā)生危險。2. 本實(shí)驗(yàn)設(shè)備加熱功率由儀表自動調(diào)節(jié), 注意控制加熱升溫要緩慢, 以免發(fā)生爆 沸(過冷沸騰 )使釜液從塔頂沖出。 若出現(xiàn)此現(xiàn)象應(yīng)立即斷電, 重新操作。 升溫和 正常操作過程中釜的電功率不能過大。3. 開車時要先接通冷卻水再向塔釜供熱,停車時操作反之。4. 檢測濃度使用酒精計(jì),使用方法見說明書。5. 為便于對全回流和部分回流的實(shí)驗(yàn)結(jié)果 (塔頂產(chǎn)品質(zhì)量)進(jìn)行比較,應(yīng)盡量使 兩組實(shí)驗(yàn)的加熱電壓及所用料液濃度相同或相近。連續(xù)開出實(shí)驗(yàn)時,
10、應(yīng)將前一次 實(shí)驗(yàn)時留存在塔釜、塔頂、塔底產(chǎn)品接受器內(nèi)的料液倒回原料液儲罐中循環(huán)使用。七、實(shí)驗(yàn)數(shù)據(jù)記錄表4精餾實(shí)驗(yàn)原始數(shù)據(jù)實(shí)際塔板數(shù):11實(shí)驗(yàn)物系:乙醇-水全回流:R = g,塔釜壓力=kPa部分回流:R =3進(jìn)料量:4 l/h進(jìn)料溫度:60 C塔頂組成塔釜組成塔頂組成塔釜組成進(jìn)料組成體積分?jǐn)?shù)附錄酒精體積分?jǐn)?shù)、質(zhì)量分?jǐn)?shù)、密度對照表體積分?jǐn)?shù)質(zhì)量分?jǐn)?shù)體積分?jǐn)?shù)質(zhì)量分?jǐn)?shù)體積分?jǐn)?shù)質(zhì)量分?jǐn)?shù)0033.427.521766.859.01810.10.079133.527.607866.959.12230.20.158233.627.69436759.22660.30.237333.727.780767.159.
11、3310.40.316333.827.86767.259.43540.50.395633.927.953267.359.53980.60.47483428.039867.459.64440.70.55434.128.126467.559.74890.80.633334.228.21367.659.85420.90.712634.328.299667.759.958910.791834.428.386367.860.06361.10.871234.528.472967.960.16841.20.950534.628.566860.27331.31.029934.728.646768.160.37
12、871.41.109234.828.733568.260.48391.51.138634.928.820268.360.58961.61.26813528.907168.460.69461.71.347535.128.993968.560.80051.81.42735.229.081168.660.90641.91.506535.329.16868.761.011621.58635.429.255268.861.11762.11.665535.529.342168.961.2232.21.745135.629.42916961.32912.31.824735.729.516469.161.43
13、532.41.904335.829.603469.261.54152.51.983935.929.690869.361.64712.62.06363629.777869.461.75352.72.143336.129.865369.561.85992.82.22336.229.952769.661.96642.92.302736.330.039869.762.072932.382536.430.127369.862.17883.12.462236.530.214969.962.28553.22.54236.630.30247062.39223.32.621836.730.3970.162.49
14、93.42.701636.830.477370.262.60583.52.781536.930.564970.362.71273.62.86143730.652570.462.81963.72.941337.130.740270.562.92673.83.021237.230.827970.663.0333.93.101237.330.91670.763.140243.181137.431.003870.863.24744.13.261137.531.091670.963.35464.23.341137.631.17947163.46194.33.421137.731.267371.163.5
15、6934.43.501237.831.355571.263.67684.53.581337.931.443471.363.78434.63.66143831.531371.463.89184.73.741538.131.619371.564.00024.83.821638.231.707671.664.10794.93.901838.331.795971.764.215653.981938.431.88471.864.32345.14.062138.531.972171.964.43135.24.142438.632.06057264.53295.34.222638.732.14972.164
16、.64725.44.302838.832.237172.264.7565.54.383138.932.325472.364.8645.64.46343932.413972.464.97315.74.543739.132.502572.565.08135.84.62439.232.591172.665.19035.94.704439.332.679472.765.299464.784839.432.768172.865.40796.14.865139.532.856872.965.51646.24.945639.632.94557365.62576.35.025939.733.034373.16
17、5.7356.45.106439.833.122773.265.84456.55.186839.933.211673.365.95326.65.26734033.300473.466.06286.75.347840.133.389373.566.17246.85.428340.233.478273.666.28216.95.508940.333.567573.766.391875.589440.433.656573.866.50097.15.670140.533.745573.966.61087.25.750640.633.83457466.72077.35.831240.733.923674
18、.166.83077.45.911840.834.013174.266.94087.55.992540.934.102274.367.0517.66.07324134.191474.467.16127.76.153941.134.280574.567.27147.86.234641.234.370174.667.38257.96.315341.334.459774.767.49386.396141.434.54974.867.60348.16.476841.534.638374.967.7148.26.557741.634.7287567.82468.36.638441.734.817875.
19、167.93528.46.719241.834.902775.268.0468.56.800141.934.996675.368.15768.66.8814235.086575.468.26848.76.961842.135.176375.568.37948.87.042742.235.266275.668.49048.97.123742.335.356275.768.601497.204642.435.446175.868.71349.17.285542.535.536175.968.82469.27.366542.635.62627668.93589.37.447542.735.71627
20、6.169.04729.47.528542.835.806376.269.15949.57.609542.935.896476.369.27089.67.69054335.986676.469.38329.77.771643.136.076876.569.49559.87.852643.236.167476.669.60739.97.933743.336.258176.769.719108.014843.436.348376.869.831610.18.10643.536.438776.969.944310.28.177143.636.52947770.056210.38.258343.736
21、.620277.170.169110.48.339543.836.710677.270.28210.58.420743.936.801177.370.394910.68.5024436.89277.470.507910.78.583244.136.982977.570.62110.88.664544.237.073877.670.734210.98.745844.337.164477.770.8475118.827144.437.255477.870.960811.18.908444.537.346577.971.074211.28.989744.637.43767871.187611.39.
22、071144.737.528778.171.301211.49.152444.837.619578.271.415611.59.233844.937.710778.371.529211.69.31524537.801978.471.64311.79.396645.137.893278.571.756811.89.478145.237.984578.671.871511.99.559545.338.075878.771.9855129.64145.438.167278.872.099512.19.722545.538.258678.972.214412.29.80445.638.3547972.
23、328612.39.885645.738.441979.172.442912.49.967145.838.533479.272.55812.510.048745.938.624979.372.672412.610.13034638.716579.472.787712.710.211846.138.808179.572.902212.810.293546.238.900279.673.017712.910.375146.338.991979.773.13321310.456846.439.08479.873.24813.110.538446.539.175879.973.362813.210.6
24、20146.639.26768073.478613.310.701846.739.359880.173.594413.410.783646.839.451780.273.710313.510.865346.939.54480.373.826313.610.9474739.63680.473.942313.711.028847.139.728480.574.058513.811.110647.239.820480.674.173813.911.192547.339.912880.774.29011411.274347.440.005380.874.406414.111.356147.540.09
25、7580.974.522914.211.437947.640.198174.639414.311.519847.740.282781.174.75614.411.601747.840.375381.274.873514.511.683647.940.467681.374.990214.611.76555042.425281.475.107914.711.847450.142.519281.575.224814.811.929450.242.612881.675.341814.912.011450.342.706881.775.45971512.093450.442.80181.875.5769
26、15.112.175450.542.894781.975.694915.212.257450.642.98888275.812215.312.339450.743.083182.175.930515.412.421450.843.177382.276.047915.512.503550.943.272182.376.166315.612.58565143.365682.476.284815.712.667751.143.459982.576.402515.812.749851.243.554482.676.521115.912.83251.343.648982.776.63991612.914
27、151.443.743482.876.758716.112.996351.543.837982.976.876716.213.078551.643.9338376.995616.313.160751.744.027683.177.114716.413.242951.844.122383.277.233816.513.325251.944.21783.377.35316.613.40735244.311883.477.472316.713.489652.144.406683.577.592616.813.571952.244.501983.677.712116.913.654252.344.59
28、6883.777.83161713.736652.444.691883.877.951217.113.818952.544.786783.978.070917.213.901152.644.88228478.190717.313.983552.744.977384.178.311517.414.06652.845.072484.278.431417.514.148452.945.16884.378.552417.614.23075345.263284.478.672517.714.313253.145.358984.578.793717.814.395753.245.454184.678.91
29、4917.914.47853.345.549984.779.03521814.560553.445.645384.879.156618.114.643153.545.741284.979.277218.214.722553.645.83718579.398718.314.808153.745.932585.179.520418.414.890553.846.028685.279.642118.514.973153.946.124185.379.763918.615.05585446.220285.479.885818.715.138354.146.316485.580.008818.815.2
30、20954.246.412585.680.130818.915.303554.346.508885.780.2531915.386254.446.60585.880.375319.115.468954.546.700885.980.497619.215.551554.646.79728680.6219.315.634154.746.893686.180.743519.415.716954.846.990186.280.866119.515.799754.947.086586.380.989819.615.88235547.183186.481.113519.715.96555.147.2797
31、86.581.237319.816.047855.247.376886.681.360319.916.130755.347.473586.781.48432016.213455.447.570286.881.608420.116.296355.547.667586.981.731620.216.379155.647.76438781.855920.316.46255.747.861187.181.980320.416.54555.847.95887.282.105820.516.62855.948.055587.382.230320.616.71085648.152487.482.35520.
32、716.793856.148.249587.582.480720.816.876956.248.347187.682.605620.916.959856.348.444287.782.73052117.042856.448.541987.882.855621.117.125956.548.639187.982.981721.217.20956.648.73638883.106921.317.29256.748.834188.183.233221.417.375156.848.931588.283.359621.517.458356.949.029488.383.486121.617.54155
33、749.126888.483.612721.717.624757.149.224888.583.739421.817.707757.249.322988.683.866221.917.79157.349.420588.783.99312217.874257.449.518688.884.120122.117.957557.549.616888.984.247222.218.040857.649.71518984.374422.318.124157.749.813489.184.502722.418.207557.849.911289.284.631122.518.290857.950.0096
34、89.384.758522.618.3745850.10889.484.887122.718.457458.150.206589.585.015922.818.540858.250.30589.685.144722.918.624358.350.403689.785.27362318.707758.450.502289.885.401623.118.791258.550.600989.985.530723.218.874758.650.69969085.659923.318.958258.750.798490.185.790223.419.011758.850.897290.285.91962
35、3.519.125458.950.996190.386.050223.619.2095951.09590.486.179823.719.292659.151.193990.586.310623.819.376259.251.292990.686.441523.919.459859.351.392690.786.57142419.543459.451.491790.886.702524.119.627159.551.590890.986.832724.219.71159.651.699186.96424.319.794759.751.789391.187.095424.419.878459.85
36、1.889191.287.22824.519.962359.951.988591.387.359624.620.04616052.087991.487.491424.720.129960.152.187391.584.624324.820.213760.252.287491.687.756324.920.297760.352.387591.787.88842520.381560.452.487191.888.020525.120.465460.552.586791.988.153925.220.549560.652.6879288.286325.320.633360.752.787392.18
37、8.419925.420.717260.852.887192.288.554725.520.801260.952.986992.388.688525.620.88536153.087492.488.823525.720.969361.153.187992.588.957625.821.053361.253.288592.689.091725.921.137561.353.388592.789.22712621.221561.453.489292.889.361526.121.305861.553.589992.989.497126.221.389961.653.69079389.631726.
38、321.474261.753.791593.189.768726.421.558361.853.891893.289.904626.521.642661.953.992793.390.041826.621.7276254.093793.490.179126.721.911262.154.194793.590.315426.821.895662.254.295893.690.45326.921.979862.354.396993.790.59072722.064262.454.498193.890.728527.122.148762.554.599393.990.865327.222.23362
39、.654.70129491.003327.322.317562.754.802594.191.142627.422.40262.854.903994.291.282127.522.486662.955.005494.391.422727.622.57096355.106894.491.562427.722.655563.155.208494.591.702227.822.740163.255.310694.691.842227.922.824563.355.412294.791.98232822.909263.455.513994.892.123628.122.993863.555.615794.992.26428.223.078563.655.71819592.404428.323.163363.755.8295.192.547328.423.24863.855.921995.292.689228.523.332863.956.024595.392.
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