皖西学浣WEST ANHUIUNIVERSITY化学工程与工艺专业《化工专业实验》指导书材料与化工学院一化工教研室编制2012年5月
１ 化学工程与工艺专业 《化工专业实验》指导书 实验指导书 材料与化工学院—化工教研室 编制 2012 年 5 月
目录实验一串联流动反应器停留时间分布的测定、实验目的二、实验原理·三、实验装置四、实验步骤·五、数据处理六、思考题·实验二固-膜分离实验2一、实验目的1. 2二、基本原理·12三、实验装置与流程4四、实验步骤5实验三管式反应器流动特性测定实验1 7一，实验目的1.7二、实验原理及要点1.7三、装置与流程19四、实验准备工作20五、实验操作指导20六、数据处理·21七、实验报告要求23实验四三组分体系液-液平衡数据测定24实验目的24实验原理·242
２ 目 录 实验一 串联流动反应器停留时间分布的测定············································７ 一、实验目的··················································································································７ 二、实验原理··················································································································７ 三、实验装置··················································································································８ 四、实验步骤··················································································································９ 五、数据处理··················································································································９ 六、思考题··················································································································１１ 实验二 固-膜分离实验 ······································································１２ 一、实验目的···············································································································１２ 二、基本原理···············································································································１２ 三、 实验装置与流程···································································································１４ 四、实验步骤···············································································································１５ 实验三 管式反应器流动特性测定实验··················································１７ 一．实验目的···············································································································１７ 二、实验原理及要点 ····································································································１７ 三、装置与流程···········································································································１９ 四、实验准备工作········································································································２０ 五、实验操作指导········································································································２０ 六、数据处理···············································································································２１ 七、实验报告要求········································································································２３ 实验四 三组分体系液-液平衡数据测定················································２４ 一、 实验目的·············································································································２４ 二、 实验原理·············································································································２４
三、实验仪器及试料2 4四、操作步骤25五、实验记录及数据处理26六、实验报告·27附录·.28实验五筛板塔精馏过程实验2 9一，实验目的·29二.基本原理2.9三。 实验装置和流程33四。实验步骤与注意事项....35五，实验报告36六．思考题36实验六乙苯脱氢制备苯乙烯37一、实验目的37二、实验原理·37三、实验装置及流程·38四、实验准备物料及仪器3 9五、实验步骤及方法39六。数据记录与处理·4.0七、实验结果与讨论1实验七液-液转盘萃取4 5实验目的45二、基本原理45三、.48实验装置与流程四、实验步骤483
３ 三、 实验仪器及试料···································································································２４ 四、 操作步骤·············································································································２５ 五、 实验记录及数据处理····························································································２６ 六、 实验报告·············································································································２７ 附录····························································································································２８ 实验五 筛板塔精馏过程实验 ······························································２９ 一．实验目的···············································································································２９ 二．基本原理···············································································································２９ 三. 实验装置和流程 ····································································································３３ 四．实验步骤与注意事项······························································································３５ 五．实验报告···············································································································３６ 六．思考题··················································································································３６ 实验六 乙苯脱氢制备苯乙烯 ······························································３７ 一、实验目的···············································································································３７ 二、实验原理···············································································································３７ 三、实验装置及流程 ····································································································３８ 四、实验准备物料及仪器······························································································３９ 五、实验步骤及方法 ····································································································３９ 六．数据记录与处理 ····································································································４０ 七、实验结果与讨论 ····································································································４１ 实验七 液-液转盘萃取 ······································································４５ 一、 实验目的···········································································································４５ 二、基本原理···············································································································４５ 三、 实验装置与流程·································································································４８ 四、 实验步骤·············································································································４８
五、实验报告4 9六、思考题50实验八填料塔间歇精馏实验5实验目的51二、基本原理·51三、技术指标与配置51四、操作方法5 1五、故障处理53附录:53实验九果胶的提取及性能测定5 555一、实验目的·55二、实验原理·三、实验药品、仪器、装置5555四、操作步骤·56五、注意事项·六、实验现象及结论记录表56七、问题与思考56实验十丙烯酸酯乳液胶粘剂的制备57、实验目的·57二、实验原理·57三、仪器试剂58四、实验操作58五、注意事项58六、胶接试验59七、思考题594
４ 五、实验报告···············································································································４９ 六、思考题··················································································································５０ 实验八 填料塔间歇精馏实验 ······························································５１ 一、 实验目的···········································································································５１ 二、基本原理···············································································································５１ 三、 技术指标与配置···································································································５１ 四、 操作方法·············································································································５１ 五、 故障处理·············································································································５３ 附录····························································································································５３ 实验九 果胶的提取及性能测定··························································５５ 一、实验目的···············································································································５５ 二、实验原理···············································································································５５ 三、实验药品、仪器、装置 ··························································································５５ 四、操作步骤···············································································································５５ 五、注意事项···············································································································５６ 六、实验现象及结论记录表 ··························································································５６ 七、问题与思考···········································································································５６ 实验十 丙烯酸酯乳液胶粘剂的制备 ···················································５７ 一、实验目的···············································································································５７ 二、实验原理···············································································································５７ 三、仪器试剂···············································································································５８ 四、实验操作···············································································································５８ 五、注意事项···············································································································５８ 六、胶接试验···············································································································５９ 七、思考题··················································································································５９
实验十一6 0防晒膏的配制一、实验目的·60-二、实验原理60三、仪器及试剂·60四、实验操作60五、思考题61实验十二抗氧剂双酚A的合成6 2实验目的·62二实验原理.62三主要仪器和药品63四实验步骤·63五注意事项6364实验十三食品抗氧剂没食子酸丙酯的合成一、实验目的·64二、实验原理·64三、仪器试剂·65四、实验操作6 5五、思考题656 6实验十四餐具洗涤剂的制备一、实验目的66二、产品特性与用途66三、实验原理66四、主要仪器与药品6.767五、实验内容与操作步骤68六、实验记录与数据处理5
５ 实验十一 防晒膏的配制 ···································································６０ 一、实验目的···············································································································６０ 二、实验原理···············································································································６０ 三、仪器及试剂···········································································································６０ 四、实验操作···············································································································６０ 五、思考题··················································································································６１ 实验十二 抗氧剂双酚 A的合成···························································６２ 一 实验目的···············································································································６２ 二 实验原理···············································································································６２ 三 主要仪器和药品 ····································································································６３ 四 实验步骤···············································································································６３ 五 注意事项···············································································································６３ 实验十三 食品抗氧剂没食子酸丙酯的合成 ···········································６４ 一、实验目的···············································································································６４ 二、实验原理···············································································································６４ 三、仪器试剂···············································································································６５ 四、实验操作···············································································································６５ 五、思考题··················································································································６５ 实验十四 餐具洗涤剂的制备 ······························································６６ 一、实验目的···············································································································６６ 二、产品特性与用途 ····································································································６６ 三、实验原理···············································································································６６ 四、主要仪器与药品 ····································································································６７ 五、实验内容与操作步骤······························································································６７ 六、实验记录与数据处理······························································································６８
七、安全与环保.·..............................................................................................八、思考题..6·8...........6
６ 七、安全与环保···········································································································６８ 八、思考题··················································································································６８
实验一串联流动反应器停留时间分布的测定一、实验目的1.通过实验了解：利用电导率测定停留时间分布的基本原理和实验方法。2.掌握停留时间分布的统计特征值的计算方法3.学会用理想反应器串联模型来描述实验系统的流动特性。4.了解微机系统数据采集的方法。二、实验原理本实验停留时间分布测定所采用的主要是示踪响应法。它的原理是：在反应器入口用电磁阀控制的方式加入一定量的示踪剂KNO3，通过电导率仪测量反应器出口处水溶液电导率的变化，间接的描述反应器流体的停留时间。常用的示踪剂加入方式有脉冲输入，阶跃输入和周期输入等。本实验选用脉冲输入法。脉冲输入法是在较短的时间内（0.1～1.0秒），向设备内一次注入一定量的示踪剂，同时开始计时并不断分析出口示踪物料的浓度c(t)随时间的变化。由概率论知识，概率分布密度E(t)就是系统的停留时间分布密度函数。因此，E(t)dt就代表了流体粒子在反应器内停留时间介于t-dt间的概率。在反应器出口处测得的示踪计浓度c(t)于时间t的关系曲线叫响应曲线。由响应曲线可以计算出E(t)与时间t的关系，并绘出E(t)一t关系曲线。计算方法是对反应器作示踪剂的物料衡算，即Qc(t)dt =mE(t)dt(1-1)式中Q表示主流体的流量，m为示踪剂的加入量，示踪剂的加入量可以用下式计算m= J, Qc(t)dt(12)在Q值不变的情况下，由（1）式和（2）式求出c(t)E(t) =(1-3)Je c(n)dt关于停留时间分布的另一个统计函数是停留时间分布函数F(t)，即F(t)= J E(t)dt(1-4)用停留时间分布密度函数E(t)和停留时间分布函数F(t)来描述系统的停留时间，给出了7
７ 实验一 串联流动反应器停留时间分布的测定 一、实验目的 1. 通过实验了解：利用电导率测定停留时间分布的基本原理和实验方法。 2. 掌握停留时间分布的统计特征值的计算方法 3. 学会用理想反应器串联模型来描述实验系统的流动特性。 4. 了解微机系统数据采集的方法。 二、实验原理 本实验停留时间分布测定所采用的主要是示踪响应法。它的原理是：在反应器入口用电 磁阀控制的方式加入一定量的示踪剂 KNO3，通过电导率仪测量反应器出口处水溶液电导率 的变化，间接的描述反应器流体的停留时间。常用的示踪剂加入方式有脉冲输入，阶跃输入 和周期输入等。本实验选用脉冲输入法。 脉冲输入法是在较短的时间内（0.1～1.0 秒），向设备内一次注入一定量的示踪剂，同 时开始计时并不断分析出口示踪物料的浓度 c(t)随时间的变化。由概率论知识，概率分布密 度 E(t)就是系统的停留时间分布密度函数。因此，E(t)dt 就代表了流体粒子在反应器内停留 时间介于 t-dt 间的概率。 在反应器出口处测得的示踪计浓度 c(t)于时间 t 的关系曲线叫响应曲线。由响应曲线可 以计算出 E(t)与时间 t 的关系，并绘出 E(t)－t 关系曲线。计算方法是对反应器作示踪剂的物 料衡算，即 Qc(t)dt = mE(t)dt （1—1） 式中 Q 表示主流体的流量，m 为示踪剂的加入量，示踪剂的加入量可以用下式计算 = 0 m Qc(t)dt （1—2） 在 Q 值不变的情况下，由（1）式和（2）式求出 = 0 ( ) ( ) ( ) c t dt c t E t （1—3） 关于停留时间分布的另一个统计函数是停留时间分布函数 F(t)，即 = 0 F(t) E(t)dt （1—4） 用停留时间分布密度函数 E(t)和停留时间分布函数 F(t)来描述系统的停留时间，给出了
很好的统计分布规律。但是为了比较不同停留时间分布之间的差异，还需引进两个统计特征即数学期望和方差。数学期望对停留时间分布而言就是平均停留时间t，即tE(t)dttE(t)dt(1-5)J. E(t)dt方差是和理想反应器模型关系密切的参数。它的定义是：o, =tE(t)dt -P(1—6)对活塞流反应器，=0：而对全混流反应器，=：的，来计算。(1-7)q?当N为整数时，代表该非理想流动反应器可用N个等体积的全混流反应器的串联来建立模型。当N为非整数时，可以用四舍五入的方法近似处理也可以用不等体积的全混流反应器串联模型。三、实验装置反应器为有机玻璃制成的搅拌釜。其有效容积为1000ml。搅拌方式为叶轮搅拌。流程中配有四个这样的搅拌釜。示踪剂是通过一个电磁阀瞬时注入反应器。示踪剂KNO3在不同时刻浓度c(t)的检测通过电导率仪完成。测量浓度电导率仪A/D转化卡微机系统的传感器图2数据采集原理方框图电导率仪的传感为铂电极，当含有KCI的水溶液通过安装在釜内液相出口处铂电极时，电导率仪将浓度c(t)转化为毫伏级的直流电压信号，该信号经放大器与A/D转机卡处理后，由模拟信号转换为数字信号。该代表浓度c(t)的数字信号在微机内用预先输入的程序进行数据处理并计算出每釜平均停留时间和方差以及N后，由打印机输出。实验仪器3个反应器为有机玻璃制成的搅拌釜（1000ml）8
８ 很好的统计分布规律。但是为了比较不同停留时间分布之间的差异，还需引进两个统计特征， 即数学期望和方差。 数学期望对停留时间分布而言就是平均停留时间 t ，即 = = 0 0 0 ( ) ( ) ( ) tE t dt E t dt tE t dt t （1—5） 方差是和理想反应器模型关系密切的参数。它的定义是： = − 0 2 2 2 t E(t)dt t t （1—6） 对活塞流反应器 2 t ＝0；而对全混流反应器 2 2 t t = ； 的 2 t 来计算。 2 2 t t N = （1—7） 当 N 为整数时，代表该非理想流动反应器可用 N 个等体积的全混流反应器的串联来建 立模型。当 N 为非整数时，可以用四舍五入的方法近似处理也可以用不等体积的全混流反 应器串联模型。 三、实验装置 反应器为有机玻璃制成的搅拌釜。其有效容积为 1000ml。搅拌方式为叶轮搅拌。流程 中配有四个这样的搅拌釜。示踪剂是通过一个电磁阀瞬时注入反应器。示踪剂 KNO3 在不同 时刻浓度 c(t)的检测通过电导率仪完成。 图 2 数据采集原理方框图 电导率仪的传感为铂电极，当含有 KCI 的水溶液通过安装在釜内液相出口处铂电极时， 电导率仪将浓度 c(t)转化为毫伏级的直流电压信号，该信号经放大器与 A／D 转机卡处理后， 由模拟信号转换为数字信号。该代表浓度 c(t)的数字信号在微机内用预先输入的程序进行数 据处理并计算出每釜平均停留时间和方差以及 N 后，由打印机输出。 实验仪器 反应器为有机玻璃制成的搅拌釜（1000ml） 3 个 测量浓度 的传感器 电导率仪 A/D 转化卡 微机系统
3个D-7401型电动搅拌器3个DDS-11C型电导率仪LZB型转子流量计（DN=10mm，L=10~100/h）1个1个DF23电磁阀（PN0.8MPa220V）3个压力表（量程0~1.6MPa.精度1.5级）1套数据采集与A/D转换系统1台控制与数据处理微型计算机打印机1台实验试剂：主流体自来水示踪剂KCI饱和溶液四、实验步骤1.打开系统电源，使电导率预热一个小时。2.打开自来水阀门向贮水槽进水，开动水泵，调节转子流量计的流量，待各釜内充满水后将流量调至30L/h，打开各釜放空阀，排净反应器内残留的空气。3.将预先配制好的饱和KNO溶液加入示踪剂瓶内，注意将瓶口小孔与大气连通。实验过程中，根据实验项目（单釜或三釜）将指针阀转向对应的实验釜。4.观察各釜的电导率值，并逐个调零和满量程，各釜所测定值应基本相同。5.启动计算机数据采集系统，使其处于正常工作状态。6.键入实验条件：将进水流量输入微机内，可供实验报告生成。7.在同一个水流量条件下，分别进行2个搅拌转速的数据采集；也可以在相同转速下改变液体流量，依次完成所有条件下的数据采集。8.选择进样时间为0.1～1.0秒，按“开始'键自动进行数据采集每次采集时间约需35～40分钟。结束时按“停止”键，并立即按“保存数据”键存储数据。9.打开“历史记录”选择相应的保存文件进行数据处理，实验结果可保存或打印。10.结束实验：先关闭自来水阀门，再依次关闭水泵和搅拌器、电导率仪、总电源；关闭计算机。将仪器复原。五、数据处理以进水流量为50升/小时的附图为例，取第三釜曲线，取20个点，计算多釜串联中的9
９ D－7401 型电动搅拌器 3 个 DDS－11C 型电导率仪 3 个 LZB 型转子流量计（DN＝10mm，L＝10～100l/h） 1 个 DF2－3 电磁阀（PN0.8MPa 220V） 1 个 压力表（量程 0～l.6MPa．精度 1.5 级） 3 个 数据采集与 A／D 转换系统 1 套 控制与数据处理微型计算机 1 台 打印机 1 台 实验试剂： 主流体 自来水 示踪剂 KCl 饱和溶液 四、实验步骤 1. 打开系统电源，使电导率预热一个小时。 2. 打开自来水阀门向贮水槽进水，开动水泵，调节转子流量计的流量，待各釜内充满 水后将流量调至 30L／h，打开各釜放空阀，排净反应器内残留的空气。 3. 将预先配制好的饱和 KNO3 溶液加入示踪剂瓶内，注意将瓶口小孔与大气连通。实 验过程中，根据实验项目（单釜或三釜）将指针阀转向对应的实验釜。 4. 观察各釜的电导率值，并逐个调零和满量程，各釜所测定值应基本相同。 5. 启动计算机数据采集系统，使其处于正常工作状态。 6. 键入实验条件：将进水流量输入微机内，可供实验报告生成。 7. 在同一个水流量条件下，分别进行 2 个搅拌转速的数据采集；也可以在相同转速下 改变液体流量，依次完成所有条件下的数据采集。 8. 选择进样时间为 0.1～1.0 秒，按“开始’键自动进行数据采集每次采集时间约需 35～ 40 分钟。结束时按“停止”键，并立即按“保存数据”键存储数据。 9. 打开“历史记录”选择相应的保存文件进行数据处理，实验结果可保存或打印。 10. 结束实验：先关闭自来水阀门，再依次关闭水泵和搅拌器、电导率仪、总电源；关 闭计算机。将仪器复原。 五、数据处理 以进水流量为 50 升/小时的附图为例，取第三釜曲线，取 20 个点，计算多釜串联中的
模型参数N，由附图可以直接读出时间及电导率的数值（由于电导率与浓度之间存在线性关系，故可以直接对电导率进行复化辛普森积分，求出平均停留时间和方差，并以此可以求出模型参数N。用复化辛普森公式求积分hlf(a)+4Zf(x.)+2Zf(x)+f(b)f(t)dt6k=lk=02h=596/10=59.6n=10hC(t)dt:=59.6/6[0.05+4×(0.192857+1.292857+1C。+4cC+2Ck+C106735714+1.478571+1.05+0.692857+0.478571+0.292857+0.192857+0.121429)+2x(0.692857+1.621429+1.65+1.221429+0.85+0.55+0.364286+0.264286+0.164286)+005]=446.7162C(t)E(t) =C(t)hltE(t)dt =tE(0)+4tE(0)+2EtE,(0)+tE(0)=59.6/6[0+4×(0.01396Lk=0k+2k=037+0.280282+0.627151+0.747935+0.682898+0.550757+0.449587+0.317447+0.236924+0.166724)+2×(0.100138+0.468686+0.715416+0.706125+0.614246+0.476944+0.368548+0.305575+0.213696)+0.072264)=241.4354h1’E(t)dt =tE(t)+4EtE1(0)+2ZtEr(t)+t'Eo()=59.6/6[0+4×(0.415316k=0k=023+25.05723+93.44547+156.0193+183.1531+180.5382+174.17+141.8987+120.0255+9439915)+2×(5.968204+55.86731+127.9165+168.3403+183.0454+170.5553+153.7582+145.698+114.6264)+43.06952)=69246.35t E(t)dt-72=10955.3J.12N==5.320811a?1 0
１０ 模型参数 N，由附图可以直接读出时间及电导率的数值（由于电导率与浓度之间存在线性关 系，故可以直接对电导率进行复化辛普森积分，求出平均停留时间和方差，并以此可以求出 模型参数 N。 用复化辛普森公式求积分 = + + + − = − = + 1 0 1 2 1 1 0 ( ) 4 ( ) 2 ( ) ( ) 6 ( ) n k n k k k f a f x f x f b h f t dt h=596/10=59.6 n=10 = + + + = = + 10 9 0 9 2 1 0 1 0 4 2 6 ( ) C C C C h C t dt k k k k =59.6/6[0.05+4×(0.192857+1.292857+1 .735714+1.478571+1.05+0.692857+0.478571+0.292857+0.192857+0.121429)+2×( 0.692857+1.621429+1.65+1.221429+0.85+0.55+0.364286+0.264286+0.164286)+0. 05]=446.7162 = 0 ( ) ( ) ( ) C t C t E t = = + + + = = + ( ) 4 ( ) 2 ( ) ( ) 6 ( ) 1 0 9 0 9 2 0 0 1 0 t E t t E t t E t t E t h t t E t dt k k k k =59.6/6[0+4×(0.0139 37+0.280282+0.627151+0.747935+0.682898+0.550757+0.449587+0.317447+0.236924+ 0.166724)+2×(0.100138+0.468686+0.715416+0.706125+0.614246+0.476944+0.368548+ 0.305575+0.213696)+0.072264]=241.4354 = + + + = = + ( ) 4 ( ) 2 ( ) ( ) 6 ( ) 1 0 2 9 0 9 0 2 2 1 2 0 2 0 2 t E t t E t t E t t E t h t E t dt k k k k =59.6/6[0+4×(0.41531 3+25.05723+93.44547+156.0193+183.1531+180.5382+174.17+141.8987+120.0255+94. 39915)+2×(5.968204+55.86731+127.9165+168.3403+183.0454+170.5553+153.7582+14 5.698+114.6264)+43.06952]=69246.35 2 0 2 2 t E(t)dt t t = − =10955.3 2 2 t t N = =5.320811