搅拌槽内微观混合特性与离集指数的无因次关联
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摘要
微观混合对结晶产物的粒径,粒度分布,形貌有不同程度的影响,视结晶时产物的特性,操作条件而定。研究表征微观混合程度的离集指数随操作变量的变化规律,可为结晶产物粒径和粒度分布等控制提供依据。本文通过改变操作变量如加料时间,加料位置,体积比,搅拌速率,粘度,反应物浓度等来考察其对微观混合程度的影响,利用因次分析法关联离集指数与操作变量的准数式。本文工作如下:
研究微观混合对反应结晶过程的影响,选择Ba(OH)_2+ NaHSO_4+ CLCH_2COOC_2H_5组成的平行竞争反应为研究体系,在以搅拌槽为结晶器内,用副产物乙醇收率测试反应物间微观混合程度,进而确定离集指数。通过单因素实验,考察搅拌速率等操作条件对微观混合效率的影响,并分析了传质系数和扩散系数对微观混合程度的影响。结果表明影响微观混合的主要操作变量为搅拌速率,反应物浓度,加料位置,粘度,传质系数和扩散系数。在此基础上,利用因次分析法中的Rayleigh法或Buckingham法推导出离集指数的准数关联式为: (?)
根据离集指数的实验值,采用多元线性方程回归得到准数式中的模型参数,相关系数为R2=0.9937。验证结果表明由关联式所得离集指数的计算值与实验值的相对误差小于18%,得到离集指数计算值与实验值较吻合的结果。准数式可计算离集准数,并确定沉淀反应中产物粒径和粒度分布的准数范围。利用粒度仪和TEM测定BaSO_4粒径和粒度分布,并考察了Reynolds准数,Schmidt准数和Sherwood准数对粒度分布的影响。研究结果表明当Re≥3800时,BaSO_4主粒度(223 nm)所占比例大于77%。离集指数随Sc的增大而增大,当2800≤Sc≤3500时,BaSO_4主粒度(223 nm)分布在86% - 65%范围内。随Sh的增大离集指数逐渐增大,当800≤Sh≤1200时,BaSO_4主粒度(223 nm)占的比列大于80%。
Influences of micromixing on particle size, particle size distribution, and morphology of crystalls were investigated. Segregation index was characterization by conditions of operating, which particle size, and particle size distribution of crystals were provided for the basis. In this paper, efficiency of micromixing was researched by changing feeding time, feeding position, stirring speed, reactant concentration, viscosity, volume ratio, mass transfer coefficient and diffusion coefficient, where the segregation index was correlationed by dimension analysis. The main work was summarited as follows:
Influences of micromixing on the reaction of crystallization were researched. Parallel competing reation system of Ba(OH)_2+ NaHSO_4+ CLCH_2COOC_2H_5 is selected as the research system with stirred tank as crystallizer. The efficiency of micromixing is valued by the yield of ethanol. To investigatting the influence of reaction conditions on the efficiency of micromixing, which affecten the micro-mixing were known by single factor experimental and theoretical analysis. The main parameters of the model were stirring speed, reactant concentration, feeding position, viscosity, mass transfer coefficient, and diffusion coefficient. Using dimensional analysis (Rayleigh Law or Buckingham Law), dimensionless number were deduced from conditions of operating and segregation index as follows: (?)
Parameter of model of Xs was obtained by using multiple linear regression, and correlation coefficient (R2) was 0.9937. The related average error of experimental value and calculated value was less than 18%. The results indicated that experimental value and calculated value was consistented. From the equation, we can get the crystal size and crystal size distribution of products and determine the range of dimensionless.
Based on the above work, and particle size and its distribution of BaSO_4 was characterized by particle size analyzers and transmission electron microscopy (TEM). The results indicated that size distribution were effected by Re, Sc, and Sh. Re≥3800, proportion of mian size BaSO_4 (223 nm) was more than 77%, ultrafine particles of narrow size distribution was obtained. Segregation index was increased follows Sc increase. 2800≤Sc≤3500, main size of BaSO_4 (223 nm) distribution was ranged from 86% to 65%. Small crystal size and narrow crystal size distribution of ultrafine can been prepared when viscosity was ranged from4.0 mp.s to6.0 mp.s. Segregation index was increased as Sh. 800≤Sh≤1200, main size of BaSO_4 distribution was more than 80%.
研究微观混合对反应结晶过程的影响,选择Ba(OH)_2+ NaHSO_4+ CLCH_2COOC_2H_5组成的平行竞争反应为研究体系,在以搅拌槽为结晶器内,用副产物乙醇收率测试反应物间微观混合程度,进而确定离集指数。通过单因素实验,考察搅拌速率等操作条件对微观混合效率的影响,并分析了传质系数和扩散系数对微观混合程度的影响。结果表明影响微观混合的主要操作变量为搅拌速率,反应物浓度,加料位置,粘度,传质系数和扩散系数。在此基础上,利用因次分析法中的Rayleigh法或Buckingham法推导出离集指数的准数关联式为: (?)
根据离集指数的实验值,采用多元线性方程回归得到准数式中的模型参数,相关系数为R2=0.9937。验证结果表明由关联式所得离集指数的计算值与实验值的相对误差小于18%,得到离集指数计算值与实验值较吻合的结果。准数式可计算离集准数,并确定沉淀反应中产物粒径和粒度分布的准数范围。利用粒度仪和TEM测定BaSO_4粒径和粒度分布,并考察了Reynolds准数,Schmidt准数和Sherwood准数对粒度分布的影响。研究结果表明当Re≥3800时,BaSO_4主粒度(223 nm)所占比例大于77%。离集指数随Sc的增大而增大,当2800≤Sc≤3500时,BaSO_4主粒度(223 nm)分布在86% - 65%范围内。随Sh的增大离集指数逐渐增大,当800≤Sh≤1200时,BaSO_4主粒度(223 nm)占的比列大于80%。
Influences of micromixing on particle size, particle size distribution, and morphology of crystalls were investigated. Segregation index was characterization by conditions of operating, which particle size, and particle size distribution of crystals were provided for the basis. In this paper, efficiency of micromixing was researched by changing feeding time, feeding position, stirring speed, reactant concentration, viscosity, volume ratio, mass transfer coefficient and diffusion coefficient, where the segregation index was correlationed by dimension analysis. The main work was summarited as follows:
Influences of micromixing on the reaction of crystallization were researched. Parallel competing reation system of Ba(OH)_2+ NaHSO_4+ CLCH_2COOC_2H_5 is selected as the research system with stirred tank as crystallizer. The efficiency of micromixing is valued by the yield of ethanol. To investigatting the influence of reaction conditions on the efficiency of micromixing, which affecten the micro-mixing were known by single factor experimental and theoretical analysis. The main parameters of the model were stirring speed, reactant concentration, feeding position, viscosity, mass transfer coefficient, and diffusion coefficient. Using dimensional analysis (Rayleigh Law or Buckingham Law), dimensionless number were deduced from conditions of operating and segregation index as follows: (?)
Parameter of model of Xs was obtained by using multiple linear regression, and correlation coefficient (R2) was 0.9937. The related average error of experimental value and calculated value was less than 18%. The results indicated that experimental value and calculated value was consistented. From the equation, we can get the crystal size and crystal size distribution of products and determine the range of dimensionless.
Based on the above work, and particle size and its distribution of BaSO_4 was characterized by particle size analyzers and transmission electron microscopy (TEM). The results indicated that size distribution were effected by Re, Sc, and Sh. Re≥3800, proportion of mian size BaSO_4 (223 nm) was more than 77%, ultrafine particles of narrow size distribution was obtained. Segregation index was increased follows Sc increase. 2800≤Sc≤3500, main size of BaSO_4 (223 nm) distribution was ranged from 86% to 65%. Small crystal size and narrow crystal size distribution of ultrafine can been prepared when viscosity was ranged from4.0 mp.s to6.0 mp.s. Segregation index was increased as Sh. 800≤Sh≤1200, main size of BaSO_4 distribution was more than 80%.
引文
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[5] Villermaux J., Blavier L..A new method for modeling free radical homogenous polymerization reactions [J].Chem. Eng. Sci.1984,39:87~99
[6] Dombrowski N., Hooper P.C..The performance characteristics of an impinging jet Atomizer in Atomospheres of high Ambient[ J].Density Fuel.1962,41:323
[7] Bhandarkar S; Brown R..Studies in rapid precipitation of Hydroxides of Calcium and Magnesium[J]. J.crystal growth .1989, 97:407
[8]Karpinski P.H..Importance of the two-step crystal growth model [J].Chem.Eng.Sci.1985, 40:641~646
[9] Nauman E.B..The droplet diffusion model for micromixing [J].Chem.Eng.Sci.1975, 30:1135
[10] Bourne J.R..The characterization of micromixing using fast multiple reactions [J]. Chem.Eng.Commun.1982, 16:79
[11] Pohorecki R;Baldyga J..The effects of micromixing and the manner of reactor feeding on precipitation in stirred tank reactors [J].Chem. Eng.Sci.1988,43:149~160
[12] Bourne J.R.,Gholap R.V.,Rewatkar V.B..The influence of viscosity on the product distribution of fast parallel reactions [J].Chem.Eng.Sci.1995,58:15~20
[13] Curl R.L..Dispersed phase mixing:(I)theory and effects in simple reactors[J]. AIChE J.1963,9:175~181
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[16] Ritchie B.W.,Tobgy A.H..A three enironment micromixing model for chemical reactors witharbitrary separate feed streams [J].Chem.Eng.J.1979,17:173~182
[17] Aubry C.,VillermauxJ..Mixing effects on complex reactions in a CSTR [J].Chem.Eng.Sci. 1975, 30:1309
[18] Mao K.W.,Toor H.L..A diffusion model for reactions with turbulent mixing [J]. AIChE J .1970,16:49~52
[19] Ottino J.M.,Ranz W.E..A lamellar model for analysis of liquid mixing [J].Chem.Eng.Sci.1979, 34:877~899
[20] Baldyga J.,Bourne.J.R..A Fluid mechanical approach to turbulent mixing and chemical reaction:Part (I)Inadequacies of available methods[J].Chem.Eng.Commun.1984,28:231~241
[21] Fournier M.-C.,Falk L.,Villermaux J..A new parallel competing reactor system for assessing micromixing efficiency (I):experimental approach[J].Chem. Eng. Sci.1996,55(22): 5053~5064
[22] Fournier M.-C.,Falk L,Villermaux J.A new parallel competing reaction system for assessing micromixing efficiency(Ⅱ):determination of micromixing time by a simple mixing model[J]. Chem.Eng.Sci.1996,51(23):5187~5196
[23]李希,陈剑峰,陈甘棠.微观混合研究现状[J].化学反应工程与工艺.1994,10(2):104～112
[24] Carretier E.,Wyart Y.,Guichardon P.etal. New insight micromixing in supercritical CO2 using a chemical model [J].J.of Supercritical Fluids.2006,38:332~338
[25] Yu S.Y..Micromixing and parallel reaction[D].Switzerland:Eidgenoessische Technisce Hochschule Zuerich,1993
[26] Bourne J.R.,Gholap R.V.,Rewatkar V.B..The influence of viscosity on the product distribution of fast parallel reactions [J].Chem.Eng.Sci.1995,58:15~20
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