MSMPR结晶器中肌肉肌醇的冷却结晶动力学

对肌肉肌醇(以下简称肌醇)在纯水中的冷却结晶动力学进行了一定的理论研究。实验测得了不同条件下肌醇晶体的粒数密度分布数据,通过粒数衡算方程,证明肌醇晶体生长过程是与粒度无关的;采用间歇动态法中的矩量变换法建立了肌醇冷却结晶过程动力学方程,利用最小二乘法回归出肌醇结晶过程中的各项动力学参数,得到肌醇晶体的成核速率方程和生长速率方程。实验结果表明,肌醇晶体的成核和生长过程均为吸热过程;在肌醇结晶过程中,成核较生长更容易发生。     

蛋氨酸CO2酸化半间歇反应结晶动力学研究

针对海因法合成蛋氨酸工艺，利用间歇动态法、以蛋氨酸钾为原料研究了CO₂酸化条件下蛋氨酸的反应结晶过程，建立结晶动力学模型。通过矩量变化法求解粒数衡算方程，利用最小二乘法对数据多元线性回归得到结晶动力学参数。结果表明：晶体生长类型为粒度无关生长，晶体生长活化能为21.01 kJ·mol^-1,成核与生长速率方程中过饱和度的指数分别为0.62和1.52,晶体聚结对结晶过程的影响不可忽略。气体表观速率、搅拌速率对晶体成核与聚结均有明显影响。高过饱和度与高搅拌转速不利于晶体平均粒径的增加。     

间歇结晶器中地塞米松磷酸钠溶析结晶动力学的研究

在间歇结晶器中,利用矩量变换法对地塞米松磷酸钠溶析结晶过程动力学进行了理论研究。由实验得到的地塞米松磷酸钠晶体的粒数密度分布数据,采用非线性最小二乘法分别对与粒度相关和与粒度无关线性生长速率模型进行了参数估值,通过由各种模型得到的晶体生长速率的计算与实验值的比较,发现与粒度无关生长速率模型不仅计算过程简单且计算的精度也更好。最后,以与粒度无关生长速率模型为基础,由不同实验条件下晶体的粒数密度分布数据非线性回归出其成核速率方程和生长速率方程。对方程的理论分析表明,低过饱和度、低悬浮密度和较高的结晶温度有利于得到平均粒径更大的地塞米松磷酸钠晶体。     

湿法磷酸介质中氟硅酸钾（钠）结晶动力学研究

运用粒数平衡方程,在MSMPR结晶器中研究了氟硅酸钾（钠）在湿法磷酸中的结晶动力学,建立了成核速率－晶体生长速率及成核速率－晶体生长速率－悬浮密度的动力学模型。     

双酚A-苯酚加合物结晶动力学

提出了一种新的间歇动态法,用来测定晶体成核与生长动力学参数。对粒数密度衡算方程进行变换,可测定晶体生长速率;通过建立晶体生长速率与成核速率之间的定量关系式,求得晶体成核速率。应用该方法,测定了双酚A-苯酚加合物结晶动力学参数。     

对二甲苯悬浮熔融结晶动力学

结晶法是工业上生产对二甲苯的主要方法之一。现有对二甲苯结晶动力学参数均单纯由结晶母液的温度和浓度变化通过非线性优化法而获得,未检测对二甲苯的晶体粒度数据,因而其准确性难以得到保证。本文利用超声在线粒度仪(OPUS)检测对二甲苯晶体的粒度分布,通过添加晶种的间歇悬浮熔融结晶实验,应用矩量变换法测定82%（质量）对二甲苯-间二甲苯体系中的对二甲苯结晶动力学。利用最小二乘法对动力学实验数据进行多元线性回归后得到了对二甲苯结晶动力学方程,研究结果表明,在对二甲苯悬浮熔融结晶过程中,溶液相对过饱和度对对二甲苯晶体成核速率的影响大于对晶体生长速率的影响,搅拌速率对成核过程影响明显,而晶浆悬浮密度对成核速率的影响不大。     

1,2,3-三硝基氮杂环丁烷溶析结晶动力学研究

基于分级法[1]求解了TNAZ间歇溶析结晶过程的粒数衡算方程,通过激光粒度分布测量仪测量了结晶过程中粒度分布随不同温度、搅拌强度、溶析剂滴加速率的变化规律。利用已建立的TNAZ间歇溶析结晶过程的粒数衡算方程求解模型得到了生长动力学参数,最后用最小二乘法模拟出了成核速率和生长速率方程[2]。成核速率和生长速率是结晶模拟过程中最核心的控制条件。     

TNAZ溶析结晶动力学研究

基于分级法[1]求解1,3,3-三硝基氮杂环丁烷(TNAZ)问歇溶析结晶过程的粒数衡算方程,通过激光粒度分布测量仪测量了结晶过程中粒度分布随温度、搅拌强度、溶析剂滴加速率的变化规律.利用已建立的TNAZ间歇溶析结晶过程的粒数衡算方程求解模型得到生长动力学参数,最后用最小二乘法模拟出成核速率和生长速率方程[2].成核速率...     

青霉素亚砜结晶生长与成核动力学

利用Mydlarz 和 Jones 模型（MJ2）,对乙酸丁酯中青霉素亚砜的成核与生长动力学进行研究。通过矩量法对MJ2模型进行处理后,利用晶体产品的粒度分布计算得到青霉素亚砜的生长速率与成核速率,然后利用最小二乘法拟合回归求解出成核与生长动力学方程参数。通过实验设计考察了过饱和度、温度与搅拌速度对青霉素亚砜晶体成核和生长过程的影响。研究表明青霉素亚砜晶体生长速率随过饱和度比的增加呈现指数型增长,确定青霉素亚砜晶体生长属于晶体表面生长控制过程。由于高速搅拌会增加青霉素亚砜晶体的破碎,促进了二次成核过程,随着搅拌速度的增加,晶体生长速率出现小幅下滑,而成核速率则明显升高。青霉素亚砜成核与生长动力学研究将有助于工业生产过程优化。     

连续结晶器中十水草酸铈反应结晶动力学研究

采用连续稳态法,对十水草酸铈在混合悬浮、混合产品排出(MSMPR)结晶器中的连续反应结晶动力学进行了研究。实验测定了十水草酸铈晶体的粒数密度分布数据,并以此为基础,基于粒度无关生长速率模型,对不同实验条件下晶体的粒数密度分布数据进行拟合,确定了十水草酸铈的成核动力学方程和生长动力学方程,并计算得到十水草酸铈晶体的成核、生长速率相对于过饱和度的指数分别为4.211和0.752。同时,对方程的理论分析表明,低过饱和度有利于得到平均粒径更大的十水草酸铈晶体。十水草酸铈结晶动力学的研究,为其大规模工业生产提供了重要的动力学数据。     

环丙沙星冷却结晶动力学测定

依据粒数衡算方程,采用分离变量方法求解粒数密度函数表达式,依据该方法通过加晶种的间歇冷却结晶实验研究了环丙沙星在23％(体积)水/乙醇溶液中的结晶动力学数据,得到了结晶动力学方程,为工业结晶动力学的测定、结晶特性辨识、粒度分布预测和控制提供了新的方法.     

CRYSTALLIZATION KINETICS AND PRODUCT PURITY OF α-GLUTAMIC ACID CRYSTAL

A continuous mixed-suspension mixed-product removal lpar;CMSMPR) crystallizer was used to study the crystallization kinetics and product purity of glutamic acid crystal in pure solution and impure solution with L-phenylanaline as the impurity. Under the assumption that the crystal growth rate was a function of crystal size, the population balance equation was solved to give the crystal growth and nucleation rates by use of the steady-state population density data. The crystal growth and nucleation rates were suppressed by the presence of impurity. The impurity contents in the crystal products, which were analyzed by a HPLC pre-column method, were found to be related to crystal size, supersaturation, and impurity concentration of solution     

间歇结晶过程中几种可能的粒度分布

对间歇溶液结晶过程,依据粒数衡算方程,在忽略二次过程如聚集、破碎和老化等且混合良好情况的假设下,采用分离变量方法对粒度相关生长或生长分散的粒度分布进行理论分析,推导出间歇结晶过程中的几个粒数密度与结晶时间和晶体粒度的关系式.这些关系式可以用于间歇结晶过程中,选择合适的晶体生长机理与测定线性晶体生长速率,预测粒度分布与优化结晶过程,以及回归粒度分布.结果表明,本方法在溶液结晶过程中具有良好的应用价值.     

MSMPR反应结晶器中地塞米松磷酸钠晶体生长模型的研究

The reactive crystallization process of dexamethasone sodium phosphate was investigated in a continuous mixed-suspension, mixed-product-removal(MSMPR) crystallizer. Analyzing experimental data, it was found that the growth of product crystal was size-dependent. The Bransom, CR, ASL, M J2 and M J3 size-dependent growth models were discussed in details. Using experimental steady state population density data of dexamethasone sodium phosphate, parameters of five size-dependent growth models were determined by the method of non-linear least-squares. By comparison of experimental population density and linear growth rate data with those obtained from the five size-dependent growth models, it was found that the MJ3 model predicts the growth more accurately than do the other four models. Based on the theory of population balance, the crystal nucleation and growth rate equations of dexamethasone sodium phosphate were determined by non-linear regression method. The effects of different operation parameters such as supersaturation, magma density and temperature on the quality of product crystal were also discussed, and the optimal operation conditions were derived.     

CRYSTALLIZATION KINETICS OF 2-CHLORO-4,6-DINITRORESORCINOL BY BATCH COOLING CRYSTALLIZATION METHOD

Crystallization kinetics of 2-chloro-4,6-dinitroresorcinol in ethanol was studied by the method of intermittent dynamic analysis. The nucleation rate and crystal growth rate of 2-chloro-4,6-dinitroresorcinol under different crystallization temperatures and stirring rates were estimated. The results show that with an increase of crystallization temperature, both the nucleation rate and crystal growth rate increase. It is further found that when the stirring rate increases, the nucleation rate increases and the crystal growth rate decreases. The technological conditions of cooling crystallization of 2-chloro-4,6-dinitroresorcinol were studied. It is found that when the stirring rate is 180 rpm and the solution is cooled slowly to - 8°C, the particle size of the products is even and the highest yield of 2-chloro-4,6-dinitroresorcinol is 40.6%.     

CRYSTALLIZATION KINETICS OF 2-CHLORO-4,6-DINITRORESORCINOL BY BATCH COOLING CRYSTALLIZATION METHOD

Crystallization kinetics of 2-chloro-4,6-dinitroresorcinol in ethanol was studied by the method of intermittent dynamic analysis. The nucleation rate and crystal growth rate of 2-chloro-4,6-dinitroresorcinol under different crystallization temperatures and stirring rates were estimated. The results show that with an increase of crystallization temperature, both the nucleation rate and crystal growth rate increase. It is further found that when the stirring rate increases, the nucleation rate increases and the crystal growth rate decreases. The technological conditions of cooling crystallization of 2-chloro-4,6-dinitroresorcinol were studied. It is found that when the stirring rate is 180 rpm and the solution is cooled slowly to ? 8°C, the particle size of the products is even and the highest yield of 2-chloro-4,6-dinitroresorcinol is 40.6%.     

一水盐酸环丙沙星初级成核机理的研究

A general expression for the ralationship between induction period and supersaturation was developed based on polynuclear approach.Different mechanism of primary nucleation in solution can be illustrated by the expression.The results of induction period determined by laser scatering method shows that the crystallization of ciprofloxacin hydrochloride monohydrate in water/ethanol or aqueous solution is by the mechanism of primary nucleation followed by one-dimensional diffusion growth,and then one-dimensional continuous or “birth and spread” growth on crystal face. The growth mechanism on the crystal face is affected by temperature and solvent.     

乙醇溶析结晶法由棉籽壳制备木糖

采用乙醇溶析结晶方法,以棉籽壳为原料,经一系列处理步骤,得到一种木糖晶体产品;对该晶体产品进行了红外光谱分析、熔程分析、环境扫描电镜分析、液相色谱分析和粒度分析。结果表明,该晶体产品与由玉米芯得到的木糖晶体具有类似的红外光谱曲线和熔程,但在晶形上,该晶体呈长棱形,而玉米芯木糖晶体呈方形;按本文优化的操作条件进行操作,结晶产品纯度为99.64%,收率为77.6%,中间粒度(M.S.)为151μm,变异系数(C.V.)为47%。表明乙醇溶析结晶是一种很有潜力的结晶方法。