挤出滚圆法制备球形颗粒的一些关键技术的研究
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摘要
使用挤出滚圆技术制备球形颗粒,具有生产效率高,产品圆整度好和机械性能高等特点；并且生产过程健康环保,制备工艺、设备简单,近半个世纪以来,在国内外医药、食品、饲料、化妆品等行业得到了广泛的应用。尽管挤出滚圆法造粒技术显示了巨大的优越性而被广泛的应用,但是仍然还有一些关键性问题没有解决。
本文针对物料适宜挤出滚圆法造粒的理想润湿混合黏-塑态的构建问题,采用颗粒制备对比实验和机理分析相结合的方法,通过对中药鼻炎康干浸膏物料降粘方法和无机氧化铝物料增粘方法的研究,深入分析了中药浸膏物料吸湿黏结的机理、无机氧化铝球形催化剂载体制备过程中操作参数的改变对产品催化性能和表观质量的影响,为实现挤出滚圆法造粒技术在更广泛的领域应用提供理论基础。论文的主要研究工作和创新成果如下：
(1)基础理论研究。
分析了水与微晶纤维素润湿机理。从氢键作用、范德华力作用、分子扩散自粘作用等角度探讨了分子问不同作用力与理想润湿混合体系黏度的关系。分析了破断过程中动能向表面能的转化机理,推导出摩擦底盘转数和物料长度与物料破断效果之间内在关系的破断势能公式。通过运动模型和颗粒受力分析模型的建立,系统分析了滚圆过程中,物料总体的运动规律、单个颗粒的运动形式和颗粒滚圆成球的主要变形力,并对起主要作用的变形力进行了定量分析。
(2)提高中药浸膏微丸载药水平的研究。
分析了水与中药浸膏的润湿过程、乙醇与中药浸膏的润湿过程,从配位化学键作用、静电作用和氢键过度缔合作用等角度讨论了中药浸膏物料的吸湿黏结机理。通过中药-β-环糊精包合物制备实验、中药鼻炎康浸膏微丸的制备实验与比较法黏度测定装置的研制,对比研究了各种有针对性的降粘方法中辅料的用量,在有效降低体系黏度的同时,达到了适度减少辅料用量的目标。
(3)无机粉体氧化铝适宜挤出滚圆造粒的粘-塑性体系构建。
通过颗粒制备实验,筛选出无机氧化铝粉体实现挤出滚圆过程必备的最佳黏结剂、助挤剂、赋形剂。通过对有机胶黏剂与无机粉体颗粒表面的黏结机理分析和应用、偶联剂改性机理分析和应用,在制备出球形氧化铝基催化剂载体的基础上,进一步研究了提高产品圆整度和强度的措施、造粒过程及工艺参数改变对最终产品性能和表观质量的影响。
(4)有极端黏度表现物料的造粒实践。
本文以本实验室自行研制的专利产品微丸造粒机为主要实验设备,以鼻炎康浸膏粉体为高黏有机物料代表,超细氧化铝粉体为低黏无机物料的典型代表,通过颗粒制备实验确定了最佳造粒配方和工艺操作参数,并重点讨论了球形氧化铝催化剂载体制备过程对催化剂载体性能的影响。
Spherical particles prepared by extrusion-spheronization technology, have higher production efficiency, better roundness characteristics and higher mechanical properties; moveover environmental health of the production process, simple of the process and equipment, nearly half a century, it is widespread use in food, feed, cosmetics and other industries at home and abroad. Although Extrusion spheronization Granulation shows its great advantage was widely used, but there are still some key issues unresolved.
This texts was aimed at construction of a ideal wetting and mixing stick-plastic,state of material which was suitable for extrusion spheronization, combined particle preparation comparative experiments with analysis of mechanism, through research on the viscosity reduction methods of dry extract of Chinese medicine Rhinitis and viscosity enhancement methods of inorganic alumina material, by depth analysis of the mechanism of moisture bonding of Chinese traditional medicine extract materials, the effect of operating parameters on product apparent quality and catalytic properties in inorganic alumina spherical catalyst preparation process, provide a theoretical basis to achieve applications in the broader field for extrusion spheronization technology. The main research work and innovations are as follows:
(1) Basic theoretical research.
This paper analyzes the wetting mechanism of water and microcrystalline cellulose, from hydrogen bonding, van der Waals force, the role of molecular diffusion bonding discussing the relationship between the different of the wetting force of molecule and the ideal viscosity mixture. Analysis the mechanism of kinetic transformation to the surface energy during breaking, derived the potential breaking formula which reflect the intrinsic relationship of breaking effect about chassis friction rotation speed and materials length. By establishing the model of motion and particle deformation, system analysis the general sports law of overall materials and the movement type of single particle during spheronization process, the main deformation force of the particles spheronization into the ball, and to quantitative analysis the deformation force of playing major role.
(2) The research of improving the level of Chinese medicine extract pellets containing drug. Issues of water and the wetting process of Chinese traditional medicine extract, ethanol extract of the wetting process and traditional Chinese medicine, from the coordination chemical bonding, electrostatic and hydrogen bond angles of over-associating traditional Chinese medicine extract materials discussed bonding mechanism of moisture. By traditional Chinese medicine-β-cyclodextrin inclusion compound experiment, comparison device for measuring the viscosity, medicine extract pellets Biyankang experimental, comparative study of various accessories targeted amount of viscosity reduction method, in effectively reduce the viscosity of the same time, reached a modest goal of reducing the amount excipients.
(3) The construction of inorganic alumina powder granulation suitable for extrusion-spheronization visco-plastic system.
Through the particles preparation experiment, selecting the best bonder, help squeeze agent, excipient which necessary to inorganic alumina powder extrusion spheronization process. Through analysis and application of the adhesive bonding mechanism of the surface of powder particle between organic and inorganic, analysis and application of coupling agent modification mechanism, based on the preparation of spherical alumina-based catalyst, further research how to improve product roundness and intensity of measures and how to change the parameters and granulation process to obtain the better final product performance and apparent quality.
(4) The granulation practice of the extremely viscosity performance of the material. In this paper, self-developed patent product pellet granulator machine was the main experimental equipment, Rhinitis extract powder was the representative of high-viscosity Chinese medicine materials, ultra-fine alumina powder was a typical representative of inorganic powders, the best formula and process operating parameters were confirmed through by a large number of experiments and the preparation process of the carrier performance was focused and discussed.
本文针对物料适宜挤出滚圆法造粒的理想润湿混合黏-塑态的构建问题,采用颗粒制备对比实验和机理分析相结合的方法,通过对中药鼻炎康干浸膏物料降粘方法和无机氧化铝物料增粘方法的研究,深入分析了中药浸膏物料吸湿黏结的机理、无机氧化铝球形催化剂载体制备过程中操作参数的改变对产品催化性能和表观质量的影响,为实现挤出滚圆法造粒技术在更广泛的领域应用提供理论基础。论文的主要研究工作和创新成果如下：
(1)基础理论研究。
分析了水与微晶纤维素润湿机理。从氢键作用、范德华力作用、分子扩散自粘作用等角度探讨了分子问不同作用力与理想润湿混合体系黏度的关系。分析了破断过程中动能向表面能的转化机理,推导出摩擦底盘转数和物料长度与物料破断效果之间内在关系的破断势能公式。通过运动模型和颗粒受力分析模型的建立,系统分析了滚圆过程中,物料总体的运动规律、单个颗粒的运动形式和颗粒滚圆成球的主要变形力,并对起主要作用的变形力进行了定量分析。
(2)提高中药浸膏微丸载药水平的研究。
分析了水与中药浸膏的润湿过程、乙醇与中药浸膏的润湿过程,从配位化学键作用、静电作用和氢键过度缔合作用等角度讨论了中药浸膏物料的吸湿黏结机理。通过中药-β-环糊精包合物制备实验、中药鼻炎康浸膏微丸的制备实验与比较法黏度测定装置的研制,对比研究了各种有针对性的降粘方法中辅料的用量,在有效降低体系黏度的同时,达到了适度减少辅料用量的目标。
(3)无机粉体氧化铝适宜挤出滚圆造粒的粘-塑性体系构建。
通过颗粒制备实验,筛选出无机氧化铝粉体实现挤出滚圆过程必备的最佳黏结剂、助挤剂、赋形剂。通过对有机胶黏剂与无机粉体颗粒表面的黏结机理分析和应用、偶联剂改性机理分析和应用,在制备出球形氧化铝基催化剂载体的基础上,进一步研究了提高产品圆整度和强度的措施、造粒过程及工艺参数改变对最终产品性能和表观质量的影响。
(4)有极端黏度表现物料的造粒实践。
本文以本实验室自行研制的专利产品微丸造粒机为主要实验设备,以鼻炎康浸膏粉体为高黏有机物料代表,超细氧化铝粉体为低黏无机物料的典型代表,通过颗粒制备实验确定了最佳造粒配方和工艺操作参数,并重点讨论了球形氧化铝催化剂载体制备过程对催化剂载体性能的影响。
Spherical particles prepared by extrusion-spheronization technology, have higher production efficiency, better roundness characteristics and higher mechanical properties; moveover environmental health of the production process, simple of the process and equipment, nearly half a century, it is widespread use in food, feed, cosmetics and other industries at home and abroad. Although Extrusion spheronization Granulation shows its great advantage was widely used, but there are still some key issues unresolved.
This texts was aimed at construction of a ideal wetting and mixing stick-plastic,state of material which was suitable for extrusion spheronization, combined particle preparation comparative experiments with analysis of mechanism, through research on the viscosity reduction methods of dry extract of Chinese medicine Rhinitis and viscosity enhancement methods of inorganic alumina material, by depth analysis of the mechanism of moisture bonding of Chinese traditional medicine extract materials, the effect of operating parameters on product apparent quality and catalytic properties in inorganic alumina spherical catalyst preparation process, provide a theoretical basis to achieve applications in the broader field for extrusion spheronization technology. The main research work and innovations are as follows:
(1) Basic theoretical research.
This paper analyzes the wetting mechanism of water and microcrystalline cellulose, from hydrogen bonding, van der Waals force, the role of molecular diffusion bonding discussing the relationship between the different of the wetting force of molecule and the ideal viscosity mixture. Analysis the mechanism of kinetic transformation to the surface energy during breaking, derived the potential breaking formula which reflect the intrinsic relationship of breaking effect about chassis friction rotation speed and materials length. By establishing the model of motion and particle deformation, system analysis the general sports law of overall materials and the movement type of single particle during spheronization process, the main deformation force of the particles spheronization into the ball, and to quantitative analysis the deformation force of playing major role.
(2) The research of improving the level of Chinese medicine extract pellets containing drug. Issues of water and the wetting process of Chinese traditional medicine extract, ethanol extract of the wetting process and traditional Chinese medicine, from the coordination chemical bonding, electrostatic and hydrogen bond angles of over-associating traditional Chinese medicine extract materials discussed bonding mechanism of moisture. By traditional Chinese medicine-β-cyclodextrin inclusion compound experiment, comparison device for measuring the viscosity, medicine extract pellets Biyankang experimental, comparative study of various accessories targeted amount of viscosity reduction method, in effectively reduce the viscosity of the same time, reached a modest goal of reducing the amount excipients.
(3) The construction of inorganic alumina powder granulation suitable for extrusion-spheronization visco-plastic system.
Through the particles preparation experiment, selecting the best bonder, help squeeze agent, excipient which necessary to inorganic alumina powder extrusion spheronization process. Through analysis and application of the adhesive bonding mechanism of the surface of powder particle between organic and inorganic, analysis and application of coupling agent modification mechanism, based on the preparation of spherical alumina-based catalyst, further research how to improve product roundness and intensity of measures and how to change the parameters and granulation process to obtain the better final product performance and apparent quality.
(4) The granulation practice of the extremely viscosity performance of the material. In this paper, self-developed patent product pellet granulator machine was the main experimental equipment, Rhinitis extract powder was the representative of high-viscosity Chinese medicine materials, ultra-fine alumina powder was a typical representative of inorganic powders, the best formula and process operating parameters were confirmed through by a large number of experiments and the preparation process of the carrier performance was focused and discussed.
引文
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