• ISSN 1008-505X
  • CN 11-3996/S

聚烯烃包膜控释肥膜层孔径测定方法研究

徐久凯, 李絮花, 杨相东, 李燕婷, 李娟, 张建君, 赵秉强

徐久凯, 李絮花, 杨相东, 李燕婷, 李娟, 张建君, 赵秉强. 聚烯烃包膜控释肥膜层孔径测定方法研究[J]. 植物营养与肥料学报, 2016, 22(3): 794-801. DOI: 10.11674/zwyf.15029
引用本文: 徐久凯, 李絮花, 杨相东, 李燕婷, 李娟, 张建君, 赵秉强. 聚烯烃包膜控释肥膜层孔径测定方法研究[J]. 植物营养与肥料学报, 2016, 22(3): 794-801. DOI: 10.11674/zwyf.15029
XU Jiu-kai, LI Xu-hua, YANG Xiang-dong, LI Yan-ting, LI Juan, ZHANG Jian-jun, ZHAO Bing-qiang. Study on measuring methods for pore size of polyolefin film coated controlled-release fertilizer[J]. Journal of Plant Nutrition and Fertilizers, 2016, 22(3): 794-801. DOI: 10.11674/zwyf.15029
Citation: XU Jiu-kai, LI Xu-hua, YANG Xiang-dong, LI Yan-ting, LI Juan, ZHANG Jian-jun, ZHAO Bing-qiang. Study on measuring methods for pore size of polyolefin film coated controlled-release fertilizer[J]. Journal of Plant Nutrition and Fertilizers, 2016, 22(3): 794-801. DOI: 10.11674/zwyf.15029

聚烯烃包膜控释肥膜层孔径测定方法研究

基金项目: 

复合乳液包膜肥料的制备及其性能研究(2011-28); 聚合物包膜控释肥膜孔结构特征研究(2013-17); 复合(混)肥农艺配方与生态工艺技术研究(2011BAD11B05); 公益性行业(农业)科研专项经费(201103003)资助。

详细信息
    作者简介:

    徐久凯(1990—), 男, 山东德州人, 硕士研究生, 主要从事新型肥料研制与应用。E-mail:xujiukai2008@163.com

  • 中图分类号: TQ449+.1

Study on measuring methods for pore size of polyolefin film coated controlled-release fertilizer

  • 摘要: 【目的】物理包覆法制备的聚合物控释膜层结构直接决定了其养分的释放,控释膜层存在的微孔和裂缝是肥芯养分进出的最主要通道。因此,控释膜层结构特征是决定包膜肥料释放性能的关键因素。泡点法能够准确测定膜的有效孔径及其分布,是一种重要的膜层孔径测试方法。本研究根据包膜肥控释膜层的特点,研究适用于测定聚烯烃包膜控释肥膜层最大孔径的泡点法,并建立测定包膜肥料最大孔径的标准方法。【方法】以泡点法为基础,建立测定膜层最大孔径的装置,确定膜层最大孔径的位置,并利用扫描电镜对膜层的孔隙结构进行观察,确定其形貌结构特征;通过对浸润剂种类、 浸润时间、 浸润温度等测定因素的比较分析,确定适合测定膜层最大孔径的最佳条件;并以释放期分别为1、 3、 5、 6月的聚烯烃包膜肥料为研究对象,研究释放期与最大孔径之间的相关关系。【结果】 1)将4种肥料放入水中浸泡,随浸泡时间的增长,膜层表面有尿素结晶的白色点位的颗粒逐渐增多,浸泡10天,80%以上颗粒均能检测到泡点,其白色点位可被认为是肥芯养分的溶出通道,以颗粒的白色点位作为膜层最大孔径的测定位置;这与扫描电镜观察到的孔隙或孔洞的特征相吻合 ;2)通过对浸润条件研究,认为在25℃,以Q-16为浸润剂,浸润5 min能够使用自制的压泡法装置直接测定控释膜层最大孔径; 3)释放期为46、 105、 160、 198天的包膜肥料的膜层平均孔径分别为1.93、 0.58、 0.45和0.41 m,最大孔径随着释放期的缩短而增大,随着微分溶出率的增加而增大,最大孔径与释放性能存在密切联系。【结论】综上所述,采用塑料管端封装浸泡10天的膜层,以Q-16作为浸润剂,在室温下浸润5 min的条件下可以测定最大孔隙结构,泡点法可作为一种标准方法用于控释膜层最大孔径的测定,其测定的最大孔径与释放期存在相关关系,对包膜控释肥控释性能和养分释放机理的深入认识有重要作用。
    Abstract: 【Objectives】 Structure of controlled-release film of polymer, prepared by physical covering methods, directly determines the mass transfer of nutrients. The main channel for the release of nutrients is the micropores and cracks in the films. Bubble point method is widely employed for measuring the diameter and their distribution of available pores in the films. In this study, the method was modified for the determination of the maximum aperture in the polyolefin films, which is used for coating of fertilizer, and the parameters for establishing a standard method were testified.【Methods】 On the base of the bubble point method, a device for the determination of maximum pore diameter of the film were installed, and the location of maximum aperture in the film was determined. The morphology and structural characteristics of pores on the film was observed by scanning electron microscope. The optimum parameters for the modified method were determined by the comparative analysis of different infiltration agents, temperatures and time. The correlation between the releasing period and the maximum pore was studied using polyolefin coated fertilizer with releasing periods of 1, 3, 5 and 6 months.【Results】 1)After the four types of fertilizers were soaked into water, the granules with urea crystallization of white point in the film surface are gradually increased with the elongation of the soaking. The white points could be thought as the releasing channel of fertilizer core nutrients. The white points of granule are set as the position for the determination of the maximum aperture film. At the 10th day of soaking, the bubble point could be detected in more than 80% of the granules. The characteristics of these pores or holes are matched with those observed by scanning electron microscope. 2)The maximum pores of the film are determined directly by the pressure bubble method with self-made apparatus at temperature of 25℃, Q-16 is selected as wetting agents and soaked for 5 min. 3)The average pore sizes of the coated fertilizer with releasing periods of 46, 105, 160 and 198 d are 1.93, 0.58, 0.45 and 0.41 m, respectively. The maximum pore sizes are increased with the shortening of releasing period and increasing of nutrients. Therefore, a close relationship exists between the maximum pore size and the release performance. 【Conclusions】 The bubble point method can be used as a standard method for the determination of maximum pore diameter, there is relationship between the determination of maximum aperture and the release time, it plays an important role in further understanding the controlled release performance and coated controlled release mechanism of fertilizer.
  • [null] [1] 张海军, 武志杰, 梁文举, 等. 包膜肥料养分控释机理研究进展[J]. 应用生态学报, 2003, 14 (12): 2337-2341.
    Zhang H J, Wu Z J, Liang W J. Research advances on controlled-release mechanisms of nutrients in coated fertilizers[J]. Chinese Journal of Applied Ecology, 2003, 14(12): 2337-2341.
    [2] 卢元东, 王登明. 膜控释药的机理及影响因素[J]. 国外医药—合成药、 生化药、 制剂分册, 1992, 13(5): 296-299.
    Lu Y D, Wang D M. Membrane and influencing factors of the mechanism of controlled release drug[J]. World Pharmacy, 1992, 13 (5): 296-299.
    [3] 杨相东, 曹一平, 江荣风, 等. 雾化状态对控释肥料膜结构和性能的影响[J]. 化工学报, 2008, 59(3): 778-784.
    Yang X D, Cao Y P, Jiang R F, et al. Effect of atomization on membrane structure and characteristics during manufacture of polymer-coated controlled-release fertilizer[J]. Journal of Chemical Industry and Engineering, 2008, 59(3):778-784.
    [4] Jarrell W M, Boersma L. Release of urea by granules of sulfur-coated urea[J]. Soil Science, 1980, 44: 418-422.
    [5] 毛小云, 冯新, 王德汉, 等. 固-液反应包膜尿素的微结构与红外光谱特征及氮素释放特性研究[J]. 中国农业科学, 2004, 37(5): 704-710.
    Mao X Y, Feng X, Wang D H, et al. Study on membrane microstructures and characteristics of infrared spectra and nitrogen release of solid-liquid reaction coated urea[J]. Scientia Agricultura Sinica, 2004, 37(5): 704-710.
    [6] Shaviv A, Raban S, Zaidel E. Modeling controlled nutrient release from polymer coated fertilizer: diffusion release from single granules[J]. Environment Science & Technology, 2003, 37: 2251-2256.
    [7] 王浩, 樊小林, 杜建军, 等.粒径和包膜厚度对控释肥氮素释放特性的影响[J]. 水土保持学报, 2007, 21: 86-89.
    Wang H, Fan X L, Du J J, et al. Effect of granular diameter and coating thickness on characteristics of nitrogen release of controlled release fertilizer[J]. Journal of Soil and Water Conservation, 2007, 21: 86-89.
    [8] 段路路, 张民, 刘刚, 等. 热塑性包膜尿素微观结构特征及养分释放机理研究[J]. 植物营养与肥料学报, 2009, 15(5): 1170-1178.
    Duan L L, Zhang M, Liu G, et al. Membrane microstructures and nutrient release mechanism of thermoplastic coated urea[J]. Plant Nutrition and Fertilizer Science, 2009, 15(5): 1170-1178.
    [9] 徐和昌, 柯以侃, 郭立新, 等. 几种缓释肥料包膜的性质和分析方法[J].中国农业科学, 1995, 28(4): 72-79.
    Xu H C, Ke Y K, Guo L X, et al. Properties and analytic methods of coated membrane of several slow-release fertilizers[J]. Scientia Agricultura Sinica, 1995, 28(4): 72-79.
    [10] Du C, Zhou J, Shaviv A, Wang H. Mathematical model for potassium release from polymer-coated fertilizer[J]. Journal of Soil and Water Conservation, 2004, 88(3): 395-400.
    [11] 李彦举. 基于恒速压汞的孔隙结构特征研究[D]. 北京: 中国地质大学硕士学位论文, 2014.
    Li Y J. Study on pore structure characteristics based on constant-rate mercury injection [D]. Beijing: MS Thesis, China University of Geosciences, 2014.
    [12] 黄培, 徐南平, 时钧. 液体排除法测定多孔陶瓷膜孔径分布[J]. 南京化工大学学报, 1998, 20(3): 45-50.
    Huang P, Xu N P, Shi J. Pore size distribution determination of inorganic membranes by liquid displacement porometry[J]. Journal of Nanjing University of Chemical Technology, 1998, 20(3): 45-50.
    [13] Mulder M (李琳译). 膜技术基本原理[M]. 北京: 清华大学出版社, 1999.
    Marcel M (Translated by Li L). Principle for membrane science and technology[M]. Beijing: Tsinghua University Press, 1999.
    [14] 黄培, 邢卫红, 徐南平, 时均. 气体泡压法测定无机微滤膜孔径分布[J]. 水处理技术, 1996, 22(2): 80-84.
    Huang P, Xing W H, Xu N P, Shi J. Pore size distribution determination of inorganic microfiltration membrane by gas bubble pressure method[J]. Technology of Water Treatment, 1996, 22(2): 80-84.
    [15] Bechhold H, Schlesinger M, Silbereisen K, et al. Pore diameters of untrafilters[J]. Kolloid Z, 1931, 55: 172-198.
    [16] 苗晓杰, 蒋恩臣, 王佳, 等. 对二甲氨基苯甲醛显色分光光度法检测水溶液中常微量尿素[J]. 东北农业大学学报, 2011, (8): 87-92.
    Miao X J, Jiang E C, Wang J, et al. Using spectrophotometry with para-dimethyl-amino-benzaldehyde as chromogenic agent to determine macro and micro urea in aqueous solution[J]. Journal of Northeast Agricultural University, 2011, (8): 87-92.
    [17] 杨相东, 曹一平, 江荣风, 张福锁. 几种包膜控释肥氮素释放特性的评价[J]. 植物营养与肥料学报, 2005, 11(4): 501-507.
    Yang X D, Cao Y P, Jiang R F, Zhang F S. Evaluation of nutrients release feature of coated controlled-release fertilizer[J]. Plant Nutrition and Fertilizer Science, 2005, 11(4): 501-507.
    [18] Kobayashi A, Fujisawa E, Hanyu T. A mechanism of nutrient release from resin-coated fertilizers and its estimation by kinetic methods.III. An improved simulation model for nutrient release from coated urea Gaussian correction[J]. Japanese Journal of Soil Science and Plant Nutrient, 1997, 68:487-492.
    [19] 段路路. 缓控释肥料养分释放机理及评价方法研究[D]. 山东农业大学博士学位论文, 2009.
    Duan L L, Mechanism and evaluation of nutrient release of slow and controlled-release fertilizers [D]. Taian: PhD Dissertation of Shandong Agricultural University, 2009.
    [20] 樊小林, 王浩, 喻建刚. 粒径厚度与控释肥料的氮素养分释放特性[J]. 植物营养与肥料学报, 2005, 11(3): 327-333.
    Fan X L, Wang H, Yu J G. Effect of granule size and coating thickness on nitrogen release characteristics of controlled release fertilizers[J]. Plant Nutrition and Fertilizer Science, 2005, 11(3): 327-333.
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出版历程
  • 收稿日期:  2015-01-18
  • 修回日期:  2016-06-01
  • 刊出日期:  2016-05-24

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