张 哲1，2，肖玮婷2，贺宇飞1，3*，闫子涵4，李殿卿1，3*，赵晓东2
（1. 北京化工大学 化学学院 化工资源有效利用国家重点实验室，北京100029；2. 黎明化工研究设计院有限责任公司，河南 洛阳 471000；3. 衢州资源化工创新研究院，浙江 衢州 324000；4. 中国石油大学 化学工程与环境学院 重质油全国重点实验室，北京 102249）
张哲，肖玮婷，贺宇飞，等. 微球形材料在三相流化时磨损指数的测试方法［J］. 中国粉体技术，2024，30（4）：94-103.
ZHANG Z， XIAO W T， HE Y F， et al. An attrition index test method for microspherical materials in gas-liquid-solid three -phase fluidization［J］. China Powder Science and Technology，2024，30（4）：94−103.
DOI：10.13732/j.issn.1008-5548.2024.04.009
收稿日期：2024-04-02，修回日期：2024-06-14，上线日期：2024-06-27。
基金项目：国家重点研发计划青年科学家项目，编号：2022YFA1506200；国家自然科学基金项目，编号：22078007；河洛青年创新创业人才项目（2022年度）
第一作者简介：张哲（1988—），男，高级工程师，博士生，研究方向为：催化剂研发及产业化，E-mail： zhgzhe@126. com
通信作者简介：
贺宇飞（1988—），男（满族），教授，博士，博士生导师，研究方向为：催化剂反应工程，E-mail： yfhe@mail. buct. edu. cn
李殿卿（1962—），男，教授，博士，博士生导师，研究方向为：无机功能材料与催化新材料，E-mail: lidq@mail.buct.edu.cn
摘要：【目的】 现有微球形材料磨损指数的测试方法均在气固两相中进行，本文建立了一种在三相流化条件下评价微球形材料耐磨性的方法，以更准确测定微球形材料在气液固三相流化时的磨损指数。【方法】 在传统气固两相耐磨性测试基础上，在体系中引入去离子水作为液相，提出并建立了一种在气液固三相体系中的微球形材料耐磨性测试方法；系统研究了样品预筛分、气体流量、样品量、加水量和测试时间等对耐磨性测定结果的影响，探索了微球形材料在气液固三相中的磨损时变规律。【结果】 气体流量对耐磨性测试结果影响最为显著，提高气体流量会使测得的磨损指数增大，且直径小于20 μm的细颗粒会干扰耐磨性测试结果的准确性，应在测试前筛除。使用3批样品开展耐磨性重复测试，相对标准偏差均小于5%。采用Gwyn模型对测试数据进行拟合，实测值与模型的吻合程度良好。【结论】 本文建立的耐磨性测试方法具有较优的准确性和重复性，能够更真实地预测微球形材料在气液固三相流化床中的耐磨性优劣。
Objective The three-phase fluidized bed is extensively employed in chemical industry due to its low mass transfer resistance，uniform temperature distribution， and maximized contact between catalysts and reactants. The attrition resistance of catalysts is a crucial parameter due to the severe collisions between catalyst particles and the inner walls of reactors， as well as among the particles themselves. However， existing attrition resistance tests are typically conducted in gas-solid two-phase environments，and the catalysts are also applied in the similar system. Therefore， designing a new method which simulates a three-phase fluidized bed is both academically and practically significant.
Methods In this paper， deionized water was introduced as the liquid phase to transform the traditional gas-solid two-phase attrition test into a gas-liquid-solid three-phase test. Attrition tests were conducted on pristine samples and samples that were prescreened to remove fines under 20 μm or 45 μm to determine the influence of sample pre-screening on test results. An orthogonal test was designed to evaluate the contributions of gas flow volume （6 to 8 L/min）， sample mass （20. 0 to 30. 0 g）， and water volume （100 to 140 mL） to the attrition index. The combination of levels that resulted in the highest attrition index from the orthogonal test was proposed as the optimal test condition for the new method， and its repeatability was evaluated. Attrition tests with durations ranging from 0. 5 to 2. 5 h were conducted to study the time-profile characteristics of microspherical materials in gas-liquid-solid three-phase fluidization.
Results and Discussion In traditional tests， fines collected in the filtering flask often contain intact microparticles， which are mistakenly calculated as attrited fines， leading to systematical bias. Additionally， fines with diameter below 20 μm in the sample can interfere with attrition test results for the same reason and should therefore be pre-screened. With these improvements， the fines collected in the novel method were solely those generated during the attrition test. The orthogonal test showed the relative significance of different factors in the following order： gas flow volume > sample mass > water volume， with the first factor positively correlated with the result and the last two negatively. The highest attrition index was observed when using 20. 0 g of the sample，100 mL of water， and a gas flow volume of 8. 0 L/min. To evaluate the repeatability of the new attrition test method， three batches of samples were tested， with five parallel experiments for each sample. The relative standard deviation ranged from 3. 48% to 4. 46%， indicating good reliability. Attrition test results over time corresponded well with the Gwyn model， indicating that the attrition mechanism in the three-phase fluidized bed was similar to that in the gas-solid two-phase system.
Conclusion A novel method for evaluating attrition resistance of microspherical materials used in three-phase fluidized beds was established. To more precisely reflect attrition resistance in real three-phase reactors， fines with diameter below 20 μm should be removed. The orthogonal test showed that gas flow volume had the most significant influence on attrition. The repeatability of the test was confirmed， with a relative standard deviation of less than 5%， indicating good reliability. The new method can be used to determine the attrition resistance of different materials used in three-phase reactors， which has important practical applications.
Keywords：microspherical material； attrition resistance； gas-liquid-solid three-phase fluidization
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