论文部分内容阅读
目的:以炮制品得率及残渣质量,粒径分布,As2S2和As2O3的含量为指标,考察不同炮制方法对纳米雄黄的影响,筛选其最佳炮制方法。方法:采用高能球磨法制备纳米雄黄生品,利用水飞法、酸水飞法和碱水飞法对其进行炮制,计算各炮制品得率及残渣质量;利用激光散射法测定粉体粒径,电镜扫描法观察粉体的表观形貌;直接碘量法和二乙基二硫代氨基甲酸银法(Ag-DDC法)分别测定各样品中As2S2与As2O3的含量。结果:水飞品、酸水飞品和碱水飞品的得率分别为96.71%,95.86%,79.08%,残渣质量分别为0.328,0.891,2.208 g;生品及各炮制品的平均粒径分别为(157.3±4.8),(143.9±6.2),(137.7±4.5),(139.8±5.3)nm;As2S2质量分数分别为(94.26±1.33)%,(98.97±0.98)%,(99.58±1.45)%,(99.37±2.60)%,As2O3质量分数分别为(9.64±0.68),(3.44±0.29),(2.83±0.27),(18.17±1.70)mg·g-1。结论:3种炮制方法均能减小纳米雄黄生品的粉体粒径,提高其As2S2的含量,且水飞法和酸水飞法均可降低其As2O3的含量。确定最佳炮制方法为酸水飞法。
OBJECTIVE: To investigate the effects of different processing methods on realgar nano-particles with the yield and residue quality, particle size distribution, As2S2 and As2O3 contents of the processed products as indexes, and to find out the best processing method. Methods: Nano-realgar was prepared by high-energy ball milling method. The products were processed by water-fly method, acid-water method and alkali-water method to calculate the yield and residue quality of the products. Laser particle scattering , And the morphology of the powder was observed by scanning electron microscopy. The content of As2S2 and As2O3 in each sample were determined by direct iodine method and silver diethyldithiocarbamate method (Ag-DDC method). Results: The yield of waterfly, sour water and alkaline waterflight products were 96.71%, 95.86%, 79.08% respectively, and the residues were 0.328,0.891,2.208g respectively. The average particle sizes of raw products and processed products were Were (157.3 ± 4.8), (143.9 ± 6.2), (137.7 ± 4.5) and (139.8 ± 5.3) nm, respectively. The contents of As2S2 were (94.26 ± 1.33)%, (98.97 ± 0.98)%, (99.58 ± 1.45 ), (99.37 ± 2.60)%, and As2O3 mass fractions were (9.64 ± 0.68), (3.44 ± 0.29), (2.83 ± 0.27) and (18.17 ± 1.70) mg · g-1, respectively. CONCLUSION: All the three processing methods can reduce the particle size of nano-realgar and increase the content of As2S2, and both As2O3 and As2O3 can reduce the content of As2O3. Determine the best method for processing sour water method.