Experiment on Production of Silicon Fertilizer from Polyaluminum Chloride Industrial Waste Residue
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摘要:
以聚合氯化铝废渣为原料，采用单因素实验和正交设计研究了焙烧温度、焙烧时间、添加剂配比等因素对聚合氯化铝废渣中二氧化硅活化效果的影响，确定了利用聚合氯化铝废渣生产硅肥的工艺技术条件。结果表明，3个因素对聚合氯化铝废渣焙烧产品的有效硅含量和废渣中硅活化率影响显著性大小为：活化剂用量 > 焙烧温度 > 焙烧时间。其中活化剂用量和焙烧温度对聚合氯化铝废渣焙烧产品中的有效硅含量有明显影响，而焙烧时间对聚合氯化铝废渣焙烧产品中的有效硅含量没有明显影响。随着活化剂用量的增加，所得产品中有效硅含量增加，活化剂用量达到41%以后，有效硅含量趋于稳定，活化剂用量与有效硅含量的相关系数达到0.9829；随着焙烧温度的升高，所得产品中有效硅含量增加，达到1250℃以后，有效硅含量达到峰值；焙烧时间对废渣中有效硅含量和硅活化率的影响不显著。温度为1240 ~ 1270℃、时间为30 ~ 40 min、活化剂用量为41% ~ 45%时，所得产品中有效硅含量较高，达到30%左右。
Abstract:Using polyaluminum chloride residue as raw material, the effects of roasting temperature, roasting time, additive ratio and other factors on the activation effect of silicon dioxide in polyaluminum chloride residue were studied by single factor experiment and orthogonal design, and the technological conditions for producing silicon fertilizer from polyaluminum chloride residue were determined. The results show that the significant influence of three factors effective silicon content and the activation rate of silicon in polyaluminum chloride waste residue is as follows: activator dosage > calcination temperature > calcination time. The amount of activator and calcination temperature have obvious influence on the content of effective silicon in the calcined product, while the calcination time has no obvious influence on the content of effective silicon in the calcined product. With the increase of the amount of activator, the effective silicon content in the product increases. When the amount of activator reaches 41%, the effective silicon content tends to be stable, and the correlation coefficient between the amount of activator and the effective silicon content reaches 0.9829; with the increase of calcination temperature, the effective silicon content in the product increases, and reaches the peak after 1250℃, when the temperature is 1240～1270℃, the time is 30～40 min and the dosage of activator is 41%～45%, the content of effective silicon in the product is the highest, reaching about 30%.
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表 1 废渣主要成分和重金属含量以及相关标准
Table 1. Main components and heavy metal content of waste residue and relevant standards
含量 聚合氯化铝废渣 粉煤灰 硅肥
（NY/T 797-2004）（≥）硅钙钾镁肥
（GB/T 36207-2018）肥料中砷、镉、铅、铬、汞
生态指标GB/T 23349-2009（≤）SiO2/% 43.5~61.1 47.8~53.6 20.0（以SiO2计） ≥9.0（以硅计） CaO/% 1.45~1.54 2.43~7.13 ≥20.0（以钙计） MgO/% 0.79~0.90 0.72~0.97 ≥2.0（以镁计） Al2O3/% 11.5~15.9 28.1~30.5 Fe2O3/% 3.05~3.15 3.37~5.32 K2O/% 1.04~1.55 ≥3.0（以K2O计） Na2O/% 0.60~0.72 Pb/（mg·kg−1） 5.19~6.02 ≤ 200 ≤ 200 200 Cd/（mg·kg−1） 未检出 ≤ 10 ≤ 10 10 Cr/（mg·kg−1） 20.1~30.5 ≤ 500 ≤ 500 500 Hg/（mg·kg−1） 未检出 ≤ 5 ≤ 5 5 As/（mg·kg−1） 未检出 ≤ 50 ≤ 50 50 Cu/（mg·kg−1） 1.38~2.70 Ni/（mg·kg−1） 6.43~8.69 
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表 2 正交实验因素水平L27 (313)
Table 2. Orthogonal experimental factor level L27(313)
水平 因素A
焙烧温度/℃因素B
焙烧时间/min因素C
活化剂用量/%1 1180 20 50.0 2 1240 35 41.2 3 1300 50 33.3
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表 3 正交实验结果
Table 3. Orthogonal experimental results
实验号 A/℃ B/min C/% 有效硅/% 硅活化率/% 1 1 1 1 16.6 54.4 2 1 1 2 17.7 49.8 3 1 1 3 9.3 22.8 4 1 2 1 17.1 56.1 5 1 2 2 19.7 55.2 6 1 2 3 9.4 23.0 7 1 3 1 19.0 62.2 8 1 3 2 20.5 57.5 9 1 3 3 10.6 26.0 10 2 1 1 22.4 73.4 11 2 1 2 24.2 68.0 12 2 1 3 9.7 23.9 13 2 2 1 28.3 92.6 14 2 2 2 30.5 85.4 15 2 2 3 10.9 26.6 16 2 3 1 29.0 95.0 17 2 3 2 31.1 87.2 18 2 3 3 11.2 27.4 19 3 1 1 26.7 87.2 20 3 1 2 30.0 84.0 21 3 1 3 11.6 28.4 22 3 2 1 28.8 94.3 23 3 2 2 30.9 86.8 24 3 2 3 12.4 30.3 25 3 3 1 27.7 90.6 26 3 3 2 31.0 86.9 27 3 3 3 11.6 28.4 ka1 15.6 18.7 24.0 ka2 21.9 20.9 26.2 ka3 23.4 21.3 10.7 Ra1) 7.5 2.6 15..5 kb1 45.2 54.7 78.4 kb2 64.4 61.1 73.4 kb3 68.5 62.4 26.3 Rb2) 23.3 7.7 52.1 1）ka1，ka2，ka3，Ra以有效硅含量为考查指标。2）kb1，kb2，kb3，Rb以硅活化率为考查指标。
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表 4 正交实验模型统计分析结果
Table 4. ANOVA for orthogonal experimental
因素 设计条件 有效硅 /% F P 硅活化率/% F P
焙烧温度/ ℃平均值 标准差 平均值 标准差 1180 15.6 b 4.5 2.659 0.091 45.2 16.3 2.033 0.153 1240 21.9 a 9.0 64.4 30.0 1300 23.4 a 8.8 68.5 29.8 焙烧时间/min 20 18.7 a 7.6 0.251 0.780 54.7 25.3 0.196 0.824 35 20.9 a 8.9 61.1 29.6 50 21.3 a 8.7 62.4 29.2 活化剂用量/% 50.0 24.0 a 5.2 31.3 0.000 78.4 17.0 41.0 0.000 41.2 26.2 a 5.6 73.4 15.7 33.3 10.7 b 1.1 26.3 2.6
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