响应面优化浮选磷尾矿制备陶粒及其对磷的吸附研究

doi:10.19964/j.issn.1006-4990.2024-0532

摘要/Abstract

摘要：

浮选磷尾矿是在磷矿浮选阶段产生的固体废物，尾矿中含有钙、镁、硅、铁、铝等有价元素，具有可资源化利用的潜力。为提高磷尾矿的资源化利用率，以湖北某化工厂的正选磷尾矿、反选磷尾矿为主要原料，辅以蒙脱石为黏结剂，经研磨、造粒、烘干和焙烧等工序制备成型吸附材料，即浮选磷尾矿陶粒。采用单因素实验并基于Box-Behnken Design模型对陶粒制备工艺进行优化，设定反选磷尾矿添加量、预热温度、焙烧温度和焙烧时间为影响因素，磷吸附率为响应值，探究各影响因素之间对磷吸附率的影响。结果表明，最佳陶粒制备工艺条件为反选磷尾矿添加量为54%（质量分数）、预热温度为401 ℃、焙烧温度为950 ℃、焙烧时间为59 min，该条件下磷吸附率为99.60%。采用XRF、XRD、SEM、EDS和BET等对陶粒进行表征分析，探究其对磷的吸附原理，该研究为磷尾矿的资源化利用提供理论依据。

关键词: 浮选磷尾矿, 响应面优化, 陶粒, 吸附除磷

Abstract:

Flotation of phosphate tailings is a solid waste generated during the flotation stage of phosphate ore.The tailings contain valuable elements such as calcium，magnesium，silicon，iron，and aluminum which have the potential for resource utilization.In order to improve the resource utilization rate of phosphate tailings，flotation phosphate tailings ceramic particles were prepared by grinding，granulation，drying，and calcination processes using primary and secondary phosphate tailings from a chemical plant in Hubei Province as the main raw materials，supplemented by montmorillonite as the binder.Single factor experiments were conducted and the Box-Behnken Design model was used to optimize the preparation process of ceramic particles.The addition amount of reverse selected phosphorus tailings，preheating temperature，roasting temperature，and roasting time were set as influencing factors，and the phosphorus adsorption rate was the response value.The influence of each influencing factor on the phosphorus adsorption rate was explored.The results showed that the optimal preparation process conditions for ceramic particles were 54% addition of reverse selected phosphorus tailings，preheating temperature of 401 ℃，roasting temperature of 950 ℃，and roasting time of 59 min.Under these conditions，the phosphorus adsorption rate was 99.60%.The ceramic particles were characterized and analyzed by using XRF，XRD，SEM，EDS，BET to explore their adsorption principle for phosphorus.This study provided a theoretical basis for the resource utilization of phosphate tailings.

Key words: phosphorus tailings, response surface, ceramsite, adsorption phosphorus removal

中图分类号:

TQ985

侯代文, 梁欢, 邢丽静, 刘海, 张华丽, 田承涛, 石通杉. 响应面优化浮选磷尾矿制备陶粒及其对磷的吸附研究[J]. 无机盐工业, 2025, 57(11): 74-82.

HOU Daiwen, LIANG Huan, XING Lijing, LIU Hai, ZHANG Huali, TIAN Chengtao, SHI Tongshan. Study on preparation and phosphorus adsorption of phosphate tailings ceramic particles by response surface method[J]. Inorganic Chemicals Industry, 2025, 57(11): 74-82.

图/表 14

表 1

图1

表2

表 3

表 4

表5

表 6

表 7

图2

表8

图3

图4

表9

图5

参考文献 15

[1]	王文浩，王春连，王连训，等.中国磷矿成因类型、成矿规律及重点找矿方向［J］.中国地质，2025，52（1）：43-60.
	WANG Wenhao， WANG Chunlian， WANG Lianxun，et al.Origin types，metallogenic regularity and prospecting direction of phosphate deposits in China［J］.Geology in China，2025，52（1）：43-60.
[2]	苗俊艳，齐帅亮，侯翠红，等.磷矿资源绿色全量利用技术研究现状及突破思路［J］.化学与生物工程，2024，41（5）：1-8.
	MIAO Junyan， QI Shuailiang， HOU Cuihong，et al.Research status and breakthrough ideas of green full utilization technology of phosphate ore resources［J］.Chemistry & Bioengineering，2024，41（5）：1-8.
[3]	张立，张晋，张朝宏，等.轻质多孔陶粒的制备及其磷吸附性能研究［J］.非金属矿，2024，47（2）：80-84.
	ZHANG Li， ZHANG Jin， ZHANG Chaohong，et al.Research on preparation of light porous ceramsites and their phosphate adsorption properties［J］.Non-Metallic Mines，2024，47（2）：80-84.
[4]	邢丽静，梁欢，田承涛，等.白云石质磷尾矿制备多孔陶粒对含磷废水吸附特性研究［J］.水处理技术，2023，49（12）：101-107，131.
	XING Lijing， LIANG Huan， TIAN Chengtao，et al.Study on the adsorption characteristics of porous ceramsite prepared from dolomitic phosphorus tailings for phosphorous wastewater［J］.Technology of Water Treatment，2023，49（12）：101-107，131.
[5]	李沧，程霄智，矫辰，等.赤泥-钢渣基免烧陶粒的制备及除磷特性研究［J］.水处理技术，2024，50（10）：38-43.
	LI Cang， CHENG Xiaozhi， JIAO Chen，et al.Study on preparation and phosphorus removal characteristics of red mud and steel slag based non-sintered ceramsite［J］.Technology of Water Treatment，2024，50（10）：38-43.
[6]	唐婧，罗胜元.碱浸和污泥强化对钢渣陶粒除磷效果的影响［J］.钢铁钒钛，2024，45（1）：96-103.
	TANG Jing， LUO Shengyuan.Effect of alkali leaching and sludge strengthening on phosphorus removal of steel slag ceramics［J］.Iron Steel Vanadium Titanium，2024，45（1）：96-103.
[7]	LV Na， LI Xiufen， QI Xiguang，et al.Calcium-modified granular attapulgite removed phosphorus from synthetic wastewater containing low-strength phosphorus［J］.Chemosphere，2022，296：133898.
[8]	冯宇博，梁欢，田承涛，等.La₂O₃负载非金属矿物基陶粒制备及其除磷性能研究［J］.环境污染与防治，2023，45（9）：1218-1222，1228.
	FENG Yubo， LIANG Huan， TIAN Chengtao，et al.Preparation of La₂O₃ loaded non-metallic mineral based ceramsite and its phosphorus removal performance［J］.Environmental Pollution & Control，2023，45（9）：1218-1222，1228.
[9]	EDWARDS D J， MEE R W.Fractional Box-Behnken designs for one-step response surface methodology［J］.Journal of Quality Technology，2011，43（4）：288-306.
[10]	RAHMATABADI D， SOLTANMOHAMMADI K， PAHLAVANI M，et al.Shape memory performance assessment of FDM 3D printed PLA-TPU composites by Box-Behnken response surface methodology［J］.The International Journal of Advanced Manufacturing Technology，2023，127（1）：935-950.
[11]	章聪华，颜文斌，肖佳俊，等.响应面法优化酒石酸还原浸出电解锰阳极渣工艺［J］.无机盐工业，2023，55（9）：106-113.
	ZHANG Conghua， YAN Wenbin， XIAO Jiajun，et al.Reductive leaching technology of manganese anode slag using tartaric acid as reducing agent optimized by RSM［J］.Inorganic Chemicals Industry，2023，55（9）：106-113.
[12]	石成龙，马淑清，秦亚茹，等.响应面法优化磷酸三丁酯-丁酸乙酯体系协同提锂工艺研究［J］.无机盐工业，2022，54（10）：37-41.
	SHI Chenglong， MA Shuqing， QIN Yaru，et al.Study on optimization of synergistic lithium extraction process of tributyl phospha-te-ethyl butyrate system by response surface method［J］.Inorganic Chemicals Industry，2022，54（10）：37-41.
[13]	李亚娇，赵艺伟，鞠恺，等.基于响应面法的粉煤灰氨含量测定过程浸提条件优化研究［J］.无机盐工业，2022，54（4）：145-151.
	LI Yajiao， ZHAO Yiwei， JU Kai，et al.Study on optimization of extraction conditions in process of determination of ammonia content in fly ash based on response surface method［J］.Inorganic Chemicals Industry，2022，54（4）：145-151.
[14]	方伟成，程星星，孙常荣.响应曲面法优化污泥/粉煤灰复合陶粒滤料的制备［J］.无机盐工业，2022，54（9）：119-125， 142.
	FANG Weicheng， CHENG Xingxing， SUN Changrong.Optimization of preparation of sludge/fly ash composite ceramsite filler materials by response surface methodology［J］.Inorganic Chemicals Industry，2022，54（9）：119-125，142.
[15]	侯黎爽，谷守玉，侯翠红，等.响应面法优化焦磷酸钠螯合锌的制备工艺研究［J］.无机盐工业，2020，52（7）：30-35，93.
	HOU Lishuang， GU Shouyu， HOU Cuihong，et al.Optimization of preparation process of sodium pyrophosphate chelates zinc by response surface analysis［J］.Inorganic Chemicals Industry，2020，52（7）：30-35，93.

编号	反选磷尾矿添加量/%	孔隙率/%	堆积密度/ （g·cm^-3）	抗压强度/MPa	磷的吸附率/%
FPTC-1	0	55.02	0.816	2.85	39.40
FPTC-2	20	56.60	0.753	2.51	59.70
FPTC-3	40	59.98	0.648	2.13	98.20
FPTC-4	60	61.30	0.625	2.11	98.60
FPTC-5	80	61.91	0.614	0.75	90.00

编号	焙烧温度/℃	孔隙率/ %	堆积密度/ （g·cm^-3）	抗压强度/MPa	磷的吸附率/%
FPTC-6	450	59.67	0.824	1.25	57.00
FPTC-7	650	59.97	0.815	1.49	68.40
FPTC-8	850	62.25	0.723	1.79	91.46
FPTC-9	950	62.75	0.758	2.13	98.80
FPTC-10	1 050	55.01	0.952	2.16	97.56

编号	焙烧时间/min	孔隙率/ %	堆积密度/ （g·cm^-3）	抗压强度/MPa	磷的吸附率/%
FPTC-11	30	62.49	0.602	1.59	98.60
FPTC-12	60	60.12	0.646	2.13	98.12
FPTC-13	90	60.31	0.687	2.15	98.72
FPTC-14	120	59.99	0.725	2.18	98.80

方差来源	平方和	自由度	均方	F值	P值	显著性
模型	252.17	14	18.01	117.85	<0.000 1	♣♣
A	145.74	1	145.74	953.57	<0.000 1	♣♣
B	0.001 4	1	0.001 4	0.008 8	0.953 7
C	0.54	1	0.54	3.55	0.080 7
D	7.41	1	7.41	50.87	<0.000 1	♣♣
AB	0.12	1	0.12	0.76	0.399 1
AC	0.24	1	0.24	1.54	0.235 1
AD	0.06	1	0.06	0.39	0.541 0
BC	0.012	1	0.012	0.079	0.782 5
BD	0.11	1	0.11	0.71	0.412 8
CD	0.58	1	0.58	3.78	0.072 3
A²	83.56	1	83.56	546.72	<0.000 1	♣♣
B²	0.51	1	0.51	3.31	0.090 4
C²	25.25	1	25.25	165.19	<0.000 1	♣♣
D²	3.80	1	3.80	24.86	0.000 2	♣♣
残差	2.14	14	0.15
失拟项	2.14	10	0.21
纯误差	0	4	0
总和	254.31	28
相关系数	0.950 9
决定相关系数	0.983 2

首页

全国无机盐信息中心

中国化工学会

无机酸碱盐专业委员会