高纯磷铁电硅热法制备影响因素实验研究

林保全; 庞建明; 宋耀欣; 李石稳; 岳锦涛

doi:10.3969/j.issn.1000-6532.2023.02.006

高纯磷铁电硅热法制备影响因素实验研究

1.
钢铁研究总院，北京　100081

2.
中国钢研科技集团有限公司资源应用与合金材料事业部，北京　100081

详细信息

作者简介: 林保全（1997-），男，硕士，研究方向为合金材料制备

通讯作者: 庞建明（1980-），男，博士，正高级工程师。研究方向为合金材料制备

中图分类号: TD985;TD95

收稿日期: 2021-03-03

刊出日期: 2023-04-25

Experimental Research on Influencing Factors of High-purity Ferro-Phosphorus and Silicon Thermal Method

1.
Central Iron & Steel Research Institute, Beijing, China

2.
Resource Application and Alloy Materials Division, China Iron and Steel Research Institute Group, Beijing, China

More Information

Corresponding author: Pang Jianming, .pangjianming198012@163.com

Received Date: 03 March 2021

Publish Date: 25 April 2023

摘要

摘要:
本研究以磷矿石和铁粉为原料，工业硅为还原剂，通过正交实验研究冶炼温度、保温时间、配硅系数对磷铁合金产品中C含量、Ti含量、P含量以及P组分收得率的影响。结果表明：实验所得磷铁合金中C含量均低于0.043%，Ti含量均低于0.036%。各因素对P含量以及P组分收得率的影响程度大小顺序为：配硅系数>冶炼温度>保温时间。电硅热法制备低C低Ti高纯磷铁合金的较佳工艺条件为冶炼温度1390 ℃，保温时间60 min，配硅系数1.2。此条件下磷铁合金成分为C含量0.010%，Ti含量0.036%，P含量27.78%，P组分收得率为96.49%。
- 磷铁合金 /
- 正交实验 /
- 电硅热法 /
- P组分收得率
Abstract:
In this study, phosphate rock and iron powder were used as raw materials, and industrial silicon is used as a reducing agent. Through orthogonal experiments, the effects of smelting temperature, holding time and silicon ratio on the carbon content, titanium content, phosphorus content and the recovery rate of phosphorus in ferro-phosphorus alloy products are studied. The results show that the carbon content in ferro-phosphorus alloys obtained in the experiment is less than 0.043%, and the titanium content is less than 0.036%. The order of the degree of influence of various factors on the phosphorus content and the recovery rate of phosphorus from large to small is: silicon ratio, smelting temperature, holding time. The best process conditions for preparing ferro-phosphorus alloy by electro-silicothermic process are smelting temperature of 1390 ℃, holding time of 60 min, and silicon ratio of 1.2. Under these conditions, the ferro-phosphorus alloy has a carbon content of 0.010%, a titanium content of 0.036%, and a phosphorus content of 27.78%. The recovery rate of phosphorus was 96.49%.
- Phosphorus ferroalloy /
- Orthogonal experiments /
- Electro-silicothermic process /
- Recovery rate of phosphorus

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图 1 反应(1)~(3)的∆G^θ与温度的关系

Figure 1.

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图 2 冶炼温度的影响

Figure 2.

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图 3 保温时间的影响

Figure 3.

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图 4 配硅系数的影响

Figure 4.

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图 5 配硅系数的影响

Figure 5.

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图 6 磷铁合金XRD

Figure 6.

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图 7 较佳工艺条件产物SEM

Figure 7.

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表 1 磷矿主要化学成分/%

Table 1. Main chemical constituents of phosphate ore

P₂O₅	MgO	Fe₂O₃	Al₂O₃	CaO	As*	Cr*
33.61	1.79	1.06	0.64	48.13	27.7	42.08

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表 2 正交实验因素与水平

Table 2. Orthogonal experimental factors and levels

水平	冶炼温度/℃	保温时间/min	配硅系数
1	1360	30	0.7
2	1390	50	0.9
3	1420	60	1.0
4	1450	80	1.2

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表 3 实验合金主要化学成分/%

Table 3. Mainchemical components of test alloy

实验序号	磷铁合金C、Ti、P含量
实验序号	P	C	Ti
1	17.38	0.030	<0.01
2	21.25	0.022	<0.01
3	23.71	0.017	<0.01
4	28.08	0.014	0.027
5	21.81	0.010	<0.005
6	17.95	0.011	<0.005
7	27.78	0.010	0.036
8	23.56	0.017	<0.01
9	23.98	0.017	<0.01
10	27.63	0.043	0.032
11	17.20	0.017	<0.005
12	21.78	0.023	<0.005
13	27.63	0.039	0.033
14	23.44	0.0099	<0.01
15	22.06	0.016	<0.005
16	17.01	0.017	<0.01

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表 4 P含量极差分析

Table 4. Phosphorus content range analysis

	冶炼温度	保温时间	配硅系数
均值1	22.61	22.70	17.39
均值2	22.78	22.57	21.73
均值3	22.65	22.69	23.67
均值4	22.54	22.61	27.78
R	0.24	0.13	10.39

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表 5 正交实验方案及P组分收得率

Table 5. Orthogonal experiment scheme and the recovery rate of phosphorus

序号	冶炼温度/℃	保温时间/min	配硅系数	P收得率/%
1	1360	30	0.7	46.21
2	1360	50	0.9	61.21
3	1360	60	1.0	72.04
4	1360	80	1.2	89.94
5	1390	30	0.9	64.96
6	1390	50	0.7	48.94
7	1390	60	1.2	96.49
8	1390	80	1.0	76.12
9	1420	30	1.0	70.35
10	1420	50	1.2	94.74
11	1420	60	0.7	49.62
12	1420	80	0.9	67.38
13	1450	30	1.2	94.42
14	1450	50	1.0	74.76
15	1450	60	0.9	63.31
16	1450	80	0.7	48.01
K₁	269.40	275.94	192.78
K₂	286.51	279.65	256.86
K₃	282.09	281.46	293.27
K₄	280.50	281.45	375.59
均值k₁	67.35	68.99	48.20
均值k₂	71.63	69.91	64.22
均值k₃	70.52	70.37	73.32
均值k₄	70.13	70.36	93.90
R	4.24	1.42	45.74

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