六氟磷酸锂副产含氟盐酸连续脱氟技术的开发与实践

doi:10.19964/j.issn.1006-4990.2023-0052

Abstract

Abstract:

Fluorinated hydrochloric acid is a by-product of lithium hexafluorophosphate，and the removal of fluorine is the key to its recycling. Based on the analysis of the problems and shortcomings of the batch defluoridation process，a continuous defluoridation technology was proposed to remove fluorine from fluorinated hydrochloric acid. Continuous defluoridation technology significantly improved the automation，quality，capacity，and environmental management of the defluoridation process.As a result，the fluoride content in HCl was decreased from 55 g/L to 11 g/L，the production capacity was enhanced by 118%，the labor efficiency per capita was improved by 337%，the particle size of calcium fluoride was increased by about 30%，the solid waste emission was reduced by 52%，and the tail gas emission reached the ultra-low emission standard（fluoride content ≤3 mg/m³ and particulate matter content ≤10 mg/m³）.

Key words: lithium hexafluorophosphate, fluorinated hydrochloric acid, defluoridation technology, recycle of calcium fluoride, drying machine

CLC Number:

TQ131.1

ZHOU Xiaoping, FENG Haoshou, ZHANG Guohui, HOU Shilei, ZHANG Shuaipeng, LIU Lixia. Development and practice of continuous defluoridation technology for by-products fluorinated hydrochloric acid of lithium hexafluorophosphate[J]. Inorganic Chemicals Industry, 2023, 55(11): 93-99.

Figures/Tables 17

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样品编号	样品	HCl质量分数%	氟质量浓度/（g·L^-1）	磷质量浓度/（g·L^-1）
202301010	含氟盐酸	38.56	62.20	4.13
202301018	含氟盐酸	37.04	54.88	4.44
202301014	含氟盐酸	37.19	56.34	3.96
202301020	含氟盐酸	37.65	54.88	4.99
202301028	含氟盐酸	38.26	54.88	5.02
202301024	含氟盐酸	37.84	53.55	4.68
202301030	含氟盐酸	37.95	54.15	5.78
202301038	含氟盐酸	38.26	51.59	5.91
202301034	含氟盐酸	37.95	53.42	5.35
202301040	含氟盐酸	38.10	52.69	4.64

批次号	过滤压力/MPa	洗饼介质	洗水用量/m³	水洗时间/min	洗涤滤饼后的洗水	压榨压力/MPa	压榨时间/min	气吹压力/MPa	气吹时间/min	备注
202202231	0.65	一次水	0.60	77	—	2.0	17	0.5	2	滤饼165 kg； w（水）=38.75%
202202232	0.70	一次水	0.16	15	—	1.2	9	0.5	2	滤饼191 kg； w（水）=33.29%
202202233	0.70	一次水	0.12	13	—	1.2	9	0.5	2	滤饼190 kg； w（水）=33.75%
202202241	0.70	一次水	0.40	79	ρ（Cl^-）=30.86 g/L ρ（Ca²⁺）=17.88 g/L	1.2	8	0.5	2	滤饼169 kg； w（水）=39.19%
202202242	0.70	一次水	0.60	132	ρ（Cl^-）=16.96 g/L ρ（Ca²⁺）=24.24 g/L	1.2	7	0.5	2	滤饼215 kg； w（水）=40.93%
202202251	0.65	—	—	—	—	2.0	15	0.5	2	滤饼215 kg； w（水）=30.51%
202202261	0.70	—	—	—	—	2.0	12	0.5	2	滤饼176.9 kg； w（水）=31.14%
202202262	0.70	一次水	0.20	42	ρ（Cl^-）=71.45 g/L ρ（Ca²⁺）=40.80 g/L	1.6	16	0.5	2	滤饼77.1 kg； w（水）=37.28%

批次	湿滤饼	进料量/ kg	进料含水率/%	出料含水率/%	干燥时间/min	切条机频率/Hz	上网带频率/Hz	下网带频率/Hz
202202231	3倍水洗；2 MPa压榨	165	38.75	7.34	41	22	12	10
202202232	1倍水洗；1.2 MPa压榨	191	33.29	25	41	22	12	10
202202233	1倍水洗；1.2 MPa压榨	190	33.75	20~28	44	20	12.8	8.9
202202241	2倍水洗；1.2 MPa压榨	169	39.19	11.7~26.8	43	24	14.5	9.9
202202242	3倍水洗；1.2 MPa压榨	215	40.93	7.8~10.1	49	24	12.8	8
202202251	未水洗；2 MPa压榨	215	30.51	16.2~27.4	48	24	12.8	8
202202261	未水洗；2 MPa压榨	176.9	31.14	10.7~21.5	87	24	12.8	8
202202262	1倍水洗；1.6 MPa压榨	77.1	37.28	11.5~28.5	89	24	15.1	7.2

编号	样品	w（HCl）%	ρ（F ^- ）/（g·L^-1）
202301010	脱氟盐酸	26.64	13.46
202301018	脱氟盐酸	25.96	9.51
202301014	脱氟盐酸	26.19	9.51
202301020	脱氟盐酸	26.33	10.24
202301028	脱氟盐酸	26.13	10.24
202301024	脱氟盐酸	26.49	12.44
202301030	脱氟盐酸	26.10	13.17
202301038	脱氟盐酸	26.21	11.71
202301034	脱氟盐酸	25.92	10.25
202301040	脱氟盐酸	26.17	10.98

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Development and practice of continuous defluoridation technology for by-products fluorinated hydrochloric acid of lithium hexafluorophosphate

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