水相法制备双乙二酸硼酸锂的中试工艺研究

doi:10.11962/1006-4990.2019-0605

Abstract

Abstract:

The double oxalate lithium borate（LiBOB） was prepared by aqueous-phase method.The effect of material ratio,reaction temperature,reaction time and amount of crystallization solvent on the product quality under the condition of pilot test was studied.The result of products was confirmed by FTIR,TG-DSC and XRD.The pilot plant had achieved a production scale of 10 t/a at present.The experimental results showed the optimum operating parameters which were material ratio（the amount-of-substance ratio of oxalic acid to lithium carbonate to boric acid） of 4∶2∶1.1,reaction temperature of 80 ℃,reaction time of 8 h,the concentration amount（the mass ratio of residual solvent to total solvent mass） of about 80% in the process of concentration and crystallization,and the addition amount of crystallization agent of 4 times of the product mass.The dynamic drying was adopted for 8 h.After analysis,the quality of the product prepared by this process exceeded the level of the market products.

Key words: double oxalate lithium borate, aqueous-phase method, crystallization agent

CLC Number:

TQ131.11

Liu Yanrui,Song Congcong,Shi Guizhen,Wang Kun. The study of double oxalate lithium borate preparation technology by aqueous phase method[J]. Inorganic Chemicals Industry, 2020, 52(10): 100-105.

Figures/Tables 18

References 11

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温度/℃	溶解度/g	温度/℃	溶解度/g
10	6.08	60	44.5
30	14.3	70	65.0
40	21.5	80	84.5
50	31.4	90	119.8

温度/℃	溶解度/g	温度/℃	溶解度/g
10	3.57	60	14.51
20	5.04	70	16.73
30	6.60	80	23.75
40	8.72	90	30.38
50	11.54	100	40.25

氧化剂Y加入量（氧化剂与产品质量比）	纯度/ %	Cl含量/ （mg·kg^-1）	色度/ APHA	浊度/NTU	SO₄^2-含量/ （mg·kg^-1）
1/2 000	99.32	1	80	2	0.2
1/1 500	99.50	1	80	2	0.2
1/1 000	99.79	1	15	2	0.2
1/800	99.10	22	15	2	19.0

项目	名称	单价/ （万元·t^-1）	所需用量/ t	成本/ 万元
原材料	二水草酸	0.48	1.30	0.62
	碳酸锂	6.00	0.21	1.26
	硼酸	0.42	0.32	0.14
	LY07	1.00	10（损耗1 t）	1.00
	LY05	0.80	5（损耗0.5 t）	0.40
直接人工费用（7人）				7.00
制造费用	辅材			0.50
	设备折旧			0.50
	电			0.80
	维修			0.30
	液氮			0.80
总成本				13.32

λ/cm^-1	振动类型	λ/cm^-1	振动类型
1 813.75、 1 777.00	C=O的离域或定域震动	1 016.30	O—B—O的伸缩振动
1 747.80	C=O的伸缩振动	983.21、956.43	O—B—O的不伸缩振动
1 638.87	COO—的不对称伸缩振动	709.82	COO—的变形振动
1 441.73	COO—的对称伸缩振动	617.15	B—O的变形振动
1 365.56	B—O的伸缩振动	478.92	BO₄键的振动
1 304.81	C—O—B—O—C的伸缩振动

National Inorganic Salts Information Center

Inorganic Acid-Base-Salt Committee of CIESC

The study of double oxalate lithium borate preparation technology by aqueous phase method

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批次	二水草酸投料量/kg	硼酸投料量/kg	碳酸锂投料量/kg	理论产量/kg	实际产量/kg	产品收率/%
QLC-1	100	24.5	16.11	76.94	75.40	98.0
QLC-2	100	24.5	16.11	76.94	75.30	97.8
QLC-3	100	24.5	16.11	76.94	75.36	97.9
QLC-4	100	24.5	16.11	76.94	75.42	97.9
QLC-5	100	24.5	16.11	76.94	75.30	97.9
QLC-6	100	24.5	16.11	76.94	75.48	98.1
QLC-7	100	24.5	16.11	76.94	76.02	98.8
QLC-8	100	24.5	16.11	76.94	75.41	98.0
QLC-9	100	24.5	16.11	76.94	75.35	97.9
QLC-10	100	24.5	16.11	76.94	75.29	97.8

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批号	纯度/ %	H₂O含量/ （mg·kg^-1）	色度/ APHA	浊度/ NTU	Ca含量/ （mg·kg^-1）	Fe含量/ （mg·kg^-1）
生产产品	99.79	16	15	2	0.2	1.2
市售产品	99.17	53	15	2	3.1	5.4