Method for recycling mother liquor during production of iron phosphate

A production process, iron phosphate master technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve environmental pollution, waste and other problems, reduce production costs, reduce investment and operating costs, and avoid waste of resources Effect

Active Publication Date: 2017-12-08
CENT SOUTH UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to provide a method for recycling mother liquor in the production process of ferric phosphate, so as to solve the technical probl...

Method used

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  • Method for recycling mother liquor during production of iron phosphate
  • Method for recycling mother liquor during production of iron phosphate
  • Method for recycling mother liquor during production of iron phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] see figure 1 The process shown produces an iron phosphate product. The ferric phosphate reaction raw material solution and H 2 o 2 Add to the reaction kettle to carry out the synthesis reaction, and the raw material solution of the ferric phosphate reaction is made of NH 4 h 2 PO 4 , FeSO 4 、H 3 PO 4 Composition, the concentration of each component in the reaction raw material liquid is as follows: NH 4 h 2 PO 4 The mass concentration is 5.3%, FeSO 4 The mass concentration is 7.0%, H 3 PO 4 The mass concentration is 0.6%. H involved in the synthesis reaction 2 o 2 The mass concentration is 0.8%. The temperature of the synthesis reaction was controlled to be 80°C.

[0040] After slurry press filtration, the phosphorus concentration in the mother liquor was 9.8g / L, and the ammonia nitrogen concentration was 8g / L.

[0041] To FeSO with a volume of 50L and a concentration of 260g / L 4 Add volume 14.7L, concentration 27% H to the solution 2 o 2 And volume...

Embodiment 2

[0048] The difference with Example 1 is that the concentration of each component in the reaction raw material liquid is as follows: NH 4 h 2 PO 4 The mass concentration is 7.6%, FeSO 4 The mass concentration is 10.0%, H 3 PO 4 The mass concentration is 0.8%. H involved in the synthesis reaction 2 o 2 The mass concentration is 1.1%. The temperature of the synthesis reaction was controlled to be 90°C.

[0049] H in the oxidation reaction 2 o 2 with FeSO 4 The molar ratio is 1.2:1, and the pH of the first reaction is 3. During the stripping process, lime slurry was added to adjust the pH of the mixed filtrate to 11.

[0050] After flash drying and calcination, 1050g of qualified ferric phosphate product was prepared from 800L mother liquor, and the recovery rate of phosphorus was 95%; 4 h 2 PO 4 (converted into a dry weight of 48kg), the recovery rate of ammonia nitrogen reaches 90%, and the recovery and utilization of phosphorus and ammonium in the mother liquor a...

Embodiment 3

[0052] The difference from Example 1 is that in the oxidation reaction H 2 SO 4 with FeSO 4 The molar ratio is 1:20, the reaction temperature is 40°C, and the reaction time is 90min. Fe in the raw material liquid of the oxidation reaction and H in the mother liquid 3 PO 4 The molar ratio is 1.2:1, and the reaction pH is 4.

[0053] The first press filter cake, H 2 O and H 3 PO 4 The mass ratio of the second reaction is 0.5:10:0.33, and the second reaction temperature is 80°C. Use 2.5mol / L phosphoric acid to absorb the blown out ammonia gas.

[0054] After flash drying and calcination, 1060g of qualified ferric phosphate product was prepared from 800L mother liquor, and the recovery rate of phosphorus was 96%. 4 h 2 PO 4 (converted into dry weight 51kg), the recovery rate of ammonia nitrogen reaches 96%, and the recovery and utilization of phosphorus and ammonium in the mother liquor are realized.

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Abstract

The invention discloses a method for recycling a mother liquor during the production of iron phosphate. The method comprises the following steps: firstly, adding iron phosphate reaction raw material liquid and H2O2 into a reaction kettle to synthesize iron phosphate; performing synthesis reaction and slurry pressing and filtration to obtain slurry and mother liquor of iron phosphate; then recovering phosphorus and ammonium in the mother liquor in the form of iron phosphate filter cakes and monoammonium phosphate solution, respectively; reusing all the recovered materials in an iron phosphate synthesizing step. The method provided by the invention regenerates and recycles the mother liquor generated during the preparation of iron phosphate, can make full use of residual nitrogen, phosphorus and other useful components in the mother liquor, avoids waste of resources, and greatly reduces comprehensives cost and matched environmental protection costs for the production of iron phosphate.

Description

technical field [0001] The invention belongs to the technical field of preparation of new energy materials, and in particular relates to a method for recycling mother liquor in the production process of ferric phosphate. Background technique [0002] With the development of the times and the advancement of science and technology, human beings have an increasing demand for new energy materials. Among them, lithium-ion batteries have been widely used in various mobile communication devices and vehicles due to their advantages such as high voltage, high energy density, good cycle performance, and good high-temperature characteristics. At present, iron phosphate is mainly used as the cathode material of lithium-ion batteries. The traditional preparation process of iron phosphate mainly includes co-precipitation method, hydrothermal method, etc., among which co-precipitation method is widely used. [0003] The co-precipitation method refers to dissolving the iron source and pho...

Claims

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Application Information

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IPC IPC(8): C01B25/37
CPCC01B25/375C01P2002/72
Inventor 周康根彭长宏何德文陈伟杨有才高峰彭佳乐姜科
Owner CENT SOUTH UNIV
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