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Method for synthesizing sodium ferric manganese phosphate by treating industrial titanium dioxide by-product

A technology of sodium iron manganese phosphate and titanium dioxide, applied in chemical instruments and methods, phosphorus compounds, structural parts, etc., can solve the problems of inability to monitor the content of various metal ions in real time and difficulties in practical application in enterprises, and achieve good economic benefits , The parameters are easy to control, and the effect with low requirements

Active Publication Date: 2022-05-06
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition to ferrous elements, titanium dioxide by-products also contain a certain amount of impurity elements such as Ti, Mg, Mn, Al, etc. Since the impurity ions in titanium dioxide by-products come from ilmenite, their content often increases with the increase of minerals. The mining area changes, and it is still impossible to monitor the content of various metal ions in the sample in real time at the same time, which leads to difficulties in the actual application of enterprises.

Method used

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  • Method for synthesizing sodium ferric manganese phosphate by treating industrial titanium dioxide by-product
  • Method for synthesizing sodium ferric manganese phosphate by treating industrial titanium dioxide by-product
  • Method for synthesizing sodium ferric manganese phosphate by treating industrial titanium dioxide by-product

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Embodiment 1

[0024] Embodiment 1 of the present invention is: a method for processing industrial titanium dioxide by-products to synthesize sodium iron manganese phosphate, comprising the following steps:

[0025] (1) Weigh 4000g of by-product ferrous sulfate produced in the process of producing titanium dioxide in a certain factory and prepare it into a solution, add deionized water to dissolve to 10L, and add 10% sodium hydroxide solution in a stirrer with a rotating speed of 40r / min , adjust the pH between 4-5, react for 60 min under the condition that the rotating speed is 40 r / min and the temperature is 25 ℃, and filter to obtain the ferrous sulfate solution for preliminary impurity removal;

[0026] (2) Adjust the pH of the filtrate to be 5-5.5 with a concentration of 10% sodium hydroxide solution, measure the concentration of ferrous sulfate to be 399 g / L, take 1 L of the solution, add 59.9 g of sodium sulfide precipitation solution under water bath stirring conditions For impurity ...

Embodiment 2

[0031] The second embodiment of the present invention is: a method for processing industrial titanium dioxide by-products to synthesize sodium iron manganese phosphate, comprising the following steps:

[0032] (1) Weigh 4000g of by-product ferrous sulfate produced in the process of producing titanium dioxide in a certain factory and prepare it into a solution, add deionized water to dissolve to 10L, and add 10% sodium hydroxide solution in a stirrer with a rotating speed of 40r / min , adjust the pH between 4-5, react for 60min under the condition that the rotating speed is 40r / min and the temperature is 35℃, and filter to obtain the ferrous sulfate solution for preliminary impurity removal;

[0033] (2) Adjust the pH of the filtrate to be 5-5.5 with a concentration of 10% sodium hydroxide solution, measure the concentration of ferrous sulfate to be 399 g / L, take 1 L of the solution, add 59.9 g of sodium sulfide precipitation solution under water bath stirring conditions For impur...

Embodiment 3

[0038] The third embodiment of the present invention is: a method for processing industrial titanium dioxide by-products to synthesize sodium iron manganese phosphate, comprising the following steps:

[0039] (1) Weigh 4000g of by-product ferrous sulfate produced in the process of producing titanium dioxide in a certain factory and prepare it into a solution, add deionized water to dissolve to 10L, and add 10% sodium hydroxide solution in a stirrer with a rotating speed of 40r / min , adjust the pH between 4-5, react for 30min under the condition that the rotating speed is 100r / min and the temperature is 25°C, and filter to obtain the ferrous sulfate solution for preliminary impurity removal;

[0040] (2) Adjust the pH of the filtrate to be 5-5.5 with a concentration of 10% sodium hydroxide solution, measure the concentration of ferrous sulfate to be 399 g / L, take 1 L of the solution, add 59.9 g of sodium sulfide precipitation solution under water bath stirring conditions For im...

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Abstract

The invention discloses a process for preparing a sodium ferric manganese phosphate positive electrode material by recovering a titanium dioxide byproduct and purifying a ferrous sulfate solution, and further synthesizing the sodium ferric manganese phosphate positive electrode material, and belongs to the field of titanium dioxide waste liquid treatment and sodium ion batteries, the main component of titanium dioxide is ferrous sulfate heptahydrate, and in addition, the titanium dioxide is mixed with elements such as Ti, Mg, Zn and Cr. The method comprises the following steps: performing precipitation separation and impurity removal treatment on titanium dioxide to remove a large amount of impurity elements, oxidizing a purified ferrous sulfate solution into a mixed solution of ferric sulfate and manganese sulfate by using an oxidant permanganate containing a manganese source, and regulating the pH value of the solution to obtain manganese source and iron source raw materials for synthesizing the sodium ferric manganese phosphate material; and mixing with sodium dihydrogen phosphate, and firing to obtain the positive electrode material.

Description

technical field [0001] The invention relates to the technical field of sodium ion battery materials, in particular to a method for recovering and purifying ferrous sulfate solution from titanium dioxide by-product ferrous sulfate to prepare a raw material of sodium iron manganese phosphate, and then synthesizing a positive electrode material of sodium iron manganese phosphate. Background technique [0002] At present, the most concerned phosphate, pyrophosphate and mixed phosphate cathode materials for sodium ion batteries are: NaMnPO 4 , Na 2 MnP 2 O 7 , NaFe 0.5 Mn 0.5 (PO 4 ) 3 , NaMnFe 2 (PO 4 ) 3 , NaCoPO 4 , Na 3 V 2 (PO 4 ) 3 , Na 7 V 4 (P 2 O 7 ) 4 PO 4 Wait. It has the higher working voltage of manganese-based materials and the cycling stability of phosphate. [0003] Due to the abundant reserves of iron and its low price, iron-based polyanionic materials have great advantages in the pursuit of large-scale production, cost-effective and environ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/45H01M4/58H01M10/054
CPCC01B25/45H01M4/5825H01M10/054C01P2004/03C01P2006/40C01P2006/80
Inventor 明磊王星元欧星张宝
Owner CENT SOUTH UNIV
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