CN102030323A - Preparation method of iron phosphate - Google Patents
Preparation method of iron phosphate Download PDFInfo
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- CN102030323A CN102030323A CN 201010565462 CN201010565462A CN102030323A CN 102030323 A CN102030323 A CN 102030323A CN 201010565462 CN201010565462 CN 201010565462 CN 201010565462 A CN201010565462 A CN 201010565462A CN 102030323 A CN102030323 A CN 102030323A
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Abstract
The invention relates to a preparation method of iron phosphate, which comprises the following steps: adopting iron sulfate and phosphoric acid as raw materials and oxydol as an oxide to be subject to complete oxidation, and adding sodium hydroxide to perform a reaction so as to obtain the iron phosphate. By adding excessive sodium hydroxide, iron in the solution can be subject to a basically complete reaction, thereby improving the utilization ratio of the raw material iron sulfate. The iron recovery rate of the product is up to 99.0%, and the product purity is up to 93%.
Description
Technical field
The invention belongs to chemical technology field, be specifically related to a kind of method for preparing tertiary iron phosphate.
Background technology
Tertiary iron phosphate is a kind of broad-spectrum industrial chemicals, can be used as the thickening material of food and mends chalybeate, can also be used for metal glaze colour glazes such as pigment, pottery.In recent years, tertiary iron phosphate as the raw material of producing lithium ion battery anode material lithium iron phosphate, has important utility value again.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method of ferric phosphate.
The object of the present invention is achieved like this: a kind of preparation method of ferric phosphate may further comprise the steps:
A. ferric sulfate is added water and dissolve, obtain ferric sulfate aqueous solution in stirred in water bath;
B. in ferric sulfate aqueous solution, add phosphoric acid and stirring;
C. add hydrogen peroxide and stirring in the solution after adding phosphoric acid;
D. slowly add sodium hydroxide and stirring in the solution after adding hydrogen peroxide;
E. the solution stirring of d step after a few hours, is filtered, will promptly get tertiary iron phosphate after the filter residue oven dry, filtrate can be returned a step, adds the ferric sulfate of equivalent and an amount of water, dissolves in stirred in water bath, repeats b again to the e step.
The temperature of water-bath is between 50 ℃ to 90 ℃ in the described a step.
The consumption mol ratio of phosphoric acid and tertiary iron phosphate is 1-7:1 in the described b step.
The consumption mol ratio of described c step hydrogen peroxide and tertiary iron phosphate is 1:1-4.
The consumption mol ratio of described d step sodium hydroxide and tertiary iron phosphate is 1-3:1, and the time of dropping sodium solution is that 0.5h is to 2.5h.
The described e step solution stirring time is that 0.5h is to 2.5h.
The invention has the advantages that to add excessive sodium hydroxide, the iron-based in the solution originally can be reacted completely, improved the utilization ratio of raw material sulphuric acid iron.The rate of recovery of iron reaches 99.0% in the product, and product purity reaches 93%.
Embodiment
The step that the present invention prepares tertiary iron phosphate is as follows:
A. ferric sulfate is added water and dissolve, obtain ferric sulfate aqueous solution in stirred in water bath;
B. in ferric sulfate aqueous solution, add phosphoric acid and stirring;
C. add hydrogen peroxide and stirring in the solution after adding phosphoric acid;
D. slowly add sodium hydroxide and stirring in the solution after adding hydrogen peroxide;
E. the solution stirring of d step after a few hours, is filtered, will promptly get tertiary iron phosphate after the filter residue oven dry, filtrate can be returned a step, adds the ferric sulfate of equivalent and an amount of water, dissolves in stirred in water bath, repeats b again to the e step.
The temperature of water-bath is between 50 ℃ to 90 ℃ in the described a step.
The consumption mol ratio of phosphoric acid and tertiary iron phosphate is 1-7:1 in the described b step.
The consumption mol ratio of described c step hydrogen peroxide and tertiary iron phosphate is 1:1-4.
The consumption mol ratio of described d step sodium hydroxide and tertiary iron phosphate is 1-3:1, and the time of dropping sodium solution is that 0.5h is to 2.5h.
The described e step solution stirring time is that 0.5h is to 2.5h.
Embodiment:
1. 10g seven ferric sulfate hydrates are joined in the 100mL water, in 85 ℃ of following stirring and dissolving of water-bath.
2. in above-mentioned solution, add 15mL phosphoric acid and stirring.
3. in solution, add 5mL hydrogen peroxide and stirring.
4. slowly drip sodium hydroxide solution 100mL and the stirring of 60g/L in solution, the time of dropping sodium solution is 2h, drips back restir 30min.
5. solution is filtered, will promptly get tertiary iron phosphate after the filter residue oven dry.Filtrate can turn back in 1 step and re-use.
6. its iron phosphorus ratio of the tertiary iron phosphate that obtains among the present invention can reach 0.93, and sodium content can be low to moderate 0.03%.
Claims (6)
1. preparation method of ferric phosphate is characterized in that: may further comprise the steps:
A. ferric sulfate is added water and dissolve, obtain ferric sulfate aqueous solution in stirred in water bath;
B. in ferric sulfate aqueous solution, add phosphoric acid and stirring;
C. add hydrogen peroxide and stirring in the solution after adding phosphoric acid;
D. slowly add sodium hydroxide and stirring in the solution after adding hydrogen peroxide;
E. the solution stirring of d step after a few hours, is filtered, will promptly get tertiary iron phosphate after the filter residue oven dry; Filtrate can be returned a step, adds the ferric sulfate of equivalent and an amount of water, in the stirred in water bath dissolving, repeats b again to the e step.
2. a kind of preparation method of ferric phosphate according to claim 1 is characterized in that: the temperature of water-bath is between 50 ℃ to 90 ℃ in the described a step.
3. a kind of preparation method of ferric phosphate according to claim 1 is characterized in that: the consumption mol ratio of phosphoric acid and tertiary iron phosphate is 1-7:1 in the described b step.
4. a kind of preparation method of ferric phosphate according to claim 1 is characterized in that: the consumption mol ratio of described c step hydrogen peroxide and tertiary iron phosphate is 1:1-4.
5. a kind of preparation method of ferric phosphate according to claim 1 is characterized in that: the consumption mol ratio of described d step sodium hydroxide and tertiary iron phosphate is 1-3:1, and the time of dropping sodium solution is that 0.5h is to 2.5h.
6. a kind of preparation method of ferric phosphate according to claim 1 is characterized in that: the described e step solution stirring time is that 0.5h is to 2.5h.
Priority Applications (1)
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CN 201010565462 CN102030323B (en) | 2010-11-30 | 2010-11-30 | Preparation method of iron phosphate |
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CN 201010565462 CN102030323B (en) | 2010-11-30 | 2010-11-30 | Preparation method of iron phosphate |
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CN102030323A true CN102030323A (en) | 2011-04-27 |
CN102030323B CN102030323B (en) | 2012-11-28 |
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CN 201010565462 Active CN102030323B (en) | 2010-11-30 | 2010-11-30 | Preparation method of iron phosphate |
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109081321A (en) * | 2018-10-29 | 2018-12-25 | 北京科技大学 | A kind of method of converter dephosphorization slag preparing phosphoric acid iron |
Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101237042A (en) * | 2008-02-26 | 2008-08-06 | 郑州瑞普生物工程有限公司 | Method for making positive material positive ferric phosphate of lithium battery |
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2010
- 2010-11-30 CN CN 201010565462 patent/CN102030323B/en active Active
Patent Citations (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101237042A (en) * | 2008-02-26 | 2008-08-06 | 郑州瑞普生物工程有限公司 | Method for making positive material positive ferric phosphate of lithium battery |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109081321A (en) * | 2018-10-29 | 2018-12-25 | 北京科技大学 | A kind of method of converter dephosphorization slag preparing phosphoric acid iron |
CN109081321B (en) * | 2018-10-29 | 2020-05-12 | 北京科技大学 | Method for preparing iron phosphate from converter dephosphorized slag |
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CN102030323B (en) | 2012-11-28 |
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