CN102030323B - Preparation method of iron phosphate - Google Patents
Preparation method of iron phosphate Download PDFInfo
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- CN102030323B CN102030323B CN 201010565462 CN201010565462A CN102030323B CN 102030323 B CN102030323 B CN 102030323B CN 201010565462 CN201010565462 CN 201010565462 CN 201010565462 A CN201010565462 A CN 201010565462A CN 102030323 B CN102030323 B CN 102030323B
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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 and benefit chalybeate of food, 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 objective of the invention is to realize 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 ydrogen peroxide 50 and stirring in the solution after adding phosphoric acid;
D. slowly add sodium hydroxide and stirring in the solution after adding ydrogen peroxide 50;
E. with behind the solution stirring number of d step hour, filter, with promptly get tertiary iron phosphate after the filter residue oven dry, filtrating 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 said a step.
The consumption mol ratio of phosphoric acid and tertiary iron phosphate is 1-7:1 in the said b step.
The consumption mol ratio of said c step ydrogen peroxide 50 and tertiary iron phosphate is 1:1-4.
The consumption mol ratio of said 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 said e step solution stirring time is that 0.5h is to 2.5h.
The invention has the advantages that to add excessive sodium hydroxide, can the iron-based in the solution originally be reacted completely, improved the utilization ratio of raw material sulphuric acid iron.The 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 following:
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 ydrogen peroxide 50 and stirring in the solution after adding phosphoric acid;
D. slowly add sodium hydroxide and stirring in the solution after adding ydrogen peroxide 50;
E. with behind the solution stirring number of d step hour, filter, with promptly get tertiary iron phosphate after the filter residue oven dry, filtrating 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 said a step.
The consumption mol ratio of phosphoric acid and tertiary iron phosphate is 1-7:1 in the said b step.
The consumption mol ratio of said c step ydrogen peroxide 50 and tertiary iron phosphate is 1:1-4.
The consumption mol ratio of said 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 said 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 ydrogen peroxide 50 and stirring.
4. in solution, slowly drip sodium hydroxide solution 100mL and the stirring of 60g/L, the time of dropping sodium solution is 2h, drips back restir 30min.
5. solution is filtered, promptly getting tertiary iron phosphate after the filter residue oven dry.Filtrating 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 (1)
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 ydrogen peroxide 50 and stirring in the solution after adding phosphoric acid;
D. slowly add sodium hydroxide and stirring in the solution after adding ydrogen peroxide 50;
E. with behind the solution stirring number of d step hour, filter, promptly getting tertiary iron phosphate after the filter residue oven dry; Filtrating 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;
The temperature of water-bath is between 50 ℃ to 90 ℃ in the said a step;
The consumption mol ratio of phosphoric acid and ferric sulfate is 1-7:1 in the said b step;
The consumption mol ratio of said c step ydrogen peroxide 50 and ferric sulfate is 1:1-4;
The consumption mol ratio of said d step sodium hydroxide and ferric sulfate is 1-3:1, and the time of dropping sodium solution is that 0.5h is to 2.5h;
The said e step solution stirring time is that 0.5h is to 2.5h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010565462 CN102030323B (en) | 2010-11-30 | 2010-11-30 | Preparation method of iron phosphate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010565462 CN102030323B (en) | 2010-11-30 | 2010-11-30 | Preparation method of iron phosphate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102030323A CN102030323A (en) | 2011-04-27 |
| CN102030323B true CN102030323B (en) | 2012-11-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 201010565462 Active CN102030323B (en) | 2010-11-30 | 2010-11-30 | Preparation method of iron phosphate |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109081321B (en) * | 2018-10-29 | 2020-05-12 | 北京科技大学 | Method for preparing iron phosphate from converter dephosphorized slag |
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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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 |
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| CN102030323A (en) | 2011-04-27 |
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