Method for continuously preparing low-cost battery grade ferric phosphate by utilizing iron filings

A ferric orthophosphate, battery-grade technology, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of increasing equipment investment and operating costs, increasing the burden of washing and filtration, and large consumption of deionized water, etc. Achieve the effect of less washing water consumption, easy selection of separation device and fast reaction speed

Active Publication Date: 2016-09-28

云图新能源材料(荆州)有限公司

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AI-Extracted Technical Summary

Problems solved by technology

If the consumption of deionized water is large, it will not only increase the cost, but also produce a large amount of sewage, which will bring great pressure to environmental protection.

On the other hand, ferrous sulfate solution is easily oxidized during the preparation process, resulting in extremely poor stability of product batches; a...

Abstract

The invention discloses a method for continuously preparing low-cost battery grade ferric phosphate by utilizing iron filings. The method comprises the following steps: deionized water is pumped into an elevated tank; phosphoric acid is added into the elevated tank to prepare a phosphoric acid solution with the concentration being 20-85%; a hydrogen peroxide solution with the concentration being 6% is prepared in the same manner; the iron filings are added into a reaction kettle, the prepared phosphoric acid solution is added into the reaction kettle through an air-pressure type nozzle mounted at a material inlet of the reaction kettle, intense stirring is performed, and a template agent and a surfactant are added after the iron filings are completely dissolved; the prepared hydrogen peroxide solution is added, and products are extracted, filtered, washed and dried; finally, a battery grade ferric phosphate product is prepared through calcination. Raw materials used in the method are easy to obtain and low in price; the technology is simple, the operation is convenient, and the industrialization can be realized easily. The battery grade ferric phosphate material prepared according to the method has controllable appearance and particle size, the iron-phosphorus ratio ranges from 0.98 to 1.02, the batch stability is good, and the cost is low.

Application Domain

Phosphorus compounds

Technology Topic

IonHydrogen peroxide +8

Image

Examples

Experimental program(3)

Example Embodiment

[0042] Example 1

[0043] (1) Phosphoric acid solution preparation

[0044] Weigh 100kg of phosphoric acid, add 325kg of deionized water and stir evenly to prepare a phosphoric acid solution with a concentration of 20% for use; weigh 100kg of hydrogen peroxide with a concentration of 30% and add 400kg of deionized water and stir to prepare a 6% hydrogen peroxide solution for use , Use an explosion-proof pump to drive the prepared phosphoric acid solution and hydrogen peroxide solution into the high tank;

[0045] (2) Dissolution-reaction

[0046] Weigh 42.5kg iron red into the reactor, add 85kg deionized water and stir vigorously. At the beginning, increase the temperature to the set temperature of 95℃. When the temperature rises to the set temperature, use the anti-corrosion pressure pump to adjust step (1) 127.5kg of good phosphoric acid solution is injected into the air pressure nozzle 7 installed at the feed port 4 of the reactor to start feeding, and keep vigorous stirring. The feeding time is 2 hours after the phosphoric acid solution is added, iron red starts to dissolve, and the process changes from red to The gray color changes; after the addition of the phosphoric acid solution, continue to stir for 1 hour, and all the iron filings in the reactor will be dissolved;

[0047] (3) Product formation

[0048] Weigh 0.2kg of nanofibers directly into the reaction kettle, stir evenly; start dropping the prepared hydrogen peroxide solution in step (1), add a total of 1.275kg hydrogen peroxide solution at a constant rate over half an hour, and the reaction solution after the addition of the hydrogen peroxide solution is complete Further turn to white; continue to react for 3 hours and then completely turn white, take out the material from the bottom of the reactor 5, the filtrate is filtered, and the filtrate is washed with 3 times the mass of deionized water until the pH of the filtrate is neutral That is; the washed filtrate is placed in an oven and dried to obtain a white powder product;

[0049] (4) calcination

[0050] The white powder product obtained in step (3) is calcined at 600° C. for 3 hours and then naturally cooled to obtain a battery-grade iron orthophosphate final product.

[0051] The main inspection indicators for the prepared battery-grade iron orthophosphate are iron-phosphorus ratio and particle size and morphology. The particle size and morphology can be clearly seen from the scanning electron microscope pictures. The iron-phosphorus ratio adopts chemical analysis methods, and phosphorus and iron are respectively measured In the test, phosphorus was analyzed by quinophos ketone weighing method, and iron was analyzed by tin tetrachloride reduction titration method. The following examples are all analyzed and tested in the same way.

[0052] See the SEM picture of the battery-grade iron orthophosphate prepared in this example figure 2 As shown, its iron-phosphorus ratio is 0.99.

Example Embodiment

[0053] Example 2

[0054] (1) Solution preparation

[0055] Weigh 120kg of phosphoric acid and add 390kg of deionized water and stir evenly to prepare a 85% phosphoric acid solution for use. Weigh 100kg of hydrogen peroxide with a concentration of 28% and add 400kg deionized water to mix evenly, and prepare a 6% hydrogen peroxide solution for use. , Use an explosion-proof pump to drive the prepared phosphoric acid solution and hydrogen peroxide solution into the high tank;

[0056] 2) Dissolution-reaction

[0057] Weigh 40kg of iron powder and pour it into the reactor, add 350kg of deionized water and stir. At the beginning, the temperature will rise to the set temperature of 45℃; when the temperature rises to the set temperature, use the anticorrosive pressure pump to transfer the prepared phosphoric acid solution in step (1) 400kg into the gas pressure nozzle 7 installed at the feed port 4 of the reactor to start feeding, and keep vigorous stirring. The feeding time takes 2 hours to add the phosphoric acid solution and maintain vigorous stirring. After the phosphoric acid solution is added in 2 hours, the iron powder starts The dissolution changes from black to brown; after the addition of the phosphoric acid solution, continue to stir for 1 hour, and all the iron filings in the reactor are dissolved;

[0058] (3) Product formation

[0059] Weigh 0.1kg of graphene directly into the reaction kettle and stir evenly; start to add the prepared hydrogen peroxide solution dropwise, and add a total of 1.85kg hydrogen peroxide solution at a constant rate over half an hour. After the addition of the hydrogen peroxide dropwise, the reaction solution further turns to grayish white Continue the reaction for 3 hours and completely turn off-white, take out the material from the outlet 5 at the bottom of the reactor, filter and wash the same as in Example 1, and then dry it in an oven to obtain off-white powder;

[0060] (3) Product formation

[0061] (4) calcination

[0062] The off-white powder obtained in step (3) is calcined at 450° C. for 5 hours and then naturally cooled to obtain a battery-grade iron orthophosphate final product.

[0063] The morphology, particle size and iron-phosphorus ratio of the product were analyzed using the same method as in Example (1).

[0064] See the SEM picture of the battery-grade iron orthophosphate prepared in this example image 3 As shown, the iron to phosphorus ratio of the material is 0.98.

Example Embodiment

[0065] Example 3

[0066] (1) Solution preparation

[0067] Weigh 100kg of phosphoric acid, add 70kg of deionized water and stir to make a 50% phosphoric acid solution for use. Weigh 100kg of hydrogen peroxide with a concentration of 30% and add 400kg of deionized water and stir evenly to prepare a 6% hydrogen peroxide solution for use. The good phosphoric acid solution and hydrogen peroxide solution are pumped into the high tank with an explosion-proof pump;

[0068] (2) Dissolution-reaction

[0069] Weigh 40 kilograms of cut iron scraps and place them in the reactor, add 200 kilograms of deionized water and stir slowly, start the temperature rise to the set temperature of 90 ℃; after the temperature rises to the set temperature, use the anti-corrosion pressure pump to adjust the step (1 ) 280 kg of the prepared phosphoric acid solution was injected into the air pressure nozzle 7 installed at the feed port 4 of the reactor to start feeding, and slowly stirred. After the phosphoric acid solution was added in 2 hours, the iron began to gradually dissolve into particles, and then the stirring rate was increased. , Stir until all the iron solids are dissolved into a brown solution;

[0070] (3) Product formation

[0071] Weigh 0.15 kg of the prepared iron orthophosphate powder directly into the reaction kettle and stir evenly; start to add the prepared hydrogen peroxide solution dropwise, add 1.5kg hydrogen peroxide solution at a constant rate for half an hour, and react after the hydrogen peroxide solution is added. The liquid further changed to white; the reaction solution was completely white after continuing the reaction for 3 hours, and finally the material was taken out from the outlet 5 at the bottom of the reactor through traditional filtration, washed in the same manner as in Example 1, and dried in an oven to obtain a white powder;

[0072] (4) calcination

[0073] The white powder obtained in step (3) is reacted at 650° C. for 2 hours and then naturally cooled to obtain the final battery-grade iron orthophosphate product.

[0074] The morphology, particle size and iron-phosphorus ratio of the product were analyzed using the same method as in Example (1).

[0075] See the SEM picture of the battery-grade iron orthophosphate prepared in this example Figure 4 As shown, the iron to phosphorus ratio of the material is 1.02.

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ActiveCN107884396ARaw materials are easy to getEasy to prepare

Owner:CAPITAL NORMAL UNIVERSITY

Classification and recommendation of technical efficacy words

Raw materials are easy to get
low cost

Method for continuously preparing low-cost battery grade ferric phosphate by utilizing iron filings

AI-Extracted Technical Summary

Problems solved by technology

Abstract

Image

Examples

Example Embodiment

Example Embodiment

Example Embodiment

PUM

Description & Claims & Application Information

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