Method for preparing battery-grade iron phosphate by utilizing iron oxide waste material in metal processing industry

A metal processing, iron oxide technology, applied in chemical instruments and methods, non-metallic elements, phosphorus compounds, etc., can solve problems such as environmental pollution, reduce production costs, facilitate promotion and popularization, and solve the effects of environmental pollution

Active Publication Date: 2017-12-22
江苏荣信环保科技有限公司
2 Cites 5 Cited by

AI-Extracted Technical Summary

Problems solved by technology

Strong acid groups (such as sulfate groups) introduced by strong acids are easy to attach to the surface of the ferric phosphate product to make the product acidic, so it is often necessary to use ammonium to adjust the pH. In addition,...
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Method used

In sum: a kind of iron oxide waste material provided by the invention utilizes metal processing industry to prepare the method for battery-grade ferric phosphate, compared with traditional preparation technology, no sulfur dioxide is produced in the present invention, and the ferric phosphate of preparation It does not contain iron oxide and chloride ions, and the quality is higher. The lithium iron phosphate battery thus prepared does not have the problem of short circuit of single iron, and can realize fast ...
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Abstract

The invention discloses a method for preparing a battery-grade iron phosphate by utilizing an iron oxide waste material in the metal processing industry. The method comprises the following steps: filtration for seven times, distillation at two times, electrolysis at two times and roasting for one time. Compared with a conventional preparation process, the method for preparing the battery-grade iron phosphate by utilizing the iron oxide waste material in the metal processing industry has the advantages that production of sulfur dioxide is avoided, and the prepared iron phosphate does not contain iron oxide and chloride ions, so that the quality is higher, and an iron phosphate lithium battery prepared by the method has no problem of short circuit of elementary iron and can realize quick charging. New energy materials are converted by utilizing solid wastes, so that the problem of environmental pollution in local places is solved, the high-quality iron phosphate also can be prepared, sustainable development of the metal product industry is promoted, and the production cost of the new energy materials is reduced; meanwhile, an elementary lead-zinc raw material can be prepared from the iron oxide waste material, ferrous chloride and sodium hypochlorite also can be prepared, and promotion and popularization are facilitated.

Application Domain

Phosphorus compounds

Technology Topic

IonBrown iron oxide +18

Examples

  • Experimental program(3)

Example Embodiment

[0025] Example 1
[0026] A method for preparing battery-grade iron phosphate from iron oxide waste in the metal processing industry, comprising the steps of:
[0027] S1. Add iron oxide waste into the reaction kettle, and add waste acid to adjust the pH value, and after stirring evenly, use a filter press to filter to obtain filter residue 1 and filtrate 1;
[0028] S2. Add the filter residue 1 in the step S1 to the reaction kettle, and add phosphoric acid and hydrochloric acid to adjust the pH value. After stirring and reacting, use a filter press to filter to obtain filter residue 2 and filtrate 2;
[0029] S3, adding sodium sulfide solution to filtrate 1, stirring and reacting, and then filtering to obtain filter residue 3 and filtrate 3;
[0030] S4. Add the filter residue 2 in the step S2 to the reaction kettle, and add tap water to wash and filter to obtain the filter residue 4 and the filtrate 4. The filter residue 4 can be directly discharged harmlessly, and the filtrate 4 can be used as waste acid recycling in the step S1;
[0031] S5 joins filtrate 2 in the distillation kettle and heats with hot steam to carry out distillation, obtains residue and steams hydrochloric acid solution, and hydrochloric acid solution can be used as the hydrochloric acid recycling in step S2;
[0032] S6. Add the residue in the step S5 to the reaction kettle, and add tap water, and filter evenly with a filter press to obtain the filtrate 5 and the filter residue 5, and the filtrate 5 can be used as waste acid recycling in the step S1;
[0033] S7. Transfer the filter residue 5 in step S6 to the reaction kettle, add pure water, stir evenly, and filter with a filter press to obtain filtrate 6 and filter residue 6;
[0034] S8. Transfer the filter residue 6 in step S7 to another reaction kettle, add dilute nitric acid, and filter evenly with a filter press to obtain filtrate 7 and filter residue 7;
[0035] S9, adding filtrate 6 to the electrolytic cell for electrolysis, removing hydrochloric acid in the water, obtaining a small amount of lead-zinc mud, chlorine gas and water, water can be recycled as pure water in step S7;
[0036] S10, adding the filtrate seven in step S8 to another electrolytic cell for electrolysis to obtain chlorine gas and nitric acid (nitric acid is still retained in the water), nitric acid can be recycled as dilute nitric acid in step S8, and the filter residue seven is dried and dehydrated to obtain ferric phosphate Crude;
[0037] S11. Calcining the crude iron phosphate in step S8 can prepare battery-grade iron phosphate.
[0038] Specifically, the filter residue 3 in the step S2 is lead-zinc slag, the lead-zinc slag can be dried and dehydrated to prepare the lead-zinc raw material, the filtrate 3 is a ferrous chloride solution, and the ferrous chloride solution can be distilled to prepare ferrous chloride iron solid.
[0039] Specifically, the chlorine gas produced in step S9 and step S10 can be directly passed into sodium hydroxide solution to prepare sodium hypochlorite.
[0040] Specifically, the rotation speed of the stirrer in the reaction kettle in the steps S1-S6 is 200r/min.
[0041] Specifically, the internal temperature of the reactor in the steps S1-S6 is set to 50°C.
[0042] Specifically, the calcination temperature in the step S11 is 300°C.

Example Embodiment

[0043] Example 2
[0044] A method for preparing battery-grade iron phosphate from iron oxide waste in the metal processing industry, comprising the steps of:
[0045] S1. Add iron oxide waste into the reaction kettle, and add waste acid to adjust the pH value, and after stirring evenly, use a filter press to filter to obtain filter residue 1 and filtrate 1;
[0046] S2. Add the filter residue 1 in the step S1 to the reaction kettle, and add phosphoric acid and hydrochloric acid to adjust the pH value. After stirring and reacting, use a filter press to filter to obtain filter residue 2 and filtrate 2;
[0047] S3, adding sodium sulfide solution to filtrate 1, stirring and reacting, and then filtering to obtain filter residue 3 and filtrate 3;
[0048] S4. Add the filter residue 2 in the step S2 to the reaction kettle, and add tap water to wash and filter to obtain the filter residue 4 and the filtrate 4. The filter residue 4 can be directly discharged harmlessly, and the filtrate 4 can be used as waste acid recycling in the step S1;
[0049]S5 joins filtrate 2 in the distillation kettle and heats with hot steam to carry out distillation, obtains residue and steams hydrochloric acid solution, and hydrochloric acid solution can be used as the hydrochloric acid recycling in step S2;
[0050] S6. Add the residue in the step S5 to the reaction kettle, and add tap water, and filter evenly with a filter press to obtain the filtrate 5 and the filter residue 5, and the filtrate 5 can be used as waste acid recycling in the step S1;
[0051] S7. Transfer the filter residue 5 in step S6 to the reaction kettle, add pure water, stir evenly, and filter with a filter press to obtain filtrate 6 and filter residue 6;
[0052] S8. Transfer the filter residue 6 in step S7 to another reaction kettle, add dilute nitric acid, and filter evenly with a filter press to obtain filtrate 7 and filter residue 7;
[0053] S9, adding filtrate 6 to the electrolytic cell for electrolysis, removing hydrochloric acid in the water, obtaining a small amount of lead-zinc mud, chlorine gas and water, water can be recycled as pure water in step S7;
[0054] S10, adding the filtrate seven in step S8 to another electrolytic cell for electrolysis to obtain chlorine gas and nitric acid (nitric acid is still retained in the water), nitric acid can be recycled as dilute nitric acid in step S8, and the filter residue seven is dried and dehydrated to obtain ferric phosphate Crude;
[0055] S11. Calcining the crude iron phosphate in step S8 can prepare battery-grade iron phosphate.
[0056] Specifically, the filter residue 3 in the step S2 is lead-zinc slag, the lead-zinc slag can be dried and dehydrated to prepare the lead-zinc raw material, the filtrate 3 is a ferrous chloride solution, and the ferrous chloride solution can be distilled to prepare ferrous chloride iron solid.
[0057] Specifically, the chlorine gas produced in step S9 and step S10 can be directly passed into sodium hydroxide solution to prepare sodium hypochlorite.
[0058] Specifically, the rotation speed of the agitator in the reaction kettle in the steps S1-S8 is 300 r/min.
[0059] Specifically, the internal temperature of the reactor in the steps S1-S8 is set to 55°C.
[0060] Specifically, the calcination temperature in the step S11 is 400°C.

Example Embodiment

[0061] Example 3
[0062] A method for preparing battery-grade iron phosphate from iron oxide waste in the metal processing industry, comprising the steps of:
[0063] S1. Add iron oxide waste into the reaction kettle, and add waste acid to adjust the pH value, and after stirring evenly, use a filter press to filter to obtain filter residue 1 and filtrate 1;
[0064] S2. Add the filter residue 1 in the step S1 to the reaction kettle, and add phosphoric acid and hydrochloric acid to adjust the pH value. After stirring and reacting, use a filter press to filter to obtain filter residue 2 and filtrate 2;
[0065] S3, adding sodium sulfide solution to filtrate 1, stirring and reacting, and then filtering to obtain filter residue 3 and filtrate 3;
[0066] S4. Add the filter residue 2 in the step S2 to the reaction kettle, and add tap water to wash and filter to obtain the filter residue 4 and the filtrate 4. The filter residue 4 can be directly discharged harmlessly, and the filtrate 4 can be used as waste acid recycling in the step S1;
[0067] S5 joins filtrate 2 in the distillation kettle and heats with hot steam to carry out distillation, obtains residue and steams hydrochloric acid solution, and hydrochloric acid solution can be used as the hydrochloric acid recycling in step S2;
[0068] S6. Add the residue in the step S5 to the reaction kettle, and add tap water, and filter evenly with a filter press to obtain the filtrate 5 and the filter residue 5, and the filtrate 5 can be used as waste acid recycling in the step S1;
[0069] S7. Transfer the filter residue 5 in step S6 to the reaction kettle, add pure water, stir evenly, and filter with a filter press to obtain filtrate 6 and filter residue 6;
[0070] S8. Transfer the filter residue 6 in step S7 to another reaction kettle, add dilute nitric acid, and filter evenly with a filter press to obtain filtrate 7 and filter residue 7;
[0071] S9, adding filtrate 6 to the electrolytic cell for electrolysis, removing hydrochloric acid in the water, obtaining a small amount of lead-zinc mud, chlorine gas and water, water can be recycled as pure water in step S7;
[0072] S10, adding the filtrate seven in step S8 to another electrolytic cell for electrolysis to obtain chlorine gas and nitric acid (nitric acid is still retained in the water), nitric acid can be recycled as dilute nitric acid in step S8, and the filter residue seven is dried and dehydrated to obtain ferric phosphate Crude;
[0073] S11. Calcining the crude iron phosphate in step S8 can prepare battery-grade iron phosphate.
[0074] Specifically, the filter residue 3 in the step S2 is lead-zinc slag, and the lead-zinc raw material can be prepared by drying and dehydrating the lead-zinc slag, and the filtrate 3 is a ferrous chloride solution, and distilling the ferrous chloride solution can prepare ferrous chloride iron solid.
[0075] Specifically, the chlorine gas produced in step S9 and step S10 can be directly passed into sodium hydroxide solution to prepare sodium hypochlorite.
[0076] Specifically, the rotation speed of the agitator in the reaction kettle in the steps S1-S8 is 400r/min.
[0077] Specifically, the internal temperature of the reactor in the steps S1-S8 is set to 60°C.
[0078] Specifically, the calcination temperature in the step S11 is 500°C.
[0079] In summary: the present invention provides a method for preparing battery-grade iron phosphate using iron oxide waste in the metal processing industry. Compared with the traditional preparation process, no sulfur dioxide is produced in the present invention, and the prepared iron phosphate does not contain Iron oxide and chloride ions are of higher quality, and the lithium iron phosphate battery produced therefrom does not have the problem of short-circuit of single-substance iron, and can realize fast charging. The use of solid waste to transform new energy materials solves the local environmental pollution problem, and can also produce high-quality iron phosphate, which promotes the sustainable development of the metal products industry and reduces the production cost of new energy materials. At the same time, it can be prepared from iron oxide waste. Elemental lead and zinc raw materials can also be used to produce ferrous oxide and sodium hypochlorite, which is conducive to promotion and popularization.
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  • Improve quality
  • Solve environmental pollution
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