CN103832990A - Method for extracting ferric phosphate from phosphorized waste residues - Google Patents
Method for extracting ferric phosphate from phosphorized waste residues Download PDFInfo
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- CN103832990A CN103832990A CN201210488837.6A CN201210488837A CN103832990A CN 103832990 A CN103832990 A CN 103832990A CN 201210488837 A CN201210488837 A CN 201210488837A CN 103832990 A CN103832990 A CN 103832990A
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- ferric phosphate
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- waste residues
- phosphatization
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Abstract
The invention relates to a method for extracting ferric phosphate from phosphorized waste residues. The method comprises the following steps: adding water into powdery phosphorized waste residues, and uniformly stirring; then, slowly adding concentrated hydrochloric acid into a reaction device till the white solids are fully dissolved; filtering the solution and removing undissolved substances; slowly dropwise adding sodium hydroxide solution into the filtrate, controlling the pH of the solution to 1.0-2.0, reacting for 3+/-0.5 hours, and filtering; washing with distilled water to neutral; and drying and smashing to obtain a battery-grade ferric pyrophosphate product. According to the process of recovering and purifying ferric phosphate provided by the invention, the recovery rate of ferric phosphate reaches 90%, the content of Fe<3+> in the ferric phosphate product is greater than or equal to 29% (dihydrate), and Fe/P is equal to 0.97-1.0. According to the method provided by the invention, waste is turned to wealth, the problem that waste residues are discharged to cause the environmental pollution is solved, and the ferric phosphate product with a wide market prospect is extracted from phosphorized waste residues.
Description
Technical field
The present invention relates to the technology of utilizing of the solid slag that produces after auto parts machinery factory, processing Zhong Zhi phosphatization workshop section of antitheft door factory.
Background technology
The enterprise such as auto parts machinery, antitheft door is in processing process, and when carrying out can producing a large amount of white waste residue---solid wastes after phosphating process, the main component of this waste material is tertiary iron phosphate, primary iron phosphate, calcium phosphate, zinc phosphate.For this waste material, enterprise all adopts the method for " burying processing ", has caused pollution to environment.
Tertiary iron phosphate is the main raw material for the preparation of ferric phosphate lithium cell, also can be used as catalyzer and manufactures pottery etc.In tertiary iron phosphate, ferrophosphorus, than being the performance index of weighing tertiary iron phosphate quality most critical, is also the key factor that determines ferric phosphate lithium cell material property quality, and the iron phosphorus ratio of the tertiary iron phosphate of lithium cell raw material is Fe: P=0.97～1.02.
In recent years, along with the development of new-energy automobile, constantly increase for the demand of heavy-duty battery, and the lithium ion cell positive that utilizes iron lithium phosphate to manufacture for raw material, be at present the most cheaply, the anode material for lithium-ion batteries of environmental protection.It serves to show, the application market prospect of tertiary iron phosphate is very wide.
Summary of the invention
The object of the invention is to, provide one to turn waste into wealth---from waste material phosphatization waste residue, reclaim the method for purification tertiary iron phosphate.
The present invention is achieved in that
First phosphatization waste residue is dissolved, then the foreign ion such as calcium, zinc is departed from alkali, thereby realize the object that reclaims purification tertiary iron phosphate.
Production Flow Chart of the present invention is as follows:
Raw material+water → add hydrochloric acid makes it dissolve → filter out insolubles → to adding sodium hydroxide solution reaction certain hour → filter → get distilled water wash → filtration drying for filter cake → pulverizing → detection → pack in filtrate completely.
Concrete grammar step of the present invention is as follows:
1. white powder phosphatization waste residue phosphatization workshop being produced, adds in reaction unit, then adds water, and weight ratio is phosphatization waste residue: water=1: 1～1.2, stir;
2. with slowly adding concentrated hydrochloric acid in backward reaction unit, dissolve completely to white solid---now solution becomes clarification, and a small amount of mechanical impurity is arranged at reaction unit bottom;
3. with sand core funnel, above-mentioned solution is filtered; Remove undissolved mechanical impurity;
4. to the sodium hydroxide solution that slowly drips 2mol/L (mol/L) in above-mentioned filtrate, control pH value of solution between 1.0-2.0, react after 3 ± 0.5 hours, filter with sand core funnel;
5. get filter cake, be washed with distilled water to neutrality: pH is 7;
6. at 100～110 ℃, dry 2～3h hour, is crushed to 300 orders, obtains the Orthophosphoric acid Ferrum product of cell-grade.
The present invention's recovery purification tertiary iron phosphate technique, the tertiary iron phosphate rate of recovery reaches 90%, the tertiary iron phosphate product obtaining: Fe
3+content>=29% (two water things), Fe/P=0.97-1.0.The present invention is turned waste into wealth, and has both solved waste sludge discharge and cause the problem of environmental pollution, has extracted again the wide tertiary iron phosphate product of market outlook from phosphatization waste residue.Create good economic benefit to enterprise.
Embodiment
Narrate two embodiment below, the present invention will be further described:
Embodiment 1 extracts one of method of tertiary iron phosphate from phosphatization waste residue
1. white powder phosphatization waste residue phosphatization workshop being produced, adds in reaction unit, then adds water, and weight ratio is phosphatization waste residue: water=1: 1, stir;
2. with slowly adding concentrated hydrochloric acid in backward reaction unit, dissolve completely to white solid;
3. with sand core funnel, above-mentioned solution is filtered; Remove insolubles:
4. to the sodium hydroxide solution that slowly drips 2mol/L in above-mentioned filtrate, control pH value of solution 1.0, react after 3.5 hours, filter with sand core funnel;
5. get filter cake, be washed with distilled water to neutrality, pH is 6;
6. at 100 ℃ of dry 3h hour, be crushed to 300 orders, obtain the Orthophosphoric acid Ferrum product of cell-grade.
Embodiment 2 from phosphatization waste residue, extract tertiary iron phosphate method two
1. white powder phosphatization waste residue phosphatization workshop being produced, adds in reaction unit, then adds water, and weight ratio is phosphatization waste residue: water=1: 1.2, stir;
2. with slowly adding concentrated hydrochloric acid in backward reaction unit, dissolve completely to white solid;
3. with sand core funnel, above-mentioned solution is filtered; Remove insolubles;
4. to the sodium hydroxide solution that slowly drips 2mol/L in above-mentioned filtrate, control pH value of solution 2.0, react after 2.5 hours, filter with sand core funnel;
5. get filter cake, be washed with distilled water to neutrality, pH is 8;
6. at 110 ℃ of dry 2h hour, be crushed to 300 orders, obtain the Orthophosphoric acid Ferrum product of cell-grade.
Claims (1)
1. a method of extracting tertiary iron phosphate from phosphatization waste residue, is characterized in that, carries out with following step:
1) white powder phosphatization waste residue phosphatization workshop being produced, adds in reaction unit, then adds water, and weight ratio is phosphatization waste residue: water=1: 1～1.2, stir;
2), with slowly adding concentrated hydrochloric acid in backward reaction unit, dissolve completely to white solid---now solution becomes clarification, and mechanical impurity is arranged at reaction unit bottom;
3) with sand core funnel, above-mentioned solution is filtered; Remove above-mentioned mechanical impurity;
4) to the sodium hydroxide solution that slowly drips 2mol/L in above-mentioned filtrate, control pH value of solution between 1.0-2.0, react after 3 ± 0.5 hours, filter with sand core funnel;
5) get filter cake, be washed with distilled water to neutrality: pH is 7 ± 1;
6), at 100～110 ℃, dry 2～3h hour, is crushed to 300 orders, obtains the Orthophosphoric acid Ferrum product of cell-grade.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210488837.6A CN103832990A (en) | 2012-11-27 | 2012-11-27 | Method for extracting ferric phosphate from phosphorized waste residues |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210488837.6A CN103832990A (en) | 2012-11-27 | 2012-11-27 | Method for extracting ferric phosphate from phosphorized waste residues |
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| CN103832990A true CN103832990A (en) | 2014-06-04 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201210488837.6A Pending CN103832990A (en) | 2012-11-27 | 2012-11-27 | Method for extracting ferric phosphate from phosphorized waste residues |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105776165A (en) * | 2016-02-29 | 2016-07-20 | 嘉兴市净源循环环保科技有限公司 | Method for extracting and preparing iron phosphate with phosphorization slag |
| CN105810943A (en) * | 2016-05-16 | 2016-07-27 | 上海第二工业大学 | Method for preparing zinc-doped lithium iron phosphate from phosphated residue |
| CN106315535A (en) * | 2016-08-09 | 2017-01-11 | 湘潭大学 | Method for preparing pure iron phosphate from phosphated residue containing iron and zinc |
| CN106976851A (en) * | 2017-05-21 | 2017-07-25 | 石家庄学院 | A kind of method that utilization phosphatization slag prepares ferric phosphate and APP fertilizer |
| CN108163827A (en) * | 2018-01-17 | 2018-06-15 | 靖西湘潭电化新能源材料有限公司 | A kind of method that nano ferric phosphate is prepared by phosphatization slag |
| CN111690280A (en) * | 2020-07-06 | 2020-09-22 | 湘潭市双马世纪新材料有限公司 | Method for producing phosphate antirust pigment by using phosphated residue |
| CN112320781A (en) * | 2020-11-23 | 2021-02-05 | 湖南金源新材料股份有限公司 | Method for regenerating iron phosphate by lithium extraction residues of lithium iron phosphate waste |
| CN112357898A (en) * | 2020-11-23 | 2021-02-12 | 湖南金源新材料股份有限公司 | Three-stage reverse impurity washing method for crude ferric phosphate |
| CN112520718A (en) * | 2020-12-04 | 2021-03-19 | 南昌航空大学 | Method for selectively recovering battery-grade iron phosphate from acid leaching solution of lithium extraction slag |
-
2012
- 2012-11-27 CN CN201210488837.6A patent/CN103832990A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105776165A (en) * | 2016-02-29 | 2016-07-20 | 嘉兴市净源循环环保科技有限公司 | Method for extracting and preparing iron phosphate with phosphorization slag |
| CN105810943A (en) * | 2016-05-16 | 2016-07-27 | 上海第二工业大学 | Method for preparing zinc-doped lithium iron phosphate from phosphated residue |
| CN106315535A (en) * | 2016-08-09 | 2017-01-11 | 湘潭大学 | Method for preparing pure iron phosphate from phosphated residue containing iron and zinc |
| CN106976851A (en) * | 2017-05-21 | 2017-07-25 | 石家庄学院 | A kind of method that utilization phosphatization slag prepares ferric phosphate and APP fertilizer |
| CN108163827A (en) * | 2018-01-17 | 2018-06-15 | 靖西湘潭电化新能源材料有限公司 | A kind of method that nano ferric phosphate is prepared by phosphatization slag |
| CN111690280A (en) * | 2020-07-06 | 2020-09-22 | 湘潭市双马世纪新材料有限公司 | Method for producing phosphate antirust pigment by using phosphated residue |
| CN112320781A (en) * | 2020-11-23 | 2021-02-05 | 湖南金源新材料股份有限公司 | Method for regenerating iron phosphate by lithium extraction residues of lithium iron phosphate waste |
| CN112357898A (en) * | 2020-11-23 | 2021-02-12 | 湖南金源新材料股份有限公司 | Three-stage reverse impurity washing method for crude ferric phosphate |
| CN112520718A (en) * | 2020-12-04 | 2021-03-19 | 南昌航空大学 | Method for selectively recovering battery-grade iron phosphate from acid leaching solution of lithium extraction slag |
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Application publication date: 20140604 |