CN109694049A - A kind of processing method containing zinc, calcium, iron phosphatization slag - Google Patents
A kind of processing method containing zinc, calcium, iron phosphatization slag Download PDFInfo
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- CN109694049A CN109694049A CN201910063369.XA CN201910063369A CN109694049A CN 109694049 A CN109694049 A CN 109694049A CN 201910063369 A CN201910063369 A CN 201910063369A CN 109694049 A CN109694049 A CN 109694049A
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- iron
- hydroxide
- phosphate
- potassium
- zinc
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/30—Alkali metal phosphates
- C01B25/301—Preparation from liquid orthophosphoric acid or from an acid solution or suspension of orthophosphates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/32—Phosphates of magnesium, calcium, strontium, or barium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/14—Sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The processing method containing zinc, calcium, iron phosphatization slag that the invention discloses a kind of, its step includes: to be reacted with potassium hydroxide solution with the heating of phosphatization slag, iron hydroxide, calcium phosphate, zinc hydroxide solid mixture are filtered to obtain, contains potassium phosphate, inclined potassium zincate, potassium hydroxide in liquid.Phosphorus acid for adjusting pH is first added in liquid to 6.5 ~ 8, filtering or standing solution obtain trbasic zinc phosphate after washing again, and phosphorus acid for adjusting pH < 4 condensing crystallizings are added in remaining liq and obtain potassium dihydrogen phosphate.Solid mixture first uses certain sulfuric acid dissolution, calcium phosphate is obtained by filtration, its solution obtains sulfuric acid iron powder after certain degree is first concentrated, the filtering of pH to 4 ~ 5.5 is adjusted with a certain amount of sodium hydroxide again, washing obtains iron hydroxide, pH to 6 ~ 8.5 being adjusted with sodium hydroxide again, zinc hydroxide being obtained by filtration, iron hydroxide is used to prepare ferric sulfate.The present invention realizes making full use of for phosphatization slag, reduces its pollution to environment.
Description
Technical field
The invention belongs to chemical industry and environmental protection technical field, and in particular to a kind of side of carbon steel Zinc-calcium series phosphatating Slag treatment
Method.
Background technique
The processing of carbon steel zinc calcium-phosphorus ratio is conducive to its protection in cold working and coating, and the process of phosphatization can generate solid
The group of phosphatization slag, phosphatization slag becomes ferric phosphate, trbasic zinc phosphate, calcium phosphate etc..Buried and other chemical treatment method is generally used,
These processing methods are not that there are biggish hidden danger to environment, are exactly handled not enough thoroughly.
Potassium dihydrogen phosphate is industrially used as buffer, nutrient chemical；Agriculturally it is being used as efficient phosphorus potassium complex fertilizer, and system
The raw material of standby potassium metaphosphate, preparation phosphoric acid and potassium hydroxide the reaction preparation of general potassium dihydrogen phosphate, if can be phosphatization
Phosphate radical in slag uses, and can reduce environmental pollution, also can save the cost.For example, Chinese patent
A kind of 201310322348.8 handle utilize phosphatization slag at phosphate and the method for iron oxide red.
Ferric sulfate is used as water purification agent in sewage, is used as chemical fertilizer and prepares ferric phosphate etc. in agricultural, there is very big economic valence
Value.The present invention makes iron in phosphatization slag be fully utilized, and reduces the pollution of environment.
Trbasic zinc phosphate is the main composition of phosphatization slag, is widely used in fire retardant, phosphating solution synthesis, coating, but general chemistry
Method is difficult ferric phosphate and trbasic zinc phosphate to separate.
The amount of zinc hydroxide is fewer, but it separates the processing difficulty that can also reduce last waste water, furthermore it is forged
Zinc oxide after burning also has very big application value.
Summary of the invention
The purpose of the present invention is for it is existing containing zinc, calcium, iron phosphatization Slag treatment technology deficiency, provide a kind of new height
The method extracted is imitated, realizes making full use of for phosphatization slag, and make the product prepared, is had in industry and agricultural larger
Application space.
The technical solution of the present invention is as follows:
A kind of processing method containing zinc, calcium, iron phosphatization slag, comprising the following steps:
(1) phosphatization slag is reacted with potassium hydroxide solution, is obtained by filtration liquid phase and solid phase, liquid phosphorus acid for adjusting pH to 6.5 ~ 8,
Filtering is washed, drying, obtains trbasic zinc phosphate, and filtrate uses phosphorus acid for adjusting pH < 4, concentration, crystallization, filtering, with saturation biphosphate again
Potassium solution washs to obtain potassium dihydrogen phosphate.
(2) solid in step (1) first uses a certain amount of sulfuric acid dissolution, and calcium phosphate is obtained by filtration in pH value of solution 4.5 ~ 6.5,
Liquid concentration filters, is dried to obtain sulfuric acid iron powder, remaining liq with 30% sodium hydroxide solution tune pH to 4 ~ 5.5, filtering,
Iron hydroxide is washed to obtain, for last remaining liquid again with sodium hydroxide solution tune pH to 6 ~ 8.5, filtering, washing obtain hydroxide
Zinc.
The beneficial effects of the present invention are:
Present invention employs new thinkings, prepare potassium dihydrogen phosphate, ferric sulfate, calcium phosphate, zinc hydroxide, very good solution phosphatization
Slag problem makes the utilization rate of phosphatization slag reach 95% or more, generates very big economic value.The product that the method for the present invention is prepared
Purity is all very high, and wherein trbasic zinc phosphate purity is up to 99% or more, and for potassium dihydrogen phosphate purity up to 96%, ferric sulfate powder purity is reachable
97%, for the main composition trbasic zinc phosphate for being phosphatization slag, the present invention becomes the extraction of zinc using the method for first dissolving recrystallization
It is simple and efficient.The present invention realizes maximally utilizing for resource, realizes the efficient utilization of solid waste phosphorized slag.
Specific embodiment
Invention is further described in detail in conjunction with specific embodiments, but protection scope of the present invention be not limited to down it is true
Apply example.
Embodiment 1
3g phosphatization slag is taken to react with 6g potassium hydroxide solution, filtering respectively obtains liquid and solid, and liquid is adjusted with phosphoric acid (85%)
Ph to 6.5 ~ 8, filtering, deionized water are washed 3 ~ 5 times, drying, obtain 98.7% trbasic zinc phosphate of content, and filtrate uses phosphoric acid (85%) to adjust again
Ph < 4 are saved, 10ml, filtering are concentrated into, 2 times is washed with saturation potassium dihydrogen phosphate and obtains 99% potassium dihydrogen phosphate, residue filter
Liquid circulation utilizes.
Solid among the above first uses a certain amount of sulfuric acid (10%) to dissolve, and calcium phosphate is obtained by filtration in solution ph4.5 ~ 6.5,
Liquid concentration is filtered, is dried to obtain sulfuric acid iron powder to 10ml, remaining liq with sodium hydroxide solution (10%) adjust ph to 4 ~
5.5 filterings, washing obtain 96% iron hydroxide, and last remaining liquid uses sodium hydroxide solution (10%) to adjust ph to 6 ~ 8.5 again
Filtering, washing obtain 95% zinc hydroxide.
Embodiment 2
9g phosphatization slag is taken to react with 17g potassium hydroxide solution, filtering respectively obtains liquid and solid, and liquid is adjusted with phosphoric acid (85%)
Ph to 6.5 ~ 8, filtering are saved, deionized water is washed 3 ~ 5 times, and drying obtains 98.7% trbasic zinc phosphate of content, filtrate uses phosphoric acid (85%) again
Ph < 4 are adjusted, 10ml, filtering are concentrated into, 2 times is washed with saturation potassium dihydrogen phosphate and obtains 98% potassium dihydrogen phosphate, it is remaining
Filtrate body circulation utilizes.
Solid among the above first uses a certain amount of sulfuric acid (15%) to dissolve, and calcium phosphate is obtained by filtration in solution ph4.5 ~ 6.5,
Liquid concentration is filtered, is dried to obtain sulfuric acid iron powder to 10ml, remaining liq with sodium hydroxide solution (15%) adjust ph to 4 ~
5.5 filterings, washing obtain 96% iron hydroxide, and last remaining liquid uses sodium hydroxide solution (13%) to adjust ph to 6 ~ 8.5 again
Filtering, washing obtain 94% zinc hydroxide.
Embodiment 3
18g phosphatization slag is taken to react with 35g potassium hydroxide solution, filtering respectively obtains liquid and solid, and liquid is adjusted with phosphoric acid (85%)
Ph to 6.5 ~ 8, filtering are saved, deionized water is washed 3 ~ 5 times, and drying obtains 98.7% trbasic zinc phosphate of content, filtrate uses phosphoric acid (85%) again
Ph < 4 are adjusted, 10ml, filtering are concentrated into, 2 times is washed with saturation potassium dihydrogen phosphate and obtains 99% potassium dihydrogen phosphate, it is remaining
Filtrate body circulation utilizes.
Solid among the above first uses a certain amount of sulfuric acid (20%) to dissolve, and calcium phosphate is obtained by filtration in solution ph4.5 ~ 6.5,
Liquid concentration is filtered, is dried to obtain sulfuric acid iron powder to 10ml, remaining liq with sodium hydroxide solution (20%) adjust ph to 4 ~
5.5 filterings, washing obtain 96% iron hydroxide, and last remaining liquid uses sodium hydroxide solution (20%) to adjust ph to 6 ~ 8.5 again
Filtering, washing obtain 95% zinc hydroxide.
Claims (2)
1. a kind of processing method containing zinc, calcium, iron phosphatization slag, it is characterised in that the following steps are included:
(1) phosphatization slag is reacted with potassium hydroxide solution, is obtained by filtration liquid phase and solid phase, liquid phosphorus acid for adjusting pH to 6.5 ~ 8,
Filtering is washed, drying, obtains trbasic zinc phosphate, and filtrate uses phosphorus acid for adjusting pH < 4, concentration, crystallization, filtering, with saturation biphosphate again
Potassium solution washs to obtain potassium dihydrogen phosphate；
(2) solid in step (1) first uses a certain amount of sulfuric acid dissolution, and calcium phosphate, liquid is obtained by filtration in pH value of solution 4.5 ~ 6.5
Concentration filters, is dried to obtain sulfuric acid iron powder, and 30% sodium hydroxide solution tune pH to 4 ~ 5.5 of remaining liq is filtered, washing
Iron hydroxide is obtained, for last remaining liquid again with sodium hydroxide solution tune pH to 6 ~ 8.5, filtering, washing obtain zinc hydroxide.
2. the processing method according to claim 1 containing zinc, calcium, iron phosphatization slag, it is characterised in that potassium hydroxide solution
3h is reacted with the heating of phosphatization solid slag.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910063369.XA CN109694049B (en) | 2019-01-23 | 2019-01-23 | Treatment method of phosphated slag containing zinc, calcium and iron |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910063369.XA CN109694049B (en) | 2019-01-23 | 2019-01-23 | Treatment method of phosphated slag containing zinc, calcium and iron |
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| CN109694049A true CN109694049A (en) | 2019-04-30 |
| CN109694049B CN109694049B (en) | 2021-10-29 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| CN103395761A (en) * | 2013-07-29 | 2013-11-20 | 丁忠华 | Method for preparing phosphate and iron oxide red by utilizing phosphated residue |
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| US20160060113A1 (en) * | 2013-05-02 | 2016-03-03 | Easyminging Sweden Ab | Production of Phosphate Compounds from Materials Containing Phosphorus and at Least One of Iron and Aluminium |
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| CN104862473A (en) * | 2014-12-31 | 2015-08-26 | 金川集团股份有限公司 | Method for recovering nickel, cobalt, iron, silicon and magnesium from laterite-nickel ore |
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Cited By (1)
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|---|---|---|---|---|
| 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 |
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| CN109694049B (en) | 2021-10-29 |
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