CN103205578A - Method for preparing iron-copper alloy by using waste pickling liquid in steelworks - Google Patents
Method for preparing iron-copper alloy by using waste pickling liquid in steelworks Download PDFInfo
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- CN103205578A CN103205578A CN201310129196XA CN201310129196A CN103205578A CN 103205578 A CN103205578 A CN 103205578A CN 201310129196X A CN201310129196X A CN 201310129196XA CN 201310129196 A CN201310129196 A CN 201310129196A CN 103205578 A CN103205578 A CN 103205578A
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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract
The invention discloses a method for preparing an iron-copper alloy by using a waste pickling liquid in steelworks. The method comprises the following process steps of: (1) adding a copper sulfate solution into the waste pickling liquid, or directly dissolving the copper sulfate solution into the waste pickling liquid so as to obtain a mixed solution; (2) adding an alkali solution into the mixed solution, stirring to react, aging and filtering so as to obtain a mixed precipitate; (3) washing, filtering and drying the mixed precipitate, and grinding to obtain precipitate powder by using a ball mill; (4) calcinating the precipitate powder, carrying out reduction reaction so as to obtain the iron-copper alloy. The method adopts the waste pickling liquid and the copper sulfate as the raw materials, a mixed oxide is obtained by directly using a coprecipitation method, and subsequently the iron-copper composite alloy powder is obtained through reduction; the main raw materials are derived from waste materials of steelworks, the raw materials are rich in resource and low in cost, and the method is simple in process, can effectively reuse wastes and reduce emission, and has the characteristics of energy conservation and environment friendliness.
Description
Technical field
The present invention relates to a kind of preparation method of iron-copper, especially a kind of method of utilizing Steel Plant's spent pickle liquor to prepare iron-copper.
Background technology
At present in the Steel Plant spent pickle liquor generally be to use the Shandong now nanofarad handle, waste liquid is carried out spray roasting obtains regeneration hydrochloric acid and red iron oxide.Because at high temperature hydrochloric acid has strong corrodibility, therefore the equipment that contacts waste liquid all needs to adopt the corrosion resistant material of high-quality, cause equipment cost height, component consumption big, simultaneously because high-temperature roasting needs a large amount of energy, the iron oxide red product of red iron oxide products production is because the pigment performance difference can not enter iron oxide pigment market, the way of some iron and steel enterprises is that cold rolled waste acid regenerating oxidation iron oxide red or part are undersold at present, or adopt and to mix iron ore and carry out secondary smelting, its working cost height, economic benefit is low.
Summary of the invention
The technical problem to be solved in the present invention provides a kind of method of utilizing Steel Plant's spent pickle liquor to prepare iron-copper, to effectively utilize spent pickle liquor in the Steel Plant.
For solving the problems of the technologies described above, processing step of the present invention is: (1) adds copper-bath in spent pickle liquor, perhaps copper sulfate directly is dissolved in the spent pickle liquor, obtains mixing solutions;
(2) add basic solution in the described mixing solutions, stir and react, obtain mixed sediment after ageing, the filtration;
(3) described mixed sediment adopts the ball mill grind away to obtain the throw out powder after washing, filtration, drying;
(4) described throw out powder carries out reduction reaction after calcining, can obtain described iron-copper.
2, the method for utilizing Steel Plant's spent pickle liquor to prepare iron-copper according to claim 1 is characterized in that: the concentration of copper-bath is 1～2mol/L in the described step (1).
Basic solution in the step of the present invention (2) is sodium hydroxide solution or ammoniacal liquor; Described basic solution is added into pH value to 7～9 of mixing solutions.The concentration of described basic solution with spent acid solution in volumetric molar concentration such as iron ion.Reaction times in the described step (2) is 30～50min, and digestion time is 3～4h.
Drying temperature in the step of the present invention (3) is 135～155 ℃.Mixed sediment is through 2～3 washings in the described step (3).Described step (3) grind away to throw out powder granularity is 1～2 micron.
Throw out powder in the step of the present invention (4) is calcined 1～3h down at 200～500 ℃.Reduction reaction temperature is 700～900 ℃ in the described step (4), and reducing gas is coke-oven gas or hydrogen, and the recovery time is 20～28 minutes.
The beneficial effect that adopts technique scheme to produce is: the main raw material that (1) the present invention adopts spent pickle liquor and copper sulfate to prepare iron copper composite alloy powder derives from steel plant wastes, its raw material sources are abundant and with low cost, the present invention can effectively make refuse reclamation reduce and efflux, and has the characteristics of energy-saving and environmental protection.
(2) to adopt spent pickle liquor and copper sulfate be main raw material in the present invention, and the method that directly adopts the method for co-precipitation to obtain recycling coke-oven gas after the mixed oxide or hydrogen reducing obtains iron copper composite alloy powder.Its preparation technology is simple, easily promotes.
(3) the present invention adopts the iron copper composite alloy powder powder of spent pickle liquor and copper sulfate preparation thinner, 1～2 micron of mean particle size range, the ratio of iron copper can freely be controlled in the iron-copper powder that the inventive method prepares, the content of copper can be controlled in 1%～4.9% in the described iron-copper alloy powder, iron level can be controlled in 95.1%～99%, other content are less than 1%, and wherein S content is less than 0.015%.
Description of drawings
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.
Fig. 1 be the iron-copper for preparing of the present invention can spectrogram.
Embodiment
The present invention is further detailed explanation below in conjunction with specific embodiment.
Embodiment 1: this utilizes the method for Steel Plant's spent pickle liquor preparation, and adopting spent pickle liquor and other copper sulfate of technical grade is raw material, and reducing gas is selected a large amount of coke-oven gas that produces in the process of coking for use, and its concrete processing step is:
(1) 1000g copper sulfate is dissolved in the copper-bath that is made into 1mol/L in the ionized water, according to the needs of the powdered alloy elemental composition prescription of Fe-2.5Cu copper-bath is joined in the spent pickle liquor, obtain mixing solutions;
(2) 1000g sodium hydroxide is mixed with spent acid solution in the basic solution of volumetric molar concentration such as iron ion; Basic solution is slowly poured in the mixing solutions, to the pH value of mixing solutions be 7; Stirring reaction 30min, ageing 3h obtain mixed sediment after the filtration;
(3) mixed sediment is through 2 washings, suction filtration, 135 ℃ of dryings, and batch mixing adopts the ball mill grind away to obtain powder granularity at 1～2 micron afterwards, obtains the throw out powder;
(4) the throw out powder is calcined 1h down at 500 ℃, obtains mixed oxide powder; Mixed oxide powder carries out reduction reaction under 700 ℃ of conditions, reducing gas is coke-oven gas, and the restoring operation time was controlled at 28 minutes, can obtain iron copper composite alloy powder.
The powder of the iron copper composite alloy powder of present method preparation is thinner, 1～2 micron of mean particle size range; Shown in Figure 1, it is 2.48% that X fluorometric assay and power spectrum are measured copper content, and iron level 96.70%, other content are less than 1%, and wherein S content 0.005%.
Embodiment 2: this utilizes Steel Plant's spent pickle liquor to prepare the method for iron-copper, and adopting spent pickle liquor and other copper sulfate of technical grade is raw material, and reducing gas is selected hydrogen for use, and its concrete processing step is:
(1) 2000g copper sulfate is dissolved in the copper-bath that is made into 2mol/L in the ionized water, according to the needs of the powdered alloy elemental composition prescription of Fe-3.5Cu copper-bath is joined in the spent pickle liquor, obtains mixing solutions;
(2) 2000g sodium hydroxide alkalescence reagent is mixed with spent acid solution in the basic solution of volumetric molar concentration such as iron ion; Then basic solution is slowly poured in the mixing solutions, to the pH value of mixing solutions be 8, stirring reaction 40Min, ageing 3.5h obtains mixed sediment after the filtration;
(3) mixed sediment is through 3 washings, suction filtration, 140 ℃ of dryings, and batch mixing adopts the ball mill grind away to obtain powder granularity at 1～2 micron afterwards, obtains the throw out powder;
(4) the throw out powder is calcined 2h down at 400 ℃, obtains mixed oxide powder; Mixed oxide powder carries out reduction reaction under 800 ℃ of conditions, reducing gas is hydrogen, and the restoring operation time was controlled at 25 minutes, can obtain iron copper composite alloy powder.
The powder of the iron copper composite alloy powder of present method preparation is thinner, 1～2 micron of mean particle size range, and it is 3.49% that X fluorometric assay and power spectrum are measured copper content, and iron level 95.66%, other content are less than 1%, and wherein S content 0.008%.
Embodiment 3: this utilizes Steel Plant's spent pickle liquor to prepare the method for iron-copper, and adopting spent pickle liquor and other copper sulfate of technical grade is raw material, and reducing gas is selected hydrogen for use, and its concrete processing step is:
(1) needs according to Fe-4.5Cu powdered alloy elemental composition prescription join copper sulfate in the spent pickle liquor, obtain mixing solutions;
(2) ammoniacal liquor is mixed with spent acid solution in the equimolar basic solution of iron concentration; Basic solution is slowly poured in the mixing solutions, to the pH value of mixing solutions be 9, stirring reaction 50min, ageing 4h filter and obtain mixed sediment;
(3) mixed sediment is through 3 washings, suction filtration, 155 ℃ of dryings, and batch mixing adopts the ball mill grind away to obtain powder granularity at 1～2 micron afterwards, obtains the throw out powder;
(4) the throw out powder is calcined 3h down at 200 ℃, obtains mixed oxide powder; Mixed oxide powder carries out reduction reaction under 900 ℃ of conditions, reducing gas is hydrogen, and the restoring operation time was controlled at 20 minutes.
The iron copper composite alloy powder powder of present method preparation is thinner, 1～2 micron of mean particle size range, and it is 4.58% that X fluorometric assay and power spectrum are measured copper content, and iron level 94.50%, other content are less than 1%, and wherein S content 0.011%.
Claims (10)
1. a method of utilizing Steel Plant's spent pickle liquor to prepare iron-copper is characterized in that, the processing step of this method is: (1) adds copper-bath in spent pickle liquor, perhaps copper sulfate directly is dissolved in the spent pickle liquor, obtains mixing solutions;
(2) add basic solution in the described mixing solutions, stir and react, obtain mixed sediment after ageing, the filtration;
(3) described mixed sediment adopts the ball mill grind away to obtain the throw out powder after washing, filtration, drying;
(4) described throw out powder carries out reduction reaction after calcining, can obtain described iron-copper.
2. the method for utilizing Steel Plant's spent pickle liquor to prepare iron-copper according to claim 1 is characterized in that: the concentration of copper-bath is 1～2mol/L in the described step (1).
3. the method for utilizing Steel Plant's spent pickle liquor to prepare iron-copper according to claim 1, it is characterized in that: the basic solution in the described step (2) is sodium hydroxide solution or ammoniacal liquor; Described basic solution is added into pH value to 7～9 of mixing solutions.
4. the method for utilizing Steel Plant's spent pickle liquor to prepare iron-copper according to claim 3 is characterized in that: volumetric molar concentration such as iron ion in the concentration of described basic solution and the spent acid solution.
5. the method for utilizing Steel Plant's spent pickle liquor to prepare iron-copper according to claim 1, it is characterized in that: the reaction times in the described step (2) is 30～50min, digestion time is 3～4h.
6. the method for utilizing Steel Plant's spent pickle liquor to prepare iron-copper according to claim 1, it is characterized in that: the drying temperature in the described step (3) is 135～155 ℃.
7. the method for utilizing Steel Plant's spent pickle liquor to prepare iron-copper according to claim 1 is characterized in that: mixed sediment is through 2～3 washings in the described step (3).
8. the method for utilizing Steel Plant's spent pickle liquor to prepare iron-copper according to claim 1, it is characterized in that: described step (3) grind away to throw out powder granularity is 1～2 micron.
9. according to any described method of utilizing Steel Plant's spent pickle liquor to prepare iron-copper of claim 1-8, it is characterized in that: the throw out powder in the described step (4) is calcined 1～3h down at 200～500 ℃.
10. according to any described method of utilizing Steel Plant's spent pickle liquor to prepare iron-copper of claim 1-8, it is characterized in that: reduction reaction temperature is 700～900 ℃ in the described step (4), reducing gas is coke-oven gas or hydrogen, and the recovery time is 20～28 minutes.
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| CN201310129196XA CN103205578A (en) | 2013-04-15 | 2013-04-15 | Method for preparing iron-copper alloy by using waste pickling liquid in steelworks |
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| CN201310129196XA CN103205578A (en) | 2013-04-15 | 2013-04-15 | Method for preparing iron-copper alloy by using waste pickling liquid in steelworks |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108672714A (en) * | 2018-04-24 | 2018-10-19 | 上海大学 | The method that alloy powder is directly prepared by cold rolling sludge |
| CN114230080A (en) * | 2021-12-24 | 2022-03-25 | 云南科力环保股份公司 | Zero-discharge treatment method for platinum noble metal wastewater |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1386710A (en) * | 2001-05-21 | 2002-12-25 | 邵建华 | Process for preparing superfine iron oxide |
| CN1388257A (en) * | 2001-05-28 | 2003-01-01 | 中国科学院山西煤炭化学研究所 | Regeneration process of copper or iron system desulfurizing agent |
| CN102180521A (en) * | 2011-03-15 | 2011-09-14 | 浙江工业大学 | Method for preparing ferric oxide red pigment by using nitryl chloride tail gas |
| CN102689930A (en) * | 2011-03-24 | 2012-09-26 | 镇江市丹徒区江南热镀锌有限公司 | Hydrochloric acid pickling waste liquid resource integrated utilization method for preparing iron oxide and ammonium sulfate |
| CN102747225A (en) * | 2012-07-10 | 2012-10-24 | 中南大学 | Method for comprehensively recycling copper, selenium and uranium from stone coal extraction vanadic acid immersion liquid |
-
2013
- 2013-04-15 CN CN201310129196XA patent/CN103205578A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1386710A (en) * | 2001-05-21 | 2002-12-25 | 邵建华 | Process for preparing superfine iron oxide |
| CN1388257A (en) * | 2001-05-28 | 2003-01-01 | 中国科学院山西煤炭化学研究所 | Regeneration process of copper or iron system desulfurizing agent |
| CN102180521A (en) * | 2011-03-15 | 2011-09-14 | 浙江工业大学 | Method for preparing ferric oxide red pigment by using nitryl chloride tail gas |
| CN102689930A (en) * | 2011-03-24 | 2012-09-26 | 镇江市丹徒区江南热镀锌有限公司 | Hydrochloric acid pickling waste liquid resource integrated utilization method for preparing iron oxide and ammonium sulfate |
| CN102747225A (en) * | 2012-07-10 | 2012-10-24 | 中南大学 | Method for comprehensively recycling copper, selenium and uranium from stone coal extraction vanadic acid immersion liquid |
Non-Patent Citations (1)
| Title |
|---|
| 张敬国等: "以含铜废液为原料制备铜铁复合粉的工艺研究", 《稀有金属》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108672714A (en) * | 2018-04-24 | 2018-10-19 | 上海大学 | The method that alloy powder is directly prepared by cold rolling sludge |
| CN114230080A (en) * | 2021-12-24 | 2022-03-25 | 云南科力环保股份公司 | Zero-discharge treatment method for platinum noble metal wastewater |
| CN114230080B (en) * | 2021-12-24 | 2024-05-24 | 云南科力环保股份公司 | Zero-emission treatment method for platinum noble metal wastewater |
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Application publication date: 20130717 |