CN104445431A - Method for preparing high-purity iron oxide red from pyrites slag - Google Patents
Method for preparing high-purity iron oxide red from pyrites slag Download PDFInfo
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- CN104445431A CN104445431A CN201410644872.1A CN201410644872A CN104445431A CN 104445431 A CN104445431 A CN 104445431A CN 201410644872 A CN201410644872 A CN 201410644872A CN 104445431 A CN104445431 A CN 104445431A
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- iron oxide
- oxide red
- pyrite cinder
- magnetic separation
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Abstract
The invention discloses a method for preparing high-purity iron oxide red from pyrites slag. The method is characterized by comprising the following steps: (1) grinding raw ore into a certain particle size, carrying out magnetic separation by a magnetic separator so as to improve the grade of iron, filtering and drying materials which are subjected to the magnetic separation; (2) carrying out acid leaching on the slag which is subjected to the magnetic separation with sulfuric acid, so as to prepare a ferric sulfate solution; (3) filtering a leaching solution, adding reduced iron powder and reacting, so as to prepare a ferrous sulphate solution; (4) filtering the ferrous sulphate solution, adding ammonium bicarbonate and reacting, so as to prepare ferrous carbonate sediments; (5) filtering reacted solution, extracting filter residues, and drying the ferrous carbonate sediments in a drying baker; and (6) calcining the burnt ferrous carbonate sediments, and reacting to obtain an iron oxide red product. The method is easy to practically apply, and good in impurity removal effect; the problem of environment pollution caused by the abandoned pyrites slag for a long period of time can be solved; and meanwhile, good economic benefits can be obtained.
Description
Technical field
The invention belongs to blast furnace ferrous furnace charge sorting enrichment and carry out the new technology of processing product, relating to a kind of pyrite cinder and clean sorting Beneficiation novel process, be i.e. " pyrite cinder is prepared high-purity iron oxide red " novel process.
Background technology
Pyrite cinder is that sulfurous iron ore produces a kind of industrial residue produced in the process of sulfuric acid.China has millions of tons pyrite cinder to discharge every year, causes severe contamination to environment.Pyrite cinder has certain damaging effect to environment, but in slag, iron-holder is higher, and containing other valuable metal element a certain amount of, can be used, and its utilization is conducive to environment sustainable development as secondary resource.
Summary of the invention
The object of the invention is to utilize pyrite cinder to prepare highly purified red iron oxide product.This technique comprises and adds iron powder and prepare copperas solution, building-up reactions generates precipitation, drying and calcining obtains the steps such as red iron oxide, and this had both achieved the object preparing high purity product, prepares high-purity iron oxide red product again provide new method for pyrite cinder.
Technical scheme of the present invention is: a kind of pyrite cinder prepares high-purity iron oxide red method, comprises the following steps:
(1) raw ore is ground certain granularity, improve the grade of iron through magnetic separator magnetic separation, the material filtering after magnetic separation is dried;
(2) by the slag after magnetic separation, ferrum sulfuricum oxydatum solutum is obtained with vitriol lixiviation;
(3) filter leach liquor, add reduced iron powder reaction, obtained copperas solution;
(4) filter copperas solution, add bicarbonate of ammonia reaction, obtained iron protocarbonate precipitation;
(5) filter reacted solution, extract filter residue, dry carbonic acid ferrous precipitation in drying baker;
(6) the iron protocarbonate precipitation that calcining is dry, reacts to obtain red iron oxide product.
Above-mentioned pyrite cinder iron-holder 39.22%, gangue mineral is mainly containing SiO
2, and containing Al
2o
3, CaO and CaSO
4.
The grinding fineness of above-mentioned pyrite cinder is that massfraction 75 ~ 80% is less than 0.178mm.
It is 15 ~ 20% that above-mentioned magnetic separator stirs feeding trough feed ore concentration, and through three stages of magnetic separation, magnetic separation electric current is respectively 10 ~ 14A, 5 ~ 7A, 2.5 ~ 3.5A; Control ore pulp to the ore deposit time, middlely rush the time, the essence time of rushing is respectively 2 ~ 4s, 10s and 10s.
Above-mentioned acidleach temperature is 100 ~ 110 DEG C; Excess sulfuric acid coefficient is 2.50 ~ 3.00; Leaching time is 60 ~ 75min.
The above-mentioned bath temperature adding Fe3+ reduction is 75 ~ 85 DEG C; Reaction times is 140 ~ 160min.
The water-bath synthesis temperature of above-mentioned building-up reactions is 45 ~ 55 DEG C; The ratio of components of bicarbonate of ammonia is 3 ~ 3.5, stirs 10 ~ 15min, leaves standstill 45 ~ 50min.
Above-mentioned drying temperature is 85 ~ 95 DEG C, and time of drying is 110 ~ 130min.
The temperature of above-mentioned calcination reaction is 650 ~ 750 DEG C, and calcination time is 50 ~ 70min, opens fire door 10 ~ 15s every 15 ~ 20min.
Beneficial effect of the present invention: (1), through repeatedly magnetic separation, can make the content minimizing of the content enrichment of iron, impurity on the one hand, can enhance productivity on the other hand.
(2) object of vitriol lixiviation is under certain condition, adds sulfuric acid by Fe in the slag after mill ore magnetic selection
2o
3convert Fe to
2(SO
4)
3, partial impurities can be made as CaO, Al simultaneously
2o
3be transformed into CaSO
4, Al
2(SO
4)
3, for next step purification is got ready.
(3) main containing Ca in the solution after acidleach
2+, Al
3+, Mg
2+deng foreign ion, can utilize these ions under some specific pH value, generate corresponding precipitation of hydroxide and carry out removal of impurities.Because ferric degree of hydrolysis is very high, be far longer than ferrous iron, ferrum sulfuricum oxydatum solutum can be made to be reacted into copperas solution, make the pH value of solution increase fast so add iron powder, the potential of hydrogen changing solution makes contamination precipitation.
(4) join in the middle of ammonium bicarbonate soln with the ferrous sulfate produced, slowly add during beginning, after waiting crystal seed to be formed, add fast, crystal seed can be made to grow up rapidly, just can obtain comparatively pure iron protocarbonate precipitation.
(5) object of calcine tests is that dried iron protocarbonate is transformed into red iron oxide product, need when testing strictly to control calcining temperature (about 200 DEG C ~ 1000 DEG C), in the process of calcining, open fire door every for some time simultaneously, its reaction raw materials air is entered, iron protocarbonate obtains enough oxygen and is transformed into red iron oxide, and discharges reaction product carbonic acid gas and sulphur trioxide.
Accompanying drawing explanation
Fig. 1 is that pyrite cinder prepares high-purity iron oxide red process flow sheet.
Embodiment
Example 1: by iron content 39.22%, gangue mineral is mainly containing SiO
2, and containing a small amount of Al
2o
3, CaO and CaSO
4pyrite cinder grind, meet 0.178mm sieving rate and reach 78%, be then modulated into the pulp density of 20%, through three stages of magnetic separation of I=12A, 6A, 3A; The processing condition of vitriol lixiviation are acidleach temperature is 105 DEG C, and excess sulfuric acid coefficient is 2.70, and leaching time is 65min; The processing condition adding Fe3+ reduction are bath temperature is 80 DEG C, and the reaction times is 150min, and the excess coefficient of iron is 1.5; The processing condition of building-up reactions are water-bath synthesis temperature is 50 DEG C, and the ratio of components of bicarbonate of ammonia is 3.3, stirs 15min, leaves standstill 45min; The processing condition of calcination reaction are calcining temperature is 700 DEG C, and calcination time is 60min, opens fire door 15s every 15min.The highly purified red iron oxide that purity is 99.21% is obtained according to above-mentioned technique.
Example 2: by iron content 39.22%, gangue mineral is mainly containing SiO
2, and containing a small amount of Al
2o
3, CaO and CaSO
4pyrite cinder grind, meet 0.178mm sieving rate and reach 75%, be then modulated into the pulp density of 20%, through three stages of magnetic separation of I=10A, 5A, 2.5A; The processing condition of vitriol lixiviation are acidleach temperature is 100 DEG C, and excess sulfuric acid coefficient is 2.50, and leaching time is 60min; The processing condition adding Fe3+ reduction are bath temperature is 75 DEG C, and the reaction times is 140min, and the excess coefficient of iron is 1.5; The processing condition of building-up reactions are water-bath synthesis temperature is 45 DEG C, and the ratio of components of bicarbonate of ammonia is 3, stirs 10min, leaves standstill 45min; The processing condition of calcination reaction are calcining temperature is 650 DEG C, and calcination time is 50min, opens fire door 15s every 10min.The highly purified red iron oxide that purity is 99.21% is obtained according to above-mentioned technique.
Example 3: by iron content 39.22%, gangue mineral is mainly containing SiO
2, and containing a small amount of Al
2o
3, CaO and CaSO
4pyrite cinder grind, meet 0.178mm sieving rate and reach 80%, be then modulated into the pulp density of 20%, through three stages of magnetic separation of I=14A, 7A, 3.5A; The processing condition of vitriol lixiviation are acidleach temperature is 110 DEG C, and excess sulfuric acid coefficient is 3.00, and leaching time is 75min; The processing condition adding Fe3+ reduction are bath temperature is 85 DEG C, and the reaction times is 160min, and the excess coefficient of iron is 1.5; The processing condition of building-up reactions are water-bath synthesis temperature is 55 DEG C, and the ratio of components of bicarbonate of ammonia is 3.5, stirs 15min, leaves standstill 50min; The processing condition of calcination reaction are calcining temperature is 750 DEG C, and calcination time is 70min, opens fire door 20s every 15min.The highly purified red iron oxide that purity is 99.21% is obtained according to above-mentioned technique.
Claims (9)
1. pyrite cinder prepares a high-purity iron oxide red method, it is characterized in that: comprise the following steps:
(1) raw ore is ground certain granularity, improve the grade of iron through magnetic separator magnetic separation, the material filtering after magnetic separation is dried;
(2) by the slag after magnetic separation, ferrum sulfuricum oxydatum solutum is obtained with vitriol lixiviation;
(3) filter leach liquor, add reduced iron powder reaction, obtained copperas solution;
(4) filter copperas solution, add bicarbonate of ammonia reaction, obtained iron protocarbonate precipitation;
(5) filter reacted solution, extract filter residue, dry carbonic acid ferrous precipitation in drying baker;
(6) the iron protocarbonate precipitation that calcining is dry, reacts to obtain red iron oxide product.
2. a kind of pyrite cinder according to claim 1 prepares high-purity iron oxide red method, it is characterized in that: above-mentioned pyrite cinder iron-holder 39.22%, and gangue mineral is mainly containing SiO
2, and containing Al
2o
3, CaO and CaSO
4.
3. a kind of pyrite cinder according to claim 1 prepares high-purity iron oxide red method, it is characterized in that: the grinding fineness of above-mentioned pyrite cinder is that massfraction 75 ~ 80% is less than 0.178mm.
4. a kind of pyrite cinder according to claim 1 prepares high-purity iron oxide red method, it is characterized in that: it is 15 ~ 20% that above-mentioned magnetic separator stirs feeding trough feed ore concentration, through three stages of magnetic separation, magnetic separation electric current is respectively 10 ~ 14A, 5 ~ 7A, 2.5 ~ 3.5A; Control ore pulp to the ore deposit time, middlely rush the time, the essence time of rushing is respectively 2 ~ 4s, 10s and 10s.
5. a kind of pyrite cinder according to claim 1 prepares high-purity iron oxide red method, it is characterized in that: above-mentioned acidleach temperature is 100 ~ 110 DEG C; Excess sulfuric acid coefficient is 2.50 ~ 3.00; Leaching time is 60 ~ 75min.
6. a kind of pyrite cinder according to claim 1 prepares high-purity iron oxide red method, it is characterized in that: the above-mentioned bath temperature adding Fe3+ reduction is 75 ~ 85 DEG C; Reaction times is 140 ~ 160min.
7. a kind of pyrite cinder according to claim 1 prepares high-purity iron oxide red method, it is characterized in that: the water-bath synthesis temperature of above-mentioned building-up reactions is 45 ~ 55 DEG C; The ratio of components of bicarbonate of ammonia is 3 ~ 3.5, stirs 10 ~ 15min, leaves standstill 45 ~ 50min.
8. a kind of pyrite cinder according to claim 1 prepares high-purity iron oxide red method, it is characterized in that: above-mentioned drying temperature is 85 ~ 95 DEG C, and time of drying is 110 ~ 130min.
9. a kind of pyrite cinder according to claim 1 prepares high-purity iron oxide red method, it is characterized in that: the temperature of above-mentioned calcination reaction is 650 ~ 750 DEG C, and calcination time is 50 ~ 70min, opens fire door 10 ~ 15s every 15 ~ 20min.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105671311A (en) * | 2016-01-21 | 2016-06-15 | 昆明理工大学 | Processing method of iron ore |
| CN105668644A (en) * | 2016-01-17 | 2016-06-15 | 济南大学 | Iron-based colouring agent prepared by using waste warm pastes |
| CN109368610A (en) * | 2018-10-09 | 2019-02-22 | 湖南雅城新材料有限公司 | A method of using pyrite cinder preparation high-speed rail phosphorus than ferric phosphate |
| CN111377484A (en) * | 2020-03-20 | 2020-07-07 | 安庆市长虹化工有限公司 | Pyrite resource recovery processing method |
| CN113104902A (en) * | 2021-04-07 | 2021-07-13 | 江西理工大学 | Method for preparing iron oxide red from magnetic material waste acid leaching residues |
| CN113426415A (en) * | 2021-07-19 | 2021-09-24 | 湖南大学 | Iron-based biochar composite material and preparation method and application thereof |
| CN113582238A (en) * | 2021-08-12 | 2021-11-02 | 山东春光磁电科技有限公司 | Preparation method of iron source for manganese-zinc ferrite |
| CN115849456A (en) * | 2022-12-14 | 2023-03-28 | 湖北虹润高科新材料有限公司 | Method for preparing iron oxide by using pyrite cinder and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105668644A (en) * | 2016-01-17 | 2016-06-15 | 济南大学 | Iron-based colouring agent prepared by using waste warm pastes |
| CN105671311A (en) * | 2016-01-21 | 2016-06-15 | 昆明理工大学 | Processing method of iron ore |
| CN109368610A (en) * | 2018-10-09 | 2019-02-22 | 湖南雅城新材料有限公司 | A method of using pyrite cinder preparation high-speed rail phosphorus than ferric phosphate |
| CN109368610B (en) * | 2018-10-09 | 2020-10-27 | 湖南雅城新材料有限公司 | Method for preparing iron phosphate with high iron-phosphorus ratio by using pyrite cinder |
| CN111377484A (en) * | 2020-03-20 | 2020-07-07 | 安庆市长虹化工有限公司 | Pyrite resource recovery processing method |
| CN113104902A (en) * | 2021-04-07 | 2021-07-13 | 江西理工大学 | Method for preparing iron oxide red from magnetic material waste acid leaching residues |
| CN113426415A (en) * | 2021-07-19 | 2021-09-24 | 湖南大学 | Iron-based biochar composite material and preparation method and application thereof |
| CN113582238A (en) * | 2021-08-12 | 2021-11-02 | 山东春光磁电科技有限公司 | Preparation method of iron source for manganese-zinc ferrite |
| CN115849456A (en) * | 2022-12-14 | 2023-03-28 | 湖北虹润高科新材料有限公司 | Method for preparing iron oxide by using pyrite cinder and application thereof |
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Application publication date: 20150325 |