CN104445429A - Method for preparing iron oxide red pigment by using pyrite cinder residue-firing hydrothermal process - Google Patents
Method for preparing iron oxide red pigment by using pyrite cinder residue-firing hydrothermal process Download PDFInfo
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- CN104445429A CN104445429A CN201410636946.7A CN201410636946A CN104445429A CN 104445429 A CN104445429 A CN 104445429A CN 201410636946 A CN201410636946 A CN 201410636946A CN 104445429 A CN104445429 A CN 104445429A
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Abstract
The invention discloses a method for preparing an iron oxide red pigment by using a pyrite cinder residue-firing hydrothermal process. The method comprises the following steps of adding sulfuric acid solutions into a reaction device for intensively stirring at the stirring velocity of 30-50 r/min; then, slowly adding pyrite cinders to react for 2-6 hours at the controlled reaction temperature of 110-120 DEG C to obtain pyrite cinder residue-firing pickle liquid containing ferric sulfate and ferrous sulfate; gradually adding hydrogen peroxide into the obtained pickle liquid; regulating the mole rate of Fe<3+> and Fe<2+> in the solution; adding ammonia water solutions until a pH value reaches the required numeric value; mixing ferric hydroxide and ferrous hydroxide obtained by the reaction with a precursor rubber matrix and turning into a high pressure kettle for performing hydrothermal reaction; washing and filtering a hydrothermal product obtained by the reaction by using deionized water; and drying for 4-6 hours at the temperature of 110-120 DEG C to obtain an iron oxide red product.
Description
Technical field
The invention belongs to pigment technology field, relate to a kind of method of Preparation of ferric oxide from pyrite cinders by hydrothermal method red.
Background technology
Red iron oxide is compound the most stable in the oxide compound of iron, due to the performance that it is superior, as nontoxicity, chemical stability, strong erosion resistance, weathering resistance and low cost etc., be used widely, as building trade pigment, inorganic dyestuff, pottery, plastics, anticorrosive paint, paper industry sorbent material etc.At present, China's red iron oxide is mainly that raw material adopts mixed acid process to produce with iron scale, and ultimate production reaches 700kt/a, occupies first place in the world.Pyrite cinder is a kind of important secondary iron resources, containing a large amount of valuable metal.Be the focus that people pay close attention to pyrite cinder resource utilization efficiency utilization, take pyrite cinder as the existing large quantifier elimination that Iron-based product prepared by raw material, as prepared iron oxide red, iron oxide yellow, barba hispanica, iron oxide black, ferrous salt, martial ethiops, Polyferric Sulfate salt etc. always.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of method of Preparation of ferric oxide from pyrite cinders by hydrothermal method red.
For achieving the above object, the invention provides following technical scheme:
A method for Preparation of ferric oxide from pyrite cinders by hydrothermal method red, comprises the steps:
Sulphuric acid soln is added people in reaction unit, strong stirring, stir speed (S.S.) is about 30 ~ 50r/min, then people's pyrite cinder is slowly added, control temperature of reaction at 110 ~ 120 DEG C, after reaction 4 ~ 6h, obtain the pyrite cinder pickling liquor of sulfur acid iron and ferrous sulfate, pickling liquor to gained adds people's hydrogen peroxide gradually, Fe in adjustment solution
3+with Fe
2+mol ratio, then people's ammonia soln is added, until pH value reaches required numerical value, the ironic hydroxide of reaction gained and ferrous hydroxide mixing precursor colloids are turned people's autoclave, carry out hydro-thermal reaction, the hydrothermal product of reaction gained through deionized water wash, filtration, and at 110 ~ 120 DEG C dry 4 ~ 6h, namely obtain red iron oxide product.
Preferably, stirring velocity is 40r/min.
Preferably, control temperature of reaction at 115 DEG C, reaction 5h.
Preferably, described Fe
3+/ Fe
2+mol ratio is 1.5 ~ 2.0.
Preferably, reaction gained hydrothermal product through deionized water wash, filtration, and at 115 DEG C dry 5h.
The method of Preparation of ferric oxide from pyrite cinders by hydrothermal method red of the present invention is that raw material can prepare high-performance bright red ferric oxide red colorant under proper condition with pyrite cinder.
Embodiment
Be described in detail to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art obtain under the prerequisite not making creative work, all belongs to the scope of protection of the invention.
Embodiment 1
Sulphuric acid soln is added people in reaction unit, strong stirring, stir speed (S.S.) is about 30r/min, then people's pyrite cinder is slowly added, control temperature of reaction at 110 DEG C, after reaction 6h, obtain the pyrite cinder pickling liquor of sulfur acid iron and ferrous sulfate, pickling liquor to gained adds people's hydrogen peroxide gradually, Fe in adjustment solution
3+with Fe
2+mol ratio is 1.5, then people's ammonia soln is added, until pH value reaches required numerical value, the ironic hydroxide of reaction gained and ferrous hydroxide mixing precursor colloids are turned people's autoclave, carry out hydro-thermal reaction, the hydrothermal product of reaction gained through deionized water wash, filtration, and at 110 DEG C dry 6h, namely obtain red iron oxide product.
Embodiment 2
Sulphuric acid soln is added people in reaction unit, strong stirring, stir speed (S.S.) is about 50r/min, then people's pyrite cinder is slowly added, control temperature of reaction at 120 DEG C, after reaction 4h, obtain the pyrite cinder pickling liquor of sulfur acid iron and ferrous sulfate, pickling liquor to gained adds people's hydrogen peroxide gradually, Fe in adjustment solution
3+with Fe
2+mol ratio is 2.0, then people's ammonia soln is added, until pH value reaches required numerical value, the ironic hydroxide of reaction gained and ferrous hydroxide mixing precursor colloids are turned people's autoclave, carry out hydro-thermal reaction, the hydrothermal product of reaction gained through deionized water wash, filtration, and at 120 DEG C dry 4h, namely obtain red iron oxide product.
Embodiment 3
Sulphuric acid soln is added people in reaction unit, strong stirring, stir speed (S.S.) is about 40r/min, then people's pyrite cinder is slowly added, control temperature of reaction at 115 DEG C, after reaction 5h, obtain the pyrite cinder pickling liquor of sulfur acid iron and ferrous sulfate, pickling liquor to gained adds people's hydrogen peroxide gradually, Fe in adjustment solution
3+with Fe
2+mol ratio is 1.8, then people's ammonia soln is added, until pH value reaches required numerical value, the ironic hydroxide of reaction gained and ferrous hydroxide mixing precursor colloids are turned people's autoclave, carry out hydro-thermal reaction, the hydrothermal product of reaction gained through deionized water wash, filtration, and at 115 DEG C dry 5h, namely obtain red iron oxide product.
In those skilled in the art, obviously the invention is not restricted to the details of above-mentioned one exemplary embodiment, and when not deviating from spirit of the present invention or essential characteristic, the present invention can be realized in other specific forms.Therefore, no matter from which point, all should embodiment be regarded as exemplary, and be nonrestrictive, scope of the present invention is limited by claims instead of above-mentioned explanation, and all changes be therefore intended in the implication of the equivalency by dropping on claim and scope are included in the present invention.
In addition, be to be understood that, although this specification sheets is described according to embodiment, but not each embodiment only comprises an independently technical scheme, this narrating mode of specification sheets is only for clarity sake, those skilled in the art should by specification sheets integrally, and the technical scheme in each embodiment also through appropriately combined, can form other embodiments that it will be appreciated by those skilled in the art that.
Claims (5)
1. a method for Preparation of ferric oxide from pyrite cinders by hydrothermal method red, is characterized in that, comprises the steps:
Sulphuric acid soln is added people in reaction unit, strong stirring, stir speed (S.S.) is about 30 ~ 50r/min, then people's pyrite cinder is slowly added, control temperature of reaction at 110 ~ 120 DEG C, after reaction 4 ~ 6h, obtain the pyrite cinder pickling liquor of sulfur acid iron and ferrous sulfate, pickling liquor to gained adds people's hydrogen peroxide gradually, Fe in adjustment solution
3+with Fe
2+mol ratio, then people's ammonia soln is added, until pH value reaches required numerical value, the ironic hydroxide of reaction gained and ferrous hydroxide mixing precursor colloids are turned people's autoclave, carry out hydro-thermal reaction, the hydrothermal product of reaction gained through deionized water wash, filtration, and at 110 ~ 120 DEG C dry 4 ~ 6h, namely obtain red iron oxide product.
2. the method for Preparation of ferric oxide from pyrite cinders by hydrothermal method red according to claim 1, is characterized in that: stirring velocity is 40r/min.
3. the method for Preparation of ferric oxide from pyrite cinders by hydrothermal method red according to claim 1, is characterized in that: control temperature of reaction at 115 DEG C, reaction 5h.
4. the method for Preparation of ferric oxide from pyrite cinders by hydrothermal method red according to claim 1, is characterized in that: described Fe
3+/ Fe
2+mol ratio is 1.5 ~ 2.0.
5. the method for Preparation of ferric oxide from pyrite cinders by hydrothermal method red according to claim 1, is characterized in that: reaction gained hydrothermal product through deionized water wash, filtration, and at 115 DEG C dry 5h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410636946.7A CN104445429A (en) | 2014-11-13 | 2014-11-13 | Method for preparing iron oxide red pigment by using pyrite cinder residue-firing hydrothermal process |
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| CN201410636946.7A CN104445429A (en) | 2014-11-13 | 2014-11-13 | Method for preparing iron oxide red pigment by using pyrite cinder residue-firing hydrothermal process |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385858A (en) * | 2015-11-03 | 2016-03-09 | 中南大学 | Method for preparing iron oxide red and recycling silver through ferroalumen residues |
| CN106430326A (en) * | 2016-10-17 | 2017-02-22 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for producing high-performance iron oxide red from hydrothermal ultra-fine grains |
| RU2655336C1 (en) * | 2017-05-23 | 2018-05-25 | Валерий Константинович Ларин | Method of obtaining iron oxide pigments |
| RU2657489C1 (en) * | 2017-05-23 | 2018-06-14 | Валерий Константинович Ларин | Method for producing iron oxide pigment |
| CN108706562A (en) * | 2018-08-14 | 2018-10-26 | 武汉轻工大学 | A method of preparing ferric phosphate using pyrite cinder |
| CN109810546A (en) * | 2019-04-04 | 2019-05-28 | 河北工业大学 | The method for preparing shiny red iron oxide red hybrid pigment using iron tailings |
| CN109912995A (en) * | 2019-04-04 | 2019-06-21 | 河北工业大学 | There is the method for far-infrared transmitting function iron oxide red hybrid pigment using iron tailings preparation |
| CN109929414A (en) * | 2019-03-20 | 2019-06-25 | 重庆三峡油漆股份有限公司 | A kind of antirusting paint comprising ferrous disulfide |
| CN114906830A (en) * | 2022-07-19 | 2022-08-16 | 昆明川金诺化工股份有限公司 | Method for controllably preparing battery-grade iron phosphate from pyrite cinder |
-
2014
- 2014-11-13 CN CN201410636946.7A patent/CN104445429A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 郑雅杰等: "用水热法从硫铁矿烧渣制备氧化铁", 《金属矿山》 * |
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105385858A (en) * | 2015-11-03 | 2016-03-09 | 中南大学 | Method for preparing iron oxide red and recycling silver through ferroalumen residues |
| CN106430326A (en) * | 2016-10-17 | 2017-02-22 | 中国有色集团（广西）平桂飞碟股份有限公司 | Method for producing high-performance iron oxide red from hydrothermal ultra-fine grains |
| CN106430326B (en) * | 2016-10-17 | 2018-02-06 | 中国有色集团（广西）平桂飞碟股份有限公司 | The method of the ultra-fine seed production high-performance iron oxide red of hydro-thermal |
| RU2655336C1 (en) * | 2017-05-23 | 2018-05-25 | Валерий Константинович Ларин | Method of obtaining iron oxide pigments |
| RU2657489C1 (en) * | 2017-05-23 | 2018-06-14 | Валерий Константинович Ларин | Method for producing iron oxide pigment |
| CN108706562A (en) * | 2018-08-14 | 2018-10-26 | 武汉轻工大学 | A method of preparing ferric phosphate using pyrite cinder |
| CN109929414A (en) * | 2019-03-20 | 2019-06-25 | 重庆三峡油漆股份有限公司 | A kind of antirusting paint comprising ferrous disulfide |
| CN109810546A (en) * | 2019-04-04 | 2019-05-28 | 河北工业大学 | The method for preparing shiny red iron oxide red hybrid pigment using iron tailings |
| CN109912995A (en) * | 2019-04-04 | 2019-06-21 | 河北工业大学 | There is the method for far-infrared transmitting function iron oxide red hybrid pigment using iron tailings preparation |
| CN109912995B (en) * | 2019-04-04 | 2020-12-25 | 河北工业大学 | Method for preparing iron oxide red hybrid pigment with far infrared emission function by using iron tailings |
| CN109810546B (en) * | 2019-04-04 | 2020-12-29 | 河北工业大学 | Method for preparing bright red iron oxide red hybrid pigment by using iron tailings |
| CN114906830A (en) * | 2022-07-19 | 2022-08-16 | 昆明川金诺化工股份有限公司 | Method for controllably preparing battery-grade iron phosphate from pyrite cinder |
| CN114906830B (en) * | 2022-07-19 | 2022-10-14 | 昆明川金诺化工股份有限公司 | Method for controllably preparing battery-grade iron phosphate from pyrite cinder |
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Application publication date: 20150325 |