CN102153148A - Method for preparing iron oxide red - Google Patents
Method for preparing iron oxide red Download PDFInfo
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- CN102153148A CN102153148A CN2011101159825A CN201110115982A CN102153148A CN 102153148 A CN102153148 A CN 102153148A CN 2011101159825 A CN2011101159825 A CN 2011101159825A CN 201110115982 A CN201110115982 A CN 201110115982A CN 102153148 A CN102153148 A CN 102153148A
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Abstract
The invention provides a method for preparing iron oxide red by utilizing a solution containing iron ions, wherein the iron ions are at least one kind of ferrous ions and ferric ions. The method comprises the following steps of: (1) adding the solution containing iron ions into a reactor; (2) adjusting the pH value of the solution to be 0.5-3.0; (3) adjusting the temperature in the reactor to be 180-220 DEG C, maintaining the temperature for a predetermined time at oxidizing atmosphere to obtain a solid-liquid mixture containing ferric oxides; and (4) carrying out solid liquid separation on the solid-liquid mixture to obtain an iron oxide red product. By utilizing the method, iron in the solution can be effectively recycled and the iron oxide red can be prepared.
Description
Technical field
The present invention relates to chemical field, particularly, relate to from the method for the formulations prepared from solutions iron oxide red that contains iron ion.
Background technology
At present when wet production zinc, nickel, cobalt or other valuable metal, adopt acid leaching process usually, when valuable metal was leached, the iron in the ore was also leached.Comprise this step of deironing in the follow-up cleaning section, usually adopt yellow (sodium, ammonium) siderotil or separation of iron in goethite form in the industry, i.e. control is leached the back liquid temp under higher level, in leach liquor, introduce sodium/potassium/ammonium ion, be combined to siderotil with iron ion wherein, or ferric iron in the leach liquor is reduced to divalence, under oxidizing condition, iron is pyrrhosiderite and removes.Sending into tailing dam after scum after the deironing washs after filtration stores up.The quantity of slag is big after this method deironing, and this slag can't use as resources circulation at present, take not only that a large amount of soils are stored up and wherein the slow stripping of unwanted component caused environmental pollution.
Summary of the invention
The present invention is intended to solve at least one of technical problem that exists in the prior art.For this reason, one object of the present invention is to propose a kind of method for preparing iron oxide red from the solution that contains iron ion.
According to embodiments of the invention, the invention provides a kind of method from the formulations prepared from solutions iron oxide red that contains iron ion, wherein, described iron ion is be selected from ferrous ion and ferric ion at least a, said method comprising the steps of: (1) joins the described solution that contains iron ion in the reactor; (2) regulate the pH value of described solution to 0.5-3.0; (3) regulate the interior temperature of described reactor to 180-220 degree centigrade, and under oxidizing atmosphere, continue preset time, obtain to contain the solidliquid mixture of ferric oxide; (4) described solidliquid mixture is carried out solid-liquid separation, obtain the iron oxide red product.
By the method for preparing iron oxide red, can from the solution that contains iron ion, prepare iron oxide red expeditiously according to the embodiment of the invention.
In addition, the method for preparing iron oxide red according to the above embodiment of the present invention can also have following additional technical characterictic:
According to one embodiment of present invention, use the pH value of the described solution of at least a adjusting that is selected from potassium hydroxide, sodium hydroxide and ammoniacal liquor.
According to one embodiment of present invention, described oxidizing atmosphere is to realize by feed the gas that contains oxygen in described reactor.
According to one embodiment of present invention, described preset time is 0.5-2.5 hour.
According to one embodiment of present invention, the part with described iron oxide red product is back in the reactor as crystal seed.
According to one embodiment of present invention, described solidliquid mixture is carried out solid-liquid separation, obtain the iron oxide red product and comprise: described solidliquid mixture is filtered, obtain containing the filter cake of ferric oxide; Described filter cake is washed, and drying obtains described iron oxide red product.Utilization prepares iron oxide red according to the method for the embodiment of the invention, can reclaim the iron more than 90% in the solution that contains iron ion.Can at utmost reclaim iron.In addition, the method for preparing iron oxide red according to the embodiment of the invention has versatility, can be applicable to the various solution that contain iron ion, for example leach liquor in the metallurgical industry etc.For leach liquor, be higher than existing ferrovanadium method for removing iron according to the efficient of its deironing of method of the embodiment of the invention, can solve scum effectively and store up problem, created condition for no slag production, alleviated environmental pressure.The quality product of the iron oxide red that obtains according to the method for the embodiment of the invention can directly apply to multiple field.
According to one embodiment of present invention, the liquid and the solid weight ratio of carrying out described washing is 3-5: 1.
According to one embodiment of present invention, under 80-120 degree centigrade temperature, carry out described drying.
According to one embodiment of present invention, regulate the pH value of described solution to 2.1-2.3.
According to one embodiment of present invention, described container is an autoclave, and the pressure in the described autoclave is 1.0-1.5MPa, and the dividing potential drop of described oxygen is 0.1-0.5MPa.
Additional aspect of the present invention and advantage part in the following description provide, and part will become obviously from the following description, or recognize by practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage are from obviously and easily understanding becoming the description of embodiment in conjunction with following accompanying drawing, wherein:
Fig. 1 is the schematic flow sheet for preparing the method for iron oxide red according to an embodiment of the invention.
Embodiment
Describe embodiments of the invention below in detail, the example of described embodiment is shown in the drawings, and wherein identical from start to finish or similar label is represented identical or similar elements or the element with identical or similar functions.Below by the embodiment that is described with reference to the drawings is exemplary, only is used to explain the present invention, and can not be interpreted as limitation of the present invention.
Unless offer some clarification on, employed term has implication known in those skilled in the art in specification sheets of the present invention and claims.In this article, term " iron oxide red ", " ferric oxide ", " red iron oxide ", " ferric oxide " can exchange use.
According to embodiments of the invention, the invention provides a kind of method from the formulations prepared from solutions iron oxide red that contains iron ion.According to embodiments of the invention, in solution, the valence state that iron presented is not particularly limited, iron ion can be for being selected from least a of ferrous ion and ferric ion, promptly, can be single ferrous ion, single ferric ion also can be the combination of ferrous ion and ferric ion.According to embodiments of the invention,, may further comprise the steps from the above-mentioned method that contains the formulations prepared from solutions iron oxide red of iron ion with reference to figure 1:
S100: the solution that will contain iron ion joins in the reactor.According to embodiments of the invention, the raw-material source of containing the solution of iron ion of conduct that can be used to prepare iron oxide red is not particularly limited.According to embodiments of the invention, the solution that contains iron ion is that nickel ores, zinc ore, cobalt ore etc. are leaching resulting leach liquor in the treating processes through wet method.Those skilled in the art are surprised to find the leach liquor that this method goes for above-mentioned ore, although wherein the content of iron is lower, the composition complexity of leach liquor, by this processing, can reduce the content of iron in the leach liquor, realize purifying the purpose of leach liquor, can reclaim iron oxide red simultaneously, improve using value, reduced the industry cost.According to embodiments of the invention, the type that can be used in container of the invention process is not particularly limited.According to embodiments of the invention, can adopt the reactor that can bear High Temperature High Pressure.Thus, can in this reactor, realize high-throughput, reaction fast and efficiently, improve the efficient of preparation iron oxide red.
S200: the pH value of regulating described solution is to 0.5-3.0, preferred 2.1-2.3.According to embodiments of the invention, the means of regulating pH are not particularly limited.According to embodiments of the invention, use the pH value of the described solution of at least a adjusting that is selected from potassium hydroxide, sodium hydroxide and ammoniacal liquor.The applicant finds, common leach liquor in the solution that contains iron ion, the especially field of metallurgy in the suitable various sources of these conditioning agents.Leach liquor when especially being fit to wet production zinc, nickel.
S300: regulate the interior temperature of described reactor to 180-220 degree centigrade, and under oxidizing atmosphere, continue preset time, obtain to contain the solidliquid mixture of ferric oxide; According to embodiments of the invention, oxidizing atmosphere is to realize by feed the gas that contains oxygen in described reactor.The gas that contains oxygen described here can be air.According to concrete example of the present invention, also can adopt pure oxygen, thus, can improve reaction efficiency.According to embodiments of the invention, reaction vessel, for example the container in the autoclave is 1.0-1.5MPa, and the dividing potential drop of oxygen is 0.1-0.5MPa.The applicant finds, under this pressure, can realize the efficient production iron oxide red.According to embodiments of the invention, the time that reaction continues, it is described preset time, be not particularly limited, as long as can successfully generate ferric oxide, according to embodiments of the invention, described preset time is 0.5-2.5 hour, thus, can carry out oxidizing reaction fully, obtain ferric oxide.
S400: described solidliquid mixture is carried out solid-liquid separation, obtain the iron oxide red product.According to embodiments of the invention, the method for carrying out solid-liquid separation is not particularly limited, can be for well known to a person skilled in the art equipment and method.For example,, can adopt described solidliquid mixture is filtered, obtain containing the filter cake of ferric oxide according to embodiments of the invention; Described filter cake is washed, and drying obtains described iron oxide red product.By filtration washing, can be further purified the purity of resulting red iron oxide.The red iron oxide of Huo Deing can be used for various fields such as metallurgy, coating, building materials directly as the industrial raw material of multiple industry at last.According to the embodiment of the invention, when washing, washings that is adopted and solid weight ratio are 3-5: 1, can improve washing effect thus.According to embodiments of the invention, wash the washings that is adopted and be not particularly limited, can be water.Carrying out the exsiccant mode and be not particularly limited, can be to carry out drying under 80-120 degree centigrade temperature, and preferred oven dry can cost realizes the drying of iron oxide red product effectively.In addition,, resulting iron oxide red product can be back in the reaction vessel,, thereby improve the iron oxide red crystalline rate as crystal seed according to embodiments of the invention.The crystal size of the final iron oxide red that obtains is the 0.5-1 micron.Return reaction vessel and be not particularly limited, can be the 1/8-1/2 of resultant iron oxide red quality product as the amount of the iron oxide red product of crystal seed, promptly the internal circulating load of crystal seed be 2-8 doubly.
Method according to the embodiment of the invention one of has the following advantages at least:
1. method is general, can effectively dock with the main flow that other valuable metals extract effectively, and technology is simple.
2. iron recovery is higher than the method for existing siderotil deironing.
3. the red iron oxide quality product height that obtains can directly apply to multiple field.
4. solved for zinc hydrometallurgy, nickel and other non-ferrous metal long-standing scum and stored up problem, for no slag production creates conditions.
5. the purity height of iron oxide red product, other compositions are low, can effectively be applied to the purification of leaching liquor deironing of ore, improve the rate of recovery of valuable metal.
Below by concrete example, method of the present invention is described.These examples can not be interpreted as limitation of the scope of the invention.
Example 1
Get liquid 1L after the nickel laterite acidleach, its iron level 42g/L (wherein 98% is ferric iron).Adjust its pH to 2.1 with NaOH, add in the autoclave, 200 ℃ of controlled temperature, oxygen partial pressure 0.2MPa, the reaction after-filtration, with 3 times of water gaging pulping and washing, 100 ℃ of oven dry.
By analysis, iron deposition rate 96.6%, red iron oxide content＞97%, Ni deposition rate＜1.9%.
Example 2
Get liquid 1L after the nickel laterite acidleach, its iron level 42g/L (wherein 98% is ferric iron).Adjust its pH to 2.3 with NaOH, add in the autoclave, 210 ℃ of controlled temperature, 4 times of circulations of crystal seed, oxygen partial pressure 0.2MPa, the reaction after-filtration, with 3 times of water gaging pulping and washing, 100 ℃ of oven dry.
By analysis, iron deposition rate 98.0%, red iron oxide＞97%, Ni deposition rate＜1.2%.
Example 3
Get the preceding liquid 1L of zinc ore siderotil precipitation, its iron level 20g/L (wherein 98% is ferric iron).Adjust its pH to 2.0 with NaOH, add in the autoclave, 190 ℃ of controlled temperature, 4 times of circulations of crystal seed, oxygen partial pressure 0.2MPa, the reaction after-filtration, with 3 times of water gaging pulping and washing, 100 ℃ of oven dry.
By analysis, iron deposition rate 95.4%, red iron oxide＞95%, Zn deposition rate＜1.4%.
Example 4
Get the acidleach of zinc ore high pressure after liquid 1L behind the sulphur dioxide reduction, its iron level 40g/L (wherein 95% is ferrous iron) adds in the autoclave, 210 ℃ of controlled temperature, 4 times of circulations of crystal seed, oxygen partial pressure 0.5MPa, the reaction after-filtration, with 3 times of water gaging pulping and washing, 100 ℃ of oven dry.
By analysis, iron deposition rate 90%, red iron oxide＞95%, Zn deposition rate＜0.4%.
In the description of this specification sheets, concrete feature, structure, material or characteristics that the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means in conjunction with this embodiment or example description are contained at least one embodiment of the present invention or the example.In this manual, the schematic statement to above-mentioned term not necessarily refers to identical embodiment or example.And concrete feature, structure, material or the characteristics of description can be with the suitable manner combination in any one or more embodiment or example.
Although illustrated and described embodiments of the invention, those having ordinary skill in the art will appreciate that: can carry out multiple variation, modification, replacement and modification to these embodiment under the situation that does not break away from principle of the present invention and aim, scope of the present invention is limited by claim and equivalent thereof.
Claims (10)
1. method from the formulations prepared from solutions iron oxide red that contains iron ion, wherein, described iron ion is be selected from ferrous ion and ferric ion at least a, said method comprising the steps of:
(1) the described solution that contains iron ion is joined in the reactor;
(2) regulate the pH value of described solution to 0.5-3.0;
(3) regulate the interior temperature of described reactor to 180-220 degree centigrade, and under oxidizing atmosphere, continue preset time, obtain to contain the solidliquid mixture of ferric oxide;
(4) described solidliquid mixture is carried out solid-liquid separation, obtain the iron oxide red product.
2. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 1 is characterized in that, uses the pH value of the described solution of at least a adjusting that is selected from potassium hydroxide, sodium hydroxide and ammoniacal liquor.
3. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 1 is characterized in that, described oxidizing atmosphere is to realize by feed the gas that contains oxygen in described reactor.
4. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 1 is characterized in that described preset time is 0.5-2.5 hour.
5. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 1 is characterized in that, the part of described iron oxide red product is back in the reactor as crystal seed.
6. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 1 is characterized in that, described described solidliquid mixture is carried out solid-liquid separation, obtains the iron oxide red product and comprises:
Described solidliquid mixture is filtered, obtain containing the filter cake of ferric oxide;
Described filter cake is washed, and drying obtains described iron oxide red product.
7. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 6 is characterized in that the liquid and the solid weight ratio of carrying out described washing are 3-5: 1.
8. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 6 is characterized in that, carries out described drying under 80-120 degree centigrade temperature.
9. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 1 is characterized in that the pH value of regulating described solution is to 2.1-2.3.
10. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 3 is characterized in that described container is an autoclave, and the pressure in the described autoclave is 1.0-1.5MPa, and the dividing potential drop of described oxygen is 0.1-0.5MPa.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603011A (en) * | 2012-02-29 | 2012-07-25 | 中国恩菲工程技术有限公司 | Method for preparing iron oxide red by utilizing valuable metal ferrous post-leaching solution of wet metallurgy |
| CN105694539A (en) * | 2016-02-29 | 2016-06-22 | 中国科学院兰州化学物理研究所 | Method for preparing iron oxide red hybridization pigment by means of clay minerals |
| CN106119539A (en) * | 2016-07-26 | 2016-11-16 | 中国恩菲工程技术有限公司 | The process technique of nickel-bearing laterite |
| CN113136488A (en) * | 2021-04-22 | 2021-07-20 | 中化化工科学技术研究总院有限公司 | Wet treatment process for iron vitriol slag in zinc hydrometallurgy |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903735A (en) * | 2006-08-10 | 2007-01-31 | 攀枝花锐龙冶化材料开发有限公司 | Method of producing iron oxide red using ferrous sulphate |
| CN101077793A (en) * | 2007-05-25 | 2007-11-28 | 宫连春 | Method for preparing iron oxide red from red mud |
-
2011
- 2011-05-05 CN CN2011101159825A patent/CN102153148B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1903735A (en) * | 2006-08-10 | 2007-01-31 | 攀枝花锐龙冶化材料开发有限公司 | Method of producing iron oxide red using ferrous sulphate |
| CN101077793A (en) * | 2007-05-25 | 2007-11-28 | 宫连春 | Method for preparing iron oxide red from red mud |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102603011A (en) * | 2012-02-29 | 2012-07-25 | 中国恩菲工程技术有限公司 | Method for preparing iron oxide red by utilizing valuable metal ferrous post-leaching solution of wet metallurgy |
| CN105694539A (en) * | 2016-02-29 | 2016-06-22 | 中国科学院兰州化学物理研究所 | Method for preparing iron oxide red hybridization pigment by means of clay minerals |
| CN105694539B (en) * | 2016-02-29 | 2018-05-08 | 中国科学院兰州化学物理研究所 | A kind of method that iron oxide red hybrid pigment is prepared using clay mineral |
| CN106119539A (en) * | 2016-07-26 | 2016-11-16 | 中国恩菲工程技术有限公司 | The process technique of nickel-bearing laterite |
| CN113136488A (en) * | 2021-04-22 | 2021-07-20 | 中化化工科学技术研究总院有限公司 | Wet treatment process for iron vitriol slag in zinc hydrometallurgy |
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