CN102153148B - Method for preparing iron oxide red - Google Patents
Method for preparing iron oxide red Download PDFInfo
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- CN102153148B CN102153148B CN2011101159825A CN201110115982A CN102153148B CN 102153148 B CN102153148 B CN 102153148B CN 2011101159825 A CN2011101159825 A CN 2011101159825A CN 201110115982 A CN201110115982 A CN 201110115982A CN 102153148 B CN102153148 B CN 102153148B
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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, introduces sodium/potassium/ammonium ion, is 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.Scum after the deironing is sent into tailing dam and is stored up behind filtration washing.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 that from the solution that contains iron ion, prepares iron oxide red.
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, Said iron ion is be selected from ferrous ion and ferric ion at least a, said method comprising the steps of: (1) joins the said solution that contains iron ion in the reactor drum; The pH value of (2) regulating said solution is to 0.5-3.0; (3) regulate temperature in the said reactor drum to 180-220 degree centigrade, and under oxidizing atmosphere lasting preset time, obtain to contain the solidliquid mixture of red stone; (4) said 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 said solution of at least a adjusting that is selected from Pottasium Hydroxide, sodium hydroxide and ammoniacal liquor.
According to one embodiment of present invention, said oxidizing atmosphere is to realize through in said reactor drum, feeding the gas that contains oxygen.
According to one embodiment of present invention, said preset time is 0.5-2.5 hour.
According to one embodiment of present invention, the part with said iron oxide red product is back in the reactor drum as crystal seed.
According to one embodiment of present invention, said solidliquid mixture is carried out solid-liquid separation, obtain the iron oxide red product and comprise: said solidliquid mixture is filtered, obtain containing the filter cake of red stone; Said filter cake is washed, and drying obtains said 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.
The liquid and the solid weight ratio of according to one embodiment of present invention, carrying out said washing are 3-5: 1.
According to one embodiment of present invention, under 80-120 degree centigrade temperature, carry out said drying.
The pH value of according to one embodiment of present invention, regulating said solution is to 2.1-2.3.
According to one embodiment of present invention, said container is an autoclave, and the pressure in the said autoclave is 1.0-1.5MPa, and the dividing potential drop of said 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 through practice of the present invention.
Description of drawings
Above-mentioned and/or additional aspect of the present invention and advantage obviously with are easily understood becoming the description of embodiment from combining figs, 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 said 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.Be exemplary through the embodiment that is described with reference to the drawings below, only be used to explain the present invention, and can not be interpreted as limitation of the present invention.
Only if 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 ", " red stone ", " red iron oxide ", " red oxide of iron " 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 appeared does not receive special restriction, and 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 drum.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 does not receive special restriction.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 of leach liquor is complicated; Through 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 the container of the present invention's enforcement does not receive special restriction.According to embodiments of the invention, can adopt the reaction kettle that can bear HTHP.Thus, can in this reaction kettle, realize high-throughput, reaction fast and efficiently, improve the efficient of preparation iron oxide red.
S200: the pH value of regulating said solution is to 0.5-3.0, preferred 2.1-2.3.According to embodiments of the invention, the means of regulating pH do not receive special restriction.According to embodiments of the invention, use the pH value of the said solution of at least a adjusting that is selected from Pottasium 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 regulators.Leach liquor when especially being fit to wet production zinc, nickel.
S300: regulate temperature in the said reactor drum to 180-220 degree centigrade, and under oxidizing atmosphere lasting preset time, obtain to contain the solidliquid mixture of red stone; According to embodiments of the invention, oxidizing atmosphere is to realize through in said reactor drum, feeding the gas that contains oxygen.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, promptly described preset time; Do not receive special restriction, as long as red stone can successfully be generated, according to embodiments of the invention; Said preset time is 0.5-2.5 hour; Thus, can carry out oxidizing reaction fully, obtain red stone.
S400: said 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 does not receive special restriction, can be for well known to a person skilled in the art equipment and method.For example,, can adopt said solidliquid mixture is filtered, obtain containing the filter cake of red stone according to embodiments of the invention; Said filter cake is washed, and drying obtains said iron oxide red product.Through filtration washing, can be further purified the purity of resulting red iron oxide.The red iron oxide that obtains at last can be used for various fields such as metallurgy, coating, building materials directly as the industrial raw material of multiple industry.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 do not receive special restriction, can be water.Carrying out the exsiccant mode and do not receive special restriction, can be under 80-120 degree centigrade temperature, to carry out drying, and preferred oven dry can cost realizes the drying of iron oxide red product effectively.In addition,, can resulting iron oxide red product 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 do not receive special restriction, 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 that obtains is high, 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 iron oxide red product gas purity is high, and other compositions are low, can effective application in the purification of leaching liquor deironing of ore, improve the recovery of valuable metal.
Through concrete example, method of the present invention is described below.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).With its pH to 2.1 of NaOH adjustment, 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.
Through analyzing 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).With its pH to 2.3 of NaOH adjustment, 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.
Through analyzing 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 deposition, its iron level 20g/L (wherein 98% is ferric iron).With its pH to 2.0 of NaOH adjustment, 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.
Through analyzing 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.
Through analyzing iron deposition rate 90%, red iron oxide＞95%, Zn deposition rate＜0.4%.
In the description of this specification sheets, the description of reference term " embodiment ", " some embodiment ", " example ", " concrete example " or " some examples " etc. means the concrete characteristic, structure, material or the characteristics that combine this embodiment or example to describe and is 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 characteristic, structure, material or the characteristics of description can combine with suitable manner 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: under the situation that does not break away from principle of the present invention and aim, can carry out multiple variation, modification, replacement and modification to these embodiment, scope of the present invention is limited claim and equivalent thereof.
Claims (7)
1. method from the formulations prepared from solutions iron oxide red that contains iron ion, wherein, said iron ion is be selected from ferrous ion and ferric ion at least a, said method comprising the steps of:
(1) the said solution that contains iron ion is joined in the reactor drum;
The pH value of (2) regulating said solution is to 0.5-3.0;
(3) regulate temperature in the said reactor drum to 180-220 degree centigrade, and under oxidizing atmosphere lasting preset time, obtain to contain the solidliquid mixture of red stone;
(4) said solidliquid mixture is carried out solid-liquid separation, obtains the iron oxide red product,
Wherein,
The said solution that contains iron ion is that nickel ores, zinc ore or cobalt ore are leaching resulting leach liquor in the treating processes through wet method;
Use is selected from the pH value of the said solution of at least a adjusting of Pottasium Hydroxide, sodium hydroxide and ammoniacal liquor;
Said reactor drum is an autoclave, and the pressure in the said autoclave is 1.0-1.5MPa, and the dividing potential drop of oxygen is 0.1-0.5MPa;
Said oxidizing atmosphere is to realize through in said reactor drum, feeding the gas that contains oxygen.
2. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 1 is characterized in that said preset time is 0.5-2.5 hour.
3. 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 said iron oxide red product is back in the reactor drum as crystal seed.
4. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 1 is characterized in that, said solidliquid mixture is carried out solid-liquid separation, obtains the iron oxide red product and comprises:
Said solidliquid mixture is filtered, obtain containing the filter cake of red stone;
Said filter cake is washed, and drying obtains said iron oxide red product.
5. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 4 is characterized in that the liquid and the solid weight ratio of carrying out said washing are 3-5: 1.
6. the method from the formulations prepared from solutions iron oxide red that contains iron ion according to claim 4 is characterized in that, under 80-120 degree centigrade temperature, carries out said drying.
7. 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 said solution is to 2.1-2.3.
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| 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 |
| 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 |
| CN113136488B (en) * | 2021-04-22 | 2022-10-18 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
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