CN101085732A - Method for producing ferrous oxalate from hematite - Google Patents
Method for producing ferrous oxalate from hematite Download PDFInfo
- Publication number
- CN101085732A CN101085732A CN 200710118677 CN200710118677A CN101085732A CN 101085732 A CN101085732 A CN 101085732A CN 200710118677 CN200710118677 CN 200710118677 CN 200710118677 A CN200710118677 A CN 200710118677A CN 101085732 A CN101085732 A CN 101085732A
- Authority
- CN
- China
- Prior art keywords
- ferrox
- ferrous oxalate
- oxalate
- hematite
- crystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- LIKBJVNGSGBSGK-UHFFFAOYSA-N iron(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Fe+3].[Fe+3] LIKBJVNGSGBSGK-UHFFFAOYSA-N 0.000 title claims abstract description 18
- 229940062993 ferrous oxalate Drugs 0.000 title claims abstract description 15
- OWZIYWAUNZMLRT-UHFFFAOYSA-L iron(2+);oxalate Chemical compound [Fe+2].[O-]C(=O)C([O-])=O OWZIYWAUNZMLRT-UHFFFAOYSA-L 0.000 title claims abstract description 15
- 229910052595 hematite Inorganic materials 0.000 title claims description 15
- 239000011019 hematite Substances 0.000 title claims description 15
- 238000004519 manufacturing process Methods 0.000 title abstract description 7
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 14
- 235000006408 oxalic acid Nutrition 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000001291 vacuum drying Methods 0.000 claims abstract description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 52
- LDHBWEYLDHLIBQ-UHFFFAOYSA-M iron(3+);oxygen(2-);hydroxide;hydrate Chemical compound O.[OH-].[O-2].[Fe+3] LDHBWEYLDHLIBQ-UHFFFAOYSA-M 0.000 claims description 32
- 229910052742 iron Inorganic materials 0.000 claims description 21
- 238000007540 photo-reduction reaction Methods 0.000 claims description 8
- 230000035484 reaction time Effects 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 238000013019 agitation Methods 0.000 claims description 5
- 238000010531 catalytic reduction reaction Methods 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 5
- 230000001699 photocatalysis Effects 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 238000002425 crystallisation Methods 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 3
- 238000001640 fractional crystallisation Methods 0.000 claims description 3
- 238000013467 fragmentation Methods 0.000 claims description 2
- 238000006062 fragmentation reaction Methods 0.000 claims description 2
- VBIXEXWLHSRNKB-UHFFFAOYSA-N ammonium oxalate Chemical compound [NH4+].[NH4+].[O-]C(=O)C([O-])=O VBIXEXWLHSRNKB-UHFFFAOYSA-N 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 5
- 238000009776 industrial production Methods 0.000 abstract description 4
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 4
- 239000011707 mineral Substances 0.000 abstract description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 238000003756 stirring Methods 0.000 abstract description 2
- 239000000843 powder Substances 0.000 abstract 2
- 238000001914 filtration Methods 0.000 abstract 1
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 abstract 1
- 238000011946 reduction process Methods 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical group O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 description 6
- 229910000359 iron(II) sulfate Inorganic materials 0.000 description 5
- 239000002253 acid Substances 0.000 description 4
- 239000011790 ferrous sulphate Substances 0.000 description 4
- 235000003891 ferrous sulphate Nutrition 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000008025 crystallization Effects 0.000 description 2
- 239000003317 industrial substance Substances 0.000 description 2
- 238000005304 joining Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000007885 magnetic separation Methods 0.000 description 2
- 235000010755 mineral Nutrition 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000010298 pulverizing process Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- 206010013786 Dry skin Diseases 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 210000003298 dental enamel Anatomy 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- XEEVLJKYYUVTRC-UHFFFAOYSA-N oxomalonic acid Chemical compound OC(=O)C(=O)C(O)=O XEEVLJKYYUVTRC-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Abstract
The invention relates to a method for producing ferrous oxalate taking bloodstone as raw material with acid- disslovation- irradiation reduction process. It is characterized in that it comprises following steps: disintegrating bloodstone, grinding, refining and getting mineral powder with TFe content larger than 65%; adding mineral powder into ferrous oxalate solution, stirring and extracting at 80- 85 Deg. C for 1- 6 hours; filtering at high temperature, stewing filterate under irradiation for 3d- 7d for reduction, getting light yellow ferrous oxalate crystal, separating crystal and getting vacuum drying it at 60 Deg. C and 13.3 Kpa for 1- 3 hours, getting ferrous oxalate. The invention employs bloodstone to replace ferric persulfate, employs oxalic acid to repalce ammonium oxalate. The invention is characterized by easy to get raw material, simple process, no environmental pollution and suitability for large- sacle industrial production.
Description
Technical field
A kind of method of producing ferrous oxalate from hematite relates to a kind of method of producing Ferrox, is that raw material adopts sour molten-photoreduction two-step approach to produce the method for Ferrox with rhombohedral iron ore particularly.
Background technology
Ferrox is a kind of organic chemical industry's product, and except making chemical reagent, it is painted also to be used for coating, dyestuff, ceramic enamel, opticglass and glassware, and nano-sized iron oxide etc. is produced in the preparation of sensitive materials.
At present, the reaction of industrial employing ammonium oxalate and ferrous sulfate forms the production method of Ferrox.Earlier ammonium oxalate and ferrous sulfate crystal are dissolved in water respectively, then ammonium oxalate solution is added in the copperas solution, continuously stirring in the stainless steel reaction pot, generate lurid Ferrox precipitation, the Ferrox slurry is through centrifugation, hot wash, 85 ℃～95 ℃ dryings are the Ferrox finished product.
The problem that aforesaid method exists is: ammonium oxalate and ferrous sulfate all are industrial chemicals, and production cost is better, and it is limited to originate, and is not suitable for large-scale industrial production.
Summary of the invention
The objective of the invention is at the production method mesoxalic acid ammonium of the Ferrox that exists in the prior art and ferrous sulfate all be industrial chemicals, production cost better, be not suitable for the problem of large-scale industrial production, provide that a kind of raw material is cheap and easy to get, technology simple, the method from producing ferrous oxalate from hematite of non-environmental-pollution.
For achieving the above object, the present invention institute by the following technical solutions.
A kind of method of producing ferrous oxalate from hematite is characterized in that rhombohedral iron ore through fragmentation, ore grinding, selected one-tenth T
Fe＞65%, granularity is the breeze of 75 μ m～180 μ m; It is that the weight percentage of solids is 2%～10% in the reaction system in 6%～20% the oxalic acid solution that breeze is joined weight percentage; Agitation leach under 80 ℃～85 ℃ conditions, the reaction times is 1h～6h; Filtered while hot, filtrate is left standstill 3d～7d under illumination condition, and the photo catalytic reduction ironic oxalate is a Ferrox, separates out flaxen Ferrox crystal, and fractional crystallization vacuum-drying gets Ferrox.
The method of a kind of producing ferrous oxalate from hematite of the present invention is characterized in that its illumination process is meant that the ironic oxalate photoreduction that carries out becomes the reaction process of Ferrox under the natural light condition.
The method of a kind of producing ferrous oxalate from hematite of the present invention is characterized in that it separates out flaxen Ferrox crystal is to be that 60 ℃, vacuum tightness are to carry out under the condition of 13.3KPa in temperature.
Method of the present invention, adopt sour molten-photoreduction two-step approach to produce the method for Ferrox, replace ferrous sulfate, replace ammonium oxalate production Ferrox with oxalic acid with rhombohedral iron ore, raw material is cheap and easy to get, technology is simple, non-environmental-pollution, is suitable for large-scale industrial production.
Embodiment
A kind of method of producing ferrous oxalate from hematite, it is characterized in that its process be with rhombohedral iron ore through Mechanical Crushing, and ore grinding is processed into granularity and is 75 μ m～180 μ m, and is selected to T
Fe＞65% breeze; It is that the weight percentage of solids is 2%～10% in the reaction system in 6%～20% the oxalic acid solution that breeze is joined weight percentage, agitation leach under 80 ℃～85 ℃ conditions, and the reaction times is 1h～6h; Filtered while hot, filtrate is left standstill 3d～7d under illumination condition, the photo catalytic reduction ironic oxalate is a Ferrox, separates out into flaxen Ferrox crystal, fractional crystallization and be that 60 ℃, vacuum tightness are vacuum-drying 1h～3h under the condition of 13.3KPa in temperature, Ferrox.
Embodiment 1
(1) sample ore is prepared
Rhombohedral iron ore through pulverizing, ore grinding is processed as granularity-150 μ m, selected with magnetic separation is 65% breeze, measures full iron and ferrous content sees Table 1:
The iron level of table 1 ground hematite
| Mineral name | Total iron T Fe％ | FeO％ | Fe 2O 3％ |
| Rhombohedral iron ore | 64.35 | 8.54 | 83.11 |
(2) acid is molten
With joining the 100mL weight percentage in the 2g ground hematite is in 15% the oxalic acid solution, agitation leach under 80 ℃ of conditions, and the reaction times is 4h, and the oxide compound of the iron of various valence states in the rhombohedral iron ore can be free in the solution, solubility rate is more than 85%.The chemical equation of the molten process of acid is: Fe
2O
3+ 6H
2C
2O
4→ 2H
3Fe (C
2O
4)
3+ 3H
2O
(3) photoreduction
Filtered while hot leaves standstill ore leachate under the natural lighting condition, carry out following photo catalytic reduction reaction:
H
3Fe(C
2O
4)+2H
2O+hv→FeC
2O
4·2H
2O+CO
2+1.5H
2C
2O
4
Reaction times is 5d, the H in the solution more than 92%
3Fe (C
2O
4)
3Can be reduced to FeC
2O
42H
2O.
(4) crystallization
Ferrox photoreduction liquid can be separated out flaxen Ferrox crystal from solution under normal temperature and pressure conditions.Add an amount of oxalic acid in the solution after separating out the Ferrox crystal, can circulate is used to leach rhombohedral iron ore.
(5) vacuum-drying
Separate out the Ferrox crystal through after the liquid-solid separation, contain residue mother liquor, be that 60 ℃, vacuum tightness are dry 2h under the condition of 13.3KPa in temperature, promptly get purity and reach Ferrox more than 96%.
Embodiment 2
(1) sample ore is prepared
Rhombohedral iron ore through pulverizing, ore grinding is processed as-75 μ m, selected with magnetic separation is 65% breeze, measures full iron and ferrous content sees Table 1:
The iron level of table 1 ground hematite
| Mineral name | Total iron T Fe％ | FeO％ | Fe 2O 3％ |
| Rhombohedral iron ore | 65.33 | 8.81 | 83.56 |
(2) acid is molten
With joining the 100mL weight percentage in the 2g ground hematite is in 20% the oxalic acid solution, agitation leach under 85 ℃ of conditions, and the reaction times is 5h, and the oxide compound of the iron of various valence states in the rhombohedral iron ore can be free in the solution, solubility rate is more than 90%.The chemical equation of the molten process of acid is: Fe
2O
3+ 6H
2C
2O
4→ 2H
3Fe (C
2O
4)
3+ 3H
2O
(3) photoreduction
Filtered while hot leaves standstill ore leachate under the natural lighting condition, carry out following photo catalytic reduction reaction:
H
3Fe(C
2O
4)
3+2H
2O+hv→FeC
2O
4·2H
2O+CO
2+1.5H
2C
2O
4
Reaction times is 7d, the H in the solution more than 95%
3Fe (C
2O
4)
3Can be reduced to FeC
2O
42H
2O.
(4) crystallization
Ferrox photoreduction liquid can be separated out flaxen Ferrox crystal from solution under normal temperature and pressure conditions.Add an amount of oxalic acid in the solution after separating out the Ferrox crystal, can circulate is used to leach rhombohedral iron ore.
(5) vacuum-drying
Separate out the Ferrox crystal through after the liquid-solid separation, contain residue mother liquor, be that 60 ℃, vacuum tightness are dry 3h under the condition of 13.3KPa in temperature, promptly get purity and reach Ferrox more than 98%.
Claims (3)
1. the method for a producing ferrous oxalate from hematite is characterized in that rhombohedral iron ore through fragmentation, ore grinding, selected one-tenth T
Fe＞65%, granularity is the breeze of 75 μ m～180 μ m; It is that the weight percentage of solids is 2%～10% in the reaction system in 6%～20% the oxalic acid solution that breeze is joined weight percentage; Agitation leach under 80 ℃～85 ℃ conditions, the reaction times is 1h～6h; Filtered while hot, filtrate is left standstill 3d～7d under illumination condition, and the photo catalytic reduction ironic oxalate is a Ferrox, separates out flaxen Ferrox crystal, and fractional crystallization vacuum-drying gets Ferrox.
2. the method for a kind of producing ferrous oxalate from hematite of the present invention is characterized in that its illumination process is meant the photoreduction reaction of carrying out under the natural light condition.
3. the method for a kind of producing ferrous oxalate from hematite according to claim 1 is characterized in that it separates out flaxen Ferrox crystal is to be that 60 ℃, vacuum tightness are to carry out under the condition of 13.3KPa in temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710118677 CN101085732A (en) | 2007-07-12 | 2007-07-12 | Method for producing ferrous oxalate from hematite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200710118677 CN101085732A (en) | 2007-07-12 | 2007-07-12 | Method for producing ferrous oxalate from hematite |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101085732A true CN101085732A (en) | 2007-12-12 |
Family
ID=38936930
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200710118677 Pending CN101085732A (en) | 2007-07-12 | 2007-07-12 | Method for producing ferrous oxalate from hematite |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101085732A (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103937980A (en) * | 2014-04-18 | 2014-07-23 | 东北大学 | Method for stripping iron-loaded P2O4 organic phase and removing iron from strip liquor |
| CN104032143A (en) * | 2014-05-15 | 2014-09-10 | 浙江省冶金研究院有限公司 | Recycling and purifying method of waste palladium-carbon catalyst |
| CN104617290A (en) * | 2013-11-04 | 2015-05-13 | 中国科学院大连化学物理研究所 | Homogenous precipitation method for preparing Fe2O3 nanobelt and Fe2O3 nanobelt-carbon composite material |
| CN107117993A (en) * | 2017-04-18 | 2017-09-01 | 中山大学 | The method that a kind of utilization oxalic acid and siderophore DFOB dissolve bloodstone |
| CN111394577A (en) * | 2020-04-30 | 2020-07-10 | 西安建筑科技大学 | Method for leaching coated hematite in secondary calcine by using oxalic acid |
| CN114105759A (en) * | 2021-08-05 | 2022-03-01 | 中南大学 | Method for synthesizing long-strip-shaped ferrous oxalate from hematite slag in one pot |
| CN114560767A (en) * | 2022-03-14 | 2022-05-31 | 四川大学 | Method for preparing ferrous oxalate by siderite |
-
2007
- 2007-07-12 CN CN 200710118677 patent/CN101085732A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104617290A (en) * | 2013-11-04 | 2015-05-13 | 中国科学院大连化学物理研究所 | Homogenous precipitation method for preparing Fe2O3 nanobelt and Fe2O3 nanobelt-carbon composite material |
| CN103937980A (en) * | 2014-04-18 | 2014-07-23 | 东北大学 | Method for stripping iron-loaded P2O4 organic phase and removing iron from strip liquor |
| CN103937980B (en) * | 2014-04-18 | 2015-11-04 | 东北大学 | A kind of P204 organic phase of back extraction load iron and the method for strip liquor deironing |
| CN104032143A (en) * | 2014-05-15 | 2014-09-10 | 浙江省冶金研究院有限公司 | Recycling and purifying method of waste palladium-carbon catalyst |
| CN107117993A (en) * | 2017-04-18 | 2017-09-01 | 中山大学 | The method that a kind of utilization oxalic acid and siderophore DFOB dissolve bloodstone |
| CN107117993B (en) * | 2017-04-18 | 2021-04-27 | 中山大学 | Method for dissolving hematite by using oxalic acid and siderophore DFOB |
| CN111394577A (en) * | 2020-04-30 | 2020-07-10 | 西安建筑科技大学 | Method for leaching coated hematite in secondary calcine by using oxalic acid |
| CN114105759A (en) * | 2021-08-05 | 2022-03-01 | 中南大学 | Method for synthesizing long-strip-shaped ferrous oxalate from hematite slag in one pot |
| CN114560767A (en) * | 2022-03-14 | 2022-05-31 | 四川大学 | Method for preparing ferrous oxalate by siderite |
| CN114560767B (en) * | 2022-03-14 | 2023-01-17 | 四川大学 | Method for preparing ferrous oxalate by siderite |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102329964B (en) | Method for separating and recovering vanadium and chromium from vanadium-chromium reduced waste residue | |
| WO2015161660A1 (en) | Method for preparing low-silicon vanadium pentoxide from solution containing vanadium, chromium and silicon | |
| CN101085732A (en) | Method for producing ferrous oxalate from hematite | |
| CN102583264B (en) | Method for leaching selenium in acid mud by using sodium sulfite | |
| CN101760613B (en) | Method for leaching zinc-containing ores | |
| CN102312090A (en) | Process for extracting scandium from ore containing scandium through pressure leaching | |
| CN102382979B (en) | Technique for extracting rare earth from rare earth tailing and preparing calcium sulfate whiskers | |
| CN103740931B (en) | Containing the method for ferronickel mixing solutions goethite precipitation iron | |
| CN102616824A (en) | Method for preparing ultrafine high-whiteness active barite powder | |
| CN106119560A (en) | Zinc-cobalt separation method | |
| CN102321809A (en) | Method for extracting cobalt and copper from cobalt-copper-iron alloy | |
| CN104073634B (en) | A kind of method of nickel minerals leachate or electrolytic anode liquid deironing | |
| CN102897804B (en) | Method for preparing lithium carbonate directly from lithium chloride and carbon dioxide | |
| CN103397209A (en) | Method for extracting vanadium from high-calcium and high-phosphorus vanadium slag | |
| CN103131862B (en) | Pretreatment decomposition method extracts high purity rare earth oxides from fluorescent powder scrap | |
| CN102167400A (en) | Method for preparing vanadium pentoxide from vanadium-containing solution | |
| CN101760614B (en) | Leaching method of nickel-containing ore | |
| CN102774870A (en) | Method for removing impurity of iron in copper sulphate | |
| CN103395751A (en) | Wet method used for extracting products from low-grade complex material containing tellurium and selenium | |
| CN105671324A (en) | Method for preparing ammonium rhenate from rhenium-enriched slags | |
| CN100480404C (en) | Method for leaching vanadium from stone-like coal by oxidation transformation | |
| CN102277481A (en) | Method for reducing lead and protecting rhenium for high-lead rhenium and molybdenum containing concentrate | |
| CN109852820B (en) | Method for producing vanadium pentoxide | |
| CN104229893A (en) | Complete-wet-method production technology for producing ammonium molybdate from nickel-molybdenum ore | |
| CN101210287A (en) | Acidolysis oxidation conversion method for extracting vanadium from stone coal |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20071212 |