CN101913657A - Preparation method of flake ferric oxide - Google Patents
Preparation method of flake ferric oxide Download PDFInfo
- Publication number
- CN101913657A CN101913657A CN 201010256444 CN201010256444A CN101913657A CN 101913657 A CN101913657 A CN 101913657A CN 201010256444 CN201010256444 CN 201010256444 CN 201010256444 A CN201010256444 A CN 201010256444A CN 101913657 A CN101913657 A CN 101913657A
- Authority
- CN
- China
- Prior art keywords
- ferric oxide
- preparation
- flake
- flake ferric
- product
- 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
Images
Abstract
The invention discloses a preparation method of flake ferric oxide, which comprises the following steps: dissolving ferric trichloride hexahydrate, a composite fused salt and an additive in dilute sulphuric acid to prepare solution of a precursor; drying at 100 to 150 DEG C for 24 to 36 hours till no water exists, grinding to obtain precursor powder, and sintering at 900 to 1,200 DEG C for 2 to 6 hours; and obtaining a flake ferric oxide product by stirring in water bath, washing, filtering and drying. In the invention, the precursor is prepared by wet-method crystallization rather than the conventional dry-method mixing, so the agglomeration problem of the product is solved effectively; an aluminum oxide or zinc oxide additive is introduced for crystal form guiding; and the product is hexagonal flakes with flat and smooth surfaces, the particle dispersing performance of the product is high, the average particle size is 20 to 60 mu m, the thickness is uniformly distributed around 0.4 mu m, and the diameter-to-thickness ratio is 50 to 150. The prepared flake ferric oxide product can be wieldy used in anticorrosion coatings, high-quality pearl pigments and cosmetics as an inorganic rust-resisting material.
Description
Technical field
The present invention relates to a kind of be raw material with the Iron(III) chloride hexahydrate, with the combine method of flake ferric oxide of the high radius-thickness ratio of preparation of wet method crystallization and fused salt calcining, be the inorganic powder material preparation field.
Background technology
Flake ferric oxide has unique scale structure, and main component is α-Fe
2O
3, be hematite-type Fe
2O
3A kind of, in fields such as anticorrosive coating, pearly pigment and makeup extensive use is arranged.Because the similar mica of its sheet structure is so claim iron mica again.Widely used in the world at present is flake hematite, and it is to be raw material with the flake hematite ore deposit, through operations such as fragmentation, ore dressing, pulverizing and make, its product foreign matter content height, do not have regular profile, surface irregularity is difficult to satisfy the requirement of high-grade fine pigments.And the synthetic flake ferric oxide is compared with natural product, has that purity height, advantages of good crystallization, particle diameter are controlled, an advantage such as sheet degree height, radius-thickness ratio are big, has very wide application prospect.Patent US5500043 can make more colorful Micaceous Iron Oxide Pearlescent Pigment by coat the metal oxide as titanium dioxide or zirconium dioxide and so on high refractive index on the flake ferric oxide matrix, and good decorating effect can be used for high-grade finish paint or makeup.And flake ferric oxide has particular requirement to its sheet structure when being used for pearly pigment substrate or makeup, mainly its particle diameter, thickness or radius-thickness ratio is proposed higher requirement, and radius-thickness ratio is big more, and its sheet degree is high more.The median size of ferric oxide should be 10～60 μ m when patent EP0191292A2 had proposed to be used for makeup, and the desirable mean thickness of sheet is 0.2～1 μ m.
At present, the method for synthetic flake ferric oxide mainly contains three kinds of hydrothermal method, high-temperature molten salt method and vapor phase processs.It is raw material with titanium white industry byproduct ferrous sulfate that patent US3987156, GBA1333788, EP0416648, CN1944274A adopt hydrothermal method, earlier make it to become trivalent iron salt, in autoclave, obtain flake ferric oxide then with alkali reaction with the direct or indirect oxidation of oxygenant.This method is withstand voltage to conversion unit, resistance to acids and bases is had relatively high expectations, and is unfavorable for suitability for industrialized production.Patent US3864463 adopts vapor phase process with oxygen-containing gas and FeCl
3Steam is at the fixing bed reaction of 400 ℃～750 ℃ spherical particle, and having obtained particle diameter is the flake ferric oxide of 2～100 μ m.Ferric oxide is easily reunited on reactor wall in this method preparation process, is difficult for peeling off, and reactor needs regular maintenance, and operation efficiency is lower, and product cut size distribution range broad.It is raw material with iron filings or scrap iron skin that patent EP0307486 A2 adopts the high-temperature molten salt method, become iron(ic) chloride or be raw material directly with chlorinated with chlorine with green vitriol, mix with alkali-metal muriate then, the high temperature fused state dioxygen oxidation obtains the iron mica of the higher hexagonal flake structure of purity.Thick 1～5 μ m of prepared ferric oxide, diameter 30～50 μ m, product radius-thickness ratio and the regulation and control of sheet degree are not very good.Patent US4676838 adds additive activated ferric oxide crystal seed in the hydrothermal method process, the product cut size that makes less (0.5～20 μ m), and radius-thickness ratio is 20～100, crystal morphology is better than not adding the product of additive.As seen, add special additive and can play the effect of crystal formation guide, comparatively favourable to improving product sheet degree.But molten-salt growth method prepares the use of flake ferric oxide technological process additive then rarely has report.In addition, the mixed effect of raw material and fused salt also has considerable influence to product performance, and molten-salt growth method all is to adopt traditional dry grinding to mix at present, and this has restricted the further raising of product performance to a certain extent.
Summary of the invention
The objective of the invention is deficiency at above-mentioned prior art existence, propose that a kind of technology is simple, the flake ferric oxide preparation method of processing ease, constant product quality, this method replaces conventional dry to mix with the wet method crystallization, and in the composite fused salt calcination process, introduce additive aluminum oxide or zinc oxide as the agent of crystal formation guide, the flake ferric oxide product pattern of its production is regular, sheet degree height, have good dispersiveness in water.
In order to solve the problems of the technologies described above, technical scheme of the present invention comprises the steps and processing condition:
(1) with Iron(III) chloride hexahydrate and composite fused salt and additive mixed grinding 5～10 minutes under room temperature, the composite fused salt consumption is 1.5～3.5 times of Iron(III) chloride hexahydrate weight, the additive add-on is 2～4% of an Iron(III) chloride hexahydrate weight, under 50 ℃～80 ℃ temperature, the solid mixture that grinds is dissolved in fully then in the dilute sulphuric acid that concentration is 0.1～0.5mol/L precursor solution, the concentration of Iron(III) chloride hexahydrate is 0.01～0.05g/ml in the precursor solution;
(2) the dry presoma that gets of precursor solution; Grind the back calcining, get the flake ferric oxide meal after the cooling;
(3) the ferric oxide meal is joined be made into suspension, agitation and filtration, distilled water wash in the distilled water; Filter cake drying gained powder is flake ferric oxide.
Composite fused salt described in the step (1) is the mixture of sodium sulfate and vitriolate of tartar, and wherein the weight ratio of sodium sulfate and vitriolate of tartar is 2: 1～5: 1, and its effect mainly provides the high-temperature fusion liquid environment.Described additive is Tai-Ace S 150 or zinc sulfate; Its effect mainly is that high-temperature calcination generates aluminum oxide or zinc oxide, thereby is present in the ferric oxide system with the ion doping form, plays the effect of sheet crystal formation guide.。
In the described step (2) precursor solution is dried to anhydrously, drying temperature is 100 ℃～150 ℃, and be 24～36 hours time of drying; Calcining is that temperature rise rate was 5～10 ℃/min 900 ℃～1200 ℃ temperature lower calcination 2～6 hours.
The actual conditions of described step (3) is as follows:
The ferric oxide meal is joined the suspension that is made into 1～10% massfraction in the distilled water, placed 50 ℃～80 ℃ water-bath mechanical stirring 1～2 hour,, filter the back and under room temperature, use distilled water wash 1～5 time so that fused salt fully dissolves; At last with filter cake through 2～10 hours gained powders of 80～100 ℃ of dryings, be flake ferric oxide.
Method of the present invention replaces conventional dry to mix by adopting the wet method crystallization, greatly improved the mixed effect of raw material molysite and composite fused salt and additive, avoided adopting the problem of conventional dry ground and mixed inequality, improved the dispersiveness of molysite in liquid fused salt in the calcination process, growth to the sheet crystal formation is very favourable, thereby has guaranteed pattern that the flake ferric oxide product is regular and good dispersing property.Calcination process has not only reduced the consumption of fused salt to a certain extent owing to added the additive aluminum oxide or zinc oxide is done the agent of crystal formation guide, and the thickness of control strip preferably, and radius-thickness ratio is effectively regulated and control.Therefore, the prepared flake ferric oxide morphology microstructure that comes out is regular, sheet degree height, and radius-thickness ratio is big, and particles dispersed is good, and the streamline time remaining is long in water.
Flake ferric oxide product of the present invention can directly use as pigment, also can be used as matrix and carry out the preparation of pearly pigment, has use properties preferably in paint field such as high-grade finish paint, anti-corrosion function coating, pearly pigments, be particularly useful for makeup, when particularly being applied to water-borne coatings, has dispersing property preferably.
The present invention compared with prior art has the following advantages:
1, raw material and fused salt and additive are dissolved in jointly are made into precursor solution in the dilute sulphuric acid, drying crystalline prepares presoma then, promptly replace traditional dry grinding, make raw material realize mixing of atomic scale, improved mixed effect with fused salt and additive with the wet method crystallization.
2, the use of additive adds additive at the presoma preparatory phase, and ferric oxide is played the effect of crystal formation guide, and product sheet degree improves.
Description of drawings
The normal direction of flake ferric oxide powder (a) and (b) form radially when Fig. 1 makes additive for Tai-Ace S 150.
The pattern of flake ferric oxide powder when Fig. 2 makes additive for zinc sulfate.
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1:
With the 10g Iron(III) chloride hexahydrate, 15g sodium sulfate, 5g vitriolate of tartar and 0.3g Tai-Ace S 150 mixed grinding 10 minutes under the room temperature in mortar, be transferred in the beaker, adding 500ml concentration is the dilute sulphuric acid of 0.2mol/L, place the fully dissolving in 30 minutes of 60 ℃ of stirred in water bath, then solution is put into baking oven 110 ℃ of dryings 24 hours, taking out the back ground 5 minutes, the corundum crucible of packing into, put into retort furnace 1100 ℃ of calcinings 4 hours, take out sample transfer behind the naturally cooling to beaker, add 500ml distilled water and be made into suspension,, filter in 60 ℃ of stirred in water bath 2 hours, distilled water wash 3 times, filter cake is put into air dry oven 90 ℃ of dryings 3 hours, take out to grind and obtain the flake ferric oxide product, its scanning electron microscope diagram is seen Fig. 1.
Embodiment 2:
With the 10g Iron(III) chloride hexahydrate, 15g sodium sulfate, 5g vitriolate of tartar and 0.3g zinc sulfate mixed grinding 10 minutes under the room temperature in mortar, be transferred in the beaker, adding 500ml concentration is the dilute sulphuric acid of 0.2mol/L, place the fully dissolving in 30 minutes of 60 ℃ of stirred in water bath, then solution is put into baking oven 110 ℃ of dryings 24 hours, taking out the back ground 5 minutes, the corundum crucible of packing into, put into retort furnace 1100 ℃ of calcinings 4 hours, take out sample transfer behind the naturally cooling to beaker, add 500ml distilled water and be made into suspension,, filter in 60 ℃ of stirred in water bath 2 hours, distilled water wash 3 times, filter cake is put into air dry oven 90 ℃ of dryings 3 hours, take out to grind and obtain the flake ferric oxide product, its scanning electron microscope diagram is seen Fig. 2.
Detect through scanning electronic microscope, the median size of product flake ferric oxide of the present invention is that 20～60 μ m, thickness are evenly distributed on about 0.4 μ m, radius-thickness ratio is greater than 50.
The flake ferric oxide that obtains is bright red or red-purple, and glossiness is good, and the energy good distribution can be observed tangible streamline after the stirring in water solvent, sustainable 60～70 seconds of streamline time, can be applied to water-borne coatings preferably.
Product detects:
One, particle diameter, thickness and morphology analysis: adopt Nova Nano SEM230 field emission scanning electron microscope (FEI) to observe the iron oxide product pattern, its particle diameter and thickness are measured, magnification is between 500～20,000 times.
Two, dispersing property (streamline time) is measured in the water: weighing 1g iron oxide product joins in the 100ml water, after the dispersed with stirring, observes the streamline phenomenon, and the flow line time length is measured.
Claims (10)
1. a preparation method of flake ferric oxide is characterized in that, comprises the steps:
(1) with Iron(III) chloride hexahydrate and composite fused salt and additive mixed grinding 5～10 minutes under room temperature, the composite fused salt consumption is 1.5～3.5 times of Iron(III) chloride hexahydrate weight, the additive add-on is 2～4% of an Iron(III) chloride hexahydrate weight, under 50 ℃～80 ℃ temperature, the solid mixture that grinds is dissolved in then in the dilute sulphuric acid that concentration is 0.1～0.5mol/L precursor solution, the concentration of Iron(III) chloride hexahydrate is 0.01～0.05g/ml in the precursor solution;
(2) the dry presoma that gets of precursor solution; Grind the back calcining, get the flake ferric oxide meal after the cooling;
(3) the ferric oxide meal is joined be made into suspension, agitation and filtration, distilled water wash in the distilled water; Filter cake drying gained powder is flake ferric oxide.
2. a kind of preparation method of flake ferric oxide according to claim 1 is characterized in that: the composite fused salt described in the step (1) is the mixture of sodium sulfate and vitriolate of tartar, and wherein the weight ratio of sodium sulfate and vitriolate of tartar is 2: 1～5: 1.
3. a kind of preparation method of flake ferric oxide according to claim 1 and 2 is characterized in that: the additive described in the step (1) is Tai-Ace S 150 or zinc sulfate.
4. a kind of preparation method of flake ferric oxide according to claim 1 is characterized in that: in the described step (2) precursor solution is dried to anhydrous.
5. according to claim 1 or 4 described a kind of preparation method of flake ferric oxide, it is characterized in that: drying temperature is 100 ℃～150 ℃, and be 24～36 hours time of drying.
6. a kind of preparation method of flake ferric oxide according to claim 1 is characterized in that: calcining is 900 ℃～1200 ℃ temperature lower calcination 2～6 hours in the described step (2).
7. according to claim 1 or 6 described a kind of preparation method of flake ferric oxide, it is characterized in that: temperature rise rate is 5～10 ℃/min during calcining.
8. a kind of preparation method of flake ferric oxide according to claim 1 is characterized in that: described step joins the suspension that is made into 1～10% massfraction in the distilled water with the ferric oxide meal in (3).
9. according to claim 1 or 8 described a kind of preparation method of flake ferric oxide, it is characterized in that: suspension was placed 50 ℃～80 ℃ water-bath mechanical stirring 1～2 hour, so that fused salt fully dissolves, filter the back filter cake and under room temperature, use distilled water wash 1～5 time.
10. a kind of preparation method of flake ferric oxide according to claim 9 is characterized in that: filter cake through 2～10 hours gained powders of 80～100 ℃ of dryings, is flake ferric oxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010256444 CN101913657A (en) | 2010-08-18 | 2010-08-18 | Preparation method of flake ferric oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010256444 CN101913657A (en) | 2010-08-18 | 2010-08-18 | Preparation method of flake ferric oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101913657A true CN101913657A (en) | 2010-12-15 |
Family
ID=43321341
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010256444 Pending CN101913657A (en) | 2010-08-18 | 2010-08-18 | Preparation method of flake ferric oxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101913657A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106865623A (en) * | 2017-04-06 | 2017-06-20 | 东北大学 | One kind prepares γ Fe using iron oxide phosphorus2O3The method of powder |
| CN109326460A (en) * | 2018-11-09 | 2019-02-12 | 天津工业大学 | A kind of preparation method of di-iron trioxide/carbon cloth composite and flexible electrode |
| CN109903875A (en) * | 2019-02-28 | 2019-06-18 | 西南科技大学 | A kind of method that phosphate polymer solidifies boracic nuclear waste |
| CN112897592A (en) * | 2021-01-25 | 2021-06-04 | 中国科学院广州地球化学研究所 | Micro-nano iron oxide mineral color developing agent and preparation method and application thereof |
| CN112919548A (en) * | 2021-03-09 | 2021-06-08 | 陕西科技大学 | Purple luster iron oxide flaky particles and preparation method thereof |
| WO2023272732A1 (en) * | 2021-07-02 | 2023-01-05 | Dic Corporation | Plate-shaped iron oxide particles and method for producing iron oxide particles |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944274A (en) * | 2006-10-24 | 2007-04-11 | 湘潭大学 | Method for preparing mica iron oxide by hydrothermal reaction and crystallizing |
-
2010
- 2010-08-18 CN CN 201010256444 patent/CN101913657A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1944274A (en) * | 2006-10-24 | 2007-04-11 | 湘潭大学 | Method for preparing mica iron oxide by hydrothermal reaction and crystallizing |
Non-Patent Citations (2)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库 工程科技IotaIota辑》 20100415 袁晰 助熔剂法制备片状氧化铁晶体及其生长机理研究 1-10 , 第4期 2 * |
| 《涂料工业》 20090831 袁晰等 珠光颜料用片状氧化铁的助熔剂法合成研究 第34-37页 1-10 第39卷, 第8期 2 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106865623A (en) * | 2017-04-06 | 2017-06-20 | 东北大学 | One kind prepares γ Fe using iron oxide phosphorus2O3The method of powder |
| CN106865623B (en) * | 2017-04-06 | 2018-04-10 | 东北大学 | One kind prepares γ Fe using scale oxide2O3The method of powder |
| CN109326460A (en) * | 2018-11-09 | 2019-02-12 | 天津工业大学 | A kind of preparation method of di-iron trioxide/carbon cloth composite and flexible electrode |
| CN109903875A (en) * | 2019-02-28 | 2019-06-18 | 西南科技大学 | A kind of method that phosphate polymer solidifies boracic nuclear waste |
| CN112897592A (en) * | 2021-01-25 | 2021-06-04 | 中国科学院广州地球化学研究所 | Micro-nano iron oxide mineral color developing agent and preparation method and application thereof |
| CN112919548A (en) * | 2021-03-09 | 2021-06-08 | 陕西科技大学 | Purple luster iron oxide flaky particles and preparation method thereof |
| CN112919548B (en) * | 2021-03-09 | 2023-08-08 | 晶瓷(北京)新材料科技有限公司 | Purple glossy iron oxide flaky particles and preparation method thereof |
| WO2023272732A1 (en) * | 2021-07-02 | 2023-01-05 | Dic Corporation | Plate-shaped iron oxide particles and method for producing iron oxide particles |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105802282B (en) | The method for preparing red hybrid pigment using red attapulgite stone clay | |
| CN101913657A (en) | Preparation method of flake ferric oxide | |
| CN101600498B (en) | Iron oxide containing precipitated crystalline titanium dioxide and process for the manufacture thereof | |
| EP2178798B1 (en) | Method of preparing a well-dispersable microcrystalline titanium dioxide product | |
| CN102492312B (en) | High-saturation iron-series pigment and production method thereof | |
| WO2013020430A1 (en) | Method for preparing high dispersion rutile product | |
| CN109370264B (en) | Method for preparing high-performance iron oxide red/clay mineral hybrid pigment by mechanochemistry | |
| CN103980739B (en) | A kind of part replaces multiple modified ultra-fine non-metallic powder of titanium dioxide and preparation method thereof | |
| Zhao et al. | Preparation of nanosized anatase TiO2-coated illite composite pigments by Ti (SO4) 2 hydrolysis | |
| EP3121150B1 (en) | Plate-like aluminum oxide and preparation method therefor | |
| CN100357187C (en) | Process for preparing nano chromium carbide powder | |
| CN107629482A (en) | The preparation method of the nanometer orange inorganic pigment of pucherite | |
| CN103570049B (en) | Method for preparing completely dispersed alpha aluminum oxide nano particles | |
| CN106801256A (en) | A kind of method that solid phase method prepares potassium hexatitanate platelet | |
| Hu-min et al. | The effects of pH and alkaline earth ions on the formation of nanosized zirconia phases under hydrothermal conditions | |
| CN111453768A (en) | Rutile metatitanic acid, titanium white and preparation method thereof | |
| JP2006328092A (en) | Iron-based black-colored particle powder and black coating, rubber and resin composition using the same | |
| CN103305032A (en) | Iron oxide yellow viscosity reduction method | |
| CN108102433B (en) | Method for preparing high-thermal stability clay mineral-iron red hybrid pigment by utilizing coprecipitation technology | |
| CN110228823B (en) | Iron oxide yellow and preparation method thereof, and iron oxide red and preparation method thereof | |
| CN107987558B (en) | Flower cluster-shaped LaFexEu1-xO3/TiO2Preparation method of composite superfine red ceramic pigment | |
| JP2007001851A (en) | Method for producing amorphous calcium phosphate-coated particle, and amorphous calcium phosphate-coated particle | |
| CN101792186A (en) | Method for preparing micaceous iron oxide by molten salt growth method | |
| CN108504165A (en) | A kind of preparation method of electrophoretic paint calcined kaolin clay filler | |
| CN108690377A (en) | A kind of pearlescent pigment and preparation method thereof with thousand pure gold effects |
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 |
Application publication date: 20101215 |