CN101947450A - Nanometer titanium dioxide-coated iron oxide yellow composite material and preparation method thereof - Google Patents
Nanometer titanium dioxide-coated iron oxide yellow composite material and preparation method thereof Download PDFInfo
- Publication number
- CN101947450A CN101947450A CN 201010266641 CN201010266641A CN101947450A CN 101947450 A CN101947450 A CN 101947450A CN 201010266641 CN201010266641 CN 201010266641 CN 201010266641 A CN201010266641 A CN 201010266641A CN 101947450 A CN101947450 A CN 101947450A
- Authority
- CN
- China
- Prior art keywords
- iron oxide
- oxide yellow
- colloidal sol
- composite
- nano titanium
- 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.)
- Granted
Links
Images
Abstract
The invention discloses a nanometer titanium dioxide-coated iron oxide yellow composite material and a preparation method thereof. The nanometer titanium dioxide-coated iron oxide yellow composite material is prepared by coating nanometer titanium dioxide on the surface of iron oxide yellow serving as a carrier, wherein the nanometer titanium dioxide belongs to an anatase phase; the composite material is in a long stick shape, the longitudinal length is between 0.5 and 1.5 mu m, and the transversal particle size is between 140 and 160 nm; and the molar ratio of Fe to Ti in the composite material is 0.5 to 1.5:1. The nanometer titanium dioxide-coated iron oxide yellow composite material prepared by the method has the advantages of uniform coating of nanometer powder, high dispersibility, high performance and wide application field. The preparation method has the advantages of high yield, low cost, easily controllable process procedure and suitability for industrialized production.
Description
(1) technical field
The present invention relates to a kind of nano titanium oxide (TiO
2) coating iron oxide yellow (alpha-feooh) composite and preparation method thereof.
(2) background technology
Iron oxide yellow (alpha-feooh) can be widely used in aspects such as novel magnetic recording material, wastewater treatment, environmental contaminants processing because of having good magnetic.Nano titanium oxide is nontoxic because of having, stable, do not produce extremely people's attention of advantage such as secondary pollution, the processing aspect of special environmental pollution.On the one hand, because nano-TiO
2Easily be distributed in the water equal solvent, be difficult to separate, cause and be difficult to realize reclaim and recycling, therefore increased TiO with the water equal solvent
2Application cost; On the other hand, because nano-TiO
2The surface is big, and is active high and easily reunite, and causes its nano effect to be difficult to embody, and reduced nano-TiO
2Practical application effect, also make TiO
2Photocatalysis efficiency is lower.For solving above-mentioned two problems, people have carried out number of research projects.Studies show that, metal ion mixing, surperficial enhanced sensitivity and with other material is compound etc. method can improve TiO
2Photocatalytic activity.In addition, nano combined also is a kind of efficient ways.This method can not only effectively improve the specific area of nano material, also can improve four big effects of nano material, also the characteristic of nano material and the structure of composite can be combined, give full play to strong point separately, thereby go out to embody the best macro property of material.
Though more both at home and abroad at the bibliographical information of nano composite material aspect preparing, adopt nano titanium oxide (TiO
2) bibliographical information that is coated to iron oxide yellow (alpha-feooh) surface do not see.
(3) summary of the invention
First technical problem that the present invention will solve is to provide a kind of nano titanium oxide (TiO
2) coating iron oxide yellow (alpha-feooh) composite, iron oxide yellow can strengthen the photocatalytic activity of titanium dioxide on the one hand after nano titanium oxide coats, it be can be applicable in the catalysis material; Can strengthen the performance of iron oxide yellow on the other hand, expand the range of application of iron oxide yellow pigments, its research has good novelty and practical value.
Nano titanium oxide of the present invention coats iron oxide yellow composite, i.e. TiO
2/ alpha-feooh composite, described composite is for long bar-shaped, and longitudinal length is between 0.5 μ m～1.5 μ m, and laterally particle diameter is at 140～160nm; Described composite is to be carrier with the iron oxide yellow, and nano titanium oxide is coated on carrier surface, and described nano titanium oxide belongs to the anatase phase; Fe is 0.5～1.5: 1 with the amount of substance ratio of Ti in the described composite.
Further, composite of the present invention is carrier with the iron oxide yellow, nano titanium oxide evenly is coated on carrier surface and forms the nanometer titanium dioxide layer of thickness at 2～5nm, and also sporadicly is distributed with the titanium dioxide nanoparticle of particle size range at 5～20nm at the outer wall of composite.Be in the described composite, described nano titanium oxide is coated on the iron oxide yellow surface in two ways, and a kind of is stratiform, and the thickness of layer is at 2～5nm; A kind of is graininess, and particle size range is at 5～20nm.
Further, the amount of substance ratio of Fe and Ti is 1: 1 in the described composite.
The nano titanium oxide that second technical problem that the present invention will solve provides a kind of cost is low, effective, technical process is controlled relatively easily coats the preparation method of iron oxide yellow composite.
For solving the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of described nano titanium oxide coats the preparation method of iron oxide yellow composite, and described method comprises the steps: titanium tetrachloride is mixed with the hydrosol, the hydrosol place aging after thin up again, obtain water white transparency colloidal sol; Get iron oxide yellow and join in the water white transparency colloidal sol, evenly stir 1～3h under the condition of 20～40 ℃ of waters bath with thermostatic control, obtain sediment, the gained sediment promptly gets described nano titanium oxide through washing, drying, grinding and coats the iron oxide yellow composite; In the iron oxide yellow that adds in the titanium tetrachloride of Fe and adding Ti amount of substance ratio be 0.5～1.5: 1.
Further, in the iron oxide yellow of adding in the titanium tetrachloride of Fe and adding Ti amount of substance ratio be 1: 1.
Further, behind the adding iron oxide yellow, it is 30 ℃ that water bath with thermostatic control is set, mixing time 2h.
Further, the present invention obtains yellow suspension after the adding iron oxide yellow fully stirs, can add entry earlier and wash.
Further, the present invention recommends the described hydrosol to prepare as follows: under-10～0 ℃ titanium tetrachloride is added drop-wise in the pure water, fully stir and be mixed with oyster colloidal sol, the volume ratio of described titanium tetrachloride and pure water is 0.1～0.9: 1, be preferably 0.5: 1.Described pure water both can be that distilled water also can be deionized water.
Further, the present invention recommends the described hydrosol to place preferred 10～14 hours aging 6～24 hours.Preferred wearing out at room temperature carried out, and room temperature of the present invention refers generally to 20-35 ℃.
Further, the present invention is after wearing out hydrosol placement, recommend to make as follows water white transparency colloidal sol: pure water is added drop-wise in the colloidal sol of aging back-10～0 ℃ of volume ratio of pressing aging back colloidal sol and pure water 0.3～0.7: 1 down, the abundant stirring is mixed with water white transparency colloidal sol.Further, preferably feed intake according to aging back colloidal sol and 0.5: 1 volume ratio of pure water.
The present invention is concrete to recommend described nano titanium oxide coating iron oxide yellow composite to be prepared according to following steps:
(A) under-10～0 ℃ titanium tetrachloride is added drop-wise in the pure water, fully stirs and be mixed with oyster colloidal sol, the volume ratio of described titanium tetrachloride and pure water is 0.1～0.9: 1;
(B) colloidal sol that (A) is made was placed 6～24 hours, and back colloidal sol must wear out; Pure water is added drop-wise in the colloidal sol of aging back-10～0 ℃ of volume ratio of pressing aging colloidal sol and pure water 0.3～0.7: 1 down, fully stirring is mixed with water white transparency colloidal sol;
(C) take by weighing iron oxide yellow and join in the water white transparency colloidal sol that (B) make, under the condition of 20～40 ℃ of waters bath with thermostatic control, evenly stir 1～3h, obtain sediment, in the iron oxide yellow of adding Fe with (A) in the titanium tetrachloride that adds the Ti amount of substance than 0.5～1.5: 1;
(D) (C) obtained sediment and filter, promptly get described nano titanium oxide through washing, drying, grinding and coat the iron oxide yellow composite.
Further recommending described nano titanium oxide to coat the iron oxide yellow composite is prepared according to following steps:
(A) under-10～0 ℃ titanium tetrachloride is added drop-wise in the pure water, fully stirs and be mixed with oyster colloidal sol, the volume ratio of described titanium tetrachloride and pure water is 0.5: 1;
(B) colloidal sol that (A) is made was placed 10～14 hours, and back colloidal sol must wear out; Pure water is added drop-wise in the colloidal sol of aging back by aging colloidal sol and 0.5: 1 volume ratio of pure water down at-10～0 ℃, fully stirs and be mixed with water white transparency colloidal sol;
(C) take by weighing iron oxide yellow and join in the water white transparency colloidal sol that (B) make, under the condition of 30 ℃ of waters bath with thermostatic control, evenly stir 2h, obtain sediment, in the iron oxide yellow of adding Fe with (A) in the titanium tetrachloride that adds the Ti amount of substance than at 1: 1;
(D) (C) obtained sediment and filter, promptly get described nano titanium oxide through washing, drying, grinding and coat the iron oxide yellow composite.
Utilization of the present invention has the iron oxide yellow (alpha-feooh) of magnetic as carrier, adopts step-by-step precipitation method will have the TiO of superior photocatalysis performance
2Be compound on the carrier, finally prepare titanium dioxide (TiO
2) composite photocatalyst material of clad nano iron oxide yellow (alpha-feooh), by with TiO
2Be coated to the iron oxide yellow surface, can strengthen TiO on the one hand
2Photocatalysis performance, make it be applied to photocatalysis field, simultaneously the antiferromagnetism (TN=393K) that has of alpha-feooh carrier itself can utilize external magnetic field to realize TiO
2Recovery and recycling, reduce cost; On the other hand, can improve the performance (as heat resistance) of iron oxide yellow, thereby expand the range of application of iron oxide yellow pigments, as make the iron oxide yellow after the coating may be used on fields such as senior paint.
Compared with prior art, beneficial effect of the present invention is embodied in:
1, the nano titanium oxide that makes of the inventive method coats the iron oxide yellow composite and coats evenly, and is better dispersed; Composite has obtained reinforcement to the absorbent properties of ultraviolet and visible light, thereby improves photocatalysis performance.The gained composite property is superior, has a extensive future.
2, the inventive method is a raw material with titanium tetrachloride and iron oxide yellow only, does not need to add other any reagent and crystal seed;
3, the inventive method productive rate height, cost is low, and amplification test is convenient in the relatively good control of technical process;
4, the inventive method is less demanding to equipment, is suitable for suitability for industrialized production;
(4) description of drawings
Fig. 1 is preparation TiO of the present invention
2The process chart of/alpha-feooh composite.
Fig. 2 is alpha-feooh and TiO among the embodiment 1
2The X-ray diffractogram of/alpha-feooh composite.Two diffraction curves among Fig. 2 are respectively the diffraction curve and the TiO of alpha-feooh
2/ alpha-feooh diffraction curve.Can observe eight main diffraction maximums from the diffraction curve of alpha-feooh, its 2 times of angles of diffraction (2 θ) are respectively 17.79 °, 21.19 °, 26.30 °, 33.17 °, 36.64 °, 41.18 °, 53.20 °, 59.00 °, by contrasting with alpha-feooh crystal XRD standard spectrogram [PDF#29-0713], eight main diffraction maximums can belong to respectively and are alpha-feooh (021) crystal face, alpha-feooh (110) crystal face, alpha-feooh (120) crystal face, alpha-feooh (130) crystal face, alpha-feooh (111) crystal face, alpha-feooh (140) crystal face, alpha-feooh (221) crystal face, alpha-feooh (151) crystal face.TiO
2Also there are eight the main diffraction curves identical with alpha-feooh in the XRD spectra of/alpha-feooh, compare not bigger variation of peak position with it, only on the peak is strong, weaken to some extent, ° locate to occur a diffraction maximum [PDF#21-1272] that can belong to anatase (101) crystal face in 2 θ=25.30, at TiO
2In/alpha-feooh the composite, titanium dioxide is that anatase form exists.
Fig. 3 is that embodiment 1 makes TiO
2The SEM of/alpha-feooh composite (SEM) photo.Wherein, Fig. 3 A is the pattern of carrier alpha-feooh, and for long bar-shaped, length range is between 0.5 μ m～1.5 μ m; Width range is between 80～120nm; Fig. 3 B is the pattern of sample, therefrom can find out TiO
2/ alpha-feooh composite is for long bar-shaped, and length range is between 0.5 μ m～1.5 μ m; Width range is between 140～160nm; Particle is more complete; Grain spacing is little, intensive; Intergranular border is comparatively clear; The surface that can clearly observe long bar-shaped composite in addition is coated with a small amount of granule.
Fig. 4 is that embodiment 1 makes TiO
2The high-resolution photo of/alpha-feooh composite.The iron oxide yellow surface successfully coats the titanium dioxide of last layer thickness range at 2～5nm as can be seen from Figure; Titanium dioxide evenly is grown in the iron oxide yellow surface; Coat in neat formation; Part titanium dioxide granule is arranged on the outer wall of composite, and this result with SEM observation is consistent.
Fig. 5, Fig. 6 and Fig. 7 are respectively titanium dioxide [P25 (weight ratio of anatase and rutile is approximately 75/25)], iron oxide yellow and TiO
2The UV, visible light of/alpha-feooh composite absorbs the light collection of illustrative plates.From Fig. 5, can observe three tangible absworption peaks, respectively at λ=293nm, λ=388nm and λ=430nm.From Fig. 6, can observe two tangible absworption peaks, respectively at λ=355nm and λ=600nm.From Fig. 7, can observe four tangible absworption peaks, respectively at λ=316nm, λ=404nm, λ=435nm and λ=505nm.The The above results explanation, after titanium dioxide and iron oxide yellow were compound, displacement (comprising blue shift and red shift) had taken place in its absorbing wavelength position to ultraviolet and visible light.This reflects that its absorbent properties to ultraviolet and visible light have obtained reinforcement.
(5) specific embodiment
Below will the present invention is further illustrated by embodiment, but protection scope of the present invention is not limited thereto.
Embodiment 1
(1) capacity is fixed in the ice-water bath for the 500mL there-necked flask, gets distilled water (H
2O) 200mL packs in the there-necked flask; On the middle port of there-necked flask, condenser pipe is installed, is utilized the running water condensation; On a mouth of there-necked flask, thermometer is installed, with the temperature of monitoring and control reaction system; Get TiCl
4100mL packs in the dry constant voltage separatory funnel, the constant voltage separatory funnel is installed on another side mouth of there-necked flask; Under the condition of magnetic agitation and ice-water bath cooling, open the switch of constant voltage separatory funnel, titanium tetrachloride solution is slowly splashed in the distilled water, the temperature that drips speed and ice-water bath by control is controlled at about 0 ℃ the temperature of whole dropping mixed process; Adding along with titanium tetrachloride, the color of system changes gradually, be transformed into oyster by water white transparency, the viscosity of system also increases gradually, and be transformed into the colloid shape by solution, treat that titanium tetrachloride dropwises after, continue again to stir 2 hours, this moment, mixed system was an oyster colloidal sol, and is aging with placing behind its cool to room temperature;
(2) the titanium tetrachloride hydrosol is at room temperature placed 12h after, obtain the aging back of 285mL colloidal sol altogether, get the above-mentioned colloidal sol of aging 60mL and pack in the there-necked flask of 500mL; There-necked flask is fixed in the ice-water bath; On the middle port of there-necked flask, condenser pipe is installed, is utilized the running water condensation; On a mouth of there-necked flask, thermometer is installed, with the temperature of monitoring and control reaction system; Get distilled water 120mL and pack in the dry constant voltage separatory funnel, the constant voltage separatory funnel is installed on another side mouth of there-necked flask; Under the condition of magnetic agitation and ice-water bath cooling, open the switch of constant voltage separatory funnel, distilled water is slowly splashed in the titanium tetrachloride colloid after aging, and the temperature by control rate of addition and ice-water bath is controlled at about-5 ℃ the temperature of whole dropping mixed process; Along with the adding mixed system of distilled water is transformed into water white transparency gradually by oyster, continue again after dropwising to stir 30 minutes;
(3) above-mentioned system is put into thermostat water bath and also slowly be warming up to 30 ℃, and be stabilized in 30 ℃, in molar ratio M
Fe: M
Ti=1: 1, take by weighing iron oxide yellow pigments 18g, it is slowly poured in the above-mentioned diluted titanium tetrachloride hydrosol, continue evenly to stir 2 hours, this moment, system was a yellow suspension;
(4) weighing 300ml distilled water joins in the suspension system after the stirring, and stirring 5min, the solution that obtains after being placed on and leaving standstill 24h in the room temperature is removed the upper strata bright yellow solution, operate a large amount of sediments that obtain for 3 times and so forth, this sediment stirring was filtered after 2 hours, and using alcohol flushing, dry 12h under 80 ℃ promptly gets TiO after the sample that will the obtain grinding then
2/ alpha-feooh composite, 36.785g altogether.Its crystalline phase is formed as shown in Figure 2, and its granularity and pattern are as shown in Figure 3 and Figure 4.
(1) adopts the described appliance arrangement of step (1) among the embodiment 1, get distilled water (H
2O) 200mL packs in the there-necked flask; Get TiCl
4100mL packs in the dry constant voltage separatory funnel; Under the condition of magnetic agitation and ice-water bath cooling, open the switch of constant voltage separatory funnel, titanium tetrachloride solution is slowly splashed in the pure water, by the temperature of controlling rate of addition and ice-water bath the temperature of whole dropping mixed process is controlled at about 0 ℃; After treating that titanium tetrachloride dropwises, continue to stir 2 hours, this moment, mixed system was an oyster colloidal sol, will place behind its cool to room temperature again;
(2) adopt the described appliance arrangement of step (2) among the embodiment 1, the titanium tetrachloride hydrosol is at room temperature placed 6 hours after, obtain aging back colloidal sol; Getting the aging back of 60mL colloidal sol packs in the there-necked flask of 500mL; Get H
2O 150mL packs in the dry constant voltage separatory funnel; Under the condition of magnetic agitation and ice-water bath cooling, open the switch of constant voltage separatory funnel, water is slowly splashed in the deionized water, by the temperature of controlling rate of addition and ice-water bath the temperature of whole dropping mixed process is controlled at about 0 ℃; Along with the adding mixed system of pure water is transformed into water white transparency gradually by oyster, continue again after dropwising to stir 30 minutes;
(3) above-mentioned system is put into thermostat water bath and also slowly be warming up to 20 ℃, and be stabilized in 20 ℃, in molar ratio M
Fe: M
Ti=0.5: 1, take by weighing iron oxide yellow pigments 9g, it is slowly poured in the above-mentioned diluted titanium tetrachloride hydrosol, continue evenly to stir 1 hour, this moment, the color of system was a yellow suspension;
(4) weighing 300ml distilled water joins in the suspension system after the stirring, and stirring 5min, the solution that obtains after being placed on and leaving standstill 24h in the room temperature is removed the upper strata bright yellow solution, operate a large amount of sediments that obtain for 3 times and so forth, this sediment stirring will be filtered after 2 hours, use alcohol flushing, dry 12h under 80 ℃ promptly gets TiO after the sample that will the obtain grinding then
2/ alpha-feooh composite.
Embodiment 3
(1) adopts the described appliance arrangement of step (1) among the embodiment 1, get distilled water (H
2O) 200mL packs in the there-necked flask; Get TiCl
4100mL packs in the dry constant voltage separatory funnel; Under the condition of magnetic agitation and ice-water bath cooling, open the switch of constant voltage separatory funnel, titanium tetrachloride solution is slowly splashed in the pure water, by the temperature of controlling rate of addition and ice-water bath the temperature of whole dropping mixed process is controlled at about 0 ℃; After treating that titanium tetrachloride dropwises, continue to stir 2 hours, this moment, mixed system was an oyster colloidal sol, will place behind its cool to room temperature again;
(2) adopt the described appliance arrangement of step (2) among the embodiment 1, the placement of titanium tetrachloride hydrosol room temperature after 24 hours, is obtained aging back colloidal sol; Getting the aging back of 60mL colloidal sol packs in the there-necked flask of 500mL; Get H
2O 90mL packs in the dry constant voltage separatory funnel; Under the condition of magnetic agitation and ice-water bath cooling, open the switch of constant voltage separatory funnel, water is slowly splashed in the deionized water, by the temperature of controlling rate of addition and ice-water bath the temperature of whole dropping mixed process is controlled at about-10 ℃; Along with the adding mixed system of pure water is transformed into water white transparency gradually by oyster, continue again after dropwising to stir 30 minutes;
(3) above-mentioned system is put into thermostat water bath and also slowly be warming up to 40 ℃, and be stabilized in 40 ℃, in molar ratio M
Fe: M
Ti=1.5: 1, take by weighing iron oxide yellow pigments 27g, it is slowly poured in the above-mentioned diluted titanium tetrachloride hydrosol, continue evenly to stir 3 hours, this moment, the color of system was a yellow suspension;
(4) weighing 300ml distilled water joins in the suspension system after the stirring, and stirring 5min, the solution that obtains after being placed on and leaving standstill 24h in the room temperature is removed the upper strata bright yellow solution, operate a large amount of sediments that obtain for 3 times and so forth, this sediment stirring will be filtered after 2 hours, use pure water rinsing, dry 12h under 80 ℃ promptly gets TiO after the sample that will the obtain grinding then
2/ alpha-feooh composite.
Claims (10)
1. a nano titanium oxide coats the iron oxide yellow composite, is to be carrier with the iron oxide yellow, and nano titanium oxide is coated on carrier surface, and described nano titanium oxide belongs to the anatase phase; Described composite is for long bar-shaped, and longitudinal length is between 0.5 μ m～1.5 μ m, and laterally particle diameter is at 140～160nm; Fe is 0.5～1.5: 1 with the amount of substance ratio of Ti in the described composite.
2. nano titanium oxide as claimed in claim 1 coats the iron oxide yellow composite, it is characterized in that described composite is carrier with the iron oxide yellow, nano titanium oxide evenly is coated on carrier surface and forms the nanometer titanium dioxide layer of thickness at 2～5nm, and also sporadicly is distributed with the titanium dioxide nanoparticle of particle size range at 5～20nm at the outer wall of composite.
3. nano titanium oxide as claimed in claim 1 coats the iron oxide yellow composite, it is characterized in that the amount of substance ratio of Fe and Ti is 1: 1 in the described composite.
4. a nano titanium oxide as claimed in claim 1 coats the preparation method of iron oxide yellow composite, it is characterized in that described method comprises the steps: titanium tetrachloride is mixed with the hydrosol, the hydrosol place aging after thin up again, obtain water white transparency colloidal sol; Get iron oxide yellow and join in the water white transparency colloidal sol, evenly stir 1～3h under the condition of 20～40 ℃ of waters bath with thermostatic control, obtain sediment, the gained sediment promptly gets described nano titanium oxide through washing, drying, grinding and coats the iron oxide yellow composite; Ti amount of substance ratio in the iron oxide yellow that adds in the titanium tetrachloride of Fe and adding is 0.5～1.5: 1.
5. nano titanium oxide as claimed in claim 4 coats the preparation method of iron oxide yellow composite, and after it is characterized in that adding iron oxide yellow, it is 30 ℃ that water bath with thermostatic control is set, mixing time 2h.
6. coat the preparation method of iron oxide yellow composites as claim 4 or 5 described nano titanium oxides, it is characterized in that the described hydrosol prepares as follows: under-10～0 ℃, titanium tetrachloride is added drop-wise in the pure water, fully stir and be mixed with oyster colloidal sol, the volume ratio of described titanium tetrachloride and pure water is 0.1～0.9: 1.
7. as the preparation method of claim 4 or 5 described nano titanium oxides coating iron oxide yellow composites, it is characterized in that aging 6～24 hours of described hydrosol placement.
8. coat the preparation method of iron oxide yellow composites as claim 4 or 5 described nano titanium oxides, after it is characterized in that hydrosol placement is aging, volume ratio at-10～0 ℃ of aging back colloidal sol and pure water 0.3～0.7: 1 is added drop-wise to pure water in the colloidal sol of aging back, fully stirs and is mixed with water white transparency colloidal sol.
9. nano titanium oxide as claimed in claim 4 coats the preparation method of iron oxide yellow composite, it is characterized in that specifically carrying out according to following steps:
(A) under-10～0 ℃ titanium tetrachloride is added drop-wise in the pure water, fully stirs and be mixed with oyster colloidal sol, the volume ratio of described titanium tetrachloride and pure water is 0.1～0.9: 1;
(B) colloidal sol that (A) is made is placed and was worn out in 6～24 hours, and the back colloidal sol that must wear out is added drop-wise to pure water in the aging colloidal sol-10～0 ℃ of volume ratio of pressing aging back colloidal sol and pure water 0.3～0.7: 1 down, fully stirs and is mixed with water white transparency colloidal sol;
(C) taking by weighing iron oxide yellow joins in the water white transparency colloidal sol that (B) make, under the condition of 20～40 ℃ of waters bath with thermostatic control, evenly stir 1～3h, obtain sediment, in the iron oxide yellow of adding Fe with (A) in Ti amount of substance ratio in the titanium tetrachloride that adds be 0.5～1.5: 1;
(D) (C) obtained sediment and filter, promptly get nano titanium oxide through washing, drying, grinding and coat the iron oxide yellow composite.
10. nano titanium oxide as claimed in claim 4 coats the preparation method of iron oxide yellow composite, it is characterized in that specifically carrying out according to following steps:
(A) under-10～0 ℃ titanium tetrachloride is added drop-wise in the pure water, fully stirs and be mixed with oyster colloidal sol, the volume ratio of described titanium tetrachloride and pure water is 0.5: 1;
(B) the colloidal sol room temperature that (A) is made is placed and was worn out in 10～14 hours, and the back colloidal sol that must wear out is added drop-wise to pure water in the aging colloidal sol by aging back colloidal sol and 0.5: 1 volume ratio of pure water down at-10～0 ℃, fully stirs and is mixed with water white transparency colloidal sol;
(C) take by weighing iron oxide yellow and join in the water white transparency colloidal sol that (B) make, under the condition of 30 ℃ of waters bath with thermostatic control, evenly stir 2h, obtain sediment, in the iron oxide yellow of adding Fe with (A) in Ti amount of substance ratio in the titanium tetrachloride that adds be 1: 1;
(D) (C) obtained sediment and filter, promptly get nano titanium oxide through washing, drying, grinding and coat the iron oxide yellow composite.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010266641 CN101947450B (en) | 2010-08-30 | 2010-08-30 | Nanometer titanium dioxide-coated iron oxide yellow composite material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201010266641 CN101947450B (en) | 2010-08-30 | 2010-08-30 | Nanometer titanium dioxide-coated iron oxide yellow composite material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101947450A true CN101947450A (en) | 2011-01-19 |
| CN101947450B CN101947450B (en) | 2012-12-12 |
Family
ID=43451151
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201010266641 Active CN101947450B (en) | 2010-08-30 | 2010-08-30 | Nanometer titanium dioxide-coated iron oxide yellow composite material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101947450B (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350352A (en) * | 2011-07-15 | 2012-02-15 | 浙江工业大学 | Preparation method of iron-doped TiO2 nanotube |
| CN102627874A (en) * | 2012-03-19 | 2012-08-08 | 电子科技大学 | Composite-structure pigment having low lightness and infrared emitting ability and preparation method thereof |
| CN102898182A (en) * | 2012-11-01 | 2013-01-30 | 景德镇陶瓷学院 | Method for preparing vanadium-zirconium yellow ceramic pigment by using sol-precipitation method |
| CN115160825A (en) * | 2022-08-18 | 2022-10-11 | 亚士创能新材料(滁州)有限公司 | Modified yellow pigment and preparation method and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1225659A (en) * | 1997-05-23 | 1999-08-11 | 默克专利股份有限公司 | Metal oxide coated titanium dioxide lamellas |
| CN1631795A (en) * | 2004-11-16 | 2005-06-29 | 浙江工业大学 | Process for preparing rutile phase titanium dioxide nano-powder |
| CN101475214A (en) * | 2008-10-21 | 2009-07-08 | 浙江工业大学 | Preparation of iron-doped nitrogen-doped nano titanium dioxide powder |
-
2010
- 2010-08-30 CN CN 201010266641 patent/CN101947450B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1225659A (en) * | 1997-05-23 | 1999-08-11 | 默克专利股份有限公司 | Metal oxide coated titanium dioxide lamellas |
| CN1631795A (en) * | 2004-11-16 | 2005-06-29 | 浙江工业大学 | Process for preparing rutile phase titanium dioxide nano-powder |
| CN101475214A (en) * | 2008-10-21 | 2009-07-08 | 浙江工业大学 | Preparation of iron-doped nitrogen-doped nano titanium dioxide powder |
Non-Patent Citations (1)
| Title |
|---|
| 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 20081115 龚潇 针铁矿负载二氧化钛制备复合光催化剂的性能研究 第14-23，41-42页 1-10 , 第11期 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102350352A (en) * | 2011-07-15 | 2012-02-15 | 浙江工业大学 | Preparation method of iron-doped TiO2 nanotube |
| CN102627874A (en) * | 2012-03-19 | 2012-08-08 | 电子科技大学 | Composite-structure pigment having low lightness and infrared emitting ability and preparation method thereof |
| CN102898182A (en) * | 2012-11-01 | 2013-01-30 | 景德镇陶瓷学院 | Method for preparing vanadium-zirconium yellow ceramic pigment by using sol-precipitation method |
| CN115160825A (en) * | 2022-08-18 | 2022-10-11 | 亚士创能新材料(滁州)有限公司 | Modified yellow pigment and preparation method and application thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101947450B (en) | 2012-12-12 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Meng et al. | Hierarchical structured ZnFe2O4@ SiO2@ TiO2 composite for enhanced visible-light photocatalytic activity | |
| Zhao et al. | Phase and morphological transitions of titania/titanate nanostructures from an acid to an alkali hydrothermal environment | |
| Zhang et al. | Synthesis and photocatalytic properties of highly stable and neutral TiO2/SiO2 hydrosol | |
| Obregón et al. | On the different photocatalytic performance of BiVO4 catalysts for methylene blue and rhodamine B degradation | |
| Lu et al. | Preparation and efficient visible light-induced photocatalytic activity of m-BiVO4 with different morphologies | |
| Karthick et al. | Formation of anatase TiO2 nanoparticles by simple polymer gel technique and their properties | |
| CN102912620B (en) | Method for modifying nanometer titanium dioxide polyester fiber with high photocatalytic activity | |
| CN101597084B (en) | Method for synthesizing anatase phase titanium dioxide nanometer particle by microreactor | |
| CN100406117C (en) | Magnetic photocatalyst and its preparing method | |
| CN104841015B (en) | High-specific-surface-area silver-loaded titanium dioxide composite antibacterial material and preparation method thereof | |
| CN103240073B (en) | Zn<2+>-doped BiVO4 visible-light-driven photocatalyst and preparation method thereof | |
| CN102600822A (en) | Carbon-doped silicon dioxide and titanium dioxide composite photocatalyst and preparation method thereof | |
| CN102616849A (en) | Method for directly synthesizing M-phase vanadium dioxide nano particles by liquid phase method | |
| CN101947450B (en) | Nanometer titanium dioxide-coated iron oxide yellow composite material and preparation method thereof | |
| Tang et al. | Degradation mechanism and pathway of tetracycline in milk by heterojunction N-TiO2-Bi2WO6 film under visible light | |
| CN101579628B (en) | Preparation method of nickel ferrite based magnetic loaded type titanium dioxide photo-catalyst | |
| CN101618342A (en) | Polymer modified high-activity nano titanium dioxide catalyst and preparation method thereof | |
| CN109529872A (en) | Amorphous nano titanium dioxide visible light catalyzer compound and preparation method thereof | |
| Zhang et al. | Enhanced photocatalytic performance of Bi4Ti3O12 nanosheets synthesized by a self-catalyzed fast reaction process | |
| Hassanzadeh-Tabrizi | Synthesis and characterization of nano Ce doped ZnO/γ-Al2O3 with improved photocatalytic activity | |
| Niu et al. | Structures and photocatalytic activity of α-Fe2O3@ TiO2 core-shell nanoparticles | |
| Sun et al. | Methods for preparing and enhancing photocatalytic activity of basic bismuth nitrate | |
| CN102219255B (en) | Preparation method for mixed crystal form nanometer titanium dioxide turbid liquor with high stability | |
| CN100389871C (en) | Magnetic nanometer photocatalyst and its prepn. method | |
| CN102350352B (en) | Preparation method of iron-doped TiO2 nanotube |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| TR01 | Transfer of patent right |
Effective date of registration: 20191224 Address after: 314400 No.2, Fengshou Avenue, Haining warp knitting industrial park, Jiaxing City, Zhejiang Province Patentee after: Zhejiang Haining Warp Knitting Industrial Park Development Co.,Ltd. Address before: 510000 unit 2414-2416, building, No. five, No. 371, Tianhe District, Guangdong, China Patentee before: GUANGDONG GAOHANG INTELLECTUAL PROPERTY OPERATION Co.,Ltd. Effective date of registration: 20191224 Address after: 510000 unit 2414-2416, building, No. five, No. 371, Tianhe District, Guangdong, China Patentee after: GUANGDONG GAOHANG INTELLECTUAL PROPERTY OPERATION Co.,Ltd. Address before: Hangzhou City, Zhejiang province 310014 City Zhaohui District Six Patentee before: Zhejiang University of Technology |
|
| TR01 | Transfer of patent right |