CN100545218C - The method of enwrapping ferric oxide by silicon dioxide - Google Patents
The method of enwrapping ferric oxide by silicon dioxide Download PDFInfo
- Publication number
- CN100545218C CN100545218C CNB2007101909350A CN200710190935A CN100545218C CN 100545218 C CN100545218 C CN 100545218C CN B2007101909350 A CNB2007101909350 A CN B2007101909350A CN 200710190935 A CN200710190935 A CN 200710190935A CN 100545218 C CN100545218 C CN 100545218C
- Authority
- CN
- China
- Prior art keywords
- ferric oxide
- tetraethoxy
- polyvinylpyrrolidone
- oxide particles
- solution
- 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.)
- Expired - Fee Related
Links
Images
Abstract
The invention discloses a kind of method of enwrapping ferric oxide by silicon dioxide, may further comprise the steps: ferric oxide particles is dispersed in the mixing solutions of pure and mild ammoniacal liquor; Under agitation condition, join then in the Pentyl alcohol solution of polyvinylpyrrolidone, continue to stir 15 minutes～1 hour; The alcoholic solution of tetraethoxy is joined under agitation condition in the above-mentioned reaction solution, continue to stir 6～24 hours; With reaction solution centrifugal after, remove liquid portion, the ferric oxide particles of silicon-dioxide parcel.The present invention utilizes polyvinylpyrrolidone to the constraint of water with to the favourable absorption effect of ferric oxide, successfully with the hydrolysis reaction local of tetraethoxy in the surface of ferric oxide, thereby realized even silicon-dioxide parcel to ferric oxide.The bed thickness of silicon-dioxide can recently increase continuously by the quality that increases tetraethoxy and ferric oxide particles simply.It is with low cost, simple to operate that the present invention has, advantage such as need not complex apparatus, can produce fast in enormous quantities.
Description
Technical field
The present invention relates to a kind of method of enwrapping ferric oxide by silicon dioxide.
Background technology
Because do not have toxicity, cheapness and relative stability, ferric oxide has at aspects such as magnetic recording medium, catalyzer, gas sensor, pigment, optics, rechargeable battery and electromagnetic devices to be used widely and becomes one of present popular research topic.For the stability of ferric oxide and the application of expansion ferric oxide, existing many such as micro emulsion method [S.Santra, R.Tapec, N, Theodoropoulou, J, Dobson, A, Hebard, W, Tan, Langmuir, 2001,17,2900], molecular template method [P.Wu, J.Zhu, Z.Xu, Adv.Funct.Mater.2004,14,345], improvement
Method [Y.Lu, Y.Yin, B.T..Mayers, Y.Xia, Nano.Lett.2002,2,183], [L.Hao, C.Zhu, W.-Q.Jiang, C.-N.Chen, Y.Hu, Z.-Y.Chen, J.Mater.Chem.2004,14,2929], [C.Yang, G.Wang, Z.Lu, J.Sun, J.Zhuang, W.Yang, J.Mater.Chem.2005,15,4252], [Y.-S.Han, G.-Y.Jeong, S.-Y.Lee, H.-K.Kim, J.Solid State Chem.2007,180,2978], [A.P.Phylipse, M.P.B.van Bruggen, C.Path, Langmuir 1994,10,92], [Z.Dai, F.Meiser, H.
J.Colloid Interface Sci.2005,288,298] etc. be developed and be used for ferric oxide is evenly superscribed silicon-dioxide.Yet all reported method have usually reunion, distortion sphere, polymolecularity, need carry out extra surface treatment in case generate limitation such as new nuclear.
Summary of the invention
Goal of the invention: the purpose of this invention is to provide a kind of method of enwrapping ferric oxide by silicon dioxide, with limitation such as the sphere that overcomes above-mentioned reunion, distortion, polymolecularity.
Technical scheme: the present invention has adopted a kind of new water/polyvinylpyrrolidone/Pentyl alcohol system, utilize polyvinylpyrrolidone in this system to the constraint of water with to the favourable absorption effect of ferric oxide, can be with the hydrolysis reaction local of tetraethoxy in the surface of ferric oxide, thus realized the even parcel of silicon-dioxide to ferric oxide.
The method of enwrapping ferric oxide by silicon dioxide of the present invention may further comprise the steps:
1, ferric oxide particles is dispersed in the mixing solutions of pure and mild ammoniacal liquor, the mass percent that ammoniacal liquor accounts for pure ammonia mixed solution is 10～50%, ammoniated mass percent is 25～28% in the ammoniacal liquor, and the mass ratio of ferric oxide particles and pure ammonia mixed solution is 0.025～2.5: 100;
2, the ferric oxide suspension with step 1 gained joins under agitation condition in the Pentyl alcohol solution of polyvinylpyrrolidone, continue to stir 15 minutes～1 hour, the mass percent that polyvinylpyrrolidone accounts for the Pentyl alcohol solution of polyvinylpyrrolidone is 0.3-2%, and the mass ratio of the Pentyl alcohol solution of ferric oxide suspension and polyvinylpyrrolidone is: 5～24: 100;
3, the alcoholic solution with tetraethoxy joins in the reaction solution of step 2 gained under agitation condition, continue to stir 6～24 hours, the mass percent that tetraethoxy accounts for the alcoholic solution of tetraethoxy is 10～50%, and the mass ratio of used ferric oxide particles is 0.5～200: 1 in tetraethoxy and the step 1;
4, with reaction solution centrifugal after, remove liquid portion, the ferric oxide particles of silicon-dioxide parcel.
Wherein, the alcohol described in the step 1 is methyl alcohol, ethanol or propyl alcohol.
Wherein, the alcohol described in the step 3 is methyl alcohol, ethanol or propyl alcohol.
Wherein, in the step 3, can increase the bed thickness of silicon-dioxide continuously, see Table 1 by the mass ratio that increases tetraethoxy and ferric oxide particles.
The relation of the mass ratio of table 1 tetraethoxy and ferric oxide particles and the bed thickness of silicon-dioxide
Beneficial effect: the present invention compared with prior art has following outstanding advantage:
1, the present invention has successfully overcome the sphere, polymolecularity of reunion common in the enwrapping ferric oxide by silicon dioxide method of the prior art, distortion, extra limitation such as surface treatment, has realized the even parcel of ferric oxide.
2, the silicon-dioxide bed thickness of the ferric oxide-silica dioxide composite particles of gained of the present invention can be regulated in the 10-200 nanometer range.
3, the prepared ferric oxide-silicon dioxide composite ball shape particle of the present invention successfully is assembled into photonic crystal first owing to having more excellent monodispersity and sphere.Fig. 2 is promptly provable, and prepared opal structural crystal has tangible photonic band gap, has shown that fully the prepared ferric oxide of present method-silicon dioxide composite ball shape particle has monodispersity and sphere preferably.
4, the present invention can realize large-scale commercial production.
5, technology of the present invention is simple, and is very low to equipment requirements, low production cost.
Description of drawings
Fig. 1 is wrapped 10 nanometers (a) for spherical iron oxide particles, 60 nanometers (b), 80 nanometers (c), and the transmission electron microscope figure of the composite particles of the thick silicon-dioxide of 200 nanometers (d).
The opal structural crystalline scanning electron microscope diagram that Fig. 2 (a) is assembled into for the composite particles (being the silicon-dioxide that spherical iron oxide particles is wrapped 60 nanometer thickness) shown in Fig. 1 (b).
The opal structural crystalline scanning electron microscope diagram that Fig. 2 (b) is assembled into for the composite particles (being the silicon-dioxide that spherical iron oxide particles is wrapped 80 nanometer thickness) shown in Fig. 1 (c).
Fig. 2 (c) is an opal structural crystalline transmitted light spectrogram, and wherein curve 1 is a crystalline transmitted spectrum shown in Fig. 2 (a), and curve 2 is a crystalline transmitted spectrum shown in Fig. 2 (b).
Embodiment
Embodiment 1:
Ferric oxide particles is dispersed in the mixing solutions of ethanol and ammoniacal liquor (ammoniated mass percent is 25～28% in the ammoniacal liquor), the mass percent that ammoniacal liquor accounts for pure ammonia mixed solution is 20%, and the mass percent of ferric oxide particles and hydramine mixed solution is 0.47: 100; Then gained ferric oxide suspension is joined under agitation condition in the Pentyl alcohol solution of polyvinylpyrrolidone, the mass percent that polyvinylpyrrolidone accounts for the Pentyl alcohol of polyvinylpyrrolidone is 1.25%, and the mass ratio of the Pentyl alcohol solution of ferric oxide suspension and polyvinylpyrrolidone is 20: 100; Stir after 30 minutes, add the ethanolic soln of tetraethoxy again in the reaction solution of above gained, tetraethoxy is 20% with the mass percent that accounts for the ethanolic soln of tetraethoxy, and the mass ratio of tetraethoxy and ferric oxide particles is controlled to be 1.2: 1; Continue to stir 12 hours, with the gained reaction soln centrifugal after, remove liquid portion, promptly get the ferric oxide particles that silicon-dioxide wraps up, its transmission electron microscope figure sees Fig. 1 a.
Embodiment 2:
Ferric oxide particles is dispersed in the mixing solutions of ethanol and ammoniacal liquor (ammoniated mass percent is 25～28% in the ammoniacal liquor), the mass percent that ammoniacal liquor accounts for pure ammonia mixed solution is 20%, and the mass percent of ferric oxide particles and hydramine mixed solution is 0.03: 100; Then gained ferric oxide suspension is joined under agitation condition in the Pentyl alcohol solution of polyvinylpyrrolidone, the mass percent that polyvinylpyrrolidone accounts for the Pentyl alcohol of polyvinylpyrrolidone is 1.25%, and the mass ratio of the Pentyl alcohol solution of ferric oxide suspension and polyvinylpyrrolidone is 20: 100; Stir after 30 minutes, add the ethanolic soln of tetraethoxy again in the reaction solution of above gained, tetraethoxy is 20% with the mass percent that accounts for the ethanolic soln of tetraethoxy, and the mass ratio of tetraethoxy and ferric oxide particles is controlled to be 186.7: 1; Continue to stir 12 hours, with the gained reaction soln centrifugal after, remove liquid portion, promptly get the ferric oxide particles that silicon-dioxide wraps up, its transmission electron microscope figure sees Fig. 1 d.
Embodiment 3:
Ferric oxide particles is dispersed in the mixing solutions of methyl alcohol and ammoniacal liquor (ammoniated mass percent is 25～28% in the ammoniacal liquor), the mass percent that ammoniacal liquor accounts for pure ammonia mixed solution is 10%, and the mass percent of ferric oxide particles and hydramine mixed solution is 0.025: 100; Then gained ferric oxide suspension is joined under agitation condition in the Pentyl alcohol solution of polyvinylpyrrolidone, the mass percent that polyvinylpyrrolidone accounts for the Pentyl alcohol of polyvinylpyrrolidone is 0.3%, and the mass ratio of the Pentyl alcohol solution of ferric oxide suspension and polyvinylpyrrolidone is 5: 100; Stir after 15 minutes, add the methanol solution of tetraethoxy again in the reaction solution of above gained, tetraethoxy is 10% with the mass percent that accounts for the methanol solution of tetraethoxy, and the mass ratio of tetraethoxy and ferric oxide particles is controlled to be 0.5: 1; Continue to stir 6 hours, with the gained reaction soln centrifugal after, remove liquid portion, promptly get the ferric oxide particles that silicon-dioxide wraps up.
Embodiment 4:
Ferric oxide particles is dispersed in the mixing solutions of propyl alcohol and ammoniacal liquor (ammoniated mass percent is 25～28% in the ammoniacal liquor), the mass percent that ammoniacal liquor accounts for pure ammonia mixed solution is 50%, and the mass percent of ferric oxide particles and hydramine mixed solution is 2.5: 100; Then gained ferric oxide suspension is joined under agitation condition in the Pentyl alcohol solution of polyvinylpyrrolidone, the mass percent that polyvinylpyrrolidone accounts for the Pentyl alcohol of polyvinylpyrrolidone is 2%, and the mass ratio of the Pentyl alcohol solution of ferric oxide suspension and polyvinylpyrrolidone is 24: 100; Stir after 1 hour, add the methanol solution of tetraethoxy again in the reaction solution of above gained, tetraethoxy is 50% with the mass percent that accounts for the methanol solution of tetraethoxy, and the mass ratio of tetraethoxy and ferric oxide particles is controlled to be 200: 1; Continue to stir 24 hours, with the gained reaction soln centrifugal after, remove liquid portion, promptly get the ferric oxide particles that silicon-dioxide wraps up.
Claims (3)
1, a kind of method of enwrapping ferric oxide by silicon dioxide is characterized in that this method may further comprise the steps:
(1) ferric oxide particles is dispersed in the mixing solutions of pure and mild ammoniacal liquor, the mass percent that ammoniacal liquor accounts for pure ammonia mixed solution is 10～50%, ammoniated mass percent is 25～28% in the ammoniacal liquor, and the mass ratio of ferric oxide particles and pure ammonia mixed solution is 0.025～2.5: 100;
(2) the ferric oxide suspension with step (1) gained joins under agitation condition in the Pentyl alcohol solution of polyvinylpyrrolidone, continue to stir 15 minutes～1 hour, the mass percent that polyvinylpyrrolidone accounts for the Pentyl alcohol solution of polyvinylpyrrolidone is 0.3～2%, and the mass ratio of the Pentyl alcohol solution of ferric oxide suspension and polyvinylpyrrolidone is 5～24: 100;
(3) alcoholic solution with tetraethoxy joins under agitation condition in the reaction solution of step (2) gained, continue to stir 6～24 hours, the mass percent that tetraethoxy accounts for the alcoholic solution of tetraethoxy is 10～50%, and the mass ratio of used ferric oxide particles is 0.5～200: 1 in tetraethoxy and the step (1);
(4) with reaction solution centrifugal after, remove liquid portion, the ferric oxide particles of silicon-dioxide parcel.
2, the method for enwrapping ferric oxide by silicon dioxide according to claim 1 is characterized in that the alcohol described in the step (1) is methyl alcohol, ethanol or propyl alcohol.
3, the method for enwrapping ferric oxide by silicon dioxide according to claim 1 is characterized in that the alcohol described in the step (3) is methyl alcohol, ethanol or propyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101909350A CN100545218C (en) | 2007-12-03 | 2007-12-03 | The method of enwrapping ferric oxide by silicon dioxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2007101909350A CN100545218C (en) | 2007-12-03 | 2007-12-03 | The method of enwrapping ferric oxide by silicon dioxide |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101186762A CN101186762A (en) | 2008-05-28 |
| CN100545218C true CN100545218C (en) | 2009-09-30 |
Family
ID=39479391
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2007101909350A Expired - Fee Related CN100545218C (en) | 2007-12-03 | 2007-12-03 | The method of enwrapping ferric oxide by silicon dioxide |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN100545218C (en) |
Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568348A (en) * | 2016-01-19 | 2016-05-11 | 上海应用技术学院 | Method for assisting composite plating with magnetic field |
| CN107286705B (en) * | 2016-03-30 | 2020-12-11 | 长城汽车股份有限公司 | Nano inorganic composite pigment and preparation method thereof |
| CN107486036A (en) * | 2017-09-13 | 2017-12-19 | 铜陵海源超微粉体有限公司 | A kind of preparation method containing modified magnetic iron oxide Vingon electrostatic spinning crosslinking filter membrane |
| CN107603082A (en) * | 2017-09-13 | 2018-01-19 | 铜陵海源超微粉体有限公司 | A kind of preparation method of the copolymerized Vingon crosslinking flaky material of porous modified oxidized iron |
| CN107715851B (en) * | 2017-09-13 | 2020-07-17 | 铜陵亿智达科技成果转化有限公司 | Preparation method of high-adsorptivity modified iron oxide composite microporous polyvinylidene chloride material |
| CN113912971A (en) * | 2021-09-29 | 2022-01-11 | 华东理工大学 | Silicon dioxide and iron oxide composite material and preparation method thereof |
| CN116179090B (en) * | 2022-11-16 | 2024-02-09 | 深圳市东升塑胶制品有限公司 | Ultrathin single-sided hot melt adhesive tape applied to lithium battery |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086232A (en) * | 1992-10-24 | 1994-05-04 | 泰奥塞集团服务有限公司 | The method of coating inorganic particles |
| US6773814B2 (en) * | 2001-08-08 | 2004-08-10 | Degussa Ag | Metal oxide particles coated with silicon dioxide |
| CN1562464A (en) * | 2004-03-31 | 2005-01-12 | 深圳清华大学研究院 | Magnetic nano T102 composite photocatalysis and preparation method |
-
2007
- 2007-12-03 CN CNB2007101909350A patent/CN100545218C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1086232A (en) * | 1992-10-24 | 1994-05-04 | 泰奥塞集团服务有限公司 | The method of coating inorganic particles |
| US6773814B2 (en) * | 2001-08-08 | 2004-08-10 | Degussa Ag | Metal oxide particles coated with silicon dioxide |
| CN1562464A (en) * | 2004-03-31 | 2005-01-12 | 深圳清华大学研究院 | Magnetic nano T102 composite photocatalysis and preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 纳米铁/SiO2核壳复合粒子的制备与性能表征. 高国华.武汉理工大学学报，第26卷第9期. 2004 |
| 纳米铁/SiO2核壳复合粒子的制备与性能表征. 高国华.武汉理工大学学报，第26卷第9期. 2004 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101186762A (en) | 2008-05-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100545218C (en) | The method of enwrapping ferric oxide by silicon dioxide | |
| Guo et al. | Synthesis and characterization of carbon sphere-silica core–shell structure and hollow silica spheres | |
| CN103317141B (en) | Method for preparing metal nanoparticles | |
| Liu et al. | Ultrasonic-assisted ultra-rapid synthesis of monodisperse meso-SiO2@ Fe3O4 microspheres with enhanced mesoporous structure | |
| US20190039142A1 (en) | A method for preparing silver powder by using micro-nano bubbles as crystal seeds | |
| CN103464065B (en) | Magnetic nanosphere with mesoporous shell and quick preparation method thereof | |
| CN101069930A (en) | Method for preparing silver/silicon dixoide nucleocapsid structure nano particles | |
| CN101599335A (en) | A kind of oxidation resistant dimethyl silicon oil based magnetic fluid and preparation method thereof | |
| Li et al. | Synthesis of octahedral and cubic Cu 2 O microcrystals in sub-and super-critical methanol and their photocatalytic performance | |
| CN106883818B (en) | Hud typed carbon ball/carbon nano tube composite wave-absorbing material and preparation method | |
| CN100531973C (en) | Method for preparing cube shaped copper particles | |
| CN106040307B (en) | One step hydro thermal method synthesizes Fe3O4(PAA) preparation method of@C-Au core-shell structure microballoon | |
| CN105536877A (en) | Preparation of superparamagnetic Fe3O4-PAMAM-ZnO / TiO2 nanoparticles with core-shell composite structure | |
| CN106674290A (en) | Preparation method of monodispersed cobalt and nickel composite MOF-74 | |
| CN110882702A (en) | Preparation method and application of catalytic material based on magnetic layered double hydroxide | |
| CN102861925A (en) | Rapid preparation method of novel stable nano zero-valent iron particle | |
| CN112429739A (en) | Method for preparing silicon dioxide/nitrogen doped carbon nano tube with wave absorption performance | |
| CN108706568A (en) | A kind of preparation method of N doping Porous hollow carbon Nano capsule material and the material of preparation | |
| Zhang et al. | Au catalyst decorated silica spheres: Synthesis and high-performance in 4-nitrophenol reduction | |
| CN102877130B (en) | Preparation method of bismuth ferrite BiFeO3 monocrystal micrometer sheet | |
| CN103172073B (en) | Preparation method of hollow silica submicron sphere having core | |
| CN104985194B (en) | A kind of preparation method at oxide dispersion intensifying iron cobalt nano composite powder end | |
| CN108017047B (en) | Rambutan-like aza-hollow mesoporous carbon sphere nano material and preparation method thereof | |
| Zhang et al. | Photo-assisted Fenton reactions and growth evolution of crack-urchined CuBi2O4 microspheres assembled by nanorods | |
| CN105597674B (en) | A kind of preparation method of iron@ferroso-ferric oxides@carbon composites |
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 | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20090930 Termination date: 20101203 |