CN103956245A - Preparation method of ferroferric oxide/silica composite powder of shell-core structure - Google Patents
Preparation method of ferroferric oxide/silica composite powder of shell-core structure Download PDFInfo
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- CN103956245A CN103956245A CN201410162015.8A CN201410162015A CN103956245A CN 103956245 A CN103956245 A CN 103956245A CN 201410162015 A CN201410162015 A CN 201410162015A CN 103956245 A CN103956245 A CN 103956245A
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Abstract
The invention discloses a preparation method of ferroferric oxide/silica composite powder of a shell-core structure. Silica powder is used as a core-covering matrix, ferric salt is used as a coating agent, a precipitation method is used for preparing a precursor of ferric hydroxide/silica, and the ferroferric oxide/silica composite powder is obtained after calcination. Ferroferric oxide is evenly coated on the surface of silica. The coating of the ferroferric oxide can effectively eliminate the hydroxyl group on the surface of the silica, and the dispersion ability is improved; the silica is enabled to be magnetic, the additional value of the silica is improved, and the application field is widened.
Description
Technical field
The present invention relates to a kind of process for modifying surface of silicon-dioxide powdery material, particularly a kind of preparation method of tri-iron tetroxide/silicon dioxide composite powder of shell-core structure.
Background technology
Along with fabrication of new materials technology is to the microcosmic development that becomes more meticulous, the reunion of powder and scattering problem have become the bottleneck of preparation and development new material and superfine powder, and the modification technology of powder becomes more and more important.
Due to activity hydroxy and water absorption thereof that poly-silica and the outer surface of silicon dioxide inside exist, make it be hydrophily, in organic phase, be difficult to moistening and disperse, and between organic matrix, adhesion is poor, easily causes boundary defect, the performance of composite material is reduced; And because its surface exists hydroxyl, surface can be larger, aggregation always tends to cohesion, thereby the application performance of product is affected.Therefore, silicon-dioxide powdery material is carried out to surface modification treatment, improving its dispersiveness has become the hot issue of research silicon-dioxide powdery.
Carry out at present silicon dioxide powder surface modification both at home and abroad and mainly contain silane coupler modified, polymer graft polymeric modification and esterification to improve its dispersed method.For silane coupler modified, best with HMDS treatment effect at present, but HMDS is expensive; For polymer graft polymeric modification, cannot avoid the existence of homopolymerization, exist so have a certain amount of homopolymers in final system, and percent grafting is not high; And ester group facile hydrolysis in esterification, and poor heat stability.
The defect existing based on above technology, the present invention proposes taking molysite as coating agent and realize the method at silica surface coated ferriferrous oxide, tri-iron tetroxide/the silicon dioxide of the shell-core structure making after modification can be eliminated the hydroxyl of silica surface effectively, improve its dispersibility, and silicon-dioxide powdery band is magnetic.
Summary of the invention
The present invention is directed to the deficiency that prior art exists, proposed a kind of preparation method of tri-iron tetroxide/silicon dioxide composite powder of shell-core structure, to realize the object of silica surface modification.
Technical problem to be solved by this invention is achieved through the following technical solutions.A kind of preparation method of tri-iron tetroxide/silicon dioxide composite powder of shell-core structure, it is characterized in that, taking silicon-dioxide powdery as bag core matrix, molysite is coating agent, adopt the precipitation method to prepare presoma iron hydroxide/silicon dioxide, then obtain tri-iron tetroxide/silicon dioxide composite powder through calcining.
3, technical problem to be solved by this invention is come further to realize by the following technical programs.A preparation method for the tri-iron tetroxide/silicon dioxide composite powder of shell-core structure, is characterized in that, its step is as follows:
(1) molysite is dissolved in deionized water, makes Fe by magnetic stirrer until aluminium salt dissolves completely
3+concentration is the solution of 0.01～0.02mol/L;
(2) getting a certain amount of silicon-dioxide powdery is dissolved in deionized water, add dispersant by its ultrasonic being uniformly dispersed, make the slurry that concentration is 0.01～0.20mol/L, then it is stirred with machine,massing, add a small amount of acid solution to regulate pH in 6～9 scopes;
(3) solution of being prepared by step (1) joins in the silicon dioxide slurry under abundant stirring with the speed of 0.02～0.10mol/s, then continues strong stirring 40～80min, obtains the precipitation of silica thing after being coated;
(4) sediment centrifugation step (3) being obtained, with deionized water washing 3～5 times, then spends absolute ethanol washing 1～2 time, finally puts into 80～100 DEG C of baking ovens and dries, and obtains clad type iron hydroxide/silicon dioxide composite powder;
(5), under inert gas shielding, can obtain tri-iron tetroxide/silicon dioxide composite powder through the calcinings of 500～800 DEG C.
Another technical problem that will solve of the present invention can also be come further to realize by the following technical programs, described silicon-dioxide powdery requires dioxide-containing silica in powder should be greater than 98%, powder granularity is at 1～20 μ m, and wherein granularity accounts for more than 90% below 10 μ m.
Another technical problem that will solve of the present invention can also be come further to realize by the following technical programs, and in described step (1), described molysite is to be selected from least one of compound in iron chloride, ferric sulfate and ferric nitrate.
Another technical problem that will solve of the present invention can also be come further to realize by the following technical programs, and in described step (2), described dispersant is sodium polymethacrylate.
Another technical problem that will solve of the present invention can also be come further to realize by the following technical programs, and in described step (5), described inert gas is argon gas or nitrogen.
The preparation method of the tri-iron tetroxide/silicon dioxide composite powder of a kind of shell-core structure that the present invention proposes, to realize taking cheap molysite as covering at silicon dioxide powder surface coated ferriferrous oxide, tri-iron tetroxide/the silicon dioxide of the shell-core structure making after modification can be eliminated the hydroxyl of silica surface effectively, improve its dispersibility, can improve the added value of silicon dioxide, expand the application of product.
Embodiment
Below further describe concrete technical scheme of the present invention, so that those skilled in the art further understands the present invention.
Embodiment 1:
(1) molysite is dissolved in deionized water, makes Fe by magnetic stirrer until molysite dissolves completely
3+concentration is the solution of 0.01mol/L;
(2) get silicon-dioxide powdery and be dissolved in deionized water, add dispersant by its ultrasonic being uniformly dispersed, make the slurry that concentration is 0.01mol/L, then it is stirred with machine,massing, add a small amount of ammoniacal liquor to regulate pH in 7 scopes;
(3) solution of being prepared by step (1) joins in the silicon dioxide slurry under abundant stirring with the speed of 0.02mol/s, then continues strong stirring 40min, obtains the precipitation of silica thing after being coated;
(4) sediment centrifugation step (3) being obtained, with deionized water washing 3 times, then spends absolute ethanol washing 1 time, finally puts into 80 DEG C of baking ovens and dries, and obtains clad type iron hydroxide/silicon dioxide composite powder;
(5) under the protection of inert gas argon gas, can obtain tri-iron tetroxide/silicon dioxide composite powder through the calcinings of 500 DEG C.
Embodiment 2:
(1) molysite is dissolved in deionized water, makes Fe by magnetic stirrer until molysite dissolves completely
3+concentration is the solution of 0.015mol/L;
(2) get silicon-dioxide powdery and be dissolved in deionized water, add dispersant by its ultrasonic being uniformly dispersed, make the slurry that concentration is 0.20mol/L, then it is stirred with machine,massing, add a small amount of ammoniacal liquor to regulate pH in 7 scopes;
(3) solution of being prepared by step (1) joins in the silicon dioxide slurry under abundant stirring with the speed of 0.016mol/s, then continues strong stirring 50min, obtains the precipitation of silica thing after being coated;
(4) sediment centrifugation step (3) being obtained, with deionized water washing 4 times, then spends absolute ethanol washing 2 times, finally puts into 90 DEG C of baking ovens and dries, and obtains clad type iron hydroxide/silicon dioxide composite powder;
(5) under inert nitrogen gas protection, can obtain tri-iron tetroxide/silicon dioxide composite powder through the calcinings of 600 DEG C.
Embodiment 3:
(1) molysite is dissolved in deionized water, makes Fe by magnetic stirrer until molysite dissolves completely
3+concentration is the solution of 0.02mol/L;
(2) get silicon-dioxide powdery and be dissolved in deionized water, add dispersant by its ultrasonic being uniformly dispersed, make the slurry that concentration is 0.20mol/L, then it is stirred with machine,massing, add a small amount of ammoniacal liquor to regulate pH in 8 scopes;
(3) solution of being prepared by step (1) joins in the silicon dioxide slurry under abundant stirring with the speed of 0.10mol/s, then continues strong stirring 80min, obtains the precipitation of silica thing after being coated;
(4) sediment centrifugation step (3) being obtained, with deionized water washing 5 times, then spends absolute ethanol washing 2 times, finally puts into 100 DEG C of baking ovens and dries, and obtains clad type iron hydroxide/silicon dioxide composite powder;
(5) under the protection of inert gas argon gas, can obtain tri-iron tetroxide/silicon dioxide composite powder through the calcinings of 700 DEG C.
Embodiment 4:
(1) molysite is dissolved in deionized water, makes Fe by magnetic stirrer until molysite dissolves completely
3+concentration is the solution of 0.018mol/L;
(2) get a certain amount of silicon-dioxide powdery and be dissolved in deionized water, add dispersant by its ultrasonic being uniformly dispersed, make the slurry that concentration is 0.014mol/L, then it is stirred with machine,massing, add a small amount of ammoniacal liquor to regulate pH in 9 scopes;
(3) solution of being prepared by step (1) joins in the silicon dioxide slurry under abundant stirring with the speed of 0.016mol/s, then continues strong stirring 70min, obtains the precipitation of silica thing after being coated;
(4) sediment centrifugation step (3) being obtained, with deionized water washing 4 times, then spends absolute ethanol washing 1 time, finally puts into 95 DEG C of baking ovens and dries, and obtains clad type iron hydroxide/silicon dioxide composite powder;
(5) under inert nitrogen gas protection, can obtain tri-iron tetroxide/silicon dioxide composite powder through the calcinings of 800 DEG C.
Although embodiment of the present invention are open as above, but it is not restricted to listed utilization in specification and execution mode, it can be applied to various applicable the field of the invention completely, for those skilled in the art, can easily realize other amendment, therefore do not deviating under the universal that claim and equivalency range limit, the present invention is not limited to specific details and illustrates here and the example of describing.
Claims (6)
1. the preparation method of the tri-iron tetroxide/silicon dioxide composite powder of a shell-core structure, it is characterized in that, taking silicon-dioxide powdery as bag core matrix, molysite is coating agent, adopt the precipitation method to prepare presoma iron hydroxide/silicon dioxide, then obtain tri-iron tetroxide/silicon dioxide composite powder through calcining.
2. a preparation method for the tri-iron tetroxide/silicon dioxide composite powder of shell-core structure, is characterized in that, its step is as follows:
(1) a certain amount of molysite is dissolved in deionized water, makes Fe by magnetic stirrer until molysite dissolves completely
3+concentration is the solution of 0.01～0.02mol/L;
(2) get silicon-dioxide powdery and be dissolved in deionized water, add dispersant by its ultrasonic being uniformly dispersed, make the slurry that concentration is 0.01～0.20mol/L, then it is stirred with machine,massing, add a small amount of ammoniacal liquor to regulate pH in 7～9 scopes;
(3) solution of being prepared by step (1) joins in the silicon dioxide slurry under abundant stirring with the speed of 0.02～0.10mol/s, then continues strong stirring 40～80min, obtains the precipitation of silica thing after being coated;
(4) sediment centrifugation step (3) being obtained, with deionized water washing 3～5 times, then spends absolute ethanol washing 1～2 time, finally puts into 80～100 DEG C of baking ovens and dries, and obtains clad type iron hydroxide/silicon dioxide composite powder;
(5), under inert gas shielding, can obtain tri-iron tetroxide/silicon dioxide composite powder through the calcinings of 500～800 DEG C.
3. the preparation method of the tri-iron tetroxide/silicon dioxide composite powder of a kind of shell-core structure as claimed in claim 1, it is characterized in that, described silicon-dioxide powdery requires dioxide-containing silica in powder should be greater than 98%, powder granularity is at 1～20 μ m, and wherein granularity accounts for more than 90% below 10 μ m.
4. the preparation method of the tri-iron tetroxide/silicon dioxide composite powder of a kind of shell-core structure as claimed in claim 2, it is characterized in that, in step (1), described molysite is to be selected from least one of compound in iron chloride, ferric sulfate and ferric nitrate.
5. the preparation method of the tri-iron tetroxide/silicon dioxide composite powder of a kind of shell-core structure as claimed in claim 2, is characterized in that, in step (2), described dispersant is sodium polymethacrylate.
6. the preparation method of the tri-iron tetroxide/silicon dioxide composite powder of a kind of shell-core structure as claimed in claim 2, is characterized in that, in step (5), described inert gas is argon gas or nitrogen.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111233046A (en) * | 2020-03-05 | 2020-06-05 | 江苏信息职业技术学院 | Hollow magnetic Fe for magnetorheological fluid3O4Nano-doped microsphere and preparation method thereof |
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| CN1380133A (en) * | 2002-03-13 | 2002-11-20 | 华东理工大学 | Silicone dioxide magnetic microsphere and its preparation method |
| CN1506407A (en) * | 2002-12-06 | 2004-06-23 | 中国科学院理化技术研究所 | Nano silicon dioxide/ferroferric oxide composite particle material and preparation method thereof |
| US20060051304A1 (en) * | 2004-09-02 | 2006-03-09 | Qinyun Peng | Special effects with mixtures of interference pigments |
| CN102732068A (en) * | 2012-04-11 | 2012-10-17 | 江苏大学 | Method for carrying out SiO2/Fe2O3 composite cladding on surface of aluminum powder |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1380133A (en) * | 2002-03-13 | 2002-11-20 | 华东理工大学 | Silicone dioxide magnetic microsphere and its preparation method |
| CN1506407A (en) * | 2002-12-06 | 2004-06-23 | 中国科学院理化技术研究所 | Nano silicon dioxide/ferroferric oxide composite particle material and preparation method thereof |
| US20060051304A1 (en) * | 2004-09-02 | 2006-03-09 | Qinyun Peng | Special effects with mixtures of interference pigments |
| CN102732068A (en) * | 2012-04-11 | 2012-10-17 | 江苏大学 | Method for carrying out SiO2/Fe2O3 composite cladding on surface of aluminum powder |
Non-Patent Citations (2)
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| 李群主: "《纳米材料的制备与应用技术》", 30 September 2008, 化学工业出版社 * |
| 雷红: "氧化硅/氧化铁复合磨粒用于硬盘基片的抛光研究", 《摩擦学学报》, vol. 30, no. 3, 31 May 2010 (2010-05-31) * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111233046A (en) * | 2020-03-05 | 2020-06-05 | 江苏信息职业技术学院 | Hollow magnetic Fe for magnetorheological fluid3O4Nano-doped microsphere and preparation method thereof |
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Address after: 221412 Xinyi City, Xuzhou Province town of Lake Town Industrial Park, No. 18, No. Patentee after: Jiangsu Kaida quartz Limited by Share Ltd Address before: The new city of Xinyi road 221400 Jiangsu city of Xuzhou province No. 10 Patentee before: Jiangsu Kaida Silica Co., Ltd. |