CN100423820C - Hollow inorganic oxide fibre, its synthesis and use - Google Patents
Hollow inorganic oxide fibre, its synthesis and use Download PDFInfo
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- CN100423820C CN100423820C CNB2006100194661A CN200610019466A CN100423820C CN 100423820 C CN100423820 C CN 100423820C CN B2006100194661 A CNB2006100194661 A CN B2006100194661A CN 200610019466 A CN200610019466 A CN 200610019466A CN 100423820 C CN100423820 C CN 100423820C
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Abstract
A hollow inorganic oxide fiber used for insulating material and microreactor is composed of a porous external inorganic oxide layer and a hollow kernel. Its preparing process includes such steps as providing hollow polymer or carbon fiber as template, adsorbing the inorganic oxide precursor, reaction, and high-temp calcining at 673-1173 deg. K in the condition of isolating air and O2.
Description
Technical field
The present invention relates to a kind of inorganic oxide doughnut and preparation method and use thereof, the inorganic oxide doughnut is a kind of new material.
Background technology
Doughnut is a kind of new structural material that newly-developed gets up, and is widely used in fields such as ultrafiltration, micro-filtration, separation, dialysis, is one of focus of research at present.At present the research of this respect is more concentrates on the polymer doughnut, as polysulfones, polyolefin, poly-cellulose esters, polyvinyl alcohol etc.The doughnut of other materials is still relatively more rare.
And relevant report is not seen in synthesizing of inorganic oxide doughnut as yet.
A kind of new synthetic technology---the template synthetic technology has caused researcher's extensive concern now.Many research groups adopt mould plate technique to synthesize the material of various novel structures, comprise poromerics, ordered mesoporous material, large pore material or the like, have realized the aperture of material, the regulation and control of pore structure.With the exception of this, the researcher has also realized the pattern regulation and control of material by mould plate technique, as nanotube, rod, ball, integral post material or the like.
The synthetic opportunity that provides of this class material of inorganic oxide doughnut is provided the new template synthetic method of this kind.
Summary of the invention
For promoting the development of prior art, the invention provides inorganic oxide doughnut material and preparation method and use thereof.This inorganic oxide doughnut has excellent mechanical property, corrosion-resistant, high temperature resistant, anti-oxidant, high adsorption capacity, and the surface is easy to modification, is easy to obtain diversified surface property, demonstrates good prospects for application at aspects such as catalysis, absorption.
Technical scheme provided by the invention is: this inorganic oxide doughnut is made up of outer inorganic oxide shell and hollow core at least; Outer inorganic oxide shell is a loose structure, and the hollow core of hole and inorganic oxide doughnut interconnects.And inorganic oxide doughnut outward appearance in a tubular form, and external diameter is 250 μ m-750 μ m, and internal diameter is 150 μ m-650 μ m, and the inorganic oxide thickness of the shell is 50 μ m-100 μ m.Wherein the inorganic oxide shell is silica, zirconium dioxide, titanium dioxide or zirconium-silicon, zirconium-titanium hydridization oxide; Hollow core is the hollow core of polymer doughnut material or the hollow core of charcoal doughnut material.
The present invention also provides the synthetic method of above-mentioned inorganic oxide doughnut: with polymer doughnut or charcoal doughnut is template, absorption inorganic oxide precursor body on polymer doughnut or charcoal doughnut, after the reaction, at 673K～1173K high temperature sintering, thereby obtain the inorganic oxide doughnut.Used inorganic oxide precursor body is silica, zirconium dioxide, titanium dioxide or zirconium-silicon, zirconium-titanium hydridization oxide.
The method that above-mentioned inorganic oxide precursor body is adsorbed on polymer doughnut surface can spray absorption or soak into absorption, and the absorption number of times can be 1-5 time.
Inorganic oxide doughnut of the present invention can be used as sorbing material, heat-insulation material, microreactor etc.
Inorganic oxide doughnut of the present invention is as a kind of new material, it has concentrated the advantage of doughnut and the characteristic of inorganic oxide material simultaneously, have excellent mechanical property, corrosion-resistant, high temperature resistant, anti-oxidant, high adsorption capacity, the surface is easy to modification, be easy to obtain diversified surface property, polymer doughnut material compared with traditional has using value widely.
Because it has loose structure, specific surface is bigger, and strong adsorption capacity is arranged, and therefore can be used as sorbing material, is used for the processing of waste water, pollutant etc.; And its loose structure, high-temperature stability also make it can be used as heat-insulation material; Again because of the inorganic oxide doughnut has the hollow core structure, so also can be used as the microreactor carrier.
The specific embodiment
Inorganic oxide doughnut of the present invention is made up of outer inorganic oxide shell and hollow core at least; Outer inorganic oxide shell is a loose structure, and the hollow core of hole and inorganic oxide doughnut interconnects.And inorganic oxide doughnut outward appearance in a tubular form, and external diameter is 250 μ m-750 μ m, and internal diameter is 150 μ m-650 μ m, and the inorganic oxide thickness of the shell is 50 μ m-100 μ m.Wherein the inorganic oxide shell is silica, zirconia, titanium dioxide or zirconium-silicon, zirconium-titanium hydridization oxide; Hollow core is the hollow core of polymer doughnut material or the hollow core of charcoal doughnut material.
Be the synthetic embodiment of inorganic oxide doughnut below.
Embodiment 1: 5mL ethyl orthosilicate, 7mL hydrochloric acid (pH=2.0), 1g polyacrylic acid (Mw=90000) are fully mixed, get polypropylene hollow fiber and put into above-mentioned mixed liquor, take out behind the immersion 2h, put into baking oven in 343K reaction 5h.Thereafter material is taken out and place crucible, 873K calcination 2h in Muffle furnace after cooling off naturally, promptly gets inorganic oxide doughnut material, the about 50 μ m of this inorganic oxide doughnut wall thickness, and its hollow core internal diameter is about 500 μ m.
Embodiment 2: at first 1g zirconium oxychloride, 12.5mL absolute ethyl alcohol, 7.5mL water are mixed, 343K insulation 2 hours, obtain zirconium colloidal sol.Hollow charcoal fiber is soaked in this zirconium colloidal sol, treat abundant wetting back taking-up, the 2K/min temperature programming is to 373K.This infiltration, dry run repeat 2 times, and are placed on Muffle furnace 1173K calcination 2h, obtain the zirconium dioxide doughnut.This doughnut wall thickness is about 100 μ m, and its internal diameter is about 250 μ m.
Embodiment 3: at first 1mL butyl titanate, 2.5mL absolute ethyl alcohol, 0.1mL hydrochloric acid (pH 2.0) are mixed, 343K insulation 2 hours, obtain zirconium colloidal sol.Hollow charcoal fiber is soaked in this zirconium colloidal sol, treat abundant wetting back taking-up, the 2K/min temperature programming is to 373K.This infiltration, dry run repeat 4 times, and are placed on Muffle furnace 1173K calcination 2h, obtain the titanium dioxide hollow fiber.This doughnut wall thickness is about 120 μ m, and its internal diameter is about 250 μ m.
Below be the embodiment of the purposes of inorganic oxide doughnut.
Embodiment 4: the inorganic oxide doughnut is used for the absorption of environmental contaminants
Polycyclic aromatic hydrocarbon is the more common environmental contaminants of a class.Get a water sample that contains polycyclic aromatic hydrocarbon, survey its UV absorption at 254nm, because the existence of polycyclic aromatic hydrocarbon, water sample has tangible UV absorption.To by the synthetic inorganic oxide doughnut material of embodiment 1 behind surface modification bonding C18, be filled in the filter post, allow water sample pass through this filter post, again water sample is carried out UV absorption and detect.The water sample of discovery after the surface bond doughnut is handled do not have obvious UV absorption, shows that this doughnut has stronger adsorption capacity to polycyclic aromatic hydrocarbon, is suitable for the removal of environmental contaminants.
Claims (7)
1. inorganic oxide doughnut, it is characterized in that: it is made up of outer inorganic oxide shell and hollow core at least; Outer inorganic oxide shell is a loose structure, and hole and hollow core interconnect, and the inorganic oxide shell is silica, zirconium dioxide, titanium dioxide or zirconium-silicon, zirconium-titanium hydridization oxide.
2. according to the described inorganic oxide doughnut of claim 1, it is characterized in that: inorganic oxide doughnut outward appearance in a tubular form, external diameter is 250 μ m-750 μ m, internal diameter is 150 μ m-650 μ m, the inorganic oxide thickness of the shell is 50 μ m-100 μ m.
3. according to claim 1 or 2 described inorganic oxide doughnuts, it is characterized in that: hollow core is the hollow core of polymer doughnut material or the hollow core of charcoal doughnut material.
4. the synthetic method of the described inorganic oxide doughnut of claim 1, it is characterized in that: with polymer doughnut or charcoal doughnut is template, absorption inorganic oxide precursor body on polymer doughnut or charcoal doughnut, after the reaction, at 673K～1173K high temperature sintering, thereby obtain the inorganic oxide doughnut.
5. according to the synthetic method of the described inorganic oxide doughnut of claim 4, it is characterized in that: used inorganic oxide precursor body is silica, zirconium dioxide, titanium dioxide or zirconium-silicon, zirconium-titanium hydridization oxide.
6. according to the synthetic method of the described inorganic oxide doughnut of claim 4, it is characterized in that: the mode of absorption inorganic oxide precursor body is for spraying absorption or soak into absorption, and the absorption number of times is 1-5 time.
7. the described inorganic oxide doughnut of claim 1 is as the application of sorbing material, heat-insulation material, microreactor.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100194661A CN100423820C (en) | 2006-06-23 | 2006-06-23 | Hollow inorganic oxide fibre, its synthesis and use |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100194661A CN100423820C (en) | 2006-06-23 | 2006-06-23 | Hollow inorganic oxide fibre, its synthesis and use |
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| CN1895758A CN1895758A (en) | 2007-01-17 |
| CN100423820C true CN100423820C (en) | 2008-10-08 |
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| CNB2006100194661A Expired - Fee Related CN100423820C (en) | 2006-06-23 | 2006-06-23 | Hollow inorganic oxide fibre, its synthesis and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103820882B (en) * | 2014-03-07 | 2015-12-30 | 武汉大学 | Hollow inorganic oxide fibre and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6503295B1 (en) * | 2000-09-20 | 2003-01-07 | Chevron U.S.A. Inc. | Gas separations using mixed matrix membranes |
| CN1587032A (en) * | 2004-09-14 | 2005-03-02 | 武汉大学 | Hollow charcoal and its synthetic method and use |
| CN1669629A (en) * | 2004-12-29 | 2005-09-21 | 浙江大学 | Process for preparing organic-inorganic hybrid nano microcapsule using polymer as core |
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2006
- 2006-06-23 CN CNB2006100194661A patent/CN100423820C/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6503295B1 (en) * | 2000-09-20 | 2003-01-07 | Chevron U.S.A. Inc. | Gas separations using mixed matrix membranes |
| CN1587032A (en) * | 2004-09-14 | 2005-03-02 | 武汉大学 | Hollow charcoal and its synthetic method and use |
| CN1669629A (en) * | 2004-12-29 | 2005-09-21 | 浙江大学 | Process for preparing organic-inorganic hybrid nano microcapsule using polymer as core |
Non-Patent Citations (2)
| Title |
|---|
| 聚合物/无机纳米粒子自组装复合膜的制备与应用. 李琰等.化学研究，第14卷第1期. 2003 |
| 聚合物/无机纳米粒子自组装复合膜的制备与应用. 李琰等.化学研究，第14卷第1期. 2003 * |
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| CN1895758A (en) | 2007-01-17 |
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