CN101143314A - Method for preparing titanium oxide cloth with fabric structure - Google Patents
Method for preparing titanium oxide cloth with fabric structure Download PDFInfo
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- CN101143314A CN101143314A CNA2007100446493A CN200710044649A CN101143314A CN 101143314 A CN101143314 A CN 101143314A CN A2007100446493 A CNA2007100446493 A CN A2007100446493A CN 200710044649 A CN200710044649 A CN 200710044649A CN 101143314 A CN101143314 A CN 101143314A
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Abstract
The invention relates to a fabric structured titania cloth preparation method. The procedures include: 1. the fiber reinforced polymer is swelled with the fiber reinforced polymer used as the template; 2. the fiber reinforced polymer is impregnated in titanium mixed salt solution to remove the remaining titanium salt adhered in the fiber reinforced polymer; 3.the fiber reinforced polymer is sintered to produce titania cloth of fabric structure similar to fiber reinforced polymer. In the sintering process, the titania salt is transformed into titania, and the fiber is oxidized and removed by various gases. The method has the characteristics of simple process, low cost, easy recycling and easy commercialization and can be widely used for degradation of organic compounds in air and water, sterilization and deodorization, etc.
Description
Technical field
The invention belongs to the preparation method field of titanium oxide cloth, particularly relate to preparation method with fabric construction titanium oxide cloth.
Background technology
A kind of important inorganic functional material of titanium oxide is widely used in modern industry, agricultural, national defence and scientific and technical numerous areas.Found that titania surface can continue organic matter in the decomposition water by photocatalysis in 1972 first, its as catalysis material in water treatment, purify air, aspects such as sterilization, deodorizing have obtained using widely.
The lot of documents report is thought: the photocatalytic activity of anatase-type titanium oxide is higher than the photocatalytic activity of Titanium Dioxide Rutile Top grade.Because nano-titanium oxide is compared with common titanium oxide, have bigger specific area, so photocatalysis efficiency is higher.At present the main method of preparation nano-anatase titanium oxide has sol-gal process, vapour deposition process, hydrothermal synthesis method etc., and the form of titanium oxide is also basically with film, fiber, powder or be deposited on other material surfaces.Each defectiveness of these methods, or complex process, the cost height, otherwise recycling is relatively more difficult.
In addition, United States Patent (USP) (the patent No.: 3663182, the metal oxide process for making such fabric) introduced with immersion process for preparing metal oxide fabric, wherein titanium oxide cloth is to use the water solution system of TiCl4 to prepare, but the water solution system of TiCl4 is very unstable, is difficult to form stable Ti solion; And the Ti ion concentration is very low in the solution, and the titanium oxide cloth intensity of preparation is just very low, does not have using value; Moreover the photocatalytic activity of the titanium oxide cloth that this patent prepares is not high.
Summary of the invention
The purpose of this invention is to provide a kind of preparation method with titanium oxide cloth of fabric construction, defectives such as the photocatalytic activity that this method solved prior art solion system instability, complex process, cost height, reclaim difficulty and prepared titanium oxide cloth is not high, intensity is low, the titanium dioxide fiber cloth of preparing has certain mechanical strength, the good light catalytic capability is arranged.
Preparation method with titanium oxide cloth of fabric construction of the present invention comprises step:
With fiber cloth as template, after this fiber cloth carried out swelling treatment, be immersed in the titanium complex salt solution, removal is attached on interfibrous residue titanium salt, obtain having titanium oxide cloth with fiber cloth identical fabric structure through sintering, in sintering process, titanium salt changes into titanium oxide, and the fiber decomposing oxidation is that all gases is removed.
Described fiber cloth is a kind of with in viscose rayon, Lycell fiber, bacteria cellulose fibre, bamboo fibre, the cotton fiber, the filament number of fiber is that the fibrage of 0.3-1 danier forms, weaving method be through compile or weft knitting in a kind of, institutional framework is a kind of in plain weave, twill-weave, satin weave, the two-sided plain weave;
Described swelling solution is meant a kind of in deionized water, NaOH solution or the urea liquid, and wherein the NaOH solution concentration is 0.1mol/L～1.5mol/L, and urea concentration is 0.5mol/L～2mol/L;
Described swelling is meant 0 ℃～100 ℃ swellings 1～10 hour;
Described titanium complex salt solution is the titanium ion solution that contains the doping ion, titanium ion solution be the benzene of the aqueous solution of metatitanic acid or titanium sulfate or butyl titanate or toluene solution the benzene or the toluene solution of tetrabutyl titanium; The doping ion be water-soluble or be dissolved in benzene or the zirconates of toluene yttrium salt aluminium salt trivalent iron salt zinc salt silicon salt Cd salt Cu salt Ni salt Ce salt Co salt Cr salt Os salt Rh salt V salt Ru salt Mo salt Hg salt in the Li salt one or several; Titanium ion concentration can be 0.1mol/L-3mol/L, and the doping ion concentration can be 0.1mol/L-2mol/L;
Described dipping is meant 0～100 ℃, floods 12～150 hours;
Described removing residue titanium salt is meant that distilled water cleans the back with centrifuge centrifuge dripping or filter paper adsorption method, removes the unnecessary salt that sticks to the looped fabric surface;
Described distilled water cleans and is meant till the distilled water pH value after the cleaning is 6～7.5;
Described sintering is meant puts into atmosphere furnace with dipping back fiber cloth, under oxidizing atmosphere, rises to certain temperature of 400～900 ℃ with 5～15 ℃/hour heating rates, be incubated after 3～10 hours, naturally cooling obtains the titanium oxide looped fabric, and its surface density is 100～200g/m
2, thickness is 0.1～0.6 micron;
Described oxidizing atmosphere is meant that oxidizing gas in the atmosphere furnace can be one or both in air or the steam.
Beneficial effect of the present invention:
(1) it is simple, with low cost to have technology, reclaims convenient, easy characteristics such as commercialization;
(2) can be widely used in organic degraded and deodorization and sterilization etc. in air, the water.
Description of drawings
Fig. 1 is the photo with titanium oxide cloth of fabric construction;
Fig. 2 is the stereoscan photograph of titanium dioxide fiber.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Select for use the viscose filament yarn fiber of 0.3d to be made into the plain weave looped fabric by weft knitting, this cloth thread density is: 16 pieces/inch of warps, parallel are 15 pieces/inch.With this looped fabric 50 ℃ of dryings 2 hours, pre-swelling is after 10 hours in water, then under 40 ℃ of conditions at the titanium complex salt aqueous solution (titanium sulfate aqueous solution, titanium ion concentration 3.0mol/L, zirconium ion concentration 0.5mol/L, ruthenium ion concentration 1.0mol/L, aluminium ion concentration 0.5mol/L) the middle dipping 24 hours.Solution centrifugal excessive in the looped fabric is removed drying.And dipping back fiber still can keep the bright and clean and pliability of original fiber.To contain zirconic viscose glue looped fabric speed with 50 ℃/hour in air and be warming up to 400 ℃, and then keep 2 hours at 400 ℃, impregnated cloth is oxidized to titanium dioxide fiber.All carbon to be from fiber, removed, fiber further 450 ℃ must be warmed up in 2 hours in air.In heating process, apply the tension force of 10 grams to fiber, guarantee that fiber is straight behind the sintering.The titanium dioxide fiber cloth that makes has compliance and intensity preferably, shows that by X-ray diffraction titanium oxide is mainly Detitanium-ore-type.
Embodiment 2
Select for use the 0.6dLycell fiber by through being woven into the twill-weave looped fabric, this cloth thread density is: 18 pieces/inch of warps, parallel are 18 pieces/inch.Pre-swelling was flooded 8 hours in the titanium complex salt aqueous solution (titanium sulfate aqueous solution, titanium ion concentration 2.0mol/L, Cd ion concentration 0.05mol/L, Ru ion concentration 0.05mol/L) under 60 ℃ of conditions after 10 hours then in water.By the method impregnation sintering in the example 1, the titanium dioxide fiber cloth surface density that obtains is 123g/m
2, have good compliance and intensity.
Embodiment 3
Select for use the bacteria cellulose fibre of 1d to be made into the satin weave looped fabric by weft knitting, this cloth thread density is: 16 pieces/inch of warps, parallel are 15 pieces/inch.With this looped fabric 50 ℃ of dryings 2 hours, pre-swelling is after 5 hours in 10 ℃, the urea liquid of 1.5mol/L, then under 10 ℃ of conditions at the titanium complex salt organic solution (benzole soln of butyl titanate, titanium ion concentration 1.0mol/L, Os ion concentration 0.03mol/L, Rh ion concentration 0.03mol/L, zinc ion concentration 0.04mol/L) the middle dipping 72 hours.Viscose glue looped fabric speed with 50 ℃/hour in air that then will contain the titanium complex salt is warming up to 400 ℃, keeps 2 hours at 400 ℃, then fiber further is warmed up to 500 ℃ in 2 hours in air, and the titanium oxide cloth that obtains is more crisp, and intensity is low.
Embodiment 4
Select for use the cotton fiber of 1d to be made into two-sided plain weave looped fabric by weft knitting, this cloth thread density is: 16 pieces/inch of warps, parallel are 15 pieces/inch.With this looped fabric 50 ℃ of dryings 2 hours, pre-swelling is after 5 hours in 80 ℃, the NaOH solution of 0.1mol/L, then under 90 ℃ of conditions the titanium complex salt aqueous solution (the metatitanic acid aqueous solution, titanium ion concentration 0.1mol/L, trivalent Ce ion concentration 0.1mol/L, ferric ion concentration 0.1mol/L, the Si ion concentration is 0.2mol/L) the middle dipping 72 hours.Looped fabric speed with 50 ℃/hour in air that then will contain the titanium complex salt is warming up to 400 ℃, keeps 2 hours at 400 ℃, then fiber further is warmed up to 800 ℃ in 2 hours in air, and the titanium oxide cloth Ti content that obtains is not high.
Embodiment 5
Select for use the bamboo fibre of 0.8d to be made into the plain stitch looped fabric by weft knitting, this cloth thread density is: 16 pieces/inch of warps, parallel are 15 pieces/inch.With this looped fabric 50 ℃ of dryings 2 hours, pre-swelling is after 5 hours in 10 ℃, the NaOH solution of 1.5mol/L, then under 10 ℃ of conditions at the titanium complex salt aqueous solution (titanium sulfate aqueous solution, titanium ion concentration 2.0mol/L, Cu ion concentration 0.1mol/L, Ni ion concentration 0.1mol/L, the Cr ion concentration is 0.2mol/L) the middle dipping 72 hours.The looped fabric that then will contain titanium complex salt speed of 200 ℃/hour in nitrogen atmosphere is warming up to 900 ℃, and insulation 10 hours in air atmosphere then obtains the titanium oxide looped fabric.
Embodiment 6
Select for use the bamboo fibre of 0.8d to be made into the plain stitch looped fabric by weft knitting, this cloth thread density is: 16 pieces/inch of warps, parallel are 15 pieces/inch.With this looped fabric 50 ℃ of dryings 2 hours, pre-swelling is after 5 hours in 10 ℃, the NaOH solution of 1.5mol/L, then under 10 ℃ of conditions at the titanium complex salt aqueous solution (titanium sulfate aqueous solution, titanium ion concentration 2.0mol/L, concentration of silver ions 0.3mol/L, Co ion concentration 0.2mol/L, the V ion concentration is 0.3mol/L) the middle dipping 72 hours.The looped fabric that then will contain titanium complex salt speed of 200 ℃/hour in nitrogen atmosphere is warming up to 900 ℃, and insulation 10 hours in air atmosphere then obtains the titanium oxide looped fabric.
Embodiment 7
Select for use the viscose filament yarn fiber of 0.5d to be made into the plain weave looped fabric by weft knitting, this cloth thread density is: 16 pieces/inch of warps, parallel are 15 pieces/inch.This looped fabric pre-swelling in water was flooded 10 hours in titanium sulfate aqueous solution (titanium ion concentration 3.0mol/L, Mo ion concentration 0.1mol/L, Hg ion concentration 0.1mol, Li ion concentration 0.2mol/L) under 50 ℃ of conditions after 10 hours then.Solution centrifugal excessive in the looped fabric is removed drying.And dipping back fiber still can keep the bright and clean and pliability of original fiber.To contain zirconic viscose glue looped fabric speed with 50 ℃/hour in air and be warming up to 400 ℃, and then keep 3 hours at 400 ℃, fiber further was warmed up to 650 ℃ in 2 hours in air, be incubated 10 hours, obtained the titanium oxide fabric.
Claims (10)
1. the preparation method who has the titanium oxide cloth of fabric construction, it is characterized in that: with fiber cloth as template, after this fiber cloth carried out swelling treatment, be immersed in the titanium complex salt solution, removal is attached on interfibrous residue titanium salt, obtains having titanium oxide cloth with fiber cloth identical fabric structure through sintering, in sintering process, titanium salt changes into titanium oxide, and the fiber decomposing oxidation is that all gases is removed.
2. the preparation method with titanium oxide cloth of fabric construction according to claim 1, it is characterized in that: described fiber cloth is a kind of with in viscose rayon, Lycell fiber, bacteria cellulose fibre, bamboo fibre, the cotton fiber, the filament number of fiber is that the fibrage of 0.3-1 danier forms, weaving method be through compile or weft knitting in a kind of, institutional framework is a kind of in plain weave, twill-weave, satin weave, the two-sided plain weave.
3. the preparation method with titanium oxide cloth of fabric construction according to claim 1, it is characterized in that: described swelling solution is meant a kind of in deionized water, NaOH solution or the urea liquid, wherein the NaOH solution concentration is 0.1mol/L～1.5mol/L, and urea concentration is 0.5mol/L～2mol/L.
4. the preparation method with titanium oxide cloth of fabric construction according to claim 1 is characterized in that: described swelling is meant 0 ℃～100 ℃ swellings 1～10 hour.
5. the preparation method with titanium oxide cloth of fabric construction according to claim 1, it is characterized in that: described titanium complex salt solution is the titanium ion solution that contains the doping ion, titanium ion solution be the benzene of the aqueous solution of metatitanic acid or titanium sulfate or butyl titanate or toluene solution the benzene or the toluene solution of tetrabutyl titanium; The doping ion be water-soluble or be dissolved in benzene or the zirconates of toluene yttrium salt aluminium salt trivalent iron salt zinc salt silicon salt Cd salt Cu salt Ni salt Ce salt Co salt Cr salt Os salt Rh salt V salt Ru salt Mo salt Hg salt in the Li salt one or several; Titanium ion concentration is 0.1mol/L-3mol/L, and the doping ion concentration is 0.1mol/L-2mol/L.
6. the preparation method with titanium oxide cloth of fabric construction according to claim 1 is characterized in that: described dipping is meant 0～100 ℃, floods 12～150 hours.
7. the preparation method with titanium oxide cloth of fabric construction according to claim 1, it is characterized in that: described removing residue titanium salt is meant that distilled water cleans the back with centrifuge centrifuge dripping or filter paper adsorption method, removes the unnecessary salt that sticks to the looped fabric surface.
8. the preparation method with titanium oxide cloth of fabric construction according to claim 7 is characterized in that: described distilled water cleans and is meant till the distilled water pH value after the cleaning is 6～7.5.
9. the preparation method with titanium oxide cloth of fabric construction according to claim 1, it is characterized in that: described sintering is meant puts into atmosphere furnace with dipping back fiber cloth, under oxidizing atmosphere, rise to certain temperature of 400～900 ℃ with 5～15 ℃/hour heating rates, be incubated after 3～10 hours, naturally cooling obtains the titanium oxide looped fabric, and its surface density is 100～200g/m
2, thickness is 0.1～0.6 micron.
10. the preparation method with titanium oxide cloth of fabric construction according to claim 1 is characterized in that: described oxidizing atmosphere is meant that oxidizing gas in the atmosphere furnace can be one or both in air or the steam.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200710044649A CN101143314B (en) | 2007-08-07 | 2007-08-07 | Method for preparing titanium oxide cloth with fabric structure |
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| CN200710044649A CN101143314B (en) | 2007-08-07 | 2007-08-07 | Method for preparing titanium oxide cloth with fabric structure |
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| CN101143314A true CN101143314A (en) | 2008-03-19 |
| CN101143314B CN101143314B (en) | 2010-05-19 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103721695A (en) * | 2012-10-12 | 2014-04-16 | 上海则轶实业有限公司 | Preparation method of titanium oxide active carbon |
| CN103908979A (en) * | 2014-04-10 | 2014-07-09 | 南京理工大学 | Supported nano TiO2 catalyst and preparation method thereof |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3860529A (en) * | 1968-01-24 | 1975-01-14 | Union Carbide Corp | Stabilized tetragonal zirconia fibers and textiles |
| US3663182A (en) * | 1968-03-29 | 1972-05-16 | Union Carbide Corp | Metal oxide fabrics |
| JPH10316444A (en) * | 1997-05-12 | 1998-12-02 | Minolta Co Ltd | Production method of metal oxide fiber, and metal oxide fiber produced by the method |
| JP4560778B2 (en) * | 2004-10-04 | 2010-10-13 | 日本エクスラン工業株式会社 | Functional fiber with photocatalytic activity |
| CN1772373A (en) * | 2005-10-31 | 2006-05-17 | 山东大学 | Prepn of photocatalytic titania fiber material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103721695A (en) * | 2012-10-12 | 2014-04-16 | 上海则轶实业有限公司 | Preparation method of titanium oxide active carbon |
| CN103908979A (en) * | 2014-04-10 | 2014-07-09 | 南京理工大学 | Supported nano TiO2 catalyst and preparation method thereof |
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| CN101143314B (en) | 2010-05-19 |
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