CN102605552A - Method for preparing nitrogen-doped nanometer TiO2 fiber cloth - Google Patents
Method for preparing nitrogen-doped nanometer TiO2 fiber cloth Download PDFInfo
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- CN102605552A CN102605552A CN2012100369182A CN201210036918A CN102605552A CN 102605552 A CN102605552 A CN 102605552A CN 2012100369182 A CN2012100369182 A CN 2012100369182A CN 201210036918 A CN201210036918 A CN 201210036918A CN 102605552 A CN102605552 A CN 102605552A
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- adhesive
- nitrogen
- doped nanometer
- fiber
- fibre web
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Abstract
The invention provides a method for preparing nitrogen-doped nanometer TiO2 fiber cloth. Nitrogen-doped nanometer TiO2 fiber precursor is used as a raw material. The method includes the particular steps: (1) web laying; (2) impregnation; (3) pressing; and (4) solidification and calcination forming. The collected nitrogen-doped nanometer TiO2 fiber precursor is sequentially loosened and carded, impurities in the shape of a bamboo joint in fibers are removed, the fibers are carded to form monofilament fiber webs, and the monofilament fiber webs are uniformly laid to form a layered net structure in a staggered manner; the laid fiber webs pass through an impregnation tank to sufficiently contact with adhesive; and the impregnated fiber webs are rolled at constant speed by rolls, redundant adhesive on the surfaces of the fiber webs are removed, and the fibers are bonded more tightly. The method has the advantages that technology of a preparation process is simple, the automation degree is high, and the method is applicable to industrial batch production; the prepared fiber cloth does not need a carrier, and has a self-supporting characteristic; and the fibers are longitudinally and transversely staggered and bonded tightly, the quantity of pores is high, and the specific surface area is large.
Description
Technical field
The present invention relates to a kind of nitrogen-doped nanometer TiO as photochemical catalyst
2The preparation method of cloth belongs to nano-TiO
2The functional fibre material preparing technical field.
Background technology
Semiconductor light-catalyst is nitrogen-doped nanometer TiO especially
2Photochemical catalyst owing to can directly utilize visible light with the pollutant mineralising, because nanoscale shows tangible skin effect and quantum size effect, has become the research focus that application field of water treatment is new in recent years simultaneously.Present TiO
2Photochemical catalyst mainly is prepared into three kinds of forms: nano-TiO
2Powder, supported titanium
2With film TiO
2Yet be applied to the suspended phase nano-TiO in the water treatment
2Powder have be prone to reunite, free settling not, and reclaim difficulty and cause shortcomings such as cost increase, be unfavorable for the regeneration of catalyst and utilization again.Supported titanium
2With film TiO
2Because specific area reduces, thereby has caused photocatalytic activity decline, has also limited practical application.
Nano-TiO
2The appearance of fiber has overcome above shortcoming, and not only easy recovery was utilized, but also can be given full play to its photocatalytic activity, thereby had bright development prospect.Present fibre spinning method is generally melt spinning process and solution spinning, and prepared fiber presoma is the fluffy structure of bulk that monofilament is interwoven, and can be divided into staple fibre and continuous fibers according to filament length.Its shortcoming is that bad mechanical strength, flow impact resistant load-bearing capacity are low, skewness during use, thus make it to bring into play photocatalysis usefulness efficiently and stably.
Summary of the invention
The purpose of this invention is to provide a kind of nitrogen-doped nanometer TiO
2The preparation method of cloth, bad mechanical strength, the flow impact resistant load-bearing capacity that exists with the nanofiber that overcomes present preparation be low, skewness when using, and can't bring into play the shortcoming of photocatalysis usefulness efficiently and stably.
Nitrogen-doped nanometer TiO of the present invention
2The preparation method of cloth adopts nitrogen-doped nanometer TiO
2The fiber presoma is a raw material, prepares cloth, the nitrogen-doped nanometer TiO of employing through lapping, impregnation, compacting, curing, roasting molding procedure
2The fiber presoma is finished fiber (generally combining the dry spinning technology to make through the modification sol-gel method), specifically may further comprise the steps:
(1) lapping: with the nitrogen-doped nanometer TiO that collects
2The fiber presoma carries out shredding and combing successively, removes the ring shape impurity in the fiber, and fiber is carded to monofilament fibre web shape, and fibre web evenly is paved into a layer network structure alternately;
(2) impregnation: the fibre web of completing was flooded in adhesive 0.5 hour-5 hours; Fibre web is fully contacted with adhesive; Thereby make adhesive fully be impregnated into fibre web surface and inner, the fiber presoma is closely combined through hole diffusion and suction-operated;
Impregnation carries out at normal temperatures, and its mode can be normal pressure impregnation or decompression impregnation.
Adhesive can be selected type thermosetting resin (like unsaturated polyester resin, epoxy resin, phenolic resins etc.) and auxiliary material, and adhesive specifically can be:
1. unsaturated polyester resin and t-butyl perbenzoate are pressed 100: 8.2 mixture of mass ratio.
2. the phenol resin solution of absolute ethyl alcohol dilution, the volume ratio of absolute ethyl alcohol and phenolic resins is 1.5～2.5: 5.
3. epoxy resin, low molecule pa resin, polybutadiene epoxy, 2-ethyl-4-methylimidazole and 260 epoxy active diluents are 100: 10: 20 by mass ratio: 5: 12 mixture.
(3) compacting: the fibre web behind the impregnation through at the uniform velocity roll-in of running roller, is made combine between the fiber more closely knit when removing surperficial unnecessary adhesive;
(4) curing and roasting moulding: the fibre web after will suppressing imports in the tube furnace; Be warming up to the adhesive setting temperature earlier, keep this temperature to adhesive to solidify fully, also keep this atmosphere through steam then always; Make tube furnace be warming up to 700 ℃; And kept 2 hours, the adhesive that solidify this moment and contained other organic matter through the carbonization oxidation by abundant removal, TiO
2It is main being changed into anatase crystal by impalpable structure, makes furnace temperature naturally cool to room temperature and stops to feed steam, obtains the nitrogen-doped nanometer TiO of white
2Cloth.
The present invention compares with other preparation method and has the following advantages:
1. preparation process technology is simple, the curing of adhesive and remove and the transformation of a crystal formation step in tube furnace accomplishes, and automaticity is high, is fit to industrialized mass production.
2. the cloth of preparation does not need carrier, has the self-supporting characteristic.Crisscross between the fiber, combine closely, hole is abundant, specific area is bigger.
3. nitrogen-doped nanometer TiO
2The cloth crystal formation is main with anatase; Can be under the exciting of visible light degradation of contaminant; Has photocatalysis effect efficiently; And by force, there is not the losing issue of catalyst in the flow impact resistant load-bearing capacity, is very easy to recycling, in the actual improvement of water pollution control, has broad application prospects.
Description of drawings
Fig. 1 is nitrogen-doped nanometer TiO among the present invention
2The sketch map of fibre web impregnation and suppression process.
Fig. 2 is nitrogen-doped nanometer TiO among the present invention
2Cloth is solidified in tube furnace and the sketch map of roasting moulding.
Wherein: 1, conveyer belt, 2, nitrogen-doped nanometer TiO
2Fibre web, 3, rotating shaft, 4, the Kun axle, 5, steeping vat, 6, tube furnace, 7, water flowing steam tubule, 8, blast pipe.
The specific embodiment
Embodiment 1
Collect nitrogen-doped nanometer TiO
2The fiber presoma; Send into successively and carry out shredding, combing in opener, the carding machine; Remove the ring shape impurity in the fiber presoma, the fiber presoma is carded to monofilament fibre web shape, the fibre web that obtains is placed on the lapping equipment; Evenly be paved into five layers of fibre web shape structure alternately, form five layers of nitrogen-doped nanometer TiO
2Fibre web 2 (referring to Fig. 1).
As shown in Figure 1; The fibre web of completing 2 imported in the steeping vat 5 through conveyer belt 1 carry out impregnation; Conveyer belt 1 drives operation by rotating shaft 3, adhesive consist of unsaturated polyester resin and t-butyl perbenzoate, both mass ratioes are 100: 8.2; Normal pressure flooded 0.5 hour down, made adhesive fully be impregnated into fibre web inside.Fibre web 2 behind the impregnation is suppressed through a pair of roll shaft 4, removes the unnecessary adhesive in surface.As shown in Figure 2, the fibre web after the compacting is imported in the tube furnace 6, rise to 150 ℃ of adhesive setting temperatures with 100 ℃/hour speed, kept 1 hour at 150 ℃, adhesive is fully solidified.From tubule 7, in tube furnace 6, feed steam; Unnecessary steam is discharged to outside the stove from discharge pipe 8, simultaneously ℃ carries out roasting with 200 ℃/hour speed kindling temperature to 700, and insulation is 2 hours under this temperature; Make furnace temperature naturally cool to room temperature then; Stop the water flowing steam, derive cloth, obtain five layers of crisscross cancellated white nitrogen-doped nanometer TiO
2Cloth.
According to the method for embodiment 1, evenly be paved into ten layers of fibre web shape structure alternately, form ten layers of nitrogen-doped nanometer TiO
2Fibre web 2 (referring to Fig. 1).
The fibre web of completing imported in the steeping vat 5 through conveyer belt 1 carry out impregnation, the phenol resin solution that consists of the absolute ethyl alcohol dilution of adhesive, both volume ratios are 1.5～2.5: 5, normal pressure dipping 2 hours makes adhesive fully be impregnated into fibre web inside.Fibre web behind the impregnation is suppressed through a pair of roll shaft 4, removes the unnecessary adhesive in surface.Fibre web after the compacting is imported in the tube furnace 6 (referring to Fig. 2), rise to 140 ℃ of adhesive setting temperatures, kept 2 hours, adhesive is fully solidified at 140 ℃ with 150 ℃/hour speed.From tubule 7, feed steam; Unnecessary steam is discharged to outdoor from discharge pipe 8, simultaneously is warming up to 700 ℃ of roastings with 250 ℃/hour speed, and insulation is 2 hours under this temperature; Make furnace temperature naturally cool to room temperature then; Stop the water flowing steam, derive cloth, obtain ten layers of crisscross cancellated white nitrogen-doped nanometer TiO
2Cloth.
Embodiment 3
According to the method for embodiment 1, evenly be paved into 15 layers of fibre web shape structure alternately, form 15 layers of nitrogen-doped nanometer TiO
2Fibre web 2 (referring to Fig. 1).
The fibre web of completing imported in the steeping vat 5 through conveyer belt 1 carry out impregnation; Adhesive consist of epoxy resin, low molecule pa resin, polybutadiene epoxy, 2-ethyl-4-methylimidazole and 260 epoxy active diluents; The mass ratio of each component is 100: 10: 20: 5: 12; Normal pressure dipping 5 hours makes adhesive fully be impregnated into fibre web inside.Fibre web behind the impregnation is suppressed through a pair of roll shaft 4, removes the unnecessary adhesive in surface.Fibre web after the compacting is imported in the tube furnace 6 (referring to Fig. 2), rise to 100 ℃ of adhesive setting temperatures, kept 4 hours, adhesive is fully solidified at 100 ℃ with 80 ℃/hour speed.From tubule 7, feed steam; Unnecessary steam is discharged to outdoor from discharge pipe 8, simultaneously is warming up to 700 ℃ of roastings with 300 ℃/hour speed, and insulation is 2 hours under this temperature; Make furnace temperature naturally cool to room temperature then; Stop the water flowing steam, derive cloth, obtain 15 layers of crisscross cancellated white nitrogen-doped nanometer TiO
2Cloth.
Claims (4)
1. nitrogen-doped nanometer TiO
2The preparation method of cloth adopts nitrogen-doped nanometer TiO
2The fiber presoma is a raw material, it is characterized in that, may further comprise the steps:
(1) lapping: with the nitrogen-doped nanometer TiO that collects
2The fiber presoma carries out shredding and combing successively, removes the ring shape impurity in the fiber, and fiber is carded to monofilament fibre web shape, and fibre web evenly is paved into a layer network structure alternately;
(2) impregnation: the fibre web of completing was flooded in adhesive 0.5 hour-5 hours; Fibre web is fully contacted with adhesive; Thereby make adhesive fully be impregnated into fibre web surface and inner, the fiber presoma is closely combined through hole diffusion and suction-operated;
(3) compacting: the fibre web behind the impregnation through at the uniform velocity roll-in of running roller, is made combine between the fiber more closely knit when removing surperficial unnecessary adhesive;
(4) curing and roasting moulding: the fibre web after will suppressing imports in the tube furnace; Be warming up to the adhesive setting temperature earlier, keep this temperature to adhesive to solidify fully, also keep this atmosphere through steam then always; Make tube furnace be warming up to 700 ℃; And kept 2 hours, the adhesive that solidify this moment and contained other organic matter through the carbonization oxidation by abundant removal, TiO
2It is main being changed into anatase crystal by impalpable structure, makes furnace temperature naturally cool to room temperature and stops to feed steam, obtains the nitrogen-doped nanometer TiO of white
2Cloth.
2. nitrogen-doped nanometer TiO according to claim 1
2The preparation method of cloth is characterized in that, the adhesive in the said step (2) is that saturated polyester resin and t-butyl perbenzoate are by 100: 8.2 mixture of mass ratio.
3. nitrogen-doped nanometer TiO according to claim 1
2The preparation method of cloth is characterized in that, the adhesive in the said step (2) is the phenol resin solution of absolute ethyl alcohol dilution, and the volume ratio of absolute ethyl alcohol and phenolic resins is 1.5～2.5: 5.
4. nitrogen-doped nanometer TiO according to claim 1
2The preparation method of cloth; It is characterized in that the adhesive in the said step (2) is that epoxy resin, low molecule pa resin, polybutadiene epoxy, 2-ethyl-4-methylimidazole and 260 epoxy active diluents are 100: 10: 20 by mass ratio: 5: 12 mixture.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210036918.2A CN102605552B (en) | 2012-02-17 | 2012-02-17 | Method for preparing nitrogen-doped nanometer TiO2 fiber cloth |
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|---|---|---|---|
| CN201210036918.2A CN102605552B (en) | 2012-02-17 | 2012-02-17 | Method for preparing nitrogen-doped nanometer TiO2 fiber cloth |
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| CN102605552A true CN102605552A (en) | 2012-07-25 |
| CN102605552B CN102605552B (en) | 2014-04-02 |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109264487A (en) * | 2018-07-31 | 2019-01-25 | 湖北中嘉新材料有限公司 | A kind of ceramic nanofibers shell process units and production method |
| CN109289890A (en) * | 2018-09-28 | 2019-02-01 | 西北工业大学 | Efficient self-supporting titanium nitride/nitrogen-doped titanium dioxide light electro catalytic electrode material and preparation method |
| CN113089187A (en) * | 2021-02-21 | 2021-07-09 | 金大付 | Medical long fiber non-woven fabric preparation device and method |
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2012
- 2012-02-17 CN CN201210036918.2A patent/CN102605552B/en not_active Expired - Fee Related
Patent Citations (5)
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| JP2003292597A (en) * | 2002-03-29 | 2003-10-15 | Toray Ind Inc | Polyethylene terephthalate for nonwoven fabric |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109264487A (en) * | 2018-07-31 | 2019-01-25 | 湖北中嘉新材料有限公司 | A kind of ceramic nanofibers shell process units and production method |
| CN109289890A (en) * | 2018-09-28 | 2019-02-01 | 西北工业大学 | Efficient self-supporting titanium nitride/nitrogen-doped titanium dioxide light electro catalytic electrode material and preparation method |
| CN113089187A (en) * | 2021-02-21 | 2021-07-09 | 金大付 | Medical long fiber non-woven fabric preparation device and method |
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| CN102605552B (en) | 2014-04-02 |
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