CN100469438C - Continuous poriferous titanium dioxide fiber and the technique of preparing the same - Google Patents
Continuous poriferous titanium dioxide fiber and the technique of preparing the same Download PDFInfo
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- CN100469438C CN100469438C CN 200710034514 CN200710034514A CN100469438C CN 100469438 C CN100469438 C CN 100469438C CN 200710034514 CN200710034514 CN 200710034514 CN 200710034514 A CN200710034514 A CN 200710034514A CN 100469438 C CN100469438 C CN 100469438C
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- tio
- colloidal sol
- fiber
- titanium dioxide
- continuous poriferous
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Abstract
The invention relates to a continuous porous titanium dioxide fiber and the preparing technology. Sol-gel method is used to prepare the continuous porous titanium oxide fiber. First, TiO2 sol with low molecular weight is compounded; by evaporating organic solvent and adding polymer, TiO2 fiber precursor with high molecular weight is prepared. Then by extruding and extending the continuous porous TiO2 fiber is compounded. The outstanding characteristic of method is that by using sol-gel method the continuous porous TiO2 fiber with new structure and good physical and chemical property is prepared so as to provide a new path for studying continuous inorganic fiber material. At the same time, the technology is simple and it is easy to industrial production. It makes active contribution to developing theory, technology and method of sol-gel filature.
Description
Technical field
The present invention relates to continuous poriferous titanium dioxide fiber and preparation technology thereof, belong to field of functional materials.
Background technology
TiO
2Because of its biologically inert and chemical inertness, photoetch and chemical attack can not take place, advantage such as cheap, and a kind of photochemical catalyst that is proved to be to be most widely used.Because TiO
2Electron distributions be characterised in that the existence that band gap is arranged between its conduction band and the valence band.When being subjected to illumination, as long as the energy of photon equals or exceeds semi-conductive band-gap energy (hv 〉=E
g), just can make electronics transit to conduction band, thereby produce conduction band electron and valence band hole from valence band.Under the electric field action of space charge layer, the free electron of conduction band is moved to semiconductive particles surface rapidly and is transferred to oxidation component in the solution, thereby light induced electron and hole form hydroxyl radical free radical OH through series reaction, and it can the nearly all organic matter of oxidation.Therefore, it (is handled as waste water and gas) in the environmental protection field and has powerful application prospect.Course of reaction is as follows:
TiO
2+hv→h
++e
-
H
2O+h
+→·OH+H
+
e
-+O
2→O2
-·
H
++O
2 -·→HO
2·
2HO
2·→H
2O
2+O
2
H
2O
2+O2
-·→·OH+OH
-+O
2
h
++OH
-→·OH
h
++ org → intermediate → CO
2+ H
2O
OH+org → intermediate → CO
2+ H
2O
Yet for wastewater treatment TiO
2Nano-powder exists and is difficult to separate the problem of recovery, thereby causes operating cost higher, has limited the application of this technology in wastewater treatment.According to Nihon Keizai Shimbun and scientific research institution's prediction, by 2007, TiO in Japan
2Nano-powder is owing to inapplicable sewage disposal causes this technology up to 12,000,000,000 dollars of economic losses.In order to solve TiO
2The difficulty that the difficulty that powder exists in water treatment reclaims, the normal at present method that adopts is with TiO
2Be fixed in (zeolite, silica gel, active carbon etc.) on the appropriate carriers.Yet the defective of this method is its specific surface area of catalyst to be reduced greatly, and the TiO of load
2Come off from carrier easily, seriously reduced its photocatalysis efficiency and activity.Other method is preparation TiO
2Fiber, but the fiber of present domestic preparation is micron-sized, in wastewater treatment, still exists and TiO
2Powder equally is difficult to the defective of separating.
TiO
2Long fibre, owing to have certain intensity, and can weave, in sewage disposal, can not be damaged to powder, thereby suitable separation fast from sewage disposal solution, sewage degradation treatment cost saved.Therefore, TiO
2Making continuous poriferous fiber is to solve photocatalysis technology to be applied to sewage degradation treatment effective method the most.Utilize the weaving of continuous poriferous titanium dioxide fiber material, segregative characteristic, nanoporous characteristic and high-specific surface area characteristic, in conjunction with concerted catalysis effect, the heterogeneous interface effect of element doping, obtain to have the continuous poriferous photocatalytic fiber material of high activity and good serviceability.Simultaneously, this technology is simple, is easy to suitability for industrialized production.
Summary of the invention
Technical problem to be solved by this invention is: solve the problem that above-mentioned prior art exists, and provide that a kind of anti-microbial property is good, avirulence, specific area are big, can be as matrix material, intensity height, can weave, processing technology is good, preparation technology is simple, be easy to the continuous poriferous titanium dioxide fiber and the preparation technology thereof of suitability for industrialized production.
The technical solution used in the present invention is: be raw material with the butyl titanate, passing through colloidal sol---gel method is prepared low-molecular-weight TiO 2 sol body, adopt evaporation and add the TiO 2 sol body of polymer synthetic high polymer amount, then, by extruding stretching, pre-oxidation and heat treatment, synthetic continuous poriferous titanium dioxide fiber.
In the technique scheme, concrete preparation technology is:
1), be initiation material with the butyl titanate, be that solvent, diethanol amine are chelating agent with the absolute ethyl alcohol, under the interaction of distilled water and concentrated hydrochloric acid, synthesize low-molecular-weight TiO
2The colloidal sol body;
2), as low-molecular-weight TiO
2The temperature of colloidal sol body adds polyethylene glycol and polyethylene, and they is dissolved fully to 180-250 ℃;
3), after the dissolving of polyethylene glycol and polyethylene, insulation is removed organic solvent by evaporation, makes TiO
2The molecular weight of colloidal sol body increases;
4), the TiO of HMW
2The colloidal sol body is put into the spinning bucket, and insulation, by to the pressurization of spinning bucket, makes TiO
2The colloidal sol body is extruded through spinneret orifice;
5), spun TiO
2The colloidal sol silk is evaporated its organic solvent through the vacuum bakeout device, and fiber is dried simultaneously, and viscosity descends, and helps curling.
In the technique scheme, the agents useful for same percentage by weight is: butyl titanate, purity〉99.0,50-65%; Diethanol amine, purity〉99.9,1-5%; Absolute ethyl alcohol, purity〉99.9,25-35%; Polyethylene glycol, purity〉99.9,2-8%; Polyethylene, purity〉99.9,6-15%.
In the technique scheme, TiO
2The colloidal sol body maintains the temperature between 200-250 ℃ after adding the dissolving of polyethylene glycol and polyethylene, and evaporation time is 3-6 hour.
In the technique scheme, the temperature in the spinning bucket remains on 200-250 ℃.
In the technique scheme, the temperature of vacuum bakeout device remains between 300-400 ℃.
The present invention adopts colloidal sol---gel method, and by extruding stretching, pre-oxidation and heat treatment synthesizing inorganic continuous fiber, at present, we utilize this technology to prepare the TiO that length reaches 2m
2Fiber.TiO
2Long fibre has following remarkable advantage effect: (a) have high anti-microbial property, do not have any toxicity; (b) this specific fiber surface is long-pending big, and can be used as matrix material; (c) this fibre strength height can weave, and processing technology is good, can carry out Quantitative design; (d) baking temperature is low, and preparation technology is simple, and production cost is low, is easy to suitability for industrialized production; (e) being widely used, is to solve photocatalysis technology to be applied to sewage degradation treatment effective method the most, has saved sewage degradation treatment cost.
The titania fiber physical and chemical performance
Continuous poriferous TiO
2Fiber is after 500 ℃ of heat treatment, and its crystalline structure is an anatase, and crystallite dimension is between 40-80nm.Under the low power Electronic Speculum, continuous poriferous TiO
2The fiber surface pattern is more even, and hole is arranged, but crackle do not occur, under the high power Electronic Speculum, and continuous poriferous TiO
2The fiber surface defective is few, only contains very a spot of impurity; Near 380nm, produce tangible UV absorption turning simultaneously.TiO
2The optical absorption band edge of fiber is greatly about 380nm, and there is strong absorption band in the ultraviolet light zone between 200nm-380nm, with TiO
2Material powder is compared, TiO
2The optical absorption band edge of nanofiber does not obviously change.
Continuous poriferous TiO
2Fiber has certain intensity, can twine and weave.Through 500 ℃ of heat treated fibers, its organic matter almost decomposes fully, and the O-H linkage content is higher relatively, and this is mainly due to due to the moisture that fiber surface absorbs.
Description of drawings
Fig. 1 is a colloidal sol of the present invention---gel spinning process schematic diagram
Fig. 2 is the X-x ray diffration pattern x of titania fiber under treatment of different temperature
Fig. 3 is the uv drs collection of illustrative plates of titania fiber
Fig. 4 is the titania fiber stereoscan photograph
Fig. 5 is the titania fiber digital photograph
Fig. 6 is the infared spectrum of titania fiber
The specific embodiment
1) TiO
2Low-molecular-weight colloidal sol preparation method is: with the butyl titanate is initiation material, is that solvent, diethanol amine are chelating agent with the absolute ethyl alcohol, under the interaction of distilled water, concentrated hydrochloric acid, synthesizes low-molecular-weight TiO by hydrolysis and polycondensation reaction
2Colloidal sol.The diethanol amine chelating agent at first adds in the there-necked flask with butyl titanate and diluent absolute ethyl alcohol, and distilled water and hydrochloric acid and absolute ethyl alcohol add simultaneously by funnel, and both rate of addition generally are controlled at 0.7-1.0mlmin
-1Between.
2) adopt sol-gel method (Sol-Gel) preparation TiO by above-mentioned prescription
2The colloidal sol body;
3) when the temperature to 200 of colloidal sol body ℃, add polyethylene glycol and polyethylene, and they are dissolved fully;
4) after polyethylene glycol and polyethylene dissolving, maintain the temperature between 200 ℃-250 ℃, remove organic solvent by evaporation, the molecular weight of titanium colloidal sol body is increased, evaporation time is between 3-6 hours;
5) the titanium colloidal sol body of HMW is put into the spinning bucket, and maintain the temperature between 200-250 ℃,, titanium colloidal sol is extruded through spinneret orifice by to the pressurization of spinning bucket; Spinning bucket pressure is at 10Pa-50Pa;
6) spun titanium colloidal sol silk is evaporated its organic solvent through the vacuum bakeout device, and fiber is dried simultaneously, thereby its viscosity is descended, and helps curling, and the temperature of vacuum bakeout device remains between 300-400 ℃;
7) to continuous poriferous TiO
2Fiber is heat-treated under 500 ℃;
8) to continuous poriferous TiO
2Specific fiber surface is long-pending to be tested with length;
The continuous poriferous TiO of preparation
2Fiber, in air through being pure anatase crystal behind 500 ℃ of heat treatment 1-2h.
Embodiment 1: adopting sol-gel method, is after 99.0% butyl titanate, 3g diethanol amine and 10g absolute ethyl alcohol mix, to join in the there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer.The absolute ethyl alcohol of getting 20g mixes with 4g distilled water, slowly splashes in the there-necked flask by separatory funnel then.Butyl titanate forms low-molecular-weight TiO by hydrolysis, condensation reaction
2Colloidal sol is heated 200 ℃ simultaneously, and adds polyethylene glycol and each 2g of polyethylene and 8g; Keep temperature evaporation 3 hours.Put it into then in the spinning bucket, 200 ℃ of pressurization spinning down, the temperature of vacuum bakeout device remains on 300 ℃ simultaneously, can get continuous poriferous TiO
2Fiber.Then under 500 ℃ to its heat treatment 2 hours, its crystal formation is an anatase, nano particle is of a size of 30-50nm.Fibre length reaches 2m, and specific area is 184m
2/ g.
Embodiment 2: adopting sol-gel method, is after 99.0% butyl titanate, 3g diethanol amine and 10g absolute ethyl alcohol mix, to join in the there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer.The absolute ethyl alcohol of getting 20g mixes with 4g distilled water, slowly splashes in the there-necked flask by separatory funnel then.Butyl titanate forms low-molecular-weight TiO by hydrolysis, condensation reaction
2Colloidal sol is heated 225 ℃ simultaneously, and adds polyethylene glycol and each 3g of polyethylene and 7g, keeps temperature evaporation 3 hours.Put it into then in the spinning bucket, 250 ℃ of pressurization spinning down, the temperature of vacuum bakeout device remains on 300 ℃ simultaneously, can get continuous poriferous TiO
2Fiber.Then under 500 ℃ to its heat treatment 2 hours, its crystal formation is an anatase, nano particle is of a size of 30-50nm.Its length reaches 3.5m, and specific area reaches 175m
2/ g.
Embodiment 3: adopting sol-gel method, is after 99.0% butyl titanate, 3g diethanol amine and 10g absolute ethyl alcohol mix, to join in the there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer.The absolute ethyl alcohol of getting 20g mixes with 4g distilled water, slowly splashes in the there-necked flask by separatory funnel then.Butyl titanate forms low-molecular-weight TiO by hydrolysis, condensation reaction
2Colloidal sol is heated 225 ℃ simultaneously, and adds polyethylene glycol and each 3g of polyethylene and 7g, keeps temperature evaporation 3 hours.Put it into then in the spinning bucket, 225 ℃ of pressurization spinning down, the temperature of vacuum bakeout device remains on 400 ℃ simultaneously, can get continuous poriferous TiO
2Fiber.Then under 500 ℃ to its heat treatment 2 hours, its crystal formation is an anatase, nano particle is of a size of 30-50nm.The length of fiber reaches 10m, and specific area reaches 195m
2/ g.
Embodiment 4: adopting sol-gel method, is after 99.0% butyl titanate, 3g diethanol amine and 10g absolute ethyl alcohol mix, to join in the there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer.The absolute ethyl alcohol of getting 20g mixes with 4g distilled water, slowly splashes in the there-necked flask by separatory funnel then.Butyl titanate forms low-molecular-weight TiO by hydrolysis, condensation reaction
2Colloidal sol is heated 250 ℃ simultaneously, and adds polyethylene glycol and each 1g of polyethylene and 9g, keeps temperature evaporation 3 hours.Put it into then in the spinning bucket, 225 ℃ of pressurization spinning down, the temperature of vacuum bakeout device remains on 400 ℃ simultaneously, can get continuous poriferous TiO
2Fiber.Then under 500 ℃ to its heat treatment 2 hours, its crystal formation is an anatase, nano particle is of a size of 30-50nm.The length of fiber reaches 4m, and specific area reaches 208m
2/ g.
Embodiment 5: adopting sol-gel method, is after 99.0% butyl titanate, 3g diethanol amine and 10g absolute ethyl alcohol mix, to join in the there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer.The absolute ethyl alcohol of getting 20g mixes with 4g distilled water, slowly splashes in the there-necked flask by separatory funnel then.Butyl titanate forms low-molecular-weight TiO by hydrolysis, condensation reaction
2Colloidal sol is heated 200 ℃ simultaneously, and adds polyethylene glycol and each 0.5g of polyethylene and 9.5g, keeps temperature evaporation 4.5 hours.Put it into then in the spinning bucket, 200 ℃ of pressurization spinning down, the temperature of vacuum bakeout device remains on 400 ℃ simultaneously, can get continuous poriferous TiO
2Fiber.Then under 500 ℃ to its heat treatment 1 hour, its crystal formation is an anatase, nano particle is of a size of 30-50nm.The length of fiber reaches 4m, and specific area reaches 208m
2/ g.
Embodiment 6: adopting sol-gel method, is after 99.0% butyl titanate, 3g diethanol amine and 10g absolute ethyl alcohol mix, to join in the there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer.The absolute ethyl alcohol of getting 20g mixes with 4g distilled water, slowly splashes in the there-necked flask by separatory funnel then.Butyl titanate forms low-molecular-weight TiO by hydrolysis, condensation reaction
2Colloidal sol is heated 180 ℃ simultaneously, and adds polyethylene glycol and each 0.5g of polyethylene and 9.5g, keeps 250 ℃ of evaporation times of temperature 6 hours.Put it into then in the spinning bucket, 225 ℃ of pressurization spinning down, the temperature of vacuum bakeout device remains on 400 ℃ simultaneously, can get continuous poriferous TiO
2Fiber.Then under 500 ℃ to its heat treatment 2 hours, its crystal formation is an anatase, nano particle is of a size of 30-50nm.The length of fiber reaches 12m, and specific area reaches 162m
2/ g.
Embodiment 7: adopting sol-gel method, is after 99.0% butyl titanate, 3g diethanol amine and 10g absolute ethyl alcohol mix, to join in the there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer.The absolute ethyl alcohol of getting 20g mixes with 4g distilled water, slowly splashes in the there-necked flask by separatory funnel then.Butyl titanate forms low-molecular-weight TiO by hydrolysis, condensation reaction
2Colloidal sol is heated 250 ℃ simultaneously, and adds polyethylene glycol and each 5g of polyethylene and 15g, evaporation time 6 hours.Put it into then in the spinning bucket, 200 ℃ of pressurization spinning down, the temperature of vacuum bakeout device remains on 400 ℃ simultaneously, can get continuous poriferous TiO
2Fiber.Then under 500 ℃ to its heat treatment 2 hours, its crystal formation is an anatase, nano particle is of a size of 30-50nm.The length of fiber reaches 6m, and specific area reaches 187m
2/ g.
Embodiment 8: adopting sol-gel method, is after 99.0% butyl titanate, 3g diethanol amine and 10g absolute ethyl alcohol mix, to join in the there-necked flask with 60g purity, stirs evenly with GS122 type electronics constant speed stirrer.The absolute ethyl alcohol of getting 20g mixes with 4g distilled water, slowly splashes in the there-necked flask by separatory funnel then.Butyl titanate forms low-molecular-weight TiO by hydrolysis, condensation reaction
2Colloidal sol is heated 250 ℃ simultaneously, and adds polyethylene glycol and each 3g of polyethylene and 10g, evaporation time 6 hours.Put it into then in the spinning bucket, 250 ℃ of pressurization spinning down, the temperature of vacuum bakeout device remains on 350 ℃ simultaneously, can get continuous poriferous TiO
2Fiber.Then under 500 ℃ to its heat treatment 2 hours, its crystal formation is an anatase, nano particle is of a size of 30-50nm.The length of fiber reaches 4m, and specific area reaches 143m
2/ g.
Claims (6)
1, a kind of continuous poriferous titanium dioxide fiber, it is characterized in that with the butyl titanate being raw material, passing through colloidal sol---gel method is prepared low-molecular-weight TiO 2 sol body, adopt evaporation and add the TiO 2 sol body of polymer synthetic high polymer amount, then, by extruding stretching, pre-oxidation and heat treatment, synthetic continuous poriferous titanium dioxide fiber.
2, a kind of preparation method of continuous poriferous titanium dioxide fiber is characterized in that:
1), be initiation material with the butyl titanate, be that solvent, diethanol amine are chelating agent with the absolute ethyl alcohol, under the interaction of distilled water and concentrated hydrochloric acid, synthesize low-molecular-weight TiO
2The colloidal sol body;
2), as low-molecular-weight TiO
2The temperature of colloidal sol body adds polyethylene glycol and polyethylene, and they is dissolved fully to 180-250 ℃;
3), after the dissolving of polyethylene glycol and polyethylene, insulation is removed organic solvent by evaporation, makes TiO
2The molecular weight of colloidal sol body increases, and synthesizes the TiO of HMW
2The colloidal sol body,
4), the TiO of HMW
2The colloidal sol body is put into the spinning bucket, and insulation, by to the pressurization of spinning bucket, makes TiO
2The colloidal sol body is extruded through spinneret orifice;
5), spun TiO
2The colloidal sol silk is evaporated its organic solvent through the vacuum bakeout device, and fiber is dried simultaneously, and viscosity descends, and helps curling.
3, the preparation method of continuous poriferous titanium dioxide fiber according to claim 2 is characterized in that the agents useful for same percentage by weight is: butyl titanate, purity〉99.0%, 50-65%; Diethanol amine, purity〉99.9%, 1-5%; Absolute ethyl alcohol, purity〉99.9%, 25-35%; Polyethylene glycol, purity〉99.9%, 2-8%; Polyethylene, purity〉99.9%, 6-15%.
4, the preparation method of continuous poriferous titanium dioxide fiber according to claim 2 is characterized in that low-molecular-weight TiO
2The colloidal sol body maintains the temperature between 200-250 ℃ after adding the dissolving of polyethylene glycol and polyethylene, and evaporation time is 3-6 hour.
5, the preparation method of continuous poriferous titanium dioxide fiber according to claim 2 is characterized in that the temperature in the spinning bucket remains on 200-250 ℃.
6, the preparation method of continuous poriferous titanium dioxide fiber according to claim 2 is characterized in that the temperature of vacuum bakeout device remains between 300-400 ℃.
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|---|---|---|---|
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|---|---|---|---|
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| CN102417738B (en) * | 2011-11-23 | 2013-03-27 | 常熟钰泰隆摩擦新材料科技有限公司 | Ageing resistant wood plastic composite modified by titanium oxide fiber and lignin and preparation method thereof |
| CN104404757B (en) * | 2014-12-15 | 2017-05-24 | 江南大学 | Preparation method of modified titanium dioxide leather fibers |
| US10655245B2 (en) | 2015-09-16 | 2020-05-19 | Soochow University | Metal oxide macroscopic fiber and preparation method thereof |
| CN111233073B (en) * | 2020-02-18 | 2021-06-15 | 苏州澄江环境科技有限公司 | Handheld photocatalytic fiber sewage treatment device and use method thereof |
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Non-Patent Citations (2)
| Title |
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| 纳米二氧化钛纤维的制备及其光催化活性. 张世英等.硅酸盐学报，第34卷第1期. 2006 |
| 纳米二氧化钛纤维的制备及其光催化活性. 张世英等.硅酸盐学报，第34卷第1期. 2006 * |
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