CN100469438C - Continuous Porous Titanium Dioxide Fiber and Its Preparation Process - Google Patents
Continuous Porous Titanium Dioxide Fiber and Its Preparation Process 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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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000000835 fiber Substances 0.000 title claims abstract description 59
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title abstract description 13
- 229910010413 TiO 2 Inorganic materials 0.000 claims abstract description 42
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000001704 evaporation Methods 0.000 claims abstract description 17
- 238000003980 solgel method Methods 0.000 claims abstract description 15
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 4
- 238000001125 extrusion Methods 0.000 claims abstract 2
- 238000009987 spinning Methods 0.000 claims description 26
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims description 24
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 23
- -1 polyethylene Polymers 0.000 claims description 19
- 239000004698 Polyethylene Substances 0.000 claims description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 18
- 229920000573 polyethylene Polymers 0.000 claims description 18
- 229920001223 polyethylene glycol Polymers 0.000 claims description 18
- 230000008020 evaporation Effects 0.000 claims description 16
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000012153 distilled water Substances 0.000 claims description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000002738 chelating agent Substances 0.000 claims description 4
- 230000003993 interaction Effects 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 2
- 230000009286 beneficial effect Effects 0.000 claims 1
- 239000003153 chemical reaction reagent Substances 0.000 claims 1
- 238000002788 crimping Methods 0.000 claims 1
- 239000007858 starting material Substances 0.000 claims 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 abstract description 17
- 238000005516 engineering process Methods 0.000 abstract description 16
- 239000000463 material Substances 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 4
- 239000002657 fibrous material Substances 0.000 abstract description 3
- 238000001891 gel spinning Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- 238000009776 industrial production Methods 0.000 abstract 1
- 239000012784 inorganic fiber Substances 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 229940043237 diethanolamine Drugs 0.000 description 12
- 239000013078 crystal Substances 0.000 description 9
- 230000007062 hydrolysis Effects 0.000 description 9
- 238000006460 hydrolysis reaction Methods 0.000 description 9
- 230000015572 biosynthetic process Effects 0.000 description 8
- 238000006482 condensation reaction Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 239000002105 nanoparticle Substances 0.000 description 8
- 238000003756 stirring Methods 0.000 description 8
- 239000010865 sewage Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 4
- 238000006731 degradation reaction Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 230000001699 photocatalysis Effects 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 229910052719 titanium Inorganic materials 0.000 description 4
- 239000010936 titanium Substances 0.000 description 4
- 230000002950 deficient Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- 230000000845 anti-microbial effect Effects 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000000977 initiatory effect Effects 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000011858 nanopowder Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000005416 organic matter Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 208000037656 Respiratory Sounds Diseases 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000000680 avirulence Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000002153 concerted effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003085 diluting agent Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000002121 nanofiber Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000006068 polycondensation reaction Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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Abstract
本发明涉及一种连续多孔二氧化钛纤维及其制备工艺。利用溶胶—凝胶法制备连续多孔氧化钛纤维，首先合成低分子量的TiO2溶胶体，通过蒸发有机溶剂和添加聚合物，制备高分子量的TiO2纤维先驱体。再通过挤出拉伸合成连续多孔TiO2纤维。该方法的突出特点是；应用溶胶—凝胶方法制备具有新奇结构和良好物理化学性质的连续多孔氧化钛纤维材料，为连续无机纤维材料的应用研究提供了一个新途径。同时，该工艺简单，易于工业化生产，并且为发展溶胶—凝胶纺丝研究理论、技术与方法体系做出积极地贡献。
The invention relates to a continuous porous titanium dioxide fiber and a preparation process thereof. The continuous porous titanium oxide fiber was prepared by sol-gel method. Firstly, low molecular weight TiO 2 sol was synthesized, and high molecular weight TiO 2 fiber precursor was prepared by evaporating organic solvent and adding polymer. Continuous porous TiO2 fibers were then synthesized by extrusion stretching. The outstanding feature of this method is that the sol-gel method is used to prepare continuous porous titanium oxide fiber materials with novel structure and good physical and chemical properties, which provides a new way for the application research of continuous inorganic fiber materials. At the same time, the process is simple, easy for industrial production, and makes positive contributions to the development of sol-gel spinning research theory, technology and method system.
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)
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|---|---|---|---|
| CN 200710034514 CN100469438C (en) | 2007-03-09 | 2007-03-09 | Continuous Porous Titanium Dioxide Fiber and Its Preparation Process |
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|---|---|---|---|
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| CN100469438C true CN100469438C (en) | 2009-03-18 |
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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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2007
- 2007-03-09 CN CN 200710034514 patent/CN100469438C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 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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| CN101041127A (en) | 2007-09-26 |
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