CN106929949B - One-step synthesis method poly-vinegar acid oxygen titanium precursors, its colloidal sol spinning solution and the oxidation long stapled preparation method of titanium crystal - Google Patents
One-step synthesis method poly-vinegar acid oxygen titanium precursors, its colloidal sol spinning solution and the oxidation long stapled preparation method of titanium crystal Download PDFInfo
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- CN106929949B CN106929949B CN201511031102.0A CN201511031102A CN106929949B CN 106929949 B CN106929949 B CN 106929949B CN 201511031102 A CN201511031102 A CN 201511031102A CN 106929949 B CN106929949 B CN 106929949B
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/003—Compounds containing elements of Groups 4 or 14 of the Periodic System without C-Metal linkages
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/0007—Electro-spinning
- D01D5/0015—Electro-spinning characterised by the initial state of the material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The present invention relates to one-step synthesis method poly-vinegar acid oxygen titanium precursors, its colloidal sol spinning solution and the oxidation long stapled preparation methods of titanium crystal.Poly-vinegar acid oxygen titanium precursors are directly prepared using four isopropyl ester of metatitanic acid and acetic acid one-step method, then directly prepare poly-vinegar acid oxygen titanium precursors colloidal sol spinning solution with anhydrous methanol, poly-vinegar acid oxygen titanium precursors fiber is made through high-voltage electrostatic spinning；The precursor fibre is heat-treated in high temperature, sintering obtains titanium oxide crystal fibre, 1~2 μm of diameter, 3~10cm of length.The method of the present invention enormously simplifies the route of synthesis of presoma, improves solid content, efficient, energy conservation, convenient for industrial production.
Description
Technical field
The present invention relates to a kind of one-step synthesis method poly-vinegar acid oxygen titanium precursors, poly-vinegar acid oxygen titanium precursors colloidal sol spinning solution
The oxidation long stapled method of titanium crystal is prepared and thus prepared, titanium oxide crystal fibre field of material technology is belonged to.
Background technique
Titanium dioxide crystal fiber has the characteristics that crystallite dimension and large specific surface area, can show good visible light
Catalytic activity is suitable as photocatalytic filter, catalyst carrier, semiconductor material.CN101421454A discloses one kind two
The manufacturing method of titanium dioxide fiber is manufactured by method of electrostatic spinning by the composition using the composition containing Titanium particles
Fiber assembly, by being burnt into the fiber assembly, in addition, being prepared with for the titania fiber that document is announced is solidifying
Glue-sol method, there are also glycol methods etc., of heap of stone etc. referring to Huang, preparation, characterization and its visible light catalytic of titania fiber
Can, petrochemical industry, the 1st phase in 2007.According to the record of document above it is found that the key technology of titanium dioxide crystal fiber preparation
First is that the preparation of colloidal sol spinning solution, prior art common problem is: the production of colloidal sol spinning solution is difficult, component is complicated, solid
Content is lower, energy consumption height is not easy to be mass produced, and fiber prepared by colloidal sol ropiness difference is mostly nanometer crystal fiber.
Summary of the invention
The present invention be directed to the production of colloidal sol in the prior art complexity, long period, energy consumption height, solid content is lower asks
Topic provides a kind of poly-vinegar acid oxygen titanium precursors, colloidal sol spinning solution and the high-quality oxidation long stapled preparation method of titanium crystal.It should
Method is more suitable for large-scale production, simple process, energy-efficient, the long fibre of oxidation titanium crystal for being able to achieve high-quality, haveing excellent performance
The industrialized production of dimension.
Technical scheme is as follows:
One, poly-vinegar acid oxygen titanium precursors
Poly-vinegar acid oxygen titanium precursors provided by the invention are obtained by the following method:
The preparation method of one-step synthesis method poly-vinegar acid oxygen titanium precursors, steps are as follows:
Tetraisopropyl titanate is dissolved in acetic acid, the ratio for being 1:1.0-5.0 by the molar ratio of tetraisopropyl titanate and acetic acid
Example stirs evenly, and controls temperature at 50~70 DEG C, obtains transparency liquid；Under stirring conditions, transparency liquid is made to be cooled to 10
~20 DEG C, there is white precipitate precipitation, be filtered by vacuum, precipitation and separation, and in 20~60 DEG C of dryings, obtains poly-vinegar acid oxygen titanium precursor
Body.Gained poly-vinegar acid oxygen titanium precursors are white powder.
Two, colloidal sol spinning solution
Colloidal sol spinning solution provided by the invention is to be formulated using poly-vinegar acid oxygen titanium precursors above-mentioned, specifically
It is bright as follows.
A kind of preparation method of poly-vinegar acid oxygen titanium colloidal sol spinning lyosol, comprises the following steps that
The poly-vinegar acid oxygen titanium precursors are dissolved in anhydrous methanol, the poly-vinegar acid oxygen titanium precursors: anhydrous methanol matter
Amount is than being 1.5~3.0:1；It is stirred at a temperature of 30~50 DEG C, until poly-vinegar acid oxygen titanium precursors are completely dissolved, obtains transparent poly-vinegar
Sour oxygen titanium colloidal sol spinning solution.
Preferably, the poly-vinegar acid oxygen titanium colloidal sol spinning fluid viscosity is 2~7Pas (25 DEG C measure).
Three, the long stapled preparation of titanium crystal is aoxidized
A kind of long stapled preparation method of oxidation titanium crystal, preparation, colloidal sol spinning solution including poly-vinegar acid oxygen titanium precursors
Preparation, electrostatic spinning, heat treatment, steps are as follows:
(1) preparation of poly-vinegar acid oxygen titanium precursors
Tetraisopropyl titanate is dissolved in acetic acid, the ratio for being 1:1.0-5.0 by the molar ratio of tetraisopropyl titanate and acetic acid
Example stirs evenly, and controls temperature at 50~80 DEG C, obtains transparency liquid；Under stirring conditions, transparency liquid is made to be cooled to 10
~30 DEG C, there is white precipitate precipitation, be filtered by vacuum, precipitation and separation, and in 20~60 DEG C of dryings, obtains poly-vinegar acid oxygen titanium precursor
Body；
(2) preparation of colloidal sol spinning solution
Poly-vinegar acid oxygen titanium precursors prepared by step (1) are dissolved in anhydrous methanol, the poly-vinegar acid oxygen titanium precursors: nothing
Water methanol mass ratio is 1.5~3.0:1；It stirs at a temperature of 30~50 DEG C, until poly-vinegar acid oxygen titanium precursors are completely dissolved, obtains
Bright poly-vinegar acid oxygen titanium colloidal sol spinning solution, viscosity are 2~7Pas；
(3) electrostatic spinning
Titanium dioxide fiber, electrostatic spinning process condition are prepared using high-pressure electrostatic mode are as follows: 10~40 DEG C of temperature, humidity 40
~70%, 10~60KV of voltage obtain titania precursor body long fibre；The titania precursor body long fibre continuous length 3~
10cm。
(4) it is heat-treated
The titania precursor body long fibre of step (3) preparation is warming up to 500 with the heating rate of 3~10 DEG C/min~
600 DEG C, constant temperature 0.5-1h, obtain anatase titanium oxide crystal long fibre.Gained aoxidizes 1~2 μm of titanium crystal long fibre diameter, length
Continuous about 3~10cm.
Preferred according to the present invention, the molar ratio of tetraisopropyl titanate described in step (1) and acetic acid is 1:2.0~4.0.
Preferred according to the present invention, drying temperature described in step (1) is 30~40 DEG C.
It is preferred according to the present invention, step (3) electrostatic spinning process condition are as follows: 20~30 DEG C of temperature, humidity 50~60%
20~50KV of voltage.
It is preferred according to the present invention, medium temperature heat treatment is carried out using program-controlled sintering furnace in step (4).Program-controlled sintering furnace is this
Field conventional equipment.It is final that 500~600 DEG C of medium temperatures heat treatment of step (4) makes poly-vinegar acid oxygen titanium precursors that crystallization conversion occur
Obtain titanium oxide (anatase) crystal long fibre.
In high-quality of the present invention oxidation titanium crystal long fibre preparation method, the poly-vinegar acid oxygen titanium precursors and colloidal sol
Chemical property stablize, purity is high, gained aoxidize the long stapled crystal phase of titanium crystal be Anatase.Titanium oxide crystal fibre crystal grain
Development completely, the continuous about 3~10cm of 1~3 μm of diameter, length, and relax it is soft it is flexible, without slimeball.
The present invention is using tetraisopropyl titanate and acetate system one-step synthesis method poly-vinegar acid oxygen titanium precursors and colloidal sol and oxygen
Change the long stapled preparation method of titanium crystal.Its excellent results is as follows compared with prior art by the present invention:
1, by adjusting the reaction ratio of tetraisopropyl titanate and acetic acid, reaction temperature, a step directly obtains poly- the present invention
Acetic acid oxygen titanium precursors solid powder is changed the prior art and is rotated using vacuum, and the mode of time-consuming and laborious high energy consumption makes the forerunner
Body is more suitable for industrialized production.And the degree of polymerization and collosol stability of poly-vinegar acid oxygen titanium are improved, it is simple process, energy-efficient.
2, the poly-vinegar acid oxygen titanium precursors that the present invention uses are dissolved in the poly-vinegar acid oxygen titanium colloidal sol that anhydrous methanol is made transparent
Spinning solution greatly reduces the content of by-product in precursor sol, and the colloidal sol for solving prior art acquisition cannot be for a long time
The problem of placing, being easily converted into gel and lose spinnability.
3, the precursor fibre that the present invention is obtained through high-pressure electrostatic, intensity is high, translucent, is to have continuous length and fixation several
The fiber of what shape brings convenience for subsequent continuous heat, greatly improves production efficiency.By improving poly-vinegar acid oxygen
The stability of the titanium degree of polymerization and colloidal sol spinning solution is completed quickly and effectively amorphous precursors and turns between titanium oxide grain
Become, obtains the titanium oxide crystal fibre of high-quality.
4, the tetraisopropyl titanate and acetic acid that the present invention uses are the common industrial chemicals of industry, are easily bought, cost is controllable.
Detailed description of the invention
Before Fig. 1 is the poly-vinegar acid oxygen titanium that the molar ratio of tetraisopropyl titanate and acetic acid is 1:3 in embodiment 1 ratio obtains
Drive body white powder photo.
Fig. 2 is that gained spinning solution photo in 100g anhydrous methanol is added in 150g poly-vinegar acid oxygen titanium in embodiment 1.
Fig. 3 is titania precursor body fibre picture made from electrostatic spinning in embodiment 1.
Fig. 4 is finished product anatase titanium oxide crystal long fibre photo in embodiment 1.
Fig. 5 is poly-vinegar acid oxygen titanium precursors XRD spectra photo in embodiment 1
Fig. 6 is finished product anatase titanium oxide crystal XRD spectra (600 DEG C of temperature, 0.5h) in embodiment 1
Fig. 7 is finished product anatase titanium oxide crystal fibre stereoscan photograph in embodiment 1.
Fig. 8 is finished product anatase titanium oxide crystal fibre stereoscan photograph (amplification) in embodiment 1.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, but not limited to this.
Embodiment 1:
(1) it is about 1:3 by the molar ratio of tetraisopropyl titanate and acetic acid, weighs 100g tetraisopropyl titanate solution and slowly drip
It adding in 63g acetum, this process is exothermic reaction, and temperature need to be controlled at 70 DEG C, stir slow cooling to 10~25 DEG C,
Generate a large amount of white poly-vinegar acid oxygen titanium precipitatings.8h is stood at 20~25 DEG C, precipitating is made sufficiently to be sunken to bottom, then passes through vacuum
It filters, 30-40 DEG C of drying obtains poly-vinegar acid oxygen titanium precursors white powder (as shown in Figure 1).Solid content reaches 39% or more.
XRD spectra show unformed substance in Fig. 5.
(2) will preparation 150g poly-vinegar acid oxygen titanium precursors be added 100g anhydrous methanol in, stirred at 30~50 DEG C to
Poly-vinegar acid oxygen titanium white powder is completely dissolved, and acquisition is colorless and transparent, has viscoelastic solution, which can be at 10~40 DEG C
It places for a long time.Viscosity is 4.6Pas (25 DEG C measure).
(3) spinning solution of step (2) is put into high-voltage electrostatic spinning machine, process conditions are as follows: 20~30 DEG C of temperature, humidity 50
~60%, 25~35KV of voltage obtain titania precursor body fiber, the continuous about 3~10cm of 1.0~3.0 μm of diameter, length.
(4) titania precursor body fiber is placed in program-controlled sintering furnace, is warming up to 600 DEG C with the heating rate of 3 DEG C/min,
And 0.5h is kept the temperature, and it can get high-purity, the complete anatase titanium oxide crystal long fibre of grain development, it is 1.0~2.0 μm of diameter long
Spend 3~10cm.Gained fiber shows good visible light catalysis activity.
Embodiment 2: as described in Example 1, except that step (1) is by the molar ratio of tetraisopropyl titanate and acetic acid
The ratio of 1:3.5 weighs 100g tetraisopropyl titanate solution and is slowly added dropwise into 73.5g acetum.Temperature is controlled at 65 DEG C,
Lower slow cooling is stirred to 15~20 DEG C, generates a large amount of white poly-vinegar acid oxygen titanium precipitatings.10h is stood at 25 DEG C, fills precipitating
Divide and be sunken to bottom, then by vacuum filtration, 30-40 DEG C of drying obtains poly-vinegar acid oxygen titanium precursors white powder.
Embodiment 3: as described in Example 1, except that step (1) is by the molar ratio of tetraisopropyl titanate and acetic acid
1:4 weighs 100g tetraisopropyl titanate solution and is slowly added dropwise into 84g acetum.Temperature is controlled at 75 DEG C, under stirring
Slow cooling generates a large amount of white poly-vinegar acid oxygen titanium precipitatings to 20 DEG C.7h is stood at 25 DEG C, precipitating is made sufficiently to be sunken to bottom,
Then by vacuum filtration, 30-40 DEG C of drying obtains poly-vinegar acid oxygen titanium precursors white powder.
Embodiment 4: as described in Example 1, except that step (1) is by the molar ratio of tetraisopropyl titanate and acetic acid
1:5 weighs 100g tetraisopropyl titanate solution and is slowly added dropwise into 105g acetum.Temperature is controlled at 60 DEG C, under stirring
Slow cooling generates a large amount of white poly-vinegar acid oxygen titanium precipitatings to 15 DEG C.6h is stood at 20 DEG C, precipitating is made sufficiently to be sunken to bottom,
Then by vacuum filtration, 30-40 DEG C of drying obtains poly-vinegar acid oxygen titanium precursors white powder.
Embodiment 5: as described in Example 1, except that 100g is added without water beetle in 200g poly-vinegar acid oxygen titanium by step (2)
In alcohol, stirring to poly-vinegar acid oxygen titanium white powder is completely dissolved at 30~50 DEG C, is obtained colorless and transparent, molten with viscoplasticity
Liquid, the spinning solution can be placed for a long time at 10~40 DEG C.
Embodiment 6: as described in Example 1, except that in step (2) that 250g poly-vinegar acid oxygen titanium addition 100g is anhydrous
In methanol.
Embodiment 7: as described in Example 1, except that 100g is added without water beetle in 300g poly-vinegar acid oxygen titanium by step (2)
In alcohol.
Claims (6)
1. a kind of long stapled preparation method of oxidation titanium crystal, preparation, colloidal sol spinning solution including poly-vinegar acid oxygen titanium precursors
Preparation, electrostatic spinning, heat treatment, steps are as follows:
(1) preparation of poly-vinegar acid oxygen titanium precursors
Tetraisopropyl titanate is dissolved in acetic acid, is stirred in the ratio that the molar ratio of tetraisopropyl titanate and acetic acid is 1:1.0-5.0
It mixes uniformly, controls temperature at 50~80 DEG C, obtain transparency liquid；Under stirring conditions, transparency liquid is made to be cooled to 10~30
DEG C, there is white precipitate precipitation, be filtered by vacuum, precipitation and separation, and in 20~60 DEG C of dryings, obtains poly-vinegar acid oxygen titanium precursors；
(2) preparation of colloidal sol spinning solution
Poly-vinegar acid oxygen titanium precursors prepared by step (1) are dissolved in anhydrous methanol, the poly-vinegar acid oxygen titanium precursors: without water beetle
Alcohol mass ratio is 1.5~3.0:1；It stirs at a temperature of 30~50 DEG C, until poly-vinegar acid oxygen titanium precursors are completely dissolved, obtains transparent
Poly-vinegar acid oxygen titanium colloidal sol spinning solution, viscosity be 2~7Pas, 25 DEG C measure；
(3) electrostatic spinning
Titanium dioxide fiber, electrostatic spinning process condition are prepared using high-pressure electrostatic mode are as follows: 10~40 DEG C of temperature, humidity 40~
70%, 10~60kV of voltage obtain titania precursor body long fibre；The titania precursor body long fibre continuous length 3~
10cm；
(4) it is heat-treated
Titania precursor body long fibre prepared by step (3) is warming up to 500~600 DEG C with the heating rate of 3~10 DEG C/min,
Constant temperature 0.5-1h obtains anatase titanium oxide crystal long fibre.
2. the oxidation long stapled preparation method of titanium crystal as described in claim 1, wherein gained oxidation titanium crystal long fibre is straight
1~2 μm of diameter, 3~10cm of length.
3. the oxidation long stapled preparation method of titanium crystal as described in claim 1, wherein metatitanic acid four described in step (1) is different
The molar ratio of propyl ester and acetic acid is 1:2.0~4.0.
4. aoxidizing the long stapled preparation method of titanium crystal as described in claim 1, wherein drying temperature described in step (1) is
30~40 DEG C.
5. the oxidation long stapled preparation method of titanium crystal as described in claim 1, wherein step (3) electrostatic spinning process item
Part are as follows: 20~30 DEG C of temperature, humidity 50~60%, 20~50kV of voltage.
6. the oxidation long stapled preparation method of titanium crystal as described in claim 1, wherein use program-controlled sintering in step (4)
Furnace carries out medium temperature heat treatment.
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| CN113957567B (en) * | 2021-12-15 | 2022-08-26 | 山东大学 | TiO 2 2 -SiO 2 Precursor sol spinning solution and preparation method of titanium-silicon composite oxide nanofiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101421454A (en) * | 2006-04-18 | 2009-04-29 | 帝人株式会社 | Titania fiber and method for manufacturing titania fiber |
| CN102286804A (en) * | 2011-06-01 | 2011-12-21 | 南京理工大学 | Preparation method of titanium dioxide fibers with photocatalysis function and polycrystalline nanostructure |
| CN102153138B (en) * | 2010-11-02 | 2013-07-24 | 中山大学 | Graded titanium dioxide microspheres consisting of nano rods and nano granules |
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| KR100666477B1 (en) * | 2005-06-16 | 2007-01-11 | 한국과학기술연구원 | Titanium dioxide nanorod and its fabrication method |
| US9267220B2 (en) * | 2006-03-31 | 2016-02-23 | Cornell University | Nanofibers, nanotubes and nanofiber mats comprising crystaline metal oxides and methods of making the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101421454A (en) * | 2006-04-18 | 2009-04-29 | 帝人株式会社 | Titania fiber and method for manufacturing titania fiber |
| CN102153138B (en) * | 2010-11-02 | 2013-07-24 | 中山大学 | Graded titanium dioxide microspheres consisting of nano rods and nano granules |
| CN102286804A (en) * | 2011-06-01 | 2011-12-21 | 南京理工大学 | Preparation method of titanium dioxide fibers with photocatalysis function and polycrystalline nanostructure |
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