CN104651976A - Preparation method of Si doped TiO2 fiber - Google Patents
Preparation method of Si doped TiO2 fiber Download PDFInfo
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- CN104651976A CN104651976A CN201310575832.1A CN201310575832A CN104651976A CN 104651976 A CN104651976 A CN 104651976A CN 201310575832 A CN201310575832 A CN 201310575832A CN 104651976 A CN104651976 A CN 104651976A
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Abstract
The preparation method of Si doped TiO2 fiber belongs to the field of chemistry. Specifically, the invention relates to a preparation method of Si doped TiO2 fiber. The preparation method of nano scale Si doped TiO2 fiber provided by the invention is low in cost, and simple in reaction conditions. The preparation method of the Si doped TiO2 fiber provided by the invention is characterized by comprising the following steps: dissolving tetrabutyl titanate, ethyl acetoacetate and distilled water in chemical dose of 1: 15 in isopropanol; conducting reflux at room temperature under N2 protection to realize complete reaction; concentrating in an oil bath and conducting rotary evaporation to dryness; dissolving the yellow powder in tetrahydrofuran, adding 10-15% of tetraethoxysilane, controlling the molar ratio of Si and Ti in the ingredients, and completely stirring to dissolve; conducting rotary evaporation condensation to obtain a sol spinning solution; controlling certain temperature and humidity, preparing precursor fibers by a dry spinning method; designing a temperature programming process, activating by steam, and insulating for 3-15 h after reaching a preset activation temperature to obtain the Si doped TiO2 long fiber.
Description
Technical field
The invention belongs to chemical field, specifically, the present invention relates to a kind of Si and adulterate to TiO
2the preparation method of fibre object.
Background technology
Nano-TiO
2to gather around in the environmental protection such as water treatment, gas purification, automatically cleaning and photodissociation hydrogen manufacturing fabrication of new materials and energy field as a class broad-spectrum light catalyst and have broad application prospects, get more and more people's extensive concerning. but the suspended phase photocatalysis system of routine also exists TiO
2the shortcomings such as micro mist difficulty reclaims and light transmittance is low, and continue after the immobilization technology [4] of development at solution TiO
2while separation and recovery problem, but greatly reduce its photocatalytic activity, and it being loosely etc. not enough to there is catalyst cupport. the intrinsic separately drawback of suspended phase and immobilization technology had become the bottleneck that photocatalysis technology move towards practicality already. new Ti O
2fiber optic catalysis material is because having modal advantage and flow impact resistant load high, although provide brand-new approach for effectively solving an above-mentioned practical difficult problem. domestic and international existing technology of preparing, as sol-gel process, KDC method and solvent-thermal method etc. cut both ways, but usually can only obtain micron-sized whisker or fibrous TiO
2.
Summary of the invention
The present invention is exactly for above-mentioned technical problem, and provide a kind of with low cost, reaction condition is simple, can reach nano level Si and adulterate to TiO
2the preparation method of fibre object.
For realizing above-mentioned purpose of the present invention, the present invention adopts following technical scheme: Si doping of the present invention is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution. and the concentrated and rotary evaporated to dryness through oil bath, obtains yellow powder.Be dissolved in by yellow powder in oxolane, the ethyl orthosilicate adding 10-15% also controls the mol ratio of Si and Ti in batching, is fully stirred to dissolve completely. and concentrate through rotary evaporation and obtain colloidal sol spinning solution.Control uniform temperature and humidity.Dry spinning obtains precursor fibre, the heating process adopt steam-activation treatment of designing program, and reaches insulation 3-15h after the activation temperature drafted, obtains Si doped Ti O
2long fiber.
Beneficial effect of the present invention: reaction condition of the present invention is simple, without the need to large-scale auxiliary equipment, is applicable to medium-sized and small enterprises and uses; Initial input is cheap, and principle is easy to obtain, and raw material require that purity is low, considerably reduce production cost.
(1) adopt sol-gel process, Bound moisture steam activation technique, can obtain the Si doped Ti O that diameter is 100 ~ 200nm, even compact
2fiber.The matrix of this fiber is by having the anatase TiO comparatively enriching meso-hole structure
2nanocrystalline formation, its structure can be regulated and controled by the Si/Ti mol ratio changed in composition.As treatment function novel photocatalyst, have form and performance advantage concurrently, there is catalytic activity in use high, use the features such as rear filtered and recycled is easy.
(2) in fiber preparation, the doping of appropriate Si is useful.By forming Ti-O-Si key, anatase TiO can be stoped on the one hand
2nanocrystalline grow up and limit its generation to rutile phase transformation, produce quantum optical field and improve the separative efficiency in light induced electron and hole; The Surface Texture characteristic of fiber product can be optimized again on the other hand, increase specific area and pore volume.And its result is all conducive to strengthening TiO
2the high temperature microstructure stability of fiber, the pre-absorption of strengthening pollutant and raising photocatalytic activity.
(3) photocatalysis result shows, when the mol ratio of Si/Ti is 0.15, and the Si doped Ti O after 700 DEG C of heat treatment
2fiber has best photocatalytic activity, is pure TiO under same condition
21.5 times of product photocatalytic activity.The crystal grain forming this fiber is about 9.0 nm, and specific area is 127.7m2g, and forms the orderly mesopore orbit of arrangement between particle.
Detailed description of the invention
Si doping of the present invention is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution.Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder.Be dissolved in by yellow powder in oxolane, the ethyl orthosilicate adding 10-15% also controls the mol ratio of Si and Ti in batching, is fully stirred to dissolve completely.Concentrate through rotary evaporation and obtain colloidal sol spinning solution.Control uniform temperature and humidity, dry spinning obtains precursor fibre, the heating process adopt steam-activation treatment of designing program, and reaches insulation 3-15h after the activation temperature drafted, obtains Si doped Ti O
2long fiber.
Embodiment 1: Si doping of the present invention is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution.Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder.Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 10%, be fully stirred to dissolve completely.Concentrate through rotary evaporation and obtain colloidal sol spinning solution.Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 4h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
Embodiment 2: Si doping of the present invention is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution. and the concentrated and rotary evaporated to dryness through oil bath, obtains yellow powder.Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 11%, be fully stirred to dissolve completely. concentrate through rotary evaporation and obtain colloidal sol spinning solution.Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 4h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
Embodiment 3: Si doping of the present invention is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution.Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder.Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 12%, be fully stirred to dissolve completely.Concentrate through rotary evaporation and obtain colloidal sol spinning solution.Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 5h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
Embodiment 4: Si doping of the present invention is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution.Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder.Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 13%, be fully stirred to dissolve completely.Concentrate through rotary evaporation and obtain colloidal sol spinning solution.Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 6h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
Embodiment 5: Si doping of the present invention is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and be made into polymerization titanium mixed solution, through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder.Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 14%, be fully stirred to dissolve completely.Concentrate through rotary evaporation and obtain colloidal sol spinning solution, control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 7h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
Embodiment 6: Si doping of the present invention is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and be made into polymerization titanium mixed solution, through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder.Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 15%, be fully stirred to dissolve completely.Concentrate through rotary evaporation and obtain colloidal sol spinning solution, control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 8h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
Claims (7)
1.Si doping is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution; Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder; Be dissolved in by yellow powder in oxolane, the ethyl orthosilicate adding 10-15% also controls the mol ratio of Si and Ti in batching, is fully stirred to dissolve completely; Concentrate through rotary evaporation and obtain colloidal sol spinning solution; Control uniform temperature and humidity, dry spinning obtains precursor fibre, the heating process adopt steam-activation treatment of designing program, and reaches insulation 3-15h after the activation temperature drafted, obtains Si doped Ti O
2long fiber.
2. Si doping according to claim 1 is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution; Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder; Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 10%, be fully stirred to dissolve completely; Concentrate through rotary evaporation and obtain colloidal sol spinning solution; Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 4h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
3. Si doping according to claim 1 is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution; Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder; Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 11%, be fully stirred to dissolve completely; Concentrate through rotary evaporation and obtain colloidal sol spinning solution; Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 4h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
4. Si doping according to claim 1 is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution; Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder; Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 12%, be fully stirred to dissolve completely; Concentrate through rotary evaporation and obtain colloidal sol spinning solution; Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 5h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
5. Si doping according to claim 1 is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution; Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder; Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 13%, be fully stirred to dissolve completely; Concentrate through rotary evaporation and obtain colloidal sol spinning solution; Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 6h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
6. Si doping according to claim 1 is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution; Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder; Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 14%, be fully stirred to dissolve completely; Concentrate through rotary evaporation and obtain colloidal sol spinning solution; Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 7h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
7. Si doping according to claim 1 is to TiO
2the preparation method of fibre object, is characterized in that: be dissolved in isopropyl alcohol by butyl titanate, ethyl acetoacetate and distilled water by the chemical dose of 1:15, N
2under protection, under room temperature, backflow makes to react completely, and is made into polymerization titanium mixed solution; Through oil bath, concentrated and rotary evaporated to dryness, obtains yellow powder; Yellow powder is dissolved in oxolane, adds the mol ratio of Si and Ti in the ethyl orthosilicate also control batching of 15%, be fully stirred to dissolve completely; Concentrate through rotary evaporation and obtain colloidal sol spinning solution; Control uniform temperature and humidity, dry spinning obtains precursor fibre, and the heating process adopt steam-activation treatment of designing program, is incubated 8h after reaching the activation temperature drafted, obtains Si doped Ti O
2long fiber.
Priority Applications (1)
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|---|---|---|---|
| CN201310575832.1A CN104651976A (en) | 2013-11-18 | 2013-11-18 | Preparation method of Si doped TiO2 fiber |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310575832.1A CN104651976A (en) | 2013-11-18 | 2013-11-18 | Preparation method of Si doped TiO2 fiber |
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| CN104651976A true CN104651976A (en) | 2015-05-27 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107008240A (en) * | 2017-04-18 | 2017-08-04 | 南京理工大学 | Nano crystal titanium dioxide light catalyst of aluminum oxide open celled foam ceramic load Si doping and preparation method thereof |
| CN113957567A (en) * | 2021-12-15 | 2022-01-21 | 山东大学 | TiO 22-SiO2Precursor sol spinning solution and preparation method of titanium-silicon composite oxide nano-fiber |
-
2013
- 2013-11-18 CN CN201310575832.1A patent/CN104651976A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107008240A (en) * | 2017-04-18 | 2017-08-04 | 南京理工大学 | Nano crystal titanium dioxide light catalyst of aluminum oxide open celled foam ceramic load Si doping and preparation method thereof |
| CN113957567A (en) * | 2021-12-15 | 2022-01-21 | 山东大学 | TiO 22-SiO2Precursor sol spinning solution and preparation method of titanium-silicon composite oxide nano-fiber |
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Application publication date: 20150527 |
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