CN104646063A - Synthetic method of porphyrin sensitized TiO2 composite microspheres - Google Patents
Synthetic method of porphyrin sensitized TiO2 composite microspheres Download PDFInfo
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- CN104646063A CN104646063A CN201310575806.9A CN201310575806A CN104646063A CN 104646063 A CN104646063 A CN 104646063A CN 201310575806 A CN201310575806 A CN 201310575806A CN 104646063 A CN104646063 A CN 104646063A
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Abstract
A synthetic method of porphyrin sensitized TiO2 composite microspheres belongs to the chemical field. Specifically, the invention relates to a synthetic method of the porphyrin sensitized TiO2 composite microspheres. The synthetic method of porphyrin sensitized TiO2 composite microspheres provided by the invention is low in cost, simple in reaction condition and good in product quality. The synthetic method of APTCPP provided by the invention is characterized by comprising the following steps: successively adding 100-300 mg of APTCPP, 100 mg of azobisisobutyronitrile, 100-300 mg of mercaptopropyltriethoxysilane and 30 ml of toluene into a 100-300 ml round bottom flask equipped with a reflux condenser tube, reacting with stirring under the protection of nitrogen in a water bath at 80 DEG C, detecting the reaction process by a thin layer chromatography method, stopping the heating after the reaction, cooling to room temperature, conducting reduced pressure distillation to remove toluene, so as to obtain the porphyrin sensitized TiO2 microspheres.
Description
Technical field
The invention belongs to chemical field, specifically, the present invention relates to the TiO of porphyrin sensitization
2the synthetic method of complex microsphere.
Background technology
TiO
2owing to having, high, the fast light corrosive power of photocatalytic activity is strong, good stability, environmental friendliness, relative low price and to advantages such as human non-toxic's property, has become in photocatalysis degradation organic contaminant field and has studied a kind of catalysis material [1 ~ 4] the most deep; But the forbidden band of TiO2 is wider, the ultraviolet only having energy higher just can excite its photocatalytic activity, though can consider to utilize sunshine as light source, its middle-ultraviolet lamp only accounts for about 4%, and light utilization ratio is lower; Therefore, often need to use ultraviolet source in application process, and the uviol lamp of additional configuration and ultraviolet limit TiO2 to the harm that human body is potential
2catalysis material is applied more widely.
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, the TiO of the porphyrin sensitization of good product quality
2the synthetic method of complex microsphere.
For realizing above-mentioned purpose of the present invention; the present invention adopts following technical scheme: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 100-300ml round-bottomed flask that reflux condensing tube is housed, add 100-300mg APTCPP successively; 100 mg azodiisobutyronitriles; 100-300 mg mercaptopropyltriethoxysilane; with 30ml toluene; under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards; be cooled to room temperature, after pressure reducing and steaming toluene, obtain the TiO of porphyrin sensitization
2complex microsphere.
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.
Sol-gel process is adopted to prepare the TiO of APTCPP sensitization
2complex microsphere. under visible light illumination, this material list reveals higher than pure TiO
2photochemical catalytic oxidation
αthe ability of-terpinene, confirms that APTCPP is to TiO
2sensibilization, improve the visible light photocatalysis active of catalyst. due to APTCPP and TiO
2between Covalently attached interaction improve the stability of catalyst and recycle effect, simultaneously the preparation of catalyst is relatively simple, is easy to operation, and can filter and reclaim, the TiO of therefore this porphyrin sensitization
2microballoon has potential application prospect in photocatalysis treatment environmental contaminants.
Detailed description of the invention
The synthetic method of APTCPP of the present invention; it is characterized in that: in the 100-300ml round-bottomed flask that reflux condensing tube is housed, add 100-300mg APTCPP successively; 100 mg azodiisobutyronitriles; 100-300 mg mercaptopropyltriethoxysilane, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
Embodiment 1: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 100ml round-bottomed flask that reflux condensing tube is housed, add 100mg APTCPP successively; 100 mg azodiisobutyronitriles; 100 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
Embodiment 2: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 300ml round-bottomed flask that reflux condensing tube is housed, add 300mg APTCPP successively; 100 mg azodiisobutyronitriles; 300 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
Embodiment 2: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 200ml round-bottomed flask that reflux condensing tube is housed, add 200mgAPTCPP successively; 100 mg azodiisobutyronitriles; 200 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
Embodiment 3: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 150ml round-bottomed flask that reflux condensing tube is housed, add 150mg APTCPP successively; 100 mg azodiisobutyronitriles; 150 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
Embodiment 4: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 250ml round-bottomed flask that reflux condensing tube is housed, add 250mg APTCPP successively; 100 mg azodiisobutyronitriles; 250 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
Embodiment 5: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 222ml round-bottomed flask that reflux condensing tube is housed, add 222mg APTCPP successively; 100 mg azodiisobutyronitriles; 222 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
Embodiment 6: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 111ml round-bottomed flask that reflux condensing tube is housed, add 111mg APTCPP successively; 100 mg azodiisobutyronitriles; 111 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
Embodiment 7: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 123ml round-bottomed flask that reflux condensing tube is housed, add 123mg APTCPP successively; 100 mg azodiisobutyronitriles; 123 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
Claims (8)
1. the TiO of porphyrin sensitization
2the synthetic method of complex microsphere; it is characterized in that: in the 100-300ml round-bottomed flask that reflux condensing tube is housed, add 100-300mg APTCPP successively; 100 mg azodiisobutyronitriles; 100-300 mg mercaptopropyltriethoxysilane, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
2. the TiO of porphyrin sensitization according to claim 1
2the synthetic method of complex microsphere; it is characterized in that: in the 100ml round-bottomed flask that reflux condensing tube is housed, add 100mg APTCPP successively; 100 mg azodiisobutyronitriles; 100 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
3. the TiO of porphyrin sensitization according to claim 1
2the synthetic method of complex microsphere; it is characterized in that: in the 300ml round-bottomed flask that reflux condensing tube is housed, add 300mg APTCPP successively; 100 mg azodiisobutyronitriles; 300 mg mercaptopropyltriethoxysilanes, and 30ml toluene, under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards, is cooled to room temperature, obtains the TiO of porphyrin sensitization after pressure reducing and steaming toluene
2complex microsphere.
4. the TiO of porphyrin sensitization according to claim 1
2the synthetic method of complex microsphere; it is characterized in that: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 200ml round-bottomed flask that reflux condensing tube is housed, add 200mgAPTCPP successively; 100 mg azodiisobutyronitriles; 200 mg mercaptopropyltriethoxysilanes; with 30ml toluene; under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards; be cooled to room temperature, after pressure reducing and steaming toluene, obtain the TiO of porphyrin sensitization
2complex microsphere.
5. the TiO of porphyrin sensitization according to claim 1
2the synthetic method of complex microsphere; it is characterized in that: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 150ml round-bottomed flask that reflux condensing tube is housed, add 150mg APTCPP successively; 100 mg azodiisobutyronitriles; 150 mg mercaptopropyltriethoxysilanes; with 30ml toluene; under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards; be cooled to room temperature, after pressure reducing and steaming toluene, obtain the TiO of porphyrin sensitization
2complex microsphere.
6. the TiO of porphyrin sensitization according to claim 1
2the synthetic method of complex microsphere; it is characterized in that: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 250ml round-bottomed flask that reflux condensing tube is housed, add 250mg APTCPP successively; 100 mg azodiisobutyronitriles; 250 mg mercaptopropyltriethoxysilanes; with 30ml toluene; under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards; be cooled to room temperature, after pressure reducing and steaming toluene, obtain the TiO of porphyrin sensitization
2complex microsphere.
7. the TiO of porphyrin sensitization according to claim 1
2the synthetic method of complex microsphere; it is characterized in that: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 222ml round-bottomed flask that reflux condensing tube is housed, add 222mg APTCPP successively; 100 mg azodiisobutyronitriles; 222 mg mercaptopropyltriethoxysilanes; with 30ml toluene; under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards; be cooled to room temperature, after pressure reducing and steaming toluene, obtain the TiO of porphyrin sensitization
2complex microsphere.
8. the TiO of porphyrin sensitization according to claim 1
2the synthetic method of complex microsphere; it is characterized in that: the synthetic method of APTCPP of the present invention; it is characterized in that: in the 111ml round-bottomed flask that reflux condensing tube is housed, add 111mg APTCPP successively; 100 mg azodiisobutyronitriles; 111 mg mercaptopropyltriethoxysilanes; with 30ml toluene; under nitrogen protection in 80 DEG C of stirring in water bath reactions; TLC detection reaction process; question response stops heating completely afterwards; be cooled to room temperature, after pressure reducing and steaming toluene, obtain the TiO of porphyrin sensitization
2complex microsphere.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107899618A (en) * | 2017-10-23 | 2018-04-13 | 中山大学 | A kind of hybrid material based on macrocyclic compound light-sensitive coloring agent and titanium dioxide and preparation method thereof and the application in photocatalysis |
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- 2013-11-18 CN CN201310575806.9A patent/CN104646063A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107899618A (en) * | 2017-10-23 | 2018-04-13 | 中山大学 | A kind of hybrid material based on macrocyclic compound light-sensitive coloring agent and titanium dioxide and preparation method thereof and the application in photocatalysis |
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