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Glutamic acid derivative and preparation method and multi-scale pore structure tio 2 Preparation method of crystalline airgel

A technology of derivatives and glutamic acid is applied in the field of preparation of TiO2 crystalline airgel with multi-scale pore structure, which can solve problems such as difficult to reuse, slow mass transfer process, and easy condensation. The method is simple and easy, The effect of simple preparation method and mild reaction conditions

Active Publication Date: 2019-08-20
SHAANXI NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Dispersed Nano TiO 2 There are disadvantages such as difficulty in separation, easy aggregation, and difficulty in recycling; supported nano-TiO 2 And because of the slow mass transfer process, the utilization rate of effective nanoparticles is low, which greatly weakens the advantages of large specific surface area of ​​nanoparticles, so the preparation of nano-TiO with novel pore structure 2 Porous blocks become an effective way to solve the above problems

Method used

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  • Glutamic acid derivative and preparation method and multi-scale pore structure tio <sub>2</sub> Preparation method of crystalline airgel
  • Glutamic acid derivative and preparation method and multi-scale pore structure tio <sub>2</sub> Preparation method of crystalline airgel
  • Glutamic acid derivative and preparation method and multi-scale pore structure tio <sub>2</sub> Preparation method of crystalline airgel

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 1. Synthesis of compounds of formula Ⅰ-1

[0048]12.4g (49.97mmol) Boc-L-glutamic acid, 38.43g (200.61mmol) 1-ethyl-(3-dimethylaminopropyl) carbodiimide hydrochloride, 0.42g (3.34mmol) 4-Dimethylaminopyridine was dissolved in 200mL of dichloromethane, and 18.54g (100.02mmol) of n-dodecylamine was added under ice bath conditions, and the ice bath was removed after stirring for 30 minutes, and the reaction was stirred and reacted at normal temperature for 24 hours, and the reaction The solution was washed with 0.1 mol / L NaOH aqueous solution, 0.1 mol / L HCl aqueous solution and distilled water successively, and the organic phase was washed with anhydrous NaOH 2 SO 4 After drying, the solvent was evaporated under reduced pressure, and the obtained crude product was separated and purified by column chromatography with chloroform and methanol in a volume ratio of 20:1 as a mobile phase and silica gel as a stationary phase to obtain the compound of formula Ⅰ-1 (white Solid 2...

Embodiment 2

[0072] Dissolve 0.076g of the glutamic acid derivative of Example 1 in 3mL of benzyl alcohol, and slowly add 0.15mL of TiCl dropwise under nitrogen protection and -15°C 4 And keep stirring, the solution turns reddish brown, after the dropwise addition, seal and age at 80°C for 3 days, then place it in a centrifuge tube, repeat centrifugation with acetone (10mL×7 times), add 100 μL of benzene, and Centrifuge at 1000r / min for 5min, freeze-dry the solid, and anneal at 450°C for 30min to obtain TiO 2 Crystalline airgel.

[0073] The obtained samples were characterized by X-ray diffractometer, scanning electron microscope and transmission electron microscope, the results are shown in Figure 1~4 . Depend on figure 1 It can be seen that the obtained sample is anatase TiO 2 . Depend on Figure 2~4 It can be seen that the anatase TiO 2 Crystalline aerogels have three-dimensional continuous micron-scale and nano-scale channels, wherein the size of the micro-channels is about 25 ...

Embodiment 3

[0075] In this example, after adding 100 μL of benzene, it was centrifuged at 2000 r / min for 5 minutes, and other steps were the same as in Example 2 to obtain TiO 2 Crystalline airgel. Depend on Figure 5 It can be seen that the obtained TiO 2 The crystalline airgel has three-dimensional continuous micron-scale and nano-scale channels, wherein the size of the micro-channel is about 20 μm, and the size of the nano-channel is 1-10 nm.

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Abstract

The invention discloses a glutamic acid derivative and its preparation method and multi-scale pore structure TiO 2 Preparation method of crystalline aerogel. The structural formula of this derivative is In the formula, n is an integer from 7 to 13, and m=0, 1 or 2. It has self-assembly properties, a simple preparation method, and mild reaction conditions. In the present invention, the compound is first covalently grafted to TiO 2 On the surface of the nanoparticles, anatase TiO with three-dimensional continuous micron-scale and nanopores is prepared by centrifugal concentration, freeze-drying and annealing. 2 Crystalline aerogel, and the pore size can be controlled by adjusting the centrifugal speed. This crystalline aerogel can be used for photocatalytic degradation of formaldehyde gas.

Description

technical field [0001] The invention belongs to the technical field of preparation of nanomaterials, in particular to a glutamic acid derivative with self-assembly function and a preparation method thereof, and the preparation of TiO with a multi-scale pore structure by using the glutamic acid derivative 2 A method for crystalline aerogels. Background technique [0002] Nano titanium dioxide (TiO 2 ) is an n-type semiconductor with a forbidden band width of 3.2 eV, which corresponds to the energy of photons with a wavelength of 387.5 nm. When the wavelength is less than 387.5nm biophoton irradiates TiO 2 When on the surface of the valence band, the electrons in the valence band are excited to the conduction band, thereby generating highly active photo-generated electrons (e - ) and photogenerated holes (h + ), under the action of an electric field, the negatively charged photogenerated electrons (e - ) and positively charged photogenerated holes (h + ) to separate and ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D249/04B01J31/38B01J21/06
CPCC07D249/04B01J21/063B01J31/0244B01J31/0271B01J31/38B01J35/23
Inventor 严军林杨颖超刘静
Owner SHAANXI NORMAL UNIV
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