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Intelligent mesoscopic structure material heterogeneous interface modification compound and functional regulation and control and preparation method thereof

A technology of structural materials and heterogeneous interfaces, which is applied in chemical instruments and methods, luminescent materials, etc., can solve the problems of low performance tunability and monotonous functions, and achieve the effects of simple synthesis method, improved mechanical properties, and easy process control.

Pending Publication Date: 2020-06-26
NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to overcome the technical defects of porous materials such as monotonous function and low performance adjustability, the present invention provides a heterogeneous interface modification compound of intelligent mesoscopic structure material, functional regulation and its preparation method, aiming at interfacial modification of mesoporous silica materials. Modification to realize the optical performance regulation of the silica porous material

Method used

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  • Intelligent mesoscopic structure material heterogeneous interface modification compound and functional regulation and control and preparation method thereof
  • Intelligent mesoscopic structure material heterogeneous interface modification compound and functional regulation and control and preparation method thereof
  • Intelligent mesoscopic structure material heterogeneous interface modification compound and functional regulation and control and preparation method thereof

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Such as figure 1 Shown:

[0035] Intermediate 2a: Add 4,4'-diaminobenzophenone (0.85g, 4.0mmol) into 35mL of concentrated hydrochloric acid, stir well, add 3.3g (28.0mmol) tin particles, and then slowly heat to reflux temperature . The reaction was stirred at reflux for 24 hours. After the reaction was completed, it was cooled to room temperature, an off-white solid was obtained by suction filtration under reduced pressure, and washed three times with deionized water to obtain 0.53 g of an intermediate product with a yield of 62%. 1H NMR (600MHz, DMSO-d6, δ) 7.10 (2H, ArH), 7.07 (2H, ArH), 3.85 (2H, NH2); 13C NMR (75MHz, DMSO-d6, δ) 121.49, 132.39, 137.10, 132.79 , 139.59, 140.70.

[0036] Organic molecule 3a: Under nitrogen protection, intermediate 2a (0.39g, 1.0mmol) and 3-isocyanatopropyltriethoxysilane (1.08g, 4.4mmol) were added to a dry 100mL three-necked flask, and Add 50 mL of dry anhydrous tetrahydrofuran, stir to dissolve and heat to reflux. After comple...

Embodiment 2

[0038] Such as figure 2 Shown:

[0039] Intermediate 2a: Add 4,4'-diaminobenzophenone (0.85g, 4.0mmol) into 50mL of concentrated hydrochloric acid, stir well, add 3.3g (28.0mmol) tin particles, and then slowly heat to reflux temperature . The reaction was stirred at reflux for 24 hours. After the reaction was completed, it was cooled to room temperature, an off-white solid was obtained by suction filtration under reduced pressure, and washed three times with deionized water to obtain 0.60 g of an intermediate product with a yield of 71%. 1H NMR (600MHz, DMSO-d6, δ) 7.10 (2H, ArH), 7.07 (2H, ArH), 3.85 (2H, NH2); 13C NMR (75MHz, DMSO-d6, δ) 121.49, 132.39, 137.10, 132.79 , 139.59, 140.70.

[0040]Organic molecule 3a: under nitrogen protection, intermediate 2a (0.39g, 1.0mmol) and 3-isocyanatopropyltriethoxysilane (1.19g, 4.8mmol) were added to a dry 100mL three-necked flask, and Add 50 mL of dry anhydrous tetrahydrofuran, stir to dissolve and heat to reflux. After comple...

Embodiment 3

[0042] CTAB (200 mg) and sodium hydroxide (700 μL, 2M) were dissolved in 100 mL of deionized water, heated to 80° C. and stirred for 30 minutes. Then 1 mL of TEOS was added to the above CTAB aqueous solution, and the mixed solution was stirred at 80° C. for 1 hour, then cooled to room temperature, and filtered by suction to obtain an inorganic mesoporous silica material. The template agent CTAB was removed by Soxhlet extraction with methanol for 48 hours.

[0043] 100 mg of organic molecules 3a were accurately weighed and dissolved in 10 mL of ethanol solution, 0.1 g of inorganic silica material was added to the ethanol solution, dispersed evenly by ultrasonication for 10 minutes, and stirred at room temperature for 4 hours. The organic-inorganic mesoporous silica material whose interface is modified by mailing molecule 3a is obtained by suction filtration. This material has good fluorescence performance and can emit strong fluorescence in solid state.

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Abstract

The invention discloses an intelligent mesoscopic structure material heterogeneous interface modification compound and a functional regulation and control and preparation method thereof. A main body of the compound is tetraphenyl ethylene, and the periphery of the compound is hydrolysable siloxane. The preparation method comprises the steps that 4,4'-diaminobenzophenone 1a serves as a raw materialto synthesize tetraamino tetraphenyl ethylene 2a through tin particle catalysis, then the tetraamino tetraphenyl ethylene 2a reacts with 3-isocyanatopropyltriethoxysilane to obtain an organic molecule 3a with the aggregation-induced fluorescence effect and a material interface modification function. By modifying the inorganic mesoporous interface with the 3a, a fluorescent porous material with high luminous efficiency can be obtained. The organic fluorescent molecules provided by the invention have covalent interaction with the porous material, and interface modification and optical propertyregulation and control of the porous material are realized on the premise of not destroying the porous property of the porous material.

Description

technical field [0001] The invention belongs to the field of organic-inorganic hybrid materials, and in particular relates to an intelligent mesostructure material heterogeneous interface modification compound, functional regulation and a preparation method thereof. Background technique [0002] Porous materials have excellent pore structure, large specific surface area, and good mechanical properties, which make them have broad application prospects in many fields such as identification and separation, catalytic synthesis, military engineering, and biotechnology. Inorganic porous materials are mainly composed of skeletons and channels, but because these pure inorganic materials do not have active centers, the further application of materials is limited. In order to expand the application of porous materials in different fields, it is often necessary to functionalize the materials to introduce various active components, such as metal heteroatoms and oxides, heteropolyacids, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K11/06
CPCC09K11/06C09K2211/1007
Inventor 高萌刘家庆李勇梁秀
Owner NEW MATERIAL INST OF SHANDONG ACADEMY OF SCI
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