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Synthesis method of 3-aminopropyltriethoxysilane modified graphene oxide

A technology of aminopropyltriethoxysilane and its synthesis method, which is applied in the fields of chemical instruments and methods, carbon compounds, inorganic chemistry, etc., and can solve the problem of high aggregate hardness, difficult grinding, and no graphene oxide electron microscope diagram, etc. problem, achieve the effect of lowering the reaction temperature and shortening the reaction time

Pending Publication Date: 2020-11-27
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, after the 3-aminopropyltriethoxysilane modified graphene oxide prepared by this method is reduced and dried with hydrazine hydrate, the corresponding modified graphene obtained in organic solvents (such as DMF, ethanol and acetone, etc.) It cannot be dispersed ultrasonically, and the aggregates after drying are very hard and difficult to grind, which is not conducive to subsequent use, and this method does not give the electron microscope images of graphene oxide and reduced graphene

Method used

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  • Synthesis method of 3-aminopropyltriethoxysilane modified graphene oxide
  • Synthesis method of 3-aminopropyltriethoxysilane modified graphene oxide
  • Synthesis method of 3-aminopropyltriethoxysilane modified graphene oxide

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Embodiment 1

[0024] Synthesis of 3-Aminopropyltriethoxysilane Modified Graphene Oxide

[0025] Add 20mg of graphene oxide into 35.6g of tetrahydrofuran, ultrasonically disperse at 25°C for 1.5h, and then add 3.76*10 -3 mg 3-aminopropyltriethoxysilane, reacted at 70°C for 8.0h, centrifuged, washed, and dried to obtain 30 mg of black powder 3-aminopropyltriethoxysilane-modified graphene oxide.

[0026] Structure Identification:

[0027] 1. Infrared analysis

[0028] In the infrared spectrum of the target compound 3-aminopropyltriethoxysilane modified graphene oxide, it can be seen that the 1740cm -1 The carbonyl stretching vibration absorption peak at has moved to 1636cm -1 , corresponding to 1248cm in graphite oxide -1 The characteristic absorption peak of the epoxy group becomes very weak or even disappears, indicating that some of the amino groups in 3-aminopropyltriethoxysilane have undergone an addition reaction with the epoxy groups in graphite oxide. Modified graphite oxide at 10...

Embodiment 2

[0038] Synthesis of 3-Aminopropyltriethoxysilane Modified Graphene Oxide

[0039] Add 40mg of graphene oxide into 100g of tetrahydrofuran, ultrasonically disperse at 25°C for 1h, and then add 9*10 -3mg3-aminopropyltriethoxysilane was reacted at 60°C for 7.0h, centrifuged, washed, and dried to obtain 58 mg of black powder 3-aminopropyltriethoxysilane-modified graphene oxide.

[0040] Reduction of Graphene Oxide Modified by 3-Aminopropyltriethoxysilane

[0041] Disperse 20 mg of 3-aminopropyltriethoxysilane-modified graphene oxide after washing and drying in 40 mL of tetrahydrofuran, after ultrasonication for 0.5 h, add 0.5 g of hydrazine hydrate, and reduce at 70 ° C for 6 h; The resulting product was washed with ethanol and distilled water, and dried to obtain 3-aminopropyltriethoxysilane-modified graphene. Weigh 10 mg of dried 3-aminopropyltriethoxysilane-modified graphene, disperse them in DMF, DMSO, ethanol, THF, and acetone respectively, and obtain a stable dispersion af...

Embodiment 3

[0043] Synthesis of 3-Aminopropyltriethoxysilane Modified Graphene Oxide

[0044] Add 60mg of graphene oxide into 140g of tetrahydrofuran, ultrasonically disperse at 30°C for 2h, then add 1.00*10 -2 mg 3-aminopropyltriethoxysilane, reacted at 65°C for 7h, centrifuged, washed, and dried to obtain 85 mg of black powder 3-aminopropyltriethoxysilane-modified graphene oxide.

[0045] Reduction of Graphene Oxide Modified by 3-Aminopropyltriethoxysilane

[0046] Disperse 20 mg of 3-aminopropyltriethoxysilane-modified graphene oxide after washing and drying in 40 mL of tetrahydrofuran, after ultrasonication for 0.5 h, add 0.5 g of hydrazine hydrate, and reduce at 70 ° C for 6 h; The resulting product was washed with ethanol and distilled water, and dried to obtain 3-aminopropyltriethoxysilane-modified graphene. Weigh 10 mg of dried 3-aminopropyltriethoxysilane-modified graphene, disperse them in DMF, DMSO, ethanol, THF, and acetone respectively, and obtain a stable dispersion after ...

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Abstract

The invention discloses a synthesis method of 3-aminopropyltriethoxysilane modified graphene oxide. The preparation method comprises the following steps: adding graphene oxide into tetrahydrofuran, wherein the dosage ratio of the graphene oxide to the tetrahydrofuran is 20-100mg: 35.6g-222.5g; carrying out ultrasonic dispersion for 1-2 hours in a temperature range of 20-35 DEG C; then, adding 3-aminopropyltriethoxysilane, wherein the dosage ratio of the graphene oxide to the tetrahydrofuran to the 3-aminopropyltriethoxysilane is 20-100mg: 35.6g-222.5g: 3.76*10<-3>mg-2.82*10<-2> mg; and carrying out stirring and reaction for 6-8 h at a temperature of 60-70 DEG C, and carrying out centrifugation, washing and drying to obtain black powder 3-aminopropyltriethoxysilane modified graphene oxide.

Description

technical field [0001] The invention belongs to the field of organic synthesis, and in particular relates to a synthesis method of 3-aminopropyltriethoxysilane-modified graphene oxide. Background technique [0002] Graphene oxide is an important graphene derivative, which has unique applications in the field of composite materials. There are a large number of oxygen-containing groups on its surface, such as hydroxyl, carboxyl, epoxy, etc., which can be functionalized on the surface of graphene oxide by covalent or non-covalent methods to obtain functionalized graphene oxide. The final modified graphene oxide can form an interaction force with rubber, polyvinyl alcohol, chitosan and other polymers to modify the properties of polymer materials, and can also interact with nano-metal oxides for solar cells. [0003] 3-Aminopropyltriethoxysilane is an important siloxane compound. The alkoxy groups in the molecule can react with the functional groups on the surface of graphene ox...

Claims

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Application Information

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IPC IPC(8): C01B32/198
CPCC01B32/198
Inventor 陆婷婷汪营磊高福磊刘英哲陈斌刘亚静丁峰
Owner XIAN MODERN CHEM RES INST