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Preparation method for upconversion graphene oxide and application in indicating pH of water sample

A graphene and graphene solution technology, applied in chemical instruments and methods, measuring devices, material analysis through optical means, etc., to achieve the effects of small size, high yield, and good water solubility

Inactive Publication Date: 2015-01-21
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the random distribution of sp3 regions and sp2 regions in the sheet, GO exhibits peculiar electrical and optical properties, and is considered to be a functionalized graphene material. Has important theoretical research and application value. At present, all research on graphene composite materials is in its infancy, and opportunities and challenges coexist.

Method used

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  • Preparation method for upconversion graphene oxide and application in indicating pH of water sample
  • Preparation method for upconversion graphene oxide and application in indicating pH of water sample
  • Preparation method for upconversion graphene oxide and application in indicating pH of water sample

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Experimental program
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Effect test

Embodiment 1

[0029] (1) Pre-oxidation process of graphite: add 1.5 g of graphite flakes into a 250 mL three-neck flask, then add 6 mL of concentrated sulfuric acid, 1.2 g of Na 2 S 2 o 8 and 1.25 g P 2 o 5 , stirred at 80°C for 4.5 h, cooled to room temperature, added 250 mL of high-purity water, and left overnight. Centrifuge to neutral, dry in vacuum at 35°C to obtain solid pre-oxidized graphite;

[0030] (2) Preparation of graphene oxide: Add 20 mL of concentrated sulfuric acid to a three-neck flask containing 0.5 g of pre-oxidized graphite flakes at 0 °C, and slowly add 2.5 g of KMnO 4 , raised the temperature to 35°C, stirred for 4 h, then slowly added 45 mL of high-purity water and stirred for another 2 h, then added 120 mL of high-purity water and 4 mL of H 2 o 2 , washed with 1 L of 1:10 HCl, centrifuged, then washed with high-purity water, centrifuged to neutral, and the obtained solution was ultrasonicated to form a graphene oxide solution for subsequent use;

[0031] (3) ...

Embodiment 2

[0035] (1) Pre-oxidation process of graphite: add 1.5 g of graphite flakes into a 250 mL three-neck flask, then add 6 mL of concentrated sulfuric acid, 1.2 g of Na 2 S 2 o 8 and 1.25 g P 2 o 5 , stirred at 50°C for 4.5 h, cooled to room temperature, added 250 mL of high-purity water, and left overnight. Centrifuge to neutral, dry in vacuum at 35°C to obtain solid pre-oxidized graphite;

[0036] (2) Preparation of graphene oxide: Add 12 mL of concentrated sulfuric acid to a three-neck flask containing 0.5 g of pre-oxidized graphite flakes at 0 °C, and slowly add 2.5 g of KMnO 4 , raised the temperature to 35°C, stirred for 2 h, then slowly added 45 mL of high-purity water and stirred for another 2 h, then added 120 mL of high-purity water and 4 mL of H 2 o 2 , washed with 1L of 1:10 HCl, centrifuged, then washed with high-purity water, centrifuged to neutral, and the obtained solution was ultrasonicated to form a graphene oxide solution for subsequent use;

[0037] (3) T...

Embodiment 3

[0041] A preparation method of graphene oxide with up-conversion properties, characterized in that it proceeds in the following steps:

[0042] (1) The pre-oxidation process of graphite: add 1.5 g of graphite flakes into the three-neck flask, then add 6 mL of concentrated sulfuric acid, 1.2 g of Na 2 S 2 o 8 and 1.25 g P 2 o 5 , stirred at 65°C for 4.5 h, cooled to room temperature, added 250 mL of high-purity water, and stood overnight; centrifuged to neutral, and dried under vacuum at 35°C to obtain solid pre-oxidized graphite;

[0043] (2) Preparation of graphene oxide: Add 16 mL of concentrated sulfuric acid to a three-neck flask containing 0.5 g of pre-oxidized graphite flakes at 0 °C, and slowly add 2.5 g of KMnO 4 , raised the temperature to 35°C, stirred for 3 h, then slowly added 45 mL of high-purity water and stirred for another 2 h, then added 120 mL of high-purity water and 4 mL of H 2 o 2 , washed with 1 L of 1:10 HCl, centrifuged, washed with high-purity wa...

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Abstract

The invention discloses a preparation method for graphene oxide with upconversion properties, good water solubility and high yield, and the graphene oxide synthesized by the method can be successfully used for indicating the pH change of a solution. In recent years, due to a unique two-dimensional structure, optical and electrical properties, and wide potential use, graphene oxide reduced grapheme and other graphene materials attract great attention from people. Especially along with the discovery of graphene oxide electroluminescence and photoluminescence phenomena, graphene oxide shows potential application in cell imaging, drug delivery and other biological nanotechnology fields. However, application of graphene oxide's upconversion luminescence properties attracts little attention. Thus, as a near-infrared probe, the graphene oxide with upconversion properties prepared by the method provided by the invention can have good application prospects in detection and imaging of solutions or water samples and the like.

Description

[0001] This invention was supported by the National Natural Science Foundation of China (funding number: 21375095); the national special funding for excellent doctoral dissertation authors (funding number: FANEDD-201023); the key project of Tianjin Applied Basic Research Program (funding number: 12JCZDJC21700); Tianjin University Supported by the "Cultivation Program for Young and Middle-aged Backbone Innovative Talents" (funding number: ZX110GG015); Tianjin University Innovation Team Training Program (funding number: TD12-5038). technical field [0002] The invention belongs to the field of preparation of fluorescent probe nanomaterials, in particular to a method for preparing graphene oxide with good water solubility, high yield and up-conversion properties, which is mainly used to indicate pH changes in solutions. Background technique [0003] Graphene oxide (GO) has a freely dispersed two-dimensional structure and abundant polar groups, which makes it show outstanding ad...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B31/04G01N21/359C09K11/65
Inventor 李妍靳晴王鲁胡悦立孙玉秀刘炳毅邵可然谷悦邬浩
Owner TIANJIN NORMAL UNIVERSITY
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