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Method for synthesizing phosphonic acid modified graphene or phosphonate modified graphene

A graphene and phosphonate technology, applied in the field of synthesizing phosphonic acid-modified graphene or phosphonate-modified graphene, can solve the problems of immature method, difficult realization, low hydrophilicity of graphene, etc., and easy to achieve. Separation, improving product stability, and the effect of high product yield

Active Publication Date: 2018-09-25
XINXIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are doping modification methods and chemical reactive modification methods, but the hydrophilicity of graphene is not high, and the methods of phosphonic acid modified graphene or phosphonate modified graphene are not mature enough, especially for stably connecting phosphorus to The modification method of the sheet layer is difficult to realize

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] In a 500 mL round bottom flask, add diethyl aminomethylphosphonate (16.7 g, 0.10 moL), sodium nitrite (7.25 g, 0.11 moL) and sulfuric acid (32.3 g, 0.33 moL). Ice-salt bath, control the reaction below 0 degrees Celsius and stir for about 60 minutes. Graphene (30 g) was added, and the reaction was carried out under temperature control for 30 minutes, and then returned to room temperature naturally. Filter to obtain diethyl phosphonate modified graphene A1 with a yield of 80%. Aminomethylphosphonic acid diethyl ester modified graphene reacts in aqueous sodium hydroxide solution, heats to 80 degrees Celsius, reacts for 300 minutes, adjusts acidity with hydrochloric acid, reaches pH=3, filters to obtain phosphonic acid modified graphene B1, The yield is 70%.

Embodiment 2

[0018] In a 500 mL round bottom flask, add diphenyl aminomethylphosphonate (26.3 g, 0.10 moL), sodium nitrite (7.25 g, 0.11 moL) and sulfuric acid (32.3 g, 0.33 moL). Ice-salt bath, control the reaction below 0 degrees Celsius and stir for about 60 minutes. Graphene (8 g) was added, and the reaction was carried out under temperature control for 240 minutes, and then returned to room temperature naturally. Filter to obtain diphenyl phosphonate modified graphene A2 with a yield of 82%. Diphenyl phosphonic acid modified graphene was reacted in aqueous sodium hydroxide solution, heated to 80 degrees Celsius, reacted for 300 minutes, adjusted the acidity with hydrochloric acid to reach pH = 3, and filtered to obtain phosphonic acid modified graphene B2 with a yield of 71 % .

Embodiment 3

[0020] In a 500mL round bottom bottle, add O,O-diphenyl-2-phenyl-aminomethylphosphonate (NH 2 CH(Ph)PO(OPh) 2 ) (33.9g, 0.10 moL) and tetrahydrofuran (20mL), sodium nitrite (7.25g, 0.11 moL) and sulfuric acid (32.3g, 0.33moL). Ice-salt bath, control the reaction below 0 degrees Celsius and stir for about 60 minutes. Graphene oxide (4 g) was added, and the reaction was carried out under temperature control for 240 minutes, and then returned to room temperature naturally. Filter to obtain diphenyl phosphonate modified graphene A3 with a yield of 78%. Diphenyl phosphonate modified graphene, react in aqueous sodium hydroxide solution, heat to 80 degrees Celsius, react for 300 minutes, adjust acidity with hydrochloric acid, reach pH=4, filter to obtain phosphonic acid modified graphene B3, yield 76%.

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PUM

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Abstract

The invention discloses a method for synthesizing phosphonic acid modified graphene or phosphonate modified graphene and belongs to the field of inorganic novel materials. The method comprises the following steps: firstly, dissolving amino phosphonate in a solvent and controlling the temperature; adding sodium nitrite and acid and uniformly stirring; then adding the graphene and reacting; filtering and washing to obtain the phosphonate modified graphene; mixing the phosphonate modified graphene, sodium hydroxide and water, and heating to react; adjusting the acidity and filtering to obtain thephosphonic acid modified graphene. The method disclosed by the invention has the advantages of simple technological flow, mild conditions, high safety and low cost, and the stability of a product isimproved; the possibility of industrialized production of synthesizing a lot of the phosphonic acid modified graphene or the phosphonate modified graphene is realized.

Description

technical field [0001] The invention relates to a method for synthesizing phosphonic acid-modified graphene or phosphonate-modified graphene, belonging to the field of new inorganic materials. Background technique [0002] Graphene is a new type of carbon material with a variety of excellent properties, such as extraordinary electrical conductivity, strength dozens of times stronger than steel, and good light transmission. It will be widely used in the future. Graphene has a large theoretical specific surface area and can easily become a good adsorbent. Recently, the introduction of carboxyl groups, amine groups, sulfonic acid groups, etc. on graphene sheets to improve its adsorption and selectivity has become a hot spot. [0003] With the continuous development of my country's science and technology, the demand for high-quality rare earth elements continues to increase. Phosphate ester extractants have good application prospects in the field of rare earth enrichment a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/40B01J20/22B01J20/30
CPCB01J20/205B01J20/22C07F9/4006C07F9/4075C07F9/4084
Inventor 王储备马新凤马月辉周建伟李晓光苏新梅黄建新
Owner XINXIANG UNIV
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