CN105107462A - Preparation method for oxidized graphene-metal organic framework nano composite material - Google Patents
Preparation method for oxidized graphene-metal organic framework nano composite material Download PDFInfo
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- CN105107462A CN105107462A CN201510446454.6A CN201510446454A CN105107462A CN 105107462 A CN105107462 A CN 105107462A CN 201510446454 A CN201510446454 A CN 201510446454A CN 105107462 A CN105107462 A CN 105107462A
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Abstract
Provided is a preparation method for an oxidized graphene-metal organic framework nano composite material. Dopamine hydrochloride, oxidized graphene and a Tris buffer solution are employed to prepare GO@PDA, and then GO@PDA, 1,3,5-trimesic acid, copper acetate monohydrate, N,N-dimethyl formamide, ethanol, deionized water and triethylamine are employed to prepare GO@PDA@MOF-199. The operation is simple, the cost is low, the particle diameters of the prepared GO@PDA@MOF-199 nano composite material are in a nano level, particles are uniform, the dispersibility is good, and the adsorption capability is strong. No environmental pollution can be caused during preparation, and the preparation method is harmless to health of operation personnel.
Description
Technical field
The present invention relates to a kind of preparation method of metallic organic framework composite, particularly a kind of preparation method of the graphene oxide-metallic organic framework nano composite material (GOPDAMOF-199) through Dopamine hydrochloride modification.
Background technology
The synthetic method of metal-organic framework materials has a lot, and common method has hydro-thermal method, diffusion method, microwave assisting method, stirring at room temperature method, ultrasonic wave added method etc.
(1) hydro-thermal method
Hydro-thermal method (also known as hydrothermal method) refers to water to be solvent, under airtight condition, by HTHP, reactant is reacted, and cultivates a kind of method of crystal.Till now, the reactive mode of hydro-thermal method and be not only confined to take water as solvent, may some or all of organic solvent, i.e. said hot solvent method when reacting.The crystallization reaction occurred under hydro-thermal method condition, thermal stress is little, and the crystal of synthesis has good crystal face, and internal flaw is few.Therefore, the general hydro-thermal method that adopts prepares metal-organic framework materials.
(2) diffusion method
Diffusion method is exactly that the material of two kinds of different shapes is contacted with each other, then can slow crystallization and generate the process of product at two kinds of material interface places.This Measures compare is gentle, easily the crystal of synthesis larger particles, but the time usually used is all long, therefore receives some restrictions in some aspects.
(3) microwave assisting method
Microwave assisting method is a kind of synthetic method being considered to transitory efficient, is exactly under the effect of high-frequency microwave usually, charged particle is clashed into mutually with very high speed, then generates the process of product.Because micro-wave frequency is very high, therefore General reactions is all occur in moment, and thermograde is very low, and selectively can heat reactant, and capacity usage ratio is very high.
(4) stirring at room temperature method
Stirring at room temperature method is also a kind of method of Fast back-projection algorithm metal-organic framework materials, and it is easy to operate, as long as equipment simple by reactants dissolved in specific solvent, under the condition of room temperature or heating, certainly can also add the carrying out that proton-removed agent carrys out accelerated reaction in system.
Summary of the invention
Object of the present invention, is to provide the preparation method of a kind of graphene oxide-metallic organic framework nano composite material (GOPDAMOF-199).Graphene oxide-metallic organic framework the nano composite material (GOPDAMOF-199) of modifying through Dopamine hydrochloride can be prepared by this method, and composite particle diameter is in Nano grade, uniform particles, and absorbent properties are good.
The technical scheme adopted:
A preparation method for graphene oxide-metallic organic framework nano composite material, comprises the following steps:
The preparation of the first step: GOPDA:
(1) get Dopamine hydrochloride, graphene oxide and three (methylol) aminomethane, the mass ratio of Dopamine hydrochloride, graphene oxide and three (methylol) aminomethane is 2:1:6.1, for subsequent use;
(2) according to the Tris cushioning liquid of the quality preparation pH=8.5 of above-mentioned three (methylol) aminomethane, for subsequent use;
(3) mix Dopamine hydrochloride, graphene oxide and Tris cushioning liquid, mixture ultrasonic wave dispersion (20kz, 10min), carries out the magnetic agitation of 24 hours after being uniformly dispersed, and after product being spent deionized water suction filtration, dries, obtains GOPDA, for subsequent use;
The preparation of second step: GOPDAMOF-199:
(1), get the raw materials ready:
The mass ratio of the equal benzoic acid of 1,3,5-, a hydration Schweinfurt green and GOPDA is 5:8.6:3, and the volume ratio of DMF, ethanol, deionized water and triethylamine is 80:80:120:1; Wherein the mass ratio of 1,3,5-equal benzoic acid and DMF is 1:64,
(2), first equal for 1,3,5-benzoic acid solution is dissolved in DMF and alcohol mixed solution, then a GOPDA hydration Schweinfurt green and step 1 prepared respectively is soluble in water, finally by three kinds of solution mixing;
(3), in mixed solution add triethylamine, at room temperature stir 3 hours;
(4), stir terminate after, washed by product DMF, suction filtration post-drying, to obtain final product.
Its advantage is:
The present invention is simple to operate, and cost is low, and prepared GOPDAMOF-199 nano composite material particle diameter is in Nano grade, uniform particles, good dispersion, high adsorption capacity.Can not environmental pollution be caused when preparation, harmless to the health of operating personnel.
Detailed description of the invention
Embodiment one
A preparation method for graphene oxide-metallic organic framework nano composite material, comprises the following steps:
The preparation of the first step: GOPDA:
First, 20mg Dopamine hydrochloride is dissolved in 10mLTris cushioning liquid, adds 10mg graphene oxide (GO) after dissolving, carry out ultrasonic disperse, the continuous room temperature magnetic agitation of lower 24 hours after being uniformly dispersed.Stirring terminates rear deionized water and thoroughly washs suction filtration, then dries, and the GOPDA finally collecting preparation is for subsequent use.
The preparation of second step: GOPDAMOF-199:
Equal for 1,3,5-benzoic acid 250mg is dissolved in the DMF and ethanolic solution that 40mL volume ratio is 1:1.Again by a hydration Schweinfurt green C
4h
6cuO
4h
2gOPDA prepared by O430mg and step one is dissolved in the water of 30mL.After being mixed by solution, in mixed liquor, add 0.25mL triethylamine, stirred at ambient temperature 3 hours.Stirring terminates rear DMF washing reaction products therefrom, and suction filtration post-drying, to obtain final product.
Embodiment two
A preparation method for graphene oxide-metallic organic framework nano composite material, comprises the following steps:
The preparation of the first step: GOPDA:
First, 20mg Dopamine hydrochloride is dissolved in 10mLTris cushioning liquid, adds 10mg graphene oxide (GO) after fully dissolving, put into ultrasonic wave and carry out ultrasonic disperse, the continuous room temperature magnetic agitation of lower 24 hours after being uniformly dispersed.Stirring terminates rear deionized water and thoroughly washs suction filtration, then dries, and finally collects for subsequent use.
The preparation of second step: GOPDAMOF-199:
Equal for 1,3,5-benzoic acid 250mg is dissolved in the DMF and ethanolic solution that 40mL volume ratio is 1:1.Again by a hydration Schweinfurt green C
4h
6cuO
4h
2o430mg is dissolved in the water of 20mL.Then 0.15gGOPDA is dissolved in 10mL water, finally three kinds of solution is blended in mixed liquor and adds 0.25mL triethylamine, stirred at ambient temperature 3 hours.Stirring terminates rear DMF washing reaction products therefrom, and suction filtration post-drying, to obtain final product.
Claims (1)
1. a preparation method for graphene oxide-metallic organic framework nano composite material, is characterized in that comprising the following steps:
(1) get Dopamine hydrochloride, graphene oxide and three (methylol) aminomethane, the mass ratio of Dopamine hydrochloride, graphene oxide and three (methylol) aminomethane is 2:1:6.1, for subsequent use;
(2) according to the Tris cushioning liquid of the quality preparation pH=8.5 of above-mentioned three (methylol) aminomethane, for subsequent use;
(3) mix Dopamine hydrochloride, graphene oxide and Tris cushioning liquid, mixture ultrasonic wave dispersion (20kz, 10min), carries out the magnetic agitation of 24 hours after being uniformly dispersed, and after product being spent deionized water suction filtration, dries, obtains GOPDA, for subsequent use;
The preparation of second step: GOPDAMOF-199:
(1), get the raw materials ready:
The mass ratio of the equal benzoic acid of 1,3,5-, a hydration Schweinfurt green and GOPDA is 5:8.6:3, and the volume ratio of DMF, ethanol, deionized water and triethylamine is 80:80:120:1; Wherein the mass ratio of 1,3,5-equal benzoic acid and DMF is 1:64;
(2), first equal for 1,3,5-benzoic acid solution is dissolved in DMF and alcohol mixed solution, then a GOPDA hydration Schweinfurt green and step 1 prepared respectively is soluble in water, finally by three kinds of solution mixing;
(3), in mixed solution add triethylamine, at room temperature stir 3 hours;
(4), stir terminate after, washed by product DMF, suction filtration post-drying, to obtain final product.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106140094A (en) * | 2016-07-04 | 2016-11-23 | 复旦大学 | The synthetic method of the magnetic graphene composite that metallic organic framework is modified and application |
| CN106237993A (en) * | 2016-08-29 | 2016-12-21 | 沈阳理工大学 | A kind of Fe3o4the preparation method of@MOF 199@C18 nano composite material |
| CN106390932A (en) * | 2016-08-29 | 2017-02-15 | 沈阳理工大学 | Preparation method of GO@PDA@MIL-101 nano composite material |
| CN106882797A (en) * | 2017-01-15 | 2017-06-23 | 复旦大学 | A kind of grapheme material of covalent organic frame modification and its synthetic method and application |
| CN108176254A (en) * | 2017-12-29 | 2018-06-19 | 山东大学 | A kind of metal organic framework/graphene oxide water-oil separationg film and preparation method thereof |
| CN108467490A (en) * | 2018-03-29 | 2018-08-31 | 中国农业科学院蔬菜花卉研究所 | Functional metal organic frame porous material and its preparation method and application |
| CN109529779A (en) * | 2018-11-14 | 2019-03-29 | 常州大学 | A kind of preparation method and applications of modified ZIF-8/GO composite membrane |
| WO2019156635A1 (en) * | 2018-02-08 | 2019-08-15 | Nanyang Technological University | Graphene frameworks membranes for separation of immiscible liquids |
| CN113083237A (en) * | 2021-04-12 | 2021-07-09 | 太原理工大学 | MOFs desulfurizing agent based on organic amine in-situ modification and preparation and application thereof |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106140094A (en) * | 2016-07-04 | 2016-11-23 | 复旦大学 | The synthetic method of the magnetic graphene composite that metallic organic framework is modified and application |
| CN106237993A (en) * | 2016-08-29 | 2016-12-21 | 沈阳理工大学 | A kind of Fe3o4the preparation method of@MOF 199@C18 nano composite material |
| CN106390932A (en) * | 2016-08-29 | 2017-02-15 | 沈阳理工大学 | Preparation method of GO@PDA@MIL-101 nano composite material |
| CN106882797A (en) * | 2017-01-15 | 2017-06-23 | 复旦大学 | A kind of grapheme material of covalent organic frame modification and its synthetic method and application |
| CN108176254A (en) * | 2017-12-29 | 2018-06-19 | 山东大学 | A kind of metal organic framework/graphene oxide water-oil separationg film and preparation method thereof |
| WO2019156635A1 (en) * | 2018-02-08 | 2019-08-15 | Nanyang Technological University | Graphene frameworks membranes for separation of immiscible liquids |
| CN108467490A (en) * | 2018-03-29 | 2018-08-31 | 中国农业科学院蔬菜花卉研究所 | Functional metal organic frame porous material and its preparation method and application |
| CN109529779A (en) * | 2018-11-14 | 2019-03-29 | 常州大学 | A kind of preparation method and applications of modified ZIF-8/GO composite membrane |
| CN113083237A (en) * | 2021-04-12 | 2021-07-09 | 太原理工大学 | MOFs desulfurizing agent based on organic amine in-situ modification and preparation and application thereof |
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