CN106390932A - Preparation method of GO@PDA@MIL-101 nano composite material - Google Patents
Preparation method of GO@PDA@MIL-101 nano composite material Download PDFInfo
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- CN106390932A CN106390932A CN201610741388.XA CN201610741388A CN106390932A CN 106390932 A CN106390932 A CN 106390932A CN 201610741388 A CN201610741388 A CN 201610741388A CN 106390932 A CN106390932 A CN 106390932A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their physical properties
- B01J20/28004—Sorbent size or size distribution, e.g. particle size
- B01J20/28007—Sorbent size or size distribution, e.g. particle size with size in the range 1-100 nanometers, e.g. nanosized particles, nanofibers, nanotubes, nanowires or the like
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
Abstract
The invention provides a preparation method of a GO@PDA@MIL-101 nano composite material. The method includes the steps of: 1. preparing GO@PDA; 2. taking para toluic acid, A GOPDAMIL 101 nano composite material preparation method comprises the following steps: 1, preparation of GOPDA, 2, take on the quality of benzoic acid, chromium nitrate nonahydrate and GO@PDA in a mass ratio of 41:100:10, and taking deionized water and 40% hydrofluoric acid in a mass ratio of 96:1 for standby use; 3. firstly dissolving para toluic acid and chromium nitrate nonahydrate in a reaction kettle holding deionized water, then dissolving the GO@PDA prepared in step 1 in the mixed solution, conducting ultrasonic treatment for 15min, and performing magnetic stirring for 20min; 4. adding hydrofluoric acid into the mixed solution, and carrying out reaction under 493k for 8h; and 5. cooling the reaction product to room temperature, then conducting washing with N, N-dimethylformamide, ethanol and distilled water in order, and then performing drying, thus obtaining the GO@PDA@MIL-101 nano composite material. The method provided by the invention has the advantages of simple operation and low cost, the prepared GO@PDA@MIL-101 nano composite material has a nano-scale particle size, uniform particles, good dispersion, and strong adsorption capacity. The preparation process does not cause environmental pollution and is harmless to the health of operators.
Description
Technical field
The present invention relates to a kind of preparation method of metallic organic framework composite, particularly to one kind through Dopamine hydrochloride
Graphene oxide-metallic organic framework the nano composite material modified（GO@PDA@MIL-101）Preparation method.
Background technology
The synthetic method of metal-organic framework materials has a lot, and common method has hydro-thermal method, diffusion method, microwave radiation technology
Method, method, ultrasonic wave added method etc. are stirred at room temperature.
（1）Hydro-thermal method
Hydro-thermal method（Also known as hydrothermal method）Refer to water as solvent, under conditions of airtight, so that reactant is occurred by HTHP
Reaction, a kind of method of culture crystal.Till now, the reactive mode of hydro-thermal method and be not solely restricted to water be molten
Agent, in reaction may some or all of organic solvent, that is, described hot solvent method.The crystallization occurring under the conditions of hydro-thermal method
Reaction, thermal stress is little, and the crystal of synthesis has good crystal face, and internal flaw is few.Therefore, typically metal is prepared using hydro-thermal method
Organic framework material.
（2）Diffusion method
Diffusion method is exactly that the material making two kinds of different shapes contacts with each other, and then can slowly crystallize at two kinds of material interfaces and give birth to
Become the process of product.This method is gentleer, is readily synthesized the crystal of larger particles, but the conventionally used time all compares
Long, therefore receive some restrictions in some aspects.
（3）Microwave assisting method
Microwave assisting method is a kind of synthetic method being considered transitory efficient, be exactly generally in the presence of high-frequency microwave so that
Powered particle is mutually clashed into very high speed, then generates the process of product.Because the frequency of microwave is very high, therefore typically
Reaction is all to occur in moment, and thermograde is very low, and can selectively heating response thing, capacity usage ratio is very high.
（4）Method is stirred at room temperature
The method of being stirred at room temperature is also a kind of method of Fast back-projection algorithm metal-organic framework materials, and easy to operate, and equipment is simple only
Reactant is dissolved in specific solvent, under conditions of room temperature or heating, certainly can also add in system
Proton-removed agent come to accelerate react carrying out.
Content of the invention
The purpose of the present invention, is to provide a kind of preparation method of GO@PDA@MIL-101 nano composite material.This method energy
Prepare the graphene oxide-metallic organic framework nano composite material modified through Dopamine hydrochloride（GO@PDA@MIL-101),
And composite particle diameter is in Nano grade, uniformly, absorbent properties are good for particle.
Employed technical scheme comprise that：
A kind of preparation method of GO@PDA@MIL-101 nano composite material, comprises the steps：
1st, the preparation of GO@PDA：
（1）It is 2 in mass ratio: 1:6.1 ratio takes Dopamine hydrochloride, graphene oxide and three（Methylol）Aminomethane is standby
With；By wherein outfit three（Methylol）The quality of aminomethane be configured to pH=8.5 Tris cushioning liquid and with hydrochloric acid DOPA
Amine and graphene oxide mixing, mixture ultrasonic wave disperses（20kz,10min）, after being uniformly dispersed, carry out the magnetic force of 24 hours
Stirring, after product is washed with deionized, dries, obtains GO@PDA, standby；
2nd, the preparation of GO@PDA@MOF-101：
（1）, get the raw materials ready：
Mass ratio is taken to be 41:100:10 para Toluic Acid, Chromium nitrate (Cr(NO3)3),nonahydrate and GO@PDA, and mass ratio be 96:1 deionization
Water and the hydrofluoric acid that concentration is 40% are standby.
（2）, first deionized water is placed in reactor, after para Toluic Acid and Chromium nitrate (Cr(NO3)3),nonahydrate are dissolved in deionized water
In, then GO@PDA prepared by step 1 is dissolved in wherein；
（3）, with 20Kz ultrasonic disperse 15min, at room temperature, stir 20min under the magnetic force of 200r/min, in mixed solution
Add hydrofluoric acid, be stirred until homogeneous, react 8h under 493K.
（4）, reactor liter be placed in warm stove carry out hydro-thermal reaction, set heating schedule as：It is warming up to 5k/min
493k, and keep 8h, after be cooled to 308k.
（5）, question response kettle be cooled to room temperature, product successively use DMF, after ethanol and water washing, dry
Dry, obtain final product material GO@PDA@MOF-101.
Have an advantage in that：
The present invention is simple to operate, low cost, and prepared GO@PDA@MOF-101 nano composite material particle diameter is in Nano grade,
Particle is uniform, good dispersion, high adsorption capacity.Environmental pollution is not resulted in when preparation, harmless to the health of operating personnel.
Specific embodiment
Embodiment one
A kind of preparation method of GO@PDA@MIL-101 nano composite material, comprises the following steps：
The first step：The preparation of GO@PDA：
First, 20mg Dopamine hydrochloride is dissolved in 10mL Tris cushioning liquid, after dissolving, adds 10mg graphene oxide
（GO）, 20KZ is ultrasonic to carry out ultrasonic disperse 10min, the continuous room temperature magnetic agitation of lower 24 hours after being uniformly dispersed.Stirring knot
After bundle, deionized water is thoroughly washed, then dries, and the GO@PDA finally collecting preparation is standby.
Second step：The preparation of GO@PDA@MIL-101：
Para Toluic Acid 410mg and Chromium nitrate (Cr(NO3)3),nonahydrate 1g is dissolved in 12mL deionized water, GO@PDA prepared by step one
It is dissolved in wherein, 20Kz ultrasonic disperse 15min, at room temperature, stirs 20min under the magnetic force of 200r/min, to mixed solution
Middle addition 0.125ml hydrofluoric acid, is stirred until homogeneous；Reactor liter is placed in warm stove and carries out hydro-thermal reaction, set heating schedule
For：493k is warming up to 5k/min, and keeps 8h, after be cooled to 308k.Question response kettle is cooled to room temperature, the product obtaining according to
Dry in 323k after secondary use DMF, ethanol and water washing 3 times, obtain final product material GO@PDA@MIL-101 nanometer multiple
Condensation material.
Embodiment two
A kind of preparation method of graphene oxide-metallic organic framework nano composite material, comprises the following steps：
The first step：The preparation of GO@PDA：
First, 20mg Dopamine hydrochloride is dissolved in 10mL Tris cushioning liquid, after fully dissolving, adds 10mg graphite oxide
Alkene（GO）, put into and in ultrasonic wave, carry out ultrasonic disperse 10min, the continuous room temperature magnetic agitation of lower 24 hours after being uniformly dispersed.
Stirring terminates rear deionized water and is thoroughly washed, then dries, and finally collects standby.
Second step：The preparation of GO@PDA@MIL-101：
Para Toluic Acid 410mg and Chromium nitrate (Cr(NO3)3),nonahydrate 1g is dissolved in 12mL deionized water, GO@prepared by step one
PDA100mg is dissolved in wherein, ultrasonic 15min, at room temperature, stirs 20min, to mixed solution under the magnetic force of 200r/min
Middle addition 0.125ml hydrofluoric acid, is stirred until homogeneous；Reactor liter is placed in warm stove and carries out hydro-thermal reaction, set heating schedule
For：493k is warming up to 5k/min, and keeps 8h, after be cooled to 308k.Question response kettle is cooled to room temperature, the product obtaining according to
Secondary use DMF, dries in 323k after ethanol and water washing, obtains final product material GO@PDA@MIL-101 nano combined
Material.
The Tris cushioning liquid of embodiment one and two kinds of embodiment is by three（Methylol）Aminomethane is configured to PH=8.5
Solution.
Claims (1)
1. a kind of preparation method of GO@PDA@MIL-101 nano composite material is it is characterised in that comprise the steps：
The preparation of GO@PDA：
（1）Take Dopamine hydrochloride, graphene oxide and three（Methylol）Aminomethane, Dopamine hydrochloride, graphene oxide and three
（Methylol）The mass ratio of aminomethane is 2:1:6.1, standby；
（2）Take above-mentioned three（Methylol）The quality of aminomethane is configured to the Tris cushioning liquid of pH=8.5, standby；
（3）Mixing Dopamine hydrochloride, graphene oxide and Tris cushioning liquid, mixture ultrasonic wave disperses 10min, and dispersion is all
Carry out the magnetic agitation of 24 hours after even, after product is washed with deionized, dries, obtain GO PDA, standby；
The preparation of GO@PDA@MIL-101：
(1), get the raw materials ready：
The mass ratio of para Toluic Acid, Chromium nitrate (Cr(NO3)3),nonahydrate and GO@PDA is 41:100:10, mass ratio is 96:1 deionized water and
Concentration be 40% hydrofluoric acid standby；
（2）, first para Toluic Acid, Chromium nitrate (Cr(NO3)3),nonahydrate are dissolved in equipped with the reactor of ionized water, then GO@prepared by step 1
PDA is dissolved in mixed liquor, ultrasonic 15min, magnetic stirring 20min；
（3）, in mixed solution add hydrofluoric acid, under 493k react 8h；
（4）, question response product be cooled to room temperature, successively use DMF, ethanol and distillation water washing post-drying, that is,
Obtain material GO@PDA@MIL-101 nano composite material.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107308987A (en) * | 2017-06-09 | 2017-11-03 | 沈阳理工大学 | A kind of Fe3O4The preparation method of the nano composite materials of@PDA@MOF 5 |
| CN107573817A (en) * | 2017-10-16 | 2018-01-12 | 沈阳顺风实业集团有限公司 | A kind of preparation method of composite water soluble anticorrosive paint |
| CN108878884A (en) * | 2018-06-01 | 2018-11-23 | 南开大学 | It is a kind of simply to prepare the method and its application of graphene nanometer sheet in lithium ion battery negative material |
| CN109627004A (en) * | 2018-12-19 | 2019-04-16 | 重庆大学 | A kind of thermal conductivity graphene film and preparation method thereof |
| WO2019156635A1 (en) * | 2018-02-08 | 2019-08-15 | Nanyang Technological University | Graphene frameworks membranes for separation of immiscible liquids |
| CN110801818A (en) * | 2019-10-25 | 2020-02-18 | 南昌大学 | Composite functional material for removing radioactive iodine and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107308987A (en) * | 2017-06-09 | 2017-11-03 | 沈阳理工大学 | A kind of Fe3O4The preparation method of the nano composite materials of@PDA@MOF 5 |
| CN107573817A (en) * | 2017-10-16 | 2018-01-12 | 沈阳顺风实业集团有限公司 | A kind of preparation method of composite water soluble anticorrosive paint |
| WO2019156635A1 (en) * | 2018-02-08 | 2019-08-15 | Nanyang Technological University | Graphene frameworks membranes for separation of immiscible liquids |
| CN108878884A (en) * | 2018-06-01 | 2018-11-23 | 南开大学 | It is a kind of simply to prepare the method and its application of graphene nanometer sheet in lithium ion battery negative material |
| CN108878884B (en) * | 2018-06-01 | 2021-01-01 | 南开大学 | Simple method for preparing graphene nanosheet and application of graphene nanosheet to lithium ion battery cathode material |
| CN109627004A (en) * | 2018-12-19 | 2019-04-16 | 重庆大学 | A kind of thermal conductivity graphene film and preparation method thereof |
| CN109627004B (en) * | 2018-12-19 | 2022-01-07 | 重庆大学 | Heat-conducting and electric-conducting graphene film and preparation method thereof |
| CN110801818A (en) * | 2019-10-25 | 2020-02-18 | 南昌大学 | Composite functional material for removing radioactive iodine and application thereof |
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Application publication date: 20170215 |