CN109292754A - A kind of preparation method of polyethyleneimine-modified graphene aerogel - Google Patents
A kind of preparation method of polyethyleneimine-modified graphene aerogel Download PDFInfo
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- CN109292754A CN109292754A CN201810888574.5A CN201810888574A CN109292754A CN 109292754 A CN109292754 A CN 109292754A CN 201810888574 A CN201810888574 A CN 201810888574A CN 109292754 A CN109292754 A CN 109292754A
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- polyethyleneimine
- modified graphene
- graphene aerogel
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- graphene oxide
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
Abstract
The invention discloses a kind of preparation methods of polyethyleneimine-modified graphene aerogel, in particular to utilize polyethyleneimine-modified graphene aerogel prepares coating material.This new method is characterized in that polyethyleneimine is selected to be modified graphene oxide, recycles ascorbic acid to carry out reduction to it and generate polyethyleneimine-modified graphene aerogel.The aeroge of preparation is ground, wire surface is glued to, polyethyleneimine-modified graphene aerogel coating solid phase micro-extraction fiber is made.Solid-phase micro-extraction fibre prepared by the present invention has many advantages, such as that high mechanical strength, coating stability are good, extraction ability is excellent, and the enrichment that can be applied to Determination of Trace Polycyclic Aromatic Hydrocarbons pollutant in environmental water sample with gas-chromatography combination is analyzed, and has good application potential.
Description
Technical field
The present invention relates to a kind of technologies for preparing polyethyleneimine-modified graphene aerogel.
Background technique
Solid phase microextraction (SPME) be last century the nineties grow up integrate sampling, enrichment, purifying, parsing
Novel sample pretreatment, have many advantages, such as it is easy, quick, sensitive, convenient for automation and Instrument crosslinking, environment, food
The fields such as product, drug and bioanalysis are applied widely.Usually signified SPME refers to fiber solid phase micro-extraction, core
It is extracting fiber.The stability and extraction ability of extracting fiber depend on carrier and extraction coating.Quartz is to prepare the micro- extraction of solid phase
The common carrier of fiber is taken, quartzy mechanical performance is poor, is easily broken in operating process, has seriously affected extracting fiber
Service life.In order to improve the mechanical strength of solid-phase micro-extraction fibre, people begin one's study wire as carrier, prepare
The solid-phase micro-extraction fibre of the carriers such as some titanium silks, nickel wire, stainless steel wire, although mechanical strength, metal surface can be improved
It is not easy to be modified processing, limits applied metal silk carrier and prepare solid-phase micro-extraction fibre.
Graphene is a kind of Two-dimensional Carbon nanometer material for forming hexangle type in honeycomb lattice with sp2 hybridized orbit by carbon atom
Material, with excellent optics, electricity, mechanical characteristic, in materialogy, micro-nano technology, the energy, biomedicine and drug delivery etc.
Aspect is with important application prospects, it is considered to be a kind of future revolutionary material.The side of the common power production of graphene
Method is mechanical stripping method, oxidation-reduction method, SiC epitaxial growth method, and film production method is chemical vapour deposition technique.Aeroge is
A kind of solid matter form, one of the solid of world's upper density very little.The preparation of aeroge usually by sol-gel process and surpasses
Critical drying process is constituted.The unique nano-porous structure of aeroge make its mechanics, acoustics, optics, in terms of property
Corresponding traditional macro vitreous material can be differed markedly from, such as high porosity, high-specific surface area, low-density, low-refraction, low
Elasticity modulus, low acoustic impedance, lower thermal conductivity, strong absorption property etc..It has ultrafast, superelevation adsorption capacity to organic solvent, is
The highest material of reported oil sucting force so far has a high potential in the application aspect of solid-phase micro-extraction coating.
Polyethyleneimine (PEI) is a kind of water soluble polymer, there is hygroscopicity, is dissolved in water, ethyl alcohol, does not dissolve in
Benzene.PEI has higher reaction vigor, and simultaneously cross-linked polymeric can be reacted with the hydroxyl in cellulose, so that paper is generated wet strength, and have
There is dry humidification.PEI can also be used in fibre modification, printing and dyeing assistant, ion exchange resin and cohesion and settle that (metal is caught
Collection, wastewater treatment) etc..PEI can prepare three-dimensional grapheme material with modified graphene oxide.PEI is modified to graphene oxide
Afterwards, graphene-based aeroge is prepared, the mechanical strength of graphene aerogel, and the adsorption capacity of PEI itself can not only be enhanced
It can make modified graphene aerogel that there is superior adsorption capacity.
Summary of the invention
The purpose of the present invention is to provide a kind of technologies for preparing polyethyleneimine-modified graphene aerogel.Base of the present invention
Graphene aerogel is modified in polyethyleneimine, acquisition polyethyleneimine-modified graphene aerogel, then as
Coating prepares solid-phase micro-extraction fibre, it is characterised in that this method has following processing step:
Aq. polyethyleneimine is added dropwise in graphene oxide aqueous dispersions, obtains polyethyleneimine after mixing evenly
Amine-graphene oxide dispersion, concentration of the polyethyleneimine in dispersion liquid are 0.1-0.5 mg/mL, and graphene oxide is dividing
Concentration in dispersion liquid is 0.5-5 mg/mL, and ascorbic acid is added, makes its concentration 5-20 mg/mL, mixed solution is placed in height
It presses in reaction kettle, in 100-150 DEG C of isothermal reaction 6-12 h, obtained solid is carried out to be freeze-dried obtained polyethyleneimine-modified
Graphene aerogel.
Present invention polyethyleneimine described in the preparation step of polyethyleneimine-modified graphene aerogel and oxidation stone
The mass ratio of black alkene is 1:5-10.
Present invention graphene oxide described in the preparation step of polyethyleneimine-modified graphene aerogel and Vitamin C
The mass ratio of acid is 1:1-5.
It is a further object of the present invention to provide polyethyleneimine-modified graphene aerogels, are ground, and gluing is used
To stainless steel wire, iron wire, titanium silk, nickel wire surface, it is micro- that polyethyleneimine-modified graphene aerogel coat metal wire solid phase is made
Extracting fiber, is combined with gas-chromatography, the analysis detection applied to polycyclic aromatic hydrocarbons in environmental water sample pollutant.
The used polyethyleneimine-modified graphene aerogel coat metal wire solid-phase micro-extraction fibre of the present invention with
Lower advantage:
(1) wire can effectively improve the frangible disadvantage of quartz fibre as fiber carrier, improve micro-extraction fabric
Mechanical strength extends its service life.
(2) use polyethyleneimine-modified graphene aerogel, effectively enhance graphene aerogel mechanical strength and
Extraction ability makes graphene aerogel that can be preferably applied for solid-phase micro-extraction fibre coating, increases its service life and expansion
Its big application range.
(3) polyethyleneimine-modified graphene aerogel coat metal wire solid-phase micro-extraction fibre and gas-chromatography are combined,
Analysis speed, shortening sample analysis time to 40 min are substantially increased, and improves 3 numbers of existing chromatographic apparatus sensitivity
Magnitude.
Specific embodiment
For a better understanding of the present invention, it is illustrated by example:
Embodiment 1:
Aq. polyethyleneimine is added dropwise in graphene oxide aqueous dispersions, obtains polyethyleneimine after mixing evenly
Amine-graphene oxide dispersion, concentration of the polyethyleneimine in dispersion liquid are 0.1 mg/mL, and graphene oxide is in dispersion liquid
In concentration be 1 mg/mL, be added ascorbic acid, make 5 mg/mL of its concentration, mixed solution be placed in autoclave,
In 100 DEG C of 12 h of isothermal reaction, obtained solid is carried out to be freeze-dried obtained polyethyleneimine-modified graphene aerogel.By its
It grinds, is glued to stainless steel wire surface, polyethyleneimine-modified graphene aerogel coating stainless steel wire solid phase is made
Micro-extraction fabric, is combined with gas-chromatography, the analysis detection applied to polycyclic aromatic hydrocarbons in environmental water sample pollutant.
Embodiment 2:
Aq. polyethyleneimine is added dropwise in graphene oxide aqueous dispersions, obtains polyethyleneimine after mixing evenly
Amine-graphene oxide dispersion, concentration of the polyethyleneimine in dispersion liquid are 0.5 mg/mL, and graphene oxide is in dispersion liquid
In concentration be 5 mg/mL, be added ascorbic acid, make 18 mg/mL of its concentration, mixed solution be placed in autoclave,
In 150 DEG C of 6 h of isothermal reaction, obtained solid is carried out to be freeze-dried obtained polyethyleneimine-modified graphene aerogel.By its
It grinds, is glued to titanium silk table face, it is fine that polyethyleneimine-modified graphene aerogel coated titanium silk solid phase microextraction is made
Dimension, is combined with gas-chromatography, the analysis detection applied to polycyclic aromatic hydrocarbons in environmental water sample pollutant.
Embodiment 3:
Aq. polyethyleneimine is added dropwise in graphene oxide aqueous dispersions, obtains polyethyleneimine after mixing evenly
Amine-graphene oxide dispersion, concentration of the polyethyleneimine in dispersion liquid are 0.3 mg/mL, and graphene oxide is in dispersion liquid
In concentration be 3 mg/mL, be added ascorbic acid, make 10 mg/mL of its concentration, mixed solution be placed in autoclave,
In 120 DEG C of 9 h of isothermal reaction, obtained solid is carried out to be freeze-dried obtained polyethyleneimine-modified graphene aerogel.By its
It grinds, is glued to nickel wire surface, it is fine that polyethyleneimine-modified graphene aerogel coating nickel wire solid phase microextraction is made
Dimension, is combined with gas-chromatography, the analysis detection applied to polycyclic aromatic hydrocarbons in environmental water sample pollutant.
Embodiment 4:
Polyethyleneimine-modified graphene aerogel coating stainless steel wire solid-phase micro-extraction fibre is inserted into 10 mL environmental water samples
In, 20 min of stirring extraction at 40 DEG C are inserted into 300 DEG C of gas chromatographic sample introduction mouth after taking-up and carry out 3 min of thermal desorption, and 40
6 kinds of polycyclic aromatic hydrocarbons in an environmental water sample are completed in min to include naphthalene, fluorenes, anthracene, fluoranthene, bend, the analysis detection of BaP, detection
It limits down to 0.005 μ g/L.
Claims (4)
1. a kind of preparation method of polyethyleneimine-modified graphene aerogel, which is characterized in that by aq. polyethyleneimine
It is added dropwise in graphene oxide aqueous dispersions, obtains polyethyleneimine-graphene oxide dispersion, poly- second after mixing evenly
Concentration of the alkene imines in dispersion liquid is 0.1-0.5 mg/mL, and concentration of the graphene oxide in dispersion liquid is 0.5-5 mg/
ML is added ascorbic acid, makes its concentration 5-20 mg/mL, mixed solution is placed in autoclave, in 100-150 DEG C of perseverance
Temperature reaction 6-12 h, obtained solid is carried out to be freeze-dried obtained polyethyleneimine-modified graphene aerogel.
2. a kind of preparation method of polyethyleneimine-modified graphene aerogel according to claim 1, feature exist
In the mass ratio of polyethyleneimine and graphene oxide is 1:5-10.
3. a kind of preparation method of polyethyleneimine-modified graphene aerogel according to claim 1, feature exist
In the mass ratio of graphene oxide and ascorbic acid is 1:1-5.
4. gathering prepared by a kind of preparation method of polyethyleneimine-modified graphene aerogel according to claim 1
Aziridine modified graphene aeroge.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111569848A (en) * | 2020-06-15 | 2020-08-25 | 甘肃政法大学 | Preparation method of solid-phase micro-extraction fiber with reduced graphene oxide as coating material |
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