CN107262036A - A kind of preparation method of adsorptivity graphene oxide hydrogel - Google Patents
A kind of preparation method of adsorptivity graphene oxide hydrogel Download PDFInfo
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- CN107262036A CN107262036A CN201710624013.XA CN201710624013A CN107262036A CN 107262036 A CN107262036 A CN 107262036A CN 201710624013 A CN201710624013 A CN 201710624013A CN 107262036 A CN107262036 A CN 107262036A
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- 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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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
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Abstract
The invention discloses a kind of preparation method of adsorptivity graphene oxide hydrogel, the preparation of graphene oxide is synthesized by improved Hummers methods, so using self assembly principle design it is synthetically prepared go out many amine hydrogels of graphene oxide.The thickness for the graphene oxide layer that the present invention is obtained is arrived at several microns between nanometers up to a hundred, and surface is smooth a certain degree of fold, integrally looks in thin sand-like, in most cases exists with multilayer form, and its thickness is about in 2nm.The many amine hydrogels of graphene oxide prepared by the present invention, in three-dimensional netted loose structure, have more folds compared to graphene oxide and thickness are significantly increased；The many amine hydrogels of graphene oxide have more preferable heat endurance and heat-resisting quantity.The many amine hydrogel heavy metal ion Pb of graphene oxide2+Deng with good adsorption capacity, there is good application prospect in the processing of industrial wastewater.
Description
Technical field
The present invention relates to a kind of preparation method of hydrogel.
Background technology
Hydrogel can absorb large quantity of moisture and these water tariff collections are lived, and can occur after it absorbs moisture substantially swollen
It is swollen, but structure does not change, therefore hydrogel can also return to original configuration state, and hydrogel will not be in water
Middle generation dissolution phenomena.We carry out preparing nano composite aquogel through conventional self assembly principle, and this method can be by nanoparticle
Son is evenly dispersed in monomer and is crosslinked, and can effectively obtain the nano composite material of good dispersion.In addition, self assembly mode
It is also prevented from high molecular polymer to degrade, and enhances stability of the nano material in water, prevents in water body
Reunite.
Graphene oxide (GO) is a kind of derivative of graphene, and abundant oxygen-containing functional group is contained on its surface, for example-
OH ,-COOH ,-O- ,-C=O etc., therefore it has an extraordinary absorption property, and its hydrophily in the solution, with polymerizeing
The compatibility of thing and dispersiveness in the solution etc. performance all improve a lot compared with graphene.Surface of graphene oxide is not only
Containing abundant oxy radical, also possess big specific surface area.Graphene oxide exclusive property and architectural feature, this is just very big
Graphene oxide is improved in degree to have an effect with other materials, finally produces out the hydrogel of good dispersion.Graphite oxide
Alkene Stability Analysis of Structures and it is difficult to be destroyed, single-layer graphene oxide mechanical performance is very strong, and graphene oxide can be used as reinforcer
The mechanical performance of enhancing material.In addition, graphene oxide possesses preferable bio-compatibility, it is nontoxic will not be to environment
Pollute.
But at present, be combined nearly all by carrier of polymer with graphene oxide and prepare hydrogel, its adsorption capacity has
Limit.
The content of the invention
Commonly be easy to get it is an object of the invention to provide a kind of raw material, with low cost, manufacturing process safety, absorption property it is good
The preparation method of good adsorptivity graphene oxide hydrogel.The present invention mainly synthesizes oxygen by improved Hummers methods
Graphite alkene, so using self assembly principle design it is synthetically prepared go out graphene oxide-many amines hydrogel.
The present invention's comprises the following steps that：
(1) every 10 milliliters of H are pressed2SO4Add 0.2-0.3g KNO3Ratio, by mass fraction be 98% H2SO4It is placed in appearance
In device, stirred under ice-water bath, while adding KNO3It is dissolved in dense H2SO4；
(2) KNO is worked as3After being completely dissolved, by KNO3：Graphite powder：The mass ratio of potassium permanganate is 2-3：1-2：6-9 ratio
In example, the container that graphite powder is added to step (1), potassium permanganate is then added within 20-40min, then container is put
6-8h is stirred in 30-40 DEG C of water bath with thermostatic control, the granularity of the graphite powder is 8000 mesh；
(3) in the ratio that 180-220ml deionized waters are added per 100g said mixtures, with separatory funnel with 1-3 drops/s
Speed deionized water is added into said vesse, container is moved on in 70-90 DEG C of thermostat water bath into constant temperature after being added dropwise to complete protects
Hold 30-40min；
(4) take out container, be cooled to room temperature, add the deionized water with the same ratio of step (3), and by hydrogen peroxide with
The volume ratio of deionized water is 1-1.5:9-11 ratio adds hydrogen peroxide, and preservative film sealing outwells upper strata after standing 12-15h
Solution, the hydrogen peroxide must be slowly added to；
(5) centrifuge is washed, and first uses salt acid elution, then is washed with deionized, until cleaning solution is in neutrality, ultrasound
4-6h, obtains graphene oxide solution, and the graphene solution is uniformly dispersed, and the number of plies is relatively fewer；
(6) 2.0-5.0mg/ml many amine aqueous solutions are prepared, the graphene oxide solution for taking step (5) to prepare is configured to 2-
4mg/ml graphene oxide dispersion, and by graphene oxide dispersion ultrasonic disperse 0.5-1h, by many amine aqueous solutions and oxidation
The volume ratio of graphene dispersing solution is 1-2:4-5 ratio, graphene oxide dispersion and many amine aqueous solutions are put into container and mixed
Close, sealing, ultrasonic 10-20min prepares graphene oxide-many amines hydrogel.
The present invention has the following advantages that compared with prior art：
1st, raw material be commonly easy to get, with low cost, manufacturing process it is safe.
2nd, the graphene oxide-many amines hydrogel prepared, in tridimensional network and with loose structure, compared to oxygen
Graphite alkene has more folds and thickness is significantly increased.
3rd, the graphene oxide-many amines hydrogel prepared has more preferable heat endurance and heat-resisting quantity, and it is to a huge sum of money
Belong to ion Pb2+Deng with good adsorption capacity, it can be used for the processing of industrial wastewater.
Brief description of the drawings
Fig. 1 is a in graphene oxide (GO) electron microscope prepared by the embodiment of the present invention 1, figure：Scanning electron microscope (SEM) photograph, b：Transmission
Electron microscope；
Fig. 2 is a in graphene oxide-many amines hydrogel electron microscope prepared by the embodiment of the present invention 1, figure：ESEM
Figure, b：Transmission electron microscope picture；
Fig. 3 is a in graphene oxide-many amines hydrogel electron microscope prepared by the embodiment of the present invention 2, figure：ESEM
Figure, b：Transmission electron microscope picture；
Fig. 4 is graphene oxide-many amines hydrogel Raman spectrograms prepared by the embodiment of the present invention 2；
Fig. 5 is adsorption rate curve of the graphene oxide-many amines hydrogel to rhodamine B of the preparation of the embodiment of the present invention 2
Figure；
Fig. 6 is graphene oxide-many amines hydrogel of the preparation of the embodiment of the present invention 2 to Pb2+Adsorption rate curve map.
Specific implementation method
Embodiment 1
Measure the dense H that 60ml mass fractions are 98%2SO4It is placed in beaker, is stirred under ice-water bath, while by 2g KNO3It is molten
In dense H2SO4In；KNO3After being completely dissolved, 1.5g granularities are added in beaker for the graphite powder of 8000 mesh, then in 30min
Within 8g potassium permanganate is added in beaker, then beaker is placed in 30 DEG C of waters bath with thermostatic control and stirs 6h；With separatory funnel with
1-3d/s speed adds 200ml deionized waters, and beaker is moved on into constant temperature in 80 DEG C of thermostat water baths after being added dropwise to complete keeps
30min；Beaker is taken out, room temperature is cooled to, 200ml deionized waters are added, 20ml hydrogen peroxide is slow added into, preservative film is sealed,
Upper solution is outwelled after standing 12h；Centrifuge is washed, and first uses salt acid elution, then is washed with deionized, until cleaning solution
In neutrality, ultrasonic 4h obtains graphene oxide solution；Finally, graphene oxide is separately put into several small containers freezing dry
In dry machine, as shown in Figure 1a, gained graphene dispersion is relatively uniform, and the number of plies is relatively fewer, and smooth lamellar structure, piece is presented in surface
The thickness of layer is at several microns between nanometers up to a hundred, and GO two-dimension plane structure makes its specific surface area big, and observes GO pieces
The fold more than comparison is showed in layer surface, this phenomenon can not only increase GO specific surface area, can also increase GO absorption
Saturation capacity；As shown in Figure 1 b, the GO prepared is in not only film-form, also there is partial plies fold.
3.0mg/ml diethylenetriamine (DETA) solution is prepared in volumetric flask, takes above-mentioned graphene oxide solution to configure
Into 2.5mg/ml graphene oxide dispersion, and ultrasonic disperse 0.5h, 10ml graphene oxide dispersion and 2ml is taken respectively
DETA solution mixed in beaker, preservative film sealing, ultrasonic 10min prepares graphene oxide-many amines hydrogel.
As shown in Fig. 2 prepared graphene oxide-many amines hydrogel, because graphene sheet layer accumulates superposition or mutual
Mutually crosslinking is in three-dimensional netted loose structure, and the three-dimensional net structure of hydrogel ensure that the solutes accumulation in water body, this point pair
It is further most important using adsorption experiment in hydrogel.
Embodiment 2
Measure the dense H that 40ml mass fractions are 98%2SO4It is placed in beaker, is stirred under ice-water bath, while by 1.5g KNO3
It is dissolved in dense H2SO4In；KNO3After being completely dissolved, 0.5g granularities are added in beaker for the graphite powder of 8000 mesh, then existed
6g potassium permanganate is added in beaker within 20min, then beaker is placed in 35 DEG C of waters bath with thermostatic control and stirs 7h；Leaked with point liquid
Struggle against and 180ml deionized waters are added with 1-3d/s speed, beaker is moved on into constant temperature in 70 DEG C of thermostat water baths after being added dropwise to complete protects
Hold 35min；Beaker is taken out, room temperature is cooled to, 180ml deionized waters is added, is slow added into 25ml hydrogen peroxide, preservative film is close
Envelope, upper solution is outwelled after standing 13h；Centrifuge is washed, and first uses salt acid elution, then is washed with deionized, until washing
Liquid is washed in neutrality, ultrasonic 5h obtains graphene oxide solution；
2.0mg/ml triethylene tetramine (TETA) solution is prepared in volumetric flask, takes above-mentioned graphene oxide solution to configure
Into 2mg/ml graphene oxide dispersion, and ultrasonic disperse 1h, 8ml graphene oxide dispersion and 2ml is taken respectively
TETA solution is mixed in beaker, and preservative film sealing, ultrasonic 15min prepares graphene oxide-many amines hydrogel.
As shown in figure 3, graphene oxide-many amines the hydrogel prepared, in tridimensional network and with porous knot
Structure, has more folds compared to graphene oxide and thickness is significantly increased, secondly, graphene oxide-many amines hydrogel
With more preferable heat endurance and heat-resisting quantity.As Fig. 4 shows that GO has three characteristic peaks in Raman spectrum：In 2692cm-1Place
2D peaks, in 1351cm-1The D peaks and 1601cm at place-1The G peaks at place, wherein 2692cm-1The 2D peaks at place are particularly susceptible to stone
The influence that black olefinic carbon layer is stacked.Data show individual layer, bilayer, three layers, multilayer (>4 layers) the 2D/G ratios of graphene are respectively>
1.60,0.80,0.30 and 0.07；It can be seen that individual layer GO G peaks and 2D peaks are generally in 1585cm-1And 2679cm-1Place, but
Multilayer GO (number of plies 2~6) G peaks are to relatively low wave-number migration and 2D peaks to higher wave-number migration.As Fig. 4 b show GO and
GO-DETA hydrogels, GO-TETA hydrogel D/G ratios are changed into 1.03 and 1.04 respectively from 0.97, and this is primarily due to GO and two
Plant the presence that amine molecule forms C-N keys on tridimensional network and carbon-coating surface.As Fig. 4 c show GO and GO-DETA water-settings
Glue, the 2D/G ratios of GO-TETA hydrogels show GO and two kinds of water-settings prepared by the present invention in the interval interior of 0.24-0.26
Glue is multilayer.
Application examples 1：
Using graphene oxide-many amines hydrogel of preparation, distinguished under field conditions (factors) using ultraviolet absorption spectrum instrument
To 1mg/L, 2mg/L, 3mg/L, 4mg/L, the rhdamine B solution of five kinds of concentration of 5mg/L is adsorbed, and show that its maximum is inhaled
Wavelength is received to be located at 554nm.The absorbance and the relation of mass concentration of the rhodamine B of various concentrations are tested, show that both have
Good linear fit relation.The rhodamine B solution for measuring 100ml is placed into three beakers, in the state of stirring, institute
The different quality concentration 0.25wt%, 0.50wt%, 1.00wt% that prepare hydrogel are respectively put into beaker；Finally, exist
Different time takes out a certain amount of solution, by centrifuge, takes upper liquid to survey absorbance, repeats experimental procedure above
Several times, until graphene oxide-absorption of many amines hydrogel to rhdamine B molecule tends to balance.Test result is such as
Shown in Fig. 5, adsorb and tend to balance after all absorption 20min, its absorption to dyestuff is increased with hydrogel mass concentration
Rate also becomes big therewith.The dye strength in dye strength and solution in starting stage hydrogel surface has one between the two
Gradient difference, and when initial hydrogel surface adsorption site it is more, because both reasons were determined in the absorption starting stage
Its adsorption rate to dyestuff is very fast；Increase with hydrogel to the adsorption time of dyestuff, concentration difference and adsorption site
Reduction finally causes slowing down for the rate of adsorption, and reach the adsorption equilibrium to dye molecule.Graphene oxide-many amines water-setting
Glue has stable three-dimensional netted loose structure due to internal, so their very strong adsorption capacities are imparted, for toxic dye
Possess good selectivity.
Described rhdamine B can also be substituted for the dyestuff such as methylene blue, methyl orange, Congo red.
Application examples 2：
100ml 15mg/L Pb (NO are prepared with volumetric flask3)2Solution, under stirring, 0.25wt% oxidation stone
Black alkene-many amines hydrogel is put into beaker, is taken out a certain amount of solution in the different time, is utilized atomic absorption spectrphotometry
Method measures ion solubility.Above step is repeated, until the absorption of hydrogel heavy metal ion tends to balance.As shown in fig. 6, institute
Having absorption, adsorbance increases rapidly about within 1h, and absorption tends to balance after 3h.GO-DETA hydrogel 0.25wt% counterweights
Metal ion Pb2+, the maximum adsorption rate being finally reached is 96.00% respectively；GO-TETA hydrogel 0.25wt% heavy metals from
Sub- Pb2+, the maximum adsorption rate being finally reached is 65.54% respectively.This powerful adsorption capacity, mainly has benefited from hydrogel
, there is electrostatic interaction, the oh group and amino base of hydrogel surface between heavy metal ion in three-dimensional network loose structure
There is complexing with the contents of many kinds of heavy metal ion in sewage in group.The graphene oxide water synthesized by intermolecular self assembly principle
Gel, it is easy to operate, not by such environmental effects, there is good application prospect in the treatment of waste water.
Described heavy metal ion solution is not limited only to Pb2+Or Fe3+、Cu2+Deng solution.
Embodiment 3
Measure the dense H that 50ml mass fractions are 98%2SO4It is placed in beaker, is stirred under ice-water bath, while by 1g KNO3It is molten
In dense H2SO4In；KNO3After being completely dissolved, by 1g granularities for 8000 mesh graphite powder add beaker in, then 40min it
It is interior that 9g potassium permanganate is added in beaker, then beaker is placed in 40 DEG C of waters bath with thermostatic control and stirs 8h；With separatory funnel with 1-
3d/s speed adds 220ml deionized waters, and beaker is moved on into constant temperature in 9 DEG C of thermostat water baths after being added dropwise to complete keeps 40n；Take
Go out beaker, be cooled to room temperature, add 220ml deionized waters, be slow added into 25ml hydrogen peroxide, preservative film sealing is stood after 15h
Outwell upper solution；Centrifuge is washed, and first uses salt acid elution, then is washed with deionized, until cleaning solution is in neutrality, is surpassed
Sound 6h, obtains graphene oxide solution；
5.0mg/ml triethylene tetramine (TETA) solution is prepared in volumetric flask, takes above-mentioned graphene oxide solution to configure
Into 4mg/ml graphene oxide dispersion, and ultrasonic disperse 1h, 9ml graphene oxide dispersion and 3ml is taken respectively
TETA solution is mixed in beaker, and preservative film sealing, ultrasonic 20min prepares graphene oxide-many amines hydrogel.
Claims (1)
1. a kind of preparation method of adsorptivity graphene oxide hydrogel, it is characterised in that：It comprises the following steps：
(1) every 10 milliliters of H are pressed2SO4Add 0.2-0.3g KNO3Ratio, by mass fraction be 98% H2SO4It is placed in container
In, stirred under ice-water bath, while adding KNO3It is dissolved in dense H2SO4；
(2) KNO is worked as3After being completely dissolved, by KNO3：Graphite powder：The mass ratio of potassium permanganate is 2-3：1-2：6-9 ratio, will
Graphite powder is added in the container of step (1), and potassium permanganate is then added within 20-40min, container then is placed in into 30-
6-8h is stirred in 40 DEG C of waters bath with thermostatic control, the granularity of the graphite powder is 8000 mesh；
(3) in the ratio that 180-220ml deionized waters are added per 100g said mixtures, with separatory funnel with 1-3 drops/s speed
Spend and deionized water is added into said vesse, container is moved on into constant temperature in 70-90 DEG C of thermostat water bath after being added dropwise to complete keeps 30-
40min；
(4) take out container, be cooled to room temperature, add the deionized water with the same ratio of step (3), and by hydrogen peroxide and go from
The volume ratio of sub- water is 1-1.5:9-11 ratio adds hydrogen peroxide, and preservative film sealing outwells upper solution after standing 12-15h,
The hydrogen peroxide must be slowly added to；
(5) centrifuge is washed, and first uses salt acid elution, then is washed with deionized, until cleaning solution is in neutrality, ultrasonic 4-
6h, obtains graphene oxide solution, and the graphene solution is uniformly dispersed, and the number of plies is relatively fewer；
(6) 2.0-5.0mg/ml many amine aqueous solutions are prepared, the graphene oxide solution for taking step (5) to prepare is configured to 2-4mg/ml
Graphene oxide dispersion, and by graphene oxide dispersion ultrasonic disperse 0.5-1h, by many amine aqueous solutions and graphene oxide
The volume ratio of dispersion liquid is 1-2:4-5 ratio, graphene oxide dispersion and many amine aqueous solutions are put into container and mixed, close
Envelope, ultrasonic 10-20min prepares graphene oxide-many amines hydrogel.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375687A (en) * | 2018-03-09 | 2018-08-07 | 北京协同创新研究院 | A method of the coated graphite alkene on atomic force microscope probe needle point |
| CN110065988A (en) * | 2019-04-23 | 2019-07-30 | 中国石油大学(华东) | A method of going heavy metal ion in water removal |
| CN110508247A (en) * | 2019-08-30 | 2019-11-29 | 方大炭素新材料科技股份有限公司 | A kind of preparation method of the graphene oxide composite material for Industrial Waste Water Treatments |
| CN113173576A (en) * | 2021-05-07 | 2021-07-27 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Graphene aerogel, preparation method and application thereof, and elution method of food-borne pathogenic microorganisms on graphene aerogel |
-
2017
- 2017-07-27 CN CN201710624013.XA patent/CN107262036A/en active Pending
Non-Patent Citations (1)
| Title |
|---|
| 朱凯: ""基于氧化石墨烯水凝胶的制备及其性能的研究"", 《中国优秀硕士学位论文全温暖数据库 工程科技I辑》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108375687A (en) * | 2018-03-09 | 2018-08-07 | 北京协同创新研究院 | A method of the coated graphite alkene on atomic force microscope probe needle point |
| CN110065988A (en) * | 2019-04-23 | 2019-07-30 | 中国石油大学(华东) | A method of going heavy metal ion in water removal |
| CN110508247A (en) * | 2019-08-30 | 2019-11-29 | 方大炭素新材料科技股份有限公司 | A kind of preparation method of the graphene oxide composite material for Industrial Waste Water Treatments |
| CN113173576A (en) * | 2021-05-07 | 2021-07-27 | 军事科学院军事医学研究院环境医学与作业医学研究所 | Graphene aerogel, preparation method and application thereof, and elution method of food-borne pathogenic microorganisms on graphene aerogel |
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Application publication date: 20171020 |