CN110152613A - A kind of aeroge adsorbent and preparation method thereof - Google Patents
A kind of aeroge adsorbent and preparation method thereof Download PDFInfo
- Publication number
- CN110152613A CN110152613A CN201810339152.2A CN201810339152A CN110152613A CN 110152613 A CN110152613 A CN 110152613A CN 201810339152 A CN201810339152 A CN 201810339152A CN 110152613 A CN110152613 A CN 110152613A
- Authority
- CN
- China
- Prior art keywords
- aeroge
- uranium
- freeze
- organically
- graphene oxide
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Classifications
-
- 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
-
- 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
-
- 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
- B01J20/28047—Gels
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Dispersion Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The present invention provides a kind of aeroge adsorbents and preparation method thereof.Organo montmorillonite and graphene oxide are prepared into aeroge using freeze-drying by the present invention.Aeroge characterization the experimental results showed that, aeroge adsorbent provided by the invention has flourishing pore structure and huge specific surface area.Using in aeroge Adsorption aqueous solution provided by the invention uranium the experimental results showed that, aeroge provided by the invention has good absorption property, when the mass ratio of GO/ organically-modified MMT in aeroge is 8:2, the removal rate of uranium reaches maximum, is 96.34%；The most economical mass ratio of GO/ organically-modified MMT is 1:1, at this point, the best solid-to-liquid ratio m/v of aeroge and uranium solution is 1.5g/l, uranium removal rate is 91.02%.
Description
Technical field
The invention belongs to new material development fields, and in particular to a kind of aeroge adsorbent and preparation method thereof.
Background technique
According to China " nuclear power Long-and Medium-term Development plan (2005-2020) " and " in defense-related science, technology and industry it is long-term it is scientific with
Technical development plan outline (2006-2020) ", in order to meet the needs of nuclear energy fast development and national defense construction, China is still needed to greatly
Power develops nuclear energy, increases the exploitation to uranium ore resource and selects smelting.Although nuclear energy is referred to as clean energy resource, potential nuclear pollution
It still has.A large amount of uranium-containing waste water will constitute very big threat to environment for human survival and social development.Therefore, understand uranium to exist
Transport And Transformation process in surrounding medium, seek a kind of effective uranium-containing waste water processing method have become it is urgently to be resolved
Problem.
All the time, domestic and foreign scholars have done a large amount of research to the processing method of uranium-containing waste water, and absorption method can be grasped because of it
The property made is strong, the at low cost, advantages such as effect is good, most widely used in uranium-containing waste water processing.Adsorbent can be divided into inorganic adsorbent, have
Machine adsorbent, compound adsorbent.Inorganic adsorbent is very common in water process inhale since its is from a wealth of sources, cost is relatively low
Attached dose.According to source difference, current common inorganic adsorbent mainly has following three classes:
(1) natural crystal
R.Donat et al. has studied natural sepiolite to the adsorption capacity of uranium, and result of study shows natural sepiolite
Specific surface area (338m with higher2/ g) and adsorption capacity (34.61mg/g).Shuguang Deng et al. has studied naturally
Absorption property of the zeolite to uranium in water body.This natural adsorbent, which has irregular pattern, to be shown to the characterization of adsorbent, ratio
Surface area is 18m2/ g, silica alumina ratio 5, Adsorption experimental results are shown in uranium initial concentration 5mg/L, and adsorbent is to uranium when pH is 6
Removal effect it is best.Although natural mineral matter can be used for the uranium in adsorbed water body, but absorption of these minerals to uranium
The universal lower and time of equilibrium adsorption of capacity is longer.This is difficult to realize minerals to the uranium pollution processing of water body and the extraction of uranium from seawater
Practical application.People are studied how to be modified the uranium absorption performance that natural minerals can be improved thus.Such as Marek
Bentonite is modified by Majdan et al. with HDTMA, and the XRD of product is as the result is shown as the increase of HDTMA dosage is modified
The interlamellar spacing of bentonite is gradually increased, so that more conducively uranyl ion enters bentonite interlayer, is reached and is increased adsorption capacity
Purpose.Sepiolites is modified with acid processing and heat-treating methods by Ayben Kilislioglu et al. respectively, and will
Modified product is used for uranium absorption, utilizes hydrochloric acid and heat treatment can increase sepiolites to a certain extent as the result is shown
To the adsorption capacity of uranium, and declined instead with adsorption capacity of the sepiolites after sulfuric acid treatment to uranium.
(2) metal oxide
The metal oxides such as titanium dioxide, aluminium oxide and iron oxide are the most extensive to the research of uranium absorption performance.Each national literature
The performance and mechanism that person is used to remove uranium in water body to them have carried out systematic research.By taking titanium dioxide as an example,
M.JosickComarmond et al. has studied specific surface area, the surface charge TiO different with impurities2Uranyl ion is inhaled
The influence of attached performance, the subsequent author have studied Fe again2O3Addition to TiO2The influence of adsorption uranium performance.G.Lefevre et al.
TiO in acid condition is studied using attenuated total reflection Fourier transform infrared spectrometry (ATR-IR)2In H2O and D2To uranium in O
Absorption, as the result is shown under weak acid to neutrallty condition, uranyl ion is in TiO2The absorption on surface rely primarily on adsorbent surface and
The terpolymer that two uranyl ions are formed.
(3) carbon material
It by the research that carbon material is used as uranium absorption agent is started in last century end.Wherein, most commonly seen adsorbent is
Active carbon, active carbon has preferable treatment effect to uranium in water body, but involves great expense.Ceren K ü tahyal et al. is respectively with wood
Charcoal and olivine are that raw material prepares active carbon, and resulting active carbon has higher removal rate to uranium in water body, and saturation absorption is held
Amount is respectively 18,40.8mg/g.The emerging carbon material such as carbon nanotube and graphite oxide pollutant process field application also by
Stepping enters the eyes of people.A.Schierz and Weiqun Shi et al. has studied carbon nanotube and graphite oxide to water body respectively
The absorption property of middle uranium, two kinds of carbon materials respectively reach 500 and 300mg/g to the saturated adsorption capacity of uranium.Graphene oxide
Large specific surface area has excellent absorption property to uranium in water body containing a large amount of hydroxyl and carboxylic group and epoxy-functional,
But it equally involves great expense.
Summary of the invention
The present invention is based on the special spatial coordination structures of uranyl ion, utilize the layer structure of graphene oxide, high ratio
Surface area and surface functional group abundant, the layer structure of organo montmorillonite, high specific surface area and cationic exchangeability characteristic,
Prepare it is a kind of with the Novel air gel adsorber GO/ organically-modified MMT that environmental-friendly, absorption property is good and preparation cost is low,
To carry out Study on adsorption properties to the uranium in waste water, for uranium-containing waste water processing provide a kind of novel reliable adsorbent material with
Processing approach.
It is an object of the present invention to provide a kind of aeroge, the aeroge includes organo montmorillonite and graphite oxide
Alkene.
Specifically, the organo montmorillonite includes the montmorillonite modified through organic compound.
Specifically, the organic compound is cetyl trimethylammonium bromide.
Specifically, the mass ratio of the graphene oxide and organo montmorillonite is 2:8~9:1.
Specifically, the mass ratio of the graphene oxide and organo montmorillonite is 1:1~8:2.
Specifically, the mass ratio of the graphene oxide and organo montmorillonite is 1:1 or the graphene oxide and organic
The mass ratio of montmorillonite is 8:2.
Specifically, the preparation method of the aeroge includes: using freeze-drying by organo montmorillonite and graphite oxide
Alkene is prepared into aeroge.
Specifically, the preparation method of the aeroge includes:
(1) disperse: dispersing organo montmorillonite in deionized water, stir 2h-4h；
(2) ultrasonic: by ultrasound 2h under dispersion liquid room temperature obtained by step (1)；
(3) it mixes: adding graphene oxide into step (2) dispersion liquid, then stir 2h；
(4) ultrasonic: by mixed liquor room temperature ultrasound 2h obtained by step (3)；
(5) dry: 55 DEG C of the resulting mixed liquor of step (4) to be dried under vacuum to sticky；
(6) ultrasonic: by the resulting mixed liquor room temperature ultrasound 2h of step (5)；
(7) it freezes: by -70 DEG C of freezing 12h of the resulting mixed liquor of step (6)；
(8) be freeze-dried: step (7) resulting materials are put into freeze drier, vacuum refrigeration at -50 DEG C~-70 DEG C, directly
It is lyophilized completely to material.
It is a further object to provide a kind of preparation methods of aeroge, which comprises dry using freezing
Organo montmorillonite and graphene oxide are prepared into aeroge by dry method.
Specifically, the organo montmorillonite includes the montmorillonite modified through organic compound；The organic compound is ten
Six alkyl trimethyl ammonium bromides；The mass ratio of the graphene oxide and organo montmorillonite is 2:8~9:1；Specifically, the oxygen
The mass ratio of graphite alkene and organo montmorillonite is 1:1~8:2；Specifically, the matter of the graphene oxide and organo montmorillonite
Amount is than being 1:1 or the mass ratio of the graphene oxide and organo montmorillonite is 8:2.
Specifically, the described method includes:
(1) disperse: dispersing organo montmorillonite in deionized water, stir 2h-4h；
(2) ultrasonic: by ultrasound 2h under dispersion liquid room temperature obtained by step (1)；
(3) it mixes: adding graphene oxide into step (2) dispersion liquid, then stir 2h；
(4) ultrasonic: by mixed liquor room temperature ultrasound 2h obtained by step (3)；
(5) dry: 55 DEG C of the resulting mixed liquor of step (4) to be dried under vacuum to sticky；
(6) ultrasonic: by the resulting mixed liquor room temperature ultrasound 2h of step (5)；
(7) it freezes: by -70 DEG C of freezing 12h of the resulting mixed liquor of step (6)；
(8) be freeze-dried: step (7) resulting materials are put into freeze drier, vacuum refrigeration at -50 DEG C~-70 DEG C, directly
It is lyophilized completely to material.
Of the invention a further object is provides a kind of method of absorption and/or removal uranium, the method includes it is following 1)-
At least one of 4):
1) using any aeroge absorption of the present invention and/or removal uranium；
2) uranium is adsorbed and/or removed using the aeroge that any the method for the present invention is directly prepared；
3) described when the uranium is the uranium in solution using any aeroge absorption of the present invention and/or removal uranium
The mass volume ratio of aeroge and the solution is 1.5g/l；
4) it adsorbs using the aeroge that any the method for the present invention is directly prepared and/or removes uranium, when the uranium
When for uranium in solution, the mass volume ratio of the aeroge and the solution is 1.5g/l.
Specifically, the method also includes, when the uranium is the uranium in solution, by any aeroge of the present invention or
The aeroge that any the method for the present invention is directly prepared is placed in the solution, adjusts the pH value of the solution to 4-6,
1h or more is shaken in water-bath；Specifically, carrying out water-bath concussion under normal temperature condition；Specifically, adjusting the pH value of the solution to 5.5；
Specifically, 4h is shaken in water-bath.
It is also another object of the present invention to provide the present invention any aeroge, any the methods of the invention to answer
With.
Specifically, the application includes following 1) -3) at least one of in application:
1) adsorption uranium；
2) adsorbent or its Related product are prepared；
3) uranium absorption agent or its Related product are prepared.
Montmorillonite (MMT) is the earthy mine formed by the silicate plate layer heap product of the nano thickness surface (1nm or so) electrification
Object, structure cell are constituted by pressing from both sides one layer of alumina octahedral between two layers of oxygen-octahedron, belong to 2:1 type silicate.Due to crystal structure spy
Very, so having unique property, such as surface polarity is big, ion-exchange capacity is strong.By inorganic ions institute table in montmorillonite
The hydrophilic and oleophobic property revealed is unfavorable for it and disperses in the polymer, so need to carry out to montmorillonite organically-modified.Carry out organic change
Property purpose be to change the polarity on montmorillonite surface, so that it is become lipophilic from hydrophily, drop low-surface-energy.Make montmorillonite simultaneously
Interlamellar spacing become larger, so that strand or monomer is entered interlayer, prepare nanocomposite.A specific embodiment of the invention makes
Montmorillonite is cetyl trimethylammonium bromide modified montmorillonoid, i.e. one of organo montmorillonite.
Graphene oxide (Grapheneoxide, abbreviation GO) is the oxidation product and derivative of graphene, structure and stone
Black alkene is similar, be single atomic layer, unlike its functional group, and mainly oxygen-containing functional group are connected on carbon skeleton, as OH,
C-O-C, C=O and COOH etc..Due to having a structure which and group, so GO can disperse well in water.In recent years, phase
Close experimental result show, GO have it is amphipathic, from graphene platelet edge to center presentation property distribution be from hydrophilic to thin
Water, therefore, graphene oxide may be present in interface, and can reduce energy between interface.GO is a kind of flexible material, has polymerization
The characteristic of object, colloid, film and amphiphatic molecule.
The principle of freeze-drying is first to freeze material, then under the vacuum condition of height, makes the moisture freezed not
It by the thawing of ice but is directly sublimed into as steam, this principle is known as ice crystal sublimation principle, and being thus freeze-dried can also cry
Do drying bu sublimation.
Novel aerogel composite provided by the invention has big specific surface area containing a large amount of functional group, can be
Quickly interact with uranyl ion in water, to the large amount of adsorption of uranium, inexpensive, preparation is simple, and it is easily de- wash, power of regeneration
It is high.
Organo montmorillonite and graphene oxide are prepared into aeroge using freeze-drying by the present invention.Aeroge characterization is real
Test the result shows that, aeroge adsorbent provided by the invention has flourishing pore structure.Utilize aeroge provided by the invention
In Adsorption aqueous solution uranium the experimental results showed that, aeroge provided by the invention have good absorption property, work as airsetting
When the mass ratio of GO/ organically-modified MMT is 8:2 in glue, the removal rate of uranium reaches maximum, is 96.34%；GO/ organically-modified MMT
Most economical mass ratio be 1:1, at this point, the best solid-to-liquid ratio m/v of aeroge and uranium solution is 1.5g/l, uranium removal rate is
91.02%.
Detailed description of the invention
It, below will be to required in embodiment or description of the prior art in order to illustrate more clearly of technical solution of the present invention
The attached drawing used is briefly described.
Fig. 1 is aeroge GO/ organically-modified MMT (GO: organically-modified MMT prepared by GO, organically-modified MMT and embodiment 1
Mass ratio be 1:1 when) SEM figure；Wherein, the SEM that Figure 1A is GO schemes；Figure 1B is that the SEM of organically-modified MMT schemes；Fig. 1 C is real
Apply the SEM figure of the aeroge GO/ organically-modified MMT (GO: when organically-modified MMT mass ratio is 1:1) of the preparation of example 1.
Fig. 2 is aeroge GO/ organically-modified MMT (GO: organically-modified MMT prepared by GO, organically-modified MMT and embodiment 1
Mass ratio be 1:1 when) infrared spectrum.
Fig. 3 is aeroge GO/ organically-modified MMT (GO: organically-modified MMT prepared by GO, organically-modified MMT and embodiment 1
Mass ratio be 1:1 when) XRD diagram.
Fig. 4 is different GO: the eliminating rate of absorption result of uranium in the uranium solution of the aeroge of organically-modified MMT mass ratio preparation
Figure.
Adsorption experimental results figure when Fig. 5 is aeroge and uranium solution different solid ratio m/v.
Specific embodiment
The present invention will be further described below in conjunction with the embodiments.
The aeroge adsorbent is the composite wood of the organo montmorillonite and graphene oxide using freeze-drying preparation
Material.
Montmorillonite used in following embodiments is cetyl trimethylammonium bromide modified montmorillonoid, i.e. organo montmorillonite
One of, this can directly be commercially available through the modified montmorillonite public of cetyl trimethylammonium bromide.For convenience of description, under
It states in embodiment and this is referred to as organically-modified MMT through the modified montmorillonite of cetyl trimethylammonium bromide.
Graphene oxide used in following embodiments (Grapheneoxide, abbreviation GO) is to utilize Hummers method, with
Graphite powder is that raw material prepares graphite oxide, then by ultrasonic disperse, graphene oxide is prepared in removing.It is used in following embodiments
The graphene oxide public can directly be commercially available.
The principle of freeze-drying preparation is first to freeze material, then under the vacuum condition of height, makes to freeze
Moisture is without the thawing of ice but is directly sublimed into as steam, this principle is known as ice crystal sublimation principle, is thus freeze-dried
Also it can be called drying bu sublimation.
The preparation of embodiment 1, aeroge
(1) preparation step of aeroge is as follows:
(1) disperse: according to GO: seven mass ratioes of organically-modified MMT: 2:8,3:7,4:6,5:5,6:4,8:2,9:1, respectively
The powdered graphene oxide and organically-modified MMT that gross mass is 500mg are weighed, the organically-modified MMT of different quality adds respectively
Enter 100ml deionized water stirring 2h-4h, obtains organically-modified MMT dispersion liquid；
(2) ultrasonic: by ultrasound 2h under organically-modified MMT dispersion liquid room temperature；
(3) it mixes: the organically-modified MMT dispersion liquid through ultrasound is added in the graphene oxide of corresponding mass, is then stirred
2h；
(4) ultrasonic: the mixed liquor room temperature ultrasound 2h that will be stirred；
(5) dry: 55 DEG C of the resulting mixed liquor of step (4) to be dried under vacuum to sticky；
(6) ultrasonic: by the resulting mixed liquor room temperature ultrasound 2h of step (5)；
(7) it freezes: by -70 DEG C of freezing 12h of the resulting mixed liquor of step (6)；
(8) be freeze-dried: step (7) resulting materials are put into freeze drier, vacuum refrigeration at -50 DEG C~-70 DEG C, directly
It is lyophilized completely to material.
(2) characterization of aeroge
Fig. 1 is the SEM figure of GO, organically-modified MMT and GO/ organically-modified MMT, can from the SEM figure of Figure 1A graphene oxide
To find out, graphene oxide is in single chip architecture.From the SEM of Figure 1B organically-modified MMT figure as can be seen that organically-modified MMT is in layer
Shape structure.Fig. 1 C is that the SEM of GO/ organically-modified MMT aeroge adsorbent schemes, and shows that Novel air gel adsorber has prosperity
Pore structure.
Fig. 2 is the infrared spectrum of GO, organically-modified MMT and GO/ organically-modified MMT.From the infared spectrum of graphene oxide
In it is found that 3416cm-1Place's absorption peak is the stretching vibration peak of O-H, 1729cm-1And 1384cm-1It is to be located at that it is corresponding, which to locate absorption peak,
The C=O stretching vibration of the carboxylic group at graphite oxide edge and the stretching vibration absworption peak of-OH, 1628cm-1The absorption peak at place is
C=C stretching vibration peak in graphene oxide, 1223cm-1And 1070cm-1Corresponding is the layer of C-O-C and graphene oxide
Between stretching vibration caused by epoxy group.It was found from the infared spectrum of organically-modified MMT, in 3628cm-1Absorption peak be
The flexible vibration peak-OH for the combination water that organically-modified MMT itself contains, 3425cm-1Appearance be organically-modified MMT Al-0H and
Caused by the intramolecular hydrogen bond hydroxyl association peak of Si-OH, 1641cm-1Absorption peak be-OH key flexural vibrations peak, 2926cm-1With
2852cm-1For the methyl of organically-modified MMT and the stretching vibration peak of methylene, 1472cm-1It shakes for the deformation of methyl and methylene
Dynamic peak, 1033cm-1For the Si-O stretching vibration peak in organically-modified MMT, 400-600cm-1Absorption peak be Si-O and Al-0
Flexural vibrations peak.It is found that there is 1729cm from the infared spectrum of GO/ organically-modified MMT-1、1628cm-1、1384cm-1、
1223cm-1And 1070cm-1The corresponding characteristic absorption peak of GO, while the intensity of the characteristic absorption peak of organically-modified MMT subtracts relatively
It is weak, illustrate that GO is effectively compound with organically-modified MMT.
Fig. 3 is the XRD diagram of GO, organically-modified MMT and GO/ organically-modified MMT, and comparison GO and GO/ organically-modified MMT can be with
To find out, prepared GO/ organically-modified MMT composite material shows the characteristic peak of GO, show there is GO in the composite material of preparation,
However, comparing organically-modified MMT and GO/ organically-modified MMT, in the XRD spectra of composite material GO/ organically-modified MMT not
Occur 21.33 °, 34.95 ° and 61.65 ° of characteristic peak of organically-modified MMT, the reason is that the strong diffraction maximum of GO mask it is organically-modified
The weak diffraction maximum of MMT, so the characteristic peak of organically-modified MMT does not display all.
(3) eliminating rate of absorption for the aeroge that the GO of different quality ratio and organically-modified MMT are prepared
Mass ratio with GO and organically-modified MMT is respectively that 2:8,3:7,4:6,1:1,6:4,8:2 and 9:1 carry out hydrogel
The preparation of adsorbent, the composite material 20mg for taking different proportion to prepare respectively, being added to 10ml concentration is 4.5*10-4Mol/L is (i.e.
In uranium solution 107.1mg/L), pH is adjusted to 5.5 or so.Under normal temperature condition, water-bath concussion 4h is adsorbed, and absorption is completed
Afterwards, it draws 1.5ml or so supernatant and is added to 12000r/min in the centrifuge tube of 1.5ml, then time 6min takes in centrifuge tube
0.1% azo arsenic of 5ml is added in 25ml volumetric flask in supernatant 1.5ml, adds 1ml 0.5ml/L hydrochloric acid, dilutes constant volume.
Absorbance is measured with ultraviolet specrophotometer.Experimental result is shown in Fig. 4.
As seen from Figure 4: with the raising of GO content, the removal rate of uranium is gradually increased, when GO/ organically-modified MMT
When GO and organically-modified MMT mass ratio are 8:2, the removal rate of uranium reaches maximum, is 96.34%；Later with the increasing of GO content
Add removal rate to decline, therefore deduces that optimal GO/ organically-modified MMT mass ratio is 8:2；But in view of GO/ is organically-modified
When the content of GO increases to 8:2 from 1:1 in MMT, removal rate merely adds 4% or so, and the price of GO be it is somewhat expensive, therefore
It is considered as GO and organically-modified MMT mass ratio economically as the adsorbent of 1:1.
The best solid-to-liquid ratio m/v of embodiment 2, aeroge and uranium solution determines experiment
Take 2 respectively, 4,10,15,20,30, (GO/ organically-modified MMT mass ratio is the aeroge adsorbent for preparing of 40mg
1:1), it is added in the uranium solution that 20ml concentration is 100mg/L, obtains the mass volume ratio of the aeroge adsorbent and uranium solution
M/v is respectively 0.1,0.2,0.5,0.75,1,1.5,2 solution, and pH is adjusted to 5.5 or so.Under normal temperature condition, 4h is shaken in water-bath
It is adsorbed, after the completion of absorption, draws 1.5ml or so supernatant and be added to 12000r/min in the centrifuge tube of 1.5ml, time
Then 6min takes supernatant 1ml in centrifuge tube that 0.1% azo arsenic of 5ml is added, adds 1ml in 25ml volumetric flask
0.5ml/L hydrochloric acid dilutes constant volume.Corresponding absorbance is measured again by concentrations above-absorbance mark with ultraviolet specrophotometer
Remaining uranium concentration calculates corresponding removal rate in turn at the end of directrix curve calculates absorption, as a result as shown in Figure 5.
As seen from Figure 5: with the raising of m/v, the removal rate of uranium, which gradually increases, finally to tend to balance, and reason may be
Since in the case where adsorption density and constant other conditions, adsorbent dosage increases, GO integrally adsorbs some bit quantities and increases
Add, so the opposite of adsorbate distribution of unit area absorption point absorption tails off, and the GO adsorbance of unit mass declines.When
When m/v reaches 1.5g/l, uranium removal rate reaches maximum, is 91.02%, therefore deduces that best m/v is 1.5g/l.
Embodiments of the present invention above described embodiment only expresses, the description thereof is more specific and detailed, but can not
Therefore limitations on the scope of the patent of the present invention are interpreted as, as long as skill obtained in the form of equivalent substitutions or equivalent transformations
Art scheme should all be fallen within the scope and spirit of the invention.
Claims (10)
1. a kind of aeroge, it is characterised in that: the aeroge includes organo montmorillonite and graphene oxide.
2. aeroge according to claim 1, which is characterized in that the organo montmorillonite includes modified through organic compound
Montmorillonite.
3. aeroge according to claim 2, which is characterized in that the organic compound is cetyl trimethyl bromination
Ammonium.
4. aeroge according to claim 1 to 3, which is characterized in that the graphene oxide and organo montmorillonite
Mass ratio is 2:8~9:1.
5. aeroge according to claim 1 to 4, which is characterized in that the preparation method of the aeroge includes: to adopt
Organo montmorillonite and graphene oxide are prepared into aeroge with freeze-drying.
6. -5 any aeroge according to claim 1, which is characterized in that the preparation method of the aeroge includes:
(1) disperse: dispersing organo montmorillonite in deionized water, stir 2h-4h；
(2) ultrasonic: by ultrasound 2h under dispersion liquid room temperature obtained by step (1)；
(3) it mixes: adding graphene oxide into step (2) dispersion liquid, then stir 2h；
(4) ultrasonic: by mixed liquor room temperature ultrasound 2h obtained by step (3)；
(5) dry: 55 DEG C of the resulting mixed liquor of step (4) to be dried under vacuum to sticky；
(6) ultrasonic: by the resulting mixed liquor room temperature ultrasound 2h of step (5)；
(7) it freezes: by -70 DEG C of freezing 12h of the resulting mixed liquor of step (6)；
(8) be freeze-dried: step (7) resulting materials are put into freeze drier, vacuum refrigeration at -50 DEG C~-70 DEG C, until material
Material freeze-drying completely.
7. a kind of preparation method of aeroge, which is characterized in that the described method includes: using freeze-drying by organo montmorillonite
Aeroge is prepared into graphene oxide.
8. preparation method according to claim 7, which is characterized in that the described method includes:
(1) disperse: dispersing organo montmorillonite in deionized water, stir 2h-4h；
(2) ultrasonic: by ultrasound 2h under dispersion liquid room temperature obtained by step (1)；
(3) it mixes: adding graphene oxide into step (2) dispersion liquid, then stir 2h；
(4) ultrasonic: by mixed liquor room temperature ultrasound 2h obtained by step (3)；
(5) dry: 55 DEG C of the resulting mixed liquor of step (4) to be dried under vacuum to sticky；
(6) ultrasonic: by the resulting mixed liquor room temperature ultrasound 2h of step (5)；
(7) it freezes: by -70 DEG C of freezing 12h of the resulting mixed liquor of step (6)；
(8) be freeze-dried: step (7) resulting materials are put into freeze drier, vacuum refrigeration at -50 DEG C~-70 DEG C, until material
Material freeze-drying completely.
At least one of 9. a kind of method of absorption and/or removal uranium, which is characterized in that the method includes following 1) -4):
1) using any aeroge absorption of claim 1-6 and/or removal uranium；
2) uranium is adsorbed and/or removed using the aeroge that any the method for claim 7-8 is directly prepared；
3) using any aeroge absorption of claim 1-6 and/or removal uranium, when the uranium is the uranium in solution, institute
The mass volume ratio for stating aeroge and the solution is 1.5g/l；
4) it adsorbs using the aeroge that any the method for claim 7-8 is directly prepared and/or removes uranium, when the uranium
When for uranium in solution, the mass volume ratio of the aeroge and the solution is 1.5g/l.
10. the application of claim 1-6 any aeroge, any the method for claim 7-9.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810339152.2A CN110152613A (en) | 2018-04-16 | 2018-04-16 | A kind of aeroge adsorbent and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810339152.2A CN110152613A (en) | 2018-04-16 | 2018-04-16 | A kind of aeroge adsorbent and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110152613A true CN110152613A (en) | 2019-08-23 |
Family
ID=67644855
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810339152.2A Pending CN110152613A (en) | 2018-04-16 | 2018-04-16 | A kind of aeroge adsorbent and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110152613A (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787773A (en) * | 2019-09-30 | 2020-02-14 | 南京工业大学 | Method for compositely modifying montmorillonite aerogel material by using blocky chitosan |
| CN111422840A (en) * | 2020-04-01 | 2020-07-17 | 东华理工大学 | Phosphorus/graphene three-dimensional aerogel material and preparation method and application thereof |
| CN111450808A (en) * | 2020-04-13 | 2020-07-28 | 东华理工大学 | Phosphonic acid functionalized polymer/graphene nanoribbon composite aerogel and preparation method and application thereof |
| CN112076727A (en) * | 2020-08-21 | 2020-12-15 | 温州大学 | Heavy metal pollution repairing agent and preparation method thereof |
| CN112573529A (en) * | 2020-12-15 | 2021-03-30 | 江苏中腾石英材料科技股份有限公司 | Preparation process and equipment of high-purity low-radiation spherical silicon micropowder for 5G base station |
| CN113526497A (en) * | 2021-08-11 | 2021-10-22 | 洛阳理工学院 | Preparation method of organic modified vermiculite/graphene composite aerogel |
| CN114181411A (en) * | 2021-12-10 | 2022-03-15 | 成都德斐生物科技有限公司 | Hydrogel material with high cold/heat insulation effect |
| CN114950354A (en) * | 2021-11-24 | 2022-08-30 | 东华理工大学 | Uranium adsorbent based on porous cobalt sulfide/carbon aerogel material and preparation method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104772113A (en) * | 2015-03-11 | 2015-07-15 | 华南理工大学 | Graphene / montmorillonite nano composite material, and preparation method and application thereof |
| CN105195090A (en) * | 2015-09-21 | 2015-12-30 | 华南理工大学 | Oxidized graphene/clay composite material and preparation method and application thereof |
| CN107159118A (en) * | 2017-06-09 | 2017-09-15 | 南华大学 | A kind of efficient uranium absorption agent of bentonite grafted graphene oxide and preparation method thereof |
| WO2017173176A1 (en) * | 2016-04-01 | 2017-10-05 | Entropy Solutions Llc | Microencapsulated composite phase change materials |
| CN107281982A (en) * | 2016-04-05 | 2017-10-24 | 中国科学院化学研究所 | A kind of adjustable graphene of hydrophilic and hydrophobic/clay composite elastic aeroge and preparation method thereof |
| CN107790074A (en) * | 2016-08-31 | 2018-03-13 | 天津城建大学 | A kind of halloysite clay doped graphene aeroge and preparation method thereof |
-
2018
- 2018-04-16 CN CN201810339152.2A patent/CN110152613A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104772113A (en) * | 2015-03-11 | 2015-07-15 | 华南理工大学 | Graphene / montmorillonite nano composite material, and preparation method and application thereof |
| CN105195090A (en) * | 2015-09-21 | 2015-12-30 | 华南理工大学 | Oxidized graphene/clay composite material and preparation method and application thereof |
| WO2017173176A1 (en) * | 2016-04-01 | 2017-10-05 | Entropy Solutions Llc | Microencapsulated composite phase change materials |
| CN107281982A (en) * | 2016-04-05 | 2017-10-24 | 中国科学院化学研究所 | A kind of adjustable graphene of hydrophilic and hydrophobic/clay composite elastic aeroge and preparation method thereof |
| CN107790074A (en) * | 2016-08-31 | 2018-03-13 | 天津城建大学 | A kind of halloysite clay doped graphene aeroge and preparation method thereof |
| CN107159118A (en) * | 2017-06-09 | 2017-09-15 | 南华大学 | A kind of efficient uranium absorption agent of bentonite grafted graphene oxide and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| YUNYUN ZHANG ET AL.: "The utilization of a three-dimensional reduced graphene oxide and montmorillonite composite aerogel as a multifunctional agent for wastewater treatment", 《RSC ADVANCES》 * |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110787773A (en) * | 2019-09-30 | 2020-02-14 | 南京工业大学 | Method for compositely modifying montmorillonite aerogel material by using blocky chitosan |
| CN111422840A (en) * | 2020-04-01 | 2020-07-17 | 东华理工大学 | Phosphorus/graphene three-dimensional aerogel material and preparation method and application thereof |
| CN111450808A (en) * | 2020-04-13 | 2020-07-28 | 东华理工大学 | Phosphonic acid functionalized polymer/graphene nanoribbon composite aerogel and preparation method and application thereof |
| CN112076727A (en) * | 2020-08-21 | 2020-12-15 | 温州大学 | Heavy metal pollution repairing agent and preparation method thereof |
| CN112573529A (en) * | 2020-12-15 | 2021-03-30 | 江苏中腾石英材料科技股份有限公司 | Preparation process and equipment of high-purity low-radiation spherical silicon micropowder for 5G base station |
| WO2022127132A1 (en) * | 2020-12-15 | 2022-06-23 | 江苏中腾石英材料科技股份有限公司 | Preparation process and device for high-purity low-radiation spherical silicon micropowder for use in 5g base station |
| CN112573529B (en) * | 2020-12-15 | 2023-08-15 | 江苏中腾石英材料科技股份有限公司 | Preparation process and equipment of high-purity low-radiation spherical silicon micro powder for 5G base station |
| CN113526497A (en) * | 2021-08-11 | 2021-10-22 | 洛阳理工学院 | Preparation method of organic modified vermiculite/graphene composite aerogel |
| CN114950354A (en) * | 2021-11-24 | 2022-08-30 | 东华理工大学 | Uranium adsorbent based on porous cobalt sulfide/carbon aerogel material and preparation method thereof |
| CN114181411A (en) * | 2021-12-10 | 2022-03-15 | 成都德斐生物科技有限公司 | Hydrogel material with high cold/heat insulation effect |
| CN114181411B (en) * | 2021-12-10 | 2023-12-08 | 马素德 | Hydrogel material with high cold/heat insulation effect |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110152613A (en) | A kind of aeroge adsorbent and preparation method thereof | |
| Jia et al. | Adsorption removal and reuse of phosphate from wastewater using a novel adsorbent of lanthanum-modified platanus biochar | |
| Huang et al. | Optimization of preparation technology for modified coal fly ash and its adsorption properties for Cd2+ | |
| Zhang et al. | Fluoride adsorption from aqueous solution by magnetic core-shell Fe3O4@ alginate-La particles fabricated via electro-coextrusion | |
| Liu et al. | Removal of uranium from aqueous solution by a low cost and high-efficient adsorbent | |
| Peng et al. | Montmorillonite–Cu (II)/Fe (III) oxides magnetic material as adsorbent for removal of humic acid and its thermal regeneration | |
| Li et al. | Removal of copper from aqueous solution by carbon nanotube/calcium alginate composites | |
| Kausar et al. | Equilibrium, kinetic and thermodynamic studies on the removal of U (VI) by low cost agricultural waste | |
| CN109589933B (en) | Magnetic nano composite material UiO-66/Fe3O4Preparation method and application of/GO | |
| Rajbhandari et al. | Nanoporous activated carbon derived from Lapsi (Choerospondias Axillaris) seed stone for the removal of arsenic from water | |
| Savova et al. | The influence of the texture and surface properties of carbon adsorbents obtained from biomass products on the adsorption of manganese ions from aqueous solution | |
| CN100460056C (en) | Method for preparing sulfate akaganeite adsorbent for de-arsenation | |
| CN106000297A (en) | Graphene loaded zirconium oxide composite material, preparing method thereof, and application thereof as desulfurizer adsorbent | |
| Krishnan et al. | Kinetic and equilibrium modeling of liquid‐phase adsorption of lead and lead chelates on activated carbons | |
| Omidi et al. | Biochar obtained from cinnamon and cannabis as effective adsorbents for removal of lead ions from water | |
| CN104549146B (en) | Multi-walled carbon nanotube nano composite material of aluminum oxide modification and its preparation method and application | |
| CN108636378A (en) | A kind of organic amino-functionalization There-dimensional ordered macroporous materials CO2Adsorbent and preparation method thereof | |
| Donat et al. | Adsorption and thermodynamic behavior of uranium (VI) on Ulva sp.-Na bentonite composite adsorbent | |
| Zhang et al. | Removal of uranium (VI) from aqueous solutions by carboxyl-rich hydrothermal carbon spheres through low-temperature heat treatment in air | |
| CN106824062A (en) | A kind of lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent and preparation method thereof | |
| CN105854744A (en) | Magnetic nanoparticle/SiO2 aerogel and preparation method thereof and method for treating high level liquid waste | |
| Jiexin et al. | Preparation of sulfhydryl functionalized magnetic SBA-15 and its high-efficiency adsorption on uranyl ion in solution | |
| CN110743503A (en) | PCN metal organic framework and graphene oxide composite adsorption material and preparation method thereof | |
| WO2021143275A1 (en) | Adsorbent based on graphene oxide, and preparation method therefor and application thereof | |
| Yuan et al. | Adsorption effect and the removal mechanism of silicate composite biochar particles on cadmium in soil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190823 |