CN110354766A - A kind of cellulose/graphene nano composite aerogel preparation method and application - Google Patents
A kind of cellulose/graphene nano composite aerogel preparation method and application Download PDFInfo
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- CN110354766A CN110354766A CN201910649073.6A CN201910649073A CN110354766A CN 110354766 A CN110354766 A CN 110354766A CN 201910649073 A CN201910649073 A CN 201910649073A CN 110354766 A CN110354766 A CN 110354766A
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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
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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
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/28047—Gels
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- 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
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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- 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
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- 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
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention discloses a kind of cellulose/graphene nanometer sheet composite aerogel preparation methods, cellulosic material and graphite are added in solvent first, under the action of mechanical force, graphite is removed into graphene nanometer sheet, in the colloidal sol that the graphene nanometer sheet of removing is dispersed in cellulose or cellulose derivative simultaneously and solvent is constituted, obtain cellulose/graphene nano complex sol, complex sol is placed in alcoholic solvent again and is sufficiently exchanged, finally rinsed with deionized water to neutrality, it is dry, obtain cellulose/graphene nano composite aerogel.Cellulose/graphene nanometer sheet composite aerogel in solution ion and dyestuff have good adsorption effect.It prepares cellulose/graphene sol by one-step method, without preparing graphene nanometer sheet in advance, reduces preparation step, the use for reducing solvent shortens preparation time, improves dispersibility of the graphene in cellulose sol, it avoids graphene from reuniting, and then improves the performance of product.
Description
Technical field:
The present invention relates to a kind of cellulose/graphene nano composite aerogel preparation method and applications, belong to biomass
Material, high molecular material and Environmental Chemistry chemical industry interleaving techniques field.
Background technique:
Heavy metal ion has been on the rise to the pollution of environment and the harm of human health.With the rapid development of industry
With the quickening of urbanization process, more and more industry and mining waste water, sanitary sewage etc. be not appropriately processed with regard to direct emission, draws
Play water pollution.Studies have shown that absorption is considered as the method for the most effective a large amount of water pollutions of processing.Absorption method refers to utilization
Porous solid substance adsorbs heavy metal ion and organic dyestuff in water, achievees the purpose that processing, reduction or even elimination, has
Efficient advantage high, speed is fast, at low cost and wide applicability.
Cellulose aerogels based on natural biological resource are low cost, biodegradable and efficient adsorbent.Fiber
Element is to be distributed that most wide, reserves are most abundant and reproducible natural high molecular substance in nature.Airsetting from cellulose resource
Glue, which has, is easy bonded different functional group, internal porous structure, environment friendly, at low cost and high specific surface area etc.
Unique advantage, therefore, cellulose aerogels have wide utilization space in heavy metal ion adsorbed field.
Cellulose aerogels are while keeping traditional aeroge basic structure characteristic, and it is distinctive to have incorporated cellulose
The advantages that raw material green is renewable, biodegradable and flexible, easy processing, so that cellulose aerogels rapidly become airsetting
The new hot spot of glue research field, however cellulose aerogels are low etc. there are poor mechanical property and adsorption efficiency applied to water process
Disadvantage, the inorganic nano sheet haveing excellent performance, which is introduced cellulose aerogels, can prepare excellent mechanical properties and high absorption property fibre
Tie up plain composite aerogel.
Graphene is one kind by single layer sp2Hydbridized carbon atoms are closely packed together the honeycomb to be formed by covalent bond
Two-dimentional (2D) nanometer sheet, because of specific surface area with higher and mechanical property, the heavy metal that is applied in water as adsorbent
With the Adsorption of the pollutants such as organic matter.However mechanical stripping method is to utilize glue in the common preparation method of graphene at present
Graphene film is adhered on adhesive tape by band removing highly oriented pyrolytic graphite, and graphene platelet is made in the operation by series.It is this
Although cost is relatively low for the graphene that method is produced, uneven, low output, cleannes are not high, therefore also limit his answer
With not can be carried out industrialized production.During chemistry redox method prepares redox graphene, use a large amount of strong
Oxidant and noxious material, such as the concentrated sulfuric acid, potassium permanganate, hydrazine hydrate and sodium borohydride, wherein hydrazine hydrate have severe toxicity and
It is highly unstable, there is biggish risk in use process, do not meet the requirement of safety and environmental protection.Pass through microwave heating chemistry
Graphene can be in high volume made in vapour deposition process, but the production cost is very high for this method, and during the preparation process can
Extra carbide and agraphitic carbon are generated in substrate.SiC epitaxial growth method needs vacuum or atmosphere of inert gases, together
When need ultra-high temperature to heat, so while SiC epitaxial growth method sounds very attractive, but these stringent systems
Standby condition limits its application range in practice.
Graphene nanometer sheet is the inorganic nano sheet for preferably enhancing in cellulose aerogels with increasing adsorptivity.However
Effective preparation of graphene nanometer sheet and the dispersion in cellulose gel are to first have to solve the problems, such as.We pass through fiber
Element mechanical stripping one-step method in dissolution solvent is prepared for cellulose/graphene nano complex sol, graphene in complex sol
It is connected with each other under certain condition with cellulose, and is full of network gap using solvent as decentralized medium, cellulose effectively promotees
Effective dispersion into the removing of graphene nanometer sheet and in colloidal sol, it is compound that one-step method prepares cellulose/graphene nano
Gel is further dried and prepares cellulose/graphene nanometer sheet composite aerogel.The composite aerogel can not only be abundant
Using the intrinsic physicochemical property of single-layer graphene, solves the problems, such as that graphene film interlayer is easy to reunite, also impart aeroge
Uniformly intensive porosity, can greatly improve adsorption effect, greatly widen cellulose and grapheme material in terms of absorption
Application range.With being constantly improve and continually developed to new adsorbent, absorption method to existing performance of the adsorbent
It will exceed plus wide in the future development in the field and application prospect.
Summary of the invention:
Present invention aims to overcome that disadvantage of the existing technology, seeking design can be improved graphene nanometer sheet point
Property is dissipated, avoids graphene nanometer sheet from reuniting, and cellulose/graphene nanometer sheet composite aerogel system that the operating process time is short
Preparation Method.
To achieve the goals above, the present invention discloses following technical scheme:
A kind of cellulose/graphene nanometer sheet composite aerogel preparation method, specifically includes the following steps:
(1) cellulosic material and graphite are added in solvent, then under the action of mechanical force, graphite is removed into graphite
Alkene nanometer sheet, at the same remove graphene nanometer sheet be dispersed in cellulose or cellulose derivative constituted with solvent it is molten
In glue, cellulose/graphene nano complex sol is obtained, the solvent can dissolve cellulosic material;
(2) complex sol is placed in alcoholic solvent and is sufficiently exchanged, formed gel, then rinsed with deionized water to neutrality,
It is dry, obtain cellulose/graphene nano composite aerogel.
The cellulosic material includes but is not limited to the native cellulose, modified cellulose and its derivative of separate sources
One of or it is a variety of.The graphite includes but is not limited to natural graphite, artificial graphite, blocky graphite, crystalline flake graphite, expansion
Graphite one or more of them.The mechanical force includes but is not limited to that strength is ultrasonic, ball milling, mill, magnetic agitation, and screw rod stirs
One of mix.The drying mode includes but is not limited to constant pressure and dry, freeze-drying, supercritical CO2Dry, spray drying
One of.
The concentration of the cellulose is 2%-8%, and the content of graphene nanometer sheet is the 0.1%-5% of cellulose.
The solvent selection alkali urea system and ionic liquid, e.g., 1- normal-butyl -3- methylimidazolium chloride, 1.3- diformazan
Base imidazoleacetic acid salt, 1.3- methylimidazole hydroxyl acetate.
The alcoholic solvent is one of ethyl alcohol, propyl alcohol, the tert-butyl alcohol or a variety of.
A kind of cellulose/graphene nanometer sheet composite aerogel is for the ion and dyestuff in adsorbent solution.Especially pair
Cu2+、Pb2+、Cr3+、Cd2+、Hg2+、Ni2+、Mn2+、Fe2+、Fe3+、Zn2+, F-,AsO4 3-, Cr2O7 2-Plasma has good go
Except effect.
A kind of regeneration method of cellulose/graphene nanometer sheet composite aerogel, specifically includes the following steps:
(1) aeroge for being up to the balance of adsorption equilibrium is filtered out from solution, is washed with distilled water, and removal is not inhaled
Attached ion or dyestuff;
(2) it is then successively immersed in 50mL 0.1M HCl and 0.1M NaOH solution, regenerates 1 hour, be washed to
Property, desorption is completed, is squeezed and realizes composite aerogel regeneration.
Compared with the prior art, the invention has the following beneficial effects: (1) one-step method prepares cellulose/graphene sol,
Without preparing graphene nanometer sheet in advance, reduces preparation step, reduce the use of solvent, shorten preparation time, graphene
Nanometer sheet is scattered in cellulose gel in the form of single layer or several layers, is improved dispersibility of the graphene in cellulose sol, is kept away
Exempt from graphene reunion, and then improves the performance of product;(2) cellulose/graphene aerogel aperture structure is more stable,
Its number that can be recycled is improved, be recycled number 40 times or more, and adsorption effect when reuse is improved, it follows
Ring keeps 70-80% or more using 10 adsorption capacities.
Detailed description of the invention:
Fig. 1 is cellulose/graphene nanometer sheet aeroge digital photograph prepared by the embodiment of the present invention 1.
Fig. 2 is cellulose/graphene nanometer sheet aeroge stereoscan photograph prepared by the embodiment of the present invention 1.
Fig. 3 is the X-ray diffractogram that different moments are total to magnetic agitation system in the embodiment of the present invention 2.
Fig. 4 is cellulose/graphene nanometer sheet aeroge absorption result figure prepared by the embodiment of the present invention 5.
Specific embodiment:
Invention is described further below by specific embodiment and in conjunction with attached drawing.
Embodiment 1
(1) 6g microcrystalline cellulose is dispersed in 100mL alkali urea solution water, while 18mg natural flake graphite is added
(0.3%), magnetic agitation, stirring rate 2500 turns/min, mixing time 8h, in mechanical force are carried out under the conditions of -12 DEG C
Under, crystalline flake graphite is removed in cellulose sol with graphene nano sheet form, and it is multiple that a step obtains cellulose/graphene nano
Close colloidal sol;
(2) complex sol is placed in ethyl alcohol and is sufficiently exchanged, then rinsed with deionized water to neutrality, freeze-drying obtains
Obtain cellulose/graphene nano composite aerogel.
Embodiment 2
(1) 6g microcrystalline cellulose is dispersed in 100mL alkali urea solution water, while 120mg natural flake graphite is added
(2%), carry out magnetic agitation under the conditions of -12 DEG C, 2500 turns/min of stirring rate, mixing time for 24 hours, under mechanical force,
Crystalline flake graphite is removed in cellulose sol with graphene nano sheet form, and it is compound molten that a step obtains cellulose/graphene nano
Glue;
(2) complex sol is placed in ethyl alcohol and is sufficiently exchanged, then rinsed with deionized water to neutrality, freeze-drying obtains
Obtain cellulose/graphene nano composite aerogel.
Cellulose solvent system is characterized in embodiment 2 in magnetic agitation system altogether to graphite using with X-ray diffractometer
Removing and peptizaiton, as shown in Figure 3.It can be seen from the figure that when cellulose and the graphite magnetic agitation 4h of 2% content,
002 region feature peak intensity of graphite drastically reduces, and the crystalline texture of cellulose also has a degree of destruction, magnetic agitation 16h
Afterwards, the characteristic diffraction peak of cellulose and graphite all completely disappears, this illustrates that graphite is completely exfoliated into graphene nanometer sheet and is dispersed in
In the cellulose sol of amorphous state, cellulose plays the role of good medium to the removing and dispersion of graphite.
Embodiment 3
(1) 12g regenerated cellulose is dissolved in 200g ionic liquid, while 36mg crystalline flake graphite (0.3%) is added, 80
Strength ultrasound 12h, ultrasonic power 1200W under the conditions of DEG C, under mechanical force, crystalline flake graphite is with graphene nano sheet form
In cellulose sol, a step obtains cellulose/graphene ionic liquid nanocomposite sol for removing;
(2) complex sol is placed in propyl alcohol and is sufficiently exchanged, then rinsed with deionized water to neutrality, overcritical dioxy
It is dry completely to change carbon, obtains cellulose/graphene nano composite aerogel.
Embodiment 4
(1) pass through dissolution 1.9644g solid CuSO4·5H2O obtains 500mg/LCu in 1000ml deionized water2+Standard
Solution, dilution obtain the Cu of various concentration2+Standard solution.
(2) Cu of various concentration is surveyed using ultraviolet specrophotometer2+It is dense to obtain copper ion in the absorbance of 810nm for solution
Standard curve between degree and absorbance;
(3) cellulose of certain mass/graphene composite aerogel is put into the Cu of 50ml 200mg/L2+Solion
In, with the rate oscillation 120min of 100rpm, supernatant is taken, it is then surveyed in the extinction of 810nm using ultraviolet specrophotometer
Degree calculates the copper ion concentration in supernatant according to standard curve, and then obtains adsorbance qeFor 76.2mg/g.
Embodiment 5
(1) certain density Zn is configured2+Standard solution, dilution obtain the Zn of various concentration2+Standard solution.
(2) Zn of various concentration is surveyed using ICPOES2+Solution obtains zinc ion concentration and extinction in the absorbance of 810nm
Standard curve between degree;
(3) the hydrogel 10mg after freeze-drying is immersed in the 100mg/L Zn of 50ml2+In standard solution, mixture is in perseverance
120min is vibrated in warm oscillator under 298K 100rpm, the concentration of heavy metal ion of supernatant is measured with ICP-OES, according to mark
Directrix curve calculates the concentration of heavy metal ion in supernatant, and then obtains adsorbance.
It adopts and obtains cellulose/graphene composite aerogel in a like fashion to Zn2+、Fe3+And Pb2+Adsorbance, tool
Body is as shown in Figure 4.
Claims (6)
1. a kind of cellulose/graphene nanometer sheet composite aerogel preparation method, which is characterized in that specifically includes the following steps:
(1) cellulosic material and graphite are added in solvent, then under the action of mechanical force, graphite is removed into graphene nano
Piece, while in the colloidal sol that the graphene nanometer sheet removed is dispersed in cellulose or cellulose derivative and solvent is constituted, it obtains
To cellulose/graphene nano complex sol, the solvent can dissolve cellulosic material;
(2) complex sol is placed in alcoholic solvent and is sufficiently exchanged, then rinsed with deionized water to neutrality, it is dry, obtain fiber
Element/graphene nano composite aerogel.
2. cellulose according to claim 1/graphene nanometer sheet composite aerogel preparation method, which is characterized in that institute
Stating cellulosic material includes one of native cellulose, modified cellulose and its derivative or a variety of;The graphite includes day
Right graphite, artificial graphite, blocky graphite, crystalline flake graphite, expanded graphite one or more of them;The mechanical force includes that strength is super
Sound, ball milling, mill, magnetic agitation, one of helical screw agitator;The drying mode includes but is not limited to constant pressure and dry, freezing
Dry, supercritical CO2One of dry, spray drying.
3. cellulose according to claim 1/graphene nanometer sheet composite aerogel preparation method, which is characterized in that institute
The concentration for stating cellulose is 2%-8%, and the content of graphene nanometer sheet is the 0.1%-5% of cellulose.
4. cellulose according to claim 1/graphene nanometer sheet composite aerogel preparation method, which is characterized in that institute
State solvent selection alkali urea system and ionic liquid.
5. cellulose according to claim 1/graphene nanometer sheet composite aerogel preparation method, which is characterized in that institute
Stating alcoholic solvent is one of ethyl alcohol, propyl alcohol, the tert-butyl alcohol or a variety of.
6. a kind of cellulose/graphene nanometer sheet composite aerogel is for the ion and dyestuff in adsorbent solution.
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Cited By (5)
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CN110841603A (en) * | 2019-10-29 | 2020-02-28 | 南京理工大学 | Preparation method of nano-cellulose-graphene oxide composite material |
CN111204829A (en) * | 2020-01-07 | 2020-05-29 | 东南大学 | Solar sewage purification aerogel based on waste paper and graphite and preparation method thereof |
CN112194819A (en) * | 2020-09-23 | 2021-01-08 | 西安理工大学 | Preparation method of graphene nanosheet/cellulose aerogel composite material |
CN113354861A (en) * | 2021-05-25 | 2021-09-07 | 同济大学 | Universal method for preparing functional nano material/cellulose composite aerogel by using paper folding principle |
CN113773664A (en) * | 2021-09-18 | 2021-12-10 | 福建农林大学 | Preparation and application of wood nano-cellulose/graphite flake layer material |
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CN113354861B (en) * | 2021-05-25 | 2022-07-22 | 同济大学 | Universal method for preparing functional nano material/cellulose composite aerogel by using paper folding principle |
CN113773664A (en) * | 2021-09-18 | 2021-12-10 | 福建农林大学 | Preparation and application of wood nano-cellulose/graphite flake layer material |
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Application publication date: 20191022 |