CN110124627A - Graphene oxide and alginate composite aerogel and its preparation method and application - Google Patents
Graphene oxide and alginate composite aerogel and its preparation method and application Download PDFInfo
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- CN110124627A CN110124627A CN201910567177.2A CN201910567177A CN110124627A CN 110124627 A CN110124627 A CN 110124627A CN 201910567177 A CN201910567177 A CN 201910567177A CN 110124627 A CN110124627 A CN 110124627A
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- 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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- 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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- 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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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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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- 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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/46—Materials comprising a mixture of inorganic and organic materials
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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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
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Abstract
The invention discloses the preparation method of a kind of graphene oxide and alginate composite aerogel, includes the following steps: that (1) reducing agent and alginate, ultrasonic disperse are added into graphene oxide water solution, obtain ultrasonic disperse liquid;Cross-linking agent solution is added into ultrasonic disperse liquid, mixed liquor is made;(2) foaming agent solution is added in mixed liquor made from step (1), foaming mixed liquor is made in stirring foaming;(3) reduction reaction, cooling reaction product to room temperature occur for the foaming mixed liquor that step (2) obtains, and washing by soaking, freezing melt, are dry, and graphene oxide and alginate composite aerogel is prepared.The graphene oxide and alginate composite aerogel adsorption capacity with higher that this method is prepared.The graphene oxide and alginate composite aerogel that are prepared the invention also discloses the above method and its application in sewage in organic dye pollutant processing.
Description
Technical field
The present invention relates to a kind of aeroge and its preparation method and application, especially graphene oxide and alginate are compound
Aeroge and its preparation method and application.
Background technique
Graphene aerogel has high-specific surface area and excellent chemical stability and thermal stability, becomes novel organic
The hot research direction of dye sorbent.But its hydrophobicity with higher, it limits it and is polluted with organic dyestuff in sewage
The contact of object, and in water to the adsorption effect of pollutant.Sodium alginate is a kind of natural polysaccharide, is widely present in nature
In, cheap, surface oxygen-containing functional group rich in has outstanding hydrophily, prepared by sodium alginate and graphene
The hydrophily of graphene can effectively be enhanced at composite aerogel.
CN106853296A discloses a kind of preparation side of oil water separation type sodium alginate/graphene oxide composite aerogel
Method, (1) prepare sodium alginate soln;(2) it is ultrasonically treated graphene oxide suspension, is added in sodium alginate soln, is made
Sodium alginate/graphene oxide dispersion;(3) sodium alginate/graphene oxide dispersion is freeze-dried, is obtained uncrosslinked
Sodium alginate/graphene oxide composite aerogel;(4) uncrosslinked sodium alginate/graphene oxide composite aerogel is placed in
It reacts, washs in calcium chloride solution, freeze-drying obtains sodium alginate/graphene oxide composite aerogel of calcium ion crosslinking.
Pattern uniformity height, the high composite hydrogel of specific surface area, composite hydrogel adsorption energy obtained can not be prepared in this method
Power is not strong.
CN109012618A discloses a kind of preparation method of graphene oxide/sodium alginate gel ball, ultrasonic oxidation stone
Black aqueous solution configures to obtain graphene oxide dispersion;Sodium alginate is configured to sodium alginate soln;By graphene oxide
Dispersion liquid and sodium alginate soln mixing ultrasonic disperse, are added dropwise crosslinking agent after defoaming, obtain gel ball;Gel ball is soaked in water
Bubble, freeze-drying, obtains graphene oxide/sodium alginate aeroge ball material.The aeroge ratio that this method is prepared
Surface area is not high, lower to the adsorption capacity of pollutant.
CN105536726A discloses a kind of compound suction of graphene oxide sodium alginate for removing Ciprofloxacin in aqueous solution
The preparation method of enclosure material: (1) configuring graphene oxide solution, and ultrasound removing obtains graphene oxide;(2) sodium alginate is molten
Solution is then sonicated in the graphene oxide solution after ultrasound;(3) it is added dropwise into the mixed liquor after step (2) ultrasonic treatment
Calcium chloride impregnates, and cleaning obtains graphene oxide sodium alginate sphere hydrogel, and after freeze-drying, graphene oxide seaweed is made
Sour sodium sphere aeroge.The aeroge specific surface area that this method is prepared is not high, lower to the adsorption capacity of pollutant.
Summary of the invention
In view of this, the first purpose of this invention is to provide a kind of graphene oxide and alginate composite aerogel
Preparation method, the aeroge adsorption capacity with higher being prepared by this method.
Second object of the present invention is to provide graphene oxide prepared by the above method and alginate is multiple
Aeroge is closed, adsorption capacity is high.
Third object of the present invention is to provide the graphene oxide that the above method is prepared and alginate is compound
The purposes of aeroge has good treatment effect to the organic dye pollutant in sewage.
In a first aspect, the present invention provides the preparation method of a kind of graphene oxide and alginate composite aerogel, including
Following steps:
(1) reducing agent and alginate, ultrasonic disperse are added into graphene oxide water solution, obtains ultrasonic disperse liquid;
Cross-linking agent solution is added into ultrasonic disperse liquid, mixed liquor is made;
(2) foaming agent solution is added in mixed liquor made from step (1), foaming mixed liquor is made in stirring foaming;
(3) reduction reaction occurs for step (2) obtains foaming mixed liquor, cooling reaction product to room temperature, washing by soaking, cold
Graphene oxide and alginate composite aerogel is prepared in freeze thawing, drying.
Preparation method according to the present invention, it is preferable that foaming agent is surfactant-based foaming agent.
Preparation method according to the present invention, it is preferable that foaming agent is sodium sulfate of polyethenoxy ether of fatty alcohol or dodecyl
Benzene sulfonic acid sodium salt.
Preparation method according to the present invention, it is preferable that the mass ratio of graphene oxide and foaming agent is 1:0.5~1.
Preparation method according to the present invention, it is preferable that the mass ratio of graphene oxide and alginate is 1:0.1~0.8.
Preparation method according to the present invention, it is preferable that crosslinking agent is metallic-ion crosslinking agent.
Preparation method according to the present invention, it is preferable that reducing agent is selected from ascorbic acid, ethylenediamine, sodium tetraborate, hydrogen iodine
One of acid, oxalic acid, potassium iodide are a variety of.
Preparation method according to the present invention, it is preferable that the mixing speed in step (2) is 5000~20000rpm, stirring
Time is 2~10min.
Second aspect, the present invention provides a kind of graphene oxide and alginate composite aerogel, by preceding method system
It is standby to obtain.
The third aspect, the present invention provides a kind of above-mentioned graphene oxide and alginate composite aerogel is organic in sewage
Application in dyestuff contaminant processing.
Foaming agent is added in the ultrasonic disperse liquid containing graphene, cellulose, reducing agent and crosslinking agent in the present invention, can
The porosity for effectively increasing aeroge, increases the adsorption capacity of aeroge, and foaming process makes prepared aeroge stomata
It is circle, stomata is isotropic, makes aeroge compression resilience having the same in all directions, is conducive to realize airsetting
The recycling of glue.Preferred technical solution according to the present invention can achieve more using neopelex as foaming agent
Good foaming effect, the aeroge adsorption capacity being prepared are stronger.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, but protection scope of the present invention is not limited to
This.
The preparation method of graphene oxide and alginate composite aerogel of the invention includes the following steps: (1) raw material
Mixing step;(2) foaming step;(3) post-processing step.
<raw material mixing step>
Reducing agent and alginate are added into graphene oxide water solution, then ultrasonic disperse, obtains ultrasonic disperse liquid;
Crosslinking agent is added into ultrasonic disperse liquid, mixed liquor is made.In the present invention, alginate is preferably water soluble algae hydrochlorate,
Such as sodium alginate.
In the present invention, the concentration of graphene oxide is 2~15mg/ml in graphene oxide water solution.Preferably, it aoxidizes
The concentration of graphene is 2~10mg/ml.It is highly preferred that the concentration of graphene oxide is 3~5mg/ml.According to the present invention one
The aqueous solution of a specific embodiment, graphene oxide can be configured by deionized water and graphene oxide, described
Graphene oxide is purchased from Changzhou No.6 Element Material Technology Co., Ltd., and piece diameter is 20~25 μm, and oxygen carbon molar ratio is
0.6。
In the present invention, the mass ratio of graphene oxide and alginate is 1:0.1~0.8.Preferably, graphene oxide
Mass ratio with alginate is 1:0.1~0.5.It is highly preferred that the mass ratio of graphene oxide and alginate be 1:0.2~
0.4.The hydrophily that can effectively improve graphene oxide in this way keeps the graphene oxide being prepared and alginate compound
Aeroge has higher adsorption capacity.
In the present invention, reducing agent is selected from ascorbic acid, ethylenediamine, sodium tetraborate, hydroiodic acid, oxalic acid, potassium iodide
One of or it is a variety of.Preferably, reducing agent is ascorbic acid, ethylenediamine or sodium tetraborate.It is highly preferred that reducing agent is anti-bad
Hematic acid.The mass ratio of graphene oxide and reducing agent is 1:2~5.Preferably, the mass ratio of graphene oxide and reducing agent is 1:
2~4.It is highly preferred that the mass ratio of graphene oxide and reducing agent is 1:2~3.It can achieve better reduction effect in this way,
Make the aeroge being prepared that there is higher adsorption capacity.
In the present invention, the time of ultrasonic disperse is 5~30min.Preferably, the time of ultrasonic disperse is 10~30min.
It is highly preferred that the time of ultrasonic disperse is 15~30min.The uniformity that can guarantee ultrasonic disperse liquid in this way, makes to be prepared
Graphene oxide and alginate compound have higher adsorption capacity.
In the present invention, crosslinking agent is metallic-ion crosslinking agent.Preferably, crosslinking agent is divalent calcium ions crosslinking agent.Root
According to a specific embodiment of the invention, crosslinking agent CaCl2.The mass ratio of crosslinking agent and graphene oxide is 1:0.2
~0.8.Preferably, the mass ratio of crosslinking agent and graphene oxide is 1:0.2~0.6.It is highly preferred that crosslinking agent and graphite oxide
The mass ratio of alkene is 1:0.3~0.5.The concentration of crosslinking agent is 0.05~0.5mol/L in cross-linking agent solution.Preferably, crosslinking agent
The concentration of crosslinking agent is 0.05~0.3mol/L in solution.It is highly preferred that in cross-linking agent solution crosslinking agent concentration be 0.1~
0.2mol/L.The degree of cross linking and mechanical strength that can guarantee aeroge in this way make the aeroge being prepared have stronger suction
Attached ability.
<foaming step>
Foaming agent solution is added in raw material mixing step in mixed liquor obtained, foaming mixing is made in stirring foaming
Liquid.
In the present invention, foaming agent can be surfactant-based foaming agent.According to some embodiments of the present invention, it sends out
Infusion is sodium sulfate of polyethenoxy ether of fatty alcohol or neopelex.A specific embodiment party according to the present invention
Formula, foaming agent are neopelex.The mass ratio of graphene oxide and foaming agent is 1:0.5~1.Preferably, it aoxidizes
The mass ratio of graphene and foaming agent is 1:0.5~0.8.It is highly preferred that the mass ratio of graphene oxide and foaming agent is 1:0.5
~0.7.The concentration of foaming agent solution is 30~80mg/L.Preferably, the concentration of foaming agent solution is 40~70mg/L.More preferably
Ground, the concentration of foaming agent solution are 50~60mg/L.Foaming agent solution can be the aqueous solution of foaming agent.It can guarantee to make in this way
Standby obtained aeroge has the aperture of uniformly rule, and large specific surface area has good adsorption capacity.
In the present invention, mixing speed is 5000~20000rpm, and mixing time is 2~10min.Preferably, mixing speed
For 10000~20000rpm, it is highly preferred that mixing speed is 10000~15000rpm.Preferably, mixing time be 3~
8min.It is highly preferred that mixing time is 3~5min.The foaming degree that can guarantee mixed ultrasonic disperse liquid in this way, so that being prepared into
The aeroge arrived has bigger specific surface area, enhances the adsorption capacity of aeroge.
<post-processing step>
Reduction reaction, cooling reaction product to room temperature, washing by soaking, freezing occur for the foaming mixed liquor that foaming step obtains
Melt, is dry, graphene oxide and alginate composite aerogel is prepared.
In the present invention, the reduction reaction time is 4~9 hours.According to some embodiments of the present invention, when reduction reaction
Between be 5~8 hours.A specific embodiment according to the present invention, the time of reduction reaction are 6~8 hours.Reduction reaction
Temperature be 50~100 DEG C.According to some embodiments of the present invention, the temperature of reduction reaction is 60~90 DEG C.According to this hair
A bright specific embodiment, the temperature of reduction reaction are 70~90 DEG C.Reduction reaction can be made to carry out ground more in this way
Completely, the aeroge being prepared has stronger adsorption capacity.
In the present invention, the washing lotion for washing by soaking is the aqueous solution of ethyl alcohol.Preferably, the concentration of alcohol of ethanol water
For 1~3vol%.The time of washing by soaking is 20~30 hours.
In the present invention, cryogenic temperature is -60~-30 DEG C.Preferably, cryogenic temperature is -50~-30 DEG C.It is highly preferred that cold
Freezing temperature is -50~-35 DEG C.Cooling time be 10~for 24 hours.Preferably, cooling time is 10~20 hours.It is highly preferred that cold
Freezing the time is 12~18 hours.Freezing melting process of the invention can be to place the reduction reaction product after washing by soaking
It is freezed 12 hours in -45 DEG C of refrigerators, taking-up is melted at room temperature.The aeroge being prepared can in this way had more strongly
Hydrophily has stronger adsorption capacity.
In the present invention, drying process carries out under normal pressure.Drying temperature is 40~100 DEG C.Preferably, drying temperature 50
~90 DEG C.It is highly preferred that drying temperature is 50~70 DEG C.Drying time is 20~40h.Preferably, drying time be 24~
35h.It is highly preferred that drying time is 24~30h.Can make in this way the aeroge being prepared have higher specific surface area with
And compression resilience.
The present invention also provides a kind of graphene oxides prepared by the above method and alginate composite aerogel.
The graphene oxide and alginate composite aerogel obtained the present invention also provides above-mentioned preparation method is in sewage
Application in organic dye pollutant processing.Preferably, the organic dye pollutant is selected from methyl orange, methylene blue, sieve
One of red bright B, crystal violet, dimethyl diaminophenazine chloride are a variety of.A specific embodiment according to the present invention, described has engine dyeing
Material is methylene blue.
Embodiment 1
480mg ascorbic acid is added in the graphene oxide water solution that 60ml concentration is 4mg/ml, under agitation
40mg sodium alginate is added, ultrasonic disperse 20min obtains ultrasonic disperse liquid.The CaCl of 10ml is added into ultrasonic disperse liquid2Water
Mixed liquor is made in solution (concentration 0.1mol/L).
150mg neopelex is dissolved in 3ml deionized water and obtains neopelex solution, so
After be added in mixed liquor, to 10000rmp revolving speed stirring foaming 3min, foaming mixed liquor is prepared.
Foaming mixed liquor is placed in 80 DEG C of baking ovens, after reduction reaction 6h, cooled to room temperature.By reduction reaction product
Washing by soaking is carried out for 24 hours with the ethanol water of 1vol%, the reduction reaction product after washing is placed in cold in -45 DEG C of refrigerators
Freeze 12h, take out, melt 6h at room temperature, drying for 24 hours, obtains graphene oxide and the compound gas of sodium alginate in 60 DEG C of baking ovens
Gel.
Embodiment 2
480mg ascorbic acid is added in the graphene oxide water solution that 60ml concentration is 4mg/ml, under agitation
80mg sodium alginate is added, ultrasonic disperse 20min obtains ultrasonic disperse liquid.The CaCl of 10ml is added into ultrasonic disperse liquid2Water
Mixed liquor is made in solution (concentration 0.1mol/L).
150mg neopelex is dissolved in 3ml deionized water and obtains neopelex solution, so
After be added in mixed liquor, to 10000rmp revolving speed stirring foaming 3min, foaming mixed liquor is prepared.
Foaming mixed liquor is placed in 80 DEG C of baking ovens, after reduction reaction 6h, cooled to room temperature.By reduction reaction product
Washing by soaking is carried out for 24 hours with the ethanol water of 1vol%, the reduction reaction product after washing is placed in cold in -45 DEG C of refrigerators
Freeze 12h, take out, melt 6h at room temperature, drying for 24 hours, obtains graphene oxide and the compound gas of sodium alginate in 60 DEG C of baking ovens
Gel.
Embodiment 3
In the graphene oxide water solution for being 4mg/ml by 480mg ascorbic acid 60ml concentration, it is added under agitation
120mg sodium alginate, ultrasonic disperse 20min obtain ultrasonic disperse liquid.The CaCl of 10ml is added into ultrasonic disperse liquid2It is water-soluble
Mixed liquor is made in liquid (concentration 0.1mol/L).
150mg neopelex is dissolved in 3ml deionized water and obtains neopelex solution, so
After be added in mixed liquor, to 10000rmp revolving speed stirring foaming 3min, foaming mixed liquor is prepared.
Foaming mixed liquor is placed in 80 DEG C of baking ovens, after reduction reaction 6h, cooled to room temperature.By reduction reaction product
Washing by soaking is carried out for 24 hours with the ethanol water of 1vol%, the reduction reaction product after washing is placed in cold in -45 DEG C of refrigerators
Freeze 12h, take out, melt 6h at room temperature, drying for 24 hours, obtains graphene oxide and the compound gas of sodium alginate in 60 DEG C of baking ovens
Gel.
Comparative example 1
In the graphene oxide water solution for being 4mg/ml by 480mg ascorbic acid 60ml concentration, ultrasonic disperse 20min is obtained
To ultrasonic disperse liquid.The CaCl of 10ml is added into ultrasonic disperse liquid2Mixed liquor is made in aqueous solution (concentration 0.1mol/L).
150mg neopelex is dissolved in 3ml deionized water and obtains neopelex solution, so
After be added in mixed liquor, to 10000rmp revolving speed stirring foaming 3min, foaming mixed liquor is prepared.
Foaming mixed liquor is placed in 80 DEG C of baking ovens, after reduction reaction 6h, cooled to room temperature.By reduction reaction product
Washing by soaking is carried out for 24 hours with the ethanol water of 1vol%, the reduction reaction product after washing is placed in cold in -45 DEG C of refrigerators
Freeze 12h, take out, melt 6h at room temperature, drying for 24 hours, obtains graphite oxide aerogel in 60 DEG C of baking ovens.
Experimental example
The aeroge that embodiment 1-3 and comparative example 1 are prepared tests the adsorption capacity of methylene blue, test
Method is as follows:
The composite aerogel sample for weighing 0.5g is added to methylene blue solution (liquor capacity 300ml, methylene blue
Concentration be 500mg/ml) in, water bath with thermostatic control concussion bed in (35 DEG C, 100r/min) concussion, after reaching adsorption equilibrium, with purple
Outer spectrophotometer measurement methylene blue solution calculates the concentration of dyestuff in the absorbance of 660nm wavelength so as to find out being adsorbed
Methylene blue amount.As a result as shown in the table:
Table 1
Test sample | The adsorbance mg/g of methylene blue |
Embodiment 1 | 200 |
Embodiment 2 | 246 |
Embodiment 3 | 240 |
Comparative example 1 | 170 |
Present invention is not limited to the embodiments described above, without departing from the essence of the present invention, this field skill
Any deformation, improvement, the replacement that art personnel are contemplated that each fall within the scope of the present invention.
Claims (10)
1. the preparation method of a kind of graphene oxide and alginate composite aerogel, which comprises the steps of:
(1) reducing agent and alginate, ultrasonic disperse are added into graphene oxide water solution, obtains ultrasonic disperse liquid;Xiang Chao
Cross-linking agent solution is added in sound dispersion liquid, mixed liquor is made;
(2) foaming agent solution is added in mixed liquor made from step (1), foaming mixed liquor is made in stirring foaming;
(3) reduction reaction, cooling reaction product to room temperature occur for the foaming mixed liquor that step (2) obtains, and washing by soaking, freezing are melted
Change, is dry, graphene oxide and alginate composite aerogel is prepared.
2. preparation method according to claim 1, which is characterized in that the foaming agent is surfactant-based foaming
Agent.
3. preparation method according to claim 1, which is characterized in that the foaming agent is fatty alcohol polyoxyethylene ether sulphur
Sour sodium or neopelex.
4. preparation method according to claim 1, which is characterized in that the mass ratio of the graphene oxide and foaming agent
For 1:0.5~1.
5. preparation method according to claim 1, which is characterized in that the quality of the graphene oxide and alginate
Than for 1:0.1~0.8.
6. preparation method according to claim 1, which is characterized in that the crosslinking agent is metallic-ion crosslinking agent.
7. preparation method according to claim 1, which is characterized in that the reducing agent be selected from ascorbic acid, ethylenediamine,
One of sodium tetraborate, hydroiodic acid, oxalic acid, potassium iodide are a variety of.
8. preparation method according to claim 1, which is characterized in that mixing speed in step (2) is 5000~
20000rpm, mixing time are 2~10min.
9. a kind of graphene oxide and alginate composite aerogel, which is characterized in that as described in any one of claim 1~8
Method be prepared.
10. graphene oxide according to claim 9 and alginate the composite aerogel organic dyestuff in sewage pollute
Application in object processing.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111036177A (en) * | 2019-12-05 | 2020-04-21 | 河南科技大学 | Preparation method and application of graphene/carrageenan aerogel |
CN113600245A (en) * | 2021-08-24 | 2021-11-05 | 上海应用技术大学 | Ferric alginate-graphene oxide catalytic material and preparation method and application thereof |
CN114307879A (en) * | 2022-01-05 | 2022-04-12 | 上海第二工业大学 | Preparation method of graphene aerogel for super-hydrophilic seawater desalination |
CN115779972A (en) * | 2022-12-27 | 2023-03-14 | 中南大学 | Graphene oxide-based composite aerogel catalyst and preparation method and application thereof |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104785177A (en) * | 2015-03-23 | 2015-07-22 | 同济大学 | Preparation method of alginate-graphene compound double-network gel beads |
CN106517160A (en) * | 2016-11-22 | 2017-03-22 | 青岛科技大学 | Method for preparing isotropic superelastic graphene aerogel |
CN106853296A (en) * | 2016-12-30 | 2017-06-16 | 福建农林大学 | A kind of oil water separation type sodium alginate/graphene oxide composite aerogel and preparation method thereof |
CN106902778A (en) * | 2017-04-28 | 2017-06-30 | 武汉理工大学 | A kind of chitosan/oxidized Graphene/polyvinyl alcohol cellular composite adsorbing material and preparation method thereof |
CN109012618A (en) * | 2018-09-12 | 2018-12-18 | 宝泰隆新材料股份有限公司北京分公司 | A kind of preparation method and application of graphene oxide/sodium alginate gel ball |
-
2019
- 2019-06-27 CN CN201910567177.2A patent/CN110124627A/en active Pending
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104785177A (en) * | 2015-03-23 | 2015-07-22 | 同济大学 | Preparation method of alginate-graphene compound double-network gel beads |
CN106517160A (en) * | 2016-11-22 | 2017-03-22 | 青岛科技大学 | Method for preparing isotropic superelastic graphene aerogel |
CN106853296A (en) * | 2016-12-30 | 2017-06-16 | 福建农林大学 | A kind of oil water separation type sodium alginate/graphene oxide composite aerogel and preparation method thereof |
CN106902778A (en) * | 2017-04-28 | 2017-06-30 | 武汉理工大学 | A kind of chitosan/oxidized Graphene/polyvinyl alcohol cellular composite adsorbing material and preparation method thereof |
CN109012618A (en) * | 2018-09-12 | 2018-12-18 | 宝泰隆新材料股份有限公司北京分公司 | A kind of preparation method and application of graphene oxide/sodium alginate gel ball |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111036177A (en) * | 2019-12-05 | 2020-04-21 | 河南科技大学 | Preparation method and application of graphene/carrageenan aerogel |
CN113600245A (en) * | 2021-08-24 | 2021-11-05 | 上海应用技术大学 | Ferric alginate-graphene oxide catalytic material and preparation method and application thereof |
CN114307879A (en) * | 2022-01-05 | 2022-04-12 | 上海第二工业大学 | Preparation method of graphene aerogel for super-hydrophilic seawater desalination |
CN115779972A (en) * | 2022-12-27 | 2023-03-14 | 中南大学 | Graphene oxide-based composite aerogel catalyst and preparation method and application thereof |
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