CN109759026A - Amido modified alginate-graphene dual network gel ball and its preparation method and application - Google Patents
Amido modified alginate-graphene dual network gel ball and its preparation method and application Download PDFInfo
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Abstract
The present invention provides a kind of amido modified alginate-graphene dual network gel balls and its preparation method and application, which includes: that graphite oxide forms graphene oxide water solution in aqueous solution；Sodium alginate is added in graphene oxide water solution and obtains the first mixed solution；Reducing agent is added in the first mixed solution and obtains the second mixed solution；Divalent metal salt is added in aqueous solution, obtains third mixed solution；Second mixed solution is instilled in third mixed solution, aminated alginic acid salt-graphene list network gel ball is obtained；It is heated in aqueous solution and obtains the dual network gel ball；The absorption property that dual network gel ball of the invention has graphene excellent, and have the characteristics that sodium alginate gel easy to form, not only adsorption effect is enhanced, but also simplifies the process of separation of solid and liquid；Reduction and cross-linking effect of this method using triethylene tetramine, further improve the absorption and mechanical performance of the dual network gel ball.
Description
Technical field
The invention belongs to environmentally conscious materials synthesis technical fields, and in particular to a kind of amido modified alginate-graphene is double
Network gel ball and its preparation method and application.
Background technique
Sodium alginate is a kind of natural polysaccharide, low in cost, and hydrophily is high, with the excellent spy such as stability and biocompatibility
Property and studied extensively.Alginate plural gel, which has become, a kind of solves the problems, such as the hot spot material of dyestuff and heavy metal in water
Material.But on the other hand, the porosity of alginate is lower, and adsorption effect is to be improved.Graphene and its derived material due to
The characteristics such as specific surface area height have excellent absorption property for water pollutant.But powdered graphite alkene is also because be difficult to point
From being easy to form secondary pollution problems after absorption.
Summary of the invention
Aiming at the shortcomings in the prior art, primary and foremost purpose of the invention is to provide a kind of amido modified alginate-graphite
Alkene dual network gel ball.
A second object of the present invention is to provide the preparations of above-mentioned amido modified alginate-graphene dual network gel ball
Method.
Third object of the present invention is to provide above-mentioned amido modified alginate-graphene dual network gel ball use
On the way.
In order to achieve the above objectives, solution of the invention is:
A kind of preparation method of amido modified alginate-graphene dual network gel ball comprising following steps:
(1) graphite oxide forms graphene oxide water solution in aqueous solution；
(2) sodium alginate is added in graphene oxide water solution and obtains the first mixed solution；
(3) reducing agent is added in the first mixed solution and obtains the second mixed solution；
(4) divalent metal salt is added in aqueous solution, obtains third mixed solution；
(5) the second mixed solution is instilled in third mixed solution, it is solidifying obtains aminated alginic acid salt-graphene list network
Glueballs；
(6) aminated alginic acid salt-graphene list network gel ball is heated in aqueous solution and obtains amido modified seaweed
Hydrochlorate-graphene dual network gel ball.
Preferably, in step (1), in graphene oxide water solution, the concentration of graphene oxide is 1-10mg/mL.
Preferably, in step (2), the concentration of sodium alginate is 5-20mg/mL.
Preferably, in step (3), reducing agent is selected from the reducing agent containing amino.
Preferably, in step (3), reducing agent is in triethylene tetramine, ethylenediamine, diethylenetriamine and m-phenylene diamine (MPD)
More than one.
Preferably, in step (1) and step (3), the ratio of reducing agent and graphite oxide is 1:5-1:80.
Preferably, in step (4), divalent metal salt ion is in addition to Mg in divalent metal salt2+All divalent in addition
Ionizable metal salt.
Preferably, in step (6), the temperature of heating is 60-95 DEG C, and the time of heating is 6-12h.
A kind of amido modified alginate-graphene dual network gel ball is obtained by above-mentioned preparation method.
A kind of above-mentioned amido modified alginate-use of the graphene dual network gel ball as adsorbent.
By adopting the above scheme, the beneficial effects of the present invention are:
The first, the present invention forms gel using sodium alginate, not only has preferable biocompatibility, but also have excellent
Good gel-forming property, gel mechanical is functional, for adsorbent efficiently separate and recycling provides convenience.
The second, surface of graphene oxide of the invention contains a large amount of oxygen-containing functional group, can be used as absorption heavy metal etc.
The adsorption site of pollutant.
Third, the present invention are using triethylene tetramine as reducing agent, and triethylene tetramine can not only restore and crosslinking-oxidization
Graphene forms second layer graphene network structure, and amino can be modified in gel network, and amino can be dirty for absorption
It contaminates object, especially heavy metal and adsorption site is provided, to improve the absorption property for pollutant.
4th, equipment is simple in preparation method of the invention, simple for process, can be with continuous operation, to be suitable for
Large-scale production.
It is formed in short, dual network gel of the invention is intertwined by two gel rubber systems, alginate-graphene is compound
Dual network gel, which has, combines the excellent absorption property of graphene, and has the characteristics that sodium alginate gel easy to form, excellent
Gesture is complementary, compensates for deficiency existing for two kinds of materials, not only adsorption effect is enhanced, but also simplifies the mistake of separation of solid and liquid
Journey also further improves mechanical performance.And reduction and cross-linking effect of this method using triethylene tetramine, further improve
The absorption and mechanical performance of gel ball.
Detailed description of the invention
Fig. 1 is amido modified alginate-graphene dual network gel ball of the invention to different pollutant absorption properties
Effect diagram.
Fig. 2 is that amido modified alginate of the invention-graphene dual network gel ball compressive stress strain curve shows
It is intended to.(abscissa Strain indicates strain, and ordinate Compression Stress indicates compression stress, and loading indicates dress
It carries, unloading indicates unloading)
Fig. 3 is amido modified alginate of the invention-graphene dual network gel ball transmission electron microscope characterization
Result schematic diagram.
Fig. 4 is aobvious for amido modified alginate of the invention-graphene dual network gel ball piece layer cross section transmitted electron
Micro mirror characterization result schematic diagram.
Fig. 5 is aobvious for amido modified alginate of the invention-graphene dual network gel ball slice plane transmitted electron
Micro mirror characterization result schematic diagram.
Specific embodiment
The present invention provides a kind of amido modified alginate-graphene dual network gel ball and preparation method thereof and answer
With.
<amido modified alginate-graphene dual network gel ball preparation method>
A kind of preparation method of amido modified alginate-graphene dual network gel ball comprising following steps:
(1) graphite oxide is added in neutral aqueous solution, it is water-soluble by stirring and being ultrasonically formed uniform graphene oxide
Liquid；
(2) sodium alginate is added in graphene oxide water solution, it is evenly dispersed to obtain by mechanical stirring and ultrasound
One mixed solution；
(3) reducing agent is added in the first mixed solution and stirs evenly, obtaining the second mixed solution, (i.e. mixing water disperses
System)；
(4) divalent metal salt is added in neutral aqueous solution, by stirring and ultrasound, obtains third mixed solution；
(5) the second mixed solution is instilled dropwise in third mixed solution, obtains aminated alginic acid salt-graphene list net
Network gel ball；
(6) aminated alginic acid salt-graphene list network gel ball is subjected in neutral aqueous solution heating water bath, obtained
Amido modified alginate-graphene dual network gel ball.
In fact, the purpose that reducing agent is added in the step (3) be since reducing agent and the first mixed solution are liquid,
Being added this moment can make the reducing agent under liquid-phase condition come into full contact with graphene oxide and be uniformly mixed, so that reduction
Agent sufficiently restores and crosslinking-oxidization graphene.
Wherein, in step (1), in graphene oxide water solution, the concentration of graphene oxide can be 1-10mg/mL,
Preferably 4mg/mL.
In step (2), the concentration of sodium alginate is 5-20mg/mL.
In step (3), reducing agent is selected from the reducing agent containing amino.
In step (3), reducing agent is selected from one of triethylene tetramine, ethylenediamine, diethylenetriamine and m-phenylene diamine (MPD)
More than.
In step (1) and step (3), the ratio of reducing agent and graphite oxide is 1:5-1:80.
Due to Mg2+Sodium alginate cannot be made to crosslink reaction, in step (4), divalent metal salt in divalent metal salt
Ion is in addition to Mg2+All divalent metal salt ions in addition.
In step (6), the temperature of heating can be 60-95 DEG C, preferably 90 DEG C；The time of heating can be 6-12h,
Preferably 5h.
<amido modified alginate-graphene dual network gel ball>
Amido modified alginate-graphene dual network gel ball is obtained by above-mentioned preparation method.
<amido modified alginate-graphene dual network gel ball purposes>
A kind of amido modified alginate-graphene dual network gel ball can be used as adsorbent use.
The present invention is further illustrated with reference to embodiments.
Embodiment 1:
The amido modified alginate of the present embodiment-graphene dual network gel ball preparation method includes the following steps:
(1) weigh 1g graphite oxide to dissolve in neutral aqueous solution, and move into the volumetric flask of 250ml, by stirring and
Ultrasonic 200min forms uniform graphene oxide water solution, wherein the concentration of graphene oxide is 4mg/mL；
(2) 5g sodium alginate is added in graphene oxide water solution, it is evenly dispersed to obtain first by mechanical stirring 4h
Mixed solution；
(3) 100mL triethylene tetramine is added in the first mixed solution and stirs 1h, obtains the second mixed solution；
(4) 4g calcium chloride is weighed in neutral aqueous solution, and 1.5min is stirred in ultrasonic machine, obtains third mixed solution,
The concentration of calcium chloride is 8mg/mL in third mixed solution；
(5) the second mixed solution is instilled in third mixed solution dropwise using peristaltic pump, obtains aminated alginic acid salt-
Graphene list network gel ball stands 7h；
(6) aminated alginic acid salt-graphene list network gel ball heats to (temperature is 90 DEG C, the time in water-bath
For 5h), amido modified alginate-graphene dual network gel ball is obtained, and it is remaining miscellaneous with distilled water to wash away the gel ball
Matter.
Embodiment 2:
The amido modified alginate of the present embodiment-graphene dual network gel ball preparation method includes the following steps:
(1) it weighs 2.5g graphite oxide to dissolve in neutral aqueous solution, and moves into the volumetric flask of 250ml, pass through stirring
With ultrasonic 200min, uniform graphene oxide water solution is formed, wherein the concentration of graphene oxide is 10mg/mL；
(2) 4g sodium alginate is added in graphene oxide water solution, it is evenly dispersed to obtain first by mechanical stirring 4h
Mixed solution；
(3) 200mL triethylene tetramine is added in the first mixed solution and stirs 1h, obtains the second mixed solution；
(4) 4g calcium chloride is weighed in neutral aqueous solution, and 1.5min is stirred in ultrasonic machine, obtains third mixed solution,
The concentration of calcium chloride is 8mg/mL in third mixed solution；
(5) the second mixed solution is instilled in third mixed solution dropwise using peristaltic pump, obtains aminated alginic acid salt-
Graphene list network gel ball stands 7h；
(6) aminated alginic acid salt-graphene list network gel ball heats to (temperature is 90 DEG C, the time in water-bath
For 5h), amido modified alginate-graphene dual network gel ball is obtained, and it is remaining miscellaneous with distilled water to wash away the gel ball
Matter.
Embodiment 3:
The amido modified alginate of the present embodiment-graphene dual network gel ball preparation method includes the following steps:
(1) weigh 1g graphite oxide to dissolve in neutral aqueous solution, and move into the volumetric flask of 250ml, by stirring and
Ultrasonic 200min forms uniform graphene oxide water solution, wherein the concentration of graphene oxide is 4mg/mL；
(2) 4g sodium alginate is added in graphene oxide water solution, it is evenly dispersed to obtain first by mechanical stirring 4h
Mixed solution；
(3) 50mL triethylene tetramine is added in the first mixed solution and stirs 1h, obtains the second mixed solution；
(4) 4g calcium chloride is weighed in neutral aqueous solution, and 1.5min is stirred in ultrasonic machine, obtains third mixed solution,
The concentration of calcium chloride is 8mg/mL in third mixed solution；
(5) the second mixed solution is instilled in third mixed solution dropwise using peristaltic pump, obtains aminated alginic acid salt-
Graphene list network gel ball stands 7h；
(6) aminated alginic acid salt-graphene list network gel ball heats to (temperature is 80 DEG C, the time in water-bath
For 6h), amido modified alginate-graphene dual network gel ball is obtained, and it is remaining miscellaneous with distilled water to wash away the gel ball
Matter.
<experiment>
It is tested as follows respectively with the product of above-described embodiment.
<experiment 1>
The purpose of this experiment is to probe into amido modified alginate-graphene dual network gel ball to different pollutants
The influence of absorption property.
As shown in Figure 1, the histogram utilizes common dual network gel (being labeled as none) and amino proposed by the invention
Modification dual network gel (be labeled as 1:50, triethylene tetramine and graphite oxide-mixed solution of sodium alginate volume ratio are 1:
50) to different pollutant MB (methylene blue), CIP (Ciprofloxacin), MO (methyl orange) and CuSO4The adsorptivity of (copper sulphate)
Can, every kind of pollutant carries out the adsorption experiment under high concentration (300mg/L) and low concentration (150mg/L) simultaneously, can be with from scheming
Find out, compared to common dual network gel, amido modified dual network gel proposed by the invention is to dirty in four kinds of typical waters
The adsorption effect of dye object has different degrees of promotion, therefore, illustrates amido modified dual network gel of the invention to pollution
The absorption property of object is preferable.
<experiment 2>
The purpose of this experiment is to probe into amido modified alginate-graphene dual network gel ball mechanical performance
It influences.
Fig. 2 is amido modified alginate-graphene dual network gel ball (NH2-DN) and amido modified alginate-stone
The compressive stress strain curve of black alkene list network gel ball (NH2-SN).Under 10%, 30% and 50% 3 kind of strained condition,
The compression stress of NH2-DN is above NH2-SN, illustrates that its mechanical strength ratio NH2-SN is strong.And the elasticity modulus of NH2-DN is about
The elasticity modulus of 3.6Kpa, NH2-SN are about 0.9Kpa, it was demonstrated that the raising of NH2-DN mechanical strength；Hysteretic loop and energy dissipation
Comparison also show identical trend, further demonstrate NH2-DN with better mechanical strength.In addition, in different pressures
Under shrinkage strain, reduced stress-strain curve slope, slope of the slope of dual network gel than single network gel is big, explanation
The elasticity of dual network gel is better than single network gel.
<experiment 3>
The purpose of this experiment is to study amido modified alginate-graphene dual network gel ball in different resolution
Under SEM shape appearance figure.
From the figure 3, it may be seen that explanation is in dual network gel spherical structure, graphene oxide exists in the form of few layer or single layer,
SEM figure i.e. in 200um, it can be seen that the lamella network consisting structure being stacked with inside gel ball.
As shown in Figure 4, lamella is that the lamella by many thickness in 100nm or so is formed by stacking, and interlamellar spacing is on the left side 400nm
It is right.
As shown in Figure 5, it is the pattern of plane at high resolutions, finds to include many various sizes of holes in plane
Road.These ducts provide active site for the absorption of pollutant, to improve the adsorption capacity of material.
The above-mentioned description to embodiment is that this hair can be understood and used for the ease of those skilled in the art
It is bright.Those skilled in the art obviously readily can make various modifications to these embodiments, and described herein one
As principle be applied in other embodiments, without having to go through creative labor.Therefore, the present invention is not limited to the above embodiments.
Those skilled in the art's principle according to the present invention, not departing from improvement that scope of the invention is made and modification all should be at this
Within the protection scope of invention.
Claims (10)
1. a kind of amido modified alginate-graphene dual network gel ball preparation method, it is characterised in that: it includes as follows
Step:
(1) graphite oxide forms graphene oxide water solution in aqueous solution；
(2) sodium alginate is added in the graphene oxide water solution and obtains the first mixed solution；
(3) reducing agent is added in first mixed solution and obtains the second mixed solution；
(4) divalent metal salt is added in aqueous solution, obtains third mixed solution；
(5) second mixed solution is instilled in the third mixed solution, obtains aminated alginic acid salt-graphene list net
Network gel ball；
(6) the aminated alginic acid salt-graphene list network gel ball is heated in aqueous solution and obtains amido modified seaweed
Hydrochlorate-graphene dual network gel ball.
2. preparation method according to claim 1, it is characterised in that: in step (1), the graphene oxide water solution
In, the concentration of graphene oxide is 1-10mg/mL.
3. preparation method according to claim 1, it is characterised in that: in step (2), the concentration of the sodium alginate is 5-
20mg/mL。
4. preparation method according to claim 1, it is characterised in that: in step (3), the reducing agent, which is selected from, contains amino
Reducing agent.
5. preparation method according to claim 1, it is characterised in that: in step (3), the reducing agent is selected from triethylene four
One or more of amine, ethylenediamine, diethylenetriamine and m-phenylene diamine (MPD).
6. preparation method according to claim 1, it is characterised in that: in step (1) and step (3), the reducing agent with
The ratio of the graphite oxide is 1:5-1:80.
7. preparation method according to claim 1, it is characterised in that: in step (4), divalent gold in the divalent metal salt
Belonging to salt ion is in addition to Mg2+All divalent metal salt ions in addition.
8. preparation method according to claim 1, it is characterised in that: in step (6), the temperature of the heating is 60-95
DEG C, the time of the heating is 6-12h.
9. a kind of amido modified alginate-graphene dual network gel ball, it is characterised in that: it is appointed by such as claim 1-8
Preparation method described in one obtains.
10. a kind of amido modified alginate-graphene dual network gel ball as claimed in claim 9 makes as adsorbent
With.
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