CN109894099A - A kind of trielement composite material and preparation method thereof based on polyethyleneimine - Google Patents
A kind of trielement composite material and preparation method thereof based on polyethyleneimine Download PDFInfo
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- CN109894099A CN109894099A CN201910206456.6A CN201910206456A CN109894099A CN 109894099 A CN109894099 A CN 109894099A CN 201910206456 A CN201910206456 A CN 201910206456A CN 109894099 A CN109894099 A CN 109894099A
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Abstract
The invention discloses a kind of trielement composite material and preparation method thereof based on polyethyleneimine, polyethyleneimine is immobilized on carboxylation konjaku glucomannan using solution blended process, then combined oxidation graphene again, is prepared polyethyleneimine/carboxylation konjaku glucomannan/graphene oxide composite material.Simple process of the invention, it is easy to operate；Composite material character prepared by the present invention is stable, environmental-friendly, and adsorpting lead ion is had excellent performance from aqueous solution, in heavy metal containing wastewater treatment field has practical application value.
Description
Technical field
The invention belongs to the preparation field of polyethyleneimine composite material, in particular to a kind of three based on polyethyleneimine
First composite material and preparation method.
Background technique
Polyethyleneimine is a kind of typical water-soluble polyamine, contains a large amount of primary amine, secondary amine, tertiary amine groups on strand
Group has very strong chelating ligands effect with metal ion under neutral or basic conditions, is a kind of novel heavy metal ion
Trapping agent.But in current practical application technology, polyethyleneimine cost price is higher and material is easy to be lost, it is difficult to return
It receives and utilizes；In addition, it is existing unsatisfactory based on immobilized and modified effect of the material of polyethyleneimine to polyethyleneimine, because
And it is difficult to embody polyethyleneimine as prominent features such as the high-adsorption-capacity of adsorbent for heavy metal and the high rates of adsorption.Evil spirit
Taro glucomannans is a kind of biological material being keyed with β (1 → 4) pyranoside, resourceful, renewable, degradable,
Nontoxicity, it is low in cost.But the hygroscopic swelling of the sweet glycan of konjaku Pu, thermal stability are insufficient, it is difficult to be applied to heavy metal ion and inhale
In attached complex environment.Graphene oxide contains a large amount of oxygen-containing functional groups (carboxyl, epoxy group, carbonyl and hydroxyl), to heavy metal
Ion has very strong complexing power.But graphene oxide is light and has biggish specific surface area, general in existing application technology
Store-through is dispersing unevenness, is being easy to the defects of reuniting.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of trielement composite material based on polyethyleneimine and its preparation
Method.The present invention is first modified konjaku glucomannan, is improved its swelling behavior, thermal stability to reach real
Border application requirement.Using solution blended process, mechanical stirring is prepared for a kind of trielement composite material based on polyethyleneimine.It is this
It is effective immobilized on carboxylation konjaku glucomannan that material and its method of preparation realize polyethyleneimine, hence it is evident that improves poly- second
Alkene imines operating difficulties, the shortcomings that being easy to run off, it is evenly dispersed and effectively compound in system to realize graphene oxide, plays
The excellent absorption property of material is a kind of effective application method.The method is easy to operate, easy, which is suitable for
Heavy metal containing wastewater treatment field.
Specific technical solution are as follows:
The material is prepared by the following method gained, and polyethyleneimine is immobilized on carboxylation konjaku Portugal using solution blended process
On sweet glycan, then combined oxidation graphene, mechanical stirring prepare polyethyleneimine/carboxylation konjaku glucomannan/oxidation stone again
Black alkene composite material.
The preparation method specifically includes the following steps:
(1) solvent is made with dehydrated alcohol, adjusts solvent pH to 7~10 with sodium hydroxide, dissolves konjaku glucomannan, chloroethene
Acid, dehydrated alcohol, konjaku glucomannan, chloroacetic mass ratio are 6~10:40~70:3~10；With monoxone to konjaku Portugal
Sweet glycan carries out deacetylated and carboxymethyl-modification, is dried to obtain carboxylation konjaku glucomannan；Reaction condition are as follows: reaction temperature
It is 30~70 DEG C；Mechanical stirring rate is 200~600rpm/min；Reaction time is 1~6 hour；Drying temperature is 10~70
℃。
(2) polyethyleneimine is dissolved in deionized water, and ultrasonic treatment obtains aq. polyethyleneimine；Polyethyleneimine
Relative molecular mass be 600~70000；The mass fraction of aq. polyethyleneimine is 2%~30%.
(3) the resulting carboxylation konjaku glucomannan of step (1) is soluble in water, it is water-soluble to form carboxylation konjaku glucomannan
Liquid；The mass fraction of carboxylation konjak portuguese gansu polyose sugar aqueous solution is 1%~10%.Step (2) resulting polyethyleneimine is water-soluble
Drop is added in konjak portuguese gansu polyose sugar aqueous solution, and glutaraldehyde solution is added, and the dosage of glutaraldehyde solution is 0.2~5mL；Stirring
Reaction, obtains polyethyleneimine/carboxylation konjaku glucomannan binary composite suspension liquid；The condition of reaction are as follows: reaction temperature does not surpass
Cross 50 DEG C；Mechanical stirring rate is 200~600rpm/min；Reaction time is 1~6 hour.The polyethylenimine solution,
The volume ratio of konjak portuguese gansu polyose sugar juice, glutaraldehyde solution are as follows: 4~10:50~100:1~10.
(4) it adds graphene oxide into water, ultrasonic disperse forms graphene oxide and disperses solution, and graphene oxide is water-soluble
The mass fraction of liquid is 0.01%~1%；The ultrasonic disperse is formed in graphene oxide dispersion solution, and ultrasonic power is
200~400w, time are 1~3h；Step (3) resulting polyethyleneimine/carboxylation evil spirit is added in graphene oxide dispersion solution
In taro Glucomannan composite suspension liquid, mechanic whirl-nett reaction, the condition of reaction are as follows: reaction temperature is no more than 50 DEG C；Mechanical stirring
Rate is 200~600rpm/min；Reaction time is 1~6 hour；Polyethyleneimine/carboxylation konjaku Portugal is obtained after reaction
Sweet glycan/graphene oxide composite material.
A kind of trielement composite material and preparation method thereof based on polyethyleneimine provided by the invention, the beneficial effect having
Fruit:
Composite property produced by the present invention is excellent, easy to use, and repeat performance is good, leads in heavy metal wastewater thereby
Domain has practical application value.
Three kinds of raw materials used in the present invention, are environment-friendly materials, during preparing material and using material
Secondary pollution will not be caused to environment.
Reaction condition of the present invention is mild, and operating process is simple, is swift in response, and yield is high, is suitble to industrialized production.
Detailed description of the invention
Fig. 1 is the scanning electron microscope diagram of composite material prepared by embodiment 1；
Fig. 2 is the FTIR spectrum figure of composite material prepared by embodiment 1.
Specific embodiment
Below in conjunction with specific embodiment, the present invention is described in detail.
Embodiment 1
Under (1) 20 DEG C of water bath condition, weighs 8g konjak portuguese gansu polyose Icing Sugar and swell in 50mL dehydrated alcohol and make solvent, stir molten
Swollen 30 minutes.It weighs 5g monoxone and is dissolved in 10mL absolute ethyl alcohol and stirring to dissolution.In the mechanical stirring rate of 200rpm/min
Under the conditions of, by monoxone-dehydrated alcohol with the drop rate of 1mL/min, it is slowly added dropwise in reaction solution, it is lasting to be mixed
3h.System is warming up to 55 DEG C after 3h, pH value of solution is adjusted to 9 with saturation sodium hydroxide alcoholic solution, reaction stirring 3h.It will after 3h
Reaction solution pours into beaker, is washed to solution and is in neutrality repeatedly with ethyl alcohol.Oven temperature is adjusted to 55 DEG C, by reactants dry
12h obtains the sweet glycan of product carboxylation konjaku Pu.
(2) it weighs 0.5g polyethyleneimine to be dissolved in 5mL deionized water, ultrasonic 2h forms uniform polyethyleneimine
Aqueous solution.
(3) 2.5g carboxylation konjaku glucomannan powder is swollen in 100mL aqueous solution, forms uniform carboxylation konjaku Portugal
Sweet water solution.Above-mentioned aq. polyethyleneimine is added dropwise to konjak portuguese gansu polyose sugar aqueous solution with the rate of 1mL/min, and
1mL glutaraldehyde solution is added.Under the conditions of 30 DEG C, 2h is stirred to react with the stirring rate of 300rpm/min, reaction stops being gathered
Aziridine/carboxylation konjaku glucomannan binary composite suspension liquid.
(4) at room temperature, 4mg graphene oxide is added in the water of 10mL, ultrasonic disperse forms graphene oxide dispersion
Graphene oxide dispersion solution is added dropwise to above-mentioned polyethyleneimine/carboxylation konjaku glucomannan with the rate of 1mL/min by solution
In composite suspension liquid, under the conditions of 30 DEG C, 3h is stirred to react with the stirring rate of 300rpm/min, after reaction fills suspension
Enter plain edition bag filter, dialyse 48h, and it is compound that freeze-drying obtains polyethyleneimine/carboxylation konjaku glucomannan/graphene oxide
Material.
Through detecting: observing that porous state is presented in product by scanning electron microscope.Fourier's infrared test distinguishes table
Contain polyethyleneimine and carboxylation konjak portuguese gansu polyose saccharic composition in bright composite material, the test of Fourier's Raman shows composite hydrogel
In contain graphite oxide olefinic constituent.Polyethyleneimine/carboxylation konjaku glucomannan/graphene oxide composite material character is stablized,
With excellent heavy metal ion adsorbed performance.The result of detection is as depicted in figs. 1 and 2.
Embodiment 2
Under (1) 20 DEG C of water bath condition, weighs 8g konjak portuguese gansu polyose Icing Sugar and swell in 50mL dehydrated alcohol and make solvent, stir molten
Swollen 30 minutes.It weighs 5g monoxone and is dissolved in 10mL absolute ethyl alcohol and stirring to dissolution.In the mechanical stirring rate of 200rpm/min
Under the conditions of, by monoxone-dehydrated alcohol with the drop rate of 1mL/min, it is slowly added dropwise in reaction solution, it is lasting to be mixed
3h.System is warming up to 55 DEG C after 3h, pH value of solution is adjusted to 9 with saturation sodium hydroxide alcoholic solution, reaction stirring 3h.It will after 3h
Reaction solution pours into beaker, is washed to solution and is in neutrality repeatedly with ethyl alcohol.Oven temperature is adjusted to 55 DEG C, by reactants dry
12h obtains the sweet glycan of product carboxylation konjaku Pu.
(2) it weighs 2.0g polyethyleneimine to be dissolved in 5mL deionized water, ultrasonic 2h forms uniform polyethyleneimine
Aqueous solution.
(3) 2.5g carboxylation konjaku glucomannan powder is swollen in 100mL aqueous solution, forms uniform carboxylation konjaku Portugal
Sweet water solution.Above-mentioned aq. polyethyleneimine is added dropwise to konjak portuguese gansu polyose sugar aqueous solution with the rate of 1mL/min, and
1mL glutaraldehyde solution is added.Under the conditions of 40 DEG C, 2h is stirred to react with the stirring rate of 600rpm/min, reaction stops being gathered
Aziridine/carboxylation konjaku glucomannan binary composite suspension liquid.
(4) at room temperature, 4mg graphene oxide is added in the water of 10mL, ultrasonic disperse forms graphene oxide dispersion
Graphene oxide dispersion solution is added dropwise to above-mentioned polyethyleneimine/carboxylation konjaku glucomannan with the rate of 1mL/min by solution
In composite suspension liquid, under the conditions of 40 DEG C, 3h is stirred to react with the stirring rate of 600rpm/min, after reaction fills suspension
Enter plain edition bag filter, dialyse 48h, and it is compound that freeze-drying obtains polyethyleneimine/carboxylation konjaku glucomannan/graphene oxide
Material.
Through detecting: observing that porous state is presented in product by scanning electron microscope.Fourier's infrared test distinguishes table
Contain polyethyleneimine and carboxylation konjak portuguese gansu polyose saccharic composition in bright composite material, the test of Fourier's Raman shows composite hydrogel
In contain graphite oxide olefinic constituent.Polyethyleneimine/carboxylation konjaku glucomannan/graphene oxide composite material character is stablized,
With excellent heavy metal ion adsorbed performance.
Embodiment 3
Under (1) 20 DEG C of water bath condition, weighs 8g konjak portuguese gansu polyose Icing Sugar and swell in 50mL dehydrated alcohol and make solvent, stir molten
Swollen 30 minutes.It weighs 5g monoxone and is dissolved in 10mL absolute ethyl alcohol and stirring to dissolution.In the mechanical stirring rate of 200rpm/min
Under the conditions of, by monoxone-dehydrated alcohol with the drop rate of 1mL/min, it is slowly added dropwise in reaction solution, it is lasting to be mixed
3h.System is warming up to 55 DEG C after 3h, pH value of solution is adjusted to 9 with saturation sodium hydroxide alcoholic solution, reaction stirring 3h.It will after 3h
Reaction solution pours into beaker, is washed to solution and is in neutrality repeatedly with ethyl alcohol.Oven temperature is adjusted to 55 DEG C, by reactants dry
12h obtains the sweet glycan of product carboxylation konjaku Pu.
(2) it weighs 1.5g polyethyleneimine to be dissolved in 5mL deionized water, ultrasonic 2h forms uniform polyethyleneimine
Aqueous solution.
(3) 2.5g carboxylation konjaku glucomannan powder is swollen in 100mL aqueous solution, forms uniform carboxylation konjaku Portugal
Sweet water solution.Above-mentioned aq. polyethyleneimine is added dropwise to konjak portuguese gansu polyose sugar aqueous solution with the rate of 1mL/min, and
1mL glutaraldehyde solution is added.Under the conditions of 20 DEG C, 2h is stirred to react with the stirring rate of 500rpm/min, reaction stops being gathered
Aziridine/carboxylation konjaku glucomannan binary composite suspension liquid.
(4) at room temperature, 4mg graphene oxide is added in the water of 10mL, ultrasonic disperse forms graphene oxide dispersion
Graphene oxide dispersion solution is added dropwise to above-mentioned polyethyleneimine/carboxylation konjaku glucomannan with the rate of 1mL/min by solution
In composite suspension liquid, under the conditions of 20 DEG C, 3h is stirred to react with the stirring rate of 500rpm/min, after reaction fills suspension
Enter plain edition bag filter, dialyse 48h, and it is compound that freeze-drying obtains polyethyleneimine/carboxylation konjaku glucomannan/graphene oxide
Material.
Through detecting: observing that porous state is presented in product by scanning electron microscope.Fourier's infrared test distinguishes table
Contain polyethyleneimine and carboxylation konjak portuguese gansu polyose saccharic composition in bright composite material, the test of Fourier's Raman shows composite hydrogel
In contain graphite oxide olefinic constituent.Polyethyleneimine/carboxylation konjaku glucomannan/graphene oxide composite material character is stablized,
With excellent heavy metal ion adsorbed performance.
It is above-mentioned provided by embodiment be schematically and not restrictive, those of ordinary skill in the art understand the present invention
To the improvement or transformation of the progress such as the dosage of reaction raw materials, time, production scale on the basis of connotation, the present invention is belonged to
Scope of protection of the claims.
Claims (10)
1. a kind of preparation method of the trielement composite material based on polyethyleneimine, which is characterized in that use solution blended process will
Polyethyleneimine is immobilized on carboxylation konjaku glucomannan, then combined oxidation graphene again, and polyethyleneimine/carboxylic is prepared
Change konjaku glucomannan/graphene oxide composite material.
2. a kind of preparation method of trielement composite material based on polyethyleneimine according to claim 1, feature exist
In: specifically includes the following steps:
(1) solvent is made with dehydrated alcohol, adjusts solvent pH with sodium hydroxide, dissolves konjaku glucomannan, monoxone, use monoxone
Deacetylated and carboxymethyl-modification is carried out to konjaku glucomannan, is dried to obtain carboxylation konjaku glucomannan；
(2) polyethyleneimine is dissolved in deionized water, and ultrasonic treatment obtains aq. polyethyleneimine；
(3) the resulting carboxylation konjaku glucomannan of step (1) is soluble in water, form carboxylation konjak portuguese gansu polyose sugar aqueous solution；It will
Step (2) resulting aq. polyethyleneimine is added dropwise in konjak portuguese gansu polyose sugar aqueous solution, and glutaraldehyde solution is added, stirring
Reaction, obtains polyethyleneimine/carboxylation konjaku glucomannan binary composite suspension liquid；
(4) it adds graphene oxide into water, ultrasonic disperse forms graphene oxide and disperses solution, graphene oxide is dispersed molten
Liquid is added in step (3) resulting polyethyleneimine/carboxylation konjaku glucomannan composite suspension liquid, mechanic whirl-nett reaction, reaction
After obtain polyethyleneimine/carboxylation konjaku glucomannan/graphene oxide composite material.
3. a kind of preparation method of trielement composite material based on polyethyleneimine according to claim 2, feature exist
In: step (1) sodium hydroxide adjusts solvent pH to 7~10；Dehydrated alcohol, konjaku glucomannan, chloroacetic mass ratio are 6
~10:40~70:3~10.
4. a kind of preparation method of trielement composite material based on polyethyleneimine according to claim 2, feature exist
In: the reaction condition of step (1) are as follows: reaction temperature is 30~70 DEG C；Mechanical stirring rate is 200~600rpm/min；Reaction
Time is 1~6 hour；Drying temperature is 10~70 DEG C.
5. a kind of preparation method of trielement composite material based on polyethyleneimine according to claim 2, feature exist
In: the relative molecular mass of polyethyleneimine described in step (2) is 600~70000；The quality of aq. polyethyleneimine point
Number is 2%~30%.
6. a kind of preparation method of trielement composite material based on polyethyleneimine according to claim 2, feature exist
In: the mass fraction of carboxylation konjak portuguese gansu polyose sugar aqueous solution described in step (3) is 1%~10%.
7. a kind of preparation method of trielement composite material based on polyethyleneimine according to claim 2, feature exist
In: the volume ratio of polyethylenimine solution described in step (3), konjak portuguese gansu polyose sugar juice, glutaraldehyde solution are as follows: 4~10:50
~100:1~10.
8. a kind of preparation method of trielement composite material based on polyethyleneimine according to claim 2, feature exist
In: the condition of the reaction of step (3) are as follows: reaction temperature is no more than 50 DEG C；Mechanical stirring rate is 200~600rpm/min；Instead
It is 1~6 hour between seasonable.
9. a kind of preparation method of trielement composite material based on polyethyleneimine according to claim 2, feature exist
In: the mass fraction of graphene oxide water solution described in step (4) is 0.01%~1%；The ultrasonic disperse is formed
Graphene oxide disperses in solution, and ultrasonic power is 200~400w, and the time is 1~3h；The condition of reaction are as follows: reaction temperature is not
More than 50 DEG C；Mechanical stirring rate is 200~600rpm/min；Reaction time is 1~6 hour.
10. a kind of trielement composite material based on polyethyleneimine, it is characterised in that: using the preparation of any one of claims 1 to 9
Obtained by method.
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| CN116764607A (en) * | 2023-08-25 | 2023-09-19 | 成都中核高通同位素股份有限公司 | Modified adsorption resin and application thereof in separating calcium and scandium |
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Application publication date: 20190618 |