CN110327895A - A kind of graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material and its preparation method and application - Google Patents
A kind of graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material and its preparation method and application Download PDFInfo
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- CN110327895A CN110327895A CN201910493371.0A CN201910493371A CN110327895A CN 110327895 A CN110327895 A CN 110327895A CN 201910493371 A CN201910493371 A CN 201910493371A CN 110327895 A CN110327895 A CN 110327895A
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- C02F1/00—Treatment of water, waste water, or sewage
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- 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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Abstract
A kind of graphene oxide of the invention/calcium alginate Supported Melamine sponge composite adsorbing material and its preparation method and application, belongs to the technical field of adsorbent material, the adsorbent material the preparation method is as follows: 1) preparing graphene oxide solution;2) sodium alginate is added into graphene oxide solution, stirs to obtain gel solution;3) it after being pre-processed melamine sponge, is sufficiently impregnated in gel solution, drying obtains graphene oxide/sodium alginate Supported Melamine sponge compound later;4) graphene oxide/sodium alginate Supported Melamine sponge compound is immersed in calcium salt soln, it carries out obtaining graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material after constant temperature oscillation, washing, drying, it is a kind of composite material with high absorption property, application field is relatively broad, can be applied to the absorption of metal ion and heavy metal ion in pollutant effluents.
Description
Technical field
The invention belongs to the technical fields of adsorbent material, more particularly to a kind of graphene oxide/calcium alginate load three
Poly cyanamid sponge composite adsorbing material and its preparation method and application.
Background technique
Heavy metal enters water environment by sources such as plating, mining, metallurgy, because of its not biodegradable, high toxicity,
Heavy metal pollution has become one of the environmental problem of most serious in the world.The processing method of heavy metal wastewater thereby mainly has chemistry heavy
Shallow lake method, absorption method, membrane filter method, ion-exchange etc..Absorption method is considered as most having application because its is inexpensive, efficient, easy to operate
The heavy metal waste water treatment process of prospect.However, there are still following problems for current adsorbent: (1) adsorbent preparation process is numerous
It is trivial, toxic compounds are commonly used in preparation process.Therefore it is necessary to which development cost is cheap, preparation is easy, environmentally friendly
Adsorbent;(2) high-efficiency adsorbent studied extensively at present mainly exists with powder morphology, in actual waste water treatment process, this
It will lead to adsorbent to be difficult to recycle.
For graphene oxide as a kind of nano-carbon material, a large amount of oxygen-containing groups are contained on surface, in terms of wastewater treatment if any
Good application prospect is shown in terms of machine Dye Adsorption, heavy metal adsorption.But graphene oxide is good water-soluble because having
Property, it is difficult to be separated from the water out after absorption;In addition, being easy to appear between graphene sheet layer tight due to the effect of Van der Waals force
The reunion of weight.Sodium alginate is a kind of natural polysaccharide, water-soluble, is rich in carboxyl and hydroxyl, such as by divalent or trivalent ion
Ca2+Etc. its crosslinking and hardening can be made to form adsorbent not soluble in water, being commonly used for chelating adsorbs heavy metal ion, has well
Biological degradability and biocompatibility.But alginate easily expands, bad mechanical strength limits it in terms of wastewater treatment
Using.
Summary of the invention
In view of the above problems, the preparation of composite adsorbing material of the invention stablizes three-dimensional network porous skeleton structure to have
Melamine sponge so that melamine sponge is filled graphene oxide/sodium alginate soln first as carrier, then pass through original
Position gelation reaction makes sodium alginate react generation calcium alginate not soluble in water with calcium chloride solution, obtain graphene oxide/
The composite adsorbing material of calcium alginate Supported Melamine sponge.
Technology contents of the invention are as follows:
The purpose of the present invention is to provide a kind of graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material,
Its structure is that graphene oxide/calcium alginate is carried in the three-dimensional network skeleton of melamine sponge, the graphene oxide/
Calcium alginate riddles in the hole of melamine sponge;
The structure of the graphene oxide/calcium alginate is that graphene oxide is embedded in calcium alginate.
The present invention also provides a kind of graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material applications
In the absorption of metal ion and the processing of heavy metal polluted waste water.
The present invention also provides a kind of graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material systems
Preparation Method includes the following steps:
1) graphene oxide solution is prepared;
2) sodium alginate is added into graphene oxide solution, gel solution is made after stirring;
3) it after taking melamine sponge to be pre-processed, is sufficiently impregnated in gel solution, is dried to obtain oxidation stone later
Black alkene/sodium alginate Supported Melamine sponge predecessor;
4) graphene oxide/sodium alginate Supported Melamine sponge predecessor is immersed in calcium salt soln, progress constant temperature oscillation,
Graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material is obtained after washing, drying;
Further, calcium salt soln described in step 4) includes CaCl2Solution, the CaCl2The mass fraction range of solution is
4%~6%;After the constant temperature oscillation, takes out sponge compound and washed and dried again;
Pretreatment described in step 3) is 80 DEG C of drying after cleaning melamine sponge with ethyl alcohol;In step 3) and step 4)
The temperature range of the drying is 60 DEG C ~ 80 DEG C.
Wherein, the method for preparation graphene oxide solution described in step 1) is as follows:
A. the concentrated sulfuric acid, phosphoric acid and crystalline flake graphite mixing are taken, is stirred evenly;
B. it is slowly added to potassium permanganate, heated at constant temperature and is sufficiently stirred later, obtains mixture A;
C. after reaction, mixture A temperature is down to room temperature;
D. deionized water and mixed solution of hydrogen peroxide are frozen into ice cube, mixture A is poured into ice cube, is stirred evenly, is obtained
Mixture B;
E. it by mixture B centrifuge washing, is freeze-dried centrifugation object to obtain solid oxidation graphite, by its ultrasonic disperse in deionization
In water, centrifuging and taking supernatant is graphene oxide solution;
Further, it is slowly added to control its temperature during potassium permanganate in step b at 35 DEG C ~ 40 DEG C, described in step e
Centrifuge washing include using reagent 5% hydrochloric acid solution, wash to centrifugate supernatant liquor can not with saturation barium chloride solution
Detect SO4 2-;It is washed with deionized again, until its supernatant liquor can not use the AgNO of 1 mol/L3Solution detects Cl-1。
Beneficial effects of the present invention are as follows:
Graphene oxide of the invention/calcium alginate Supported Melamine sponge adsorbent material has copper ion in water excellent
Absorption property, and the adsorbent material have good hydrophily, be a kind of composite material with high absorption property, to other
Metal ion such as Pb2+、Hg2+、Cd2+Also there is preferable absorption property, have and easily recycle, is reusable, high absorption property
Feature, application field is relatively broad, can be applied to the absorption of metal ion and heavy metal ion in pollutant effluents;
Graphene oxide/calcium alginate is carried on melamine sponge by the present invention, and metal ion species height can be prepared
Imitate adsorbent.Using melamine sponge as carrier, the expansion of calcium alginate can be effectively suppressed, improve the mechanical performance of adsorbent;
Secondly, what the present invention was prepared is macroscopic body adsorbent, in actual waste water treatment process, it is easy recycling;In addition, oxidation stone
Black alkene/calcium alginate Supported Melamine sponge composite material and preparation method thereof is simple, and agents useful for same is environmentally friendly, adsorbent
Preparation cost is low, is expected to be mass produced, and efficiently solves existing adsorbent there are absorption properties that low, powder sorbent is difficult to back
It receives, the problems such as preparation process is cumbersome.
Detailed description of the invention
Fig. 1 is melamine sponge, graphene oxide/calcium alginate Supported Melamine sponge pictorial diagram;
Fig. 2 is graphene oxide/calcium alginate Supported Melamine sponge scanning electron microscope (SEM) photograph;
Fig. 3 is graphene oxide/calcium alginate-melamine sponge microscopic appearance enlarged drawing;
Fig. 4 is melamine sponge, graphene oxide/calcium alginate Supported Melamine sponge absorption property figure.
Specific embodiment
Below by way of specific case study on implementation and Detailed description of the invention, the present invention is described in further detail, it should be understood that this
Embodiments are merely to illustrate of the invention without limiting the scope of the invention a bit, after the present invention has been read, this field skill
It is as defined in the appended claims that art personnel fall within the application to the modification of various equivalent forms of the invention.
If all raw materials and reagents of the invention are the raw material of conventional market, reagent without specified otherwise.
Embodiment 1
A kind of graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material the preparation method is as follows:
1) graphene oxide solution is prepared:
A. by the dense H of 360 mL2SO4With 40 mL H3PO4It successively pours into the three neck round bottom of 1 L, is slow added into 3.0 g
Crystalline flake graphite, mechanical stirring is uniform, and control revolving speed is 500 r/min;
B. under mechanical stirring, 18.0 g potassium permanganate are slowly added to be placed in round-bottomed flask after potassium permanganate all adds
In 50 DEG C of constant temperature oil baths, 12 h of mechanical stirring;
C. after reaction, round-bottomed flask is taken out, is down to room temperature to it;
D. the beaker equipped with 400 ml deionized waters and 3 ml mixed solution of hydrogen peroxide is placed in refrigerator, mixed solution is cold
It is frozen into ice cube;Solution in round-bottomed flask after reaction is poured into the above-mentioned beaker equipped with deionized water and hydrogen peroxide ice cube
In, it is stirred evenly with glass bar;
E. after the multiple centrifuge washing of hydrochloric acid solution (10000 r/min, every time 5 min) for being 5% by said mixture content again
With deionized water centrifuge washing 8 ~ 10 times;By the graphite oxide freeze-drying after centrifuge washing, solid oxidation graphite is obtained;Accurately
The solid oxidation graphite for weighing 200 mg, by its ultrasonic disperse in 100 ml deionized waters, then 3000 in low speed centrifuge
Rpm is centrifuged 30min, takes supernatant liquor, obtains the graphene oxide solution that concentration is 2 mg/mL;
2) 0.4 g sodium alginate is added into 20 ml graphene oxide solutions, stirs to obtain gel solution;
3) melamine sponge (2 × 2 × 0.5 cm is taken3) pre-processed, i.e., after melamine sponge being cleaned with ethyl alcohol, 80
DEG C drying, is sufficiently impregnated in above-mentioned gel solution 12h, gel solution is made to enter aperture inside sponge, dry at 60 DEG C later
Obtain graphene oxide/sodium alginate-melamine sponge predecessor;
4) graphene oxide/sodium alginate-melamine sponge predecessor is immersed into 4wt%CaCl2In solution, in constant temperature oscillation
React 6 h in device, then sponge block taken out, after being washed with deionized several times, be dried to obtain in 60 DEG C of baking ovens graphene oxide/
Calcium alginate Supported Melamine sponge composite adsorbing material.
Embodiment 2
A kind of graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material the preparation method is as follows:
1) gel solution that step 2 obtains in Example 1;
2) melamine sponge (2 × 2 × 0.5 cm is taken3) pre-processed, i.e., after melamine sponge being cleaned with ethyl alcohol, 80
DEG C drying, is sufficiently impregnated in above-mentioned gel solution 12h, gel solution is made to enter aperture inside sponge, dry at 70 DEG C later
Obtain graphene oxide/sodium alginate-melamine sponge predecessor;
3) graphene oxide/sodium alginate-melamine sponge predecessor is immersed into 5wt%CaCl2In solution, in constant temperature oscillation
React 6 h in device, then sponge block taken out, after being washed with deionized several times, be dried to obtain in 70 DEG C of baking ovens graphene oxide/
Calcium alginate Supported Melamine sponge composite adsorbing material.
Embodiment 3
A kind of graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material the preparation method is as follows:
1) gel solution that step 2 obtains in Example 1;
2) melamine sponge (2 × 2 × 0.5 cm is taken3) pre-processed, i.e., after melamine sponge being cleaned with ethyl alcohol, 80
DEG C drying, is sufficiently impregnated in above-mentioned gel solution 12h, gel solution is made to enter aperture inside sponge, dry at 80 DEG C later
Obtain graphene oxide/sodium alginate-melamine sponge predecessor compound;
3) graphene oxide/sodium alginate-melamine sponge compound is immersed into 6wt%CaCl2In solution, in constant temperature oscillation
React 6 h in device, then sponge block taken out, after being washed with deionized several times, be dried to obtain in 80 DEG C of baking ovens graphene oxide/
Calcium alginate Supported Melamine sponge composite adsorbing material.
Fig. 1 be melamine sponge, graphene oxide/calcium alginate Supported Melamine sponge pictorial diagram, can from figure
Find out, the purer melamine sponge of the graphene oxide after drying/calcium alginate Supported Melamine sponge has in volume
Certain diminution, but still good macroscopic body structure is maintained, it is good that three-dimensional sponge skeleton assigns graphene oxide/calcium alginate
Mechanical performance.
Fig. 2 is graphene oxide/calcium alginate-melamine sponge scanning electron microscope (SEM) photograph made from embodiment 1, Cong Tuzhong
As can be seen that graphene oxide/calcium alginate is filled in matrix porosity, this is illustrated using melamine sponge as carrier
Graphene oxide/calcium alginate successfully loads on melamine sponge.
Fig. 3 is graphene oxide/calcium alginate-melamine sponge microscopic appearance enlarged drawing made from embodiment 1.
By graphene oxide/calcium alginate-melamine sponge made from melamine sponge (MS) and embodiment 1
(GO/CA-MS) initial pH=6.0 are respectively placed in, in the copper ion solution that volume is 50 ml, concentration is 100 mg/L, 25 DEG C,
24 h are adsorbed in the constant temperature oscillator that revolving speed is 150 rpm, absorption property is as shown in Figure 4.Melamine sponge (MS) is to copper
The eliminating rate of absorption of ion only has 0.46%, and graphene oxide/calcium alginate-melamine sponge goes the absorption of copper ion
Except rate up to has 81.2%, absorption property is significantly improved, therefore graphene oxide/calcium alginate-three manufactured in the present embodiment
Poly cyanamid sponge is the high-efficiency adsorbent of a kind of pair of metal ion.
Claims (9)
1. a kind of graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material, which is characterized in that its structure is
Graphene oxide/calcium alginate is carried in the three-dimensional network skeleton of melamine sponge, the graphene oxide/calcium alginate
In the hole for riddling melamine sponge.
2. by graphene oxide described in claim 1/calcium alginate Supported Melamine sponge composite adsorbing material, feature
It is, the structure of the graphene oxide/calcium alginate is that graphene oxide is embedded in calcium alginate.
3. a kind of graphene oxide of any of claims 1 or 2/calcium alginate Supported Melamine sponge composite adsorbing material is answered
For the absorption of metal ion and the improvement of heavy metal polluted waste water.
4. a kind of graphene oxide of any of claims 1 or 2/calcium alginate Supported Melamine sponge composite adsorbing material
Preparation method, which is characterized in that include the following steps successively to carry out:
1) graphene oxide solution is prepared;
2) sodium alginate is added into graphene oxide solution, gel solution is made after stirring;
3) it after melamine sponge is pre-processed, is sufficiently impregnated in gel solution, is dried to obtain graphite oxide later
Alkene/sodium alginate Supported Melamine sponge predecessor;
4) graphene oxide/sodium alginate Supported Melamine sponge predecessor is immersed in calcium salt soln, progress constant temperature oscillation,
Graphene oxide/calcium alginate Supported Melamine sponge composite adsorbing material is obtained after washing, drying.
5. by the preparation of graphene oxide as claimed in claim 4/calcium alginate Supported Melamine sponge composite adsorbing material
Method, which is characterized in that calcium salt soln described in step 4) includes CaCl2Solution, the CaCl2The mass fraction range of solution
It is 4% ~ 6%.
6. by graphene oxide described in claim 4 or 5/calcium alginate Supported Melamine sponge composite adsorbing material system
Preparation Method, which is characterized in that after constant temperature oscillation described in step 4), take out sponge compound and washed and dried again.
7. by the preparation of graphene oxide as claimed in claim 6/calcium alginate Supported Melamine sponge composite adsorbing material
Method, which is characterized in that dry temperature range described in step 3) and step 4) is 60 DEG C ~ 80 DEG C.
8. by graphene oxide described in claim 4 or 5/calcium alginate Supported Melamine sponge composite adsorbing material system
Preparation Method, which is characterized in that the method for preparation graphene oxide solution described in step 1) is as follows:
A. the concentrated sulfuric acid, phosphoric acid and crystalline flake graphite mixing are taken, is stirred evenly;
B. it is slowly added to potassium permanganate, heated at constant temperature and is sufficiently stirred later, obtains mixture A;
C. after reaction, mixture A temperature is down to room temperature;
D. deionized water and mixed solution of hydrogen peroxide are frozen into ice cube, mixture A is poured into ice cube, is stirred evenly, is obtained
Mixture B;
E. it by mixture B centrifuge washing, is freeze-dried centrifugation object to obtain solid oxidation graphite, by its ultrasonic disperse in deionization
In water, centrifuging and taking supernatant is graphene oxide solution.
9. by graphene oxide according to any one of claims 8/calcium alginate Supported Melamine sponge adsorbent material preparation method,
It is characterized in that, being slowly added to control its temperature in step b during potassium permanganate at 35 DEG C ~ 40 DEG C.
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CN111672487A (en) * | 2020-06-22 | 2020-09-18 | 中国矿业大学 | Selective heavy metal ion adsorption material and preparation method and application thereof |
CN113308088A (en) * | 2021-06-24 | 2021-08-27 | 中国科学院兰州化学物理研究所 | Double-network graphene epoxy composite material and preparation method thereof |
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CN116618030A (en) * | 2023-06-07 | 2023-08-22 | 华东理工大学 | Preparation method of melamine sponge modified adsorbent and application of melamine sponge modified adsorbent in cationic dye wastewater treatment |
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